XPert PRO UG

X’PERT PRO
User’s Guide
The Analytical X-ray Company

X’Pert PRO
X-ray Diffraction System
User’s Guide
EDITION NOTICE: This is the Sixth Edition of this publication.

X’Pert PRO - User’s Guide
ACKNOWLEDGMENTS
All registered and unregistered Trademarks ™, Domain Names and Copyrights © are the property of their
respective owners.
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Copyright © PANalytical B.V. 2007. All rights reserved worldwide. This manual has been provided pursuant to
an agreement containing restrictions on its use. This manual is also covered by Federal Copyright Law and
International Copyright Law. No part of this manual may be copied, distributed, transmitted, stored in a retrieval
system or translated into any human or computer language, in any form or by any other means, electronic,
mechanical, magnetic, manual, or otherwise or disclosure to third parties without the express written permission
of PANalytical B.V.
DISCLAIMER
This manual is supplied by PANalytical B.V. on an as is basis, under a non-exclusive licence, authorizing the
manual’s use solely for and in conjunction with the products supplied by PANalytical B.V. terms and conditions
of sale, governing the contract of sale for the products supplied. Further, PANalytical B.V. reserves the right to
revise or change this manual without the obligation to notify any person or organization of such revision or
change.
This instrument complies with the requirements for CE marking and is manufactured by:
PANalytical B.V.
Lelyweg 1
7602 EA Almelo
The Netherlands
Tel: +31 546 534444
Fax: +31 546 534577
Internet: http://www.PANalytical.com
PAGE ii 07.03.27
General Pages
Contents
Part I General
Chapter 1 Introduction to X’Pert PRO
Chapter 2 Safety
Chapter 3 Applications and Optics
Chapter 4 General Operations
Chapter 5 General Maintenance
Chapter 6 Fault Correction
Part II Components
Chapter 1 X-ray Tubes
Chapter 2 Beam Attenuators and Filters
Chapter 3 Incident Beam Slits
Chapter 4 Incident Beam Masks
Chapter 5 Soller Slits
Chapter 6 X-ray Mirrors
Chapter 7 Incident Beam Monochromators
Chapter 8 Incident Beam Collimators
Chapter 9 X-ray Lenses
Chapter 10 Mono-capillaries
Chapter 11 MRD Cradle
Chapter 12 Platforms for Horizontal and Vertical Systems
Chapter 13 Non-ambient Chambers
Chapter 14 Beam Knives
Chapter 15 Sample Changers
Chapter 16 Diffracted Beam Slits
Chapter 17 Diffracted Beam Masks
Chapter 18 Diffracted Beam Collimators
Chapter 19 Diffracted Beam Monochromators
Chapter 20 Anti-scatter Devices
Chapter 21 Detectors
Appendix A Sample Holders
Appendix B Sample Preparation
Appendix C X-ray Topography
07.03.27 Page iii

X’Pert PRO - User’s Guide
PAGE iv 07.03.27
Part I
Chapter 1
Introduction to X’Pert PRO
Contents
1.1 General................................................................................................................................. 1 - 3
1.2 How to Read this Guide...................................................................................................... 1 - 3
1.3 Basics of the X’Pert PRO X-ray Diffraction System ....................................................... 1 - 4
1.3.1 The PreFIX Concept............................................................................................................... 1 - 5
1.4 PW3040/60 X’Pert PRO Instrument Enclosure .............................................................. 1 - 6
1.4.1 Working Environment............................................................................................................ 1 - 6
1.4.2 X-rays ON Lamp .................................................................................................................... 1 - 7
1.4.3 Instrument Enclosure Lower Part........................................................................................... 1 - 7
1.4.4 Control and Display Panel...................................................................................................... 1 - 7
1.4.5 High Tension Generator ......................................................................................................... 1 - 8
1.4.6 Accessories............................................................................................................................. 1 - 8
1.4.6.1 Tube Shield ............................................................................................................ 1 - 8
1.4.6.2 High Tension Cable ............................................................................................... 1 - 9
1.4.6.3 Cooling System.................................................................................................... 1 - 10
1.4.6.4 Tube Support Stand ............................................................................................. 1 - 10
1.4.6.5 Filter Slit Puller.................................................................................................... 1 - 10
1.4.6.6 Pipette .................................................................................................................. 1 - 11
1.4.6.7 Tube of Silicon Grease ........................................................................................ 1 - 11
1.4.6.8 Silicon Disk.......................................................................................................... 1 - 11
1.4.6.9 Fluorescence Disk................................................................................................ 1 - 11
1.4.6.10 Single Knife Edge ................................................................................................ 1 - 11
1.4.6.11 Copper Attenuation Foils..................................................................................... 1 - 12
1.4.6.12 Bottle of Oil ......................................................................................................... 1 - 12
1.4.6.13 Chamois Leather .................................................................................................. 1 - 12
1.4.6.14 Set of Tools .......................................................................................................... 1 - 12
1.4.6.15 PW3096/60 Second Diffracted Beam PreFIX Carrier......................................... 1 - 12
1.4.6.16 PW3132/61 Reference Samples for Stress and Texture Measurements.............. 1 - 13
1.4.6.17 PW3132/62 Reference Samples for High Resolution and Reflectivity ............... 1 - 14
1.4.6.18 PW3719/10 Display Unit..................................................................................... 1 - 14
continued on next page
07.03.27
X’Pert PRO System - User’s Guide
1.5 PW3050/6x X’Pert PRO Goniometer..............................................................................1 - 15

1.5.1 PW3050/60 X’Pert PRO Standard Resolution Goniometer ................................................. 1 - 15
1.5.2 PW3050/65 X’Pert PRO High Resolution Goniometer ....................................................... 1 - 15
1.6 Basic X-ray Diffraction Systems in X’Pert PRO............................................................1 - 15
1.6.1 Horizontal X’Pert PRO Systems .......................................................................................... 1 - 15
1.6.1.1 X’Pert PRO MRD Systems .................................................................................. 1 - 15
1.6.1.2 X’Pert PRO Extended MRD Systems.................................................................. 1 - 16
1.6.2 Vertical X’Pert PRO Systems...............................................................................................1 - 19
1.6.2.1 X’Pert PRO MPD Theta-Theta Systems.............................................................. 1 - 19
1.6.2.2 X’Pert PRO MPD Omega-2Theta Systems ......................................................... 1 - 20
1.6.2.3 X’Pert PRO Alpha-1 System ............................................................................... 1 - 21
1.7 Terms Used in this Guide .................................................................................................1 - 22
1.8 References ..........................................................................................................................1 - 23
Page 1.2 07.03.27

Part I - Chapter 1: Introduction to X’Pert PRO
1.1 GENERAL
The PANalytical X’Pert PRO X-ray diffraction system is the basic platform for a wide variety of applications
in analytical X-ray diffraction, in both scientific and industrial research environments. These applications
comprise:
• Phase analysis of samples with flat or irregular surfaces; of thin films, and of samples in glass capillaries.
• Quantitative phase analysis on batches of samples.
• Crystallography and Rietveld analysis on samples with flat or irregular surfaces; or powder samples in
glass capillaries.
• Residual stress analysis of flat samples or irregularly shaped materials.
• Reflectometry on thin layers and substrate materials.
• High resolution rocking curve analysis, reciprocal space mapping and X-ray topography on (epitaxial)
layers on single crystal substrates.
• Texture analysis on all kinds of materials with a preferred orientation of the crystallites.
• Analysis of small spots on inhomogeneous samples.
• In-plane diffraction on thin films.
• Transmission measurements through (samples between) foils.
• Analysis of changes in the crystal structure in changing environmental conditions.
• High-throughput X-ray diffraction for automated analyses of large numbers of samples.
The modular design of X’Pert PRO utilizing the PreFIX concept makes it possible to perform more than one
type of analysis on one system.
PreFIX enables you to re-configure the system from one application setup to another within a few minutes
without the need for additional system alignment.
1.2 HOW TO READ THIS GUIDE

This X’Pert PRO User’s Guide gives you an overview of the diffraction system and its applications. It provides
you with sufficient information to enable you to operate and maintain the system safely and efficiently.
This Guide is in two parts:
Part I: This part of the Guide provides all the general information about the system and its use,
including safety information. It also describes the system concepts (what optical modules you
need for a certain application), system operations and general maintenance.
Part II: This part of the Guide provides a chapter for each of the component groups in the diffraction
system from the X-ray tube through to the X-ray detector.
Each chapter provides information about the applications in which this type of component
could (or should) be used in, how to install and use the component; and how to use it together
with other products such as beam masks and slits and so on.
If it is relevant the chapter lists the different kinds of module available to you (for example:
in the chapter about incident beam monochromators it describes the three sorts of
monochromator that are available: high-resolution monochromators, focusing beam
Johansson monochromators, or hybrid monochromators).
07.03.27 Page 1.3

1.3 BASICS OF THE X’PERT PRO X-RAY DIFFRACTION SYSTEM

The X’Pert PRO X-ray diffraction system basically consists of the following items:
• A PW3040/60 Instrument Enclosure which provides the working environment for the X’Pert PRO
system; it includes measuring and control electronics using a microprocessor system, and a high tension
generator. This instrument enclosure is described in section 1.4 of this chapter.
• A PW3050/6x Goniometer; the central part of the diffractometer. This goniometer is described in section
1.5 of this chapter.
• A ceramic diffraction X-ray tube mounted onto the goniometer in a tube shield. X-ray tubes are described
in Chapter 1 in Part II of this User’s Guide.
• Optical modules for the incident and the diffracted X-ray beams. These modules can be mounted on
PreFIX positions on the goniometer’s arms. Incident beam modules are described in Chapters 2 - 10 in
Part II of this User’s Guide; diffracted beam modules are described in Chapters 16 - 20.
• A sample stage on which to mount a sample so that its characteristics can be measured. Sample stages
and their accessories are described in Chapters 11 - 15 in Part II of this User’s Guide.
• A detector to measure the intensity of the diffracted X-ray beam. Detectors are described in Chapter 21 in
Part II of this User’s Guide.
Figure 1.1: PW3040/60 X’Pert PRO Instrument Enclosure
Page 1.4 07.03.27

1.3.1 The PreFIX Concept

A large variety of optical and sample handling accessories for use with the X’Pert PRO system are designed
according to the PreFIX concept of modular exchange of functional components.
PreFIX stands for: Pre-aligned Fast Interchangeable X-ray modules. The basic principle of the PreFIX concept
is that the only item that may need adjusting is the tube height. When the tube is correctly positioned with respect
to the diffraction plane, no further system alignment is required.
PreFIX modules and accessories are factory aligned, which means that they can be dismounted from the system
and then mounted again without the need for system alignment by the user. This means that it is possible to re-
configure the system from one application specific setup to another in minutes.
Alignment of PreFIX components is goniometer specific. This means that when a certain PreFIX module is
factory aligned for a specific X’Pert PRO goniometer, it IS NOT aligned for use on any other X’Pert PRO
goniometer.
The PreFIX concept comprises:
• Rotation of the X-ray tube between line focus and point focus positions and back. Only in certain cases,
for instance: when the tube is changed to the line focus position, or when it is used in combination with
an X-ray mirror or a hybrid monochromator, we advise you to check the tube height position. Procedures
for tube rotation, tube height alignment check and adjustment are given in section 1.4.9 of Chapter 1 in
• Re-positioning of the X-ray tube in the X’Pert PRO Alpha-1 system, from the standard X-ray tube posi-
tion to the alpha-1 position in front of the incident beam Johansson monochromator and vice versa. This
tube re-positioning procedure is described in section 7.3.3.2 of Chapter 7 in Part II of this User’s Guide.
• Re-positioning of the X-ray tube in the X’Pert PRO Extended MRD system, from the standard X-ray
tube position to the extended position and back again. When the tube is mounted in the extended position
it is possible to mount an X-ray mirror and a high-resolution monochromator behind each other. This
option is only available on the extended arm of the X’Pert PRO Extended MRD system which is
described in section 1.6.1.2 of this chapter. The procedure for changing the tube shield position is
described in section 1.4.8 of Chapter 1 in Part II of this User’s Guide.
• Installation and locking into position of incident beam optical modules on the incident beam PreFIX
position. Incident beam optical modules include a shutter lever to close the X-ray safety circuit.
Mounting of incident beam PreFIX modules is described in Chapter 4 in Part I of this User’s Guide.
Maintenance of PreFIX modules is described in Chapter 5 in Part I of this User’s Guide.
• Mounting of sample stages onto the PreFIX stage interface on the X’Pert PRO goniometer. The only
exception to this is the PW3060/20 MRD Cradle used with the X’Pert PRO MRD system, this cradle is
factory fixed to the goniometer and cannot be removed. Exchanging sample stages is described in
Chapters 12 and 13 in Part II of this User’s Guide; standard stages in section 12.1.1, the stage for high-
throughput diffraction in section 12.15.2, non-ambient chambers in section 13.2.1.1, the temperature
controlled humidity chamber in section 13.3.2.2 and the cryogenic samples stages in sections 13.4.2.2
and 13.5.2.1.
• Mounting of diffracted beam optical modules onto the 2theta arm of the goniometer. It is possible to
have a second diffracted beam PreFIX position available on the 2theta arm, this allows two different
modules to be used in the diffracted beam path in the same configuration. Mounting of diffracted beam
PreFIX modules is described in Chapter 4 in Part I of this User’s Guide. Maintenance of PreFIX modules
is described in Chapter 5 in Part I of this User’s Guide.
• Inserting of detectors into the detector interface on the diffracted beam modules. The exceptions to this
are the X’Celerator and the PIXcel used as a line detector, which are mounted onto PreFIX interfaces so
that they can be mounted directly on the diffracted beam PreFIX position. Detectors are described in
Chapter 21 in Part II of this User’s Guide.
• Installation of sample changers, used in X’Pert PRO MPD systems for the automatic loading and unload-
ing of samples onto and from the sample spinner. Sample changers are PreFIX mounted onto the floor of
the PW3040/60 enclosure. When they are not in use they can be moved from their position in front of the
goniometer. Re-positioning the sample changer back in its PreFIX position in front of the goniometer is
achieved without the need for further alignment. Sample changers are described in Chapter 15 in Part II
of this User’s Guide.
07.03.27 Page 1.5
1.4 PW3040/60 X’PERT PRO INSTRUMENT ENCLOSURE

The PW3040/60 Instrument Enclosure provides the working environment for an X’Pert PRO X-ray diffraction
system. It is shown in Figure 1.1. The instrument enclosure comprises two major parts: an upper part and a lower
part. The upper part of the instrument enclosure contains an X’Pert PRO diffractometer. An X-rays ON warning
lamp is fitted on top of the enclosure. The lower part contains the power supplies, measuring and control
electronics using a microprocessor, and a high tension generator. Two 19 inch racks, accessible from the front
of the system are available for the mounting of control units for non-ambient chambers and special detectors. A
control and display panel is fitted on the front of the lower part of the instrument enclosure.
Technical details of the PW3040/60 Instrument Enclosure are given in Table 1.1.
Table 1.1: PW3040/60 X’Pert PRO Instrument Enclosure - Technical Specifications
Item Specification
Mains supply 200 - 240 V, single phase, 50 or 60 Hz

Maximum loading current 45 A
System dimensions 1975 mm x 1132 mm x 1371 mm

(height x depth x width)
System weight 11000 N to 12500 N, depending on the system configuration
Maximum floor loading 3200 kN/m2 (3.2 MPa) on the system’s four feet,
12.8 kN/m2 (12.8 kPa) average floor pressure
1.4.1 Working Environment

The working environment, which forms the upper part of the PW3040/60 Instrument Enclosure, is constructed
from steel. Those parts of the enclosure in the direct X-ray beam are 12 mm thick. Access to the inner part of the
enclosure is via two fully interlocking sliding doors at the front of instrument enclosure. The windows in the
sliding doors are made of lead glass with an X-ray absorption equivalent to 1 mm of lead.
WARNING
IF EITHER OF THE WINDOWS IS BROKEN, SWITCH THE SYSTEM OFF
IMMEDIATELY.
Access to the instrument enclosure from the rear is provided by two hinged doors. All of the doors, front and
rear, have microswitches fitted in order to prevent accidents. As a safety measure, the tube shield shutters cannot
be opened if the doors are not securely closed. An additional safety precaution is that the enclosure doors cannot
be opened if the tube shield shutter is open, when the system is moving, or being initialized. The X’Pert PRO
safety circuits are described in detail in Chapter 2 in Part I of this User’s Guide.
The construction conforms with the most stringent X-ray safety standards: the absorbed dose equivalent rate is
less than 1 μSv/h at 10 cm distance from the outside surface of the enclosure.
The instrument enclosure contains sufficient room for an X’Pert PRO system. Two interior inspection lamps are
fitted inside the enclosure. The lights can be switched on and off with the “Lights” button on the control and
display panel. Replacement of these lamps is described in section 5.6.1 of Chapter 5 in Part I of this User’s
Guide.
Page 1.6 07.03.27

1.4.2 X-rays ON Lamp

The X-rays ON lamp fitted on the top of the enclosure is lit whenever high tension is applied to the X-ray tube.
It is a “fail safe” lamp and forms part of the safety circuit, so that if the lamp fails, the shutter cannot be opened.
Replacing the X-rays ON lamp is described in section 5.6.2 of Chapter 5 in Part I of this User’s Guide.
1.4.3 Instrument Enclosure Lower Part

The lower part of the instrument enclosure contains the following items:
• Power supply racks.
• Measuring and control electronics using a microprocessor system.
• A high stability 3 kW high tension generator.
• Two 19 inch racks, accessible from the front, where control units for non-ambient chambers and/or
detectors can be mounted.
• Mounting space for a vacuum pump. A connection is provided at the rear of the instrument enclosure to
allow the safe removal of unwanted gases from the outlet of the pump.
• A connector for an external X-RAYS ON lamp.
The panels can be removed from the lower part of the instrument enclosure to allow easy access for service and
maintenance.
This lower part of the instrument enclosure also has a microprocessor cooling fan. Some systems may have an
additional cooling fan for the electronic circuitry. Dust filters in front of these fans must be regularly replaced.
The replacement procedures are described in section 5.5 of Chapter 5 in Part I of this User’s Guide.
1.4.4 Control and Display Panel

The control and display panel is mounted on the front of the lower part of the instrument enclosure. It has four
push-button switches and a key switch. These have indicator lamps associated with them, below the indicator
lamps are five LED displays. The control and display panel is shown in Figure 1.2. The function of the switches
is described in Table 1.2. The information provided by the five LED displays on the panel is listed in Table 1.3.
Figure 1.2: Control and Display Panel
07.03.27 Page 1.7

Table 1.2: Control Panel Switches and their Functions
Indicator
Switch Function
Lamp
Power on To turn the power on. Yes

Standby To turn the high tension generator off. Allows the peripherals to Yes
work without generating X-rays and to switch the interior light
on.
Light To switch the interior inspection lights on and off. No
HT (key) To turn the high tension generator on (if the power is switched Yes
on) or off (irrespective of the system’s current operating state).
Shutter To close the shutters on the tube shield irrespective of the system’s No
close current operating state.
Table 1.3: The LED Displays and their Functions
LED Display Function
θ, 2θ, c/s To display the θ angle, the 2θ angle, or the intensity (in counts per second) of the
X-ray beam measured by the detector. The choice of information displayed is
made in the data collector software.
kV, mA To display the high tension generator high voltage and anode current settings.
Shutter To display the number of the shutter that is currently open, or three dots.
open If the safety circuit is closed (all the doors are correctly closed) and a shutter is
open, that shutter number is displayed.
If the doors are not all closed (correctly), three static dots are shown. The shutter
cannot be opened.
If the system has been given the command to initialize, but one or more of the
doors or rear panels is not correctly closed, or the HT key switch is turned off,
three moving dots are shown. The system cannot be initialized.
1.4.5 High Tension Generator

A high stability high tension generator is built into the lower part of the instrument enclosure. Its maximum
output power is 3 kW, the maximum high voltage is 60 kV and the maximum anode current is 60 mA. The
stability of both the high voltage and the anode current is less than 0.01% per 10% mains fluctuation.
The high tension generator is directly controlled by the data collector software.
1.4.6 Accessories
A large variety of accessories for safe and efficient operation and maintenance of the X’Pert PRO X-ray
diffraction system is included with the PW3040/60 Instrument Enclosure. These accessories are shown in Figure
1.4, they are summarized in this section.
1.4.6.1 Tube Shield

The tube shield which is delivered with the PW3040/60 Instrument Enclosure is especially designed to fit a
PW337x/x0 XRD X’Pert Tube. The tube shield is fitted on the incident beam arm of the PW3050/6x
Goniometer. The tube height adjustment range is 6 mm.
Page 1.8 07.03.27

A shutter assembly is fitted to one of the exit ports. The unused exit ports, which do not have shutter assemblies,
are covered by radiation safety plates.
The shutters on the tube shield can be opened and closed using the data collector software. You can also close
the shutter by using the Shutter close push button switch on the control and display panel (see section 1.4.4).
Pressing this push button overrides any software commands.
The shutter cannot be opened unless both the X-ray safety circuit and the high tension safety circuit are closed
(see section 2.3 of Chapter 2 in Part I of this User’s Guide).
If the X-ray safety circuit is broken for any reason during normal operation the shutter(s) will automatically
close.
In addition, if the HT safety circuit is broken during normal operation the shutter(s) will close and the high
tension generator will automatically switch off.
Installing, removing and rotating the X-ray tube in the tube shield is described in section 1.4 of Chapter 1 in Part
II of this User’s Guide.
1.4.6.2 High Tension Cable

The high tension cable which is delivered with the PW3040/60 X’Pert PRO Instrument Enclosure is designed
to connect the PW337x/x0 XRD X’Pert Tube to the high tension generator in the lower part of the instrument
enclosure. A high tension cable safety plug is attached to the cable.
The tube high tension cable plug is fitted into the X-ray tube and fixed in place by four Allen screws. The tube
and its attached cable can then be inserted into X’Pert PRO system’s tube shield. The high tension cable safety
plug that is attached to the cable must then be plugged into its socket on the tube shield. This closes the high
tension safety circuit; the high tension generator cannot be switched on if the high tension safety circuit is not
closed (see section 2.3 of Chapter 2 in Part I of this User’s Guide).
Figure 1.3: Tube High Tension Cable Plug

07.03.27 Page 1.9
If, for any reason, the high tension safety circuit is broken during normal operation the tube shield shutters will
close and the high tension generator will automatically switch off.
Installing, removing and rotating the X-ray tube in the tube shield is described in section 1.4 of Chapter 1 in Part
1.4.6.3 Cooling System

A water cooling system is supplied with the PW3040/60 Instrument Enclosure. This cooling system is used to
cool the X-ray tube anode during production of X-rays. An uninterrupted cooling water flow of at least 3.5 liter
per minute with a maximum inlet temperature of 35 °C (308 K) is required for effective anode cooling. A safety
switch in the cooling system will switch the high tension generator off if the water flow falls below the required
flow rate.
The cooling water system consists of a water filter assembly with a spare water filter and a hose. Maintenance
of this cooling system is described in section 5.4 of Chapter 5 in Part I of this User’s Guide.
Cooling water conditions are given in section 1.2.5 of Chapter 1 in Part II of this User’s Guide, and in the XRD
X’Pert Tube Instruction Manual [2].
1.4.6.4 Tube Support Stand

The tube support stand is used to securely place the X-ray tube during maintenance so that it cannot easily fall
over. Tube maintenance is described in section 1.4.10 of Chapter 1 in Part II of this User’s Guide.
Figure 1.4: X’Pert PRO General Accessories
1.4.6.5 Filter Slit Puller

A filter slit puller is supplied to help you remove the water filter built into the X-ray tube. Removal and installing
the filter using this filter slit puller is described in section 1.4.10 of Chapter 1 in Part II of this User’s Guide.
Page 1.10 07.03.27

1.4.6.6 Pipette
The pipette supplied with the system is used to insert cleaning fluid into the X-ray tube’s water cooling system.
1.4.6.7 Tube of Silicon Grease

The tip of the X-ray tube’s high tension plug is covered with a film of silicon high tension grease. This film of
grease enhances the contact between the high tension plug and the HT connector on the X-ray tube. The
application of silicon grease during tube installation is described in section 1.4.5 of Chapter 1 in Part II of this
User’s Guide.
1.4.6.8 Silicon Disk

A silicon pressed powder sample with a diameter of 32 mm and a thickness of 2 mm is supplied with the system
to allow standard verification tests with X-rays, it is shown in Figure 1.5. The sample is used to perform the
measurements as described in the Acceptance Test Form delivered with the X’Pert PRO system. This sample is
also used in the worked examples provided in the X’Pert Data Collector Quick Start Guide.
Figure 1.5: Silicon Pressed Powder Sample Figure 1.6: Fluorescence Disk
1.4.6.9 Fluorescence Disk

The fluorescence disk supplied with the X’Pert PRO system has a diameter of 32 mm, it is shown in Figure 1.6.
Some reference lines can be seen on the fluorescent side of the disk. This disk is used in a number of alignment
procedures using X-rays, for instance, the tube height alignment, or alignment of the beam mask holder. When
the disk is irradiated by an X-ray beam an illuminated spot showing the position and size of the X-ray beam can
be seen.
1.4.6.10 Single Knife Edge

The single knife edge shown in Figure 1.7 is supplied together with the X’Pert PRO system so that tube height
alignment can be correctly (and accurately) performed. This single knife edge can be mounted onto the
alignment shaft that contains a spring-loaded sample holder for flat solid samples or samples in a flat holder.
Tube height alignment using the single knife edge is described in section 1.4.9.1.2 in Chapter 1 in Part II of this
User’s Guide. The alignment shaft for X’Pert PRO MRD systems is described in section 11.2.1.2 in Chapter 11
in Part II of this User’s Guide. The alignment shaft for X’Pert PRO MPD systems is described in section 12.10
07.03.27 Page 1.11

Figure 1.7: Single Knife Edge
1.4.6.11 Copper Attenuation Foils

Two copper attenuation foils (with foil thicknesses of 0.1 mm and 0.2 mm) are included with the system. They
are used in a large number of alignment procedures to reduce the intensity of the (direct) X-ray beam in order to
protect the detector. These beam attenuators are described in section 2.2.1 of Chapter 2 in Part II of this User’s
Guide.
1.4.6.12 Bottle of Oil

The polished reference surfaces of the precision locating and locking devices on the PreFIX modules, and the
mounting interfaces of the optical modules, must be regularly coated with a thin film of Shell Tellus 10 oil. This
oil is delivered with the X’Pert PRO system in a small plastic bottle. Refer to section 5.2 of Chapter 5 in Part I
of this User’s Guide for more information about the maintenance of the PreFIX modules.
1.4.6.13 Chamois Leather

A chamois leather dipped in Shell Tellus 10 oil is used to clean the polished reference surfaces on the PreFIX
modules, stages and mounting interfaces. The maintenance of the PreFIX modules is described in section 5.2 of
Chapter 5 in Part I of this User’s Guide.
1.4.6.14 Set of Tools

A set of tools to facilitate the efficient operation and maintenance of the system is delivered with the X’Pert PRO
diffraction system. This set of tools comprises:
• A hexagonal screwdriver in the shape of a T-bar for mounting the PreFIX optical modules.
• A set of 10 Torx keys (T7 - T40).
• Two Torx screwdrivers (T6 and T30).
• An open ended/ring spanner (14 mm).
1.4.6.15 PW3096/60 Second Diffracted Beam PreFIX Carrier

PW3096/60 is a diffracted beam PreFIX carrier which is factory mounted onto the 2theta arm of an X’Pert PRO
goniometer to allow a second diffracted beam PreFIX module to be mounted. It is shown in Figure 1.8. This
PreFIX carrier is standardly mounted at the same goniometer radius as the standard diffracted beam PreFIX
position. It can, if so requested when ordering, be fitted with its distance to the goniometer axis down to 30 mm
less than, or up to 30 mm more than the standard goniometer radius. The actual position and the 2θ angle offset
with respect to the standard PreFIX position are given in the Acceptance Test Form delivered with your system.
Page 1.12 07.03.27

Figure 1.8: PW3096/60 Second Diffracted Beam PreFIX Carrier
1.4.6.16 PW3132/61 Reference Samples for Stress and Texture Measurements

PW3132/61 consists of two reference samples: a stress-free tungsten sample for residual stress measurements,
a rolled copper specimen for texture analysis; and a flat metal plate.
The stress-free tungsten sample consists of tungsten powder sprinkled onto an area 25 mm x 15 mm on a glass
plate with dimensions 35 mm x 25 mm, it is shown together with a flat metal plate in Figure 1.9.
Figure 1.9: Stress-free Tungsten Sample Figure 1.10: Rolled Copper Specimen
This sample can be mounted onto a sample stage for residual stress analysis. Stress measurements according to
the sin2ψ method will show a straight horizontal line, indicating that there is no stress present in the sample. A
flat metal plate with a thickness of 0.1 mm is included to protect the sample from mechanical damage during
sample height adjustment.
The rolled copper specimen is a 22 mm x 22 mm plate with a thickness of 1.5 mm, it is shown in Figure 1.10.
A line is engraved on one side of the plate. This line is perpendicular to the direction in which the sample was
rolled (the rolling direction). When this plate is mounted onto a texture cradle with the engraved line parallel to
the diffraction plane, pole figures showing a rolling texture can be recorded. The rolling or reference direction
(RD) is then in the direction of ϕ = 0º.
07.03.27 Page 1.13

1.4.6.17 PW3132/62 Reference Samples for High Resolution and Reflectivity

PW3132/62 consists of two reference samples; a silicon (111) single crystal for high resolution experiments and
a chromium film for reflectivity experiments.
The Si(111) single crystal is a rectangular piece of silicon single crystal with its surface parallel to the (111)
planes, it is shown in Figure 1.11. The crystal has a surface area 15 mm x 10 mm and is mounted onto a 32 mm
diameter steel plate.
Figure 1.11: Si(111) Single Crystal Figure 1.12: Thin Film Sample
The thin film sample is a 60 mm x 40 mm glass plate onto which a chromium film (between 10 nm and 40 nm
thick) has been applied, it is shown in Figure 1.12. This film was used for the reflectivity measurement shown
on the Acceptance Test Form delivered with the system. It can be used to reproduce this test. It is also used as
an example measurement in the X’Pert Data Collector Quick Start Guide.
1.4.6.18 PW3719/10 Display Unit

PW3719/10 is a display unit enabling the external reading of system parameters, for instance: the actual 2θ angle
and the count rate. It is shown in Figure 1.13. PW3719/10 includes a magnetic bracket to mount the display unit
to the walls or ceiling of the PW3040/60 Instrument Enclosure.
Which of the system parameters are displayed is selected in the data collector software.
Figure 1.13: PW3719/10 Display Unit
Page 1.14 07.03.27

1.5 PW3050/6X X’PERT PRO GONIOMETER

X’Pert PRO X-ray diffraction systems are based on the PW3050/6x Goniometer. The goniometer contains the
basic axes in X-ray diffractometry: the omega and 2theta axes. The X-ray tube, incident beam optics, the sample
stage and the diffracted beam optics including the detector are mounted on specific positions on the goniometer.
Two types of goniometer are used in X’Pert PRO systems: the PW3050/60 Standard Resolution Goniometer,
and the PW3050/65 High Resolution Goniometer.
1.5.1 PW3050/60 X’Pert PRO Standard Resolution Goniometer

The PW3050/60 Standard Resolution Goniometer is used in X’Pert PRO MPD and X’Pert PRO MRD systems.
It can be set up in horizontal or vertical mode.
In the vertical mode the goniometer is configured as a Theta-Theta diffractometer, or as an Omega-2Theta
diffractometer. The goniometer radius is between 130 and 240 mm; depending on the optics and sample stage
used.
In the horizontal mode the goniometer is configured as a Omega-2Theta diffractometer. The goniometer radius
is between 130 and 240 mm, or 320 mm if a PW3060/20 MRD Sample Cradle is mounted.
The actual radius of the goniometer is given on the Acceptance Test Form delivered with the system.
The minimum step size in ω and 2θ is 0.001º and the maximum step size is 1.27º.
The minimum step size and resolution to be used in experiments can be changed in the data collector software.
For the PW3050/60 Standard Goniometer the possible choices are: “Normal resolution (0.001º)” or “Low
resolution (0.005º)”. If you choose a lower resolution mode the generator’s setting times are reduced.
1.5.2 PW3050/65 X’Pert PRO High Resolution Goniometer

The PW3050/65 High Resolution Goniometer is used in X’Pert PRO MRD systems. It is set up in horizontally
as a Omega-2Theta diffractometer with a PW3060/20 MRD Cradle. The goniometer radius is 320 mm.
The minimum step size in ω and 2θ is 0.0001º and the maximum step size is 1.27º.
The PW3050/65 is especially designed for high resolution measurements.
The minimum step size and resolution to be used in experiments can be changed in the data collector software.
For the PW3050/65 High Resolution Goniometer the possible choices are: “High Resolution (0.0001º)”,
“Normal resolution (0.001º)” or “Low resolution (0.005º)”. If you choose a lower resolution mode the
generator’s setting times are reduced.
1.6 BASIC X-RAY DIFFRACTION SYSTEMS IN X’PERT PRO

The X’Pert PRO diffraction systems are set up according to the user’s requirements. Based on the diffractometer
configurations, several X’Pert PRO systems can be discerned. An overview of these basic systems is given in
this section. This overview will enable you to determine which basic type of X’Pert PRO system you have,
which will in turn, help you to follow the correct procedures for the safe and efficient operation of your system.
1.6.1 Horizontal X’Pert PRO Systems

In horizontal X’Pert PRO systems the PW3050/6x Goniometer is positioned horizontally. The equatorial (or
diffraction) plane (the plane set up by the incident and diffracted beams) is also horizontal. The goniometer axes
are placed vertically. All horizontal X’Pert PRO systems are right-handed Omega-2Theta diffractometers.
1.6.1.1 X’Pert PRO MRD Systems

X’Pert PRO MRD (Materials Research Diffractometer) systems are fitted with the PW3060/20 MRD Sample
Cradle. This cradle is fixed to the system and cannot be removed. The X’Pert PRO MRD system is shown in
Figure 1.14.
The goniometer in these systems can be either the PW3050/65 High Resolution Goniometer (minimum step size
in ω and 2θ is 0.0001º) or the PW3050/60 Standard Resolution Goniometer (minimum step size in ω and 2θ is
0.001º). The goniometer radius is 320 mm.
07.03.27 Page 1.15
1.6.1.1.1 X’Pert PRO MRD Systems for In-plane Diffraction

X’Pert PRO MRD (Materials Research Diffractometer) systems which include the 9430 920 04651 Option for
In-plane Diffraction can be used to measure the lattice spacing (d-spacing) between the crystal planes that are
oriented perpendicularly to the sample surface using the in-plane diffraction method. This option is described in
more detail in section 11.2.1.3 of Chapter 11 in Part II of this User’s Guide.
Figure 1.14: X’Pert PRO MRD System
1.6.1.2 X’Pert PRO Extended MRD Systems

X’Pert PRO Extended MRD (Materials Research Diffractometer) systems include not only the PW3060/20
MRD Sample Cradle, but also another unique item: the PW3032/45 Extended Arm. The X’Pert PRO Extended
MRD system is shown in Figure 1.15. A detailed view of the extended arm is shown in Figure 1.16. The X-ray
tube is PreFIX mounted onto this extended arm and can be positioned in one of two positions:
• When the X-ray tube is fitted at the standard position (position 2 in Figure 1.16), the X’Pert PRO
Extended MRD is the same as an X’Pert PRO MRD system.
• When the X-ray tube is fitted at the extended position (position 1 in Figure 1.16), two PreFIX modules
can be fitted in front of the X-ray tube: an X-ray mirror and a high-resolution monochromator.
The distance from the tube focus to the goniometer axis is 320 mm when the tube is at the standard position, and
427 mm when it is at the extended position.
Page 1.16 07.03.27

Figure 1.15: X’Pert PRO Extended MRD System
1.6.1.2.1 X’Pert PRO Extended MRD Systems for In-plane Diffraction

X’Pert PRO Extended MRD systems which include the 9430 920 04651 Option for In-plane Diffraction can be
used to measure the lattice spacing (d-spacing) between the crystal planes that are oriented perpendicularly to
the sample surface using the in-plane diffraction technique. This option is described in more detail in section
11.2.1.3 of Chapter 11 in Part II of this User’s Guide.
07.03.27 Page 1.17

Tube Shield on
PreFIX Unit
X-ray
Mirror
PreFIX
Ge
(220
Ge
)
(220
)
Interface
Ge [220]
Monochromator 1
2 PreFIX
Mounting
Fitment
U-block PreFIX
Locking
PreFIX Screws
Mounting
Platform PA000107
Figure 1.16: PW3032/45 Extended Arm
Page 1.18 07.03.27

1.6.2 Vertical X’Pert PRO Systems

In vertical X’Pert PRO systems the PW3050/60 Standard Resolution Goniometer is positioned vertically. The
equatorial (or diffraction) plane (the plane set up by the incident and diffracted beams) is also vertical. The
goniometer axes are placed horizontally. The vertical X’Pert PRO systems can be configured as a Theta-Theta
diffractometer, a Omega-2Theta diffraction system, or as an Alpha-1 diffractometer.
1.6.2.1 X’Pert PRO MPD Theta-Theta Systems

X’Pert PRO MPD (Multi-Purpose Diffractometer) Theta-Theta systems are equipped with a PreFIX stage
interface for rapid exchange of sample stages without additional stage alignment. The X’Pert PRO MPD Theta-
Theta system is shown in Figure 1.17. The sample stages are fixed to the goniometer and do not rotate around
the omega axis as in Omega-2Theta diffractometers. The X-ray tube is fitted onto a moveable goniometer arm.
During measurements the sample is kept horizontal; this means that this kind of system is especially useful if
you need to measure loosely prepared powder samples or extremely large and/or heavy samples.
The goniometer radius in these systems is between 130 and 240 mm, the actual radius of the goniometer is given
on the Acceptance Test Form delivered with the system.
Figure 1.17: X’Pert PRO MPD Theta-Theta System
07.03.27 Page 1.19

1.6.2.2 X’Pert PRO MPD Omega-2Theta Systems

In X’Pert PRO MPD (Multi-Purpose Diffractometer) Omega-2Theta systems the sample stages are mounted
onto a PreFIX stage interface for rapid exchange of sample stages. The X’Pert PRO MPD Omega-2Theta system
is shown in Figure 1.17. In Omega-2Theta systems the X-ray tube is fixed to the goniometer, the sample stage
is mounted on the omega axis, and the diffracted beam optics and the detector are mounted on the 2theta axis.
The goniometer radius in these systems is between 130 and 240 mm, the actual radius of the goniometer is given
on the Acceptance Test Form delivered with the system.
Figure 1.18: X’Pert PRO MPD Omega-2Theta System
Page 1.20 07.03.27

1.6.2.3 X’Pert PRO Alpha-1 System

Characteristic of an X’Pert PRO Alpha-1 system is the presence of PW3113/60 Incident Beam Monochromator
mounted onto a bracket with two PreFIX positions for the X-ray tube. The X’Pert PRO Alpha-1 system is shown
in Figure 1.19. When the tube is fixed at the standard tube position the X’Pert PRO Alpha-1 system is the same
as an X’Pert PRO MPD Omega-2Theta system. When the tube is mounted at the alpha-1 position the X-rays
emitted by the X-ray tube are accepted by the incident beam monochromator. Changing the tube shield position
is described in detail in section 7.3.3.2 of Chapter 7 in Part II of this User’s Guide.
The X’Pert PRO Alpha-1 system can be used with either Cu Kα radiation or Co Kα radiation. This setting is
determined when the system is assembled. The type of radiation used with the Johansson monochromator is
given on the Acceptance Test Form delivered with the system.
The goniometer radius is 200 mm, 220 mm, or 240 mm. The actual value is given in the Acceptance Test Form
delivered with the system.
Figure 1.19: X’Pert PRO Alpha-1 System
07.03.27 Page 1.21

1.7 TERMS USED IN THIS GUIDE
Term Explanation
Alpha-1 system An Omega-2Theta system with an incident beam focusing monochromator

(Johansson type).
Angle of incidence (ω) Angle between the incoming X-ray beam and sample surface.
Axial divergence Divergence of the X-ray beam perpendicular to the diffraction plane.
Bragg-Brentano Para-focusing geometry. In Bragg-Brentano geometry the incident beam from the
geometry line focus of the X-ray tube diverges in the diffraction plane until it irradiates the
sample. The diffracted X-ray beam converges from the sample until it passes
through the receiving slit (the natural focusing point on the goniometer circle)
before being accepted by the detector.
cps Counts per second, unit to express the intensity of an X-ray beam.
Diffracted beam optics The optical components between sample stage and detector.
Diffraction plane Plane defined by the incoming and diffracted X-ray beams; also called the
equatorial plane.
Goniometer radius The distance between the tube focus and the center of the goniometer, or the
distance between the center of the goniometer and the receiving slit.
Incident beam optics The optical components between X-ray tube and sample stage.
In-plane diffraction A method of measuring the lattice spacing between the crystal planes that are
oriented perpendicularly with respect to the sample surface.
Irradiated length Size of the irradiated area on the sample parallel to the diffraction plane.
Irradiated width Size of the irradiated area on the sample perpendicular to the diffraction plane.
Medipix2 Photon counting technology for the conversion of X-rays into electrical signals with
high spatial resolution and a high contrast. Applied in the PIXcel.
Mirror-mirror geometry Geometry in which an X-ray mirror is used as an incident beam PreFIX module, and
an X-ray mirror combined with a programmable receiving slit is used as a diffracted
beam PreFIX module.
Peak positions determined from symmetrical scans (2θ−θ scans) measured with the
mirror-mirror geometry are not sensitive to sample height misalignment. This means
that this geometry can be usefully used on loosely prepared powder samples, or
samples with ill-defined surfaces.
Observed length Size of the area parallel to the diffraction plane, as seen by the detector.
Omega-2Theta system The tube is fixed, the sample stage and the detector are moving.
Parallel beam Diffraction geometry in which the diverging X-ray beam from the tube is converted
geometry into a small value in the equatorial plane for line focus, or in two dimensions
(equatorial and axial) for point focus applications.
If the appropriate optics are used on the diffracted beam side, parallel beam
measurements are not sensitive to the exact height position of the sample, or to
sample tilt. This geometry is also suitable for loosely prepared powder specimens, or
samples with irregularly shaped surfaces.
Page 1.22 07.03.27

Term Explanation
PHD Pulse Height Distribution. X-ray intensities are measured via a cascade of ionizations
in a gas filled tube. Eventually, the electrons hit a wire at high tension, which leads
to an electrical pulse. The height of this pulse is a/o proportional to the energy of
the incoming photons. The detector is adjusted to optimize the PHD for the
characteristic radiation of the X-ray tube (e.g. Cu Kα).
PreFIX Pre-aligned Fast Interchangeable X-ray modules. Concept of modular exchange of

components without additional alignment by the user.
RTMS Real Time Multiple Strip. Detection technology for fast X-ray diffraction data
acquisition. Applied in the X’Celerator.
Scattering angle (2θ) Diffraction angle. Angle between the incoming and diffracted X-ray beams.
Theta-Theta system The sample stage is fixed, the tube and the detector are moving. Only for single
vertical systems.
Transmission geometry Diffraction geometry in which the X-ray beam passes through the sample.
Used for those sample which mainly comprise light elements, such as pharmaceuti-
cal materials.
1.8 REFERENCES
In this guide we occasionally refer to other publications, when we refer to other publications the reference is
always a number enclosed in square brackets (for example: [3]). The number refers to one of the following
publications:
[1] : PANalytical Safety Manual - order code number: 4022 339 04531.
[2] : XRD X’Pert Tube Instruction Manual - order code number: 4022 196 71701.
[3] : X’Pert PRO Systems, Pre-installation Manual - order code number: 4022 339 04821.
[4] : W. J. Bartels, (1983) Journal of Vacuum Science and Technology B1, 338.
[5] : R. W. James, “The Optical Principles of the Diffraction of X-rays, The Crystalline State - Vol. II”, L.
Bragg (editor), G. Bell and Sons Ltd., 1962.
[6] : P. van der Sluis (1994), Journal of Applied Crystallography 27, 50-55.
[7] : P. F. Fewster, “X-ray Scattering from Semiconductors”, Chapter 3, Imperial College Press (London,
UK) 2003. ISBN 1 - 86094 - 360 - 8. Distributed by World Scientific Publishing Co.
[8] : P. van der Sluis (1994), Journal of Applied Crystallography 27, 1015-1019.
07.03.27 Page 1.23

General information about X-ray diffraction and its applications can be found in the following publications:
- F. H. Chung, D. K. Smith (editors), “Industrial Applications of X-ray Diffraction”, Marcel Dekker, Inc.,
(New York, NJ, USA) 2000. ISBN 0 - 8247 - 1992 - 1.
- B. D. Cullity, “Elements of X-ray Diffraction”, Addison Wesley Publishing Company, Inc. (Reading,
MA, USA) 1978. ISBN 0 - 201 - 01174 - 2.
- P. F. Fewster, “X-ray Scattering from Semiconductors”, Imperial College Press (London, UK) 2003.
ISBN 1 - 86094 - 360 - 8. Distributed by World Scientific Publishing Co.
- C. Giacovazzo, “Fundamentals of Crystallography”, Published for the International Union for
Crystallography by Oxford University Press (Oxford, UK) 1992. ISBN 0 - 19 - 855578 - 4 (paperback),
ISBN 0 - 19 - 855579 - 2 (hard back).
- U. Pietsch, V. Holý, T. Baumbach, “High-Resolution X-ray Scattering from Thin Films”, Springer-
Verlag (Berlin, Germany) 2004. ISBN 0 - 387 - 40092 - 3.
- International Tables for Crystallography:
Volume A: Space-group Symmetry; T. Hahn (editor) 2005. ISBN 0 - 7923 - 6590 - 9.
Volume B: Reciprocal Space; U. Shmueli (editor) 2001. ISBN 0 - 7923 - 6592 - 5.
Volume C: Mathematical, Physical and Chemical Tables; E. Prince (editor) 2004.
ISBN 1 - 4020 - 1900 - 9.
Published for the International Union for Crystallography by Springer.
Information about other volumes published in this series can be found at: www.iucr.org.
- R. Jenkins, R. L. Snyder, “Introduction to X-ray Powder Diffractometry”, J. Wiley & Sons Inc.
(New York, USA) 1996. ISBN 0 - 471 - 51339 - 3.
- H. P. Klug, L. E. Alexander, “X-ray Diffraction Procedures for Polycrystalline and Amorphous
Materials”, J. Wiley & Sons Inc. (New York, USA) 1974. ISBN 0 - 471 - 46369 - 4.
- U. F. Kocks, C. N. Tomé, H. - R. Wenk, “Texture and Anisotropy”, Cambridge University Press
(Cambridge, UK) 1998. ISBN 0 - 521 - 46516 - 8.
- D. M. Moore, R. C. Reynolds Jr., “X-ray Diffractometry and the Identification and Analysis of Clay
Minerals”, Oxford University Press Inc. (New York, USA) 1997. ISBN 0 - 19 - 508713 - 5.
- I. C. Noyan, J. B. Cohen, “Residual Stress”, Springer-Verlag New York, Inc., (New York, USA) 1986.
ISBN 0 - 387 - 96378 - 2 (New York, USA), ISBN 0 - 540 - 96378 - 2 (Berlin, Germany).
- R. A. Young (editor), “The Rietveld Method”, IUCr Monographs on Crystallography No. 5, Published
for the International Union for Crystallography by Oxford University Press (Oxford, UK) 1993.
ISBN 0 - 19 - 855577 - 6.
- L. S. Zevin, G. Kimmel, “Quantitative X-ray Diffractometry”, Springer-Verlag New York, Inc.,
(New York, USA) 1995. ISBN 0 - 387 - 94541 - 5.
Page 1.24 07.03.27

Chapter 2
Safety
Contents
2.1 Introduction......................................................................................................................... 2 - 3
2.1.1 Explanation of Warning, Caution and Note ........................................................................... 2 - 3
2.1.2 Symbols .................................................................................................................................. 2 - 4
2.2 General Safety Precautions................................................................................................ 2 - 5
2.2.1 Servicing Precautions ............................................................................................................. 2 - 5
2.2.2 EMC Precautions.................................................................................................................... 2 - 5
2.2.3 X-rays ..................................................................................................................................... 2 - 6
2.2.4 Beryllium................................................................................................................................ 2 - 6
2.2.5 Gas System ............................................................................................................................. 1 - 6
2.2.6 Cooling System ...................................................................................................................... 2 - 6
2.2.7 Liquid Nitrogen ...................................................................................................................... 2 - 7
2.2.7.1 Handling................................................................................................................. 2 - 7
2.2.7.2 Precautions............................................................................................................. 2 - 7
2.2.7.3 Emergency Actions................................................................................................ 2 - 7
2.2.7.4 Reading Matter ...................................................................................................... 2 - 7
2.3 X’Pert PRO Safety Circuits ............................................................................................... 2 - 8
2.3.1 X-ray Safety Loop .................................................................................................................. 2 - 8
2.3.2 HT Safety Loop ...................................................................................................................... 2 - 8
2.4 Safety Information .............................................................................................................. 2 - 9
2.4.1 Electrical Safety Standards..................................................................................................... 2 - 9
2.4.2 Radiation Safety Standards .................................................................................................... 2 - 9
07.03.27 Page 2.1

Page 2.2 07.03.27

Part I - Chapter 2: Safety
2.1 INTRODUCTION
The X’Pert PRO X-ray diffraction system is perfectly safe if installed and operated as described in this User’s
Guide.
This chapter contains safety information relating to the operation and servicing of the X’Pert PRO X-ray
diffraction systems. For further general safety information relating to X-ray equipment, refer to the PANalytical
Safety Manual [1].
Read this chapter carefully before you install or use any of the equipment.
• Adjustments, maintenance and repair of the equipment must only be performed by personnel who are
aware of the radiation hazards involved and (where necessary) work to an approved scheme of work.
• Anybody operating or servicing X-ray apparatus must be aware of the requirements of all the applicable
regulations, local or otherwise.
• It is essential for the safe use of the equipment that both operating and service personnel follow accepted
safety procedures in addition to the safety precautions as specified in the PANalytical Safety Manual [1].
• Where necessary, specific warnings and cautions can be found throughout this User’s Guide.
• Where necessary, warning and caution stickers displaying the appropriate symbol are displayed on the
equipment.
2.1.1 Explanation of Warning, Caution and Note

Actions detailed within this manual that require special attention are indicated as follows:
WARNING
THIS DENOTES INFORMATION THAT, IF IGNORED, MAY RESULT IN A
DANGER TO THE HEALTH OR SAFETY OF THE OPERATOR, SERVICE
ENGINEER OR OTHER PERSONS IN THE VICINITY.
CAUTION
This denotes information that, if ignored, may result in damage to,
excessive wear or unsatisfactory performance of the equipment.
NOTE: This denotes information of particular importance to help the user understand or adjust the
equipment.
07.03.27 Page 2.3

2.1.2 Symbols
The following symbols are displayed on PANalytical equipment:
Electrical hazard (BLACK/YELLOW)
Read the operating instructions (BLACK/YELLOW)
Pinch hazard (BLACK/YELLOW)
Heavy weight (BLACK/YELLOW)

>25 kg
Hot surface (BLACK/YELLOW)
Protective earth (ground) terminal (BLACK)
Measuring earth (BLACK/WHITE)
Radiation danger
Lit: Generating X-rays (BLACK/YELLOW)
Not Lit: Not generating X-rays
Equipment produces high intensity X-ray

beams.
(BLACK/YELLOW)
Symbol is on control panel, adjacent to
warning labels in appropriate language/s
Laser danger
See also any other labels attached adjacent to (BLACK/YELLOW)
this symbol
Poison (BLACK/YELLOW)
Page 2.4 07.03.27

Extreme cold
(BLACK/YELLOW)
Recycling symbol (BLACK/WHITE)
Strictly obey all instructions and warning text on the labels attached to the various parts of the equipment.
2.2 GENERAL SAFETY PRECAUTIONS

Strictly adhere to all local safety procedures and working practices.
The diffractometer is a Safety Class 1 apparatus (Pollution Degree 2 Installation category II) and all accessible
parts of the unit which could become live in the event of fault are provided with safety earth terminals. These
earth connections must not be removed whilst power is applied to the equipment.
When the equipment is connected to the supply some terminals may be live, therefore exercise extreme care
when removing covers and panels for servicing.
If it seems likely that the system safety or protection has been impaired, switch the system off and disconnect
the supply and contact your local PANalytical service organization.
The Control Panel HT ON switch is key operated and the key should be kept in a safe place when the equipment
is not in use.
2.2.1 Servicing Precautions

All repairs, adjustment or alignment must be carried out strictly in accordance with the approved work practices
of the country where the equipment is installed.
Before use and at regular time intervals have the PANalytical engineer check the operation of all safety circuits
and devices.
When working with X-rays, monitor the radiation level to make sure that the working environment is always at
a safe level. Ensure that all protective shielding (radiation or electrical) is replaced immediately after servicing.
2.2.2 EMC Precautions

As PANalytical equipment is currently manufactured with Electromagnetic Interference (EMI) Proof
provisions, special attention should be paid to the connection and clamping of the shielded cables. Shielded
cables coming from the equipment must be clamped with their open shielding beneath cable clamps to prevent
EMI. Most current equipment is equipped with the necessary facilities for this. After servicing or repair, always
check that shielded cables are properly connected to their appropriate connectors and are clamped beneath
suitable cable clamps.
Modifications to the system configuration may result in decreasing EMC behavior. Therefore before you modify
the system you should contact the EMC specialist at PANalytical in Almelo, The Netherlands.
07.03.27 Page 2.5

2.2.3 X-rays
WARNING 1. X-RAYS ARE HARMFUL. THE X-RAY DIFFRACTION SYSTEM
PRODUCES X-RAYS WHICH CAN BE DANGEROUS TO HEALTH IF THE
PROPER PRECAUTIONS ARE NOT TAKEN.
2. IT IS IMPORTANT FOR THE HEALTH AND SAFETY OF THE OPERATOR
AND/OR SERVICE ENGINEER THAT THE RECOMMENDATIONS GIVEN
IN THIS USER’S GUIDE, THE VARIOUS EQUIPMENT MANUALS, AND
IN THE SAFETY MANUAL, ARE CAREFULLY OBSERVED.
3 LOCAL SAFETY REGULATIONS MUST BE STRICTLY COMPLIED WITH.
When properly operated within the specifications the radiation level at distance of 10 cm from the PW3040/60
Enclosure is less than 1 μSv/h.
2.2.4 Beryllium
The windows of X-ray tubes and detectors are made of beryllium.
WARNING FUMES OR THE DUST FROM BERYLLIUM AND ITS COMPOUNDS, CAN
BE HAZARDOUS IF INHALED. DURING USE, CORROSION OF
BERYLLIUM MAY OCCUR. THE BERYLLIUM MUST NOT BE CUT,
MACHINED OR HANDLED IN ANY WAY. DISPOSAL OF BERYLLIUM
PRODUCTS MUST COMPLY WITH ALL APPLICABLE NATIONAL
REGULATIONS.
Refer to the PANalytical Safety Manual [1].

Tube disposal must comply with all national and local registrations governing beryllium. You can, if you wish,
send a used tube back to the PANalytical tube factory. Please fill in the Tube End-of-Life Report supplied with
the X-ray tube, this information helps us in improving our X-ray tubes.
2.2.5 Gas System

The detector gases used in non-ambient chambers are often supplied in pressurized cylinders.
WARNING 1. ENSURE THAT GAS CYLINDERS ARE SECURED AGAINST A WALL OR

IN AN APPROVED STAND. IF A GAS CYLINDER IS ALLOWED TO FALL
IT MAY EXPLODE.
2. IF GAS LINES FROM THE CYLINDERS TO THE EQUIPMENT CROSS

THE FLOOR, ENSURE THAT THEY ARE PROTECTED.
2.2.6 Cooling System

The high tension generator will be switched off if the cooling water flow falls below 3.5 l/min. Therefore, always
ensure (even when the system equipment is switched off) that all the water exhaust outlets are not blocked and
that the water pressure or flow limits are not exceeded.
Page 2.6 07.03.27

A low water temperature in combination with a high amount of humidity in the air can cause condensation to
form on the metal parts of the cooling circuit and the metal parts of the rack. This condensation could cause flash-
overs which may damage the system. In order to reduce condensation forming we recommend that the water
temperature is kept at a level such that the temperature of the metal parts is always above the dew point. This
can be achieved by installing a closed cooling water circuit.
2.2.7 Liquid Nitrogen

Liquid nitrogen is used for cooling purposes in non-ambient chambers to allow measurements to be performed
at temperatures down to -193°C (80 K). It is a non-toxic, inert, colorless and odorless liquid with an extremely
low temperature (-196°C). Small volumes of liquid give large volumes of gas at evaporation; one volume of
liquid nitrogen expands to approximately 700 volumes of gas at ambient conditions. Consequently, it can easily
deplete the oxygen content of the air in enclosed spaces, thus causing asphyxiation. Liquid nitrogen can cause
severe cold burns if the liquid is allowed to come into contact with bare skin or delicate tissues such as your eyes.
2.2.7.1 Handling
Liquid nitrogen should be handled with care in well-ventilated rooms. Use only containers specifically designed
for cryogenic service. Use proper transfer equipment such as a stainless steel flexible hose or a special filling
adaptor to prevent splashing or spillage.
2.2.7.2 Precautions
Liquid nitrogen is safe to work with, if the following safety precautions are maintained
• Use safety glasses to protect your eyes.
• Wear warm dry non-absorbent gloves to handle cold parts.
• Wear protective clothing.
Ensure the vessel is operated in an area that has adequate ventilation. An oxygen meter can be used to warn of
potential nitrogen inhalation hazards.
WARNING
LIQUID NITROGEN AND NITROGEN GAS ARE NOT TOXIC. HOWEVER
THEY MAY DISPLACE ATMOSPHERIC OXYGEN WHEN PRESENT IN
LARGE QUANTITIES OR WHEN USED IN CONFINED POORLY
VENTILATED SPACES, RESULTING IN A SUFFOCATION HAZARD.
2.2.7.3 Emergency Actions

The following emergency actions should be taken in the case of an accident with liquid nitrogen:
Flush the affected areas of skin or eyes with copious quantities of lukewarm water, and do not apply
any form of direct heat. Move casualty to a warm place (about 22° C). Contact a medical center.
In the case of a nitrogen gas leak:
Persons showing symptoms of oxygen deprivation should be moved immediately to a well-ventilated
room. If the breathing stops, perform artificial respiration until medical help arrives.
2.2.7.4 Reading Matter

Further information about handling liquid nitrogen is delivered with the devices using liquid nitrogen.
Carefully read the operation and safety instructions supplied with these devices before starting to work with
them.
07.03.27 Page 2.7

2.3 X’PERT PRO SAFETY CIRCUITS

There are two basic safety loops in X’Pert PRO systems. Both of these loops must indicate a “Safe” status before
the system will allow High Tension (HT) to be applied to the X-ray tube.
2.3.1 X-ray Safety Loop

The upper part of the instrument enclosure is the X-ray enclosure. All access panels and doors to this enclosure
make contact with microswitches when they are closed. These microswitches form a series safety loop which
must be complete before the shutter can be opened. The safety loop and microswitches are doubled, forming a
second independent safety system.
A yellow LED next to the tube shield’s shutter assembly illuminates when the shutter is open. If the safety circuit
is broken during operation, a relay on the shutter assembly will automatically close the shutter.
A “Shutter Close” switch on the Control panel allows you to close the shutters manually. This allows you to open
the doors for sample changing and so on. In this situation HT will remain on the tube and all safety indicators
will remain lit.
The PreFIX incident beam optical module must be fitted correctly so that the shutter actuator closes the safety
microswitch on the tube shield.
2.3.2 HT Safety Loop

The HT Safety loop protects the system by automatically closing the shutter on the tube shield and shutting down
or preventing the application of HT if any of the following situations apply:
• The front or rear doors are not correctly closed when the shutter on the tube shield is open.
• The cooling water supply is not functioning.
• The tube is not fitted correctly in the tube shield assembly.
• The HT cable safety and the tube indication plug are not correctly fitted into their sockets in the tube
shield and the X-ray tube (respectively).
• The yellow X-RAYS ON lamp on top of the instrument enclosure, or the X-RAYS ON lamp on the con-
trol and display panel are not functioning.
• The cylinder through which the HT cable passes from the HT tank to the X-ray enclosure is not correctly
fitted (this is unlikely).
WARNING
NEVER OVERRIDE ANY SAFETY DEVICE.
If the HT is switched off for any reason at all, the water valve in the cooling system automatically closes after 5
seconds. It is not possible to switch the HT on again until this 5 seconds has elapsed.
Page 2.8 07.03.27

2.4 SAFETY INFORMATION

2.4.1 Electrical Safety Standards
PANalytical systems meet the following electrical safety standards:
Standard Description
EN61010/IEC1010 Safety requirements for electrical equipment, for
CSA - C22.2 - No. 1010 measurement, control and laboratories. Class II,
Pollution degree 2.
73/23/EEC Low Voltage Directive
89/336/EEC EMC Directive, in which the following norms are
laid down:
EN55011/CISPR11: 1993 - Class A Group 1
EN55022/CISPR22: 1989 - Class B
IEC801 - 2/EN6100-4-2: 8k VCD, 15kVAD Level 4
IEC801 - 3: 1992 3V/m 27MHz → 1GHz
ENV50140 10V/m 30 MHz → 1 GHz
IEC801-4/EN61000-4-4: 4kV PL, 4kV SL Level 4
IEC801-5/EN61000-4-5
IEC801-6/EN61000-4-6 10Vrms Level 3
2.4.2 Radiation Safety Standards

PANalytical systems meet the following radiation safety standards:
Country Description
Germany Verordnung über den Schutz vor Schaden durch Röntgenstrahlen (German
X-ray decree - RöV) 1987. Classification Vollschutz (Full Protection
Equipment).
United Kingdom The Ionising Radiations Regulations 1999.
USA Radiation Safety for X-ray Diffraction and Fluorescence Analysis
Equipment. (NBS Handbook 111, 1977.)
USA Department of Health, Education and Welfare (DHEW). FDA 75 8003.
Canada Radiation Emitting Devices Act SOR/DORS/81 545. Part XVIII Cabinet X-ray
Equipment Consultative Document. Part XIV X-ray Diffraction Equipment.
Australia Code of Practice for Protection against Ionising Radiation Emitted from
X-ray Analysis Equipment (1984).
07.03.27 Page 2.9

Page 2.10 07.03.27

Chapter 3
Applications and Optics
Contents
3.1 Equipment and Applications ............................................................................................. 3 - 3
07.03.27 Page 3.1

Page 3.2 07.03.27

Part I - Chapter 3: Applications and Optics
3.1 EQUIPMENT AND APPLICATIONS

X’Pert PRO X-ray diffraction systems with the PreFIX optical modules and sample stages are designed to
support a wide variety of measurements. Table 3.1 helps you to select the main components to be mounted on
your system in order to perform certain applications (for example: phase analysis). Table 3.2 and Table 3.3
explain the abbreviations used in Table 3.1.
Table 3.1: Applications and Required Equipment
Incident Diffracted
MRD MRD
Applications Beam Beam MPD Remarks
HR NR
Optics Optics
Phase analysis, FDS PRS + FASS • • • Normal powder diffraction,

Omega-stress, Crys- higher resolution,
PDS PRS + PASS • • •
tallography on FLAT high dynamic range
SAMPLES
FDS + RTMS or • • • Fast powder diffraction,
IBASHDS Medipix2 higher resolution,
high dynamic range
PDS + RTMS or • • •
IBASHDS Medipix2
Crystallography on α1 + FDS PRS + FASS • ⊗ ⊗ Highest resolution, Alpha-1
FLAT SAMPLES system, Kα1 only
α1 + PDS PRS + PASS • ⊗ ⊗
α1 + FDS + RTMS or • ⊗ ⊗ Highest resolution, fast data
IBASHDS Medipix2 acquisition,
alpha-1 system, Kα1 only
α1 + PDS + RTMS or • ⊗ ⊗
IBASHDS Medipix2
Phase analysis, XM PPC • • • Default
Omega-stress, Crys-
HM PPC • • • Kα1 only
tallography on
ROUGH SAMPLES
Phase analysis and XM XM + PRS • • • Default
Crystallography on
HM XM + PRS • • • Kα1 only
LOOSELY PREPARED
POWDER SAMPLES
Phase analysis of FDS PPC • • • With low angle slits
THIN FILMS
PDS • • •
XM • • •
HM • • • Kα1 only
07.03.27 Page 3.3

Incident Diffracted
MRD MRD
HR NR
Optics Optics
Phase analysis and

Crystallography on FXM + RTMS +
• ⊗ ⊗ Default
SAMPLES IN GLASS IBASHFXM DBAS
CAPILLARIES
Medipix2 + • ⊗ ⊗
DBAS
PRS • ⊗ ⊗ Slow
PPC • ⊗ ⊗ Slow, low resolution
HM + RTMS + • ⊗ ⊗ Default, Kα1 only

IBASHHM DBAS
Medipix2 + • ⊗ ⊗ Kα1 only
DBAS
PRS • ⊗ ⊗ Slow
PPC • ⊗ ⊗ Slow, low resolution
Reflectometry FDS PPC • • • Use collimator slit
PDS PRS + PASS • • • Variable acceptance
PPC • • • Use collimator slit
XM PRS + PASS • • • Variable acceptance
PPC • • • Use collimator slit
HM PRS + PASS • • • Thick layers, Kα1 only
PPC • • • Thick layers, use collimator

slit, Kα1 only
High Resolution HM RC • • • Line focus, fast reciprocal

diffraction space mapping
HM TA/RC ⊗ • ⊗ Line focus, copper radiation
only
HM Medipix2 • • • Line focus, fast reciprocal
space mapping
XM (Cu) + RC ⊗ • ⊗ Line focus, Extended MRD,
Ge copper radiation only
TA/RC ⊗ • ⊗
Ge RC • • • Point focus
TA/RC ⊗ • ⊗
Ge (440) RC ⊗ • ⊗ Point focus, highest resolu-
tion for rocking curves
Page 3.4 07.03.27

Incident Diffracted
MRD MRD
HR NR
Optics Optics
Texture, Psi-stress PFO PRS • ⊗ ⊗ Standard
CSC PRS ⊗ • • Standard
RTMS or ⊗ • • Fast data acquisition

Medipix2
XRL PPC • • • Less defocusing, better peak
separation
Spot analysis Monocap RTMS or • • • Phase analysis & stress;
Medipix2 micro-texture in receiving
slit mode
PRS • • • Micro-texture
PPC • • • Spots > 0.5 mm
In-plane diffraction XRL PPC ⊗ • • Point focus
Ge PPC ⊗ • • Point focus, highest resolu-

tion, Kα1 only
Transmission through FXM RTMS + • ⊗ ⊗ Line focus

(samples between) DBAS
foils
Medipix2 + • ⊗ ⊗ Line focus
DBAS
HM PPC • ⊗ ⊗ Line focus, Kα1 only
XRL PPC • ⊗ ⊗ Point focus, for orientation

measurements
Legend: • = Available
⊗ = Not available
07.03.27 Page 3.5

Table 3.2: Explanation of the Abbreviations used in Table 3.1
Type Chapter
Abbreviation Full Name
Number in Part II
α1 Focusing Incident Beam Monochromator PW3113/60 7
CSC Crossed Slits Collimator PW3084/62 8
DBAS Diffracted Beam Anti-scatter Device for X’Celerator PW3x94/30 20

Diffracted Beam Anti-scatter Device for PIXcel PW3490/00
FASS Fixed Anti-scatter Slit PW3092/00 16

FDS Fixed Divergence Slit PW3082/60 3
FXM Focusing X-ray Mirror PW3152/63 6
Ge Germanium Four-crystal Monochromator PW3110/6x 7

HM Hybrid Monochromator PW3147/x0 7
PW3149/63
PW3150/63
IBASHDS Incident Beam Anti-scatter Slit Holder for Divergence Slit PW3086/00 20
IBASHFXM Incident Beam Anti-scatter Slit Holder for Focusing X-ray PW3086/7x 20
Mirror
IBASHHM Incident Beam Anti-scatter Slit Holder for Hybrid Mono- PW3086/65 20
chromator
IBASHXM Incident Beam Anti-scatter Slit Holder for X-ray Mirror PW3086/60 20
Medipix2 Medipix2 Detector (PIXcel) PW3018/00 21
Monocap Mono-capillary PW3145/00 10
PASS Programmable Anti-scatter Slit PW3091/x0 16
PDS Programmable Divergence Slit PW3081/60 3
PFO Incident Beam Collimator PW3084/60 8

PPC Parallel Plate Collimator PW3098/xx 18
PRS Programmable Receiving Slit PW3093/60 16
RC Rocking Curve Optics PW3097/60 16
RTMS Real Time Multiple Strip Detector (X’Celerator) PW3015/x0 21
TA/RC Triple Axis and Rocking Curve Attachment PW3120/6x 16,19
XRL X-ray Lens PW3146/xx 9

XM X-ray Mirror PW3088/6x 6
PW3148/6x
Page 3.6 07.03.27

Table 3.3: Explanation of the Diffractometers Referred to in Table 3.1
Diffractometer Description
Alpha-1 Multi-Purpose Diffractometer with focusing incident beam

monochromator.
Equipped with special incident beam attachment.
Monochromator is factory aligned for Cu or Co radiation.
Goniometer is vertical.
Goniometer radius is 200, 220 or 240 mm.
Extended MRD Materials Research Diffractometer with extended incident

beam arm to mount two incident beam PreFIX modules behind
each other.
MPD Multi-Purpose Diffractometer.

Equipped with PreFIX Stage Interface.
Goniometer can be vertical or horizontal.
Maximum goniometer radius is 240 mm.
MRD Materials Research Diffractometer.

Equipped with fully motorized 1/2 circle Eulerian cradle (MRD
sample cradle).
Goniometer is horizontal.
NR Normal Resolution Diffractometer.

Minimum step size is 0.001º in ω or 2θ.
HR High Resolution Diffractometer.

Minimum step size is 0.0001º in ω or 2θ.
07.03.27 Page 3.7

Page 3.8 07.03.27

Chapter 4
General Operations
Contents
4.1 Introduction......................................................................................................................... 4 - 3
4.2 Environmental Operating Conditions .............................................................................. 4 - 3
4.2.1 Climate ................................................................................................................................... 4 - 3
4.2.2 Protection Degree ................................................................................................................... 4 - 3
4.2.3 Other Environmental Conditions............................................................................................ 4 - 4
4.3 Switching the System On.................................................................................................... 4 - 4
4.4 Selecting and Fitting Hardware......................................................................................... 4 - 5
4.4.1 X-ray Tube ............................................................................................................................. 4 - 5
4.4.2 Sample Stages......................................................................................................................... 4 - 6
4.4.3 PreFIX Modules ..................................................................................................................... 4 - 6
4.4.3.1 Incident Beam PreFIX Modules ............................................................................ 4 - 7
4.4.3.2 Diffracted Beam PreFIX Modules ......................................................................... 4 - 8
4.4.4 Detectors................................................................................................................................. 4 - 9
4.4.5 Safe Angle Settings ................................................................................................................ 4 - 9
4.4.6 Sample Preparation................................................................................................................. 4 - 9
4.4.7 Sample Mounting ................................................................................................................... 4 - 9
4.5 Switching the System Off ................................................................................................. 4 - 10
07.03.27 Page 4.1

Page 4.2 07.03.27

Part I - Chapter 4: General Operations
4.1 INTRODUCTION
X’Pert PRO systems are installed and aligned for use by a PANalytical Service Engineer. Once the acceptance
tests are completed, the system is ready for use. This chapter describes the operation procedures that you need
for safe and efficient operation of the system. General maintenance is described in Chapter 5 in Part I of this
User’s Guide.
Before you start to use the system you should first read Chapter 2 “Safety” in Part I of this User’s Guide, and
the PANalytical Safety Manual [1].
This chapter describes the following:
• The environmental conditions for optimal use of the system (section 4.2).
• Switching the system on (including the high-tension generator) (section 4.3).
• Selecting and fitting the hardware (X-ray tubes, sample stage, incident and diffracted beam optics, and
detectors) (section 4.4).
• Sample mounting and alignment (section 4.4).
• Switching the system off (section 4.5).
4.2 ENVIRONMENTAL OPERATING CONDITIONS

X’Pert PRO systems can be used in an industrial environment as well as in a research laboratory. In order to
ensure reliable operation of the X’Pert PRO system, there are several requirements that are applicable to the
environmental conditions of the location of where the system is being used. This section provides an overview
of these conditions. A full description can be found in the X’Pert PRO Pre-installation Manual [3].
4.2.1 Climate
Before starting to collect diffraction data the X’Pert PRO system must be at a stable temperature. The room
temperature must be between +5 ºC and +40 ºC (278 K - 313 K). We advise room temperatures between +15 ºC
and +25 ºC (288 K - 298 K). Temperature variation in the room must be less than 1 ºC per 30 minutes.
For high resolution measurements you must have a room temperature of 22 ºC ± 1 ºC (295 K ± 1 K).
The temperature inside the instrument enclosure should not exceed 26 ºC (299 K).
The relative humidity must be between 20% and 80%. The standard maximum altitude of the working
environment is 2000 m.
The sample must have the same temperature as the instrument. It is therefore advisable to store samples that are
going to be measured in the near future inside the instrument enclosure to save time.
Direct solar radiation on the system is not allowed.
In order to ensure a stable temperature of the working environment, please note that the heat dissipation of one
X’Pert PRO system in the room is between 7 kW and 11.8 kW depending on the configuration and the X-ray
tube settings used.
4.2.2 Protection Degree

The X’Pert PRO system includes an instrument enclosure to ensure a safe working environment with respect to
X-rays. The enclosure also restricts the access of dust to the system. However, we recommend that the
environment is clean. The protection provided by the instrument enclosure complies with IEC529 class IP40.
This means that:
• Solid particles larger than 1.0 mm will not penetrate the enclosure.
• There is no special protection against dripping or splashed water.
Very fine dust can penetrate into the upper part of the instrument enclosure. This will not be harmful to the
equipment provided that the quantity of dust is low and regular routine maintenance procedures are strictly
adhered to.
07.03.27 Page 4.3

Special attention must be paid to sample preparation in order to maintain accuracy when an analysis is
performed. Dust from the sample surface, or particles that fall off the sample, can accumulate in important parts
of the system and interfere with the correct operation of the equipment.
Regularly remove excess dust from the system using a hand-held vacuum cleaner.
4.2.3 Other Environmental Conditions

For proper operation of the X’Pert PRO system it is advisable to work in an environment free of noise and
vibration. The system should not be subject to excessive external vibrations, such as those from a rolling mill or
a steel plant. The maximum allowable vibration levels are:
• less than 60 μm for frequencies below 20 Hz.
• less than 25000 μm/Hz2 for frequencies above 20 Hz.
The maximum allowable acceleration is 0.05 m/s2.
The magnetic field variation around the X’Pert PRO system must be less than 10-5 T.
4.3 SWITCHING THE SYSTEM ON
CAUTION Before switching the system on, ensure that the goniometer
cannot collide with the sample or the sample stage during the
initialization procedure. If the automatic reset is not disabled and
a collision is possible, remove the sample (stage) and/or the optical
modules before switching on.
If the automatic reset is disabled, an initialization wizard will be
activated to guide you through the initialization procedures. This
gives you the opportunity to remove hardware components, the
sample stage and the sample before the system is reset.
Proceed as follows to switch the X’Pert PRO system on:

1. Turn on the cooling system’s water: first, fully open the tap on the return line; and then the tap on the
supply line.
2. Switch the system’s mains supply on. The “Standby” indicator lamp on the control and display panel
should now be lit.
3. Turn the HT key switch on the control and display panel clockwise.
4. Close the doors (and rear doors if necessary) on the instrument enclosure.
5. Press the “Power on” button on the control and display panel. The “Standby” indicator lamp will go out
and the “Power on” lamp will be lit.
6. Wait until the LEDs on the control and display panel are lit. When no dots are shown on the “Shutter
open” LED the system starts its initialization procedure. The HT generator will switch on to a generator
setting of 30 kV, 10 mA. The X-rays On lamp on top of the enclosure will light. If three moving dots are
shown on the “Shutter open” LED it indicates that the enclosure doors and/or the rear panels are not
correctly closed, or that the HT key is not turned on. In this condition the system cannot be initialized;
either close the doors or turn the HT key switch key clockwise, in order to let the system continue its
initialization procedure.
Page 4.4 07.03.27

7. The system has now got power supplied to all the relevant circuits. If the automatic reset is enabled in
the data collector software the system, the goniometer axes, the automated optics (and if applicable, the
sample cradle axes movements) will be initialized. If the automatic reset is disabled in the data collector
software, the system will not start the initialization procedure, but will ask you if it is safe to initialize
when you go on-line using the data collector software.
The automatic reset can be disabled in the data collector software when you are on line with the system. It will
become effective when the system is next started. It also enables a “Initialization Wizard” that becomes active
each time that the system is started. For more information about this “Initialization Wizard” please refer to the
X’Pert Data Collector’s help. Deactivation of the automatic reset will become effective when the system is next
started.
NOTE: The automatic reset option should be disabled:

If you are measuring large or unusually shaped samples which may clash with the optical
modules during initialization. For instance: if you are measuring 6 inch or 8 inch wafers (refer
to Chapter 11 in Part II of this User’s Guide; section 11.2.1.7).
or
When collisions are likely to occur during resetting, between the optical modules and the
sample or the sample stage, for instance: when you use a mono-capillary (refer to Chapter 10
in Part II of this User’s Guide; section 10.2), or the diffracted beam anti-scatter slit mounted
onto the X’Celerator or the PIXcel (refer to Chapter 21 in Part II of this User’s Guide; sections
21.4 and 21.5).
or
When your X’Pert PRO MRD system is equipped with the 9430 920 04651 Option for In-
plane Diffraction. Special information about the initialization of these systems is given in
section 11.2.2.4 in Chapter 11 in Part II of this User’s Guide.
8. Use the data collector software to go on-line.
9. If an X-ray tube is new, or if the HT has not been applied to the tube in the last 100 hours, or if the tube
has only just been installed in the system; we advise you to start a tube breeding procedure in order to
ensure stable operating conditions. Automatic conditioning procedures on X’Pert PRO systems can be
performed with the use of the data collector software. For more information on tube breeding refer to the
XRD X’Pert Tube Instruction Manual [2].
The X’Pert PRO system is now ready for use.
NOTE: We advise you to make sure that your system is switched on with the generator operating at 75%
of the maximum tube rating for between four and eight hours before you start to perform
measurements. This will ensure that the temperature of various components has stabilized. Eight
hours of stabilization time is especially advisable when you are working with optical modules like
X-ray mirrors and hybrid monochromators.
4.4 SELECTING AND FITTING HARDWARE

Once you have switched your system on you can set the X’Pert PRO system up for your measurements. An
overview of the possible combinations of applications and optics is given in Chapter 3 in Part I of this User’s
Guide. This section provides a survey of the options for setting up and aligning your system for the application.
4.4.1 X-ray Tube

The X-ray tube can be mounted in the tube shield in two focus positions: line focus and point focus. Rotating
the X-ray tube from the point focus to the line focus position and vice versa is described in Chapter 1 in Part II
of this User’s Guide, section 1.4.7.
If your application requires a different type of radiation, you can exchange the currently fitted X-ray tube with
a tube with a different anode material. Removal and installation of tubes is described in Chapter 1 in Part II of
this User’s Guide, sections 1.4.4 and 1.4.5.
07.03.27 Page 4.5
In most situations the X-ray tube is mechanically aligned. How to check the tube height alignment to see if this
is in fact so, is given in Chapter 1 in Part II of this User’s Guide, section 1.4.9. Should they be necessary,
alignment procedures are also provided in that section.
If you have an X’Pert PRO Extended MRD system, or an X’Pert PRO Alpha-1 system (refer to section 1.6 in
Chapter 1 in Part I of this User’s Guide) you can mount the X-ray tube in two positions. Which of these positions
you use depends on the optical configuration that you select for your application. Moving the X-ray tube from
the standard position to the extended position and vice versa in an extended system is described in Chapter 1 in
Part II of this User’s Guide, section 1.4.8. Placing the X-ray tube at the alpha-1 position, or at the standard
position in an X’Pert PRO Alpha-1 system is described in Chapter 7 in Part II of this User’s Guide, section
7.3.3.2.
4.4.2 Sample Stages

All of the sample stages used in X’Pert PRO MPD systems are PreFIX mounted onto the goniometer and can be
interchanged without the need for realignment. The PW3060/20 MRD Cradle used in X’Pert PRO MRD systems
is not removable. Exchanging sample stages is described in Chapters 12 and 13 in Part II of this User’s Guide;
standard stages in section 12.1.1, the stage for high-throughput diffraction in section 12.15.2, non-ambient
chambers in section 13.2.1.1, the temperature controlled humidity chamber in section 13.3.2.2, and the
cryogenic sample stages described in section 13.4.2.2 and 13.5.2.2.
The choice of which sample stage you use for your measurements is determined by the type of sample you have
and the type of application you have selected.
Accessories to sample stages (including the sample stages themselves) are described in Part II of this User’s
Guide in Chapters 11 to 15.
4.4.3 PreFIX Modules

The PreFIX modules used in the incident and diffracted beam paths comprise two main parts: a precision placing
and locking device (T-block), and the module itself, see Figure 4.1.
All of the PreFIX optical modules are supplied with a wooden storage support. This wooden support enables you
to store the PreFIX module safely and conveniently so that it cannot fall over and scratch or damage the reference
surfaces.
PreFIX modules fit onto the PreFIX position U-block on the incident and diffracted beam arms of the X’Pert
PRO goniometer. The module is locked into position accurately and reproducibly by means of the special PreFIX
locking screw.
Mount a PreFIX module onto its position on the goniometer as follows:
1. Use the T-bar Allen key to loosen the locking screw so that it does not protrude into the inside surface
of the U-block.
2. Carefully place the PreFIX optical module in the U-block optical module holder on the incident or
diffracted beam arm.
3. Secure the module in place by tightening the locking screw.
CAUTION
Do not over-tighten the PreFIX locking screw; the required torque
is 2.0 Nm to 2.5 Nm.
Page 4.6 07.03.27

PreFIX
Module
T-block
Countersunk
Lock Pin
U-block
PreFIX
Locking Screw
Figure 4.1: PreFIX Module Construction
NOTE: Alignment of PreFIX modules is goniometer specific. This means that when a PreFIX module is
aligned for one X’Pert PRO Goniometer, it CANNOT be used on a different X’Pert PRO
goniometer.
The T-block and the U-block have highly polished reference surfaces. Maintenance of these surfaces is
described in Chapter 5 of Part I of this User’s Guide (section 5.2).
CAUTION Be very careful to treat the reference surfaces of the PreFIX modules
with care.
4.4.3.1 Incident Beam PreFIX Modules

Incident beam PreFIX modules must be equipped with a shutter lever. This shutter lever is used to close the
microswitches on the tube shield. The microswitches are part of the X-ray safety loop (refer Chapter 2 in Part I
of this User’s Guide, section 2.3.1). The shutter can only be opened if this X-ray safety loop is closed. When the
shutter is opened, the yellow LED next to the shutter assembly on the tube shield is lit.
When you are mounting an incident beam PreFIX module, always make sure that the shutter lever activates the
microswitches on the tube shield. Figure 4.2 shows a shutter lever mounted onto a Soller slits assembly. If it
does not activate the microswitches, adjust the lever as follows:
1. Mount the incident beam PreFIX module onto its position at the incident beam PreFIX position.
2. Loosen the screws that secure the shutter lever to the PreFIX module (see Figure 4.2).
3. Adjust the position of the shutter lever so that both microswitches are actuated.
4. Tighten the securing screws to fix the shutter lever into position.
07.03.27 Page 4.7

Figure 4.2: Shutter Lever on Soller Slits Assembly

Please note that although the shutter lever is in most cases attached to the incident beam PreFIX module, in the
case of the PW3081/60 Programmable Divergence Slit and the PW3082/60 Fixed Divergence Slit, the shutter
lever is attached to the Soller slits. The Soller slits must be inserted into the slot for Soller slits to enable the
shutter to be actuated. In the case of the PW3084/60 Incident Beam Collimator the shutter lever is attached to
the incident beam channel block.
Incident beam PreFIX modules and (mounting of) their accessories are described in Part II of the User’s Guide
in Chapters 2 to 10.
4.4.3.2 Diffracted Beam PreFIX Modules

Diffracted beam PreFIX modules are mounted onto the PreFIX position on the 2theta arm of the goniometer. If
a PW3096/60 Second Diffracted Beam PreFIX Carrier (see Figure 1.8 in Chapter 1 in Part I of this User’s Guide)
is mounted onto the 2theta arm a second diffracted beam PreFIX module can be mounted, for instance: to
automatically switch from a programmable receiving slit to an X’Celerator or a PIXcel detector between two
measurements.
CAUTION Always have a diffracted beam optical module mounted at the

PreFIX position of the 2theta arm when you move the 2theta arm.
If you have a second PreFIX position in your system we recommend
that you have a module mounted at both of the PreFIX positions
when you move the 2theta arm.
NOTE: Some diffracted beam PreFIX modules can only be used at a specific distance from the heart of the
X’Pert PRO goniometer, related to a specific diffracted beam PreFIX position. If your X'Pert PRO
system comprises a PW3096/60 Second Diffracted Beam PreFIX Carrier, this specific position is
indicated on the Acceptance Test Form delivered with your system.
Diffracted beam PreFIX modules and (mounting of) their accessories are described in Part II of the User’s Guide
in Chapters 16 to 20.
Page 4.8 07.03.27

4.4.4 Detectors
Detectors can be inserted into the detector interfaces on the diffracted beam PreFIX modules. The detector is
fixed into position by two spring-loaded balls. The exceptions to this are the X’Celerator and the PIXcel used as
a line detector which are mounted on a PreFIX interface to allow them to be directly mounted at the PreFIX
position on the 2theta arm. Detectors are described in Chapter 21 in Part II of this User’s Guide.
4.4.5 Safe Angle Settings

In some situations, collisions between two hardware components or between a hardware component and the
sample could occur. For instance: when a mono-capillary is mounted on an X’Pert PRO MRD system. In these
circumstances we recommend the following course of actions:
1. Determine the safe range of the various goniometer and stage settings (including the samples to be
measured) in the configuration used.
2. Enter the minimum and maximum of the safe goniometer and stage settings into the data collector
software. This prevents the goniometer and the sample stage from being sent to a position where a
collision is possible. Please note that hardware stops are set in the factory to limit the ω and 2θ angle
settings to a safe range.
CAUTION Normally the X’Pert PRO system resets itself automatically when it
is switched on, or after power is restored after a power failure. This
reset procedure involves driving the goniometer to its hardware
zero points (and, if present, driving all of the motions of a sample
cradle or a sample changer through their full range). This could
cause collisions between the sample stage or the sample and other
hardware components. If collisions are likely to occur you should
disable the automatic reset in the data collector software. This
activates an initialization wizard that guides you through the
procedure. This gives you the opportunity to remove hardware
components and/or the sample stage and the sample before the
system is reset.
4.4.6 Sample Preparation

Correct sample handling is an important part of the X-ray diffraction measurement. In order to obtain accurate
analytical results; samples must be carefully and correctly prepared, mounted and aligned, prior to the
measurements. Considerations for the preparation of powder samples are given in Appendix B to this User’s
Guide. This appendix also provides information about the preparation of different types of samples in PW18xx
Circular Sample Holders, PW1172/01 Stationary Sample Holders, and powder samples prepared in glass
capillaries.
4.4.7 Sample Mounting

Different sample types and different sample characteristics to be measured require different sample holders and
sample stages. The range of sample stages available for X’Pert PRO diffraction systems is given in Chapters 11
to 13 in Part II of this User’s Guide. These chapters also provides information about the types of sample and
their characteristics that can be measured with the various sample stages.
Mounting and alignment procedures are given for each sample stage. When these procedures are correctly
followed, the sample will be flush with the reference height of the sample stage and unwanted tilts in the surface
orientation are minimized.
07.03.27 Page 4.9

CAUTIONS 1. It is essential that samples are mounted securely. Loose samples

and sample holders can damage the diffraction system.
2. Powders falling out of a sample holder can contaminate the
system.
Misalignment of samples in the diffractometer causes sample height displacement errors. These errors may cause
shifts of the diffraction peaks in the measurement. Sample tilt may cause defocusing of the X-ray beam, leading
to broadening of the peaks and a decrease in peak intensity.
When the sample is correctly mounted and aligned you can begin your measurements.
4.5 SWITCHING THE SYSTEM OFF

When you have completed your measurements, or if the exchange of optical modules or sample stages requires
that you initialize the system, you can switch the system off according to the following procedure:
1. Set the HT generator X-ray tube settings to minimum values (15 kV and 5 mA).
2. Switch the HT generator off by turning the HT key switch on the control and display panel counter-
clockwise. The “X-rays On” lamp on top of the enclosure will go out.
3. Press the “Standby” button on the control and display panel. The “Power On” indicator lamp will go out
and the “Standby” indicator lamp will light.
4. Completely close the cooling water system’s taps: first, the tap on the supply line; and then the tap on
the return line.
5. If you are not going to use the X’Pert PRO system for some time you can also switch the system’s mains
supply off.
Page 4.10 07.03.27

Chapter 5
General Maintenance
Contents
5.1 Introduction......................................................................................................................... 5 - 3
5.2 PreFIX Modules .................................................................................................................. 5 - 3
5.3 Spinner Changer ................................................................................................................. 5 - 4
5.4 Cooling System.................................................................................................................... 5 - 4
5.4.1 Water Filters ........................................................................................................................... 5 - 5
5.4.1.1 Main Water Inlet Filter .......................................................................................... 5 - 5
5.5 Instrument Enclosure Fan Dust Filter.............................................................................. 5 - 6
5.6 Lights.................................................................................................................................... 5 - 7
5.6.1 Interior Inspection Lamps ...................................................................................................... 5 - 7
5.6.2 X-RAYS ON Lamp ................................................................................................................ 5 - 7
5.7 Replacement Parts .............................................................................................................. 5 - 9
07.03.27 Page 5.1

Page 5.2 07.03.27

Part I - Chapter 5: General Maintenance
5.1 INTRODUCTION
X'Pert PRO systems are installed and aligned by a PANalytical Service Engineer. In addition the system has its
acceptance tests completed by the engineer. To ensure that your system works efficiently there are some
maintenance procedures you will need to carry out at specific intervals, the maintenance schedule is given in
Table 5.1. This table shows the recommended frequency of checking the items to be maintained.
This chapter contains instructions that will enable you to replace the water filters, a dust filter on the enclosure
fan and lamps that may eventually become defective. Where necessary the type number for parts that may need
replacement have been included at the end of this chapter. Information about the care of the surfaces of the
PreFIX mountings is also provided.
Maintenance procedures for the X-ray tubes are given in Part II of this User’s Guide - Chapter 1. For
maintenance procedures for the non-ambient stages and their related equipment, please refer to the
documentation supplied with these items.
Table 5.1: Maintenance Schedule
Items Maintenance Frequency Section
PreFIX surfaces Every two months, or after 10 5.2

exchanges; whichever comes first
Spinner changer When necessary 5.3
X-ray tube filters and O-rings We strongly advise that this is II - 1.4.10
performed every six months
Main cooling water filters Every six months 5.4
Enclosure fan dust filter Every six months 5.5
5.2 PREFIX MODULES

The polished reference surfaces of the precision locating and locking devices of all PreFIX optical modules, as
well as the U-shaped optics holder must be regularly examined for possible signs of corrosion.
If no corrosion is found we recommend that you cover the reference surfaces with a thin film of oil (Shell Tellus
10). Use a Chamois leather cloth, with its tip dipped in some oil.
The PreFIX modules must be stored in dry conditions on the wooden supports provided. A PreFIX module on
a wooden support is shown in Figure 5.1.
If there is evidence of corrosion, the corroded surfaces must be cleaned by rubbing it with a Chamois leather
cloth, dipped in thin oil (Shell Tellus 10). The Chamois leather cloth and oil are supplied with the system. Check
that the PreFIX optics securing screw and the spring loaded countersunk locking screw is covered with a film
of grease. If the screws are dry use a small clean paint brush dipped in some Shell Tivela Compound A to grease
them.
07.03.27 Page 5.3

Figure 5.1: PreFIX Module on its Wooden Support
5.3 SPINNER CHANGER

If your system includes a sample changer and/or spinner, remove any excess dust from them using a small hand-
held vacuum cleaner.
5.4 COOLING SYSTEM

Production of X-rays in a tube is a very inefficient process, 99% of the applied energy is converted into heat
within the anode, this heat would melt the tube anode if the anode is not properly cooled. Water is used as the
cooling medium and a continuous water flow must be guaranteed for efficient operation of the X-ray tube.
CAUTION
Effective cooling of the anode is essential to prevent the anode
melting.
An uninterrupted flow of cooling water of at least 3.5 liter per minute with a maximum inlet temperature of
35 ºC is required for adequate heat transfer. If the water flow drops below this flow rate, safety device switches
will switch off the high tension.
Cooling water conditions are given in Part II of this User’s Guide - Chapter 1 - section 1.2.5, more information
is provided in the XRD X’Pert Tube Instruction Manual [2].
Page 5.4 07.03.27

5.4.1 Water Filters

Water filters are built into the cooling system to protect the system from dirt deposits. There are two filters:
• Between the tap and the main water inlet of the generator (see Figure 5.2).
• At the water inlet of the X-ray tube, just before the water reaches the rear of the tube anode (see XRD
X’Pert Tube Instruction Manual [2]).
The main filter can be cleaned or changed as required. The procedures for changing or cleaning the main water
filter is described in section 5.4.1.1. The procedures for changing or cleaning the water filter in the X-ray tube
is described in Chapter 5 of the XRD X’Pert Tube Instruction Manual [2].
5.4.1.1 Main Water Inlet Filter

The water filter assembly should be attached firmly to the wall to allow you to unscrew the blue water filter
container easily. The following procedure tells you how to change and/or clean the water inlet filter:
1. Switch off the high tension and the mains power supply according to the procedure given in Chapter 4
in Part I of this User’s Guide.
2. Ensure that the water taps are closed.
3. Press the red bleed button on top of the filter holder to release any residual water pressure. A little water
might flow out.
NOTE: We advise you to have some tissues or a cloth ready to wipe away any spilled water.
4. Unscrew the blue water filter container. You will probably spill some water.
5. Remove the used filter and replace it with a new or clean filter.
NOTE: The filter can be cleaned by rinsing it in clean water or in a 10% solution of hydrochloric acid
(HCl).
6. Screw the blue water filter container onto the filter assembly.
7. Turn the water tap on and press the red bleed button until water starts to flow from it.
8. Check the filter assembly for leaks. If there are any leaks turn the tap off, remove the filter assembly and
then refit it.
The system is now ready for use.
07.03.27 Page 5.5

Bleed
Button
IN OUT
Figure 5.2: Water Filter Assembly
5.5 INSTRUMENT ENCLOSURE FAN DUST FILTER

The instrument enclosure has a dust filter in front of the MPPC cooling fan (Figure 5.3). This dust filter will need
to be removed and cleaned or replaced regularly (every six months). The dust filter is mounted on the inside of
the left-hand bottom panel. To remove the dust filter:
1. Switch off the high tension and mains supply to the system according to the procedure given in Chapter
4 in Part I of this User’s Guide.
2. Remove the left-hand bottom cover of the enclosure.
3. Undo the two knurled screws that hold the dust filter cover in place and remove the cover.
4. Lift the dust filter out; clean or replace the filter as necessary.
5. Replace the dust filter and fit the cover back on, securing the cover with two knurled screws.
6. Fit the cover back onto the system.
7. Switch on the mains supply and the high tension according to the procedure given in Chapter 4 in Part I
Some systems are equipped with an additional fan at the rear of the enclosure to cool the electronic circuitry.
This fan is also equipped with a dust filter. The dust filter can be taken off the fan for cleaning by just pulling its
securing cover off.
Page 5.6 07.03.27

CAUTION
Do not operate the system if the dust filters are not fitted.
Enclosure Fan
Dust Filter
Figure 5.3: Instrument Enclosure Fan and Dust Filter Location
5.6 LIGHTS
There are three lamps that can be replaced by the user. They are the two fluorescent inspection lamps inside the
enclosure and the X-RAYS ON lamp, inside the cover on top of the enclosure.
5.6.1 Interior Inspection Lamps

The two lamps inside the enclosure are push fit lamps. You can replace them as follows:
1. Switch the enclosure light off by pressing the “Light” push-button on the enclosure display panel.
2. Replace the lamp. Be careful when you pull them out not to pull too hard and break them on the side of
the enclosure.
3. Switch the light on and check that the new lamp functions correctly.
5.6.2 X-RAYS ON Lamp

The X-RAYS ON lamp forms part of the safety circuit and must be changed if it is not functioning.
Proceed as follows to replace the X-RAYS ON lamp inside the cover on top of the enclosure:
1. Switch off the high tension and mains supply to the system according to the procedure given in Chapter
4 in Part I of this User’s Guide.
2. Loosen the four screws that hold the X-RAYS ON cover in position (refer to Figure 5.4).
3. Slide the clamps sufficiently sideways to lift the cover off the enclosure.
07.03.27 Page 5.7

4. Replace the long life lamp as follows (refer to Figure 5.5):

a. Make a note of which color power wire is in which connector, loosen the two screws holding the
power wires in place and disconnect the wires.
b. Undo the four securing screws at the corners of the lamp’s board.
c. Replace the lamp board and reverse steps a and b, making sure that you reconnect the wires to the
connectors as noted in step a.
5. Refit the cover, slide the clamps back into position and tighten the four screws.
6. Switch on the mains supply and the high tension according to the procedure given in Chapter 4 in Part I
NOTE: We advise you to keep a spare long life lamp near to the system.
Figure 5.4: X-RAYS ON Lamp Cover
Figure 5.5: Long Life Lamp
Page 5.8 07.03.27

5.7 REPLACEMENT PARTS

The replacement parts that you will need to perform the procedures described in this chapter are shown in Table
5.2. They are delivered as part of the system. We have also included the part numbers of the items in case you
wish to order any of the parts as spare parts.
Table 5.2: Spare Parts
Items Part Number Details
Shell Tivela Compound A grease 5322 390 20155 5.2

Main water filter 5322 694 14813 5.4
Filter cartridge 5322 480 54034 5.4.1
Enclosure fan dust filter 5322 480 10208 5.5

Lamps (inside the enclosure) 5322 134 50042 5.6.1
X-RAYS ON lamp 5322 134 41155 5.6.2
07.03.27 Page 5.9

Page 5.10 07.03.27

Chapter 6
Fault Correction
Contents
6.1 Introduction......................................................................................................................... 6 - 3
6.2 Instrument off-line.............................................................................................................. 6 - 3
6.2.1 Resetting the Thermal Fuses in the Regulated and Unregulated Mains Supply .................... 6 - 4
6.3 HT Generator Will Not Switch On ................................................................................... 6 - 5
6.3.1 Front and/or Rear Doors are not Correctly Closed................................................................. 6 - 6
6.3.2 Resetting the Thermal Fuse in the MPPC .............................................................................. 6 - 6
6.4 Shutter Will Not Open........................................................................................................ 6 - 7
6.4.1 Microswitches on the Tube Shield are Opened...................................................................... 6 - 7
6.4.2 Door Lock Stuck .................................................................................................................... 6 - 8
6.5 Incorrect (Diffracted) X-ray Beam 2Theta Position........................................................ 6 - 8
6.6 Intensity Incorrect .............................................................................................................. 6 - 9
6.7 Spurious Peaks in the Diffractogram.............................................................................. 6 - 10
6.8 Sample Fluorescence......................................................................................................... 6 - 11
07.03.27 Page 6.1

Page 6.2 07.03.27

Part I - Chapter 6: Fault Correction
6.1 INTRODUCTION
X'Pert PRO systems can be operated safely and efficiently after installation and alignment by a PANalytical
Service Engineer. General procedures for the correct operation of the equipment are given in Chapter 4 in Part
I of this User’s Guide. If, however, your system does not operate correctly, or the results (intensity, peak
position) are not according to the specifications, you must take corrective action to remove the problem. This
chapter provides an overview of the possible solutions to problems that may appear, as listed in Table 6.1. If
your problem persists after you have attempted to correct the fault, or if your problem is not listed in this chapter,
make a note of the complete problem including all relevant information and contact your nearest PANalytical
service organization.
Table 6.1: Overview of Problems Described in this Chapter
Described in
Problem Detected
Section
It is not possible to make a connection between the PC (data collector 6.2

software) and the diffractometer: Instrument off-line.
It is not possible to switch on the high tension generator 6.3

OR
the high tension generator has been unintentionally switched off.
Shutter will not open. 6.4

The 2θ position of a (diffracted) X-ray beam is wrong. 6.5
The intensity of the (diffracted) X-ray beam is incorrect. 6.6
Unexplained (and unidentified) peaks occur in the diffraction pattern. 6.7
6.2 INSTRUMENT OFF-LINE

The X’Pert PRO system is controlled by data collector software running on a PC. If it is not possible to go on-
line (make a connection between the diffractometer and the PC) check the situations given in Table 6.2.
Table 6.2: Probable Causes for Instrument Off-line and their Solutions
Described in
Cause Solution
Section
The system is not switched on (Power Switch the system on. I - 4.3
indicator lamp is not lit).
Incorrect setting of the COM port and Enter the correct parameters for the Data collector
baud rate in the data collector COM port and baud rate. software’s help
software.
Thermal fuses in the unregulated mains Reset the thermal fuses. 6.2.1
supply are open circuit.
Thermal fuses in the regulated mains Reset the thermal fuses. 6.2.1
supply are open circuit.
07.03.27 Page 6.3

6.2.1 Resetting the Thermal Fuses in the Regulated and Unregulated

Mains Supply
The thermal fuses in the unregulated mains supply (with code numbers F601 and F602) are thermal cut-out fuses
that reset by pressing them in so that they are almost flush with the panel. The location of these fuses is given in
Figure 6.1.
The thermal fuses in the regulated mains supply (with code numbers F401, F402 and F403) are thermal cut-out
fuses that reset by pressing them on like a switch.
Fixing Screw Fixing Screw

Fixing Screw
F401 F403 F601 F602

Regulated F402 Unregulated
Mains Mains
Figure 6.1: Rear View of the PW3040/60 X’Pert PRO Instrument Enclosure
Proceed as follows to reset the thermal fuses:
1. Remove the lower rear panel by unscrewing the three fixing screws and lifting the panel away from the
instrument enclosure to gain access to the fuses F401, F402, F403, F601 and F602.
2. Reset the fuse(s).
3. Replace the panel.
4. Switch the system on again according to the procedure given in Chapter 4 of Part I of this User’s Guide.
If the fault persists, switch the system off and call your local PANalytical service organization.
Page 6.4 07.03.27

6.3 HT GENERATOR WILL NOT SWITCH ON

If the HT generator cannot be switched on it is not possible to produce X-rays for diffraction measurements. The
cause of this problem is usually an unsafe signal coming from the HT safety loop which is described in section
2.3.2 of Chapter 2 in Part I of this User’s Guide, or an unsafe signal from the Multi Purpose Power Converter
(MPPC) unit. An overview of the possible reasons for unsafe signals and their suggested solutions is given in
Table 6.3.
Table 6.3: Probable Causes for HT Generator Failure and their Solutions
Described in
Cause Solution
Section
HT key turned off. Turn the HT key on. I - 4.3

Somebody tried to open the front or rear Open the instrument enclosure doors, 6.3.1
doors of the X’Pert PRO instrument close them correctly; and then switch the
enclosure when the shutter on the tube generator on again.
shield was open.
Water flow interrupted during a Clean or replace the water filters. I - 5.4.1
measurement, or, Check that the water hoses are not -
the water flow is less than 3.5 liter/minute. kinked or compressed.
Clean or replace the X-ray tube filter. II - 1.4.10
The X-ray tube is not correctly fitted in the Install the X-ray tube correctly. II - 1.4.5
tube shield.
The identification plug and/or the HT cable Insert the plugs firmly into their sockets. II - 1.4.5
safety plug are not (correctly) inserted into
their sockets.
One of the X-RAYS ON lamps is defective:

1. The yellow X-RAYS ON lamp on top of
the instrument enclosure (E702). Replace the X-RAYS ON lamp. I - 5.6.2
2. The X-RAYS ON lamp on the control
and display panel.
3. The external X-RAYS ON lamp Call your local PANalytical service -
connected to X602. organization.
Call your local X-ray Safety Officer. -
No high tension supplied by the MPPC Reset thermal cut-out fuse F301 on the 6.3.2
because the thermal cut-out fuse is open MPPC.
circuit.
The X-ray tube is defective and flashes Replace the X-ray tube with a new one. II - 1.4
during the start-up procedure.
If the HT generator still cannot be switched on after you have checked the possible causes of failure given in
Table 6.3, switch the system off and call your local PANalytical service organization.
07.03.27 Page 6.5

6.3.1 Front and/or Rear Doors are not Correctly Closed

If the front and/or rear doors are not correctly closed (somebody tried to open them) when the shutter on the tube
shield was open, the HT generator will be automatically switched off. In this situation not all of the
microswitches in the safety loop are closed. The location of the microswitches is given in Figure 6.2.
To rectify this problem, close the front and rear doors correctly so that all of the microswitches are closed and
switch the generator on again.
Lamp
Back Door
Door Door
Back Door
Back Door
HT Cable Back Door

Door
Door
Door Lock
Shutter Close
X-rays On lamp
Connectors for
external X-rays
On lamp
Figure 6.2: Location of the Microswitches in the PW3040/60 Instrument Enclosure
6.3.2 Resetting the Thermal Fuse in the MPPC

The thermal fuse in the MPPC (code number F301) is a thermal cut-out fuse that is reset by switching it on. The
location of this switch is shown in Figure 6.3.
Reset the thermal fuse as follows:
1. Remove the lower front panel by unscrewing the two fixing screws and lifting the panel away from the
instrument enclosure to gain access to the fuse F301.
2. Switch the fuse to reset it.
3. Replace the panel.
4. Switch the system on again according to the procedure described in Chapter 4 in Part I of this User’s
Guide.
If the problem persists, switch the system off and contact your nearest PANalytical service organization.
Page 6.6 07.03.27

Figure 6.3: Location of the MPPC Thermal Cut-out Fuse in the PW3040/60 Instrument Enclosure
6.4 SHUTTER WILL NOT OPEN

The shutter on the tube shield closes automatically if the HT or shutter safety circuits are not completely
(correctly) closed (give an unsafe signal). Fault correction in the HT safety circuit is described in section 6.3.
This section describes fault correction on the shutter safety circuit.
6.4.1 Microswitches on the Tube Shield are Opened

The shutter will not open if the safety microswitches on the tube shield next to the shutter are open. These
microswitches will be activated when you fit an incident beam PreFIX module on the incident beam PreFIX
position of a PW3050/6x Goniometer. Check that the shutter lever correctly actuates the microswitch.
Information about adjusting the shutter lever is given in section 4.4.3.1 in Chapter 4 in Part I of this User’s
Guide.
07.03.27 Page 6.7

6.4.2 Door Lock Stuck

When a “Shutter open” command is sent to the system, the front doors are automatically locked by a solenoid
operated lock. This prevents the door being opened when the shutter is open. To ensure system safety, a
microswitch (“Doors Lock”, see Figure 6.2) monitors the functioning of the lock.
If the doors do not lock, the microswitch will not close, the shutter will not open and a message is sent to the data
collector software. If this happens, try to rectify the problem by moving the doors so that the locking mechanism
will work, and try to open the shutter again.
6.5 INCORRECT (DIFFRACTED) X-RAY BEAM 2THETA POSITION

If the position of a diffraction peak is measured at an incorrect 2θ position in the diffractogram, or if the direct
X-ray beam is not centered around 2θ = 0º, the following corrective actions may help:
• Measure a 2theta - theta scan on a standard sample (for example: the Si pressed powder reference sample
(refer to section 1.4.6.8 in Chapter 1 of Part I of this User’s Guide), or the Si(111) single crystal (part of
PW3132/62) and check the peak positions with those given in the Acceptance Test Form. This will help
you determine whether the problem is sample dependent or not.
• Check if the actual configuration of the X’Pert PRO system matches the configuration being used by the
data collector software.
• Check if the (application) offsets in ω and 2θ have been correctly introduced. The X-ray mirror on the
standard incident beam PreFIX position and the hybrid monochromator both offset the incident beam by a
certain amount (refer to Chapters 6 and 7 in Part II of this User’s Guide). These offsets must be entered
into the data collector software.
• Check if the sample is correctly mounted so that its surface is flush with the sample height reference plane.
For more information refer to section 4.4.7 in Chapter 4 in Part I of this User’s Guide.
• Check if the correct characteristic radiation is being used. If necessary you can change the X-ray tube with
another tube which has the required anode material according to the procedure as described in sections
1.4.4 and 1.4.5 in Chapter 1 in Part II of this User’s Guide. If your system is an X’Pert PRO Alpha-1
system, comprising a PW3113/60 Incident Beam Johansson Monochromator, you can tune the
monochromator crystal to the correct (Kα1) wavelength setting. This procedure is described in section
7.3.3.4 in Chapter 7 in Part II of this User’s Guide.
• Check if the X-ray tube’s focus is in the correct position (point or line). If necessary you can change the
tube focus position according to the procedure as given in section 1.4.7 in Chapter 1 in Part II of this User’s
Guide.
• Check if the X-ray tube height is correctly positioned. A tube height alignment check is described in section
1.4.9 in Chapter 1 in Part II of this User’s Guide.
Page 6.8 07.03.27

6.6 INTENSITY INCORRECT

If the intensity of a diffracted or direct X-ray beam is not as expected or not in accordance with the specifications,
the corrective actions given in this section may help rectify the problem.
NOTES: 1. Direct beam intensities are determined using a new X-ray tube. X-ray tube intensities decrease
10% per 1 000 hours of normal operation.
2. Incident beam modules are subject to X-ray beams with a high intensity. When an incident
beam module has been extensively used, the materials from which it is constructed begin to
show degraded surfaces. This means that extensively used incident beam modules may not
completely reach the intensities specified on the Acceptance Test Form delivered with the
instrument, which were determined with a new X-ray tube.
• Check that there are no (unintended) beam attenuators or filters in the X-ray beam path.
• Check if the automatic beam attenuator (if present) is switching in and out correctly.
• Check if the attenuator factors for the beam attenuators used have been correctly entered into the data
collector software.
• Check if the slits and mask sizes used in the X-ray beam path are correctly set.
• Check if the correct type of Soller slits are being used.
• If you have more than one diffracted beam path on your system, check
a. that you have selected the correct one in the data collector software,
b. that you have the correct diffracted beam optical modules mounted, and
c. that two diffracted beam optical modules mounted on adjacent positions do not touch each other,
causing an incorrect mounting of at least one of the modules.
• Check that you have selected the right detector in accordance with the configuration used in the data
collector software.
• Check if you have set the correct values for the high voltage and the anode current from the high tension
generator.
• Check that the X-ray beam is not obstructed by the sample, the sample stage, or the incident or diffracted
beam optics.
• Check to see if the X-ray beam is completely accepted by the sample, and that the incident beam is not
irradiating the sample stage or any other mounting device.
• Check if the X-ray tube’s focus is in the correct position (point or line). If necessary you can change the
tube focus position according to the procedure as given in section 1.4.7 in Chapter 1 in Part II of this User’s
Guide.
• Make sure that the sample is correctly mounted and aligned. Sample misalignment can cause peak shifts
and/or loss of detected intensity, procedures for the correct alignment of samples are given in Chapters 11
to 13 in Part II of this User’s Guide.
• Check if the (application) offsets in ω and 2θ have been correctly introduced. The X-ray mirror on the
standard incident beam PreFIX position and the hybrid monochromator both offset the incident beam by
a certain amount (refer to Chapters 6 and 7 in Part II of this User’s Guide). These offsets must be entered
into the data collector software.
• Check if the PreFIX modules are correctly mounted. The PreFIX mounting screws should always be
tightened using a torque of between 2.0 Nm and 2.5 Nm, avoiding the use of excessive force. For more
information about mounting PreFIX modules refer to section 4.4.3 in Chapter 4 of Part I of this User’s
Guide.
07.03.27 Page 6.9

• Check if the X-ray tube height is correctly positioned. A tube height alignment check is described in section
• Check that the flat crystal monochromator, if present, is correctly aligned for the wavelength used.
Alignment of the flat crystal monochromator is described in section 19.2.1.2.1 in Chapter 19 in Part II of
this User’s Guide.
• Check that the incident beam Johansson monochromator, if present, is correctly aligned for the Kα1
characteristic radiation. Alignment of the incident beam Johansson monochromator is described in section
7.3.3.4 in Chapter 7 in Part II of this User’s Guide.
• Check if the PHD levels for the detector are correctly set in the data collector software. Typical PHD levels
for proportional detectors are: 35% for the lower level and 80% for the upper level. More information about
detectors and PHD levels is given in Chapter 21 in Part II of this User’s Guide.
6.7 SPURIOUS PEAKS IN THE DIFFRACTOGRAM

Diffractograms may contain unexpected (and not identified) peaks. These spurious peaks are not caused by the
normal Bragg diffraction of the X-ray tube anode’s Kα radiation. They may have been created by one of the
following phenomena:
• Beta-peaks
Beta-peaks in a diffractogram are caused by characteristic Kβ radiation from the X-ray spectrum of the
X-ray tube. The position of the beta-peak relative to the alpha-peak can be visually observed in the
phase identification program X’Pert HighScore, or in the X’Pert Data Collector.
Beta-peaks can be suppressed by placing either a monochromator or a beta-filter in the X-ray beam
path.
• Tungsten Lα peaks
In old tubes the anode may become contaminated with tungsten deposit, which gives rise to an
additional characteristic W Lα line in the X-ray tube’s spectrum. As a result, small peaks related to the
W Lα radiation (with a wavelength of 0.14767 nm (1.4767Å)) may show up in the diffractogram. If a
diffractogram is recorded with copper radiation the W Lα peaks will appear at the low angle side of
strong reflections. If a nickel foil is used as a beta-filter with copper radiation the W Lα peak is masked
by the K-absorption edge of nickel (see the bullet point about absorption edges below).
The position of the W Lα peak relative to the alpha-peak can be visually observed in the phase
identification program X’Pert HighScore.
If the intensity of the W Lα peak becomes too high it may become necessary to replace the X-ray tube
with a new one. Tube removal and installation is described in section 1.4 in Chapter 1 in Part II of this
User’s Guide.
• White radiation peaks (or humps)
The spectrum emitted by an X-ray tube contains, not only the characteristic radiation, but also a
significant amount of white radiation. If you are working with a single beta-filter, part of this radiation
may pass the filter and cause broad humps at low angles in the diffractogram.
The amount of white radiation is strongly influenced by the kV setting of your generator.
You can test for the presence of white radiation by experimenting with the kV settings for your X-ray
tube.
Page 6.10 07.03.27

• Escape peaks in the low angle regions of diffractograms

Peaks in the low angle regions of diffractograms may be caused by the interaction of high energy
X-rays with the detecting medium in X-ray detectors. Because of the nature of their origin they are
called escape peaks. The creation of escape peaks in the low angle regions of diffractograms is
described in more detail in section 21.1.3.2 in Chapter 21 in Part II of this User’s Guide.
Production of escape peaks in the low angle regions of a diffractogram can be avoided in two ways:
1. Place an incident or a diffracted beam monochromator the X-ray beam path so that only the
characteristic radiation used in the experiment will be detected.
2. Set the generator voltage at a level lower than the absorption edge of the element giving rise to the
X-ray fluorescence.
• Absorption Edges
Absorption edges are the discontinuous changes in the absorption coefficient of a material used as a
beta-filter. They may appear as almost vertical steps at the low angle side of a strong reflection in a
diffractogram recorded with a beta-filter in the X-ray beam path. Sometimes these edges are seen as
peaks by peak search algorithms.
Absorption edges can be avoided by using a monochromator instead of a beta-filter in the X-ray beam
path.
• Scatter from surfaces other than the sample
Any polycrystalline material is capable of diffracting X-rays at certain angles. Depending on the
position of these materials in the X-ray path, their diffracted X-rays could reach the detector. A well
known source of these spurious peaks is the powder sample holder. If the size of the divergence slit is
so large that not only the sample, but also the sample holder is irradiated; it could result in the
appearance of spurious peaks, or an unexpected increase in background. Make sure that you do not
over-irradiate your sample at any 2θ angle, or use programmable slits in constant length mode.
You can use the data collector software to display the irradiated length on your sample as a function of
the actual incident beam angle. Please refer to the on-line help of your data collector software for more
information.
When working with non-ambient chambers, a small hump may be visible in the diffractogram at around
7º 2θ, this hump is caused by the chamber’s windows. You can remove this hump by using either a
PW3x94/32 Anti-scatter Slit, or a programmable anti-scatter slit.
6.8 SAMPLE FLUORESCENCE

A good peak-to-background ratio is of great importance when it comes to correctly interpreting diffractograms.
In order to get a high peak-to-background ratio, the background intensity must be suppressed as much as
possible. One of the possible sources of background in a diffractogram is sample fluorescence, that is:
characteristic radiation of the elements in the sample produced by the incident X-ray beam. Almost all elements
will emit fluorescence radiation. However, fluorescence radiation is most visible when its energy is close to that
of the characteristic radiation used to generate the diffractogram.
There are several methods of suppressing as much as possible of sample fluorescence:
• Use of an incident or diffracted beam monochromator
Monochromators are very efficient in selecting the characteristic radiation used in the diffraction
experiment and reducing the fluorescent radiation of other elements. Monochromators are used in the
incident as well as in the diffracted beam path.
When a diffracted beam monochromator is used, the main source of fluorescent radiation entering the
detector is when the sample has a high concentration of the same element as that of the X-ray tube's
anode material. For instance, copper samples show a significant background in diffractograms recorded
with Cu Kα radiation.
07.03.27 Page 6.11

When an incident beam monochromator is used, the monochromatic incident beam creates sample
fluorescence from elements with an atomic number two lower than that of the X-ray tube's anode
material. For instance, monochromatic Cu Kα radiation creates fluorescence from Co atoms; Co Kα
radiation excites fluorescence from Mn atoms.
• Use of a beta-filter
Beta-filters reduce the characteristic Kβ radiation and the high energy part of the X-ray tube's spectrum.
If atoms in the sample are excited by X-rays of the incident beam and thus create fluorescence radiation
a higher background is observed in the diffractogram. Beta-filters are most efficient when they are
placed in the diffracted beam path. If, however, the sample contains a high concentration of the same
element as that of the beta-filter material, the filter should be placed in the incident beam path between
the X-ray tube and the sample. For instance, when you are working with nickel samples and Cu Kα
radiation, the beta-filter must be inserted close to the X-ray tube.
• Choice of appropriate characteristic radiation
An alternative to reduce sample fluorescence from samples containing a high concentration of the
transition metals from the fourth row in the periodic system is to use Mo Kα radiation. Please note that
the short wavelength of Mo Kα radiation condenses the diffractogram along the 2theta axis.
• Setting Pulse Height Discrimination (PHD) levels of the detector used
Detectors generally have the capability to define an energy window for the detected pulses, controlled
by the pulse height discrimination (PHD) electronics. This window has a lower level (usually set to
35% for proportional detectors) and an upper level (usually set to 80%). If sample fluorescence is
causing the background in your diffractogram to be very high, increasing at higher 2theta angles, you
may reduce this effect by choosing a lower level closer to the 50% level of the main energy peak, for
example: 45%. However, remember that when you do that, you also discard part of the diffraction
signal.
This section has provided you with general information about reducing background intensities caused by sample
fluorescence. However, we advise you to make your own investigations into how to obtain the best peak-to-
background ratios in the diffractograms recorded from your particular samples.
Page 6.12 07.03.27

Part II
Chapter 1
X-ray Tubes
Contents
1.1 General................................................................................................................................. 1 - 3
1.1.1 Applications............................................................................................................................ 1 - 3
1.2 Ceramic Diffraction X-ray Tubes ..................................................................................... 1 - 3
1.2.1 General Tube Specifications .................................................................................................. 1 - 6
1.2.2 Power Characteristics ............................................................................................................. 1 - 6
1.2.3 Spectral Purity ........................................................................................................................ 1 - 6
1.2.4 Environmental Conditions...................................................................................................... 1 - 6
1.2.5 Cooling Water Conditions...................................................................................................... 1 - 6
1.3 Tubes .................................................................................................................................... 1 - 7
1.3.1 PW3373/00 XRD X’Pert Tube Cu LFF ................................................................................. 1 - 7
1.3.2 PW3373/10 Special XRD X’Pert Tube Cu LFF .................................................................... 1 - 7
1.3.3 PW3376/00 XRD X’Pert Tube Co LFF ................................................................................. 1 - 8
1.3.4 PW3378/00 XRD X’Pert Tube Cr LFF.................................................................................. 1 - 8
1.3.5 9430 922 00051 XRD X’Pert Tube Mo LFF ......................................................................... 1 - 8
1.3.6 9430 922 00151 XRD X’Pert Tube Fe LFF........................................................................... 1 - 8
1.4 Use ........................................................................................................................................ 1 - 9
1.4.1 General ................................................................................................................................... 1 - 9
1.4.2 Safety Precautions .................................................................................................................. 1 - 9
1.4.2.1 High Tension.......................................................................................................... 1 - 9
1.4.2.2 Beryllium ............................................................................................................. 1 - 10
1.4.3 Unpacking the X-ray Tube ................................................................................................... 1 - 10
1.4.4 Removal of the X-ray Tube from the Tube Shield............................................................... 1 - 10
1.4.5 Tube Installation................................................................................................................... 1 - 12
1.4.6 Tube Storage......................................................................................................................... 1 - 13
1.4.7 Changing the X-ray Tube Focus .......................................................................................... 1 - 14
1.4.8 Changing the Tube Shield Position (Extended MRD Systems)........................................... 1 - 15
1.4.8.1 Placing the Tube Shield at the Extended Position ............................................... 1 - 15
1.4.8.2 Placing the Tube Shield at the Standard Position ................................................ 1 - 16
1.4.9 Tube Alignment Check and Adjustment .............................................................................. 1 - 16
1.4.9.1 Tube Height Coarse Check and Adjustment........................................................ 1 - 16
1.4.9.2 Tube Height Fine Check and Adjustment............................................................ 1 - 19
1.4.10 X-ray Tube Maintenance...................................................................................................... 1 - 22
07.03.27 Page 1.1

Page 1.2 07.03.27

Part II - Chapter 1: X-ray Tubes
1.1 GENERAL
An X-ray tube basically consists of an evacuated envelope containing an anode, a cathode (filament), a focusing
cylinder and exit windows. The working principle of an X-ray tube is shown in Figure 1.1.
When a current is passed through the tungsten filament, electrons are thermally emitted. These electrons are then
accelerated towards the anode by the high voltage differential between the anode and the cathode. The electrons
striking the anode cause emission of X-rays. The X-ray emission spectrum is a superposition of a broad band of
continuous radiation (also called Bremsstrahlung or white radiation) and discrete lines, characteristic for the
anode material. These X-rays exit the tube through thin beryllium windows.
The conversion of electrons into X-rays is a very inefficient process, only about 1% of the applied energy is
converted to X-rays. The remainder of the energy is converted to heat within the anode. Because of this the back
of the anode is cooled.
Electrons can also be scattered from the anode and strike other parts of the tube such as the window. The
temperature of the window can therefore rise to hundreds of degrees centigrade. The window is made of
beryllium (atomic weight 4) in order to minimise the absorption of X-rays.
1.1.1 Applications
The wavelength of the characteristic radiation from an X-ray tube depends on the anode material, therefore,
tubes with various anode materials are available. The most commonly used tube anode material is Cu. Table 1.1
shows the available tube anode materials and their applications.
1.2 CERAMIC DIFFRACTION X-RAY TUBES

The type of X-ray tube used in X’Pert PRO is the ceramic diffraction X-ray tube. The appearance of the ceramic
diffraction X-ray tube is shown in Figure 1.2. The ceramic tube consists of a metal body containing a grounded
anode, four beryllium windows, an electronic tube recognition connector, a shielded HT (High Tension)-
connection, a radiation shield and water cooling facilities, and of a ceramic insulator part, containing a focusing
cylinder, a cathode and an ion getter vacuum pump. A point focus mark indicates the position of the point focus
window.
When it is mounted inside a suitable tube shield, the tube is held by its reference plane at the top ensuring that
the thermal expansion of the tube only minimally affects the distance between the anode and the reference plane
of the tube.
During operation the anode is kept at ground potential.
The ceramic tube fits in the tube shield which is delivered with the PW3040/60 X’Pert PRO Instrument
Enclosure. A socket on the tube enables the type of tube to be electronically identified. The position of the
X-ray tube in the tube shield with respect to line or point focus is automatically recognized.
General and particular specifications and operating instructions for ceramic diffraction X-ray tubes are given in
this section and in sections 1.3 and 1.4. For more detailed information refer to the instruction manual [2]
delivered with your tube.
07.03.27 Page 1.3

Coolant Be Window Ceramic Insulator
Water Out
HT Connection
Contacts
Anode
Automatic
Tube Recognition
High Vacuum
Water In
Cathode / Focusing Metal Tube RD9173
Filament Cylinder Body
Figure 1.1: XRD X’Pert Tube - Schematic Drawing
Figure 1.2: XRD X’Pert Tube - Physical View
Page 1.4 07.03.27

Figure 1.3: XRD X’Pert Tube - Socket for High Tension Cable
Table 1.1: X-ray Tube Anode Material, Characteristic Wavelength and Usage
Anode Wavelength Wavelength Wavelength

Most Common Use
Material Kα1 (Å) Kα2 (Å) Kα (Å)
Mo 0.709317 0.71361 0.71075 For highly absorbing materials and materials

that exhibit very small unit cell dimensions
like metals. Extensively used for structure
determination on single crystals.
Cu 1.540593 1.54442 1.54187 Normal powder diffraction work. Phase

identification, quantitative analysis. High
resolution diffraction.
Co 1.78900 1.79289 1.79030 Normal powder diffraction work on speci-
mens containing large amounts of Fe in order
to avoid fluorescence in Cu Kα radiation.
Fe 1.93608 1.94002 1.93739 For applications where Cu and Co tubes

cause undesired sample fluorescence.
Cr 2.28975 2.29365 2.29105 Residual stress analysis in steels, for materials

with large unit cell dimensions like clay miner-
als, organic materials, superconductors.
07.03.27 Page 1.5

1.2.1 General Tube Specifications

Focus type LFF (Long Fine Focus)
Focus dimensions 12 mm x 0.4 mm
Focus quality To COCIR specifications
Take-off angle (with no intensity loss over range)
line focus 0º - 17º (also dependent on shutter opening)
point focus 0º - 20º (also dependent on shutter opening)
Be window diameter 14 mm
Be window thickness 300 μm
1.2.2 Power Characteristics

Maximum high tension 60 kV
Maximum anode current 55 mA
Maximum anode power Dependent on anode material
Advised power settings 80% - 85% of maximum power
Advised standby ratings 30 - 40 kV, 10 - 20 mA
1.2.3 Spectral Purity

Foreign lines measured with a beta-filter at 40 kV relative to the Kα line:
On delivery <1%
Increase per 1000 hours of tube life
<1% for tubes with Cu or Fe anode
<2% for tubes with Cr or Co anode
<6% for tubes with Mo anode
1.2.4 Environmental Conditions

Operating temperature +5 °C to +40 °C
Storage temperature -40 °C to +70 °C
Electrical safety IEC1010-1
1.2.5 Cooling Water Conditions

The cooling water used should not cause corrosions or deposit sediment in the tube. If the water is dirty or
contains an unduly high concentration of salts, use of a closed cooling system employing clean, not distilled
water, may be necessary.
Quality See Appendix C of the XRD X’Pert Tube Instruction Manual [2].
Flow 3.5-6 l/minute
Maximum pressure 0.8 MPa
Minimum pressure 0.35 MPa
Pressure drop at
3.5 l/minute 0.2 +/- 0.04 MPa
Max. temperature 35 °C
Min. temperature Depends on dew point of air
NOTE: It is better, and safer, to keep the water flow well above the minimum suggested.
Page 1.6 07.03.27

CAUTIONS 1. Do not use distilled water or de-ionized water because this

will attack the metal.
2. Do not use anti-freeze liquids in your closed cooling circuit as

this may lead to deposits building up on the anode causing
inadequate cooling.
For further cooling water conditions refer to the XRD X’Pert Tube Instruction Manual [2].
Low water temperature combined with high air humidity can lead to condensation on the metal parts of the tube.
This could lead to tube damage. In order to prevent such condensation, the temperature of these parts should be
kept above the dew point.
1.3 TUBES
This section describes the particular specifications of the ceramic X-ray tubes used in X’Pert PRO. General
specifications are given in section 1.2.
1.3.1 PW3373/00 XRD X’Pert Tube Cu LFF

High power ceramic diffraction X-ray tube with copper anode.
Maximum power 2.2 kW
Maximum voltage 60 kV
Maximum current 55 mA
Recommended
maximum settings 40 kV, 55 mA, or 45 kV, 45 mA
Be window transmission
for Cu Kα radiation 94%
NOTE: If your system includes an X-ray Mirror for Cu radiation (PW3088/60, PW3148/63, PW3152/63),
a Hybrid Monochromator (PW3147/x0, PW3149/63, PW3150/63), or a PW3113/60 Incident Beam
(Johansson) Monochromator used with Cu radiation, you should use the PW3373/10 X-ray tube
(section 1.3.2) and NOT this one.
1.3.2 PW3373/10 Special XRD X’Pert Tube Cu LFF

High power ceramic diffraction X-ray tube with copper anode. Specifically designed for use with X-ray Mirrors
(PW3088/60, PW3148/63, PW3152/63), Hybrid Monochromators (PW3147/x0, PW3149/63, PW3150/63) and
PW3113/60 Incident Beam Curved Crystal (Johansson) Monochromator.
Recommended
maximum settings 45 kV, 40 mA
for Cu Kα radiation 94%
07.03.27 Page 1.7

1.3.3 PW3376/00 XRD X’Pert Tube Co LFF

High power ceramic diffraction X-ray tube with cobalt anode.
Recommended
for Co Kα radiation 92%
NOTE: If you are using the ceramic cobalt X-ray tube together with an X-ray Mirror for Co radiation
(PW3088/66, PW3148/66), or a PW3113/60 Incident Beam (Johansson) Monochromator, the
recommended high-tension generator settings are 40 kV and 40 mA.
1.3.4 PW3378/00 XRD X’Pert Tube Cr LFF

High power ceramic diffraction X-ray tube with chromium anode.
Recommended
for Cr Kα radiation 82%
1.3.5 9430 922 00051 XRD X’Pert Tube Mo LFF

High power ceramic diffraction X-ray tube with molybdenum anode.
Recommended
for Mo Kα radiation 98%
1.3.6 9430 922 00151 XRD X’Pert Tube Fe LFF

High power ceramic diffraction X-ray tube with iron anode.
Recommended
for Fe Kα radiation 86%
Page 1.8 07.03.27

1.4 USE
1.4.1 General
The following remarks should be taken into consideration in order to make sure that you use the tube properly.
X-ray tubes are delicate components and must be handled with care at all times. A minor shock, such as can
occur when a tube is placed on a table, can cause damage.
Maximum ratings must not be exceeded. Exceeding these limits can cause unacceptable heat levels which will
damage the tube target, lower the efficiency of the focal spot, or even destroy the tube. The advised maximum
power settings depend on the anode material of the X-ray tube. They are specified in section 1.3. If your
application does not require the X-ray tube’s maximum output intensity we recommend that you use a power
setting that is approximately 80% - 85% of the maximum setting.
Every time a tube is switched on, first increase the voltage (kV) and then the current (mA). When switching off
the tube, first decrease the current, and then the voltage.
If an X-ray tube is new or if the HT has not been applied to the tube in the last 100 hours, we advise you to start
the normal tube breeding procedure in order to ensure stable operating conditions. A fast breeding should be
used for tubes which have not been switched on in the last 24 hours. Automatic conditioning procedures on
X’Pert PRO systems can be performed with the use of the data collector software. For more information on tube
breeding refer to the XRD X’Pert Tube Instruction Manual [2].
Do not leave the X-ray tube in stand-by mode at high current settings, as this may unnecessarily reduce the
lifetime of the filament. The advised stand-by ratings are: between 30 kV and 40 kV, and between 10 mA and
20 mA.
The output intensity of the X-ray tube will decrease in time. This means that the X-ray tube will need to be
replaced when the intensity has dropped considerably. Normally, X-ray tubes are replaced when the intensity
has decreased to 70% of the original value.
Never switch off the water supply as a means of switching off the instrument.
1.4.2 Safety Precautions

There are two major safety precautions that need to be observed when removing, installing or maintaining
X-ray tubes; High Tension and Beryllium.
1.4.2.1 High Tension

Before removing the HT cable from the X-ray tube the high tension generator and mains must be switched off.
Refer to the switching off procedure given in Chapter 4 in Part I of this User’s Guide.
WARNINGS 1. THE VOLTAGE ON THE HT CABLE, CONNECTED TO THE X-RAY

TUBE, DECAYS SLOWLY TO ZERO WHEN THE GENERATOR IS
SWITCHED OFF. ALWAYS WAIT FOUR MINUTES AFTER SWITCHING
OFF BEFORE DISCONNECTING THE CABLE AND AS AN ADDITIONAL
PRECAUTION ALWAYS TOUCH THE CENTRAL POINTS OF THE HT
CONNECTOR TO AN EARTHED POINT ON THE ENCLOSURE EACH
TIME IT IS DISCONNECTED. THIS WILL ENSURE THAT THE HT
CAPACITOR IN THE GENERATOR IS FULLY DISCHARGED.
2. IT IS ESSENTIAL THAT THE WATER CONNECTIONS DO NOT LEAK

AS THIS COULD CAUSE FLASH OVERS IN THE GENERATOR OR THE
HT CABLE WHICH MAY RESULT IN INJURY OR DAMAGE TO THE
EQUIPMENT.
07.03.27 Page 1.9

1.4.2.2 Beryllium
The X-ray tube has four beryllium windows which are coated with a protective layer. Contact with beryllium
must be avoided because it is poisonous.
WARNING FUMES AND DUST FROM BERYLLIUM METAL (OR ITS COMPOUNDS)
ARE HAZARDOUS IF INHALED. DURING USE, CORROSION OF THE
BERYLLIUM WINDOW MAY OCCUR (WHITE POWDER FORMS ON THE
WINDOW SURFACE), BUT THE WINDOW SHOULD NOT BE CUT,
MACHINED OR OTHERWISE REMOVED.
NOTE: Any parts of the human body that accidentally come in contact with beryllium must be washed
immediately in soap and water.
Tube disposal must comply with all national and local registrations governing beryllium. You can, if you wish,
send a used tube back to the PANalytical tube factory. Please fill in the Tube End-of-Life Report supplied with
the X-ray tube, this information helps us in improving our X-ray tubes.
1.4.3 Unpacking the X-ray Tube

When you unpack a new X-ray tube:
Check the tubes for obvious signs of damage.
Check that there are no smears, cracks or burn marks on the beryllium windows.
If you are not satisfied with the condition in which you have received the X-ray tube, contact the supplier
immediately.
1.4.4 Removal of the X-ray Tube from the Tube Shield

If another characteristic wavelength is required, or the X-ray output of ceramic X-ray tube falls too low, the tube
needs to be replaced. This section describes the procedure to disconnect the high tension cable and water hoses
and how to remove a tube from the tube shield.
NOTE: The following sections are written based on a vertical system. If you have a horizontal system you
should approach the tasks via the doors at the back of the PW3040/60 Instrument Enclosure.
1. Switch off the high tension and the mains power supply in accordance with the procedure given in
Chapter 4 in Part I of this User’s Guide. If you are going to replace the X-ray tube with another one,
first check that the new tube has been announced in the “Tube Administration” of the “System Settings”
of the X’Pert Data Collector software. If it has not been announced already, do so yourself in the “Tube
Administration”. Then select the new tube on the “X-ray” tab of the “Instrument Settings” window
when you are connected to the instrument. This will start the wizard for changing X-ray tubes.
2. Turn off the cooling water supply line; first the supply line, and then the return line.
3. Disconnect the high tension cable safety plug and the tube identification plug from their respective
sockets (see Figure 1.4).
4. Loosen the four ball headed spring loaded screws that hold the tube in position (see Figure 1.4).
5. Press the securing ring upward and turn it counter-clockwise until it clears the locating lugs, then lower
it over the hoses and cable connected to the bottom of the tube.
The securing ring, shown in Figure 1.4, is a bayonet fit over the two locating lugs shown in Figure 1.1.
6. Pull the tube gently out of the tube shield, holding it by its base, and lay it on its side on the enclosure
base.
Page 1.10 07.03.27

WARNING
DO NOT TOUCH ANY OF THE FOUR BERYLLIUM WINDOWS ON THE
TUBE.
Allen Screws (4x)
Bayonet Connector Water Hose

Ring
Spring-loaded
Screw (4x)
High Tension
Cable
Earth Cable
Tube Identification
Cable
High Tension Cable

Safety Plug
Figure 1.4: X-ray Tube and Tube Shield
CAUTIONS 1. The internal water pipes on the tube can be easily damaged if
care is not taken when sliding the tube in or out of the tube
shield. If the pipes are damaged the water flow will be restricted
which will damage the tube anode.
2. The tube and hoses will still have some water in them when they
are disconnected so put some absorbent paper under the tube
to soak up any possible spillage.
7. Use a spanner to undo the water hose connectors and remove them from the tube.
NOTE: Do not undo the jubilee clips that attach the hoses to the connectors because the hose will be
damaged if the clips are removed and refitted a few times.
07.03.27 Page 1.11

WARNING THE VOLTAGE ON THE HT CABLE, CONNECTED TO THE X-RAY TUBE,

DECAYS SLOWLY TO ZERO WHEN THE GENERATOR IS SWITCHED OFF.
ALWAYS WAIT FOUR MINUTES AFTER SWITCHING OFF BEFORE
DISCONNECTING THE CABLE AND AS AN ADDITIONAL PRECAUTION
ALWAYS TOUCH THE CENTRAL POINTS OF THE HT CONNECTOR TO AN
EARTHED POINT ON THE ENCLOSURE EACH TIME IT IS DISCONNECTED.
THIS WILL ENSURE THAT THE HT CAPACITOR IN THE GENERATOR IS
FULLY DISCHARGED.
8. Undo the four Allen screws (first the two short screws, and then the two long screws) holding the HT
connector in place (see Figure 1.4). Pull the connector away from the base of the tube. If necessary you
can screw the two long screws into the extra screww holes to give you more grip in order to help pull
the plug out. Do not forget to touch the central parts of the HT connector to an earthed ground.
9. Move the X-ray tube to a safe place in accordance with local regulations. If the tube is at its end-of-life,
you can send it back to the PANalytical tube factory. Refer to the XRD X’Pert Tube Instruction Manual
[2] for more information about tube disposal and return. Please fill in the Tube End-of-Life Report
supplied with the X-ray tube, this information is valuable for improving the quality of our X-ray tubes.
1.4.5 Tube Installation

This section describes how to mount an (new) X-ray tube into the tube shield. Before mounting the tube, please
take the following remarks into account. Never use excessive force. When you are inserting the tube into the tube
shield take care to protect the beryllium windows. Mechanical connections to the tube must be firm and secure,
but not so tight as to cause damage to either the tube or the tube shield.
1. Clean the rubber tip and the yellow plug of the high tension plug and cover it with a film of silicon
grease (see Figure 1.5), a tube of this grease is delivered with the system. Also clean the high tension
socket.
2. Remove the plastic covers from the tube.
3. Remove any dust from the tube using a clean cloth. In extreme cases, use a soft clean cloth dipped in
alcohol to clean the beryllium windows.
4. Slide the HT connector into the tube, making sure that the cutouts match the connections on the tube
base.
5. Fit and tighten the HT connector Allen screws (see Figure 1.4). Tighten the two long screws first and
then the two short ones.
6. Fit the water hoses making sure that the IN hose matches the IN connector (indicated on the X-ray tube)
and the OUT hose matches the OUT connector. Ensure that the bayonet ring can pass over the
connections and fit into place.
7. Slide the X-ray tube carefully into the tube shield making sure you do not touch the sides of the shield,
particularly the internal water pipes. The lugs on the side of the tube will locate in the tube shield
channels.
8. Check that the tube is fitted correctly for the type of focus required (Line or Point). The point focus
position is marked on the tube body.
NOTE: If the tube is in the wrong position, rotate it by 90º to select the correct focus option.
9. Slide the securing ring over the hoses and after locating the ring on the bayonet pins push the ring
upward and tighten it by turning it clockwise. Take care that the HT safety cable is not clamped
between the tube shield and the bayonet ring.
Page 1.12 07.03.27

Figure 1.5: Tube High Tension Cable Plug

10. Connect the high tension cable safety plug and the tube identification plug into their sockets (see Figure
1.4).
11. Secure the tube in position with the four ball headed screws as follows:
Turn the screws until they are tight.
Release each screw by 20°, this is necessary to compensate for tube expansion during operation.
12. Turn the water on and check for leaks.
13. Check the valve, used to pump the water out of the system earlier, for leaks.
14. Switch on the mains and the high tension according to the procedure given in Chapter 4 in Part I of this
User’s Guide. Use an automatic conditioning procedure for tube breeding. If you are using the data
collector software’s X’Pert Wizard for tube exchange the software will automatically handle this for
you. Refer to the XRD X’Pert Tube Instruction Manual [2] for more information about tube breeding.
15. Check the water flow using the data collector software. The water flow must be between 3.5 l/min and
5 l/min.
16. Check tube alignment as described in section 1.4.9.
1.4.6 Tube Storage

X-ray tubes must be stored in a clean container (for example: the standard packaging) in a clean environment.
The storage temperature must be between -40 °C (233 K) and +70 °C (343 K). Drain all water from the tube
cooling system before storing the tube. The tube cooling system must be really dry, if necessary use an air dryer
with a maximum pressure of 1 atmosphere to dry the tube out. Fit the plastic covers delivered with the tube onto
the tube for storage.
07.03.27 Page 1.13

1.4.7 Changing the X-ray Tube Focus

The position of the tube Point Focus is marked as shown in Figure 1.2. To change the focus from Point to Line
or from Line to Point the tube will need to be rotated through 90° in the tube shield. To do this:
1. Switch off the high tension according to the procedure given in Chapter 4 in Part I of this User’s Guide.
2. Select the new focus position on the “X-ray” tab in the X’Pert Data Collector’s “Instrument Settings”
window when you are connected to the instrument. This starts the wizard for changing the the tube’s
focus.
3. Loosen the four ball headed spring loaded screws that hold the tube in position (see Figure 1.4).
4. Remove the tube identification plug and the HT cable safety interlock plug (Figure 1.4).
5. Unlock the knurled bayonet connector ring (Figure 1.4) by pressing and turning it 90° counter-
clockwise then pulling it away from the tube.
6. Carefully pull the tube a few centimeters out of the tube shield, taking care not to touch the X-ray
windows (Figure 1.6).
7. Rotate the tube to the desired position.
8. Carefully slide the tube back into the tube shield.
9. Replace the bayonet ring, the safety plug and the tube recognition plug.
10. Secure the tube in position with the four ball headed screws as follows:
Turn the screws until they are tight.
Release each screw by 20°, this is necessary to compensate for tube expansion during operation.
The data collector software switches the generator on automatically as soon as the wizard for changing the tube’s
focus is finished. If the power does not come on check that the safety plug and the tube recognition plug are
secure. If you opened the rear doors during the previous steps, check that they are closed, that the screw securing
the rear door is tightened, and all the microswitches are activated. The control and display panel on the X’Pert
PRO instrument enclosure will show three static illuminated dots on the “Shutter open” position if the doors are
not correctly closed.
If you have rotated the tube from point focus to line focus, we advise you to check the tube height alignment
according to the procedure given in section 1.4.9.
Locating Lug
Position Tube Identification
Socket
Locating
Lug
Figure 1.6: Rotating the X-Ray Tube
Page 1.14 07.03.27

1.4.8 Changing the Tube Shield Position (Extended MRD Systems)

In X’Pert PRO Extended MRD system the tube shield is mounted onto the PW3032/45 Extended Arm by means
of a PreFIX mounting fitment (T-block). There are two mounting positions for the tube shield on the extended
arm: the standard position and the extended position. These positions correspond to goniometer radii of 320 mm
and 427 mm respectively for the PW3032/45. This section describes how to move the tube shield from the
standard position to the extended position, and vice-versa.
Tube Shield on
PreFIX Unit
X-ray
Mirror
PreFIX
Ge
(220
Ge
)
(22
0)
Interface
Ge [220]
Monochromator 1
2 PreFIX
Mounting
Fitment
U-block PreFIX
Locking
PreFIX Screws
Mounting
Platform
Figure 1.7: Mounting the Tube Shield on the PW3032/45 Extended Arm
NOTE: If the X-ray tube is frequently moved between the standard and extended positions, we recommend
that you regularly clean the polished PreFIX surfaces as described in section 5.2 of Chapter 5 in
Part I of this User’s Guide.
1.4.8.1 Placing the Tube Shield at the Extended Position

Move the tube shield from the standard to the extended position as follows:
1. Dismount any incident beam optical modules.
2. Loosen the PreFIX locking screw on the PreFIX mounting platform underneath the X-ray tube, using
the T-bar PreFIX screwdriver.
3. Carefully slide the tube shield along the mounting platform to the extended position (position 1 in
Figure 1.7).
4. Fix the tube shield at the extended position by tightening the PreFIX locking screw.
5. Mount the PreFIX interface at the standard position (position 2 in Figure 1.7) on the mounting
platform.
6. Mount the X-ray mirror onto the PreFIX interface. Make sure that the shutter lever closes the shutter
microswitch on the tube shield.
7. Mount a PW3110/6x High-resolution Monochromator with 12 mm crystals onto the PreFIX position
for incident beam optical modules.
When you have placed the tube at the extended position, we advise you to check the direct beam intensity
according to the procedure given in section 6.2.4.3.2 in Chapter 6 in Part II of this User’s Guide).
07.03.27 Page 1.15
1.4.8.2 Placing the Tube Shield at the Standard Position

1. Dismount the PW3110/6x High-resolution Monochromator from the incident beam PreFIX position.
2. Dismount the X-ray mirror from the PreFIX interface.
3. Dismount the PreFIX interface from the mounting arm.
4. Loosen the PreFIX locking screw on the PreFIX mounting platform underneath the X-ray tube, using
the T-bar PreFIX screwdriver.
5. Carefully slide the tube shield along the mounting platform to the standard position.
6. Fix the tube shield at the standard position by tightening the PreFIX locking screw.
7. Mount an incident beam PreFIX module at the incident beam PreFIX position.
When you have placed the tube at the standard position, we advise you to check the tube height alignment
according to the procedure given in section 1.4.9.
1.4.9 Tube Alignment Check and Adjustment

According to the basic principle of the PreFIX concept, the tube height adjustment is the only adjustment that
needs to be done by the user (see also: section 1.3 in Chapter 1 in Part I of this User’s Guide).
In most cases the tube should be mechanically aligned so that the X-ray beam passes symmetrically through the
goniometer axes; but it may be necessary to check whether in fact this is so.
We especially advise you to perform the tube height alignment check if you have:
• just installed a (new) X-ray tube
or
• rotated the tube from point focus to line focus.
NOTE: This section describes the general procedure for checking and adjusting the tube height. Special
procedures are required for hybrid monochromators and X-ray mirrors, those procedures are given
in Part II of this User’s Guide, in Chapter 7 - section 7.4.4 and Chapter 6 - sections 6.2.4.3 and
6.3.4.3 respectively.
The procedure for checking and adjusting the tube height can be done in two steps: a coarse check and
adjustment, described in section 1.4.9.1; and a fine check and adjustment, described in section 1.4.9.2. Usually,
you only need to do the fine check and adjustment. If you want to check the position of the X-ray beam visually,
you can use the coarse adjustment procedure using the fluorescence disk.
1.4.9.1 Tube Height Coarse Check and Adjustment

This section describes the tube alignment coarse checking procedure. This check is performed visually using the
fluorescence sample disk delivered with your system (see section 1.4.6.9 in Chapter 1 in Part I of this User’s
Guide).
To check the tube alignment:
1. Check that the X-ray tube is in the line focus position. If it is not, rotate the tube as described in section
1.4.7.
2. Mount an incident beam PreFIX module for line focus applications (for example: a programmable
divergence slit).
3. Mount the fluorescence sample disk on the sample holder reference plane, with the fluorescent side
towards the tube and the three parallel lines in the direction of the goniometer axis.
4. Use the data collector software to rotate the omega axis to 90° so that the sample faces the tube at
almost right angles. This will enable you to see the fluorescence line more clearly.
5. If you are using a fixed or programmable divergence slit, set it to 1/2°.
6. Set the generator to the recommended tube settings (see section 1.3).
Page 1.16 07.03.27

7. Switch the instrument enclosure light off and then open the tube shield shutter and look at where the
X-ray beam illuminates the fluorescence disk. If the line is exactly centered around the center black line
(1 in Figure 1.8) proceed with step 8 following; if the line is at 2 or 3 shown in Figure 1.8 close the
shutter and adjust the height of the tube as described in section 1.4.9.1.1 if you have an X’Pert PRO
Extended MRD system. For other X’Pert PRO diffraction systems the procedure is given in section
1.4.9.1.2.
8. Change the divergence slit setting to 1/4° and repeat step 7.
9. You can if you wish check this alignment even more precisely by “tilting” the sample at an angle to the
beam (for example: rotate the omega axis to 45°) and repeating step 7 again.
a. When you have completed the coarse alignment procedure you can continue with the fine check
and adjustment procedure (section 1.4.9.2).
X'Pert PRO X'Pert

Reference Line Reference Line
1
Tube
Anode 3
Divergence Sample
3 Slit (Fluorescence disk)
1
2 2
1
3
Sample Reference Cross
Center
1 = Tube in the correct position

2 = Tube position too low
3 = Tube position too high
Figure 1.8: Movement of Tube Height in relation to the X-ray Beam
1.4.9.1.1 Tube Adjustment for X’Pert PRO Extended MRD Systems

This section describes the tube height adjustment for X’Pert PRO Extended MRD systems.
1. If the line is at position 2 (or anywhere above line 1), the tube height is too low and must be raised. You
do that as follows:
a. Insert an Allen key into the tube height adjustment screw underneath the top of the X-ray tube
shield.
b. Turn the Allen key 45º counter-clockwise.
c. Repeat the tube height alignment check.
d. Continue repeating actions a through c until the X-ray beam is at position 1.
2. If the line is at position 3 (or anywhere below line 1), the tube height is too high and must be lowered.
You do that as follows:
shield.
b. Turn the Allen key 45º clockwise.
NOTE: The tube height adjustment screw has some play built into it to allow for when the adjustment
direction is changed. When you change from adjusting the tube height upwards, to downwards (or
vice-versa) the adjustment screw must be turned through approximately two full rotations before
the tube height starts to change.
07.03.27 Page 1.17

1.4.9.1.2 Tube Adjustment for Systems other than X’Pert PRO Extended MRD
This section describes the tube height adjustment as is used with X’Pert PRO systems other than X’Pert PRO
Extended MRD.
1. If the line is at position 2 (or anywhere above line 1), the tube height is too low and must be raised. You
do that as follows (refer to Figure 1.9):
a. Loosen (turn 45º counter-clockwise) the upper (nearest to the top of the X-ray tube) of the two
knurled knobs at the back of the tube housing.
b. Tighten (turn 45º clockwise) the lower of the two knurled knobs at the back of the tube housing.
e. Now tighten both knobs (ONLY hand tight, no more) to lock the tube into position.
2. If the line is at position 3 (or anywhere below line 1), the tube height is too high and must be lowered.
You do that as follows (refer to Figure 1.9):
a. Loosen (turn 45º counter-clockwise) the lower (furthest away from the top of the X-ray tube) of the
two knurled knobs at the back of the tube housing.
b. Tighten (turn 45º clockwise) the upper of the two knurled knobs at the back of the tube housing.
Upper Knurled
Adjusting Knob
Lower Knurled
Adjusting Knob
Figure 1.9: Tube Height Adjusting Knobs
Page 1.18 07.03.27

1.4.9.2 Tube Height Fine Check and Adjustment

This section describes the tube height fine check and adjustment procedures. This procedure uses the single knife
edge delivered with your system (see section 1.4.6.10 in Chapter 1 in Part I of this User’s Guide).
To check the tube alignment:
1. Check that the X-ray tube is in the line focus position. If it is not, rotate the tube as described in section
1.4.7.
2. Mount an incident beam PreFIX module for line focus applications (for example: a programmable
divergence slit).
3. Mount a programmable receiving slit, or an X’Celerator rotated through 90º (see section 21.4 in
Chapter 21 in Part II of this User’s Guide), or a PIXcel, or a rocking curve attachment, or a triple axis
and rocking curve attachment onto the diffracted beam PreFIX position.
4. Insert a copper (0.2 mm) attenuation foil into the incident beam PreFIX module in order to protect your
detector from being saturated.
6. Insert a beam mask marked 10 into the incident beam PreFIX module.
7. Depending on your diffracted beam path components:
a. If you are using a programmable receiving slit, set it to 3 mm.
b. If a programmable or a fixed anti-scatter slit assembly is mounted onto the programmable
receiving slit, set it to 4º.
c. If you are using an X’Celerator, set it into receiving slit mode and use the maximum active length
(9 mm). Do not insert a slit into the fixed anti-scatter slit holder.
d. If you are using a PIXcel, set it into receiving slit mode and use the maximum active length
e. If you are using a rocking curve attachment, do not insert a slit.
f. If you are using a triple axis and rocking curve attachment, use the data collector software to select
the beam path with the rocking curve assembly. Do NOT insert a slit into the rocking curve
assembly.
8. Mount the alignment shaft onto the goniometer. The alignment shaft for X’Pert PRO MRD systems is
described in section 11.2.1.2 in Chapter 11 in Part II of this User’s Guide). The alignment shaft for
X’Pert PRO MPD systems is described in section 12.10 in Chapter 12 in Part II of this User’s Guide).
9. If you are using an X’Pert PRO MRD system, read the following caution carefully before proceeding.
CAUTION Normally the MRD cradle automatically resets when the system is
switched on or when power is restored after a power failure. The
reset procedure involves driving all motions of the cradle through
their full range. This would cause the cradle and the alignment shaft
to collide. To prevent this happening, use the data collector software
to disable this automatic reset. You then have the opportunity to
remove the alignment shaft before resetting the cradle.
10. Set 2θ to 0º.

11. Set the high tension generator to 30 kV, 40 mA (if you have the ceramic X-ray tube with an iron anode
set the generator to 30 kV, 30 mA).
12. Open the shutter and make a note of the direct beam intensity. If you are using an X’Celerator or a
PIXcel detector, make a stationary measurement and measure for about 10 seconds.
13. Close the shutter and mount the single knife edge (see section 1.4.6.10 in Chapter 1 in Part I of this
User’s Guide) on the alignment shaft. The single knife edge mounted onto the alignment shaft for an
X’Pert PRO MRD system is shown in Figure 1.10.
14. Open the shutter again and measure the intensity. This new value must be between 40% and 60% of the
direct beam intensity without the single knife edge measured in step 11 (see Figure 1.11 and Figure
1.12).
07.03.27 Page 1.19
• If the intensity is within this range, the tube is at the correct height.
• If the intensity is more than 60% of the direct beam intensity without the single knife edge as meas-
ured in step 11, the tube is too low and must be raised.
• If the intensity is less than 40% of the direct beam intensity without the single knife edge as measured
in step 11, the tube is too high and must be lowered.
15. If the tube height is not correct, close the shutter and adjust the tube height as described in section
1.4.9.2.1 (for X’Pert PRO Extended MRD systems) or section 1.4.9.2.2 (for other X’Pert PRO
systems).
Figure 1.10: Single Knife Edge Mounted onto an Alignment Shaft

for X’Pert PRO MRD Systems
1.4.9.2.1 Tube Height Fine Adjustment for X’Pert PRO Extended MRD Systems
This section describes the tube height fine adjustment for X’Pert PRO Extended MRD systems.
1. If the intensity is more than 60% of the direct beam intensity without the single knife edge as measured
in step 11 of section 1.4.9.2, the tube is too low and must be raised, see Figure 1.11 and Figure 1.12.
shield.
b. Turn the Allen key 45º counter-clockwise.
c. Open the shutter and measure the intensity value.
d. Continue repeating actions a through c until the intensity is between 40% and 60% of the direct
beam intensity without the single knife edge measured in step 11 of section 1.4.9.2.
Page 1.20 07.03.27

2. If the intensity is less than 40% of the direct beam intensity without the single knife edge as measured
in step 11 of section 1.4.9.2, the tube is too high and must be lowered (see Figure 1.11 and Figure 1.12).
shield.
b. Turn the Allen key 45º clockwise.
d. Continue repeating actions a through c until the X-ray beam is between 40% and 60% of the direct
beam intensity without the single knife edge measured in step 11 of section 1.4.9.2.
Divergence
Too High Slit
Correct
Position
Detector
Too Low
Tube Focus
Single Knife Edge
Figure 1.11: Direct Beam with Single Knife Edge Intersecting it

Intensity
Maximum
Intensity
60%
Half of
Maximum
Intensity
40%
Minimum
Intensity
Tube Tube Tube Height
too Low Tube in the too High
Correct Position RD9664
Figure 1.12: Direct Beam Intensity with Single Knife Edge Mounted as a Function of Tube Height
Position
07.03.27 Page 1.21

1.4.9.2.2 Tube Height Fine Adjustment for Systems other than X’Pert PRO Extended MRD
This section describes the tube height adjustment as is used with X’Pert PRO systems other than X’Pert PRO
Extended MRD.
1. If the intensity is more than 60% of the direct beam intensity without the single knife edge as measured
in step 11 of section 1.4.9.2, the tube is too low and must be raised, see Figure 1.11 and Figure 1.12.
a. Loosen (turn 45º counter-clockwise) the upper (nearest to the top of the X-ray tube) of the two
knurled knobs at the back of the tube housing.
b. Tighten (turn 45º clockwise) the lower of the two knurled knobs at the back of the tube housing.
d. Continue repeating actions a through c until the X-ray beam is between 40% and 60% of the
direct beam intensity without the single knife edge measured in step 11 of section 1.4.9.2.
2. If the intensity is less than 40% of the direct beam intensity without the single knife edge as measured in
step 11 of section 1.4.9.2, the tube is too high and must be lowered, see Figure 1.11 and Figure 1.12.
a. Loosen (turn 45º counter-clockwise) the lower (furthest away from the top of the X-ray tube) of
the two knurled knobs at the back of the tube housing.
b. Tighten (turn 45º clockwise) the upper of the two knurled knobs at the back of the tube housing.
d. Continue repeating actions a through c until the X-ray beam is between 40% and 60% of the
direct beam intensity without the single knife edge measured in step 11 of section 1.4.9.2.
1.4.10 X-ray Tube Maintenance

Maintenance of the ceramic X-ray tubes should be carried out at least every six months.
Maintenance procedures are provided in Chapter 5 of the X-ray Diffraction XRD X’Pert Tube Instruction
Manual [2].
Page 1.22 07.03.27

Chapter 2
Beam Attenuators and Filters
Contents
2.1 General................................................................................................................................. 2 - 3
2.1.1 Beam Attenuators ................................................................................................................... 2 - 3
2.1.1.1 Applications ........................................................................................................... 2 - 3
2.1.2 Beta-filters .............................................................................................................................. 2 - 3
2.1.2.1 Applications ........................................................................................................... 2 - 4
2.2 Beam Attenuators ............................................................................................................... 2 - 4
2.2.1 Standard Copper Foil Beam Attenuators................................................................................ 2 - 4
2.2.2 PW3087/6x Automatic Beam Attenuator............................................................................... 2 - 6
2.2.2.1 PW3087/60 Automatic Beam Attenuator Nickel (0.125 mm) .............................. 2 - 6
2.2.2.2 PW3087/62 Automatic Beam Attenuator Nickel (0.15 mm) ................................ 2 - 6
2.2.2.3 PW3087/63 Automatic Beam Attenuator Nickel (0.2 mm) .................................. 2 - 6
2.2.2.4 PW3087/66 Automatic Beam Attenuator Iron (0.1 mm) ...................................... 2 - 7
2.2.2.5 Accessories ............................................................................................................ 2 - 7
2.2.3 Beam Attenuators for X-ray Mirrors and Hybrid Monochromators ...................................... 2 - 9
2.2.3.1 Copper Foil (0.1 mm) & Combined Copper / Nickel Beam Attenuators .............. 2 - 9
2.2.3.2 Iron Foil Beam Attenuators ................................................................................... 2 - 9
2.2.4 Use........................................................................................................................................ 2 - 10
2.2.4.1 Beam Attenuator Modes ...................................................................................... 2 - 10
2.2.4.2 Measuring the Attenuation Factor ....................................................................... 2 - 10
2.2.4.3 Exchanging Automatic Beam Attenuators .......................................................... 2 - 10
2.3 Beta-filters ......................................................................................................................... 2 - 11
2.3.1 Standard Beta-filters............................................................................................................. 2 - 11
2.3.1.1 PW3151/03 Nickel Filter ..................................................................................... 2 - 11
2.3.1.2 PW3151/00 Set of Beta-filters ............................................................................. 2 - 11
2.3.2 Beta-filters for X-ray Mirrors............................................................................................... 2 - 12
2.3.2.1 Nickel Filter for X-ray Mirror ............................................................................. 2 - 12
2.3.2.2 Iron Filter for X-ray Mirror ................................................................................. 2 - 12
2.3.3 Large Beta-filters.................................................................................................................. 2 - 13
2.3.3.1 PW 3158/03 Large Nickel Filter.......................................................................... 2 - 13
2.3.3.2 PW3158/00 Set of Large Beta-filters................................................................... 2 - 13
07.03.27 Page 2.1

Page 2.2 07.03.27

Part II - Chapter 2: Beam Attenuators and Filters
2.1 GENERAL
Beam attenuators and filters are described in this chapter. The general use of beam attenuators and filters is
described in this section. The specific beam attenuators and filters used in X’Pert PRO are described in sections
2.2 (attenuators) and 2.3 (filters).
2.1.1 Beam Attenuators

The beam attenuator is an absorber which is placed in the X-ray beam to reduce its intensity by a specific factor.
The attenuation factor is defined as the ratio between the intensity measured without the absorber and the
intensity measured with the absorber. Once it has been defined in the data collector software, this attenuation
factor will be used to correct the observed intensities.
CAUTION
An attenuation foil MUST be mounted in the housing slot in the
beam path in order to attenuate the beam whenever the
measured intensity is expected to exceed the maximum count
rate of the detector being used.
2.1.1.1 Applications
Beam attenuators are used when the intensity of the X-ray beam entering the detector exceeds the maximum
count rate. In this case, a beam attenuator must be inserted into the X-ray path in order to decrease the intensity
to a value low enough to be accepted by the detector.
Beam attenuators can also be used to extend the dynamic range of measurements in which the difference in
intensity between the features being observed is very large. This large intensity difference is often observed in
reflectivity experiments at low angles of incidence. Another example is given by high resolution measurements
where the intensity of the substrate reflections can be much higher than that of, for example: the layer fringes.
2.1.2 Beta-filters
A beta-filter is used to keep as much as possible of the characteristic Kα radiation from the tube whilst
suppressing the Kβ and white radiation.
The filter material that exhibits an absorption edge between the Kα and the Kβ line of an anode material is
selected. By inserting a beta-filter with an appropriate thickness into the X-ray beam, the Kβ line almost
disappears. The effect of the beta-filter material in conjunction with the most used anode materials is illustrated
in the following table.
Table 2.1: Combination of Tube Anode and Beta-filter Materials
K absorption
Tube Anode Beta-filter
Edge of Beta-
Material Material
filter [Å]
Mo Zr 0.68896
Cu Ni 1.488
Co Fe 1.744
Cr V 2.269
07.03.27 Page 2.3

2.1.2.1 Applications
Beta-filters can be placed in either the incident or the diffracted beam path. The choice depends on the type of
sample to be measured. Generally it is advised to place the beta-filter in the diffracted beam path. If, for example,
the atoms in a sample are excited by the incident radiation and thus, in turn, give fluorescence radiation from the
sample, this leads to an increased level of the background. Placing the beta-filter between the sample and the
detector will reduce this background more efficiently.
If, however, the sample contains a high concentration of the same element as the beta-filter material which would
give rise to a high level of sample fluorescence, the filter should be placed in the incident beam path between the
X-ray tube and the sample.
When further reduction of Kβ radiation is required, for instance in situations where the residual Kβ reflection
impairs proper analysis, you can use another beta-filter or a diffracted beam monochromator. Using two beta-
filters or a diffracted beam monochromator will reduce the Kβ intensity to approximately 10-4 of the Kα1
intensity.
We advise you to use a diffracted beam monochromator if sample fluorescence is to be reduced as well as the
Kβ radiation.
2.2 BEAM ATTENUATORS

There are three types of beam attenuator:
• The standard copper foil beam attenuators that are delivered with all X’Pert PRO systems. They are
described in section 2.2.1.
• The automatic beam attenuators PW3087/6x; these beam attenuators are described in section 2.2.2.
• Specific beam attenuators that are delivered as part of the PW3088/6x, PW3148/6x, PW3152/63 and
9430 920 05441 X-ray Mirrors and as part of the Hybrid Monochromators (PW3147/x0, PW3149/63 and
PW3150/63). They are described in section 2.2.3.
2.2.1 Standard Copper Foil Beam Attenuators

Two copper foil beam attenuators are delivered with all X’Pert PRO systems The foil thicknesses are 0.1 mm
and 0.2 mm. The standard copper foil attenuator is shown in Figure 2.1. Their attenuation factors for Cu Kα
radiation are:
Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
The copper foil beam attenuators can be used together with the items listed in Table 2.2. Information on their use
is included in the chapters as listed in the table.
Page 2.4 07.03.27

Table 2.2: Devices that the Standard Attenuators and Beta-filters can be used with
Beam Path Number Item Chapter
I PW3081/60 Programmable Divergence Slit II - 3
I PW3082/60 Fixed Divergence Slit Holder II - 3

I PW3084/60 Incident Beam Collimator with II - 8
exchangeable cups
I PW3084/62 Crossed Slits Collimator II - 8
I PW3145/00 Mono-capillary II - 10
I PW3146/60 X-ray Lens II - 9
D PW3015/x0 X’Celerator II - 21
D PW3093/60 Programmable Receiving Slit II - 16
I = Incident Beam Path

D = Diffracted Beam Path
Figure 2.1: Standard Copper Foil Beam Attenuator
07.03.27 Page 2.5

2.2.2 PW3087/6x Automatic Beam Attenuator

The PW3087/6x Automatic Beam Attenuators contain a metal foil that can be set to be switched in and out of
the X-ray beam either at a fixed angle or at a fixed intensity. The operation is controlled by the data collector
software. The automatic beam attenuator is shown in Figure 2.2.
They can be used together with the items listed in Table 2.3. Mounting instructions are given in the chapters as
shown in Table 2.3.
Table 2.3: Devices that the Automatic Beam Attenuator can be used with
Number Item Chapter
PW3081/60 Programmable Divergence Slit II - 3

PW3082/60 Fixed Divergence Slit Holder II - 3
PW3088/60 X-ray Mirror for Cu Kα radiation II - 6
PW3088/66 X-ray Mirror for Co Kα radiation II - 6
PW3091/x0 Programmable Anti-scatter Slit II - 16
PW3097/60 Rocking Curve Attachment II - 16
PW3120/60 Triple Axis and Rocking Curve Attachment II - 16/19
PW3120/65 Asymmetric Triple Axis and Rocking Curve II - 16/19
Attachment
PW3147/x0 Hybrid Monochromator II - 7
PW3148/63 X-ray Mirror for Cu Kα radiation II - 6
PW3148/66 X-ray Mirror for Co Kα radiation II - 6
PW3149/63 Hybrid Monochromator 2X II - 7
PW3152/63 Focusing X-ray Mirror for Cu Kα radiation II - 6
It is possible to mount more than one automatic beam attenuator on an X’Pert PRO system. However, only one
beam attenuator at a time can be controlled by the data collector software. This automatic beam attenuator must
be connected to the system via the PW3087/61 Beam Attenuator Cable. How to exchange automatic beam
attenuators is described in section 2.2.4.3.
2.2.2.1 PW3087/60 Automatic Beam Attenuator Nickel (0.125 mm)

PW3087/60 is an automatic beam attenuator with a nickel foil intended for use with Cu Kα radiation. The foil is
0.125 mm thick. The attenuation factor is ≈ 200; the exact value is given on the Acceptance Test Form delivered
with the system.

with the system.

0.2 mm thick. The attenuation factor is ≈ 6 000; the exact value is given on the Acceptance Test Form delivered
with the system.
Page 2.6 07.03.27

Connector for Beam

Attenuator Cable
Screws A
Figure 2.2: PW3087/6x Automatic Beam Attenuator Mounted on a PreFIX Module
2.2.2.4 PW3087/66 Automatic Beam Attenuator Iron (0.1 mm)

PW3087/66 is an automatic beam attenuator with an iron foil intended for use with Co Kα radiation. The foil is
with the system.
2.2.2.5 Accessories
2.2.2.5.1 Beam Mask Holder
If you have mounted an automatic beam attenuator onto a programmable or fixed divergence slit, you can also
mount a beam mask holder (that you had to take off the divergence slit in order to mount the automatic beam
attenuator) onto the automatic beam attenuator. If you have mounted an automatic beam attenuator onto an
X-ray mirror and have either a programmable or fixed divergence slit available to you, you can take the beam
mask holder off one of them and mount it onto the automatic beam attenuator.
Mount the beam mask holder onto the automatic beam attenuator by fixing the four screws that hold the beam
mask holder on the appropriate position on the front of the automatic beam attenuator.
Mount the beam mask holder in such a way that the beam masks can be easily inserted and removed.
2.2.2.5.1.1 Aligning the Beam Mask Holder
Align the beam mask holder as follows:
1. Ensure that the X-ray tube is in the line focus position.
2. Mount the fluorescence disk on the sample holder reference plane, with the fluorescent side towards the
tube and the three parallel lines in the direction of the goniometer axis.
3. Insert the 5 mm beam mask into the beam mask holder.
4. Set the generator to the recommended X-ray tube settings (see Part II - Chapter 1, section 1.3).
X-ray beam irradiates the fluorescence disk. If the line is exactly centered around the reference cross
shown in Figure 2.3 the beam mask holder alignment is completed; if the line is not at the reference
cross, close the shutter and adjust the alignment as described in step 6.
07.03.27 Page 2.7

6. Loosen the four screws holding the beam mask holder and adjust its position by shifting along the line
focus orientation and try step 5 again.
7. When you are satisfied that the beam mask holder is correctly aligned, tighten the four screws that you
loosened in step 6.
Reference Cross
Figure 2.3: Beam Mask Holder Adjustment Position on Fluorescence Disk

2.2.2.5.2 Brass Plate
A brass fill plate is included with the beam attenuator. It should be placed between the attenuator and the
programmable divergence slit or the programmable anti-scatter slit when the attenuator is mounted.
2.2.2.5.3 PW3087/61 Beam Attenuator Cable
PW3087/61 is a cable to connect the PW3087/6x Automatic Beam Attenuator to the X’Pert PRO system.
Exchanging automatic beam attenuators is described in section 2.2.4.3.
2.2.2.5.4 Anti-scatter Slit (1.4 mm)
If you have mounted the automatic beam attenuator onto an X-ray mirror you can mount the anti-scatter slit
(provided with the X-ray mirror) onto the automatic beam attenuator.
Mount the anti-scatter slit onto the automatic beam attenuator by fixing the four screws that hold the reflectivity
slit on the appropriate position on the front of the automatic beam attenuator (see Figure 6.4 in Chapter 6 in Part
II of this User’s Guide).
Page 2.8 07.03.27

2.2.3 Beam Attenuators for X-ray Mirrors and Hybrid Monochromators

Specific beam attenuators are designed for use with X-ray mirrors and hybrid monochromators. Those
attenuators are described in this section.
2.2.3.1 Copper Foil (0.1 mm) & Combined Copper / Nickel Beam Attenuators
A copper foil beam attenuator (0.1 mm) and a combined copper (0.2 mm) / nickel (0.02 mm) beam attenuator
are delivered together with the X-ray Mirrors for Cu radiation (PW3088/60 and PW3148/63) and the Hybrid
Monochromators (PW3147/00, PW3147/20, PW3149/63 and PW3150/63). The combined copper/nickel beam
attenuator is also included with the PW3152/63 Focusing X-ray Mirror for Cu radiation. The copper foil
attenuator is shown in Figure 2.4. The combined copper/nickel attenuator has the same appearance. Information
about their use is included in Chapters 6 and 7 in Part II of this User’s Guide. Their attenuation factors for Cu
Kα radiation are:
Copper (0.1 mm): ≈ 100
Combined (0.2 mm / 0.02 mm): ≈ 18 000
The exact attenuation value is given in the Acceptance Test Form delivered with the X-ray mirror or hybrid
monochromator and on the beam attenuator itself.
2.2.3.2 Iron Foil Beam Attenuators

Two iron foil beam attenuators with foil thicknesses of 0.1 mm and 0.2 mm are delivered together with the
X-ray Mirrors for Co radiation (PW3088/66 and PW3148/66). The iron foil (0.2 mm) is also included with the
9430 920 05441 Focusing X-ray Mirror for Co radiation. The physical appearance of the iron foil attenuator is
the same as that of the copper foil beam attenuator shown in Figure 2.4. Information about their use is included
in Chapter 6 in Part II of this User’s Guide. Their attenuation factors for Co Kα radiation are:
Iron (0.1 mm): ≈ 90
Iron (0.2 mm): ≈ 8 000
The exact attenuation value is given in the Acceptance Test Form delivered with the system and on the beam
attenuator itself.
Figure 2.4: Copper Foil Attenuator
07.03.27 Page 2.9

2.2.4 Use
2.2.4.1 Beam Attenuator Modes
How your beam attenuator is used is controlled by the data collector software. There are three modes in which
the beam attenuator can be used, they are given in Table 2.4.
Table 2.4: Beam Attenuator Operating Modes
Mode Application
Do not switch The beam attenuator stays either inserted into (Activated) the X-ray beam
(Activated/Deactivated) path or removed (Deactivated) from the X-ray beam path over the whole
of the measured angular range and for the full measuring time.
At pre-set intensity The beam attenuator is inserted into the X-ray beam path when the
specified count rate (the 'activate' level) is reached, and/or is removed
from the X-ray beam path when the count rate drops below another
specified count rate (the 'deactivate' level).
At pre-set axis position The beam attenuator is inserted into the X-ray beam path when the
diffractometer position on the scan axis is inside the specified interval.
This interval is given by the activate and deactivate axis positions. The
beam attenuator is removed from the beam path when the
diffractometer position on the scan axis is outside the specified interval.
If you have a manual beam attenuator, the data collector software prompts you to insert or remove the attenuator
at the appropriate moments. If you are using an automatic beam attenuator, the nickel or iron foil is inserted into
or removed from the X-ray path fully automatically.
2.2.4.2 Measuring the Attenuation Factor

To determine the attenuation factor of a beam attenuator (either automatic or manual), proceed as follows:
1. Perform a stationary measurement with the beam attenuator not inserted into the X-ray beam path
(deactivated). Make a note of the intensity (I1).
2. Insert the beam attenuator into the X-ray beam path. In the data collector software, set the attenuation
factor to 1.
3. Repeat the measurement and make a note of the intensity (I2).
4. The attenuation factor is the ratio between the intensities (I1 / I2). This factor can be entered into the
data collector software in order to automatically correct the observed intensities.
2.2.4.3 Exchanging Automatic Beam Attenuators

If your system contains more than one PW3087/6x Automatic Beam Attenuator and you want to change the
incident beam PreFIX modules which have an automatic beam attenuator mounted on them, proceed as follows:
1. Switch off your system according to the procedure given in Chapter 4 in Part I of this User’s Guide.
2. Disconnect the connecting cable from the active automatic beam attenuator.
3. Dismount the incident beam PreFIX module on which the automatic beam attenuator (just
disconnected) is mounted.
4. Mount the incident beam PreFIX module that you want to use (which includes an automatic beam
attenuator).
5. Connect the cable disconnected in step 2 to the “new” automatic beam attenuator.
Page 2.10 07.03.27

6. Switch your system on according to the procedure given in Chapter 4 in Part I of this User’s Guide.
7. Report the attenuation factor of the new beam attenuator to the data collector software.
NOTE: In order to avoid “undefined” electrical situations occurring, ensure that you never leave the
connecting cable disconnected from an automatic beam attenuator, even if the beam attenuator is
not being used.
2.3 BETA-FILTERS
Three types of beta-filter are available for all X’Pert PRO diffraction systems, they are:
• Standard beta-filters are described in section 2.3.1. They can be used in a number of incident and dif-
fracted beam PreFIX modules.
• Specific beta-filters to be used together with the X-ray mirrors. These filters are described in section
2.3.2.
• Specific beta-filters which are designed for use with the PIXcel or parallel plate collimators. They are
described in sections 2.3.3.
2.3.1 Standard Beta-filters

2.3.1.1 PW3151/03 Nickel Filter
The PW3151/03 Nickel Filter is a beta-filter that is intended for use with Cu radiation. It can be used as an
incident beam filter and as a diffracted beam filter. It is shown in Figure 2.5. The thickness and intensity
reduction for Kα and Kβ radiation for this filter is given in Table 2.5. Information about mounting and how to
use this Ni filter is given in the chapters listed in Table 2.2.
2.3.1.2 PW3151/00 Set of Beta-filters

PW3151/00 is a set of three beta-filters: iron for Co, vanadium for Cr and zirconium for Mo radiation. The
physical appearance of these filters is the same as the Ni filter (Figure 2.5). The filters can be used in X'Pert PRO
diffraction systems as incident beam filter and as diffracted beam filter. A manganese filter for Fe radiation is
not available. The thickness and intensity reduction for Kα and Kβ radiation for these filters are given in Table
2.5.
How to mount the filter is described in the chapter which covers the device that the filter is fitted into, those
devices and their chapters are shown in Table 2.2.
Table 2.5: Beta-filters
Kβ Intensity Kα Intensity
Tube Anode Beta-filter Thickness
Reduction Reduction
Material Material [μm]
[%] [%]
Mo Zr 80 98 57
Cu Ni 20 99 58
Co Fe 16 99 51
Cr V 13 98 45
07.03.27 Page 2.11

Figure 2.5: Standard Nickel Filter
2.3.2 Beta-filters for X-ray Mirrors

2.3.2.1 Nickel Filter for X-ray Mirror
A nickel filter is included with the PW3088/60, PW3148/63 and PW3152/63 X-ray Mirrors. This beta-filter is
intended for use with Cu radiation. The physical appearance of these filters is shown in Figure 2.6. The thickness
of the filter is 0.02 mm; the intensity reduction is given in Table 2.5.
Information about the use of this filter together with the X-ray mirror is given in Chapter 6 in Part II of this User’s
Guide.
2.3.2.2 Iron Filter for X-ray Mirror

An iron filter with a foil thickness of 16 μm is included with the PW3088/66, PW3148/66 and 9430 920 05441
X-ray Mirrors for use with Co Kα radiation. The physical appearance of this filter is shown in Figure 2.6. The
intensity reduction is given in Table 2.5.
Information about the use of this filter together with the X-ray mirror is given in Chapter 6 in Part II of this User’s
Guide.
Figure 2.6: Nickel Filter for X-ray Mirror
Page 2.12 07.03.27

2.3.3 Large Beta-filters

2.3.3.1 PW 3158/03 Large Nickel Filter
PW3158/03 Nickel Filter is a beta-filter that is intended for use with Cu radiation. The filter can be used with
the PW3018/00 PIXcel detector and PW3017/00 PreFIX Interface for PIXcel or with the PW3098/xx Parallel
Plate Collimators. This foil type is shown in Figure 2.7. How to mount the foil is described in Chapters 18
and 21 in Part II of this User's Guide. The thickness and intensity reduction for Kα and Kβ radiation is given in
Table 2.5.
Figure 2.7: Large Nickel Filter
2.3.3.2 PW3158/00 Set of Large Beta-filters

PW3158/00 is a set of three beta-filters: iron for use with Co, vanadium for Cr and zirconium for Mo radiation.
The physical appearance of these filters is the same as the Ni filter shown in Figure 2.7. The filters can be used
with the PW3018/00 PIXcel detector and PW3017/00 PreFIX Interface for PIXcel or with the PW3098/xx
Parallel Plate Collimators. The thickness and intensity reduction for Kα and Kβ radiation is given in Table 2.5.
How to mount these filters is described in Chapters 18 and 21 in Part II of this User's Guide.
07.03.27 Page 2.13

Page 2.14 07.03.27

Chapter 3
Incident Beam Slits
Contents
3.1 General................................................................................................................................. 3 - 3
3.1.1 Applications............................................................................................................................ 3 - 3
3.1.1.1 Phase Analysis ....................................................................................................... 3 - 3
3.1.1.2 Omega-stress Analysis........................................................................................... 3 - 3
3.1.1.3 Reflectivity & Thin Film Phase Analysis .............................................................. 3 - 3
3.2 PW3081/60 Programmable Divergence Slits.................................................................... 3 - 3
3.2.1 Accessories............................................................................................................................. 3 - 4
3.2.1.1 Beam Masks........................................................................................................... 3 - 4
3.2.1.2 Beta-filters ............................................................................................................. 3 - 5
3.2.1.3 Attenuation Foil ..................................................................................................... 3 - 5
3.2.1.4 PW3085/x0 Soller Slits.......................................................................................... 3 - 6
3.2.1.5 PW3086/00 Incident Beam Anti-scatter Slit Holder ............................................. 3 - 6
3.2.1.6 PW3087/6x Automatic Beam Attenuators ............................................................ 3 - 8
3.2.2 Using Programmable Divergence Slits ................................................................................ 3 - 10
3.2.2.1 Operating Modes.................................................................................................. 3 - 10
3.2.2.2 Determination of Irradiated Length in Fixed Slit Mode ...................................... 3 - 11
3.3 PW3082/60 Fixed Divergence Slit Holder ...................................................................... 3 - 11
3.3.1 Accessories........................................................................................................................... 3 - 12
3.3.1.1 Fixed Divergence Slits......................................................................................... 3 - 12
3.3.1.2 PW3083/00 Fixed Slits for Low Angle Measurements ....................................... 3 - 13
3.3.1.3 Beam Masks......................................................................................................... 3 - 13
3.3.1.4 Beta-filters ........................................................................................................... 3 - 13
3.3.1.5 Attenuation Foil ................................................................................................... 3 - 13
3.3.1.6 PW3085/x0 Soller Slits........................................................................................ 3 - 14
3.3.1.7 PW3086/00 Incident Beam Anti-scatter Slit Holder ........................................... 3 - 14
3.3.1.8 PW3087/6x Automatic Beam Attenuators .......................................................... 3 - 16
3.3.2 Using Fixed Divergence Slits............................................................................................... 3 - 17
3.3.2.1 Determination of Irradiated Length ..................................................................... 3 - 17
3.4 Use of Fixed Slits in Other Devices.................................................................................. 3 - 18
07.03.27 Page 3.1

Page 3.2 07.03.27

Part II - Chapter 3: Incident Beam Slits
3.1 GENERAL
Divergence slits are fitted in the incident beam path to control the equatorial divergence of the incident beam,
and thus, the amount (length) of the sample that is irradiated by the incident X-ray beam.
Divergence slits can also be used in combination with an X-ray mirror or a hybrid monochromator. When used
together with these devices, the slit controls the height of the emerging X-ray beam rather than the divergence.
Two types of slit are available on X’Pert PRO systems: Programmable Divergence Slit (PDS) and Fixed
Divergence Slit(s) (FDS).
This chapter describes the divergence slits that are used with line focus applications. If your application uses
point focus the task of controlling beam divergence is performed by incident beam collimators which are
described in Part II - Chapter 8.
3.1.1 Applications
Typical applications in which the divergence slits are used are: phase analysis, omega-stress analysis,
reflectivity, and thin-film phase analysis.
3.1.1.1 Phase Analysis

In Bragg-Brentano para-focusing geometry, the incident X-ray beam from the line focus of the X-ray tube
diverges in the diffraction plane until it irradiates the sample. The diffracted X-ray beam converges from the
sample until it passes through the receiving slit (the natural focusing point on the goniometer circle) before
diverging again.
Divergence slits are used in Bragg-Brentano geometry for phase analysis to control the divergence of the
incident beam. The divergence angle must be set such that the X-ray beam is completely accepted by the sample.
On the diffracted beam side an anti-scatter slit is used with an acceptance angle the same as the divergence angle.
3.1.1.2 Omega-stress Analysis

Divergence slits can be used for omega-stress analysis where the sample is inclined in the equatorial plane. The
diffracted beam is accepted by a combination of an anti-scatter slit and a receiving slit.
3.1.1.3 Reflectivity & Thin Film Phase Analysis

A combination of a very small divergence slit together with a parallel plate collimator (or a “beam tunnel”
formed by an anti-scatter slit and a receiving slit) is used in the quasi-parallel beam geometry. This set-up is used
for measurements at a fixed angle of incidence on thin films and for reflectivity.
3.2 PW3081/60 PROGRAMMABLE DIVERGENCE SLITS

PW3081/60 is an incident beam PreFIX module with a programmable divergence slit.
The PreFIX programmable divergence slit is shown in Figure 3.1. This module incorporates:
• a slot for an attenuation foil or a beta-filter
• a slot for Soller slits
• a beam mask holder
When the programmable divergence slit is used in the incident beam path a Soller slits assembly with a shutter
lever mounted must be inserted into the slot for Soller slits. This allows the shutter to be actuated.
The distance between the focus of the X-ray tube and the divergence slit is 100 mm.
The distance between the X-ray tube’s focus and the mask position is 115 mm; if an automatic divergence slit
is mounted (see section 3.2.1.6.1) this distance is 136 mm. A set of four incident beam width masks is included
with the programmable divergence slit.
07.03.27 Page 3.3
The divergence slit is software controlled to operate in one of two modes:

• the fixed divergence slit mode, to provide a defined divergence of 4º, 2º, 1, 1/2º, 1/4º, 1/8º, 1/16º or 1/32º.
• the automatic divergence slit mode, to provide a defined irradiated length of 20 to 0.5 mm in 0.1 mm
steps, with the divergence changing automatically as a function of the angle between the incident beam
and the sample surface ω.
The irradiated area can also be offset from the goniometer axis in order to asymmetrically select the area to be
measured on the sample. The offset distance can be applied using the data collector software.
More information about using the programmable divergence slit is given in section 3.2.2.
Figure 3.1: PW3081/60 Programmable Divergence Slit (PDS)
3.2.1 Accessories
3.2.1.1 Beam Masks
Four beam masks marked 5, 10, 15 and 20 are supplied together with the programmable divergence slit. These
masks are used to control the irradiated width on the sample. Beam masks must be installed into the beam mask
holder on the programmable divergence slit. The relationship between the beam mask marking, the goniometer
radius and the irradiated width on the sample for the programmable divergence slit is given in Table 4.1.
Mount the beam mask holder onto the programmable divergence slit by fixing the four screws that hold the beam
mask holder on the appropriate position on the front of the programmable divergence slit. Mount the holder so
that the beam masks can be easily inserted and removed.
Page 3.4 07.03.27

3.2.1.1.1 Aligning the Beam Mask Holder

4. Set the generator to the recommended settings (see Part II - Chapter 1, section 1.3).
loosened in step 6.
Reference Cross
Figure 3.2: Beam Mask Holder Adjustment Position on the Fluorescence Disk
3.2.1.2 Beta-filters
There are four beta-filters that can be used with the programmable divergence slit, they are:
Ni filter (PW3151/03) for Cu Kα radiation
Fe filter (part of set PW3151/00) for Co Kα radiation
V filter (part of set PW3151/00) for Cr Kα radiation
Zr filter (part of set PW3151/00) for Mo Kα radiation
The filter must be installed (mounted) in the slot for attenuation foil or beta-filter as shown in Figure 3.1.
3.2.1.3 Attenuation Foil

A 0.1 mm and a 0.2 mm copper foil are delivered with the X’Pert PRO diffraction system. These foils can be
inserted into the slot for attenuation foil or beta-filter as indicated in Figure 3.1.
Under typical operating conditions the beam from the system can have an intensity which is much greater than
1 000 000 cps. The Miniprop detector (PW3011/20) becomes non-linear in response above 1 000 000 cps and
can be damaged by higher count rates. Please refer to Table 21.1 for a summary of the detectors used in X’Pert
PRO.
07.03.27 Page 3.5

CAUTION An attenuation foil MUST be mounted in the attenuation foil or

beta-filter slot on the programmable divergence slit in order to
attenuate the beam whenever the measured intensity is expected
to exceed the maximum count rate of the detector used.
The attenuation factors of the copper foils for Cu Kα radiation are:

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
The exact value of the attenuation factor for the foil supplied with an X’Pert PRO diffraction system are shown
on the Acceptance Test Form for the system, which is supplied when the system is delivered. This value can be
entered in the data collector software and is used to automatically adjust the measured intensity values. For more
information about the use of a copper attenuation foil refer to Part II - Chapter 2 (section 2.2).
3.2.1.4 PW3085/x0 Soller Slits

Soller slits are used together with the programmable divergence slit to control the axial divergence of the X-ray
beam. Soller slits with a shutter lever must be inserted into the programmable divergence slit in order to activate
the shutter safety switch. The slot for the Soller slits is shown in Figure 3.1.
Three Soller slits are available, their sizes are:
PW3085/10 0.01 rad Soller Slits
WARNING FOR RADIATION SAFETY REASONS, YOU MUST NOT USE THE PW3085/80
0.08 RAD SOLLER SLITS, OR THE PW3085/81 0.08 RAD SOLLER SLITS
(WITH LARGE APERTURE), OR THE PW3085/41 0.04 RAD SOLLER SLITS
(WITH LARGE APERTURE) TOGETHER WITH THE PW3081/60
PROGRAMMABLE DIVERGENCE SLIT.
3.2.1.5 PW3086/00 Incident Beam Anti-scatter Slit Holder

The use of an incident beam anti-scatter slit is advisable when the programmable divergence slit is used together
with the X’Celerator or the PIXcel. In order to use the anti-scatter slit you must first install a PW3086/00 Incident
Beam Anti-scatter Slit Holder. PW3086/00 consists of two anti-scatter slit holders: a short one and a long one.
We advise you to always use the long one unless it does not fit in your diffractometer configuration for geometric
reasons. For more information about the use of an incident beam anti-scatter slit holder refer to Part II - Chapter
20 (section 20.2.1).
You should always use an incident beam anti-scatter slit with an opening one step larger than the (fixed)
divergence slit setting of the programmable divergence slit. For example: use a 1º incident beam anti-scatter slit
when the programmable divergence slit is set to 1/2º.
Page 3.6 07.03.27

3.2.1.5.1 Mounting the Incident Beam Anti-scatter Slit Holder

Mount the anti-scatter slit holder as follows:
1. Remove the beam mask holder from the programmable divergence slit by unscrewing the four screws.
2. Place the anti-scatter slit holder in the position that you just removed the beam mask holder from and
secure it in place using the screws that you just removed in step 1.
3.2.1.5.2 Aligning the Incident Beam Anti-scatter Slit Holder
3. Insert the 5 mm beam mask into the beam mask holder. Do NOT insert an anti-scatter slit.
loosened in step 6.
8. Insert a 1/32º slit into the anti-scatter slit holder until it clicks into place.
9. Set the detector at 0º 2θ and make sure that the direct beam is not obstructed by the sample or the
sample stage.
10. Check (visually) to see if the aperture of the 1/32º slit that you inserted is parallel to the side of the anti-
scatter slit holder. If it is not, use the black adjusting screws on the side of the holder to make it parallel
(you may need to adjust the spring-loaded ball on the other side of the holder to achieve the required
result).
11. Set the programmable divergence slit to a fixed angle of 1º. Insert a copper (0.2 mm) attenuation foil
into the programmable divergence slit.
12. Make a 2θ scan to find the peak position of the direct beam.
13. If the peak is located at 0º 2θ, the incident beam anti-scatter slit is aligned and ready for use.
14. If the peak is not at 0º 2θ, you must turn both of the adjusting screws on the side of the incident beam
anti-scatter slit holder in the same direction and the same amount (for example: both 90º clockwise).
You may need to adjust the spring-loaded ball on the other side of the holder to allow both the screws to
turn the required amount. Make a 2θ scan and check the peak position of the direct beam. Continue
with this step until the peak is located at 0º 2θ, at which time the incident beam anti-scatter slit is
aligned and ready for use.
07.03.27 Page 3.7

Figure 3.3: PW3086/00 Incident Beam Anti-scatter Slit Holder

Mounted on a Programmable Divergence Slit
3.2.1.6 PW3087/6x Automatic Beam Attenuators

The PW3087/6x Automatic Beam Attenuator can be mounted on the front of the programmable divergence slit
replacing the beam mask holder and used in place of the foil described in section 3.2.1.3. The attenuation factor
is entered in the data collector software and is used to automatically adjust the measured intensity values. The
attenuation factor for the automatic beam attenuator is given in the Acceptance Test Form delivered with the
system.
3.2.1.6.1 Mounting the Automatic Beam Attenuator onto a PDS
1. Remove the three screws (marked A in Figure 2.2 in Part II, Chapter 2 of this User’s Guide).
2. Split the automatic beam attenuator apart, the metal part from the painted part. This can be quite
difficult to do, persevere.
3. Remove the four screws holding the beam mask holder in place and then remove the beam mask holder
itself.
4. Place the brass fill plate onto the programmable divergence slit and then fit the metal part (NOT the side
with the alignment pins) of the automatic beam attenuator onto the programmable divergence slit. Use
the four screws supplied with the automatic beam attenuator into the four holes that you just removed
the mask holder screws from and secure it into place.
5. Replace the painted part of the automatic beam attenuator and use the three screws you removed in step
1 to secure it into place.
6. If required you can remount the beam mask holder onto the automatic beam attenuator using the four
small holes in the holder. Mounting instructions are given in section 2.2.2.5.1 of Chapter 2 in Part II of
Page 3.8 07.03.27

Figure 3.4: PW3087/6x Automatic Beam Attenuator

Mounted onto a Programmable Divergence Slit
07.03.27 Page 3.9

3.2.2 Using Programmable Divergence Slits

This section describes the operating modes and the determination of the irradiated area as a function of the
sample position and the size of the incident beam.
3.2.2.1 Operating Modes

The Programmable Divergence Slit (PDS) can be programmed using the data collector software to operate in
two modes, fixed or automatic. These modes are described in Table 3.1.
Table 3.1: PDS Operating Modes and their Application
Mode Size Application
Fixed 4º, 2º, 1º, 1/2º, 1/4º, The size of the divergence slit can be set to one of these fixed
1/8º, 1/16º, 1/32º values.
Automatic 0.5 to 20 mm in steps of 0.5 The irradiated length of the sample can be defined.
mm Depending on the measured ω angle the divergence is auto-
matically changed to ensure that the irradiated length of the
sample remains constant over full measured angular range.
Offset: 0 to minimum value When the programmable divergence slit is used in automatic
of: mode the irradiated length on the sample can be offset by
(irradiated length/2) and setting an offset value in the data collector software. When
(20 - irrad. length/2) mm the offset is set to 0 mm (standard setting) the sample is
in steps of 0.25 mm. symmetrically irradiated with respect to the goniometer axis.
The offset can be set either When a negative value is entered the irradiated area on the
positive or negative. sample is moved towards the X-ray tube, when a positive
value is entered the irradiated area on the sample is moved
towards the detector. The offset value can be set in the range
0 mm to 5 mm in steps of 0.25 mm).
Please note that the relative intensities measured with a PDS in automatic mode will considerably differ from
those measured in fixed mode. If you want to compare the results with data measured with fixed slits you can
use the conversion formula given below.
I FDS R × ( sin ω × sin δ )

F = ----------- = -------------------------------------------------------
-
I ADS L a ( sin2 ω – sin2 ( δ ⁄ 2 ) )
where F = the conversion factor,
IFDS = intensity as measured in fixed divergence slit mode,
IADS = intensity as measured in automatic divergence slit mode,
R = radius of the goniometer,
δ = divergence angle in fixed divergence slit mode,
La = irradiated length on the sample in automatic divergence slit mode,
ω = angle between incident beam and sample surface.
Although the above formula is an approximation it gives sufficiently accurate results for general diffraction
purposes.
Page 3.10 07.03.27

3.2.2.2 Determination of Irradiated Length in Fixed Slit Mode

The length of the area on the sample that is irradiated by the incident beam is dependant on the divergence of
the X-ray beam and the position of the sample with respect to the beam. In the automatic divergence slit mode
the irradiated length on the sample is fixed, the divergence angle is automatically changed as the ω angle
changes. In the fixed divergence slit mode the irradiated length is a function of the divergence angle set in the
data collector software. It can be calculated as follows:
R × ( sin ω × sin δ )
L = -------------------------------------------------
-
( sin2 ω – sin2 ( δ ⁄ 2 ) )
where L = irradiated length on the sample,

δ = divergence angle as set in the data collector software,
3.3 PW3082/60 FIXED DIVERGENCE SLIT HOLDER

The PW3082/60 is an incident beam PreFIX module with a holder for exchangeable fixed divergence slits. It is
shown in Figure 3.5.
It incorporates:
• a slot for an attenuation foil or a beta-filter
• a slot for fixed divergence slits
• a beam mask holder.
When the fixed divergence slit holder is used in the incident beam path a Soller slit with a shutter lever mounted
must be inserted into the slot for Soller slits. This allows the shutter to be actuated (see section 3.3.1.6).
Fixed divergence slits are inserted into the PreFIX module to control the divergence of the incident beam when
the line focus of the X-ray tube is used. The fixed divergence slits come in two size ranges:
4°, 2°, 1°, 1/2° and 1/4° used for standard applications
1/8°, 1/16° and 1/32° used for glancing angle applications
The distance between the focus of the X-ray tube and the divergence slit is 87 mm.
The distance between the X-ray tube’s focus and the mask position is 96 mm; if an automatic beam attenuator
is mounted (see section 3.3.1.8) this distance is 117 mm. A set of four width masks is included with the fixed
divergence slit holder.
07.03.27 Page 3.11

Figure 3.5: PW3082/60 Fixed Divergence Slit Holder
3.3.1 Accessories
3.3.1.1 Fixed Divergence Slits
Six fixed divergence slits marked 4º, 2º, 1º, 1/2º, 1/4º and 1/32º are supplied together with the PW3082/60 Fixed
Divergence Slit Holder. These slits are used to control the divergence of the incident X-ray beam, and thus the
irradiated length on the sample. The fixed divergence slits must be inserted into the slot for fixed divergence slits
on the PreFIX module.
Figure 3.6: Fixed Divergence Slits
Page 3.12 07.03.27

3.3.1.2 PW3083/00 Fixed Slits for Low Angle Measurements

PW3083/00 is a set of fixed slits for low angle measurements, as in thin film phase analysis or reflectivity
applications. It consists of three slits marked 1/8º, 1/16º and 1/32º. These slits must be inserted into the slot for
fixed divergence slits on the PreFIX module.
3.3.1.3 Beam Masks

Four beam masks marked 20, 15, 10 and 5 are supplied together with the fixed divergence slit holder. These
masks are used to control the irradiated width on the sample. Beam masks must be installed into the beam mask
holder on the fixed divergence slit holder. The relationship between the beam mask marking, the goniometer
radius and the irradiated width on the sample for the fixed divergence slit is given in Table 4.2.
Mount the beam mask holder onto the fixed divergence slit holder by fixing the four screws that hold the beam
mask holder on the appropriate position on the front of the fixed divergence slit. Mount the holder so that the
beam masks can be easily inserted and removed.
3.3.1.3.1 Aligning the Beam Mask Holder
loosened in step 6.
There are four beta-filters that can be used with the fixed divergence slit holder, they are:

inserted into the slot for attenuation foil or beta-filter as indicated in Figure 3.5.
can be damaged by higher count rates. Please refer to Table 21.1 for a summary of the detectors used in X’Pert
PRO.
07.03.27 Page 3.13


beta-filter slot on the fixed divergence slit in order to attenuate the
beam whenever the measured intensity is expected to exceed the
maximum count rate of the detector used.

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
The exact values of the attenuation factor for the foils supplied with an X’Pert PRO diffraction system are shown
on the Acceptance Test Form for the system, which is supplied when the system is delivered. This value can be
entered in the data collector software and is used to automatically adjust the measured intensity values. For more
Alternatively, the PW3087/60 Automatic Beam Attenuator can be used instead if the attenuation foil, please
refer to section 3.3.1.8.

Soller slits are used together with the fixed divergence slit holder to control the axial divergence of the X-ray
beam. A Soller slit with a shutter lever must be inserted into the fixed divergence slit holder in order to activate
the shutter safety switch. The slot for the Soller slit is shown in Figure 3.5.
Three Soller slits are available, their sizes are:
(WITH LARGE APERTURE) TOGETHER WITH THE PW3082/60 FIXED
DIVERGENCE SLIT HOLDER.
3.3.1.7 PW3086/00 Incident Beam Anti-scatter Slit Holder

The use of an incident beam anti-scatter slit is advisable when the fixed divergence slit holder is used together
with the X’Celerator or the PIXcel. In order to use the anti-scatter slit you must first install a PW3086/00 Incident
Beam Anti-scatter Slit Holder. PW3086/00 consists of two anti-scatter slit holders: a short one and a long one.
We advise you to always use the long one unless it does not fit in your diffractometer configuration for geometric
reasons. For more information about the use of an incident beam anti-scatter slit holder refer to Part II - Chapter
20 (section 20.2.1).
You should always use an incident beam anti-scatter slit with an opening one step larger than the fixed
divergence slit. For example: use a 1º incident beam anti-scatter slit when a 1/2º fixed divergence slit is inserted.
Page 3.14 07.03.27

3.3.1.7.1 Mounting the Anti-scatter Slit Holder

To mount the anti-scatter slit holder, proceed as follows:
1. Remove the beam mask holder from the fixed divergence slit by unscrewing the four screws.
2. Place the anti-scatter slit holder in the position that you just removed the beam mask holder from and
secure it in place using the screws that you just removed in step 1.
3.3.1.7.2 Aligning the Incident Beam Anti-scatter Slit Holder
3. Insert the 5 mm beam mask into the beam mask holder. Do NOT insert an anti-scatter slit.
loosened in step 6.
8. Insert a 1/32º slit into the anti-scatter slit holder until it clicks into place.
9. Set the detector at 0º 2θ and make sure that the direct beam is not obstructed by the sample or the
sample stage.
10. Check (visually) to see if the aperture of the 1/32º slit that you inserted is parallel to the side of the anti-
scatter slit holder. If it is not, use the black adjusting screws on the side of the holder to make it parallel
(you may need to adjust the spring-loaded ball on the other side of the holder to achieve the required
result).
11. Insert a 1º slit and a copper (0.2 mm) attenuation foil into the fixed divergence slit holder.
12. Make a 2θ scan to find the peak position of the direct beam.
13. If the peak is located at 0º 2θ, the incident beam anti-scatter slit is aligned and ready for use.
14. If the peak is not at 0º 2θ, you must turn both of the adjusting screws on the side of the incident beam
anti-scatter slit holder in the same direction and the same amount (for example: both 90º clockwise).
You may need to adjust the spring-loaded ball on the other side of the holder to allow both the screws to
turn the required amount. Make a 2θ scan and check the peak position of the direct beam. Continue
with this step until the peak is located at 0º 2θ, at which time the incident beam anti-scatter slit is
aligned and ready for use.
07.03.27 Page 3.15


Mounted on a Fixed Divergence Slit Holder
3.3.1.8 PW3087/6x Automatic Beam Attenuators

The PW3087/6x Automatic Beam Attenuator can be mounted onto a fixed divergence slit holder (replacing the
beam mask holder) as shown in Figure 3.8 and is used in place of the foil described in section 3.3.1.5. The
attenuator is used to increase the dynamic range of reflectivity measurements, and to prevent exceeding the linear
range of the detector when measuring the reflected intensity close to the critical angle. The attenuation factor is
entered in the data collector software and is used to automatically adjust the measured intensity values.
3.3.1.8.1 Mounting the Automatic Beam Attenuator onto an FDS
1. Remove the three screws (marked A in Figure 2.2 in Part II, Chapter 2 of this User’s Guide).
3. Remove the four screws holding the beam mask holder in place and then remove the beam mask holder
itself.
4. Fit the metal part (NOT the side with the alignment pins) of the automatic beam attenuator onto the
fixed divergence slit; using the four screws supplied with the automatic beam attenuator into the four
holes that you just removed the mask holder screws from and secure it into place. Ensure that the
automatic beam attenuator is correctly orientated.
6. If required you can remount the beam mask holder onto the automatic beam attenuator using the four
small holes around the slit.
Page 3.16 07.03.27

Figure 3.8: PW3087/6x Automatic Beam Attenuator

Mounted on a Fixed Divergence Slit Holder
3.3.2 Using Fixed Divergence Slits

This section describes the determination of the irradiated area as a function of the sample position and the size
of the incident beam.
3.3.2.1 Determination of Irradiated Length

The length of the area on the sample that is irradiated by the incident beam is dependent on the divergence of
the X-ray beam and the position of the sample with respect to the beam. It can be calculated as follows:
L = -------------------------------------------------
-
( sin2 ω – sin2 ( δ ⁄ 2 ) )
where L = irradiated length on the sample,

δ = divergence angle as is engraved on the fixed divergence slit used,
07.03.27 Page 3.17

3.4 USE OF FIXED SLITS IN OTHER DEVICES

Fixed slits are not only used in the PW3082/60 Fixed Divergence Slit Holder, but also in a number of other
incident and diffracted beam modules to control the height of the X-ray beam.
Information about the use of fixed slits in those devices is given in the chapters listed in Table 3.2.
Fixed Slits that are designed for use as anti-scatter slits in combination with the X’Celerator or PIXcel are
described in Chapter 20 in Part II of this User’s Guide.
Table 3.2: Devices that Fixed Slits can be used with
Type
Fixed Slit Sizes Item Chapter
Number
4º - 1/32º PW3082/60 Fixed Divergence Slit Holder II - 3

PW3092/00 Fixed Anti-scatter Slit Assembly II - 16
4º - 1/16º PW3086/00 Incident Beam Anti-scatter Slit Holder for Divergence Slit II - 20
1/ º - 1/4º PW3086/60 Incident Beam Anti-scatter Slit Holder for X-ray Mirror II - 20
2
PW3086/65 Incident Beam Anti-scatter Slit Holder for Hybrid Monochromator II - 20
PW3086/7x Incident Beam Anti-scatter Slit Holder for Focusing X-ray Mirror II - 20
1/ º - 1/32º PW3088/6x X-ray Mirror II - 6
2
PW3148/6x
PW3147/x0 Hybrid Monochromator for MRD II - 7
PW3149/63 Hybrid Monochromator 2X for MPD II - 7
PW3150/63 Hybrid Monochromator 4X for MPD II - 7
PW3152/63 Focusing X-ray Mirror for Cu Kα Radiation II - 6
1º - 1/32º PW3097/60 Rocking Curve Attachment II - 16

PW3120/65 Asymmetric Triple Axis and Rocking Curve Attachment II - 16/19
0.1 mm PW3098/xx Parallel Plate Collimator II - 18
1 mm PW3097/60 Rocking Curve Attachment II - 16
PW3120/65 Asymmetric Triple Axis and Rocking Curve Attachment II - 16/19
1.4 mm PW3088/6x X-ray Mirror II - 6
PW3148/6x
PW3152/63 Focusing X-ray Mirror for Cu Kα Radiation II - 6
Page 3.18 07.03.27

Chapter 4
Incident Beam Masks
Contents
4.1 General................................................................................................................................. 4 - 3
4.1.1 Applications............................................................................................................................ 4 - 3
4.2 Beam Mask Set (Accessory to PW3081/60 or PW3082/60)............................................. 4 - 3
4.2.1 Irradiated Width ..................................................................................................................... 4 - 4
4.3 PW3089/00 Beam Mask Set ............................................................................................... 4 - 5
07.03.27 Page 4.1

Page 4.2 07.03.27

Part II - Chapter 4: Incident Beam Masks
4.1 GENERAL
Beam masks are fitted in the incident beam path to control the axial width of the incident beam, thus defining
the amount (width) of the sample that is irradiated by the incident X-ray beam. Control of the axial divergence
of the X-ray beam is performed by Soller slits.
This chapter describes the beam masks that are used with line focus applications. If your application uses point
focus the task of controlling beam divergence is performed by incident beam collimators which are described in
Part II - Chapter 8. Diffracted beam masks are described in Part II - Chapter 17.
There are two sets of incident beam masks, one set is delivered as part of the PreFIX divergence slits
(PW3081/60 or PW3082/60), and the other set is supplied as an accessory for use with the X-ray mirror
(PW3088/6x, PW3148/6x, or PW3152/63).
4.1.1 Applications
Incident beam masks are used in all line focus applications (phase analysis, omega-stress analysis, reflectivity
and thin film phase analysis) in both para-focusing and parallel beam geometry. Their function in all of these
configurations is the same; beam masks define the irradiated width of the sample. The size of the beam mask
opening must be such that the incident X-ray beam is completely accepted by the sample during the complete
measurement.
4.2 BEAM MASK SET (ACCESSORY TO PW3081/60 OR PW3082/60)

A set of four beam masks is included with the programmable divergence slit (PW3081/60) and the fixed
divergence slits (PW3082/60). These beam masks are used to define the amount (width) of the sample that is
irradiated by the incident beam. They are shown in Figure 4.1. The beam masks can also be used in combination
with the PW3086/00 Incident Beam Anti-scatter Slit Holder and a PW3087/6x Automatic Beam Attenuator.
Figure 4.1: Incident Beam Masks

The four beam masks have markings of 20, 15, 10, and 5. This number defines the full width at half maximum
of the irradiated area on the sample (in millimeters) when the beam masks are used in a goniometer system with
a radius of 200 mm in combination with 0.04 rad Soller slits and placed at a distance of 115 mm from the line
focus of an X-ray tube. The focus-to-mask distance of the PW3081/60 Programmable Divergence Slit is 115
mm; for the PW3082/60 Fixed Divergence Slit Holder this distance is 96 mm. When a PW3087/6x Automatic
Beam Attenuator is mounted these distances change to 136 mm for the PW3081/60 and 117 mm for the
PW3082/60. Placing (mounting) these masks is described in Part II - Chapter 3, section 3.2.1.1 for the
programmable divergence slit and in section 3.3.1.1 for the fixed divergence slit holder.
07.03.27 Page 4.3

4.2.1 Irradiated Width

The total width of the area on the sample irradiated by the incident beam is dependent on the size of the X-ray
beam and the position of the sample with respect to the beam. The irradiated width as a function of the beam
mask and Soller slits used and the sample position can be calculated as follows:
W = (M - 3) + α (R - f)
where W = the irradiated width on the sample in millimeters
M = the mask’s marking,
R = the radius of the goniometer,
f = the distance from the focus of the X-ray tube to the beam mask,
α = the axial divergence angle of the Soller slits used.
The relationship between the mask’s marking and the total irradiated width on the sample at ψ = 0º at three
different goniometer radii is given in Table 4.1 for the programmable divergence slit and in Table 4.2 for the
fixed divergence slit holder.
Table 4.1: Relationship between Mask’s Marking and Irradiated Width in millimeters at three
Different Radii for the Programmable Divergence Slit
Soller Slits 0.01 rad 0.02 rad 0.04 rad
Radius (mm) Radius (mm) Radius (mm)

Mask
Marking
200 240 320 200 240 320 200 240 320
20 17.9 18.3 19.1 18.7 19.5 21.1 20.4 22.0 25.2
15 12.9 13.3 14.1 13.7 14.5 16.1 15.4 17.0 20.2
10 7.9 8.3 9.1 8.7 9.5 11.1 10.4 12.0 15.2
5 2.9 3.3 4.1 3.7 4.5 6.1 5.4 7.0 10.2
Table 4.2: Relationship between Mask’s Marking and Irradiated Width in millimeters at three
Different Radii for the Fixed Divergence Slit Holder
Soller Slits 0.01 rad 0.02 rad 0.04 rad
Radius (mm) Radius (mm) Radius (mm)

Mask
Marking
200 240 320 200 240 320 200 240 320
20 18.0 18.4 19.2 19.1 19.9 21.5 21.2 22.8 26.0

15 13.0 13.4 14.2 14.9 14.9 16.5 16.2 17.8 21.0
10 8.0 8.4 9.2 9.1 9.9 11.5 11.2 12.8 16.0
5 3.0 3.4 4.2 4.1 4.9 6.5 6.2 7.8 11.0
If your goniometer has a radius other than those shown in Table 4.1 or Table 4.2 you can interpolate (extrapolate)
the values shown in the tables. Select a beam mask with such a size that the irradiated width on the sample is
smaller than the size (width) of the sample in the axial direction.
Page 4.4 07.03.27

Part II - Chapter 4: Incident Beam Masks
4.3 PW3089/00 BEAM MASK SET

The PW3089/00 Beam Mask Set comprises two metal strips each with two openings for the incident beam to
pass through. The size of the openings are marked on the strip, they are: 20 mm, 10 mm, 4 mm and 2 mm.
Figure 4.2 shows the two beam masks.
The metal strip can be mounted into the X-ray mirror (PW3088/6x, PW3148/6x and PW3152/63), or into the
hybrid monochromators (PW3147/x0, PW3149/63, PW3150/63) in combination with the PW3086/20 Soller
Slits Holder or into the anti-scatter device for focusing X-ray mirrors (PW3086/7x) mounted onto a PW3152/63
Focusing X-ray Mirror, in order to reduce the width of the X-ray beam emerging from the PreFIX module into
which they are fitted. This, in turn causes the irradiated width on the sample surface to be reduced.
Placing (mounting) these masks is described in Part II - Chapter 6, sections 6.2.2.3.8 and 6.2.3.3.9 (X-ray
mirrors). Information about the relationship between the mask size and the width of the X-ray beam is also
provided in this section.
Figure 4.2: PW3089/00 Beam Mask Set
07.03.27 Page 4.5

Page 4.6 07.03.27

Chapter 5
Soller Slits
Contents
5.1 General................................................................................................................................. 5 - 3
5.1.1 Applications............................................................................................................................ 5 - 3
5.1.1.1 Para-focusing Geometry ........................................................................................ 5 - 3
5.1.1.2 Parallel Beam Geometry ........................................................................................ 5 - 3
5.2 Types and Where Used....................................................................................................... 5 - 5
5.2.1 PW3085/10 Soller Slits Assembly (0.01 rad) ........................................................................ 5 - 6
07.03.27 Page 5.1

Page 5.2 07.03.27

Part II - Chapter 5: Soller Slits
5.1 GENERAL
Soller slits are a set of parallel plates which are fitted into the incident and diffracted beam path parallel to the
diffraction plane to control the axial divergence of the X-ray beam. Using Soller slits improves the peak shape
and the resolution in 2θ based scans, especially at low scattering angles.
This chapter deals with the types of Soller slits which are used in X’Pert PRO systems. Soller slits only control
the axial divergence or acceptance of the X-ray beam; the axial width of the X-ray beam is controlled by the use
of incident and diffracted beam masks. Refer to Chapters 4 and 17 in Part II of this User’s Guide for information
about the use of these masks.
5.1.1 Applications
5.1.1.1 Para-focusing Geometry
In Bragg-Brentano para-focusing geometry Soller slits can be used in combination with slit optics. Control of
the equatorial divergence of the incident beam and the acceptance of the diffracted beam is performed by slits.
Control of the axial divergence of the X-ray beam is performed by Soller slits.
Figure 5.1: PW3085/x0 Soller Slits Assembly
5.1.1.2 Parallel Beam Geometry

Soller slits can also be used in the parallel beam geometry in combination with an X-ray mirror or a hybrid
monochromator. These devices only control the divergence in the equatorial plane. Control of the axial
divergence is performed by Soller slits.
In the diffracted beam path of the parallel beam geometry, Soller slits are used to control the axial acceptance,
whereas the equatorial acceptance is limited by using parallel plate collimators.
07.03.27 Page 5.3

Figure 5.2: PW3085/x1 Soller Slits Assembly
Page 5.4 07.03.27

5.2 TYPES AND WHERE USED

Within X’Pert PRO systems four different sizes of Soller slits are used: 0.01, 0.02, 0.04 and 0.08 radians. These
Soller slits are always used together with other PreFIX incident or diffracted beam components. Table 5.1 shows
the relationship between the Soller slits, the devices that they are used with, where they are used (in the incident
or diffracted beam path) and where their mounting is described.
Table 5.1: Devices that the Soller Slits can be used with
Beam Type
Soller Slits Item Chapter
Path Number
I PW3085/x0 PW3081/60 Programmable Divergence Slit (see caution below) II - 3
I PW3082/60 Fixed Divergence Slit Holder (see caution below) II - 3

I PW3088/6x X-ray Mirror for MRD II - 6
I PW3147/x0 & Hybrid Monochromator for MRD with Soller Slits II - 7

PW3086/20 Holder
I PW3148/6x X-ray Mirror for MPD II - 6
I PW3148/6x & X-ray Mirror with Incident beam Anti-scatter Slit II - 6

PW3086/60 Holder
I PW3149/63 & Hybrid Monochromator for MPD with Soller Slits II - 7

PW3086/20 Holder
I PW3149/63 & Hybrid Monochromator 2X for MPD with Incident II - 7

PW3086/65 beam Anti-scatter Slit Holder
I PW3150/63 & Hybrid Monochromator 4X for MPD with Soller Slits II - 7

PW3086/20 Holder
I PW3150/63 & Hybrid Monochromator 4X for MPD with Incident II - 7

PW3086/65 beam Anti-scatter Slit Holder
I PW3152/63 Focusing X-ray Mirror fo Cu Kα radiation II - 6
I PW3152/63 & Focusing X-ray Mirror with Incident Beam Anti- II - 6

PW3086/70 scatter Slit Holder
D PW3093/60 Programmable Receiving Slit II - 16
D PW3098/xx Parallel Plate Collimator II - 18
D PW3085/x1 PW3015/x0 X’Celerator II - 21
D PW3018/00 PIXcel II - 21
I = Incident Beam Path

D = Diffracted Beam Path
07.03.27 Page 5.5

(WITH LARGE APERTURE) TOGETHER WITH THE PW3081/60
PROGRAMMABLE DIVERGENCE SLIT.
CAUTION Be careful when storing Soller slits that you are not using. The thin
parallel plates that make up the slits are quite fragile and can easily
be bent. Try to store them on a flat surface with the plates
protected.
5.2.1 PW3085/10 Soller Slits Assembly (0.01 rad)

PW3085/10 is a Soller slits assembly which limits the axial divergence or acceptance to 0.01 radians (half of the
opening angle). This assembly is used for applications that require an improved peak shape, especially at low
angles. The devices that this assembly is used together with are indicated in Table 5.1. The physical appearance
is shown in Figure 5.1. A shutter lever and mounting screws are provided.
NOTE: When the Soller slits assembly is inserted in the PW3081/60 Programmable Divergence Slit or in
the PW3082/60 Fixed Divergence Slit Holder, the lever for the shutter actuator must be mounted
on the top of the Soller slits assembly.
Mounting instructions are given in Part I - Chapter 4 (section 4.4.3.1) of this User’s Guide. When you are
mounting the shutter lever, make sure that it positioned in such a way that it closes the shutter actuator
microswitch in the tube housing.

PW3085/11 is a Soller slits assembly with a large aperture for use with the X’Celerator or the PIXcel (see Table
5.1). It limits the axial acceptance to 0.01 radians (half of the opening angle). This assembly is used for
applications that require an improved peak shape, especially at low angles, it is shown in Figure 5.2.
For radiation safety reasons, the PW3085/11 0.01 rad Soller Slits Assembly must NOT be used together with the
PW3081/60 Programmable Divergence Slit or the PW3082/60 Fixed Divergence Slit Holder.

opening angle). This assembly is used for applications that require an improved peak shape, especially at low
angles. The devices that this assembly is used together with are indicated in Table 5.1. The physical appearance
is shown in Figure 5.1. A shutter lever and mounting screws are provided.
Page 5.6 07.03.27

5.1). It limits the axial acceptance to 0.02 radians (half of the opening angle). This assembly is used for
applications that require an improved peak shape, especially at low angles, it is shown in Figure 5.2.
For radiation safety reasons, the PW3085/21 0.02 rad Soller Slits Assembly must NOT be used together with
the PW3081/60 Programmable Divergence Slit or the PW3082/60 Fixed Divergence Slit Holder.

opening angle). This assembly is used for “standard” applications. The devices that this assembly is used
together with are indicated in Table 5.1. The physical appearance is shown in Figure 5.1.

5.1). It limits the axial acceptance to 0.04 radians (half of the opening angle). This assembly is used for all
“standard” applications, it is shown in Figure 5.2.

opening angle). This Soller slits assembly is used for applications where intensity is more important than
resolution. The devices that this assembly is used together with are indicated in Table 5.1. The physical
appearance is shown in Figure 5.1.

5.1). It limits the axial acceptance to 0.08 radians (half of the opening angle). This assembly is used for all
“standard” applications, it is shown in Figure 5.2.
07.03.27 Page 5.7

Page 5.8 07.03.27

Chapter 6
X-ray Mirrors
Contents
6.1 General................................................................................................................................. 6 - 3
6.2 Parabolic X-ray Mirrors .................................................................................................... 6 - 3
6.2.1 Applications............................................................................................................................ 6 - 4
6.2.1.1 Thin Film Phase Analysis and Reflectivity ........................................................... 6 - 4
6.2.1.2 Omega-stress Analysis........................................................................................... 6 - 4
6.2.1.3 Analysis of Samples in Glass Capillaries .............................................................. 6 - 4
6.2.1.4 Phase Analysis ....................................................................................................... 6 - 5
6.2.1.5 Transmission .......................................................................................................... 6 - 5
6.2.1.6 High Resolution ..................................................................................................... 6 - 5
6.2.2 X-ray Mirrors for X’Pert PRO MRD Systems....................................................................... 6 - 5
6.2.2.1 PW3088/60 X-ray Mirror for Cu Radiation .......................................................... 6 - 6
6.2.2.2 PW3088/66 X-ray Mirror for Co Radiation .......................................................... 6 - 7
6.2.2.3 Accessories ............................................................................................................ 6 - 7
6.2.3 X-ray Mirrors for X’Pert PRO MPD Systems ..................................................................... 6 - 12
6.2.3.1 PW3148/63 X-ray Mirror for Cu Radiation ........................................................ 6 - 12
6.2.3.2 PW3148/66 X-ray Mirror for Co Radiation ........................................................ 6 - 13
6.2.3.3 Accessories .......................................................................................................... 6 - 14
6.2.4 Use........................................................................................................................................ 6 - 18
6.2.4.1 Recommended X-ray Tube Setting...................................................................... 6 - 18
6.2.4.2 Measuring the X-ray Mirror Offset Value ........................................................... 6 - 18
6.2.4.3 Optimizing the Intensity ...................................................................................... 6 - 19
6.3 Focusing X-ray mirror ..................................................................................................... 6 - 24
6.3.1 Applications.......................................................................................................................... 6 - 25
6.3.1.1 Powders on Foil(s) ............................................................................................... 6 - 25
6.3.1.2 Pharmaceutical Formulations (Tablets) ............................................................... 6 - 25
6.3.1.3 Foil or Fiber Samples........................................................................................... 6 - 25
6.3.1.4 Samples in Glass Capillaries................................................................................ 6 - 25
07.03.27 Page 6.1

6.3.2 PW3152/63 Focusing X-ray Mirror for Cu Radiation.......................................................... 6 - 26

6.3.2.1 Focusing X-ray Mirror Housing........................................................................... 6 - 26
6.3.2.2 Mirror offset ......................................................................................................... 6 - 27
6.3.3 Accessories ........................................................................................................................... 6 - 27
6.3.3.1 ½° and ¼° Divergence Slits ................................................................................. 6 - 27
6.3.3.2 Attenuation Foil ................................................................................................... 6 - 27
6.3.3.3 Anti-scatter Slit (1.4 mm) .................................................................................... 6 - 28
6.3.3.4 Beta-filters for X-ray Mirrors............................................................................... 6 - 28
6.3.3.5 PW3085/x0 Soller Slits ........................................................................................ 6 - 28
6.3.3.6 PW3086/7x Incident Beam Anti-scatter Device for Focusing X-ray Mirror....... 6 - 28
6.3.3.7 PW3087/60 Automatic Beam Attenuator ............................................................ 6 - 30
6.3.3.8 PW3089/00 Beam Mask Set ................................................................................ 6 - 31
6.3.4 Use ........................................................................................................................................ 6 - 31
6.3.4.1 Recommended X-ray Tube Setting ...................................................................... 6 - 31
6.3.4.2 Measuring the X-ray Mirror Offset Value ........................................................... 6 - 32
6.3.4.3 Optimizing the Intensity....................................................................................... 6 - 32
6.3.4.4 Tube Height Adjustment ...................................................................................... 6 - 33
6.3.4.5 Selection of Anti-scatter Devices......................................................................... 6 - 34
Page 6.2 07.03.27

Part II - Chapter 6: X-ray Mirrors
6.1 GENERAL
X-ray mirrors are beam conditioners that are able to reshape the divergent X-ray beams coming from the line
focus of an X-ray tube.
There are two types of X-ray mirror associated with X’Pert PRO, they are classified according to the shape of
the X-ray beam they produce:
- The parabolic X-ray mirror. This type converts a divergent X-ray beam into a monochromatic quasi-
parallel X-ray beam. These X-ray mirrors are described in section 6.2.
- The focusing X-ray mirror. This type converts a divergent X-ray beam into a monochromatic
focusing X-ray beam. These X-ray mirrors are described in section 6.3.
6.2 PARABOLIC X-RAY MIRRORS

The graded multilayer parabolic X-ray mirror (see Figure 6.1) is a special kind of beam conditioner, which is
able to convert the divergent X-ray beam from a line focus tube to an intense monochromatic quasi parallel
beam. This is possible because of the combination of the parabolic shape of the mirror and the changing of
multilayer period over the length of the mirror. X-ray mirrors are designed to work with a line focus as they are
curved in only one dimension.
The X-ray mirrors provided with the X’Pert PRO diffraction system are designed to diffract characteristic
Kα radiation. The Kβ radiation is suppressed to a level below 0.5% of its original level. Because of the
monochromatic beam, measurements with the mirror typically do not require a beta-filter. A diffracted beam
monochromator is only needed with mirror measurements to reduce the background intensity if the incident
beam evokes fluorescence radiation on the sample.
The X-ray mirror accepts approximately 0.8º of the X-ray beam from the line focus of the X-ray tube. The quasi
parallel beam diffracted by the mirror has a small horizontal (equatorial) divergence depending on the take-off
angle used. The axial divergence of the beam is not controlled by the X-ray mirror, it can be controlled with the
use of Soller slits. Beam masks are used to control the axial width of the X-ray beam.
When using the X-ray mirror in combination with parallel beam optics on the diffracted beam side, the
measurements are not sensitive to the exact height position of the sample. This geometry is also suitable for
irregularly shaped samples.
The intensity per unit area of the X-ray beam coming out of the X-ray mirror is larger than that of the X-ray
beam emitted directly by the X-ray tube. This is a result of the mirror collimating the divergent beam from the
X-ray tube into a parallel beam.
Mirror
Parabolic
Shape
Quasi-parallel
Diffracted Beam
Divergent
Incident
Beam
MRDUB1.CDR
X-ray Tube
Focus
Figure 6.1: The Graded Multilayer Parabolic X-ray Mirror
07.03.27 Page 6.3

Two types of parabolic X-ray mirror are available for use on X’Pert PRO systems:
• X-ray mirror for X’Pert PRO MRD systems.
This type of X-ray mirror is designed for use on an X’Pert PRO MRD system with a goniometer radius
of 320 mm. These X-ray mirrors are described in section 6.2.2.
• X-ray mirror for X’Pert PRO MPD systems.
This type of X-ray mirror is designed for use on an X’Pert PRO MPD system with a goniometer radius
of 240 mm. These X-ray mirrors are described in section 6.2.3.
6.2.1 Applications
The mirror can be applied for measuring polycrystalline thin films, stressed materials, powders, irregularly
shaped samples and epitaxial layers.
6.2.1.1 Thin Film Phase Analysis and Reflectivity

The X-ray mirror can be applied for measurements at a fixed angle of incidence on (polycrystalline) thin films
and for reflectivity. The intense monochromatic quasi parallel incident beam results in measurements with a high
peak intensity combined with a low background intensity and a good resolution.
At very low angles of incidence the X-ray beam may over-irradiate the sample. The irradiated length of the
sample should always be less than the sample length (these dimensions are in the equatorial plane) and is worked
out as follows:
h
Irradiated length = ---------------- < sample length
sin ( ω )
where h = the height of the incident beam emerging from the X-ray mirror,
ω = the angle between the sample surface and the incident beam.
A typical value for the beam height from the X-ray mirror is 1.2 mm. This height can be reduced by installing a
divergence slit with a small aperture in the X-ray mirror.

The X-ray mirror can be applied for omega-stress analysis, in which the sample is inclined in the equatorial
plane. The measurements with the monochromatic beam have a low background intensity which makes an
accurate determination of the peak position possible. The parallel beam geometry makes peak positions in the
measurements insensitive to misalignment of the sample height. This also means that no defocusing effects occur
in stress measurements over a wide range of ω tilts.
The parallel beam geometry is also suited for measurements on irregularly shaped samples.
6.2.1.3 Analysis of Samples in Glass Capillaries

Sealed glass capillaries are used to investigate materials that should not be exposed to air, or could be a danger
to the operator’s health. Because the amount of material that can be analyzed is small, a high intensity narrow
beam is required to irradiate the sample. The X-ray beam emitted by an X-ray mirror fulfills this requirement.
Together with a capillary spinner sample stage, a line detector and anti-scatter devices in the incident and
diffracted beam paths, the X’Pert PRO MPD system can be configured to perform measurements on this kind of
sample.
Page 6.4 07.03.27


The X-ray mirror can be used as an incident beam module for phase analysis of polycrystalline (powder)
samples. A parallel plate collimator (with a fixed acceptance angle) is used on the diffracted beam side.
Alternatively, a programmable receiving slit with a diffracted beam X-ray mirror can be used on the diffracted
beam side to form an analysis module with variable resolution. This latter configuration is called the mirror-
mirror geometry. It is especially suitable for phase analysis on loosely prepared powder samples.
The use of a monochromatic beam results in a good signal-to-noise ratio. The parallel beam geometry ensures
that the measured peak positions are insensitive to sample shift and sample roughness.
When the X-ray mirror is used for phase analysis on polycrystalline samples, the irradiated area is generally less
than when a divergent beam in the Bragg-Brentano geometry is used.
The highly parallel beam in combination with the limited irradiated area leads to a reduced number of crystallites
from a random powder contributing to the measured intensity. The particle statistics become a special problem
in materials with a large grain size. In this case sample oscillation may be necessary.
6.2.1.5 Transmission
The X-ray mirror can be used to measure thin foils in the transmission mode. A parallel plate collimator is used
on the diffracted beam side. The transmission geometry is especially useful for measurements on polymer foils,
which have low X-ray absorption and often show a preferred orientation of their molecular structure.
6.2.1.6 High Resolution

A Ge four-crystal high-resolution monochromator for line focus applications (see also section 7.2 of Chapter 7
in Part II of this User’s Guide) positioned after the X-ray mirror emits a higher percentage of the output of the
X-ray tube than a configuration without an X-ray mirror. This set-up is possible in the X’Pert PRO Extended
MRD configuration. The gain measured on the Si(111) reflection of a (111) oriented silicon wafer compared
with that measured on a standard X’Pert PRO MRD high resolution set-up is approximately 8 to 10 times. This
significantly reduces the measurement time for reciprocal space maps and rocking curves.
6.2.2 X-ray Mirrors for X’Pert PRO MRD Systems

X-ray mirrors for X’Pert PRO MRD systems are PreFIX modules that can be used at different positions on the
PW3050/6x Goniometer for different applications:
• The standard incident beam PreFIX position for standard measurements using a parallel beam (refer to
Part I - Chapter 4, section 4.4.3.1 of this User’s Guide).
• The extended incident beam PreFIX position on an X’Pert PRO Extended MRD system in combination
with a high-resolution monochromator for high resolution studies (see also Part II - Chapter 1, section
1.4.8 of this User’s Guide).
• The diffracted beam PreFIX position in combination with a programmable receiving slit, supporting the
mirror-mirror geometry. More information about this configuration is given in Part II - Chapter 16,
section 16.3 of this User’s Guide.
This section describes the two types of X-ray mirror for X’Pert PRO MRD systems:
• PW3088/60 for Cu radiation, in section 6.2.2.1.
• PW3088/66 for Co radiation, in section 6.2.2.2.
07.03.27 Page 6.5

6.2.2.1 PW3088/60 X-ray Mirror for Cu Radiation

The PW3088/60 X-ray Mirror is a PreFIX module which is designed for use with an X’Pert PRO MRD system
in combination with Cu Kα radiation. The X-ray mirror is shown in Figure 6.2.
The mirror has a reflectivity factor of about 65% for the Cu Kα1 and Cu Kα2 lines. The Cu Kβ is virtually
eliminated, only 0.5% of the Kβ line is diffracted by the mirror. The acceptance angle from the line focus of the
X-ray tube is approximately 0.8º. The beam from the X-ray mirror is about 1.2 mm high and up to 20 mm wide.
The equatorial divergence of the beam is less than 0.05°. The axial width and divergence are not controlled by
the mirror. A width mask can be mounted onto the X-ray mirror to control the axial width of the beam. Soller
slits can be used to control the axial divergence.
A summary of the intensities of the direct X-ray beam coming out of the X-ray mirror in various configurations
is given in Table 6.7 and Table 6.9.
6.2.2.1.1 X-ray Mirror Housing

The PreFIX module housing is shown in Figure 6.2. It incorporates:
• a lever to activate the safety shutter on the X-ray tube
• a holder for an equatorial slit (a 1/2° slit is standard, smaller slits may be used for special applications)
• a slot for an attenuation foil or beam mask
• a holder to accommodate Soller slits with an additional slot for an attenuation foil or the anti-scatter slit.
Figure 6.2: PW3088/6x X-ray Mirror
Page 6.6 07.03.27

6.2.2.1.2 Mirror Offset

In X’Pert PRO systems the beam emitted from the X-ray mirror is offset relative to the direct beam from the
X-ray tube. This offset angle is referred to as the “mirror offset”. The value of the mirror offset is dependent on
the radius of the goniometer used; the exact value for your system is given in the Acceptance Test Form
delivered together with your X-ray mirror. The zero positions of the omega and 2theta axes of the goniometer
must be adjusted by the value of the mirror offset in order to compensate for it. The data collector software will
always apply an offset whenever the X-ray mirror is present in the incident beam path (and not use it if the
X-ray mirror is not present in the system); this offset is a default (calculated) value until you enter the exact offset
value for your system as given in the Acceptance Test Form.
The exact value of the X-ray mirror offset can also be determined experimentally, the procedure to do this is
given in section 6.2.4.2.
This offset does not apply if you are using an X-ray mirror at the extended position of an X’Pert PRO Extended
MRD system, as under these conditions the beam passes over the omega and 2theta axes at 0°.
6.2.2.2 PW3088/66 X-ray Mirror for Co Radiation

The PW3088/66 X-ray Mirror is a PreFIX module which is designed for use with an X’Pert PRO MRD system
in combination with Co Kα radiation. The physical appearance of this X-ray mirror is the same as the X-ray
mirror for Cu radiation (described in section 6.2.2.1 and shown in Figure 6.2).
The mirror has a reflectivity factor of 65% for the Co Kα1 and Co Kα2 lines. The Co Kβ is virtually eliminated,
only 0.5% of the Kβ line is diffracted by the mirror. The acceptance angle from the line focus of the X-ray tube
is approximately 0.8º. The beam from the X-ray mirror is about 1.2 mm high and up to 20 mm wide. The
equatorial divergence of the beam is about 0.06°. The axial width and divergence are not controlled by the
mirror. A width mask can be mounted onto the X-ray mirror to control the axial width of the beam. Soller slits
can be used to control the axial divergence.
is given in Table 6.7. The X-ray mirror for Co radiation cannot be used together with the PW3110/6x High-
resolution Monochromators on X’Pert PRO Extended MRD systems, since these monochromators are only used
in combination with Cu Kα radiation.
The PreFIX module housing is the same as that of the PW3088/60 X-ray Mirror described in section 6.2.2.1.1.
The offset angle of the X-ray beam emerging from the X-ray mirror relative to the direct beam from the X-ray
tube is referred to as the mirror offset. This mirror offset is described in more detail in section 6.2.2.1.2.
6.2.2.3 Accessories
The accessories that can be used together with mirrors fall into two groups:
Those that are delivered with the mirror (a 1/2° and a 1/4° divergence slit, attenuation foils and beta-
filters, and an anti-scatter slit),
and
Those that must be ordered separately (low angle fixed slits, Soller slits, automatic beam attenuators
and a beam mask set.
Information about these accessories, their use, and mounting instructions are described in this section.
07.03.27 Page 6.7

6.2.2.3.1 1/2º and 1/4º Divergence Slits

You can use a divergence slit together with an X-ray mirror in order to control the height of the X-ray beam
coming out of the X-ray mirror, and therefore the amount (length) of the sample that is irradiated.
A 1/2° and a 1/4° divergence slit are supplied with the PreFIX module. When the 1/2° divergence slit is used,
the X-ray mirror is irradiated over its complete length by the X-ray beam coming from the X-ray tube’s line
focus. The height of the X-ray beam emitted by the mirror is then 1.2 mm. The beam height can be reduced by
choosing a divergence slit with a smaller aperture. When making measurements that use small incident angles
(<4°) we recommend that smaller divergence slits are used. Divergence slits are available as accessories in the
following sizes: 1/8°, 1/16° and 1/32° (see section 6.2.2.3.5). The divergence slit should be installed in the slit
holder nearest to the X-ray tube.
The relationship between the slit marking, the height of the X-ray beam emerging from the mirror and the
irradiated length on the sample when the X-ray mirror is placed on the standard incident beam PreFIX position
and on the extended position (only for X’Pert PRO Extended MRD systems) is given in Table 6.1. The data in
this table takes into account the (small) equatorial divergence of the X-ray beam.
Table 6.1: Slit Size and Irradiated Length
Height of Irradiated Length (mm) Irradiated Length (mm)

Slit Marking
Beam (mm) on Standard Position on Extended Position
1/2° 1.2 0.12 + 1.2 / sin (ω) 0.2 + 1.2 / sin (ω)
1/4° 0.6 0.12 + 0.6 / sin (ω) 0.2 + 0.6 / sin (ω)
1/8° 0.3 0.12 + 0.3 / sin (ω) 0.2 + 0.3 / sin (ω)
1/16° 0.15 0.12 + 0.15 / sin (ω) 0.2 + 0.15 / sin (ω)
In this table ω is the angle between the incident beam and the sample surface.
NOTES: 1. We advise you to make a mark on the 1/2° slit that comes with the X-ray mirror so that you can
identify it as the slit to be used with the mirror. You should not use any other 1/2° slit (other than
the one you just marked) with the X-ray mirror.
2. Although the slit marking reads 1/2°, the actual position of the slit with respect to the line focus of
the X-ray tube determines the acceptance angle of the X-ray mirror to be 0.8°.
6.2.2.3.2 Attenuation Foils

Attenuation foils are delivered together with the PW3088/6x X-ray Mirror to reduce the intensity of the direct
X-ray beam coming out of the X-ray mirror. Under typical operating conditions the beam from the X-ray mirror
can have an intensity which is much greater than 1 000 000 cps. The Miniprop detector (PW3011/20) becomes
non-linear in response above 1 000 000 cps and can be damaged by higher count rates. For more details about
the maximum count rates for the detectors used in X’Pert PRO refer to Chapter 21 in Part II of this User’s Guide.
CAUTION An attenuation foil MUST be mounted in the housing slot in the

mirror housing in order to attenuate the beam whenever the
measured intensity is expected to exceed the maximum count rate
of the detector used.
Which foil is delivered with which X-ray mirror is given in Table 6.2 together with their attenuation factor for
the characteristic radiation used.
Page 6.8 07.03.27

The exact values for the attenuation factors for foils supplied with a mirror are shown on the attenuators
themselves and on the Acceptance Test Form for the mirror, which is supplied when the module is delivered.
These values can be entered in the data collector software and are used to automatically adjust the measured
intensity values.
The attenuation foil must be installed into one of the slots for attenuation foil (see Figure 6.2).
More information about this type of attenuation foil is given in Part II - Chapter 2, section 2.2.3.
Table 6.2: Attenuation Foil Attenuation Factors and Parent Device
Attenuation Foil Attenuation Factor Measured Using Accessory To
Cu (0.1 mm) ~ 100 Cu Kα PW3088/60
Cu (0.2 mm)/ ~ 18 000

Ni (0.02 mm)
Fe (0.1 mm) ~ 90 Co Kα PW3088/66
Fe (0.2 mm) ~ 8 000

The anti-scatter slit with an aperture of 1.4 mm supplied with the X-ray mirror should be used for all reflectivity
measurements and for any other measurements involving small 2θ angles (<4°). It is shown in Figure 6.3. The
slit should be inserted in the front of the Soller slits holder (see Figure 6.2) or mounted on the front of the X-ray
mirror module (when the Soller slits module is removed) or mounted on the front of the automatic beam
attenuator as shown in Figure 6.4 (see also Part II - Chapter 2, section 2.2.2.5.4).
Figure 6.3: Anti-scatter Slit (1.4 mm) for X-ray Mirror
6.2.2.3.4 Beta-filters for X-ray Mirrors

Beta-filters can be used to further reduce the amount of Kβ radiation emitted by the X-ray mirror. One beta-filter
is supplied with the X-ray mirror. It should be inserted into the slot which can also be used for the attenuation
foil.
07.03.27 Page 6.9

A Ni filter intended for use with Cu radiation is included with the PW3088/60 X-ray Mirror for Cu radiation.
The filter’s foil thickness is 0.02 mm. An Fe filter intended for use with Co radiation is included with the
PW3088/66 X-ray Mirror for Co radiation. The filter’s foil thickness is 0.016 mm.
More information about this type of beta-filter is given in Part II - Chapter 2, section 2.3.2.
6.2.2.3.5 PW3083/00 Low Angle Fixed Slits

You can use low angle fixed slits together with the mirror in order to control the amount (length) of the sample
that is irradiated. Table 6.1 shows the relationship between the various slits and the amount of the sample
irradiated. The slit should be inserted into the divergence slit holder nearest to the X-ray tube.
When they are delivered, these slits are aligned for the X-ray mirror in your system. Do not use any other low
angle slits as they may not be correctly aligned for use with your mirror.
6.2.2.3.6 PW3085/x0 Soller Slits

You can use Soller slits together with the mirror in order to control the axial divergence of the incident beam
emerging from the mirror.
Soller slits are available in different sizes as follows:
The Soller slits must be installed in the Soller slits holder at the front of the X-ray mirror. For more information
about Soller slits refer to Part II - Chapter 5. This Soller slits holder can be removed in order to make it possible
to mount an automatic beam attenuator or an anti-scatter device. If you are not actually using these devices we
advise you to mount the Soller slits holder onto the X-ray mirror.
The Soller slits holder can be mounted onto the X-ray mirror by placing the holder in location (refer to Figure
6.2) and tightening the two screws marked B.
6.2.2.3.7 PW3087/6x Automatic Beam Attenuator

The PW3087/6x Automatic Beam Attenuator can be mounted on the front of the mirror housing replacing the
Soller slits holder and used in place of the foils described in section 6.2.2.3.2. The attenuation factor is entered
in the data collector software and is used to automatically adjust the measured intensity values. The anti-scatter
slit described in section 6.2.2.3.3 is required if the automatic beam attenuator is used at low 2θ angles. More
information about the automatic beam attenuators is given in Part II - Chapter 2, section 2.2.3.
6.2.2.3.7.1 Mounting the Automatic Beam Attenuator onto an X-ray Mirror

1. Remove the three screws (marked A in Figure 6.4) at the back (metal part) of the automatic beam
attenuator.
3. Remove the Soller slits holder by removing the screws marked B in Figure 6.2.
4. Fit the metal part (NOT the side with the alignment pins) onto the brass end of the mirror; line it up with
the slit of the automatic beam attenuator to the slit on the mirror and ensure that the four screw holes
line up. Use the four short screws (M2 x 4) supplied with the automatic beam attenuator and secure it
into place.
Page 6.10 07.03.27

Now you can mount a reflectivity slit or the beam mask holder. Mounting instructions are given in Part II -
Chapter 2. Figure 6.4 shows the automatic beam attenuator with a anti-scatter slit mounted onto the X-ray mirror.
Screws A
Figure 6.4: PW3088/6x X-ray Mirror with a PW3087/6x Automatic Beam Attenuator with Anti-
scatter Slit Mounted
6.2.2.3.8 PW3089/00 Beam Mask Set

You can use beam masks together with the X-ray mirror in order to control the amount (width) of the sample
that is irradiated. The following masks are supplied in the PW3089/00 Beam Mask Set: 20, 10, 4 and 2. Table
6.3 shows the relationship between the various masks positioned in the slot for the mask in the Soller slits holder
and the amount of the sample irradiated, when used in combination with the 0.08 rad, 0.04 rad, 0.02 rad and
0.01 rad Soller slits.
Table 6.3: Beam Masks and Irradiated Width
Mask 0.08 rad Soller Slits 0.04 rad Soller Slits 0.02 rad Soller Slits 0.01 rad Soller Slits
20 34 mm 27 mm 24 mm 22 mm
10 24 mm 17 mm 14 mm 12 mm
4 18 mm 11 mm 8 mm 6 mm
2 16 mm 9 mm 6 mm 4 mm
The beam mask must be installed into one of the slots for beam masks (see Figure 6.2).
For more information about beam masks, refer to Part II - Chapter 4.
07.03.27 Page 6.11

6.2.3 X-ray Mirrors for X’Pert PRO MPD Systems

X-ray mirrors for X’Pert PRO MPD systems are PreFIX modules that are specifically designed for use on
different positions on the PW3050/60 Goniometer for different applications:
• The standard incident beam PreFIX position for standard measurements using a parallel beam.
• The diffracted beam PreFIX position in combination with a programmable receiving slit, supporting the
mirror-mirror geometry. More information about this configuration is given in Part II - Chapter 16,
section 16.3 of this User’s Guide.
This section describes the two types of X-ray mirror for X’Pert PRO systems:
• PW3148/63 for Cu radiation, in section 6.2.3.1.
• PW3148/66 for Co radiation, in section 6.2.3.2.
6.2.3.1 PW3148/63 X-ray Mirror for Cu Radiation

The PW3148/63 X-ray Mirror is a PreFIX module which is designed for use with an X’Pert PRO MPD system
with a goniometer radius of 240 mm in combination with Cu Kα radiation. The X-ray mirror is shown in Figure
6.5.
eliminated, only 0.5% of the Kβ line is diffracted by the mirror. The acceptance angle from the line focus of the
X-ray tube is approximately 0.8º. The beam from the X-ray mirror is about 1.3 mm high and up to 30 mm wide.
The equatorial divergence of the beam is less than 0.055°. The axial width and divergence are not controlled by
the mirror. A width mask can be mounted onto the X-ray mirror to control the axial width of the beam. Soller
slits can be used to control the axial divergence.
is given in Table 6.8.
6.2.3.1.1 X-ray Mirror Housing

The PreFIX module housing is shown in Figure 6.5. It incorporates:
• a holder for an equatorial slit (a 1/2° slit is standard, smaller slits may be supplied for special applica-
tions)
• a holder to accommodate Soller slits with an additional slot for an attenuation foil or the anti-scatter slit
Page 6.12 07.03.27

Figure 6.5: PW3148/6x X-ray Mirror for X’Pert PRO MPD Systems
6.2.3.1.2 Mirror Offset

In X’Pert PRO systems the beam emitted from the X-ray mirror is offset relative to the direct beam from the
X-ray tube. This offset angle is referred to as the “mirror offset”. The value of mirror offset is dependent on the
radius of the goniometer used; the exact value for your system is given in the Acceptance Test Form delivered
together with your X-ray mirror. The zero positions of the omega and 2theta axes of the goniometer must be
adjusted by the value of the mirror offset in order to compensate for it. The data collector software will always
apply an offset whenever the X-ray mirror is present in the incident beam path (and not use it if the X-ray mirror
is not present in the system); this offset is a default (calculated) value until you enter the exact offset value for
your system as given in the Acceptance Test Form.
The exact value of the X-ray mirror offset can also be determined experimentally, the procedure to do this is
6.2.3.2 PW3148/66 X-ray Mirror for Co Radiation

The PW3148/66 X-ray Mirror is a PreFIX module which is designed for use with an X’Pert PRO MPD system
with a 240 mm goniometer radius in combination with Co Kα radiation. The physical appearance of this X-ray
mirror is the same as the X-ray mirror for Cu radiation (described in section 6.2.3.1 and shown in Figure 6.5).
The mirror has a reflectivity factor of 65% for the Co Kα1 and Co Kα2 lines. The Co Kβ is virtually eliminated,
only 0.5% of the Kβ line is diffracted by the mirror. The acceptance angle from the line focus of the X-ray tube
is approximately 0.8º. The beam from the X-ray mirror is about 1.3 mm high and up to 30 mm wide. The
equatorial divergence of the beam is less than 0.07°. The axial width and divergence are not controlled by the
mirror. A width mask can be mounted onto the X-ray mirror to control the axial width of the beam. Soller slits
can be used to control the axial divergence.
07.03.27 Page 6.13

The PreFIX module housing is the same as that of the PW3148/63 X-ray Mirror described in section 6.2.3.1.1.
tube is referred to as the mirror offset. This mirror offset is described in more detail in section 6.2.3.1.2.
6.2.3.3 Accessories
Those that are delivered with the mirror (a 1/2° and a 1/4° divergence slit, attenuation foils and beta-
filters, and an anti-scatter slit),
and
Those that must be ordered separately (low angle fixed slits, Soller slits, an anti-scatter slit holder, an
automatic beam attenuator and a beam mask set).
Information about these accessories, their use, and mounting instructions are described in this section.

You can use a divergence slit together with an X-ray mirror in order to control the height of the
X-ray beam coming out of the X-ray mirror, and therefore the amount (length) of the sample that is irradiated.
A 1/2° and a 1/4° divergence slit are supplied with the PreFIX module. When the 1/2° divergence slit is used,
the X-ray mirror is irradiated over its complete length by the X-ray beam coming from the X-ray tube’s line
focus. The height of the X-ray beam emitted by the mirror is then 1.3 mm. The beam height can be reduced by
choosing a divergence slit with a smaller aperture. When making measurements that use small incident angles
(<4°) we recommend that smaller divergence slits are used. Divergence slits are available as accessories in the
following sizes: 1/8°, 1/16° and 1/32° (see section 6.2.2.3.5). The divergence slit should be installed in the slit
holder nearest to the X-ray tube.
The relationship between the slit marking, the height of the X-ray beam emerging from the mirror and the
irradiated length on the sample when the X-ray mirror is placed on the incident beam PreFIX position and on an
X’Pert PRO MPD system (with a goniometer radius of 240 mm) is given in Table 6.1. The data in this table takes
into account the (small) equatorial divergence of the X-ray beam.
Table 6.4: Slit Size and Irradiated Length
Height of Irradiated
Slit Marking
Beam (mm) Length (mm)
1/2° 1.3 0.10 + 1.3 / sin (ω)
1/4° 0.65 0.10 + 0.65 / sin (ω)
1/8° 0.33 0.10 + 0.33 / sin (ω)

1/16° 0.16 0.10 + 0.16 / sin (ω)
2. Although the slit marking reads 1/2°, the actual position of the slit with respect to the line focus of
the X-ray tube determines the acceptance angle of the X-ray mirror to be 0.8°.
Page 6.14 07.03.27


Attenuation foils are delivered together with the PW3148/6x X-ray Mirror to reduce the intensity of the direct
X-ray beam coming out of the X-ray mirror. Under typical operating conditions the beam from the X-ray mirror
can have an intensity which is much greater than 1 000 000 cps. The Miniprop detector (PW3011/20) becomes
non-linear in response above 1 000 000 cps and can be damaged by higher count rates. For more details about
the maximum count rates for the detectors used in X’Pert PRO refer to Chapter 21 in Part II of this User’s Guide.

Which foil is delivered with which X-ray mirror is given in Table 6.5 together with their attenuation factor for
the characteristic radiation used.
Table 6.5: Attenuation Foil Factors and Parent Device
Attenuation Foil Attenuation Factor Measured Using Accessory To
Cu (0.1 mm) ~ 100 Cu Kα PW3148/63
Cu (0.2 mm)/ ~ 18 000

Ni (0.02 mm)
Fe (0.1 mm) ~ 90 Co Kα PW3148/66
Fe (0.2 mm) ~ 8 000
The exact values for the attenuation factors for foils supplied with a mirror are shown on the attenuators
themselves and on the Acceptance Test Form for the mirror, which is supplied when the module is delivered.
These values can be entered in the data collector software and are used to automatically adjust the measured
intensity values.

The anti-scatter slit with an aperture of 1.4 mm supplied with the X-ray mirror should be used for all reflectivity
measurements and for any other measurements involving small 2θ angles (<4°). It is shown in Figure 6.3. The
slit should be inserted in the front of the Soller slits holder or mounted on the front of the X-ray mirror module
(when the Soller slits holder is removed) or mounted on the front of the automatic beam attenuator (see also Part
II - Chapter 2, section 2.2.2.5.4).
6.2.3.3.4 Beta-filters for X-ray Mirrors

Beta-filters can be used to reduce the amount of Kβ radiation emitted by the X-ray mirror. One beta-filter is
supplied with the X-ray mirror. It should be inserted into the slot which can also be used for the attenuation foil.
A Ni filter intended for use with Cu radiation is included with the PW3148/63 X-ray Mirror for Cu radiation.
The filter’s foil thickness is 0.02 mm. An Fe filter intended for use with Co radiation is included with the
PW3148/66 X-ray Mirror for Co radiation. The filter’s foil thickness is 0.016 mm.
07.03.27 Page 6.15


You can use low angle fixed slits together with the mirror in order to control the amount (length) of the sample
that is irradiated. Table 6.1 shows the relationship between the various slits and the amount of the sample
irradiated. The slit should be inserted into the divergence slit holder nearest to the X-ray tube.
When they are delivered, these slits are aligned for the X-ray mirror in your system. Do not use any other low
angle slits as they may not be correctly aligned for use with your system.

emerging from the mirror.
The Soller slits are available in different sizes as follows:
The Soller slits must be installed in the Soller slits holder at the front of the X-ray mirror. For more information
about Soller slits refer to Part II - Chapter 5. This Soller slits holder can be removed in order to make it possible
to mount an automatic beam attenuator or an anti-scatter device. If you are not actually using these devices we
advise you to mount the Soller slits holder onto the X-ray mirror.
6.2.3.3.7 PW3086/60 Incident Beam Anti-scatter Slit Holder for X-ray Mirror
If you want to use an X-ray mirror in a capillary spinner configuration you must use an anti-scatter slit. In order
to mount the slit you must first install the PW3086/60 Incident Beam Anti-scatter Slit Holder.
This holder includes a direct beam stop to protect the detector from being exposed to the high intensity of the
direct beam; and to allow measurements from 3º 2θ upwards in the capillary spinner configuration.
Fastening
Screw
Fastening
Screw

Mounted onto an X-ray Mirror
Page 6.16 07.03.27
6.2.3.3.7.1 Mounting an Incident Beam Anti-scatter Slit Holder onto an X-ray Mirror
Mount the anti-scatter slit holder on the X-ray mirror as follows:
1. Remove the Soller slits holder by unscrewing the screws marked B in Figure 6.5. If a beam attenuator is
mounted, refer to section 6.2.3.3.8.1 for information about removing it.
2. Place the anti-scatter slit holder in the location where you just removed the Soller slits holder or
automatic beam attenuator and secure it using the two screws used to mount the Soller slits holder onto
the X-ray mirror.
Alignment of the incident beam anti-scatter slit holders is described in Part II - Chapter 20.

The PW3087/6x Automatic Beam Attenuator can be mounted on the front of the mirror housing replacing the
Soller slits holder and used in place of the foil described in section 6.2.3.3.2. The attenuation factor is entered in
the data collector software and is used to automatically adjust the measured intensity values. The anti-scatter slit
described in section 6.2.3.3.2 is required if the automatic beam attenuator is used at low 2θ angles. More
information about the automatic beam attenuator is given in Part II - Chapter 2, section 2.2.2.
Figure 6.7: PW3087/6x Automatic Beam Attenuator Mounted onto an X-ray Mirror
6.2.3.3.8.1 Mounting the Automatic Beam Attenuator onto an X-ray Mirror

attenuator.
4. Fit the metal part (NOT the side with the alignment pins) onto the brass end of the mirror; line it up
with the slit of the automatic beam attenuator to the slit on the mirror and ensure that the four screw
holes line up. Use the four short screws (M2 x 4) supplied with the automatic beam attenuator and
secure it into place.
Now you can mount an anti-scatter slit or the beam mask holder. Mounting instructions are given in Part II -
Chapter 2.
07.03.27 Page 6.17

6.2.3.3.9 PW3089/00 Beam Mask Set

You can use beam masks together with the X-ray mirror in order to control the amount (width) of the sample that
is irradiated. The following masks are supplied in the PW3089/00 Beam Mask Set: 20, 10, 4 and 2. Table 6.6
shows the relationship between the various masks positioned in the slot for the mask in the Soller slits holder and
the amount of the sample irradiated, when used in combination with the 0.08 rad, 0.04 rad 0.02 rad and 0.01 rad
Soller slits.
Table 6.6: Beam Masks and Irradiated Width
0.08 rad 0.04 rad 0.02 rad 0.01 rad

Mask
Soller Slits Soller Slits Soller Slits Soller Slits
20 28 mm 24 mm 22 mm 21 mm
10 18 mm 14 mm 12 mm 11 mm
4 12 mm 8 mm 6 mm 5 mm
2 10 mm 6 mm 4 mm 3 mm
The beam mask must be installed into one of the slots for beam masks (see Figure 6.2).
For more information about beam masks, refer to Part II - Chapter 4.
6.2.4 Use
This section deals with measuring the X-ray mirror offset value and with checking the intensity of the output
from the X-ray mirror.
6.2.4.1 Recommended X-ray Tube Setting

If your X’Pert PRO diffraction system includes an X-ray mirror for Cu radiation you must use the PW3373/10
XRD X’Pert Tube (see Part II - Chapter 1, section 1.3.2). The recommended high-tension maximum generator
settings for this X-ray tube are 45 kV and 40 mA.
If your X’Pert PRO diffraction system includes an X-ray mirror for Co radiation you must use the PW3376/00
XRD X’Pert Cobalt Tube. The recommended high-tension generator settings for this X-ray tube together with
an X-ray mirror for Co radiation are 40 kV and 40 mA.
6.2.4.2 Measuring the X-ray Mirror Offset Value

The X-ray beam emerging from the X-ray mirror is offset by a certain angle. The exact value of this angle is
given in the Acceptance Test Form supplied with your X-ray mirror.
If you want to measure the offset value, you do so as follows:
1. Install a non-offset incident beam PreFIX module (for example: a fixed divergence slit or a
programmable divergence slit) and report this to the data collector software. Use a fixed divergence slit
(setting) of 1/4º or smaller.
2. Insert a 0.2 mm copper attenuation foil.
3. Set ω = 0º and make sure that the direct beam is not obstructed by a sample or a sample stage.
4. Make a 2θ scan to find the peak position of the direct X-ray beam, note this as 2θA.
5. Replace the incident beam PreFIX module used in step 1 with the X-ray mirror. Do NOT report this to
the data collector software. Insert an attenuation foil into the X-ray mirror: the combined copper/nickel
attenuation foil when you are using Cu radiation and the iron (0.2 mm) attenuation foil when you are
using Co radiation.
Page 6.18 07.03.27
6. Make a 2θ scan to find the peak position of the direct X-ray beam from the X-ray mirror. Note this
position as 2θB.
7. The X-ray mirror offset is calculated by (2θB - 2θA).
8. Enter the reverse of the offset value into the data collector software, so that the 2theta and omega axes
are automatically offset when you select the X-ray mirror as the incident beam PreFIX module. This
means, for example: if your calculation of the offset results in -1.1º you actually enter 1.1º, whereas if
your calculation resulted in +1.1º you enter -1.1º.
6.2.4.3 Optimizing the Intensity

To maintain the optimum intensity from the X-ray mirror the output should be checked on the following
occasions:
• After rotating the X-ray tube to the line focus position.
• After replacing the X-ray tube.
• After repeatedly mounting and dismounting the X-ray mirror module.
Sometimes the tube height needs to be adjusted in order to obtain an optimum intensity. This tube height
adjustment procedure is described in section 6.2.4.3.3.
6.2.4.3.1 Checking the Intensity from the X-ray Mirror

When the X-ray mirror is used as a single incident beam PreFIX module, the intensity can be checked as follows:
1. Set the following parameters:
Tube power : 30 kV, 50 mA
Divergence slit : 1/2° (in the holder for an equatorial (divergence) slit)
Attenuator : Combined copper/nickel attenuation foil in combination with Cu radiation
Iron (0.2 mm) attenuation foil in combination with Co radiation
Soller slits : None
2. Set ω = 0º and make sure that the direct beam is not obstructed by the sample or the sample stage.
3. Make a 2θ scan to find the peak position of the direct X-ray beam.
4. Note the peak intensity value.
5. Note the value of 2θ.
6. Set 2θ at the peak position.
If there is no peak registered near 2θ = 0º, check that the offset value was properly introduced.
The absolute intensity values must meet the specifications listed in Table 6.7 and Table 6.8. The intensity data
as given in Table 6.7 include both intensities measured with the PW3088/6x X-ray Mirror on the standard
incident beam PreFIX position in the X’Pert PRO MRD system and intensities measured with the X-ray mirror
on the extended incident beam PreFIX position in the X’Pert PRO Extended MRD system. Table 6.8
summarizes the intensities measured with a PW3148/6x X-ray Mirror on an X’Pert PRO MPD system.
If these intensity values are not met, refer to section 6.2.4.3.3.
07.03.27 Page 6.19

Table 6.7: Summary of Absolute Intensities of the Direct Beam of a

PW3088/6x X-ray Mirror for X’Pert PRO MRD Systems
Type Number Diffracted Beam Optics Standard Extended
PW3097/60 or Rocking Curve Optics > 3.4 x 109 cps > 2.1 x 109 cps
PW3120/6x
PW3093/60 & Programmable Receiving Slit (3 mm) and > 3.4 x 109 cps > 2.1 x 109 cps
PW3091/x0 Programmable Anti-scatter Slit (4°) (no Soller slits)
PW3015/x0 & X’Celerator (90º rotated, receiving slit mode, > 1.2 x 109 cps > 0.8 x 109 cps
maximum active length (9 mm)) and
PW3x94/30 Fixed Anti-scatter Slit Holder (with 13 mm slit
inserted), (no Soller slits)
PW3018/00 & PIXcel (receiving slit mode, maximum active length > 2 x 109 cps > 1.2 x 109 cps
(14 mm)) and
PW3490/00 Fixed Anti-scatter Slit Holder (no slit inserted)
(no Soller slits)
PW3098/09 Parallel Plate Collimator, 0.09° (no Soller slits) > 1.8 x 109 cps > 0.9 x 109 cps
PW3098/18 Parallel Plate Collimator, 0.18° (no Soller slits) > 2 x 109 cps > 1.3 x 109 cps
PW3098/27 Parallel Plate Collimator, 0.27° (no Soller slits) > 3 x 109 cps > 1.8 x 109 cps

PW3148/6x X-ray Mirror for X’Pert PRO MPD Systems
Type Number Diffracted Beam Optics PW3148/63 PW3148/66
PW3097/60 Rocking Curve Optics > 6 x 109 cps > 5.5 x 109 cps
PW3093/60 & Programmable Receiving Slit (3 mm) and > 6 x 109 cps > 5.5 x 109 cps
PW3091/60 Programmable Anti-scatter Slit (4°) (no Soller slits)
PW3015/x0 & X’Celerator (90º rotated, receiving slit mode, > 2.1 x 109 cps > 2.0 x 109 cps
maximum active length (9 mm)) and
PW3x94/30 Fixed Anti-scatter Slit Holder (with 13 mm slit
inserted) (no Soller slits)
PW3098/09 Parallel Plate Collimator, 0.09° (No Soller slits) > 3 x 109 cps >2.7 x 109 cps
PW3098/18 Parallel Plate Collimator, 0.18° (No Soller slits) > 3.8 x 109 cps > 3.5 x 109 cps
PW3098/27 Parallel Plate Collimator, 0.27° (No Soller slits) > 4.8 x 109 cps > 4.4 x 109 cps
PW3018/00 & PIXcel (receiving slit mode, maximum active length > 3.5 x 109 cps > 3.2 x 109 cps
(14 mm)) and
PW3490/00 Fixed Anti-scatter Slit Holder (no slit inserted) (no
Soller slits)
NOTES: 1. When you use 0.04 rad Soller slits in the Soller slits holder of the X-ray mirror, you must expect
an intensity drop of around 30%.
2. The direct beam intensities were determined with a new tube, be aware that the X-ray tube
intensities decrease in time.
3. After intensive use in the incident beam the X-ray mirror will show degraded surfaces. Therefore,
the X-ray mirror may not completely reach the specified intensities. If this is the case call your
local PANalytical Service Engineer.
Page 6.20 07.03.27
6.2.4.3.2 Checking Intensity from X-ray Mirror with a Ge Monochromator

When the PW3088/60 X-ray Mirror is used in combination with high-resolution monochromators (this is only
applicable for X’Pert PRO Extended MRD systems employing copper radiation) the intensity can be checked
according to the procedure described below.
Tube power: 45 kV, 40 mA
Divergence slit: 1/2° (in the holder for an equatorial (divergence) slit)
Attenuator: Combined copper/nickel attenuation foil (the attenuation factor is shown on the
attenuator)
Soller slits: None
The absolute intensities must meet the values given in Table 6.9.
Table 6.9: Summary of Absolute Intensities of the Direct Beam of a PW3088/60 X-ray Mirror in
combination with a Ge Monochromator (12 mm) for X’Pert PRO Extended MRD Systems
PW3110/66
PW3110/65
Ge (220)
Type Number Diffracted Beam Optics Ge (220)
Asymmetrical
12 mm
12 mm
PW3097/60 or PW3120/60 Rocking Curve Optics

or or
PW3093/60 & PW3091/x0 Programmable Receiving Slit (3 mm) & > 18 x 106 cps > 45 x 106 cps
Programmable Anti-scatter Slit (4°)
PW3018/00 & PIXcel (receiving slit mode, maximum > 10 x 106 cps > 26 x 106 cps
active length (14 mm)); and
PW3490/00 & PW3490/32 Fixed Anti-scatter Slit Holders (no slit
inserted), (no Soller Slits)
NOTE: When a crossed slits assembly is fitted onto the high-resolution monochromator the intensity is
reduced by approximately 10%.
6.2.4.3.3 Tube Height Adjustment

There are three factors that can lead to reduced intensity:
• A change in the position of the tube focus relative to the X-ray mirror.
• A reduction in the output intensity from the X-ray tube.
• A change in the X-ray mirror alignment. (This is less probable).
During the life of an X-ray tube the focus position can change slightly and the output intensity slowly drops.
When a ceramic Cu or Co X-ray tube is used with an X-ray mirror the drop of intensity should be less than 15%
per 1000 hours of use. If the output from the X-ray mirror drops more than 15% per 1000 hours of use, adjust
the tube height to reposition the focus relative to the X-ray mirror.
07.03.27 Page 6.21

6.2.4.3.3.1 Tube Height Adjustment for Systems other than X’Pert PRO Extended MRD
This section describes the tube height adjustment procedures for X’Pert PRO diffraction systems other than
X’Pert PRO Extended MRD.
To adjust the height position of the X-ray tube relative to the X-ray mirror, proceed as follows:
1. Mount the X-ray mirror onto the incident beam PreFIX position. Place a 1/2° divergence slit and an
attenuation foil into the X-ray mirror to protect the detector. Use a combined copper/nickel attenuation
foil when you are using Cu radiation and an iron (0.2 mm) attenuation foil when you are using Co
radiation. Make sure that the mirror offset (see section 6.2.4.2) is correctly introduced in the data
collector software.
2. Mount one of the diffracted beam optics as summarized in Table 6.7 or Table 6.8. Use the settings given
in these tables.
3. Set ω = 0°, 2θ = 0° and make sure that the direct beam is not obstructed by the sample or the sample
stage.
4. Set the tube power to 30 kV and 50 mA.
8. Close the shutter, open the enclosure doors and proceed as follows:
a. Loosen (turn 45º anti-clockwise) the upper (nearest the top of the X-ray tube) of the two knurled
knobs at the back of the X-ray tube housing (refer to Part II - Chapter 1 - Figure 1.9).
b. Tighten (turn 45º clockwise) the lower of the two knurled knobs at the back of the X-ray tube
housing to move the X-ray tube (approximately 25 μm).
c. Close the enclosure doors, open the shutter and note the intensity value.
9. If the intensity is higher than that noted in step 7, continue repeating step 8 until the intensity does not
increase any further (if necessary you can make smaller steps, say: approximately 10 μm); then
continue with step 11. If the intensity is lower than that noted in step 7, continue with step 10.
a. Loosen (turn 45º anti-clockwise) the lower (furthest from the top of the X-ray tube) of the two
knurled knobs at the back of the X-ray tube housing (refer to Part II - Chapter 1 - Figure 1.9).
b. Tighten (turn 45º clockwise) the upper of the two knurled knobs at the back of the X-ray tube
housing to move the X-ray tube in the opposite direction (approximately 25 μm).
d. If the intensity is higher than that noted in step 7, continue repeating this action until the intensity
does not increase any further (if necessary you can make smaller steps, say: approximately 10 μm);
then continue with step 11.
11. Tighten both screws (only hand tight, no more) to lock the tube into position.
Page 6.22 07.03.27

6.2.4.3.3.2 Tube Height Adjustment for X’Pert PRO Extended MRD Systems
This section describes the tube height adjustment procedures for X’Pert PRO Extended MRD systems.
To adjust the height position of the X-ray tube relative to the X-ray mirror, proceed as follows:
1. Mount the X-ray tube on the standard tube position on the extended arm, or on the extended tube
position. Make sure that the mirror offset (see sections 6.2.2.1.2 and 6.2.4.2) is correctly introduced in
the data collector software.
2. Mount one of the diffracted beam optics as summarized in Table 6.7. Use the settings given in these
tables.
3. Mount the X-ray mirror onto the incident beam PreFIX position. Place a 1/2° divergence slit and an
attenuation foil into the X-ray mirror to protect the detector. Use a combined copper/nickel attenuation
foil when you are using Cu radiation and an iron (0.2 mm) attenuation foil when you are using Co
radiation.
stage.
5. Set the tube power to 45 kV and 40 mA if you have a copper tube, and to 40 kV and 40 mA if you have
a cobalt tube.
shield.
b. Turn the Allen key 45º counter-clockwise to move the X-ray tube (approximately 25 μm).
10. Check the intensity:
a. If the intensity is higher than that noted in step 8, continue repeating step 9 until the intensity does
not increase any further (if necessary you can make smaller steps, say: approximately 10 μm); then
continue with step 12.
b. If the intensity is lower than that noted in step 8, you must change the adjustment direction. Turn
the screw through a complete rotation clockwise (until the play is taken up) and then continue with
step 11.
c. If the intensity is unchanged from that noted in step 8, the play in the adjustment mechanism is in
effect. In this case turn the screw through a complete rotation counter-clockwise (until the play is
taken up) and then perform step 9 again.
a. Turn the Allen key 45º clockwise to move the X-ray tube in the opposite direction (approximately
25 μm).
b. Close the enclosure doors, open the shutter and note the intensity value.
c. If the intensity is higher than that noted in step 8, continue repeating this action until the intensity
does not increase any further; then continue with step 12.
12. The adjustment procedure is complete. Remove the Allen key.
07.03.27 Page 6.23

6.3 FOCUSING X-RAY MIRROR

The graded multilayer focusing X-ray mirror (see Figure 6.8) is a special kind of beam conditioner, which is able
to convert the divergent X-ray beam from a tube in line focus position to an intense monochromatic beam that
focuses onto the goniometer circle. This is possible because of the combination of the elliptical shape of the
mirror and the change in multilayer period over the length of the mirror. Focusing X-ray mirrors are designed to
work with line focus as they are only curved in one dimension.
The focusing X-ray mirrors provided with X'Pert PRO diffraction systems are designed to diffract characteristic
Kα radiation. The Kβ radiation is suppressed to a level below 0.5% of its original level. Because of the
monochromatic beam, measurements with the mirror typically do not normally require a beta-filter. When you
are making measurements using an X-ray mirror you only need a diffracted beam monochromator, to reduce the
background intensity, if the incident beam evokes fluorescence radiation on the sample.
The X-ray mirror accepts approximately 0.8º of the X-ray beam from the line focus of the X-ray tube. The beam
emitted from the mirror has its secondary focus on the goniometer circle, as a result of that, focusing X-ray
mirrors are designed not only for a particular wavelength, but also for a specific goniometer radius. The focusing
X-ray mirror does not control the axial divergence of the beam; this can be controlled with the use of Soller slits.
Beam masks are used to control the axial width of the X-ray beam.
Figure 6.8: The Graded Multilayer Focusing X-ray Mirror

The main application for the focusing mirror is for X-ray powder diffraction measurements using transmission
geometry. Samples can be either: in glass capillaries, on thin X-ray transparent foil, between two foils, or,
directly mounted (foils, fibers, tablets).
The intensity per unit area of the X-ray beam coming out of the X-ray mirror is larger than that of the X-ray beam
emitted directly by the X-ray tube. This is a result of the mirror collimating the divergent beam from the X-ray
tube into a focusing beam. As a result of that, much higher intensities are obtained in the transmission geometry
than can be expected from a narrow divergence slit.
Page 6.24 07.03.27

6.3.1 Applications
The mirror can be applied for measuring powders between foils, tablets, polymeric foils and fibers, or samples
in glass capillaries.
6.3.1.1 Powders on Foil(s)

A useful method for dealing with preferred orientation problems with certain crystallite shapes is to combine
transmission and reflection measurements. In order to get good transmission results, the sample generally needs
to be prepared on an carrier that is transparent to X-rays, typically a foil with a thickness of a few micrometers.
We recommend using Kapton or Mylar foils for this purpose. These foils contribute slightly to the diffraction
pattern. Measuring the foils both with and without sample material can help to distinguish between contributions
from the sample and the carrier foil.
An important aspect of sample preparation is the effect of X-ray absorption. As a rule of thumb, samples should
be prepared so that their thickness is apprximately the absorption length of the sample material.
6.3.1.2 Pharmaceutical Formulations (Tablets)

The high penetration depth of Cu radiation in organic materials can be exploited when investigating
pharmaceutical formulations (tablets) in transmission geometry.
6.3.1.3 Foil or Fiber Samples

The focusing mirror can be used to measure the orientation distribution of (polymer) foils and fibers by varying
the angle of incidence (ω) and the rotation angle (ϕ). A transmission sample stage with the capability to step in
ϕ is required for these measurements.
6.3.1.4 Samples in Glass Capillaries

In some situations powdered materials need to be prepared in glass capillaries, some of these situations are:
• when the shape of the crystallites in the powder is such (tiles, plates, needles) that it is difficult to obtain
a random orientation distribution of the crystallites when preparing flat samples, for instance with the
backloading technique,
• when there is only a small amount of material available,
• when the sample is toxic, sensitive to air or hygroscopic (glass capillaries can be easily sealed by melting
their ends after filling.
In the focusing geometry, the 2θ resolution of a measurement depends to only a very small amount on the
diameter of the capillary; it is therefore possible to work with capillaries of up to 1 mm in diameter (or even
larger ones, depending on sample absorption or resolution required). The height of the beam at the sample
position is about 0.7 mm. When working with smaller diameter capillaries, we recommend that you reduce the
beam height in order to avoid the direct beam spilling over the capillary and to obtain a lower background.
When working with samples in glass capillaries, you should always take into account the strong dependence of
the absorption of X-rays on the atomic number of the element(s) present in the sample. Cu Kα radiation can
travel several millimeters into an organic material, but for inorganic materials the absorption depth can be much
less, and you may need to 'dilute' the sample with amorphous light element material, like crushed glass or carbon
in order to get enough transmission.
07.03.27 Page 6.25

6.3.2 PW3152/63 Focusing X-ray Mirror for Cu Radiation

The PW3152/63 Focusing X-ray mirror is an incident beam PreFIX module that is designed for use with an
X'Pert PRO MPD system with a goniometer radius of 240 mm in combination with Cu Kα radiation. It is shown
in Figure 6.9.
Figure 6.9: The PW3152/63 Focusing X-ray Mirror

eliminated, only ca. 0.5% of the Kβ line is diffracted by the mirror. The acceptance angle from the line focus of
the X-ray tube is approximately 0.8º. The beam from the X-ray mirror is a line with a thickness of about 0.7 mm
high at the position of the sample. The axial divergence and width are not controlled by the mirror. Soller slits
can be used to control the axial divergence. Optionally, a width mask can be inserted into the X-ray mirror
housing to control the axial width of the beam.
6.3.2.1 Focusing X-ray Mirror Housing

The PreFIX module housing of the focusing X-ray mirror is shown in Figure 6.9. It incorporates:
• a slot for an equatorial slit (a ½° slit is standard, smaller slits may be supplied for special applications)
• a holder to accommodate Soller slits with an additional slot for an attenuation foil or the anti-scatter
slit.
Page 6.26 07.03.27

6.3.2.2 Mirror offset

In X'Pert PRO systems the beam emitted from the X-ray mirror is offset relative to the direct beam from the
X-ray tube. This offset angle is referred to as the "mirror offset". The exact value of the mirror offset for your
system is given in the Acceptance Test Form delivered together with your focusing X-ray mirror. The zero
positions of the omega and 2theta axes of the goniometer must be adjusted by the value of the mirror offset in
order to compensate for it. The data collector software will always apply an offset whenever the focusing X-ray
mirror is present in the incident beam path (and not use it if the focusing X-ray mirror is not present in the
system); this offset is a default (calculated) value until you enter the exact offset value for your system as given
in the Acceptance Test Form.
The exact value of the X-ray mirror offset can also be determined experimentally; the procedure to do this is
6.3.3 Accessories
Those that are delivered together with the mirror: two divergence slits (a 1/2° and a 1/4°), an attenua-
tion foil, a beta-filter, and an anti-scatter slit,
and
those that must be ordered separately: Soller slits, an anti-scatter device, an automatic beam attenuator
and a beam mask set.
Information about these accessories, their use, and their mounting instructions are described in this section.
6.3.3.1 ½° and ¼° Divergence Slits

You can use a divergence slit together with an X-ray mirror in order to control the height of the X-ray beam
coming out of the X-ray mirror, and therefore the amount (length) of the sample that is irradiated.
A ½° and a ¼° divergence slit are supplied with the PreFIX module. The divergence slit should be installed in
the slit holder nearest to the X-ray tube. When the ½°divergence slit is used, the focusing X-ray mirror is
irradiated over its complete length by the X-ray beam coming from the X-ray tube's line focus. The height of the
X-ray beam emitted by the mirror at the position of the sample is then 0.7 mm. This beam height can be reduced
at the cost of intensity by choosing the ¼° slit or a divergence slit with a smaller aperture.
2. Although the slit marking reads 1/2°, the actual position of the slit with respect to the line focus
of the X-ray tube determines the acceptance angle of the X-ray mirror to be 0.8°.

An attenuation foil (Cu (0.2 mm)/Ni (0.02 mm)) is delivered together with the PW3152/63 Focusing X-ray
Mirror to reduce the intensity of the direct X-ray beam coming out of the X-ray mirror. Under typical operating
conditions the beam from the focusing X-ray mirror can have an intensity which is much greater than 1 000 000
cps. The Miniprop detector (PW3011/20) becomes non-linear in response above 1 000 000 cps and can be
damaged by higher count rates. For more details about the maximum count rates for the detectors used in X'Pert
PRO refer to Chapter 21 in Part II of this User's Guide.
CAUTION
An attenuation foil MUST be mounted in the housing slot in the
07.03.27 Page 6.27

The attenuation factor of the foil supplied with the focusing X-ray mirror is about 18 000. The exact value is
shown on the attenuator itself and on the Acceptance Test Form for the mirror, which is supplied when the
module is delivered. This value can be entered into the data collector software and is then used to automatically
adjust the measured intensity values.
6.3.3.3 Anti-scatter Slit (1.4 mm)

If you are making measurements involving small 2θ angles (<4°) and are not using any other incident beam anti-
scatter device in combination with the focusing X-ray mirror; you must use the anti-scatter slit with an aperture
of 1.4 mm that is supplied with the focusing X-ray mirror. It is shown in Figure 6.3. The slit should be inserted
in the front of the Soller slits holder or mounted on the front of the X-ray mirror module (when the Soller slits
holder is removed) or mounted on the front of the automatic beam attenuator (see also Part II - Chapter 2, section
2.2.2.5.4).
6.3.3.4 Beta-filters for X-ray Mirrors

A Ni filter intended for use with Cu radiation is included with the PW3152/63 Focusing X-ray Mirror for Cu
radiation. The filter's foil thickness is 0.02 mm. It can be used to further reduce the amount of Kβ radiation
emitted by the X-ray mirror. The beta-filter should be inserted into the slot that can also be used for the
attenuation foil.

emerging from the mirror. The Soller slits are available in different sizes as follows:
Typically, Soller slits also improve the peak-to-background ratio. The Soller slits must be installed in the Soller
slits holder at the front of the X-ray mirror. For more information about Soller slits refer to Part II - Chapter 5.
This Soller slits holder at the front of the X-ray mirror can be removed in order to make it possible to mount an
automatic beam attenuator or an anti-scatter device. If you are not actually using these devices we advise you to
mount the Soller slits holder onto the X-ray mirror.
6.3.3.6 PW3086/7x Incident Beam Anti-scatter Device for Focusing X-ray Mirror
If you want to use a focusing X-ray mirror, we advise you to have an incident beam anti-scatter slit mounted in
order to reduce the background radiation. In order to mount this slit you must first install an incident beam anti-
scatter slit holder onto the X-ray mirror. There are two types of incident beam anti-scatter slit holder that can be
used with the focusing X-ray mirror:
- The PW3086/70 Incident Beam Anti-scatter Device is designed for use in combination with a
PW3063/00 Capillary Spinner, a PW3076/00 Transmission Spinner or in high-throughput
applications.
- The PW3086/75 Incident Beam Anti-scatter Device is designed for use in combination with a
PW3064/60 Reflection-transmission Spinner.
Page 6.28 07.03.27

The PW3086/7x Incident Beam Anti-scatter Device comes with two anti-scatter slits, marked 1/2° and 1/4°. If
you would like to make use of the full beam coming off the focusing X-ray mirror, you should use the 1/2° slit.
You can use the 1/4° slit when you are working with thin capillaries or when you would like to measure at very
low angles, close to 1° 2θ. In this case it is advisable to insert a 1/4° slit in the slot for the equatorial slit on the
focusing X-ray mirror module.
The PW3086/7x Incident Beam Anti-scatter Device also contains a slot that can be used to insert a beam mask
from the PW3089/00 Beam Mask Set.
The PW3086/70 Incident Beam Anti-scatter Device includes a direct beam stop to protect the detector from
being exposed to the direct beam; and to allow measurements from 1º 2θ upwards in the capillary spinner
configuration. A special direct beam stop is delivered with Oxford Cryosystem’s Cryostream Plus. This beam
stop is used for capillary sample measurements at non-ambient temperatures (see also section 13.4.1.4 in
Chapter 13 in Part II of this User’s Guide).
For configurations in which the focusing X-ray mirror is used in combination with a PW3064/60 Reflection-
transmission Spinner, a PW3064/20 Direct Beam Stop can be mounted onto the spinner. Please refer to section
12.5.1.4 of Chapter 12 of Part II of this User's Guide for more information about this beam stop.
Information about the selection of incident and diffracted beam anti-scatter devices and in combination with
sample stages and direct beam stops is given in section 6.3.4.3.
More information about PW3086/7x Anti-scatter Devices, including mounting the beam stop, is given in
sections 20.2.4 and 20.2.5 in Chapter 20 of Part II of this User's Guide.
Figure 6.10: PW3086/70 Incident Beam Anti-scatter Device Mounted onto a Focusing X-ray Mirror
07.03.27 Page 6.29

Figure 6.11: PW3086/75 Incident Beam Anti-scatter Device Mounted onto a Focusing X-ray Mirror
6.3.3.6.1 Mounting an Incident Beam Anti-scatter Device onto a Focusing X-ray Mirror
Mount the PW3086/7x Anti-scatter Device onto the focusing X-ray mirror as follows:
1. Remove the Soller slits holder by unscrewing the screws marked B in Figure 6.9. If a beam attenuator is
mounted, refer to section 6.3.3.7.1 for information about removing it.
2. Place the anti-scatter device in the location where you just removed the Soller slits holder or automatic
beam attenuator and secure it using the two screws used to mount the Soller slits holder onto the X-ray
mirror.
Use of the incident beam anti-scatter devices is described in Part II - Chapter 20.
6.3.3.7 PW3087/60 Automatic Beam Attenuator

The PW3087/60 Automatic Beam Attenuator can be mounted on the front of the mirror housing replacing the
Soller slits holder and used in place of the foil described in section 6.3.3.2. The attenuation factor is entered into
the data collector software and is then used to automatically adjust the measured intensity values. The anti-scatter
slit (1.4 mm) described in section 6.3.3.2 is required if the automatic beam attenuator is used at low 2θ angles.
More information about the automatic beam attenuator is given in Part II - Chapter 2, section 2.2.2.
Page 6.30 07.03.27

6.3.3.7.1 Mounting the Automatic Beam Attenuator onto an X-ray Mirror

Mount the automatic beam attenuator as follows:
attenuator.
2. Split the automatic beam attenuator apart (the metal part from the painted part). This can be quite
4. Fit the metal part (NOT the side with the alignment pins) onto the brass end of the mirror; line it up
with the slit of the automatic beam attenuator to the slit on the mirror and ensure that the four screw
holes line up. Use the four short screws (M2 x 4) supplied with the automatic beam attenuator and
Now you can mount a reflectivity slit or the beam mask holder. Mounting instructions are given in Part II -
Chapter 2.
6.3.3.8 PW3089/00 Beam Mask Set

You can use beam masks together with the focusing X-ray mirror in order to control the amount (width) of the
sample that is irradiated. The following masks are supplied in the PW3089/00 Beam Mask Set: 20, 10, 4 and 2.
Table 6.10 shows the relationship between the various masks positioned in the slot for the mask in the Soller
slits holder and the amount of the sample irradiated, when used in combination with the 0.04 rad, 0.02 rad and
0.01 rad Soller slits. The beam mask must be installed into the slot for beam masks in the Soller slits holder (see
Figure 6.9).
Alternatively you can insert a beam mask into the slot for beam masks in the PW3086/7x Incident Beam Anti-
Scatter Device for Focusing X-ray Mirror. When you are using the focusing X-ray mirror in high-throughput
applications, we advise you to insert the 4 mm mask into the incident beam anti-scatter device for well plates
with a specific well distance of 9 mm.
Table 6.10: Relationship between Beam Masks and Irradiated Width
Mask 0.04 rad Soller Slits 0.02 rad Soller Slits 0.01 rad Soller Slits
20 24 mm 22 mm 21 mm
10 14 mm 12 mm 11 mm
4 8 mm 6 mm 5 mm
2 6 mm 4 mm 3 mm
For more information about beam masks, refer to Chapter 4 of Part II of this User's Guide.
6.3.4 Use
This section deals with measuring the X-ray mirror offset value and with checking the intensity of the output
from the X-ray mirror.

If your X'Pert PRO diffraction system includes a focusing X-ray mirror you must use the PW3373/10 Special
XRD X’Pert Copper X-ray Tube (see Part II - Chapter 1, section 1.3.2). The recommended high-tension
maximum generator settings for this X-ray tube are 45 kV and 40 mA.
07.03.27 Page 6.31
6.3.4.2 Measuring the X-ray Mirror Offset Value

The X-ray beam emerging from the focusing X-ray mirror is offset by a certain angle. The exact value of this
angle is given in the Acceptance Test Form supplied with your focusing X-ray mirror.
If you want to measure the offset value, you do so as follows:
1. Install a non-offset incident beam PreFIX module (for example: a fixed divergence slit or a
5. Replace the incident beam PreFIX module used in step 1 with the X-ray mirror. Do NOT report this to
the data collector software. Insert the combined copper/nickel attenuation foil into the X-ray mirror.
6. Make a 2θ scan to find the peak position of the direct X-ray beam from the X-ray mirror. Note this
position as 2θB.
7. The X-ray mirror offset is calculated by (2θB - 2θA).
are automatically offset when you select the X-ray mirror as the incident beam PreFIX module. This
means, for example: if your calculation of the offset results in -1.1º you actually enter 1.1º, whereas if
your calculation resulted in +1.1º you enter -1.1º.

To maintain the optimum intensity from the X-ray mirror the output should be checked on the following
occasions:
- After rotating the X-ray tube to the line focus position.
- After replacing the X-ray tube.
- After repeatedly mounting and dismounting the X-ray mirror module.
adjustment procedure is described in section 6.3.4.4.
6.3.4.3.1 Checking the Intensity from the X-ray Mirror

When the X-ray mirror is used as a single incident beam PreFIX module, the intensity can be checked as follows:
Tube power: 30 kV, 50 mA
Divergence slit: ½° (in the holder for an equatorial (divergence) slit)
Attenuator: Combined copper/nickel attenuation foil
Soller slits: None
If there is no peak registered near 2θ = 0º, check that the offset value was properly introduced. The absolute
intensity values must meet the specifications listed in Table 6.11. If these intensity values are not met, refer to
section 6.3.4.4.
Page 6.32 07.03.27


PW3152/63 X-ray Mirror for X'Pert PRO MPD Systems
Type Number Diffracted Beam Optics Standard
PW3093/60 & Programmable Receiving Slit (3 mm) and Programmable Anti-

PW3091/0x scatter Slit (4°) (no Soller slits) > 5.5 x 109 cps
PW3015/x0 & X'Celerator (90° rotated, receiving slit mode, maximum active > 2.4 x 109 cps
length (9 mm)) and Fixed Anti-scatter Slit Holder (no slit
PW3x94/30 inserted) (no Soller slits)
PW3015/x0 & X’Celerator (90º rotated, receiving slit mode, maximum active > 2.4 x 109 cps
length (9 mm)) and
PW3091/x0 Programable Anti-scatter Slit (4°), (no Soller slits)
PW3018/00 & PIXcel (receiving slit mode, maximum active length (14 mm)) > 3.2 x 109 cps
and
PW3490/00 Fixed Anti-scatter Slit Holder (no slit inserted) (no Soller slits)
PW3018/00 & PIXcel (receiving slit mode, maximum active length (14 mm)) > 3.2 x 109 cps
and
PW3091/70 Programable Anti-scatter Slit (4°), (no Soller slits)
NOTES: 1. When you use 0.04 rad Soller slits in the Soller slits holder of the focusing X-ray mirror, you must
expect an intensity drop of around 30%.
2. The direct beam intensities were determined with a new tube, be aware that the X-ray tube
intensities decrease in time.
3. After intensive use in the incident beam the focusing X-ray mirror will show degraded surfaces.
Therefore, the focusing X-ray mirror may not completely reach the specified intensities. If this is
the case call your local PANalytical Service Engineer.
6.3.4.4 Tube Height Adjustment

There are three factors that can lead to a reduction in intensity:
· A change in the position of the tube focus relative to the X-ray mirror.
· A reduction in the output intensity from the X-ray tube.
· A change in the X-ray mirror alignment. (This is less probable).
The focus position of an X-ray tube can change slightly over its life and because of this the output intensity
slowly drops. When a ceramic Cu X-ray tube is used with an X-ray mirror the drop of intensity should be less
than 15% per 1000 hours of use. If the output from the X-ray mirror drops more than 15% per 1000 hours of use,
adjust the tube height to reposition the focus relative to the X-ray mirror as described in the following section.
6.3.4.4.1 Tube Height Adjustment

This section describes the tube height adjustment procedure for X'Pert PRO MPD systems.
To adjust the height position of the X-ray tube relative to the focusing X-ray mirror, proceed as follows:
1. Mount the X-ray mirror onto the incident beam PreFIX position. Place a ½° divergence slit and the
combined copper/nickel attenuation foil into the focusing X-ray mirror to protect the detector. Make
sure that the mirror offset (see section 6.3.4.2) is correctly introduced in the data collector software.
2. Mount one of the diffracted beam optics as summarized in Table 6.12. Use the settings given in this
table.
stage.
07.03.27 Page 6.33

knobs at the back of the X-ray tube housing (refer to Part II - Chapter 1 - Figure 1.9).
housing to move the X-ray tube (approximately 25 µm).
increase any further (if necessary you can make smaller steps, say: approximately 10 µm); then
continue with step 11. If the intensity is lower than that noted in step 7, continue with step 10.
knurled knobs at the back of the X-ray tube housing (refer to Part II - Chapter 1 - Figure 1.9).
housing to move the X-ray tube in the opposite direction (approximately 25 µm).
does not increase any further (if necessary you can make smaller steps, say: approximately 10 µm);
6.3.4.5 Selection of Anti-scatter Devices

X-rays that are scattered by air or by the sample holder may give rise to an increased background in the
diffractogram. Anti-scatter devices are used in diffraction experiments in order to reduce the amount of scattered
radiation. This ensures that the background intensity is reduced to a low value and good signal-to-background
ratios are obtained. Which combination of incident beam and diffracted beam anti-scatter devices and beam stops
is selected in experiments employing the focusing X-ray mirror depends on the sample stage used and the
measurement requirements. Table 6.12 and Table 6.13 below give the advised combinations for a selection of
sample stages commonly used with the focusing X-ray mirror used in combination with the X’Celerator and
PIXcel, respectively.
Page 6.34 07.03.27

Table 6.12: Advised Combinations of Anti-scatter Devices, Beam Stops and Sample Stages used in
Combination with the Focusing X-ray Mirror and the X’Celerator
Incident Beam Anti- Diffracted Beam Anti-

X'Pert PRO Sample
scatter Device for scatter Device for Comments
Stage
Focusing X-ray Mirror X'Celerator Detector
PW3063/00 PW3086/70 with direct PW3x94/30 + PW3x94/35 Always use direct beam stop.
Capillary Spinner beam stop mounted Minimum 2θ angle in
measurement > 1°
PW3064/60 PW3086/75 PW3494/30 + PW3494/35 Minimum 2θ angle in

Reflection- measurement > 2.5°
transmission Spinner
PW3086/75 + PW3064/ PW3494/30 + PW3494/35 Minimum 2θ angle in
20 Direct Beam Stop measurement between 1° and
2.5°;
maximum 2θ angle: 43°
PW3076/00 PW3086/70 with direct PW3091/x0 Programma- Minimum 2θ angle in
Transmission Spinner beam stop mounted ble Anti-scatter slit (1/32°) measurement between 1° and
or 2.5°
PW3x94/30 with 5.0 mm
slit inserted
PW3086/70 PW3x94/30 + PW3x94/35 Minimum 2θ angle in

measurement > 2.5°
High-throughput measurement > 2.5°
Attachment

High-throughput measurement between 1° and
Attachment with 2.5° for 2θ scans at ω = 0°;
direct beam stop maximum 2θ angle dependent
on sample holder
NOTE: PW3x94/30 indicates that you can either use a PW3094/30 or a PW3494/30 Diffracted Beam Anti-
scatter Slit with the X'Celerator. PW3x94/35 means that you can use either a PW3094/35 or a
PW3494/35.
07.03.27 Page 6.35

Table 6.13: Advised Combinations of Anti-scatter Devices, Beam Stops and Sample Stages used in
Combination with the Focusing X-ray Mirror and the PIXcel
Incident Beam Anti-

Diffracted Beam Anti-
X'Pert PRO Sample scatter Device for
scatter Device for PIXcel Comments
Stage Focusing X-ray
Detector
Mirror
PW3063/00 PW3086/70 with PW3490/00 + PW3494/35 Always use direct beam stop.
Capillary Spinner direct beam stop Minimum 2θ angle in
mounted measurement > 1°

Reflection- measurement > 2.5°
transmission Spinner
PW3086/75 + PW3490/00 + PW3494/35 Minimum 2θ angle in
PW3064/20 Direct measurement between 1° and
Beam Stop 2.5°;maximum 2θ angle: 43°
PW3076/00 PW3086/70 with PW3091/60 Programmable Minimum 2θ angle in

Transmission direct beam stop Anti-scatter slit (1/32°) or measurement between 1° and
Spinner mounted PW3490/00 with 7.5 mm 2.5°
slit inserted
PW3086/70 PW3490/00 + PW3494/35 Minimum 2θ angle in

measurement > 2.5°
PW3077/00 High- PW3086/70 PW3490/00 + PW3494/35 Minimum 2θ angle in

throughput measurement > 2.5°
Attachment

High-throughput measurement between 1° and
Attachment with 2.5° for 2θ scans at ω = 0°;
direct beam stop maximum 2θ angle dependent
on sample holder
Page 6.36 07.03.27

Chapter 7
Incident Beam Monochromators
Contents
7.1 General................................................................................................................................. 7 - 3
7.2 High-resolution Monochromators..................................................................................... 7 - 3
7.2.1 PreFIX High-resolution Monochromators ............................................................................. 7 - 4
7.2.2 PW3110/61 Ge(220) Asymmetrical Monochromator............................................................ 7 - 7
7.2.3 PW3110/62 Ge(220) Monochromator.................................................................................... 7 - 7
7.2.4 PW3110/64 Ge(440) Monochromator.................................................................................... 7 - 7
7.2.5 PW3110/65 Ge(220) 12 mm Monochromator ....................................................................... 7 - 7
7.2.6 PW3110/66 Ge(220) Asymmetrical 12 mm Monochromator................................................ 7 - 7
7.2.7 Accessories............................................................................................................................. 7 - 8
7.2.7.1 PW3143/20 Crossed Slits Assembly for X’Pert PRO MRD Systems................... 7 - 8
7.2.7.2 PW3144/60 Crossed Slits Assembly for X’Pert PRO MPD Systems ................... 7 - 8
7.2.8 Using the High-resolution Monochromator ........................................................................... 7 - 8
7.2.8.1 Adjusting the Beam Size........................................................................................ 7 - 8
7.3 Focusing Beam Johansson Monochromators................................................................... 7 - 9
7.3.1 Applications............................................................................................................................ 7 - 9
7.3.2 PW3113/60 Focusing Beam Johansson Monochromator ...................................................... 7 - 9
7.3.2.1 Accessories .......................................................................................................... 7 - 10
7.3.3 Use........................................................................................................................................ 7 - 12
7.3.3.1 Recommended X-ray Tube Setting...................................................................... 7 - 12
7.3.3.2 Changing the Tube Shield Position ..................................................................... 7 - 12
7.3.3.3 Tube Focus Height Positioning............................................................................ 7 - 13
7.3.3.4 Tuning the Monochromator Crystal .................................................................... 7 - 14
7.3.3.5 Irradiated Length.................................................................................................. 7 - 19
07.03.27 Page 7.1

7.4 Hybrid Monochromators..................................................................................................7 - 20

7.4.1 Applications.......................................................................................................................... 7 - 20
7.4.1.1 High Resolution Applications .............................................................................. 7 - 20
7.4.1.2 Thin-film Phase Analysis & Reflectivity ............................................................. 7 - 21
7.4.1.3 Phase Analysis ..................................................................................................... 7 - 21
7.4.1.4 Omega-stress Analysis ......................................................................................... 7 - 21
7.4.1.5 Transmission ........................................................................................................ 7 - 21
7.4.2 Hybrid Monochromators for X’Pert PRO MRD Systems.................................................... 7 - 22
7.4.2.1 PW3147/00 Hybrid Monochromator 2X ............................................................. 7 - 22
7.4.2.3 Accessories........................................................................................................... 7 - 23
7.4.3 Hybrid Monochromators for X’Pert PRO MPD Systems .................................................... 7 - 27
7.4.3.3 Accessories........................................................................................................... 7 - 30
7.4.4 Using the Hybrid Monochromator........................................................................................ 7 - 36
7.4.4.1 Recommended X-ray Tube Setting ...................................................................... 7 - 36
7.4.4.2 Measuring the Offset value .................................................................................. 7 - 36
7.4.4.3 Optimizing the Intensity....................................................................................... 7 - 36
7.4.4.4 Tube Height Adjustment ...................................................................................... 7 - 40
Page 7.2 07.03.27

Part II - Chapter 7: Incident Beam Monochromators
7.1 GENERAL
Incident beam monochromators are used when, rather than the Kα doublet, the Kα1 single line of a specific
anode material is needed. In analyses where the resolution is of high importance and when the shape of the
reflection should be described accurately, the incident beam monochromator is an important tool. The
monochromator is placed in the incident beam path between the X-ray tube and the sample.
There are three types of monochromator associated with X’Pert PRO:
• High-resolution monochromators
High-resolution monochromators are four-crystal monochromators which are commonly used for
measurements on nearly perfect semiconductor crystals and epitaxial layers. They select a narrow band
out of the Kα1 line. High-resolution monochromators are described in section 7.2.
• Focusing beam Johansson monochromators
Focusing beam Johansson monochromators consist of a symmetrically cut “Johansson” Ge (111)
crystal. The monochromator provides pure Kα1 radiation; the Kα2 component of the radiation from the
X-ray tube is completely removed. The Johansson monochromator is useful for phase analysis and
crystallography using Bragg-Brentano geometry. This monochromator is described in section 7.3.
• Hybrid monochromators
Hybrid monochromators consist of a parabolic X-ray mirror and a channel-cut Ge crystal combined in
one module. Its applications range from phase analysis with parallel beam to high resolution analysis of
epitaxial layers. Hybrid monochromators are described in section 7.4.
7.2 HIGH-RESOLUTION MONOCHROMATORS

High-resolution monochromators are based on two U-shaped blocks of single-crystal nearly perfect germanium.
The crystals have (110) surfaces and are preset for Ge (220) or Ge (440) Cu Kα1 reflections. The principle of
high-resolution monochromators according to Bartels [4] can be described using Figure 7.1 as follows:
The source of an X-ray tube with a copper anode emits a full X-ray spectrum, including the Cu Kα doublet. The
first U-block in the monochromator (crystal 1 in Figure 7.1) is set at the correct Bragg angle for the Cu Kα1 line.
The X-rays are diffracted twice at the surfaces of the first crystal towards the second germanium channel cut
crystal. The second U-block is set at the same Bragg angle but the channel is not parallel to that of the first
crystal. The Cu Kα1 line is diffracted twice at the surfaces of the second crystal and emerges from the
monochromator housing parallel to the original input beam.
Now consider the beam paths of X-rays with wavelengths slightly different to that of Cu Kα1. In Figure 7.1 the
dotted line represents the beam path of a longer wavelength and the dashed line that of a shorter wavelength.
These X-rays are diffracted by the first crystal at Bragg angles respectively higher and lower than that of the Cu
Kα1 radiation. However, because the channel of the second crystal is not parallel to the first channel, the X-rays
will intercept crystal 2a at a different angle than the Bragg angle and therefore diffraction will not occur. Thus
the second channel cut crystal acts as a monochromator crystal restricting the range of wavelengths which exit
the monochromator housing. Crystal 2b reflects the monochromatic beam back to its original direction.
07.03.27 Page 7.3

Monochromator Housing
Crystal 2b Crystal 1a
X-ray
Source
Crystal 2a Crystal 1b
Figure 7.1: The principle of the Bartels Monochromator
The wavelength spread is less than the natural line width of the Cu Kα1 line. The divergence of the beam exiting
the housing is approximately equal to the width of the Darwin-Prins [5] curve, which defines the angular range
of the Bragg reflections that will occur in a perfect crystal. Each reflection at the crystal surfaces sharpens the
flanks of the diffraction profile, thus giving a very low background intensity at angles only a few seconds away
from the main peak. A more detailed description of the principles of high-resolution monochromators is given
in [4].
A variant on these channel cut monochromators are the high-resolution monochromators with asymmetrically
cut channels. In these asymmetrically cut channels the surfaces are inclined a pre-determined angle to the (110)
lattice plane. This modified diffraction geometry leads to an increase in the intensity of the monochromatic beam
at the cost of a higher angular divergence and a larger wavelength spread. For more information refer to [6].
7.2.1 PreFIX High-resolution Monochromators

Five PreFIX high-resolution monochromators which give highly monochromatic beams with well-defined
wavelengths and equatorial divergence are available for X’Pert PRO systems. Figure 7.3 shows the PreFIX high-
resolution monochromators.
Three of the monochromators are used in combination with the point focus of the X-ray tube, they are described
in sections 7.2.2 to 7.2.4.
The other two monochromators with a channel depth of 12 mm are used in combination with the line focus of
the X-ray tube, they are described in sections 7.2.5 and 7.2.6. In X’Pert PRO Extended MRD systems they are
used as the second incident beam PreFIX module, placed after the X-ray mirror.
An overview of the characteristics of these high-resolution monochromators is given in Table 7.1. The intensities
and Full Widths at Half Maximum given in Table 7.1 are measured on an X’Pert PRO MRD system with a
PW3097/60 Rocking Curve Assembly or a PW3093/60 Programmable Receiving Slit set to 3 mm without Soller
slits inserted, at the diffracted beam PreFIX position; alternatively, you can use a PIXcel (receiving slit mode,
maximum active length (14 mm)). For two of the high-resolution monochromators (PW3110/61 and
PW3110/62) data measured on an X’Pert PRO MPD system (with a goniometer radius of 240 mm) are also
given. The diffracted beam optics used for these measurements are the same as those used for measurements on
the X’Pert PRO MRD system. For the measurements with an X-ray mirror, the measurements were performed
on an X’Pert PRO Extended MRD system. The FWHMs are determined from the (111) reflection of the Si(111)
Single Crystal Reference Sample (part of PW3132/62).
Page 7.4 07.03.27

OUT IN
Ge (220) Asym.
OUT IN
Ge (440)
Shutter
Lever
Adjustment Knob
for Beam Width
OUT IN
Beam Height Adjustment Knob
Scale for Beam Height
Ge (220)
Crossed Slits
Assembly
Crossed Slits Beam Width

Scale
Holder
Figure 7.2: The Three Types of High-resolution Monochromators
Figure 7.3: The Three High-resolution Monochromators with PW3143/20 Crossed Slits Assembly
Mounted
07.03.27 Page 7.5

Table 7.1: Characteristics of High-resolution Monochromators
FWHM
Type Focus Direct Beam
Item (deg) Applications
Number type Intensity
(arc seconds)
PW3110/61 Ge(220) Point ≤ 0.0053º ≥ 650 000 cps To observe weak

Asymmetric (≤ 19”) at 35 kV, 5 mA features at
Four-crystal medium resolution
PW3110/61 Ge(220) Point ≤ 0.0059º ≥ 750 000 cps To observe weak
Asymmetric (≤ 21”) at 35 kV, 5 mA features at
Four-crystal on MPD medium resolution
PW3110/62 Ge(220) Point ≤ 0.0039º ≥ 350 000 cps Standard high

Four-crystal (≤ 14”) at 35 kV, 10 mA resolution setting
PW3110/62 Ge(220) Point ≤ 0.0039º ≥ 450 000 cps Standard high

on MPD
PW3110/64 Ge(440) Point ≤ 0.0028º ≥ 45 000 cps To resolve closely

Four-crystal (≤ 10”) at 35 kV, 40 mA spaced peaks
PW3110/65 & Ge(220) Line ≤ 0.0035º ≥ 18 000 000 cps Routine high
(12 mm) & with rocking curve at high intensities
PW3088/60 X-ray mirror assembly or
programmable
receiving slit
≥ 10 000 000 cps
with PIXcel
PW3110/66 & Ge(220) Line ≤ 0.0059º ≥ 45 000 000 cps Fast high
Asymmetric (≤ 21”) at 45 kV, 40 mA resolution
Four-crystal with rocking curve measurements at
(12 mm) assembly or medium resolution
PW3088/60 & X-ray Mirror programmable
receiving slit
≥ 26 000 000 cps
with PIXcel
NOTES: 1. The direct beam intensities were determined with a new X-ray tube. The X-ray beam emitting from
a tube decreases in time.
2. The optional crossed slits assembly should be fully opened.
3. The intensities were measured without a crossed slits assembly. If your system includes one you
should reduce the expected intensities by 10% for line focus.
4. You can only compare FWHMs values that you measure, with the values in the above table; if you
measure them on the (111) reflection of the Si(111) Single Crystal Reference Sample (part of
PW3110/62).
5. Count rates above 1 000 000 cps can saturate the detector. Make sure that you use an attenuator if
you expect values at or above this level.
6. After extensive use of high-resolution monochromators the germanium crystals will show degraded
surfaces. Therefore, extensively used monochromators may not completely reach the specified
intensities. If this is the case call your local PANalytical Service Engineer.
Page 7.6 07.03.27

Line Focus
Entrance (12 mm)
Point Focus
Entrance (5 mm)
Figure 7.4: High-resolution Monochromators - Line and Point Focus Entrances
7.2.2 PW3110/61 Ge(220) Asymmetrical Monochromator

The Ge(220) asymmetrical four-crystal monochromator provides monochromatic Cu Kα1 radiation. This
monochromator offers a very high intensity at the expense of high divergence and wavelength broadening. It is
intended for use with both X’Pert PRO MPD and X’Pert PRO MRD systems.
7.2.3 PW3110/62 Ge(220) Monochromator

The Ge(220) four-crystal monochromator provides monochromatic Cu Kα1 radiation. This monochromator is
suitable for most routine semiconductor measurements. The high intensity enables diffraction data to be
recorded with a large dynamic range providing a more detailed analysis of the sample. It is intended for use with
both X’Pert PRO MPD and X’Pert PRO MRD systems.
7.2.4 PW3110/64 Ge(440) Monochromator

The Ge(440) four-crystal monochromator provides monochromatic Cu Kα1 radiation. This monochromator is
suitable for measuring Bragg peaks of high quality semiconductor substrate materials, where peak widths below
12 arc sec are expected. The four reflections give a beam profile which is close to rectangular - leading to an
extremely low background count rate.
The Ge(440) four-crystal monochromator is intended for use with X’Pert PRO MRD systems.
7.2.5 PW3110/65 Ge(220) 12 mm Monochromator

The Ge(220) four-crystal monochromator provides monochromatic Cu Kα1 radiation. The channels are 12 mm
high, therefore this monochromator is suitable for use in combination with the line focus of the X-ray tube and
an X-ray mirror on an X’Pert PRO Extended MRD system. This monochromator is especially recommended for
use with the X-ray mirror where high intensities are required and a higher background intensity can be tolerated.
7.2.6 PW3110/66 Ge(220) Asymmetrical 12 mm Monochromator

The Ge(220) asymmetrical four-crystal monochromator provides monochromatic Cu Kα1 radiation. The
channels are 12 mm high, therefore this monochromator is suitable for use in combination with the line focus of
the X-ray tube and an X-ray mirror on an X’Pert PRO Extended MRD system. This monochromator offers high
intensity at the expense of a high divergence and wavelength broadening.
07.03.27 Page 7.7
7.2.7 Accessories
7.2.7.1 PW3143/20 Crossed Slits Assembly for X’Pert PRO MRD Systems
The PW3143/20 Crossed Slits Assembly (see Figure 7.3) is an optional device for use with a high-resolution
monochromator on an X’Pert PRO MRD system. It controls how much of the sample that is irradiated (both
length and width) by the beam emitting from the high-resolution monochromator. The slit opening can be
continuously adjusted between 0 mm and 10 mm. The accuracy of the opening is ± 0.02 mm.
This accessory is factory aligned and therefore should not be removed from the PreFIX module.
NOTE: When a crossed slits assembly is fitted onto a line focus high-resolution monochromator the direct
beam intensity with the crossed slits fully open is reduced by approximately 10% with respect to
the intensity given in Table 7.1.
7.2.7.2 PW3144/60 Crossed Slits Assembly for X’Pert PRO MPD Systems
Figure 7.5: PW3144/60 Crossed Slits Assembly Mounted onto a

High-resolution Monochromator
The PW3144/60 Crossed Slits Assembly for X’Pert PRO MPD systems (see Figure 7.5) is an optional device for
use with PW3110/61 and PW3110/62 High-resolution Monochromators on an X’Pert PRO MPD system. It
controls how much of the sample that is irradiated (both length and width) by the beam emitting from the high-
resolution monochromator. The slit height and mask width apertures can be set to the following sizes: 5.00 mm,
4.00 mm, 3.00 mm, 2.00 mm, 1.00 mm, 0.75 mm, 0.50 mm and 0.25 mm. Any combination of slit and mask
openings is possible. The accuracy of the slit and mask opening size is ± 0.05 mm.
This accessory is factory aligned, and therefore should not be removed from the PreFIX module.
7.2.8 Using the High-resolution Monochromator

The general set-up for high resolution experiments (rocking curve measurements, reciprocal space maps and so
on) is described in Chapters 16 and 19 in Part II of this User’s Guide. This section describes how to use the
crossed slits assembly to adjust the beam size.
7.2.8.1 Adjusting the Beam Size

If you have the accessory PW3143/20 Crossed Slits Assembly for X’Pert PRO MRD systems you can adjust the
aperture by means of two knobs (one vertical and one horizontal) to allow a gap of between 0 and 10 mm to be
set. The knob scales are graduated in steps of 0.02 mm. The knob nearest to the X-ray tube controls the width of
the X-ray beam and the knob furthest away from the tube controls the height of the beam.
Page 7.8 07.03.27

If a PW3144/60 Crossed Slits Assembly for X’Pert PRO MPD systems is mounted onto a high-resolution
monochromator you can set the aperture by rotating the metal disks to the selectable openings of between 0.25
mm and 5.00 mm. The disk nearest to the X-ray tube controls the width of the X-ray beam and the disk furthest
away from the tube controls the height of the beam.
The height of the X-ray beam passing through the high-resolution monochromator is 1.2 mm. This size can be
reduced by making the aperture smaller.
For a detailed description of the relationship between the size (height and width) of the beam coming out of the
high-resolution monochromator and the irradiated area on the sample, refer to Fewster [7].
7.3 FOCUSING BEAM JOHANSSON MONOCHROMATORS

Focusing beam Johansson monochromators are designed to provide a pure Kα1 line out of the spectrum emitted
from an X-ray tube. Furthermore, they reduce the axial divergence of the X-ray beam, which improves the shape
of the peaks in a diffractogram. As a result, powder patterns measured using these monochromators are easier
to interpret and are more suitable to use for various types of analyses, such as: Rietveld analysis, and size-strain
analysis.
The focusing beam Johansson monochromator basically consists of a curved crystal which accepts the line focus
from an X-ray tube and focuses the monochromatic beam on the focusing circle of the X-ray diffractometer.
7.3.1 Applications
The Johansson monochromator is used in experiments where the peak shape and/or the integrated intensities of
the diffraction peaks must be determined very accurately. Use of the Kα doublet results in broadened or doubled
peaks in the diffractogram. Procedures for mathematical “stripping” of the Kα2 exist, but they are not ideal. They
sometimes leave “ripples” in the tails of the peaks, or they change the peak shape slightly. Using a Johansson
monochromator circumvents the requirement to apply Kα2 stripping to experimental data. The use of a
monochromator enables the production of data which allow crystal structure solving from powder diffraction
measurements, indexing of powder patterns, Rietveld refinement and size-strain analysis.
7.3.2 PW3113/60 Focusing Beam Johansson Monochromator

The Johansson monochromator available in X’Pert PRO Alpha-1 systems consists of a symmetrically cut curved
Ge(111) crystal. The Johansson monochromator can be used on an X’Pert PRO MPD system with copper or
cobalt radiation at a goniometer radius of 240 mm. The actual configuration which is factory aligned is indicated
on the Acceptance Test Form delivered with your system. The Johansson monochromator is shown in Figure
7.6. It comprises a monochromator assembly which is factory mounted onto a special interface and two anti-
scatter pipes. An entrance nozzle with a lever is used to activate the safety switch on the X-ray tube. An
irradiation slit must be inserted into the monochromator assembly. The irradiation slit limits the germanium
crystal’s acceptance of the X-ray beam from the line focus of the X-ray tube to 2º. The equatorial and axial
divergences of the incident X-ray beam emerging from the monochromator are 2º. The equatorial divergence
can be further controlled by using a divergence slit mounted on the PreFIX incident beam module position. The
axial divergence is controlled by Soller slits, however, you should note that the axial divergence of the
monochromator (2º) is about the same as that of a 0.04 rad Soller slits assembly. This means that, in general,
there is no need to use incident beam Soller slits in combination with a Johansson monochromator. The intensity
of the Kα2 line is reduced by the monochromator to less than 2% of the intensity of the Kα1 line.
The interface onto which the monochromator is mounted has two positions where the tube shield can be placed:
the standard position and the α1 position. When the tube shield is placed in the α1 position the X-rays from the
tube are accepted by the monochromator as is shown in Figure 7.8. The X-ray beam is focused on the (virtual)
line focus position of the Bragg-Brentano geometry. This geometry is called the α1 reflection geometry. When
the tube is placed in the standard position as is shown in Figure 7.9, all other diffraction geometries applicable
to X’Pert PRO MPD can be configured.
07.03.27 Page 7.9

Figure 7.6: PW3113/60 Focusing Beam Johansson Monochromator with Anti-scatter Pipes
7.3.2.1 Accessories
7.3.2.1.1 Irradiation Slits
Two irradiation slits marked Cu and Co are included with the PW3113/60 Focusing Beam Johansson
Monochromator. They are for use with copper and cobalt radiation respectively. They are shown in Figure 7.7.
When this slit is inserted, it limits the germanium crystal’s acceptance of the X-ray beam from the line focus of
the X-ray tube to 2º. The crystal is then irradiated over its complete length by the X-ray beam.
Figure 7.7: Irradiation Slits for Copper and Cobalt Radiation
Page 7.10 07.03.27

7.3.2.1.2 Alignment Shaft

An alignment shaft for X’Pert PRO MPD systems is included with the incident beam monochromator. This
alignment shaft is used in the procedure for tube height fine adjustment employing the single knife edge (refer
to section 1.4.9.2 of Chapter 1 in Part II of this User’s Guide).
The alignment shaft is described in more detail in section 12.10 of Chapter 12 in Part II of this User’s Guide).
Figure 7.8: Tube Shield in α1 Position
Figure 7.9: Tube Shield in Standard Position
07.03.27 Page 7.11

7.3.3 Use
If you have an X’Pert PRO Alpha-1 system that is aligned for use with copper radiation you must use the special
ceramic copper X-ray tube (see Part II - Chapter 1, section 1.3.2). The recommended high-tension generator
maximum settings for this X-ray tube are 45 kV and 40 mA.
If your incident beam monochromator is aligned for use with cobalt radiation you must use the PW3376/00
Ceramic Cobalt X-ray Tube. The recommended high-tension generator settings for this X-ray tube used together
with a Johansson monochromator are 40 kV and 40 mA.
7.3.3.2 Changing the Tube Shield Position

The tube shield can be mounted on two positions on the monochromator interface. This section describes how
to move the tube shield from the standard position to the α1 position, and vice versa.
7.3.3.2.1 Placing the Tube Shield at the α1 Position
Move the tube shield from the standard to the α1 position as follows:
1. Use the data collector software to switch the generator off.
CAUTION
Failure to switch the generator off could result in flashovers and/or
tube damage.
2. Dismount any incident beam PreFIX modules.

3. Insert the T-bar shaped PreFIX key into the PreFIX locking screw located behind the X-ray tube
(between the tube and the mounting arm).
4. Use one hand to hold the tube in place against the PreFIX mounting block to prevent it falling into the
enclosure and undo the locking screw. Be careful here as the tube shield is heavy; if you are not sure
about your ability to do this yourself we suggest that you use two hands to hold the tube shield and get
somebody else to undo the locking screw.
5. Put the PreFIX key into the PreFIX locking screw of the α1 position ready for the next step.
6. Move the tube shield from the standard position out to the α1 position. Tighten the PreFIX locking
screw.
7. Mount the incident beam PreFIX module, usually a fixed or programmable divergence slit.
8. Insert the long anti-scatter pipe between the incident beam PreFIX module and the Johansson
monochromator (see Figure 7.6). Slide the upper inner part of the pipe into the monochromator housing
and secure it in place with the knurled knob.
9. Locate the shorter anti-scatter pipe between the monochromator and the tube shield, undo the shutter
lever positioning screw and slide the inner part of the pipe into the monochromator housing and secure
it in place with the knurled knob (see Figure 7.6). Tighten the shutter lever positioning screw enough to
actuate the shutter microswitch.
10. Use the data collector software to switch the generator on again.
11. It should not need adjusting, but you can if you wish at this time, check the alignment of the
monochromator as described in section 7.3.3.4.
Page 7.12 07.03.27

7.3.3.2.2 Placing the Tube Shield at the Standard Position

Move the tube shield from the α1 to the standard position as follows:
1. Use the data collector software to switch the generator off.
CAUTION
Failure to switch the generator off could result in flashovers and/or
tube damage.
2. Undo the shutter lever positioning screw and the knurled knob on the short anti-scatter pipe (see Figure
7.6). Slide the anti-scatter pipe carefully out of the monochromator housing and remove it.
3. Undo the knurled knob on the long anti-scatter pipe (see Figure 7.6). Slide the anti-scatter pipe
carefully out of the monochromator housing and remove it.
4. Dismount the divergence slit module.
5. Insert the T-bar shaped PreFIX key into the PreFIX locking screw located behind the X-ray tube
(between the tube and the mounting arm).
6. Use one hand to hold the tube in place against the PreFIX mounting block to prevent it falling into the
enclosure and undo the locking screw. Be careful here as the tube shield is heavy; if you are not sure
about your ability to do this yourself we suggest that you use two hands to hold the tube shield and get
somebody else to undo the locking screw.
7. Put the PreFIX key into the PreFIX locking screw of the standard position ready for the next step.
8. Move the tube shield from the α1 position out to the standard position. Tighten the PreFIX locking
screw.
9. Mount the incident beam PreFIX module that you are going to use in your next experiment.
10. Use the data collector software to switch the generator on again.
We advise you to check the tube height position according to the procedure given in section 1.4.9 in Chapter 1
in Part II of this User’s Guide.
7.3.3.3 Tube Focus Height Positioning

Generally, mechanical alignment of the X-ray tube with respect to the Johansson monochromator is not required,
however, it may sometimes be necessary to check if this is in fact the case. Operation of the monochromator
requires optimal alignment and is sensitive to the relative position of the tube focus and the monochromator
crystal. If, for example, the focus position is changed, it may cause the Kα2 spectral line to be reflected instead
of the Kα1. Even worse, both spectral lines may not be reflected at all.
The procedure to adjust the tube height requires that the tube is mounted at the standard position on the
monochromator interface. Placing the tube shield in this position is described in section 7.3.3.2.2. The tube
height alignment check and adjustment can then be performed according to the procedures given in section 1.4.9
of Chapter 1 in Part II of this User’s Guide.
When the tube height is correct at the standard position it is automatically correct for the α1 position.
07.03.27 Page 7.13

7.3.3.4 Tuning the Monochromator Crystal

Under normal operating conditions the monochromator crystal does not need to be re-adjusted. If however, the
measured peaks show a fraction of the Kα2 line, or if the tube shield has just been moved to the α1 position, then
one of the following procedures should be carried out to fine-tune the monochromator crystal. Before you start
the monochromator re-alignment procedure ensure that the tube focus is correctly aligned as described in section
7.3.3.3 above.
There are two procedures for aligning the monochromator. One procedure is for when there is a proportional
point detector or a PIXcel on the diffracted beam side (section 7.3.3.4.1), the other procedure describes the
monochromator alignment with the use of an X'Celerator (section 7.3.3.4.2).
7.3.3.4.1 Tuning the Monochromator Crystal for a Point Detector
This section describes how to align the monochromator crystal when your system has a point detector or a
PIXcel. If your system has an X’Celerator detector you should align the monochromator crystal as described in
section 7.3.3.4.2.
Proceed as follows to tune the monochromator crystal:
1. Mount the tube shield at the α1 position as described in section 7.3.3.2.1.
2. Mount a programmable receiving slit with a (fixed or programmable) anti-scatter slit and point detector
onto the diffracted beam position. Alternatively, you can mount a PIXcel detector with an anti-scatter
slit (fixed or programmable).
3. Insert the Cu attenuator (0.1 mm) supplied with the X’Pert PRO system into the divergence slit holder.
4. Set the HT generator to 45 kV and 40 mA when you are using copper radiation, or to 40 kV and 40 mA
if you are using cobalt radiation.
5. Move the 2theta and omega axes of the goniometer to 0º and make sure that the direct beam is not
obstructed by the sample or the sample holder.
6. Set the (fixed or programmable) divergence slit to 1º, the (fixed or programmable) anti-scatter slit to 1º
and the programmable receiving slit to 0.1 mm. If you have a PIXcel, set it to receiving slit mode with
an active length of 0.165 mm, set the anti-scatter slit to 1° or insert a 9.1 mm slit into the fixed anti-
scatter slits holder.
7. Use the utility in the data collector software for the alignment of motorized monochromators (System
Maintenance - Monochromator Alignment) to perform a “scan up” with the following settings:
Step size 10
Time per step (s) 0.1
Number of steps 100
Stop level (cps) unchecked
NOTES: a. In order for the System Maintenance - Monochromator alignment tool to be available, the
monochromator must have been reported in the configuration.
b. During the scan set the scaling to counts per second and select automatic change of intensity
scaling on the measurement graph displayed by the data collector software.
Page 7.14 07.03.27

A typical monochromator alignment scan is shown in Figure 7.10. Two peaks can be observed on this scan: the
Kα1 and the Kα2 peak. Please note that in a monochromator alignment scan the Kα2 peak is on the left-hand
side of the Kα1 peak.
8. The following actions depend on the plot displayed on your screen:
a. If your scan shows two peaks, go to step 9.
b. If your plot shows a graph in which the intensity decreases with increasing incremental numbers,
perform a “scan down” with the following settings:
Step size 10
Number of steps 200
Repeat this “scan down” procedure until you have found the maximum Kα1 peak, then go to step 9.
Incremental number
Figure 7.10: Typical Monochromator Alignment Scan (Point Detector)
c. If your plot shows a graph in which the intensity increases with increasing incremental numbers, or
if only the left-hand part of the Kα2-Kα1 profile (below the maximum of the Kα1 peak) is
displayed, perform a “scan up” with the following settings:
Step size 10
Number of steps 200
Repeat this “scan up” procedure until you have found the maximum Kα1 peak, then go to step 9.
d. If your plot does not show any peaks, or decreasing intensity on the left, or increasing intensity on
the right, the monochromator is a long way from its correct position. To find the Kα2-Kα1 profile
as shown in Figure 7.10 perform a scan down with the following settings:
Step size 10
Number of steps 200
07.03.27 Page 7.15

If your scan now fits the description of cases a, b or c, continue with the procedure given in that
step. Otherwise perform a “scan up” employing a longer measurement range with the following
settings:
Step size 10
Number of steps 400
Repeat this procedure doubling the number of steps and scanning in opposite directions until your
scan fits the description of one of the cases a, b or c, then continue with the procedure given in that
step.
9. Take a note of the maximum intensity.
10. Select a “Stop level” that is approximately 10% below the maximum intensity noted in step 9.
11. Depending on the current position, scan up or down to the stop level as determined in step 10 with the
following settings:
Step size 5
Number of steps 100
Step level (cps) as determined in step 10.
12. Repeat the “scan up” and “scan down” routines in a “trial and error” method using a step size of 5, a
time per step of 1 second or longer without using a stop level, until the monochromator is tuned to the
maximum intensity (±1%) of the Kα1 peak.
13. To check an optimum monochromator setting is reached, perform a stationary measurement with the
following parameters:
2θ 0°
ω 0°
Mode Pre-set time
Time (s) 30.0
Receiving slit 0.1 mm
or
PIXcel mode Receiving slit = 0.165 mm.
14. As soon as the stationary measurement has been executed you can read out the measured value below
the intensity bar on the data collector window. The value should match the earlier noted value for the
maximum intensity (±1%) of the Kα1 peak.
a. If the value matches the earlier noted value for the maximum intensity (±1%) of the Kα1 peak you
have correctly aligned the monochromator.
b. If it does not, repeat the procedure from step 11 on.
This completes the monochromator alignment; the system is ready for use.
NOTE: After intensive use in the incident beam the germanium crystal may show a degraded surface.
Therefore, the intensity coming of an extensively used Johansson monochromator as determined
during first time use, may not be reached completely.
Page 7.16 07.03.27

7.3.3.4.2 Tuning the Monochromator Crystal for an X’Celerator Detector

This section describes how to align the monochromator crystal when your system has an X’Celerator detector.
If your system has a point detector or a PIXcel you should align the monochromator crystal as described in
section 7.3.3.4.1.
1. Mount the tube shield at the α1 position as described in section 7.3.3.2.1.
2. Mount a programmable or fixed divergence slit holder onto the incident beam PreFIX position. Mount
the Cu attenuator (0.1 mm) supplied with the X’Pert PRO system into the divergence slit holder.
3. Mount the X'Celerator with a fixed or programmable anti-scatter slit at the diffracted beam PreFIX
position on the goniometer. Insert 0.04 rad Soller slits into the X'Celerator module. Do not use a Ni
filter.
4. Insert a beam mask with mask marking 10, and 0.04 rad Soller slits into the programmable or fixed
divergence slit holder. Set the (fixed or programmable) divergence slit to 1º.
5. Depending on the anti-scatter device used, either set the programmable anti-scatter slit to 1º, or insert a
6.6 mm slit into the fixed anti-scatter slit holder. Set the X'Celerator in Receiving Slit mode with an
active length of 2.17 mm.
6. Set the HT generator to 45 kV and 40 mA when you are using copper radiation, or to 40 kV and 40 mA
if you are using cobalt radiation.
7. Move the 2theta and omega axes of the goniometer to 0º and make sure that the direct beam is not
obstructed by the sample or the sample holder.
8. Use the utility in the data collector software for the alignment of motorized monochromators (System
Maintenance - Monochromator Alignment) to perform a “scan down” with the following settings:
Step size 10
Number of steps 400
NOTES: a. In order for the System Maintenance - Monochromator alignment tool to be available, the
monochromator must have been reported in the configuration.
b. During the scan set the scaling to counts per second and select automatic change of intensity
scaling on the measurement graph displayed by the data collector software.
A typical monochromator alignment scan is shown in Figure 7.11. Two peaks can be observed on this
scan: the Kα1 and the Kα2 peak. Please note that in a monochromator alignment scan the Kα2 peak is
on the left-hand side of the Kα1 peak.
Figure 7.11: Typical Monochromator Alignment Scan (X’Celerator Detector)
07.03.27 Page 7.17

NOTE: After execution of the first monochromator scan it may turn out that you have to fine tune the
settings in such a way that the maximum intensity value of the Kα1 peak reaches about 100 000 cps.
9. The following actions depend on the plot displayed on your screen:

a. If your scan shows two peaks, go to step 10.
b. If your plot shows a graph in which the intensity decreases with increasing incremental numbers,
perform a “scan down” with the following settings:
Step size 10
Number of steps 400
Repeat this “scan down” procedure until you have found the maximum Kα1 peak, then go to step
10.
c. If your plot shows a graph in which the intensity increases with increasing incremental numbers, or
if only the left-hand part of the Kα2-Kα1 profile (below the maximum of the Kα1 peak) is
displayed, perform a “scan up” with the following settings:
Step size 10
Number of steps 400
Repeat this “scan up” procedure until you have found the maximum Kα1 peak, then go to step 10.
d. If your plot does not show any peaks, or decreasing intensity on the left, or increasing intensity on
the right, the monochromator is a long way from its correct position. To find the Kα2-Kα1 profile
as shown in Figure 7.11 perform a scan down with the following settings:
Step size 10
Number of steps 400
If your scan now fits the description of cases a, b or c, continue with the procedure given in that
step. Otherwise perform a “scan down” employing a longer measurement range with the following
settings:
Step size 10
Number of steps 800
Repeat this procedure doubling the number of steps and scanning in opposite directions until your
scan fits the description of one of the cases a, b or c, then continue with the procedure given in that
step.
10. Zoom into the top peak area of the Kα1 peak, move the cursor to the maximum intensity value and take
a note of the maximum intensity. Calculate the 95% level of the maximum intensity.
11. Perform a scan in the opposite direction to the scan that you last performed, with the following settings:
Step size 5
Number of steps 200
Stop level (cps) 95% of the maximum intensity, as calculated in step 10.
Page 7.18 07.03.27

12. To check if optimum monochromator setting is reached, perform a stationary measurement with the
following parameters:
2θ: 0°
ω: 0°
Mode: Pre-set time
Time (s): 30.0
X'Celerator mode: Receiving slit = 2.17 mm
13. After execution of the stationary measurement, you can immediately read out the measured value
below the intensity bar on the data collector window. The value should match the earlier noted value for
the maximum intensity (± 1%) of the Kα1 peak.
a. If the value matches the earlier noted value for the maximum intensity of the Kα1 peak, you have
correctly aligned the monochromator.
b. If this is not the case, perform a scan in the same direction as in step 11 with the following
parameters:
Step size 5
Number of steps 200
After you have performed this scan, repeat this alignment procedure from step 10 onwards. Use a
higher percentage of the maximum intensity as stop level, for instance 96%, until the value measured in
step 12 matches the value of the maximum intensity of the Kα1 peak.
This completes the monochromator alignment; the system is ready for use.
NOTE: After intensive use in the incident beam the germanium crystal may show a degraded surface.
Therefore, the intensity coming of an extensively used Johansson monochromator as determined
during first time use, may not be reached completely.
7.3.3.5 Irradiated Length

The size of the monochromator crystal limits the maximum divergence of the incident X-ray beam emitted by
the monochromator to 2º. This value is also the maximum setting of the divergence slit used in combination with
the monochromator. Selecting a divergence slit setting larger than 2º will not increase the measured intensities.
As a result of this, the maximum irradiated length that can be used with a programmable divergence slit depends,
amongst other parameters, on the maximum 2θ angle that is to be measured. In a symmetrical (θ-2θ) scan this
means that the maximum angle of incidence ω equals the maximum 2θ angle divided by 2.
The relationship between the irradiated length on the sample and the incident beam angle is given by:
L = -------------------------------------------------
-
( sin2 ω – sin2 ( δ ⁄ 2 ) )
where L = the irradiated length on the sample,

δ = the divergence slit opening in degrees,
ω = the angle between the incident beam and the sample surface in degrees.
The maximum irradiated length for a programmable divergence slit used in the automatic mode can be
calculated using the above formula. To do so, choose the maximum incident beam angle in the scan for ω. The
maximum divergence angle (2º) is chosen for δ.
07.03.27 Page 7.19

7.4 HYBRID MONOCHROMATORS

The hybrid monochromator (see Figure 7.12) is a special kind of beam conditioner, which is able to convert the
divergent X-ray beam from a line tube focus to a quasi-parallel beam with a pure Kα1 radiation component. A
hybrid monochromator consists of a parabolic shaped graded multi layer (X-ray mirror) and a special channel-
cut germanium crystal. The X-ray mirror performs a pre-collimation of the divergent beam to a quasi-parallel
beam. Thereafter the Kα1 spectral component is separated by the monochromator crystal.
Parabolic To the Sample

Shape X-ray Mirror
Crystal
Line Focus of Hybrid Monochromator

X-ray Tube
Figure 7.12: The Beam Path in a Hybrid Monochromator
Using a hybrid monochromator will cause the X-ray beam to be offset.
The major characteristic of the hybrid monochromator is in the unique combination of the parameters of beam
coming out of it. By passing a slightly more broad spectral range than traditional four-crystal dispersive high-
resolution monochromators, the hybrid monochromators delivers a much more intense parallel beam of Kα1
radiation. The Kα2 component is suppressed to a level below 0.1%. This makes it suitable for many different
applications, ranging from high resolution measurements to phase analysis.
The use of hybrid monochromators in various applications is described in section 7.4.1.
Two types of the hybrid monochromators are available, the Hybrid Monochromator 2X (PW3147/00) and the
Hybrid Monochromator 4X (PW3147/20). They differ by the size of the channel cut crystal and are intended for
different application areas (section 7.4.1). Their descriptions are given in sections 7.4.2.1 and 7.4.2.2.
There are two types of hybrid monochromator are available for use on X’Pert PRO systems, they are:
• Hybrid monochromator for X’Pert PRO MRD systems
This type of hybrid monochromator is designed for use on an X’Pert PRO MRD system with a
goniometer radius of 320 mm. These hybrid monochromators are described in section 7.4.2.
• Hybrid monochromator for X’Pert PRO MPD systems
This type of hybrid monochromator is designed for use on an X’Pert PRO MPD system with a
goniometer radius of 240 mm. These hybrid monochromators are described in section 7.4.3.
7.4.1 Applications
The hybrid monochromator can be applied for measuring epitaxial layers, thin polycrystalline films, powders
and stressed materials, or samples between foils.
7.4.1.1 High Resolution Applications

The major advantage of using hybrid monochromators for measuring rocking curves and reciprocal space maps
on the epitaxial layers is the intensity in combination with the high resolution. The gain measured on the Si(111)
reflection of a Si(111) single crystal substrate, compared to an X-ray mirror with a Ge(220) asymmetric four-
crystal monochromator, is approximately 2 (and 8) times higher for the high-resolution monochromator 4X (and
2X). This may significantly reduce measuring time for maps and rocking curves.
Page 7.20 07.03.27

The hybrid monochromators are less applicable for rocking curve measurements at 2θ angles above 90°. The
hybrid spectral band-pass of a hybrid monochromator is broader than that of four-crystal high-resolution
monochromators. At high 2θ angles the wavelength dispersion causes broad diffraction peaks, leading to a
decrease in system resolution.
A small fraction of the Kα2 radiation (0.05%-0.1%) is present in the X-ray spectrum emitting from a hybrid
monochromator. It may become visible during reciprocal space mapping with large dynamic range.
7.4.1.2 Thin-film Phase Analysis & Reflectivity

The hybrid monochromators can be applied for measurements at a fixed low angle of incidence on thin films,
and reflectivity. The monochromatic parallel incident beam reduces the background intensity and improves the
resolution.

The hybrid monochromator 2X can be applied for powder diffraction in combination with a parallel plate
collimator. The absence of the Kα2 component simplifies interpretation of data. Also the monochromatization
of the incident beam improves the signal-to-background ratio. This makes the measurements suitable for phase
analysis and Rietveld analysis. The application of parallel beam geometry ensures that the peak positions are
insensitive to sample shift and roughness.
The hybrid monochromator can also be used together with the combination of a programmable receiving slit and
a secondary mirror on the diffracted beam side. In this configuration the resolution of the diffracted X-ray beam
by the analysis module is continuously variable. The geometry formed in this configuration is a variant of the
mirror-mirror geometry with pure Kα1 radiation. It is suitable for phase analysis on loosely prepared powder
samples.
The small height and the high intensity of the X-ray beam coming out of the hybrid monochromator makes it
also suitable for use in measurements on powder samples in sealed glass capillaries.
When the hybrid monochromator is used for phase analysis of polycrystalline samples the irradiated area of the
sample is normally less than with the divergent beam in Bragg-Brentano geometry. The parallel beam geometry
and the reduced irradiated area both lead to a reduced number of crystallites from a random powder contributing
to the measured intensity. The particle statistics can be a serious problem for materials with large grain size. It
often results in the increase of the measurement time and the necessity for sample oscillation. If the particle
statistics are poor, the peak from the powder sample will show the internal structure from different crystallites.

The hybrid monochromator 2X in combination with parallel plate collimators can be used for omega-stress
measurements, where the sample is inclined in the equatorial plane. The hybrid monochromator can be used to
determine the peak position accurately since Kα2 stripping is not necessary and the background intensity is very
low. The parallel beam geometry makes the measurement insensitive to sample misalignment. It is also suited
for irregularly shaped samples.
7.4.1.5 Transmission
The hybrid monochromator 2X can be used to measure thin foils in the transmission mode with Kα1 radiation
only. A parallel plate collimator is used on the diffracted beam side. The transmission geometry is especially
useful for measurements on polymer foils, which have low X-ray absorption and often show a preferred
orientation of their molecular structure.
07.03.27 Page 7.21

7.4.2 Hybrid Monochromators for X’Pert PRO MRD Systems

There are two types of hybrid monochromator for X’Pert PRO MRD systems, differing by the number of
reflections in the channel cut crystal.
• PW3147/00 Hybrid Monochromator 2X with two reflections in the channel cut crystal. This is described
in section 7.4.2.1.
• PW3147/20 Hybrid Monochromator 4X with four reflections in the channel cut crystal. This is described
in section 7.4.2.2.
7.4.2.1 PW3147/00 Hybrid Monochromator 2X

The hybrid monochromator 2X is an incident beam PreFIX module, consisting of a combination of an X-ray
mirror and a two-crystal Ge(220) two-bounce monochromator. It is shown in Figure 7.13.
This monochromator provides monochromatic Cu Kα1 radiation. The acceptance angle from the line focus of
the X-ray tube is 0.8°. The Cu Kα2 radiation is suppressed to a level below 0.1%.
The height of the X-ray beam emerging from the hybrid monochromator is 1.2 mm. The axial divergence and
width are not controlled by the hybrid monochromator. A beam mask can be used to control the width; Soller
slits are used to control the axial divergence of the X-ray beam. A summary of the characteristic intensities and
Full Widths at Half Maximum as measured on the Si(111) reflection on the Si Single Crystal Reference Sample
(part of PW3132/62) is given in Table 7.4 and Table 7.6.
7.4.2.1.1 Hybrid Monochromator Housing

The hybrid monochromator housing is shown in Figure 7.13.
Figure 7.13: PW3147/x0 Hybrid Monochromator for X’Pert PRO MRD Systems
Page 7.22 07.03.27

The module housing incorporates:

• a holder for an equatorial slit (a 1/2° slit is standard, smaller slits may be supplied for special
applications)
• a slot for an attenuation foil
• a housing to accommodate the Ge crystal.
CAUTION
The slit holder and the crystal housing must never be removed.
7.4.2.1.2 Hybrid Monochromator Offset

In X’Pert PRO systems the beam emitted from the hybrid monochromator is offset relative to the direct beam
from the X-ray tube. This offset is referred to as the hybrid monochromator offset.
The offset of the beam coming out of the hybrid monochromator is approximately 3°. The exact value is given
in the Acceptance Test Form supplied with the hybrid monochromator. The zero positions of the omega and
2theta axes of the goniometer must be adjusted by the value of the hybrid monochromator offset in order to
compensate for it. The data collector software will always apply an offset whenever the hybrid monochromator
is present in the incident beam path (and not use it if the hybrid monochromator is not present in the system);
this offset is a default (calculated) value until you enter the exact offset value for your system as given in the
Acceptance Test Form. The method of measuring the offset is given in section 7.4.4.2.

mirror and a two-crystal Ge(220) four-bounce monochromator. This monochromator provides monochromatic
Cu Kα1 radiation. The acceptance angle from the line focus of the X-ray tube is 0.8°. The Cu Kα2 radiation is
suppressed to a level below 0.1%. The height of the X-ray beam emerging from the hybrid monochromator is
1.2 mm. The axial divergence and width are not controlled by the hybrid monochromator. A beam mask can be
used to control the width; Soller slits are used to control the axial divergence of the X-ray beam. A summary of
the characteristic intensities and Full Widths at Half Maximum as measured on the Si(111) reflection on the Si
Single Crystal Reference Sample (part of PW3132/62) is given in Table 7.4 and Table 7.6.
The physical appearance of the hybrid monochromator 4X is the same as that of the hybrid monochromator 2X
tube is referred to the hybrid monochromator offset. This offset is described in more detail in section 7.4.2.1.2.
7.4.2.3 Accessories
The accessories that can be used together with hybrid monochromators fall into two groups:
Those that are delivered with the hybrid monochromator (1/2º and a 1/4º divergence slit, and
attenuation foils),
and
those that must be ordered separately (low angle fixed slits, an incident beam anti-scatter slit holder,
Soller slits and automatic beam attenuators).
07.03.27 Page 7.23


You can use a divergence slit together with a hybrid monochromator in order to control the height of the X-ray
beam coming off the hybrid monochromator and therewith the amount (length) of the sample that is irradiated.
A 1/2º and a 1/4° divergence slits are supplied with the PreFIX module. When the 1/2° slit is used, the X-ray
mirror inside the hybrid monochromator module is irradiated by the X-ray beam coming from the X-ray tube’s
focus over the complete length. The height of the X-ray beam emitted by the hybrid monochromator is 1.2 mm.
The beam height can be reduced by choosing a divergence slit with a smaller aperture. When making
measurements that use small incident angles (<4°) we recommend that smaller divergence slits are used.
Divergence slits are available as accessories in the following sizes: 1/8°, 1/16° and 1/32° (see section 7.4.2.3.3).
The divergence slit should be installed in the slit holder nearest to the X-ray tube. The relationship between the
slit marking, the height of the beam emerging from the hybrid monochromator and the irradiated length is given
in Table 7.2.
NOTES: 1. We advise you to make a mark on the 1/2° slit that comes with the hybrid monochromator so that
you can identify it as the slit to be used with the hybrid monochromator. You should not use any
other 1/2° slit (other than the one you just marked) with the hybrid monochromator.
2. Although the slit marking reads 1/2º, the actual position of the slit with respect to the line focus of
the X-ray tube determines the acceptance angle of the hybrid monochromator to be 0.8º.

A copper attenuation foil (0.1 mm) and a combined copper (0.2 mm)/nickel (0.02 mm) attenuation foil are
supplied with the hybrid monochromators (see Figure 2.4).
Under typical operating conditions the beam from the hybrid monochromator can have an intensity which is
much greater than 1 000 000 cps. The Miniprop detector (PW3011/20) becomes non-linear in response above
1 000 000 cps and can be damaged by higher count rates.
For more details on detector maximum count rates see Chapter 21 in Part II of this User’s Guide.

hybrid monochromator housing in order to attenuate the beam
whenever the measured intensity is expected to exceed the
Their attenuation factors for copper radiation of the attenuation foils supplied are approximately:
copper (0.1 mm) ~ 100 times
combined copper/nickel ~ 18 000 times
The exact values for the attenuation factors for foils supplied with a hybrid monochromator are shown on the
attenuators themselves and on the Acceptance Test Form for the hybrid monochromator, which is supplied when
the module is delivered. These values can be entered in the data collector software and are used to automatically
The attenuation foil should be inserted into the slot for attenuation foil (see Figure 7.13).

You can use low angle fixed slits together with the hybrid monochromator in order to control the amount (length)
of the sample that is irradiated. PW3083/00 consists of three slits, marked: 1/8°, 1/16° and 1/32°. A 1/2° and a
1/4° slit are supplied with the hybrid monochromator. Table 7.2 shows the relationship between the various slits
and the amount of the sample irradiated.
The slit should be inserted into the divergence slit holder nearest to the X-ray tube (see also Figure 7.13).
Page 7.24 07.03.27

Table 7.2: Slit Marking and Irradiated Length
Height of Irradiated Length

Slit Marking
Beam (mm) (mm)
1
/2° 1.2 1.2
/sin(ω)
1
/4° 0.6 0.6
/sin(ω)
1
/8° 0.3 0.3
/sin(ω)
1
/16° 0.15 0.18
/sin(ω)
7.4.2.3.4 PW3086/20 Soller Slits Holder for Hybrid Monochromator
If you want to use Soller slits in combination with a hybrid monochromator in order to control the axial
divergence, you must mount a PW3086/20 Soller Slits Holder onto the PW3047/x0 Hybrid Monochromator.
The Soller slits holder is shown in Figure 7.14. The PW3086/20 includes a slot for the PW3085/x0 Soller Slits,
and an additional slot for the attenuation foils or beam masks.
Figure 7.14: PW3086/20 Soller Slits Holder for Hybrid Monochromator
The Soller slits holder can be mounted onto the hybrid monochromator by placing the holder in its location (see
Figure 7.13) and tightening the two screws into the indicated screw holes.
07.03.27 Page 7.25

Figure 7.15: PW3147/x0 Hybrid Monochromator with PW3086/20 Soller Slits Holder Mounted

If you have mounted the PW3086/20 Soller Slits Holder onto the hybrid monochromator you can use Soller slits
to control the axial divergence of the incident beam emerging from the hybrid monochromator.
The Soller slits are available in the following sizes:
For more information about Soller slits refer to Chapter 5 in Part II of this User’s Guide.

You can mount a PW3087/6x (with x = 0, 2 or 3) Automatic Beam Attenuator (see Figure 2.2) onto the
PW3047/x0 Hybrid Monochromator. This beam attenuator is used in place of the Cu attenuation foils described
in section 7.4.2.3.2. The attenuation factor is entered into the data collector software and is used to automatically
Page 7.26 07.03.27

Figure 7.16: PW3087/6x Automatic Beam Attenuator Mounted onto a

Hybrid Monochromator
7.4.2.3.6.1 Mounting Automatic Beam Attenuator onto a Hybrid Monochromator

1. Remove the three screws (marked A in Figure 2.2 in Chapter 2 in Part II of this User’s Guide).
3. Fit the metal part (NOT the side with the alignment pins) onto the brass end of the hybrid
monochromator; line it up with the slit of the automatic beam attenuator to the slit on the hybrid
monochromator and ensure that the four screw holes line up. Use the four short screws (M2 x 4)
supplied with the automatic beam attenuator and secure it into place.
7.4.2.3.7 PW3089/00 Beam Mask Set

If you have mounted the PW3086/20 Soller Slits Holder onto the hybrid monochromator you can use beam
masks to control the irradiated width of the sample. The following masks are supplied in the PW3089/00 Beam
Mask Set: 20, 10, 4 and 2. The beam mask must be inserted into the slot for beam masks in the Soller slits holder
(see Figure 7.15). For more information about beam masks, refer to Chapter 4 in Part II of this User’s Guide.
7.4.3 Hybrid Monochromators for X’Pert PRO MPD Systems

There are two types of hybrid monochromator for X’Pert PRO MPD systems, differing by the number of
reflections in the channel cut crystal.
• PW3149/63 Hybrid Monochromator 2X with two reflections in the channel cut crystal. This is described
in section 7.4.3.1.
• PW3150/63 Hybrid Monochromator 4X with four reflections in the channel cut crystal. This is described
in section 7.4.3.2.
07.03.27 Page 7.27


mirror and a two-crystal Ge(220) two-bounce monochromator. It is shown in Figure 7.17.
This monochromator provides monochromatic Cu Kα1 radiation. The acceptance angle from the line focus of
the X-ray tube is 0.8°. The Cu Kα2 radiation is suppressed to a level below 0.1%. The height of the X-ray beam
emerging from the hybrid monochromator is 1.2 mm. The axial divergence and width are not controlled by the
hybrid monochromator. A beam mask can be used to control the width; Soller slits are used to control the axial
divergence of the X-ray beam. A summary of the characteristic intensities and Full Widths at Half Maximum as
measured on the Si(111) reflection on the Si Single Crystal Reference Sample (part of PW3132/62) is given in
Table 7.5 and Table 7.6.
7.4.3.1.1 Hybrid Monochromator Housing

The hybrid monochromator housing is shown in Figure 7.17.
Figure 7.17: PW3149/63 Hybrid Monochromator 2X for X’Pert PRO MPD Systems
The module housing incorporates:
• a holder for an equatorial slit (a 1/2° slit is standard, smaller slits may be supplied for special
applications)
• a slot for an attenuation foil
• a housing to accommodate the Ge crystal.
Page 7.28 07.03.27

CAUTION
The slit holder and the crystal housing must never be removed.
7.4.3.1.2 Hybrid Monochromator Offset

In X’Pert PRO systems the beam emitted from the hybrid monochromator is offset relative to the direct beam
from the X-ray tube. This offset is referred to as the hybrid monochromator offset.
The offset of the beam coming out of the hybrid monochromator is approximately 3°. The exact value is given
in the Acceptance Test Form supplied with the hybrid monochromator. The zero positions of the omega and
2theta axes of the goniometer must be adjusted by the value of the hybrid monochromator offset in order to
compensate for it. The data collector software will always apply an offset whenever the hybrid monochromator
is present in the incident beam path (and not use it if the hybrid monochromator is not present in the system);
this offset is a default (calculated) value until you enter the exact offset value for your system as given in the
Acceptance Test Form. The method of measuring the offset is given in section 7.4.4.2.

mirror and a two-crystal Ge(220) four-bounce monochromator. This monochromator provides monochromatic
Cu Kα1 radiation. The acceptance angle from the line focus of the X-ray tube is 0.8°. The Cu Kα2 radiation is
suppressed to a level below 0.1%. The height of the X-ray beam emerging from the hybrid monochromator is
1.2 mm. The axial divergence and width are not controlled by the hybrid monochromator. A beam mask can be
used to control the width; Soller slits are used to control the axial divergence of the X-ray beam. A summary of
the characteristic intensities and Full Widths at Half Maximum as measured on the Si(111) reflection on the Si
Single Crystal Reference Sample (part of PW3132/62) is given in Table 7.5 and Table 7.6.
The physical appearance of the hybrid monochromator 4X is the same as that of the hybrid monochromator 2X
tube is referred to the hybrid monochromator offset. This offset is described in more detail in section 7.4.3.1.2.
07.03.27 Page 7.29

Figure 7.18: PW3150/63 Hybrid Monochromator 4X for X’Pert PRO MPD Systems
7.4.3.3 Accessories
The accessories that can be used together with hybrid monochromators fall into two groups:
Those that are delivered with the hybrid monochromator (1/2º and a 1/4º divergence slit, and
attenuation foils),
and
those that must be ordered separately (low angle fixed slits, an incident beam anti-scatter slit holder,
Soller slits, and automatic beam attenuators).

You can use a divergence slit together with a hybrid monochromator in order to control the height of the X-ray
beam coming off the hybrid monochromator and therewith the amount (length) of the sample that is irradiated.
A 1/2º and a 1/4º divergence slits are supplied with the PreFIX module. When the 1/2º slit is used, the X-ray
mirror inside the hybrid monochromator module is irradiated by the X-ray beam coming from the X-ray tube’s
focus over the complete length. The height of the X-ray beam emitted by the hybrid monochromator is 1.2 mm.
The beam height can be reduced by choosing a divergence slit with a smaller aperture. When making
measurements that use small incident angles (<4º) we recommend that smaller divergence slits are used.
Divergence slits are available as accessories in the following sizes: 1/8º, 1/16º and 1/32º (see section 7.4.3.3.3).
The divergence slit should be installed in the slit holder nearest to the X-ray tube. The relationship between the
slit marking, the height of the beam emerging from the hybrid monochromator and the irradiated length is given
in Table 7.3.
NOTE: We advise you to make a mark on the 1/2° slit that comes with the hybrid monochromator so that
you can identify it as the slit to be used with the hybrid monochromator. You should not use any
other 1/2° slit (other than the one you just marked) with the hybrid monochromator.
Although the slit marking reads 1/2º, the actual position of the slit with respect to the line focus of
the X-ray tube determines the acceptance angle of the hybrid monochromator to be 0.8º.
Page 7.30 07.03.27

7.4.3.3.2 Attenuation foils

A copper attenuation foil (0.1 mm) and a combined copper (0.2 mm)/nickel (0.02 mm) attenuation foil are
supplied with the hybrid monochromators (see Figure 2.4).
Under typical operating conditions the beam from the hybrid monochromator can have an intensity which is
much greater than 1 000 000 cps. The Miniprop detector (PW3011/20) becomes non-linear in response above
1 000 000 cps and can be damaged by higher count rates.
For more details on detector maximum count rates see Chapter 21 in Part II of this User’s Guide.

hybrid monochromator housing in order to attenuate the beam
Their attenuation factors for copper radiation of the attenuation foils supplied are approximately:
copper (0.1 mm) ~ 100 times
combined copper/nickel ~ 18 000 times
The exact values for the attenuation factors for foils supplied with a hybrid monochromator are shown on the
attenuators themselves and on the Acceptance Test Form for the hybrid monochromator, which is supplied when
the module is delivered. These values can be entered in the data collector software and are used to automatically
The attenuation foil should be inserted into the slot for attenuation foil (see Figure 7.17).

You can use low angle fixed slits together with the hybrid monochromator in order to control the amount (length)
of the sample that is irradiated. PW3083/00 consists of three slits, marked: 1/8°, 1/16° and 1/32°. A 1/2° and a
1/4° slit are supplied with the hybrid monochromator. Table 7.3 shows the relationship between the various slits
and the amount of the sample irradiated.
The slit should be inserted into the divergence slit holder nearest to the X-ray tube (see also Figure 7.17).
Table 7.3: Slit Marking and Irradiated Length
Height of Irradiated Length

Slit Marking
Beam (mm) (mm)
1/ ° 1.2 1.2/
2 sin(ω)
1
/4° 0.6 0.6/
sin(ω)
1
/8° 0.3 0.3
/sin(ω)
1
/16° 0.15 0.18
/sin(ω)
where ω is the angle between the incident beam and the sample surface.
7.4.3.3.4 PW3086/20 Soller Slits Holder for Hybrid Monochromator

If you want to use Soller slits in combination with a hybrid monochromator in order to control the axial
divergence, you must mount a PW3086/20 Soller Slits Holder onto the PW3047/x0 Hybrid Monochromator.
The Soller slits holder is shown in Figure 7.19. The PW3086/20 includes a slot for the PW3085/x0 Soller Slits,
and an additional slot for the attenuation foils or beam masks.
07.03.27 Page 7.31
Figure 7.19: PW3086/20 Soller Slits Holder for Hybrid Monochromator
The Soller slits holder can be mounted onto the hybrid monochromator by placing the holder in its location
(cross-ref to Figure 7.17) and tightening the two screws into the two screw holes marked “B”.
Figure 7.20: PW3149/63 Hybrid Monochromator with PW3086/20 Soller Slits Holder Mounted
Page 7.32 07.03.27

CAUTIONS 1. If you have a hybrid monochromator with Soller slits holder

mounted on your system be careful to avoid collisions between the
monochromator and the sample stage.
2. Normally the X’Pert PRO system automatically resets when it is

reset procedure involves driving the goniometer back to its
hardware zero points which may cause collisions between the
sample stage or sample and the monochromator. You should
disable this automatic reset using the data collector software if you
use a hybrid monochromator with Soller slits holder. You then have
the opportunity to remove the hybrid monochromator with Soller
slits holder before resetting the system.
7.4.3.3.5 PW3086/65 Incident Beam Anti-scatter Slit Holder

If you want to use a hybrid monochromator in a capillary spinner configuration you must use an anti-scatter slit.
In order to mount the slit you must first install the anti-scatter slit holder (PW3086/65). Refer to Chapter 20 in
Part II of this User’s Guide for more information about the selection of slit sizes in capillary spinner applications.
The PW3086/65 Anti-scatter Slit Holder includes a slot for Soller slits and a direct beam stop to protect the
detector from being exposed to the high intensity of the direct beam and to allow measurements from 3° 2θ
upwards in the capillary spinner configuration.
7.4.3.3.5.1 Mounting an Incident Beam Anti-scatter Slit Holder onto a Hybrid Monochromator
Mount the incident beam anti-scatter slit holder onto the hybrid monochromator as shown in Figure 7.21 by first
using the locating pins to position it correctly and then tightening the two screws shown in Figure 7.21.
CAUTION
Do NOT remove or loosen the two screws holding the metal
monochromator housing onto the mirror part of the hybrid
monochromator.
Alignment of the incident beam anti-scatter slit holder is described section 20.2.3.2 in Chapter 20 in Part II of
07.03.27 Page 7.33

Figure 7.21: PW3086/65 Incident Beam Anti-scatter Slit Holder mounted on a


If you have mounted the PW3086/20 Soller Slits Holder or the PW3086/65 Incident Beam Anti-scatter Slit
Holder onto the hybrid monochromator you can use Soller slits to control the axial divergence of the incident
beam emerging from the hybrid monochromator.
The Soller slits are available in different sizes as follows:
More information about Soller slits is given in Chapter 5 in Part II of this User’s Guide.

You can mount a PW3087/6x (with x = 0, 2 or 3) Automatic Beam Attenuator (see Figure 2.2) onto the
PW3149/63 Hybrid Monochromator 2X or the PW3150/63 Hybrid Monochromator 4X. This beam attenuator is
used in place of the Cu attenuation foils described in section 7.4.3.3.2. The attenuation factor is entered into the
data collector software and is used to automatically adjust the measured intensity values.
NOTES: a If the space between the hybrid monochromator and the sample stage on your system is too
small to mount an automatic beam attenuator, you might consider mounting the automatic
beam attenuator onto the diffracted beam PreFIX module used in your system. Refer to Table
2.3 in Chapter 2 in Part II of this User’s Guide to see which diffracted beam modules the
automatic beam attenuator can be mounted onto.
b If you use the automatic beam attenuator mounted onto the hybrid monochromator, use the
data collector software to check the safe ranges of the sample stage movements and of the
goniometer θ and 2θ angles.
Page 7.34 07.03.27
Figure 7.22: PW3087/6x Automatic Beam Attenuator mounted on a Hybrid Monochromator
CAUTION
If collisions between the automatic beam attenuator and the
sample stage are possible at low ω angles, you must use the data
collector software to disable the automatic reset option.
7.4.3.3.7.1 Mounting Automatic Beam Attenuator onto a Hybrid Monochromator

1. Remove the three screws (marked A in Figure 2.2 in Chapter 2 in Part II of this User’s Guide).
3. Fit the metal part (NOT the side with the alignment pins) onto the brass end of the hybrid
monochromator; line it up with the slit of the automatic beam attenuator to the slit on the hybrid
monochromator and ensure that the four screw holes line up. Use the four short screws (M2 x 4)
supplied with the automatic beam attenuator and secure it into place.
07.03.27 Page 7.35

7.4.4 Using the Hybrid Monochromator

If your X’Pert PRO diffraction system includes a hybrid monochromator you must use the PW3373/10 Special
XRD X’Pert Copper Tube (see Part II, Chapter 1, section 1.3.2).
The recommended high-tension generator settings for this X-ray tube are 45 kV and 40 mA.
7.4.4.2 Measuring the Offset value

The X-ray beam emerging from the hybrid monochromator is offset by certain angle. The exact value of this
angle is given in the Acceptance Test Form supplied with your hybrid monochromator.
If you need to check the offset value you do so as follows:
1. Install a non-offset incident beam PreFIX module (for example: a fixed divergence slit holder or a
5. Replace the incident beam PreFIX module used in step 1 with the hybrid monochromator. Do NOT
report this to the data collector software. Insert the combined copper/nickel attenuation foil into the
hybrid monochromator.
6. Make a 2θ scan to find the peak position of the direct X-ray beam from the hybrid monochromator.
Note this position as 2θB.
7. The hybrid monochromator offset is calculated by (2θB - 2θA).
are automatically offset when you select the hybrid monochromator as the incident beam PreFIX
module. This means, for example: if your calculation of the offset results in -1.1º you actually enter
1.1º, whereas if your calculation resulted in +1.1º you enter -1.1º.

To maintain the optimum intensity from the hybrid monochromator the output should be checked on the
following occasions:
• After rotating the X-ray tube to the line focus position.
• After replacing the X-ray tube.
• After repeatedly mounting and dismounting the hybrid monochromator module.
adjustment procedure is described in section .
7.4.4.3.1 Checking the Intensity from the Hybrid Monochromator

The intensity from the hybrid monochromator can be checked as follows:
Tube power : 45 kV, 40 mA
Divergence slit: 1/2° (in the holder for an equatorial (divergence) slit)
Attenuator : Combined copper/nickel attenuation foil (the attenuation factor is shown on the
attenuator)
2. Set ω = 0º, 2θ = 0º and make sure that the direct beam is not obstructed by the sample or sample stage.
Page 7.36 07.03.27
If there is no peak registered near 2θ = 0°, check that the offset value was properly introduced.
The absolute intensity values must meet the specifications listed in Table 7.4 and Table 7.5. The intensities are
calculated from the measured count rate using the attenuation factor of the combined copper/nickel attenuation
foil. The intensity data given in Table 7.4 are measured on an X’Pert PRO MRD system with a goniometer radius
of 320 mm. The intensity data given in Table 7.5 are measured on an X’Pert PRO MPD system with a
goniometer radius of 240 mm. If these intensity values are not met, refer to section 7.4.4.4.
Table 7.4: Summary of Absolute Intensities of the Direct Beam of a PW3147/x0 Hybrid Monochromator
for X’Pert PRO MRD Systems
PW3147/20 PW3147/00
Type Hybrid Hybrid
Diffracted Beam Optics
Number Monochromator Monochromator
4X 2X
PW3097/60 Rocking Curve Optics > 108 cps > 3.3 x 108 cps
or
PW3120/6x
PW3093/60 & Programmable Receiving Slit (3 mm) > 108 cps > 3.3 x 108 cps
PW3091/x0 and Programmable Anti-scatter Slit (4°)
(no Soller slits)
PW3015/x0 & X’Celerator (90º rotated, receiving slit > 2.5 x 107 cps > 1.1 x 108 cps
mode, maximum active length (9 mm))
PW3x94/30 and Fixed Anti-scatter Slit Holder (with
13 mm slit inserted), (no Soller slits)
PW3018/00 & PIXcel (receiving slit mode, maximum > 5.8 x 107 cps > 1.9 x 108 cps
active length (14 mm)) and
PW3490/00 Fixed Anti-scatter Slit Holder (no slit
PW3098/09 Parallel Plate Collimator, 0.09° (no > 2 x 107 cps > 1.9 x 107 cps
Soller slits)
Soller slits)
PW3098/27 Parallel Plate Collimator, 0.27° (no > 5 x 107 cps > 2 x 108 cps
Soller slits)
07.03.27 Page 7.37

Table 7.5: Summary of Absolute Intensities of the Direct Beam of a PW3149/63 and a
PW3150/63 Hybrid Monochromator for X’Pert PRO MPD Systems
PW3150/63 PW3149/63
Type Hybrid Hybrid
Diffracted Beam Optics
Number Monochromator Monochromator
4X 2X
PW3097/60 Rocking Curve Optics > 1.2 x 108 cps > 4 x 108 cps
PW3093/60 & Programmable Receiving Slit (3 mm) > 1.2 x 108 cps > 4 x 108 cps
PW3091/x0 and Programmable Anti-scatter Slit (4°)
(no Soller slits)
PW3015/x0 & X’Celerator (90º rotated) receiving slit > 5 x 107 cps > 1.5 x 108 cps
mode, maximum active length (9 mm)
and
PW3x94/30 Fixed Anti-scatter Slit Holder (no slit
PW3018/00 & PIXcel (receiving slit mode, maximum > 7 x 107 cps > 2.4 x 108 cps
active length (14 mm)) and
PW3490/00 Fixed Anti-scatter Slit Holder (no slit
Soller slits)
Soller slits)
Soller slits)
NOTES: 1. The direct beam intensities were determined with a new X-ray tube. The X-ray beam emitting from
a tube decreases in time.
2. After extensive use of hybrid monochromators the X-ray mirror and the germanium crystals will
show degraded surfaces. Therefore, extensively used hybrid monochromators may not completely
reach the specified intensities. If this is the case call your local PANalytical Service Engineer.
The Full Widths at Half Maximum are determined on the (111) reflection of the Silicon (111) Single Crystal
Reference Sample (part of PW3132/62). The FWHMs as measured on an X’Pert PRO MRD system (goniometer
radius 320 mm), or on an X’Pert PRO MPD system (goniometer radius 240 mm) equipped with a PW3069/00
Open Eulerian Cradle with PW3069/10 Z-translation Stage are given in Table 7.6.
Page 7.38 07.03.27

Table 7.6: Summary of FWHMs on Si(111) Reflection of the

PW3132/62 Si(111) Reference Sample
Hybrid Hybrid Hybrid Hybrid

Monochr. Monochr. Monochr. Monochr.
Type
Diffracted Beam Optics 2X 4X 2X 4X
Number
PW3147/00 PW3147/20 PW3149/63 PW3150/63
PW3097/60 Rocking Curve Optics

or PW3120/6x
PW3093/60 & Programmable Receiving Slit
(3 mm) and
PW3091/60 Programmable Anti-scatter Slit
(4º) (no Soller slits)
≤ 0.0068º ≤ 0.0052º ≤ 0.007º ≤ 0.006º
PW3015/x0 & X’Celerator (not rotated) (≤ 25”) (≤ 19”) (≤ 26”) (≤ 22”)
receiving slit mode, maximum
active length (9 mm) and
PW3x94/30 Fixed Anti-scatter Slit Holder (no
slit inserted)
PW3018/00 & PIXcel (receiving slit mode,

maximum active length
(14 mm)) and
PW3490/00 Fixed Anti-scatter Slit Holder (no
slit inserted)
07.03.27 Page 7.39

7.4.4.4 Tube Height Adjustment

There are three factors that can lead to reduced intensity:
• A change in the position of the tube focus relative to the hybrid monochromator.
• A reduction in the output intensity from the X-ray tube.
• A change in the hybrid monochromator alignment. (This is less probable).
During the life of an X-ray tube the focus position can change slightly and the output intensity slowly drop. When
a ceramic Cu X-ray tube is used with a hybrid monochromator the drop of intensity should be less than 15% per
1000 hours of use. If the output from the hybrid monochromator drops more than 15% per 1000 hours of use,
adjust the tube height to reposition the focus relative to the hybrid monochromator.
7.4.4.4.1 Tube Height Adjustment for Systems other than X’Pert PRO Extended MRD
This section describes the tube height adjustment procedures for X’Pert PRO diffraction systems other than
X’Pert PRO Extended MRD.
To adjust the height position of the X-ray tube relative to the hybrid monochromator, proceed as follows:
1. Mount the hybrid monochromator onto the incident beam PreFIX position. Place a 1/2° divergence slit
and a combined copper/nickel attenuation foil into the hybrid monochromator to protect the detector.
Make sure that the hybrid monochromator offset (see sections 7.4.2.1.2, 7.4.3.1.2 and 7.4.4.2) is
correctly introduced to the data collector software.
2. Mount one of the diffracted beam optics as summarized in Table 7.4 and Table 7.5. Use the settings
given in the tables.
stage.
knobs at the back of the X-ray tube housing (refer to Part II, Chapter 1 - Figure 1.9).
housing to move the X-ray tube (approximately 25 μm).
increase any further (if necessary you can make smaller steps, approximately 10 μm); then continue
with step 11. If the intensity is lower than that noted in step 7, continue with step 10.
knurled knobs at the back of the X-ray tube housing (refer to Part II, Chapter 1 - Figure 1.9).
housing to move the X-ray tube in the opposite direction (approximately 25 μm).
does not increase any further (if necessary you can make smaller steps, approximately 10 μm); then
Page 7.40 07.03.27

7.4.4.4.2 Tube Height Adjustment for X’Pert PRO Extended MRD Systems
This section describes the tube height adjustment procedures for X’Pert PRO Extended MRD systems.
To adjust the height position of the X-ray tube relative to the hybrid monochromator, proceed as follows:
1. Mount the X-ray tube on the standard tube position on the extended arm.
2. Mount the hybrid monochromator onto the incident beam PreFIX position. Place a 1/2° divergence slit
and a combined copper/nickel attenuation foil into the hybrid monochromator to protect the detector.
Make sure that the hybrid monochromator offset (see sections 7.4.2.1.2 and 7.4.4.2) is correctly
introduced to the data collector software.
3. Mount one of the diffracted beam optics as summarized in Table 7.4. Use the settings given in the table.
stage.
shield.
b. Turn the Allen key 45º counter-clockwise to move the X-ray tube (approximately 25 μm).
10. Check the intensity:
a. If the intensity is higher than that noted in step 8, continue repeating step 9 until the intensity does
not increase any further (if necessary you can make smaller steps, say: approximately 10 μm); then
b. If the intensity is lower than that noted in step 8, you must change the adjustment direction. Turn
the screw through a complete rotation clockwise (until the play is taken up) and then continue with
step 11.
c. If the intensity is unchanged from that noted in step 8, the play in the adjustment mechanism is in
effect. In this case turn the screw through a complete rotation counter-clockwise (until the play is
taken up) and then perform step 9 again.
a. Turn the Allen key 45º clockwise to move the X-ray tube in the opposite direction (approximately
25 μm).
b. Close the enclosure doors, open the shutter and note the intensity value.
c. If the intensity is higher than that noted in step 8, continue repeating this action until the intensity
does not increase any further (if necessary you can make smaller steps, say: approximately 10 μm);
12. The adjustment procedure is complete. Remove the Allen key.
07.03.27 Page 7.41

Page 7.42 07.03.27

Chapter 8
Incident Beam Collimators
Contents
8.1 General................................................................................................................................. 8 - 3
8.1.1 Applications............................................................................................................................ 8 - 3
8.1.1.1 Texture Analysis .................................................................................................... 8 - 3
8.1.1.2 Residual Stress Analysis ........................................................................................ 8 - 3
8.2 PW3084/60 Incident Beam Collimator ............................................................................. 8 - 4
8.2.1 Accessories............................................................................................................................. 8 - 5
8.2.1.1 Allen Key ............................................................................................................... 8 - 5
8.2.1.2 Beta-filters ............................................................................................................. 8 - 5
8.2.2 Use.......................................................................................................................................... 8 - 6
8.2.2.1 How to Mount the Cups......................................................................................... 8 - 6
8.2.2.2 Determination of the Irradiated Area..................................................................... 8 - 6
8.3 PW3084/62 Adjustable Crossed Slits Collimator ............................................................ 8 - 7
8.3.1 Accessories............................................................................................................................. 8 - 8
8.3.1.1 Beta-filters ............................................................................................................. 8 - 8
8.3.2 Use.......................................................................................................................................... 8 - 8
8.3.2.1 Setting the Aperture of the Crossed Slits Collimator ............................................ 8 - 8
8.3.2.2 Determination of the Irradiated Area..................................................................... 8 - 9
8.4 Crossed Slits Assemblies .................................................................................................... 8 - 9
8.4.1 PW3143/20 Crossed Slits Assembly ...................................................................................... 8 - 9
8.4.2 PW3144/60 Crossed Slits Assembly for X’Pert PRO MPD Systems.................................. 8 - 10
07.03.27 Page 8.1

Page 8.2 07.03.27

Part II - Chapter 8: Incident Beam Collimators
8.1 GENERAL
An incident beam collimator is a device that combines a divergence slit and a beam width mask in one optical
module. It is used in combination with the point focus of an X-ray tube.
The divergence slit part of the collimator is fitted in the incident beam path to control the equatorial divergence
of the incident beam emitted from the X-ray tube, this defines the amount (length) of the sample that is irradiated
by the incident X-ray beam.
The beam mask part of the collimator is fitted in the incident beam path to control the axial divergence of the
incident beam emitted from the X-ray tube, this defines the amount (width) of the sample that is irradiated by
the incident X-ray beam.
Two types of incident beam collimator are available on X’Pert PRO systems: one type for X’Pert PRO MPD
systems utilizes fixed slit and mask sizes, the other type for X’Pert PRO MRD systems utilizes crossed slits with
which the aperture can be continuously adjusted.
This chapter describes the collimator that is used with point focus applications. If your application uses line
focus the task of controlling beam divergence and dimensions is performed by divergence slits, beam masks and
Soller slits, they are described respectively in Chapter 3, Chapter 4 and Chapter 5 in Part II of this User’s Guide.
8.1.1 Applications
The main applications using incident beam collimators are texture and psi-stress analysis. In both applications
care has to be taken that the incident beam hits the sample (and not the sample holder) and that the defocusing
effects do not complicate the interpretation of the data. Correctly setting the slit and mask sizes is therefore of
great importance in both applications.
8.1.1.1 Texture Analysis

The incident beam collimators are used for quantitative texture analysis according to the Schulz reflection
method. In this type of measurement the sample is tilted around the psi axis in combination with a rotation
around the omega axis. The incident X-ray beam must be completely accepted by the sample at all ω and ψ
settings at all the 2θ angles where the pole figures are recorded. This requirement can be met by selecting the
correct collimator slit and mask sizes.
Defocusing effects will appear in the Schulz geometry at higher ψ tilts. Corrections for these defocusing effects
can be applied with the use of a ψ scan. This scan must be measured under the same experimental conditions as
the pole figures on a random (non-textured) sample of the same material as the textured sample.
8.1.1.2 Residual Stress Analysis

The incident beam collimators can also be used for residual stress analysis with ψ tilts (psi-stress measurements).
As is also the case in texture analysis, defocusing effects will appear in the diffraction pattern measured at the
higher ψ tilt angles. These effects will complicate accurate peak position determination. Defocusing effects can
be controlled by adjusting the slit size of the collimator.
07.03.27 Page 8.3

8.2 PW3084/60 INCIDENT BEAM COLLIMATOR

The PW3084/60 is an incident beam PreFIX module onto which two exchangeable collimator cups (one for
equatorial divergence and one for axial divergence) can be mounted. The incident beam collimator is shown in
Figure 8.1. Width mask cups of 2, 1, 0.5 and 0.25 mm and divergence cups of 4, 2 and 1 mm are included. This
PreFIX module is intended for use with X’Pert PRO MPD systems.
The PreFIX module incorporates an incident beam channel block, a collimator pipe and a slot for an attenuation
foil or a beta-filter. The incident beam channel block is equipped with a shutter lever which is used to close the
X-ray safety circuit when the incident beam collimator is fitted in the incident beam path.
The distance between the X-ray tube’s focus and the position of the collimator cups is 144 mm, if an extension
block is used this distance is 160 mm. This value is called the focus-collimator-distance and is used in defocusing
correction in quantitative texture analysis.
Shutter Attenuation Foil

Lever or β-filter
Incident Beam
Collimator Channel Block
Pipe
Width Mask
Cup
Locating Pin
Extension
Block
Divergence
Cup
Allen Key
Grooves for
Cup Alignment
PA000148
Figure 8.1: PW3084/60 Incident Beam Collimator
Page 8.4 07.03.27

8.2.1 Accessories
8.2.1.1 Allen Key
An Allen key is included with the PW3084/60 Incident Beam Collimator. This Allen key is used to (dis)mount
the divergence and width mask cups onto and from the collimator pipe. Mounting cups is described in section
8.2.2.1.
There are four beta-filters that can be used with the incident beam collimator, they are:
The filter must be installed (mounted) in the slit for attenuation foil or beta-filter as shown in Figure 8.1.

A 0.1 mm and a 0.2 mm copper foil are delivered with the X’Pert PRO X-ray diffraction system. These foils can
be inserted into the slot for attenuation foil or beta-filters as indicated in Figure 8.1.
can be damaged by higher count rates. Refer to Table 21.1 for more information about detectors used in X’Pert
PRO systems.

beta-filter slot on the collimator in order to attenuate the beam

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
The exact values of the attenuation factor for the foils supplied are shown on the Acceptance Test Form for the
system, which is supplied when the system is delivered and on the attenuator itself. This value can be entered in
the data collector software and is used to automatically adjust the measured intensity values. For more
information about the use of a copper attenuation foil refer to Chapter 2 in Part II of this User’s Guide.
07.03.27 Page 8.5

8.2.2 Use
This section provides information about mounting the collimator cups, how to determine the irradiated area on
the sample as a function of the sample position and the size of the incident beam.
8.2.2.1 How to Mount the Cups

Width mask cups of 2, 1, 0.5 and 0.25 mm and divergence cups of 4, 2 and 1 mm are included with the
PW3084/60 collimator. These cups must be mounted onto the texture pipe as follows:
1. First mount the width mask cup that you want to use (the width mask cups fit onto the texture pipe, the
divergence cups are too big). You mount the cup by sliding it onto the pipe, slotting it into the locating
pin so that the aperture is in the same axis as the X-ray tube (see Figure 8.1)
2. Tighten the Allen screw so that the mask cup stays in place.
3. Mount the divergence cup that you want to use onto the width mask cup that you just fitted. You mount
the cup by sliding it onto the mask cup, slotting it into the locating pin so that the slit is at 90º to the slit
on the mask cup.
4. Tighten the Allen screw so that the divergence cup stays in place.
NOTE: Although it is not normally necessary, the mask cups can be rotated through 90° and used as a
divergence cup, and the divergence cups can be rotated through 90° and used as a mask cup. For
example you could use the 0.25 mm beam mask as a divergence slit or the 4 mm divergence slit as
a beam mask.
8.2.2.2 Determination of the Irradiated Area

The size (length and width) of the area on the sample irradiated by the incident beam is dependent on the size of
the X-ray beam and the position of the sample with respect to the beam. The height and width of the beam can
be adjusted by mounting width masks and divergence slit cups onto the collimator pipe (see section 8.2.2.1).
The irradiated length and width as a function of the height and width of the X-ray beam as set by the collimator
cups, and of the sample position can be calculated as follows:
⎧ Rh + p h ( R – f ) ⎫
- ⎬ + W sin ψ cot ω
L = ⎨ ----------------------------------
⎩ f sin ω ⎭
h = the height of the incident X-ray beam, as set by the divergence slit cup,
ph = the height of the point focus of the X-ray tube, usually 1.2 mm,
f = the distance from the focus of the X-ray tube to the collimator cups,
ψ = the tilt angle, which is the angle between the sample surface normal and the
equatorial plane,
ω = the angle between the incident beam and the sample surface.
Rw + p w ( R – f )
W = -------------------------------------
f cos ψ
where W = the irradiated width on the sample,
pw = the width of the point focus of the X-ray tube, usually 0.4 mm,
w = the width of the incident X-ray beam, as set by the width mask cup,
f = the distance from the focus of the X-ray tube to the collimator cups,
equatorial plane.
Page 8.6 07.03.27

8.3 PW3084/62 ADJUSTABLE CROSSED SLITS COLLIMATOR

The PW3084/62 is an incident beam PreFIX module consisting of a collimator pipe with a crossed slits
assembly.
The crossed slits assembly consists of two manually adjustable orthogonal slits with a maximum size of 10 mm
to define both axial and equatorial divergence of the X-ray beam emitted by the point focus of the X-ray tube.
The crossed slit collimator acts like a divergence slit and an incident beam mask at the same time. It can be used
in texture or psi-stress applications.
The distance between the X-ray tube’s focus and the position of the crossed slits is 150 mm, this value is used
in defocusing correction in quantitative texture analysis.
The crossed slits collimator is shown in Figure 8.2.
Shutter
Lever
Adjustment Knob Attenuation Foil
Equatorial for Beam Width or Beta-filter
Divergence Slit
Scale
Crossed Slits
Assembly
Adjustment Knob
for Beam Height
Axial Width
Mask Scale
Figure 8.2: PW3084/62 Crossed Slits Collimator

The housing incorporates:
• a slot for attenuation foil or beta-filter
• a crossed slits assembly (see section 8.4).
The slits can be manually adjusted (the scales are marked 0.02 mm divisions). The adjustment accuracy is
± 0.02 mm.
07.03.27 Page 8.7

8.3.1 Accessories
There are four beta-filters that can be used with the crossed slits collimator, they are:
The filter must be installed (mounted) in the slit for attenuator foil or beta-filter as shown in Figure 8.2.

A 0.1 mm and a 0.2 mm copper foil are delivered with the X’Pert PRO X-ray diffraction system. These foils can
be inserted into the slot for attenuation foil or beta-filters as indicated in Figure 8.2.
can be damaged by higher count rates. Refer to Chapter 21 in Part II of this User’s Guide for more information
about detectors used in X’Pert PRO systems.

beta-filter slot in the crossed slits collimator in order to attenuate
the beam whenever the measured intensity is expected to exceed
the maximum count rate of the detector used.

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
The exact values of the attenuation factor for the foils supplied with the system are shown on the Acceptance
Test Form for the system, which is supplied when the system is delivered and on the attenuation foil itself. This
value can be entered in the data collector software and is used to automatically adjust the measured intensity
values. For more information about the use of a copper attenuation foil refer to Chapter 2 in Part II of this User’s
Guide.
8.3.2 Use
This section provides information about setting the aperture of the crossed slits assembly and how to determine
the irradiated area on the sample as a function of the sample position and the size of the incident beam.
8.3.2.1 Setting the Aperture of the Crossed Slits Collimator

The aperture on the crossed slits collimator is adjustable by means of two knobs (one vertical and one horizontal)
to allow a gap of between 0 and 10 mm to be set. The knob scales are graduated in steps of 0.02 mm. The knob
nearest the X-ray tube controls the width of the irradiation and the knob furthest away from the tube controls the
irradiated length.
Page 8.8 07.03.27

8.3.2.2 Determination of the Irradiated Area

the X-ray beam and the position of the sample with respect to the beam. The height and width of the beam can
be adjusted by turning the adjusting knobs on the crossed slits assembly.
The irradiated length and width as a function of the height and width of the X-ray beam as set by the crossed
slits assembly, and of the sample position can be calculated as follows:
⎧ Rh + p h ( R – f ) ⎫
L = ⎨ ----------------------------------- ⎬ + W sin ψ cot ω
⎩ f sin ω ⎭
h = the height of the incident X-ray beam, as set by the divergence slit on the crossed
slits assembly,
ph = the height of the point focus of the X-ray tube, usually 1.2 mm,
f = the distance from the focus of the X-ray tube to the crossed slits,
equatorial plane,
ω = the angle between the incident beam and the sample surface.
Rw + p w ( R – f )
W = -------------------------------------
f cos ψ
pw = the width of the point focus of the X-ray tube, usually 0.4 mm,
w = the width of the incident X-ray beam, as set by the axial mask on the crossed slits
assembly,
equatorial plane.
8.4 CROSSED SLITS ASSEMBLIES

8.4.1 PW3143/20 Crossed Slits Assembly
The PW3143/20 Crossed Slits Assembly is a device to control how much of the sample is irradiated (both length
and width) by the beam emitting from the incident beam PreFIX module onto which it is mounted. It is
standardly fitted on the PW3146/60 X-ray Lens, it can be fitted as an accessory on the high-resolution
monochromators (PW3110/6x) used with X’Pert PRO MRD systems.
Please refer to section 9.2.1 in Chapter 9 of Part II of this User’s Guide (if it is mounted on an X-ray lens) or
section 7.2.7.1 in Chapter 7 in Part II of this User’s Guide (if it is mounted on a high-resolution monochromator)
for information about how to use this device to adjust the irradiated area.
07.03.27 Page 8.9

Figure 8.3: PW3143/20 Crossed Slits Assembly
8.4.2 PW3144/60 Crossed Slits Assembly for X’Pert PRO MPD Systems
The PW3144/60 Crossed Slits Assembly is an optical device for use with a PW3110/61 or a PW3110/62 High-
resolution Monochromator on an X’Pert PRO MPD system. It controls the area on the sample (both length and
width) that is irradiated by the beam emerging from the high-resolution monochromator.
The slit and mask apertures can be set in seven different sizes: 5.00 mm, 4.00 mm, 3.00 mm, 2.00 mm, 1.00 mm,
0.75 mm, 0.50 mm and 0.25 mm. The accuracy of the openings is ± 0.05 mm. Any combination of slit and mask
size is possible.
For more information about the use of this crossed slits assembly on a high-resolution monochromator, refer to
sections 7.2.7.2 and 7.2.8.1 in Chapter 7 in Part II of this User’s Guide.
Figure 8.4: PW3144/60 Crossed Slits Assembly Mounted onto a

High-resolution Monochromator
Page 8.10 07.03.27

Chapter 9
X-ray Lenses
Contents
9.1 General................................................................................................................................. 9 - 3
9.1.1 Applications............................................................................................................................ 9 - 4
9.1.1.1 Texture Analysis .................................................................................................... 9 - 4
9.1.1.2 Residual Stress Analysis ........................................................................................ 9 - 4
9.1.1.3 Phase Analysis on Irregularly Shaped Surfaces .................................................... 9 - 4
9.1.1.4 In-plane Diffraction ............................................................................................... 9 - 4
9.2 PW3146/60 X-ray Lens....................................................................................................... 9 - 5
9.2.1 Crossed Slits Assembly .......................................................................................................... 9 - 5
9.3 Accessories ........................................................................................................................... 9 - 6
9.3.1 Beta-filters .............................................................................................................................. 9 - 6
9.3.2 Attenuation Foil...................................................................................................................... 9 - 6
9.3.3 9430 920 03571 Mylar Foil.................................................................................................... 9 - 6
9.4 Use ........................................................................................................................................ 9 - 7
9.4.1 Determination of the Irradiated Area ..................................................................................... 9 - 7
07.03.27 Page 9.1

Page 9.2 07.03.27

Part II - Chapter 9: X-ray Lenses
9.1 GENERAL
The X-ray lens (or poly-capillary optics) consists of a few million glass capillaries (with an approximate
diameter of 5 µm) formed together with a round cross-section and bent in a parabolic shape. X-rays are
transported through these very narrow glass capillaries using the effect of total external reflection inside the
capillary. The principle is shown in Figure 9.1.
Glass capillary
X-ray beam
Figure 9.1: Total Reflection Inside Glass Capillary
The capillaries act in effect as a waveguide, and this together with the curvature of the capillaries results in the
diverging X-ray beam being turned into a quasi-parallel beam. It is designed with a circular cross-section in
order to be used with the point focus of the X-ray tube. A schematic view of the lens is shown in Figure 9.2.
Quasi-parallel
beam
Point
focus
Divergent
Front view X-ray lens beam
Figure 9.2: Schematic View of the X-ray Lens

The X-ray lens collimates a divergent beam into a quasi-parallel beam in two dimensions (equatorial and axial).
This is in contrast to the X-ray mirror which is used with the line focus of the X-ray tube to collimate the
divergent beam into a quasi-parallel beam in one dimension (equatorial).
Photons, with an energy of more than 10 keV (wavelengths shorter than 1.2 Å (0.12 nm)) pass through the
curved capillaries less efficiently. Because of this, the X-ray lens not only collimates the X-ray beam but also
has a low pass energy filtering effect on the beam - white radiation will be suppressed strongly by the lens. The
X-ray lens is optimized for use with Cu Kα radiation, but it can also be used for other types of radiation with an
energy less than 10 keV, such as Cr, Fe and Co Kα radiation. The transmission for Cu Kα radiation is
approximately 25%. The X-ray lens is not intended for use together with a molybdenum tube.
Because of the suppression of white radiation by the X-ray lens, a diffracted beam monochromator is only
needed with lens measurements to reduce the background intensity if the incident beam invokes fluorescence
radiation from the sample or to eliminate Kβ radiation. Alternatively you can use a beta-filter to suppress the Kβ
radiation emitted by the X-ray tube.
When the X-ray lens is used together with the appropriate parallel beam optics on the diffracted beam side the
measurements are not sensitive to the exact height position of the sample, or to sample tilt. This geometry is also
suitable for irregularly shaped samples.
07.03.27 Page 9.3

9.1.1 Applications
The quasi-parallel beam in two dimensions means that the system is not sensitive to sample shift or tilt in the psi
or omega axes; this is particularly useful in:
• Stress measurement
• Texture measurement
Because the X-ray lens acts as a low pass energy filter (suppresses the white noise background) you only need
to use the flat graphite monochromator if there is strong fluorescence from the sample, or to eliminate Kβ
radiation. Kβ radiation can also be reduced using a beta-filter.
9.1.1.1 Texture Analysis

The X-ray lens can be used for quantitative texture analysis in the reflection geometry on solid samples. In this
type of measurement the sample is tilted around the psi axis in combination with a rotation around the phi axis.
The parallel beam geometry makes the measurements insensitive to sample tilt around the psi axis. Defocusing
effects, as appear in texture measurements using standard texture optics, especially at high ψ tilts, are virtually
non-existent in measurements with the X-ray lens. The suppression of white radiation considerably reduces the
influence of background intensities on texture measurements.
9.1.1.2 Residual Stress Analysis

The X-ray lens can be used for residual stress analysis with ψ tilts or ω tilts. The parallel-beam geometry makes
the measurements insensitive to both sample tilt and sample height misalignment. Therefore, no defocusing
effects occur in the measurements at the various tilt angles, used to evaluate the residual stress according to, for
example: the sin2ψ method. The absence of defocusing, combined with the low background intensities as a result
of the suppression of white radiation by the X-ray lens, makes an accurate determination of the peak position
possible. The parallel beam geometry is also suited for samples with rough surfaces or irregularly shaped
samples.
9.1.1.3 Phase Analysis on Irregularly Shaped Surfaces

The X-ray lens can be applied for phase analysis of poly crystalline samples where a moderate resolution
(approximately 0.4º) is required. A parallel plate collimator is used at the diffracted beam side. The parallel beam
geometry ensures that the measured peak positions are insensitive to sample shift and sample roughness.
Therefore the use of the X-ray lens is especially suited for samples with rough surfaces.
9.1.1.4 In-plane Diffraction

The X-ray lens can be used as incident beam module in in-plane diffraction measurements on specially equipped
X’Pert PRO MRD systems. In these measurements the lattice spacings between the crystal planes perpendicular
to the sample surface are measured.
The incident X-ray beam hits the (flat) sample surface at very low angles (~ 1º); this means that a beam with low
divergence and very small height and width is required. A parallel plate collimator is used at the diffracted beam
side.
Using the X’Pert PRO MRD system for in-plane diffraction is described in section 11.2.2.4 of Chapter 11 in Part
Page 9.4 07.03.27

9.2 PW3146/60 X-RAY LENS

The PW3146/60 X-ray lens is an incident beam PreFIX module designed for use with X’Pert PRO
configurations. The X-ray lens is shown in Figure 9.3.
The acceptance angle of the X-ray beam from the point focus of an X-ray tube is approximately 3.5°. The
equatorial and axial divergence of the quasi-parallel X-ray beam emerging from the X-ray lens is determined by
the critical angle for total external reflection of the glass and by the radiation used. For Cu Kα radiation this angle
has a typical value of approximately 0.3°.
The effective beam diameter is 7 mm. The height and width of the X-ray beam can be controlled by using a
crossed slits assembly mounted at the exit of the X-ray lens.
The distance between the X-ray’s tube’s focus and the crossed slits is 145 mm.
The housing incorporates:
• a slot for attenuation foil or beta-filter.
Figure 9.3: PW3146/60 X-ray Lens

The beam entrance on the housing is covered by a mylar foil.
9.2.1 Crossed Slits Assembly

The crossed slits assembly is mounted on the X-ray lens to control the area of the sample that is irradiated (both
length and width) by the beam emitted by the X-ray lens. The slit openings can be continuously varied between
0 mm and 10 mm. The knobs are graduated in 0.02 mm steps.
This assembly is factory aligned and therefore should not be removed.
07.03.27 Page 9.5

9.3 ACCESSORIES
9.3.1 Beta-filters
There are three beta-filters that can be used with the X-ray lens, they are:
Ni filter (PW3151/03)for Cu Kα radiation
The filter must be installed (mounted) in the slot for attenuation foil or beta-filter as shown in Figure 9.3. For
more information about the use of a beta-filter refer to Chapter 2 (section 2.3) in Part II of this User’s Guide.
9.3.2 Attenuation Foil

inserted into the slot for attenuation foil or beta-filters as indicated in Figure 9.3.
can be damaged by higher count rates. For more information about maximum count rates for the detectors used
in X’Pert PRO refer to Part II - Chapter 21.

beta-filter slot in the lens housing in order to attenuate the beam
maximum count rate of the detector being used.

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
The exact values of the attenuation factor for the foils supplied with the system are shown on the Acceptance
Test Form which is supplied when the system is delivered, and on the attenuator itself. This value can be entered
in the data collector software and is used to automatically adjust the measured intensity values. For more
9.3.3 9430 920 03571 Mylar Foil

The entrance of the X-ray lens module is covered by a removable mylar foil (6 μm thick). This mylar foil protects
the X-ray lens from dust and moisture. It can be replaced with a new one if necessary.
Type number 9430 920 03571 consists of a set of five mylar foils.
Page 9.6 07.03.27

9.4 USE
This section describes the determination of the irradiated area on the sample as a function of the sample position
and the size of the incident beam.
9.4.1 Determination of the Irradiated Area

the X-ray beam and on the position of the sample with respect to the incident beam.
The effective beam diameter emitted by the X-ray lens is 7 mm. This size can be reduced by using a crossed slits
assembly mounted at the exit of the PreFIX module.
The aperture on the crossed slits collimator is adjustable by means of two knobs (one vertical and one horizontal)
to allow an aperture of between 0 and 10 mm to be set. The knob scales are graduated in steps of 0.02 mm. The
knob nearest the X-ray tube controls the width of the irradiated area and the knob furthest away from the tube
controls the irradiated length.
The irradiated length and width as a function of the height and width of the X-ray beam as set by the crossed
slits, and of the sample position can be calculated as follows:
h + δ(R – f)
L = ---------------------------- + W sin ψ cot ω
sin ω
h = the height of the incident X-ray beam, as set by the divergence slit on the crossed
slits assembly,
W = the irradiated width on the sample (see below),
equatorial plane,
ω = the angle between the incident beam and the sample surface,
δ = the divergence of the of the X-ray beam emerging from the X-ray lens (in radians).
w + δ( R – f)
W = -----------------------------
cos ψ
w = the width of the incident X-ray beam, as set by the axial mask on the crossed slits
assembly,
equatorial plane,
δ = the divergence of the of the X-ray beam emerging from the X-ray lens (in radians).
Please note that since the effective diameter of the X-ray lens is 7 mm, the maximum values to be entered for h
and w in the formulas given above are also 7 mm.
07.03.27 Page 9.7

Page 9.8 07.03.27

Chapter 10
Mono-capillaries
Contents
10.1 General............................................................................................................................... 10 - 3
10.1.1 Applications.......................................................................................................................... 10 - 3
10.2 The PreFIX Mono-capillary Module .............................................................................. 10 - 4
10.2.1 PW3145/00 PreFIX Mono-capillary Holder ........................................................................ 10 - 4
10.2.2 Cylindrical Mono-capillary Collimator................................................................................ 10 - 4
10.2.2.1 9430 500 20291 Collimator Tube 230 mm x 0.1 mm ......................................... 10 - 4
10.3 Accessories ......................................................................................................................... 10 - 5
10.3.1 Beta-filters ............................................................................................................................ 10 - 5
10.3.2 Attenuation Foil.................................................................................................................... 10 - 5
10.3.3 9430 500 28341 Alignment Microscope .............................................................................. 10 - 6
10.4 Use ...................................................................................................................................... 10 - 7
10.4.1 Alignment of a Sample for Micro-diffraction Using the Alignment Microscope................ 10 - 7
10.4.2 Determination of the Size of the Irradiated Spot.................................................................. 10 - 8
07.03.27 Page 10.1

Page 10.2 07.03.27

Part II - Chapter 10: Mono-capillaries
10.1 GENERAL
The mono-capillary is a hollow glass tube. X-rays are transported through this tube using the effect of total
external reflection inside the capillary. The principle is shown in Figure 10.1. The diameter of the X-ray beam
at the end of a mono-capillary ranges from 10 μm to 2 mm.
Mono (glass) Capillary Point

Focus
Divergent
Beam
Figure 10.1: Total Reflection Inside Glass Capillary

The tube acts in effect as a wave guide which results in the diverging X-ray beam being turned into a narrow
quasi-parallel beam. It is designed to be used with the point focus of the X-ray tube. Photons, with an energy of
more than 10 keV (wavelengths shorter than 1.2 Å (0.12 nm)) pass through the mono-capillary less efficiently.
Because of this, the mono-capillary not only collimates the X-ray beam but also has a low pass energy filtering
effect on the beam - white radiation will be suppressed strongly by the mono-capillary. Mono-capillaries are
optimized for Cu Kα radiation, they can also be used for other types of radiation with an energy less than 10
keV, such as Cr, Fe and Co Kα radiation. Mono-capillaries are not intended for use with Mo Kα radiation.
Because the mono-capillary acts as a low pass energy filter (suppresses the white noise background) you only
need to use a diffracted beam monochromator if there is strong fluorescence from the sample or to reduce Kβ
radiation. Alternatively, you can use a beta-filter to suppress the Kβ radiation emitted by the X-ray tube.
10.1.1 Applications
The main application of the mono-capillary is X-ray diffraction analysis of small spots on a sample. Because of
the efficient collimation of the X-ray beam, a very small area of the sample is irradiated. The diameter of the
irradiated area is dependent on the inner diameter of the mono-capillary and the distance between the exit of the
mono-capillary and the center of the goniometer.
Analysis of small spots on a sample is useful if you have a sample with an inhomogeneous composition, or if
your sample has a laterally inhomogeneous distribution of residual stresses and/or texture.
07.03.27 Page 10.3

10.2 THE PREFIX MONO-CAPILLARY MODULE

The mono-capillary is an incident beam PreFIX module, consisting of two parts: the mono-capillary collimator
tube and a holder for the mono-capillary to mount it on the incident beam PreFIX position on the goniometer.
10.2.1 PW3145/00 PreFIX Mono-capillary Holder

The incident beam PreFIX module mono-capillary holder with the mono-capillary collimator tube mounted is
Figure 10.2: PW3145/00 PreFIX Mono-capillary Holder with Mono-capillary Mounted

The module incorporates:
• a slot for attenuation foil or beta-filter
• a receptacle for the tube.
10.2.2 Cylindrical Mono-capillary Collimator

There are three mono-capillary collimator tubes available (see sections 10.2.2.1, 10.2.2.2 and 10.2.2.3), other
sizes (internal diameter and length) can be ordered on special request.
The acceptance angle of the X-ray beam from the point focus of the X-ray tube on the mono-capillary and the
equatorial and axial divergence of the quasi-parallel X-ray beam emerging from the mono-capillary are
determined by the critical angle for total reflection of the glass, and therefore, by the radiation used. For Cu Kα
radiation this angle has a typical value of 0.3°.
10.2.2.1 9430 500 20291 Collimator Tube 230 mm x 0.1 mm

The cylindrical mono-capillary collimator tube (wave guide) is a glass tube 230 mm long with an exit beam
diameter of 0.1 mm. The external tube diameter is 10 mm, the tube fits into the PW3145/00 Mono-capillary
Holder. This mono-capillary is intended for use with X’Pert PRO MRD systems with a goniometer radius of 320
mm. The distance from the X-ray tube’s focus to the end of the collimator tube f (see section 10.4.2) is 297 mm.
Page 10.4 07.03.27


Holder. This mono-capillary can be used on all X’Pert PRO systems with a goniometer radius of 210 mm and
larger, depending on the sample stage used. The distance from the X-ray tube’s focus to the end of the collimator
tube f (see section 10.4.2) is 202 mm.

Holder. This mono-capillary is intended for use with X’Pert PRO MPD systems with a goniometer radius of 240
mm. The distance from the X-ray tube’s focus to the end of the collimator tube f (see section 10.4.2) is 232 mm.
CAUTIONS 1. If you have a mono-capillary mounted on your system be careful to

avoid collisions between the collimator tube and the sample stage.
2. Normally the X’Pert PRO system automatically resets when it is

switched on or when power is restored after a power failure.
The reset procedure involves driving the goniometer back to its
hardware zero points which may cause collisions between the
sample stage or sample and the collimator tube. You should
disable this automatic reset using the data collector software if
you use a mono-capillary. This activates an initialization wizard
which guides through the initialization procedure. You then have
the opportunity to remove the mono-capillary before resetting the
system.
10.3 ACCESSORIES
10.3.1 Beta-filters
There are three beta-filters that can be used with the mono-capillary, they are:
The filter must be installed (mounted) in the slot for attenuation foil or beta-filter as shown in Figure 10.2. For
more information about the use of beta-filters, refer to Part II - Chapter 2.
10.3.2 Attenuation Foil

A 0.1 mm and a 0.2 mm copper foil are delivered with the X’Pert PRO system. These foils can be inserted into
the slot for attenuation foil or beta-filters as indicated in Figure 10.2.
can be damaged by higher count rates. For more information about the detectors used in X’Pert PRO, refer to
Part II - Chapter 21, Table 21.1.
07.03.27 Page 10.5

CAUTION An attenuation foil MUST be mounted in the attenuation foil or beta-

filter slot in the lens housing in order to attenuate the beam whenever
the measured intensity is expected to exceed the maximum count rate

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
The exact values of the attenuation factor for the foils supplied are shown on the Acceptance Test Form for the
mono-capillary, which is supplied when the module is delivered and on the attenuation foil itself. This value can
be entered in the data collector software and is used to automatically adjust the measured intensity values.
10.3.3 9430 500 28341 Alignment Microscope

The spot on the sample that is to be irradiated by the incident X-ray beam can be determined with the use of an
alignment microscope which is shown in Figure 10.3. The alignment microscope (9430 500 28341) is attached
to a PW3019/10 PreFIX Microscope Interface which can be mounted on the diffracted beam PreFIX position on
the PW3050/6x X’Pert PRO Goniometer (with a radius of 200 mm or more). The alignment microscope has a
cross-hair with a division of 50 μm. The viewing diameter is 6 mm.
How to use the alignment microscope is described in 10.4.1.
Figure 10.3: 9430 500 28341 Alignment Microscope with PW3019/10 PreFIX Microscope Interface
Page 10.6 07.03.27

10.4 USE
This section describes using the alignment microscope to position the spot to be analyzed and the determination
of the size of the irradiated spot on the sample.
10.4.1 Alignment of a Sample for Micro-diffraction Using the

Alignment Microscope
You can align a micro-diffraction sample as follows:
1. Mount the prepared sample on the sample stage.
2. Mount the sample stage onto the X’Pert PRO diffractometer.
3. Mount the mono-capillary onto the incident beam PreFIX position, check that no collisions can occur
between the sample, the sample stage and the mono-capillary.
4. Mount the alignment microscope on the diffracted beam PreFIX position. Make sure that the
alignment microscope does not touch the other diffracted beam PreFIX module when mounted (only
applicable when two diffracted beam PreFIX positions are available).
5. Move the goniometer using the data collector software to such a position that you can observe the
sample from the side in order to check the correct height and tilt (for a Theta-Theta system: 2θ = 0º,
offset = 0º; for an Omega-2Theta system: 2θ = 96º, offset = 48º; for an Alpha-1 system: 2θ = 120º,
offset = 60º; for an MRD system: 2θ = 90º, offset = 45º). You should now be able to look through the
microscope when standing in front of the enclosure.
6. Look through the microscope and focus onto the edge of the sample. Using a sheet of white paper to
reflect the light, or using a light directed onto the sample helps to enhance the contrast.
7. You can now start to align the sample:
a. Rotate the sample stage in such a way that the tilt axis is parallel to the microscope's optical axis.
b. Adjust the tilt until the sample surface is lined up with the cross-hair of the ocular of the
microscope.
c. Check the correct alignment by rotating the sample around the axis normal to the surface back
and forth over 180º and comparing the position of the sample surface. If the two situations do
not correspond, it may well be that the cross-hair of the microscope is not correctly oriented.
8. Repeat the previous step with the sample rotated 90º on its normal axis with respect to the situation in
step 7.
9. Rotate the sample over 360º around its normal axis and check the sample to see if it wobbles at all. If
it does wobble, repeat steps 7 and 8.
10. Adjust the height of the sample until its edge matches the cross-hair of the microscope.
11. Move the goniometer (using the data collector software) to such a position that you can observe the
sample from the top in order to find the position on the sample that you want to analyze (for a Theta-
Theta system: 2θ = 90º, offset = -45º; for an Omega-2Theta system: 2θ = 96º, offset = -42º; for an
Alpha-1 system: 2θ = 120º, offset = -30º; for an MRD system: 2θ = 90º, offset = -45º). Align the
sample using the translational movements of the sample stage. The center of the area that will be
measured corresponds to the cross-hair of the microscope.
12. Replace the alignment microscope with the diffracted beam PreFIX module that you want to use for
the X-ray experiment. You are now ready to start collecting data!
07.03.27 Page 10.7

CAUTION The end of the mono-capillary is close to the sample. As a result of this,
there is a chance for a collision between the sample or sample stage
and the mono-capillary. Before collecting data, make sure that there is
no chance for such a collision at any diffractometer setting that is used
in your program(s). Also disable the automatic reset of the instrument
in the data collector software. This activates an initialization wizard
which guides through the initialization procedure. You then have the
opportunity to remove the mono-capillary before resetting the
system.
10.4.2 Determination of the Size of the Irradiated Spot

The maximum size (length and width) of the spot on the sample that is irradiated by the incident beam is not only
dependent on the diameter of the mono-capillary collimator, but also on geometric factors such as: the angle at
which the incident beam hits the sample surface, the tilt (ψ) angle, and the distance between the end of the mono-
capillary tube and the center of the goniometer. A good approximation, sufficiently accurate for general purposes
can be calculated using the following formulas:
d + δ( R – f)
L = ---------------------------- + W sin ψ cot ω
sin ω
in which:
L = the irradiated length on the sample,
d = the exit beam diameter of the mono-capillary collimator,
f = the distance from the focus of the X-ray tube to the end of the mono-capillary
collimator tube,
W = the irradiated width on the sample,
ω = the angle between the incident beam and the sample surface,
δ = the divergence of the quasi-parallel X-ray beam emerging from the mono-capillary in
radians,
ψ = the tilt angle, which is the angle between the sample surface normal and the equatorial
plane.
d + δ(R – f)
W = ----------------------------
cos ψ
in which:
W = the irradiated width on the sample,
d = the exit diameter of the mono-capillary collimator,
f = the distance from the focus of the X-ray tube to the end of the mono-capillary
collimator tube,
δ = the divergence of the quasi-parallel X-ray beam emerging from the mono-capillary in
radians,
ψ = the tilt angle, which is the angle between the sample surface normal and the equatorial
plane.
Page 10.8 07.03.27

Chapter 11
MRD Cradle
Contents
11.1 General................................................................................................................................. 11 - 3
11.2 PW3060/20 All-purpose MRD Cradle .............................................................................. 11 - 3
11.2.1 Accessories ............................................................................................................................. 11 - 6
11.2.1.1 Dial Gauge .............................................................................................................. 11 - 7
11.2.1.2 Alignment Shaft for X’Pert PRO MRD Systems ................................................... 11 - 7
11.2.1.3 9430 920 04651 Option for In-plane Diffraction.................................................... 11 - 8
11.2.1.4 0.2 mm Mask for In-plane Diffraction.................................................................. 11 - 10
11.2.1.5 PW3061/21 Sample Holder for Solid Samples..................................................... 11 - 11
11.2.1.6 PW3061/22 4 Inch Wafer Holder ......................................................................... 11 - 12
11.2.1.7 PW3061/2x 6 & 8 Inch Wafer Holders................................................................. 11 - 12
11.2.1.8 PW3061/25 Adjustable “De Wolff’s” Knife ........................................................ 11 - 14
11.2.1.9 9430 500 20351 Magnetic Ring............................................................................ 11 - 14
11.2.1.10 9430 500 20361 Sample Platform......................................................................... 11 - 14
11.2.1.11 9430 500 20491 Domed Hot Stage DHS 900 ....................................................... 11 - 14
11.2.2 Use ........................................................................................................................................ 11 - 22
11.2.2.1 Mechanically Aligning the Sample....................................................................... 11 - 22
11.2.2.2 Aligning the Sample Using X-rays ....................................................................... 11 - 23
11.2.2.3 Use of the MRD Cradle with more than one Sample ........................................... 11 - 24
11.2.2.4 Using the X’Pert PRO MRD System for In-plane Diffraction ............................. 11 - 25
11.2.2.5 Using the Domed Hot Stage DHS 900 with X'Pert PRO MRD ........................... 11 - 27
11.2.2.6 Using the Domed Hot Stage DHS 1100 with X'Pert PRO MRD ......................... 11 - 33
07.03.27 Page 11.1

Page 11.2 07.03.27

Part II - Chapter 11: MRD Cradle
11.1 GENERAL
Sample platform (or stage) is the generic name given to any device onto which a sample is mounted so that it
can be measured or analyzed. The sample platforms used on X'Pert PRO systems can be divided into six groups,
they are:
• the all-purpose MRD cradle described in this chapter.
• PreFIX sample stages for X’Pert PRO MPD systems described in Chapter 12.
• PreFIX high-throughput sample stage described in Chapter 12.
• PreFIX non-ambient sample stages described in Chapter 13.
• PreFIX temperature controlled humidity chamber described in Chapter 13.
• PreFIX cryogenic temperature controlled sample stages described in Chapter 13.
In this chapter we will provide you with instructions on how to mount samples onto the MRD cradle, including
alignment.
11.2 PW3060/20 ALL-PURPOSE MRD CRADLE

The all-purpose MRD cradle shown in Figure 11.1 is a Eulerian cradle designed to accommodate large samples
and provide five motorized movements (ϕ, ψ, X, Y and Ζ). The mounting disk is parallel to the X-Y plane, the
Z direction is perpendicular to the mounting disk. The sample can be rotated (ϕ movement) and tilted (ψ
movement). The cradle is designed for high resolution measurements, stress, texture, reflectivity, thin-film
phase analysis and standard phase analysis.
The surface of the sample can be moved to coincide with the diffraction plane (Z movement). In addition X and
Y movements are available to alter the measurement position on the sample to map wafer properties or to allow
more than one sample to be loaded and measured in sequence. The data collection software can use the X and
Y movements to oscillate the sample perpendicular to the diffraction plane during measurements.
This cradle can only be used in X’Pert PRO MRD systems that include a horizontal PW3050/6x X’Pert PRO
goniometer. The goniometer radius in this configuration is 320 mm. The cradle cannot be dismounted from the
goniometer by the user.
The five motorized movements are shown in Figure 11.2. Technical specifications are given in Table 11.1.
The sample mounting disk can be oscillated perpendicularly to both the phi and psi axes in order to bring more
crystallites into the diffraction position. The influence of particle statistics is reduced in this way. This oscillation
is especially useful in texture and psi-stress analyses where spinning the sample during the measurement is not
an option. It can also be used for other applications such as phase analysis and omega-stress analysis. The
oscillation range can be set in the data collector software to be 5, 10, 15 and 20 mm. The oscillation frequencies
related to the oscillation ranges are respectively, in the order of: 1.5 Hz, 0.8 Hz, 0.6 Hz and 0.45 Hz.
07.03.27 Page 11.3

Figure 11.1: PW3060/20 MRD Cradle Mounted onto a Horizontal X’Pert PRO Goniometer
Page 11.4 07.03.27

Ψ− Y-
(-90°)
X–
Φ−
Z–
X+ Φ+ Z+
Ψ+
(90°)
Θ+ Θ−
Y+
Figure 11.2: The Five Motorized Movements of the MRD Cradle
Table 11.1: MRD Cradle Specifications of Adjustable Axes
Axis Psi Phi X Y Z
Range 180° (± 90°) 2 x 360° 100 mm 100 mm 11 mm

Minimum step 0.01° 0.01° 0.01 mm 0.01 mm 1 μm
size
Reproducibility ≤ 0.01° ≤ 0.01° 0.1 mm 0.1 mm 1 μm
Slew speed 2.5°/s 70°/s 20 mm/s 20 mm/s 1 mm/s
maximum sample height: 24 mm

maximum sample mass: 0.5 kg (including sample holder)
Samples up to 100 mm x 100 mm can be fully scanned. There is space to mount larger samples if required
although measurements will be limited to an area 100 mm x 100 mm.
07.03.27 Page 11.5

CAUTIONS 1. You must watch out for collisions between the optics and
oversize samples when large angular movements (for example:
with in-plane diffraction) are requested.
2. Normally the X’Pert PRO goniometer and the MRD cradle

automatically reset when the system is switched on or when
power is restored after a power failure. The reset procedure
involves driving all motions of the cradle through their full
range and would damage any oversize sample. You should
disable this automatic reset using the data collector software if
you have large samples, or if you have the alignment shaft
mounted, or if you are performing in-plane diffraction
experiments. This activates an initialization wizard that guides
you through the initialization procedure. You then have the
opportunity to remove the sample before resetting the system.
11.2.1 Accessories
The MRD sample cradle can be used together with a dial gauge, a beam knife and a variety of sample and/or
wafer holders. These accessories are described in this section.
You can also mount your own sample holder onto the MRD cradle as long as you take into consideration the
specifications given in Table 11.1. A schematic diagram of the mounting platform is provided for you in Figure
11.3 to facilitate the design of your own sample holders.
Figure 11.3: MRD Cradle’s Sample Mounting Platform - Schematic Diagram

Page 11.6 07.03.27
11.2.1.1 Dial Gauge

A dial gauge for sample height alignment purposes is supplied with the MRD sample cradle. It can be mounted
onto the dial gauge holder as indicated in Figure 11.16. The use of the dial gauge for mechanical alignment of
the height (Z position) of the sample mounted onto the MRD cradle is described in section 11.2.2.1.
11.2.1.2 Alignment Shaft for X’Pert PRO MRD Systems

An alignment shaft is included with the X’Pert PRO MRD systems. This shaft is used when you are aligning the
X-ray tube’s height so that the X-ray beam passes symmetrically through the goniometer axes. The alignment
shaft is shown in Figure 11.4. The tube height fine check and adjustment procedure is described in section
1.4.9.2 of Chapter 1 in Part II of this User’s Guide.
11.2.1.2.1 Mounting the Alignment Shaft onto the MRD cradle
Mount the alignment shaft in the MRD cradle as follows:
1. Use the data collector software to ensure that the system’s automatic resetting is switched off (System
Settings - Automatic Reset).
2. Set all of the axes: X, Y, Z, 2theta, omega and psi to 0. Make sure that all of the application offsets are
set to 0 in the data collector software.
3. If there is a sample holder mounted; remove it.
4. Remove the black plastic cover from the hole in the center of the alignment shaft location (see Figure
11.1).
5. Remove the three securing screws from the metal plug and then remove the plug by putting a finger
through the hole in the center and lifting the plug out. This at first lifts out easily, but the last part is
more difficult and you may need to wriggle the plug about a little in order to get it out. Keep trying, it
will come out!
6. Place the alignment shaft into the hole that you just removed the metal plug from. MAKE SURE that
you align the screw holes and that the aligning slit on the shaft is directly over the aligning hole in the
base (the only hole without screw threads). This ensures that the reference line on the alignment shaft is
in the correct position and perpendicular to the direct beam.
7. Insert and tighten the three securing screws.
CAUTION
When the alignment shaft is mounted onto the MRD cradle make
sure that you do NOT move any of the motorized cradle motions; or
you may cause the alignment shaft to collide with the MRD cradle.
When you have completed the above mounting procedure you can start the tube height fine check and
adjustment procedure is described in section 1.4.9.2 of Chapter 1 in Part II of this User’s Guide.
07.03.27 Page 11.7

Reference Line
Aligning Slit
Figure 11.4: Alignment Shaft for X’Pert PRO MRD Systems
11.2.1.3 9430 920 04651 Option for In-plane Diffraction

X’Pert PRO MRD systems equipped with the 9430 920 04651 Option for In-plane Diffraction can be used to
measure the lattice spacing (d-spacing) between the crystal planes that are orientated (almost) perpendicularly
to the sample surface. In-plane diffraction refers to incident and diffracted beam directions that are very shallow
(almost parallel to the sample’s surface).
The in-plane geometry is used in measurements on samples where only a very small penetration of the X-ray
incident beam is required, such as: phase analysis of ultra-thin films, lateral grain size determination, and the
direct measurement of in-plane lattice parameters. Typical values for the penetration depth are within the range
of 1 nm to 100 nm. The penetration depth can be changed by varying the angle between the incident beam and
the sample surface.
The option for in-plane diffraction as is available for X’Pert PRO MRD systems makes it possible to move the
MRD cradle to a position with ψ = 90º (the sample is positioned horizontally) and ω = -90º. In this configuration
the psi axis can be used to set the angle of incidence.
Page 11.8 07.03.27

Figure 11.5: X’Pert PRO MRD System set to the In-plane Position
The phi axis of the cradle is used to rotate the sample around the surface normal.
When the option for in-plane diffraction is implemented, the automatic system reset is disabled. This prevents
the system from causing collisions between the MRD and the (parts mounted onto) the goniometer during
automatic initialization.
Using the X’Pert PRO MRD system for in-plane diffraction is described in section 11.2.2.4.
07.03.27 Page 11.9

CAUTIONS 1. You must watch out for and prevent collisions between the
cradle, oversize samples, and the (modules mounted onto) the
goniometer when performing in-plane experiments.
2. Normally, the MRD cradle automatically resets when the system

is switched on or when power is restored after a power failure.
The reset procedure involves driving all motions of the cradle
through their full range. In X’Pert PRO MRD systems equipped
with the option for in-plane diffraction this reset procedure
could cause collisions between the MRD cradle and the (optical
modules mounted onto the) goniometer. You must disable the
automatic reset using the data collector software. This activates
an initialization wizard that guides you through the
initialization procedure. You then have the opportunity to make
sure that all the goniometer and cradle axes are in a safe
position before proceeding with the procedure for (re)starting
the system as described in section 11.2.2.4.1.
11.2.1.4 0.2 mm Mask for In-plane Diffraction

A special mask is included in the delivery. It is shown in Figure 11.6. This mask is used in combination with the
PW3098/27 Parallel Plate Collimator for alignment purposes.
How to use this mask to align the sample for in-plane diffraction is described in section 11.2.2.4.2.
Figure 11.6: Alignment Mask for In-plane Diffraction
Page 11.10 07.03.27

11.2.1.5 PW3061/21 Sample Holder for Solid Samples

The PW3061/21 Sample Holder for Solid Samples is used to hold irregularly shaped samples securely in
position on the cradle. This holder comprises a V-block and clamping block as shown in Figure 11.7. The
positions of these blocks can be changed to accommodate a wide variety of sample shapes as well as samples
mounted in PW18xx sample holders (see Appendix A). The maximum sample height is 20 mm. The sample
diameter must be between 10 mm and 93.5 mm.
Hole for Mounting

Screw (3x)
V-block
Clamping Block
Clamping Screw
V-block Mounting
Holes (5 positions)
Figure 11.7: PW3061/21 Sample Holder for Solid Samples

11.2.1.5.1 Mounting the Sample Holder onto the MRD Sample Cradle
The sample holder can be secured to the mounting disk on the MRD sample cradle by the three screws supplied.
Alternatively the holder can be fitted onto the 4 inch wafer holder (PW3061/22) which is supplied with the MRD
sample cradle. Longer screws (M3 x 25) are required to do this. The sample clamps on the 4 inch wafer holder
must be removed first.
11.2.1.5.2 Mounting Irregularly Shaped Samples
Irregularly shaped samples can be clamped between the V-block and the clamping block as shown in Figure
11.7.
To mount a sample proceed as follows:
1. Move the MRD sample cradle to ψ = 90º in order to have the sample holder horizontal.
2. Secure the V-block at one of its five specific positions on the sample holder, refer to Figure 11.7.
3. Position the sample to be mounted against the V-block.
4. Loosen the clamping screw on the clamping block and slide the block along its groove until it is firmly
up against the sample.
5. Tighten the clamping screw to lock the sample in position.
6. Move ψ to 0º and check that the sample is still securely held in the correct position.
If measurements at low angles are required, take care that the mounting blocks (or any other material used to
secure the sample) do not obstruct the X-ray beam path.
07.03.27 Page 11.11

11.2.1.6 PW3061/22 4 Inch Wafer Holder

The PW3061/22 4 Inch Wafer Holder is a 100 mm (4 inch) diameter wafer mounting plate for semiconductor
wafers and other thin parallel sided samples.
One of these holders is delivered together with the MRD sample cradle, it can also be ordered as an accessory.
The 4 inch wafer holder is fitted onto the cradle by three screws.
Figure 11.8: 4 Inch, 6 Inch and 8 Inch Wafer Holders

Clips are provided on the wafer holder which can be used to gently and securely hold full wafers or large pieces
of a wafer. Alternatively some form of adhesive tape or plasticine may be used. Care should be taken to avoid
straining the sample as this will alter the diffraction profile. The footprint of the incident beam should be well
away from the mounting area if there is any doubt about the strain-free nature of the mounting. When
measurements at low angles are required care should be taken to avoid obstructing the X-ray beam path with
mounting clips or other mounting material.
11.2.1.7 PW3061/2x 6 & 8 Inch Wafer Holders

Two wafer holders are available within X’Pert PRO MRD to allow the mounting of wafers up to 6 inches (150
mm) or 8 inches (200 mm) in diameter to be mounted onto the MRD sample cradle. They are shown in Figure
11.8. The relationship between the type numbers and the maximum wafer diameter is given in Table 11.2. The
maximum X and Y ranges are also given in that table. The X and Y limiters (included) are used to limit the X
and Y ranges of the MRD cradle. They are shown in Figure 11.8. Mounting the X and Y limiters onto the MRD
cradle is described in section 11.2.1.7.1.
Page 11.12 07.03.27

Table 11.2: Maximum Wafer Diameter & X and Y ranges

for the PW3061/2x Wafer Holders
Type Maximum Wafer X and Y

Number Diameter Range
PW3061/22 4 inch (100 mm) 100 mm

PW3061/23 6 inch (150 mm) 60 mm
PW3061/24 8 inch (200 mm) 25 mm
11.2.1.7.1 Mounting the PW3061/2x Wafer Holder onto the MRD Sample Cradle
Before you start this action you must have the system switched on and the data collector software running, then
proceed as follows:
1. Use the data collector software to ensure that the system’s automatic resetting is switched off (System
Settings - Automatic Reset).
2. Set all of the axes: X, Y, Z, 2theta, omega, phi and psi to 0. Make sure that the application offsets are
set to 0 in the data collector software.
3. Remove (if one is fitted) the existing sample holder.
4. Mount and secure the X limiter onto the small actuator pin located between the X limit micro switches
(see Figure 11.16). The actuator pin can be found at the rear of the X manipulator. Ensure that the
limiter is fitted parallel to the X ruler.
5. Move ψ to -90º so that you can see the Y actuator pin, then mount and secure the Y limiter onto the
small actuator pin located between the Y limit micro switches (see Figure 11.16). The actuator pin can
be found at the rear of the Y manipulator. Ensure that the limiter is fitted parallel to the Y ruler.
6. Move ψ to +90º to make mounting the wafer holder easier. Fit the wafer holder onto the MRD
mounting disk for sample mounting devices, using the screws supplied.
7. Use the data collector software to set the movement limits to +30 mm (+12.5 mm for 8 inch holder) and
-30 mm (-12.5 mm for 8 inch holder) for both X and Y movements.
8. Rotate ϕ through both limits of X and Y checking that the wafer holder does not collide with any other
parts of the cradle or system.
9. Move X and Y back to their central positions.
10. It is now possible to mount a wafer as described in section 11.2.1.7.2.
11.2.1.7.2 Mounting a Wafer onto the PW3061/2x Wafer Holder
Mount a wafer onto the wafer holder as follows:
1. Move the MRD sample cradle to ψ = 90º in order to set the wafer holder to the horizontal position.
2. Slide the three wafer clamps to the edge of the wafer holder.
3. Carefully place the wafer onto the holder, slide the clamps into position to hold it and secure the clamps
in position.
4. Check that the wafer is mounted flat onto the wafer holder and is not bent.
5. Move the MRD sample cradle to ψ = 0º to set the holder into the vertical position and check that the
wafer is still in the correct position.
The wafer is now correctly mounted and ready for measurements.
07.03.27 Page 11.13

11.2.1.8 PW3061/25 Adjustable “De Wolff’s” Knife

The PW3061/25 Adjustable “De Wolff’s” Knife is a beam knife used in reflectivity measurements to reduce the
reflecting area on the sample. It can be mounted onto the dial gauge holder on the MRD sample cradle as is
shown on Figure 11.1. The use of the beam knife on the X’Pert PRO MRD is described in Chapter 14 in Part II
11.2.1.9 9430 500 20351 Magnetic Ring

The magnetic ring can be fitted onto the MRD sample cradle in order to enable the 9430 500 20361 Sample
Platform to be magnetically mounted.
The magnetic ring is secured to the MRD sample cradle with the six screws supplied with the magnetic ring.
Figure 11.9: 9430 500 20351 Magnetic Ring and 9430 500 20361 Sample Platform
11.2.1.10 9430 500 20361 Sample Platform

The 9430 500 20361 Sample Platform is used to mount thin parallel sided samples (for example: pieces of a
semiconductor wafer) onto the MRD sample cradle.
The 9430 500 20351 Magnetic Ring must be mounted onto the MRD sample cradle and then the sample platform
(with the samples already fixed onto it) can be magnetically attached to it.
Adhesive tape or plasticine can be used to affix the samples onto the sample holder. Alternatively, you can use
the magnetic strips delivered with the sample platform. Care should be taken to avoid straining the sample as this
will alter the diffraction profile. The footprint of the incident beam should be well away from the mounting area
if there is any doubt about the strain-free nature of the mounting. When measurements at low angles are required
care should be taken to avoid obstructing the X-ray beam path with the mounting material.
11.2.1.11 9430 500 20491 Domed Hot Stage DHS 900

The 9430 500 20491 Domed Hot Stage DHS 900 is a non-ambient chamber that can be mounted onto an MRD
cradle. It is designed for in situ X-ray diffraction studies that require psi tilt or phi rotation, such as measurements
on epitaxial layers or psi-stress analysis. The temperature range is from room temperature up to 900 °C
(1173 K). The Domed Hot Stage 900 is shown in Figure 11.10.
Page 11.14 07.03.27

Figure 11.10: 9430 500 20491 Domed Hot Stage DHS 900
Samples can be measured in air at atmospheric pressure, in inert gas (nitrogen) at a maximum over pressure of
0.2 bar, or in a vacuum (a vacuum of 0.5 mbar can be achieved). For investigations at temperatures ranging from
room temperature up to 200 °C (473 K), it is not necessary to use any cooling gas. For measurements at heating
plate temperatures above 200 °C (473 K), cooling gas (compressed air) must be used in order to guarantee
sufficient heat removal from the dome and the housing of the DHS 900.
The DHS 900 should be used with flat or flake-shaped samples with a maximum diameter of 25 mm and a
maximum height of 4 mm.
The 9430 500 20491 Domed Hot Stage 900 comprises:
- a domed hot stage housing with heating plate, thermocouple and spring grips,
- an X-ray transparent dome,
- a cooling air attachment with nozzle for cooling air,
- a connection device for gas/vacuum and temperature control,
- a TCU 150 Temperature Control Unit (see Figure 11.11).
Use of vacuum equipment is optional.
Use of the Domed Hot Stage in combination with the MRD cradle is described in section 11.2.2.5. Please refer
to the Anton Paar manuals “DHS 900 Domed Hot Stage for PANalytical MRD” (document number C17IB03),
“TCU 150 Temperature Control Unit” (document number B39IB16) and “General Information Vacuum
Systems” (document number B34IE13) for further details.
07.03.27 Page 11.15

11.2.1.11.1 Accessories
11.2.1.11.1.1 DHS 900 Housing and Heating Plate
The domed hot stage housing is made of eloxadized aluminium and has cooling fins that provide sufficient heat
transfer from the heating plate to the surrounding atmosphere. There are four holes are in the housing to mount
the DHS 900 onto the MRD cradle.
The housing contains a relief pressure valve that opens if an over-pressure of approximately 0.2 to 0.3 bar is
generated inside the dome.
The heating plate is made of Inconel, a nickel-chromium alloy with good oxidation resistance at high
temperatures. A thermocouple is located below the center of the heating plate.
The heating plate has four Inconel clamps for sample mounting purposes.
Further information about the heating plate and its use is given in the DHS 900 instruction manual.
11.2.1.11.1.2 X-ray Transparent Dome

The DHS 900’s dome is made from PEEK, a synthetic material based on polyetheretherketone resin. The
stainless steel ring at the rim of the dome has three clasps to fix the dome to the DHS 900. An O-ring in the DHS
900 guarantees vacuum.
Further information about the dome and its use is given in the DHS 900 instruction manual.
11.2.1.11.1.3 Cooling Air Attachment

The cooling air attachment is used to cool the dome and the DHS 900 housing. It uses clean, compressed air. The
cooling air attachment is mounted onto the MRD cradle and connected to the cooling gas supply with a black
hose which is attached to the TCU 150 Temperature Control Unit. The TCU 150 switches the device off as soon
as the cooling gas pressure drops.
If the laboratory does not have any compressed air available, a small compressor can be used to supply the
cooling gas. The pressure of the cooling air must be higher than 2.0 bar and the flow rate must be over 100 liters
per minute.
Further information about the cooling air attachment and its use is given in the DHS 900 instruction manual.
11.2.1.11.1.4 Connection Device for Gas/Vacuum and Temperature Control

The connection device contains a 4-pin connector for the thermocouple, a 2-pin connector for heating and a
flange (DN16KF) for the gas/vacuum supply. It is connected to the DHS 900 housing and heating plate by means
of a black hose.
Using the gas/vacuum supply, samples can be investigated under vacuum (minimum pressure 0.5 mbar) or inert
gas with an overpressure of approximately 0.2 bar. Above that pressure the relief pressure valve will open.
Further information about the connection device and its use is given in the DHS 900 instruction manual.
11.2.1.11.1.5 TCU 150 Temperature Control Unit

The TCU 150 Temperature Control Unit is used to control the temperature and the cooling gas supply of the DHS
900. It is integrated in X'Pert PRO MRD systems in such a way that it can be operated using the data collector
software. It automatically switches on the cooling gas supply when the temperature of the heating plate is above
200 °C (473 K). If the cooling gas supply is too low, it switches the heating of the DHS 900 off.
Further information about the temperature control unit and its use is given in the TCU 150 instruction manual.
Page 11.16 07.03.27

Figure 11.11: TCU 150 Temperature Control Unit
11.2.1.11.1.6 9430 500 20521 Air Service Unit

The air service unit is a combination of a filter and a pressure regulator. It is to be used with an external supply
of compressed air. It is shown in Figure 11.12. The filter is required because a lot of compressed air systems
contain oil vapors. This vapor could form a film on the hot PEEK dome and reduce the life of the dome. We
therefore strongly advise you to use this unit in the compressed gas supply.
The filter is equipped with a 5 μm pore size filter and a 0.01 μm pore size filter. The latter must be regularly
replaced.
07.03.27 Page 11.17

Figure 11.12: 9430 500 20521 Air Service Unit
11.2.1.11.1.7 9430 500 20531 Spare Filter Cartridge

The spare filter cartridge contains the 0.01 μm pore size filter for the air service unit of the DHS 900.
For the maintenance of the air service unit refer to the description by Festo, supplied with the air service unit.
Figure 11.13: 9430 500 20531 Spare Filter Cartridge
11.2.1.12 9430 500 21091 Domed Hot Stage DHS 1100

The 9430 500 21091 Domed Hot Stage DHS 1100 is a non-ambient chamber that can be mounted onto an MRD
cradle. It is designed for in situ X-ray diffraction studies that require psi tilt or phi rotation, such as measurements
on epitaxial layers or psi-stress analysis. The temperature range is from room temperature up to 1100 °C
(1373 K), in helium atmosphere up to 1050 °C (1323 K). The Domed Hot Stage 1100 is shown in Figure 11.14.
Page 11.18 07.03.27

Figure 11.14: 9430 500 21091 Domed Hot Stage DHS 1100
Samples can be measured in air at atmospheric pressure, in inert gas (nitrogen) at a maximum over pressure of
0.3 bar, or in vacuum (a vacuum of 10-2 mbar can be achieved). For investigations at temperatures ranging from
room temperature up to 200 °C (473 K), it is not necessary to use any cooling gas. For measurements at
temperatures above 200 °C (473 K), cooling gas (compressed air) must be used in order to guarantee sufficient
heat removal from the dome and the housing of the DHS 1100.
The DHS 1100 is preferably used with flat or flake-shaped samples with a maximum diameter of 25 mm and a
maximum height of 2 mm.
The 9430 500 21091 Domed Hot Stage 1100 comprises:
- a domed hot stage housing with heating plate, thermocouple and sample fixing springs,
- an X-ray transparent dome, made of graphite,
- a cooling air attachment,
- a connection device for gas/vacuum and temperature control,
- a TCU 200 Temperature Control Unit (see Figure 11.15).
Use of vacuum equipment is optional.
Use of the Domed Hot Stage in combination with the MRD cradle is described in section 11.2.2.6. Please refer
to the Anton Paar manuals “DHS 1100 Domed Hot Stage Version PANalytical” (document number C58IB01),
Systems” (document number B34IE13) for further details.
07.03.27 Page 11.19

11.2.1.12.1 Accessories
11.2.1.12.1.1 DHS 1100 Housing and Heating Plate
The domed hot stage housing is made of anodized aluminium and has cooling fins that provide sufficient heat
transfer from the heating plate to the surrounding atmosphere. Four holes are present in the housing to mount the
DHS 1100 onto the MRD cradle.
The housing contains a relief pressure valve that opens if an over-pressure of approximately 0.2 to 0.3 bar is
generated inside the dome.
The sample holder is made of aluminium nitride (AlN), a ceramic material with excellent temperature
conductivity and good chemical resistance, The heater is located just under the sample holder. A thermocouple
is located below the center of the heating plate.
The sample holder has two Inconel sample fixing springs for sample mounting purposes.
Further information about the heating plate and its use is given in the Anton Paar instruction manual “DHS 1100
Domed Hot Stage Version PANalytical” (document number C58IB01).
11.2.1.12.1.2 X-ray Transparent Dome

The dome of the DHS 1100 is made of graphite. The aluminium ring at the rim of the dome has three clasps to
fix the dome to the DHS 1100. An O-ring in the DHS 1100 guarantees vacuum.
Further information about the dome and its use is given in the DHS 1100 instruction manual.
11.2.1.12.1.3 Cooling Air Attachment

The cooling air attachment is used to cool the dome and the DHS 1100 housing. It uses clean, compressed air.
The cooling air attachment is mounted onto the MRD cradle and connected to the cooling gas supply with a black
hose attached to the TCU 200 Temperature Control Unit. The TCU 200 switches the device off if the cooling
gas pressure drops.
If the laboratory does not have any compressed air, a small compressor can be used to supply the cooling gas.
The pressure of the cooling air must be between 2.0 bar and 4.0 bar overpressure, the flow rate must be 120 liters
per minute.
Further information about the cooling air attachment and its use is given in the Anton Paar instruction manual
“DHS 1100 Domed Hot Stage Version PANalytical” (document number C58IB01).
11.2.1.12.1.4 Connection Device for Gas/Vacuum and Temperature Control

The connection device contains a 6-pin connector for the thermocouple, a 2-pin connector for heating and a
flange (DN16KF) for the gas/vacuum supply. It is connected to the DHS 1100 housing and heating plate by
means of a black hose.
The gas/vacuum supply allows samples can be investigated under vacuum (minimum pressure 10-2 mbar) or
inert gas with an overpressure of approximately 0.2 bar. Above that pressure the relief pressure valve opens.
Further information about the connection device and its use is given in the Anton Paar instruction manual “DHS
1100 Domed Hot Stage Version PANalytical” (document number C58IB01).
11.2.1.12.1.5 TCU200 Temperature Control Unit
The TCU 200 Temperature Control Unit is used to control the temperature and the cooling gas supply pressure
of the DHS 1100. It is integrated in X'Pert PRO MRD systems such that it can be operated by the data collector
software. It automatically switches on the cooling gas supply when the temperature of the heating plate is above
200 °C (473 K). If the pressure of the cooling gas supply is too low, it switches the heating of the DHS 1100 off.
Further information about the temperature control unit and its use is given in the TCU 200 instruction manual.
Page 11.20 07.03.27

11.2.1.12.1.6 9430 500 20521 Air Service Unit

The air service unit is a combination of a filter and a pressure regulator. It is to be used with an external supply
of compressed air. It is shown in Figure 11.12. The filter is required because a lot of compressed-air systems
contain oil vapors. This vapor could form a film on the hot graphite dome and reduce the life of the dome. We
therefore strongly advise you to use this unit in the compressed gas supply.
The filter is equipped with one filter with a pore size of 5 mm and another with a pore size of 0.01 mm. This
latter filter must be regularly replaced.
11.2.1.12.1.7 9430 500 20531 Spare Filter Cartridge
The spare filter cartridge contains the 0.01 mm pore size filter for the air service unit of the DHS 1100. It is
For the maintenance of the air service unit refer to the description by Festo, supplied with the air service unit.
07.03.27 Page 11.21

11.2.2 Use
When high resolution measurements are required you are advised to allow the complete system to reach a stable
temperature before starting to collect data. This should include allowing the sample temperature to be the same
as the mounting plate. Time can be saved by storing future samples within the instrument enclosure ready for use.
11.2.2.1 Mechanically Aligning the Sample

The sample should be positioned on the diffractometer axis using the Z movement of the sample cradle. For most
applications this can be done mechanically using the dial gauge supplied (see Figure 11.16). The reading
corresponding to the Z = 0 position (that is, the correct sample height) is provided by the PANalytical Service
Engineer when the system is installed. Where the application requires data collection at very low angles of
incidence the sample will need to be positioned so that it exactly intercepts the incident beam when set parallel
to it. This procedure is described in section 11.2.2.2. Sample alignment for in-plane diffraction experiments is
described in 11.2.2.4.2.
CAUTION The dial gauge has been accurately calibrated by the PANalytical
Service Engineer to ensure that the correct sample height position
is known to within a few micrometers. Do not therefore turn the
adjustment screw, pull on the long arm of the dial gauge assembly,
rotate the outer rim of the gauge or drop the gauge as these
actions are likely to cause the gauge to lose calibration.
Where it is undesirable to make mechanical contact with the top surface of a sample, for example: a partially
processed semiconductor wafer, a sample of identical thickness should be aligned and the same Z setting used
for the delicate sample. Alternatively delicate samples can be aligned using the X-ray method describe in section
11.2.2.2.
Alignment of a sample for micro-diffraction experiments using an alignment microscope is described in section
In order to mechanically align the sample height position proceed as follows:
1. Move the sample platform (with the sample mounted) to the lowest possible Z position.
2. Mount the dial gauge onto the dial gauge holder on the MRD Sample Cradle.
3. Use the data collector software to carefully move the sample platform upwards in the Z direction. The
sample surface is at the correct height when the dial gauge reading matches the reference value of the
dial gauge as provided by the PANalytical Service Engineer when the system was installed.
4. Make a note of the actual Z position as given by the data collector software.
5. Move the sample platform to the lowest Z position.
6. Remove the dial gauge onto the dial gauge holder from the MRD Sample Cradle.
7. Move the sample platform to the Z position noted in step 4 of this procedure.
The sample height is now correctly adjusted.
Page 11.22 07.03.27

Dial Gauge
Holder
Actuator Pin
for X-ruler
Psi-yoke
Y-translation
Limit Switch
4 Inch
Wafer Holder
Dial Actuator Pin

Gauge for Y-ruler
(not visible)
X-translation
Limit Switches
Figure 11.16: MRD Cradle with Dial Gauge Indicating Z position
11.2.2.2 Aligning the Sample Using X-rays

When mechanical contact with the surface of the sample should be avoided, or when measurements are to be
performed at very low angles, the sample must be positioned so that it exactly intersects the incident beam when
set parallel to it. This section describes the procedure for standard experiments. Sample alignment for in-plane
diffraction is described in section 11.2.2.4.2. Alignment of a sample for micro-diffraction experiments using an
alignment microscope is described in section 10.4.1 in Chapter 10 in Part II of this User’s Guide.
In order to align the sample using X-rays, the sample must be large and flat. The alignment procedure is as
follows:
1. Mount a non-offset incident beam PreFIX module (for example: a fixed or programmable divergence
slit) and report this to the data collector software. Use a fixed divergence (setting) of 1/4º or smaller.
2. Center the sample in the heart of the goniometer. You can use the dial gauge as an indication of the
center.
3. Set all of the axes: Z, 2theta, omega, phi and psi to 0 and make sure that the direct X-ray beam is not
obstructed by the sample or the MRD cradle.
4. Insert a 0.2 mm Cu attenuation foil into the incident beam path in order to protect the detector.
5. Perform a 2θ scan through the 2θ = 0º position using a small receiving slit or the X’Celerator, or the
PIXcel in scanning mode to find the peak position of the direct X-ray beam. Make a note of the 2θ peak
position.
07.03.27 Page 11.23

6. Use the data collector software to recalibrate the 2θ = 0º position to coincide with the peak position of
the direct beam.
7. Depending on the diffracted beam optics used, perform one of the following actions:
a. If you are using the PW3093/60 Programmable Receiving Slit, set it to 3 mm.
b. If a programmable or fixed anti-scatter slit assembly is mounted onto the programmable receiving
slit, set it to 4º.
c. If you are using an X’Celerator, rotate it 90º (see section 21.4 in Chapter 21 of Part II of this User’s
Guide) and set it to receiving slit mode. Use the maximum length of 9 mm. Do not use a slit in the
fixed anti-scatter slits holder.
d. If you are using a PIXcel, set it to receiving slit mode and use the maximum active length. Do not
use a slit in the fixed anti-scatter slits holder.
e. If you are using the PW3097/60 Rocking Curve Attachment, do not insert a slit.
f. If you are using the PW3120/60 Triple Axis and Rocking Curve Attachment, or a PW3120/65
Asymmetric Triple Axis and Rocking Curve Attachment, select the beam path with the rocking
curve arm of the attachment in the data collector software. Do not insert a slit into the rocking
curve part of the attachment.
8. Open the shutter and make a note of the peak intensity (Ip). If you are using an X’Celerator or a PIXcel
detector, make a stationary measurement for about 10 seconds in order to determine the peak intensity
(Ip).
9. Set 2θ = 0º and move the sample with small increments of Z until the direct beam intensity is equal to
Ip/2.
10. Make a small ω scan and note the maximum intensity Im.
11. The next action depends on whether Im > Ip/2 (step a), or Im < Ip/2 (step b).
a. If Im > Ip/2, move the sample forward with small increments of Z until the maximum intensity
measured in an ω scan (Im) equals Ip/2.
b. If Im < Ip/2, move the sample backwards with small increments of Z until the maximum intensity
12. Move the goniometer to the peak position of the ω scan where Im equals Ip/2 and make a note of the Full
Width at Half Maximum (FWHM) of the peak.
13. Measure the FWHM of the peaks in a series of ω scans with the ψ angle changing in steps of 0.5º
around the starting position.
14. Set the ψ angle at the value that produces the minimum FWHM.
Alternatively you can automatically optimize the ψ setting in a series of ω scans using the
optimize program in the data collector software.
15. Move ω to the peak position and re-calibrate the ω = 0º position using the data collector software. The
sample is now aligned at optimal 2θ, ω, ψ and Z settings.
NOTE: If you are using an X’Celerator, rotate it back to its normal position before starting the
measurement.
Reset ω and 2θ to the original offset values at the end of the measurement.
11.2.2.3 Use of the MRD Cradle with more than one Sample
It is possible to mount a variety of samples onto the MRD sample cradle and use the cradle as a sample changer.
When measurements are going to be made using the same incident beam and diffracted beam optics, the batch
program in the data collector software can be used to perform a series of measurements on a group of samples.
After each measurement the cradle can be moved to the correct X, Y and Z position for the next sample to be
measured. These sample positions must be determined before data collection is started.
Page 11.24 07.03.27

11.2.2.4 Using the X’Pert PRO MRD System for In-plane Diffraction
This section describes the use of X’Pert PRO MRD systems equipped with the 9430 920 04651 Option for In-
plane Diffraction. Operation of the system is the same as operating a standard X’Pert PRO MRD system;
however, for in-plane diffraction measurements the MRD cradle must be set to ω = -90º. This makes collisions
between the MRD cradle and the incident beam optics possible.
CAUTION
Always make sure that a collision will NOT occur before you move
either the psi or omega axes.
The procedure for starting (or restarting) the system avoiding collisions is described in 11.2.2.4.1.
The procedure for aligning the sample for in-plane diffraction experiments is given in 11.2.2.4.2.
11.2.2.4.1 Starting or Restarting the System

In order to enable the possibility of measuring in-plane diffraction, the lower limit of the omega axis of the
goniometer has been changed. This means that under certain conditions the cradle can collide with the incident
beam optical module or the tube shield. In order to prevent a collision during start-up and initialization, the
system is not allowed to start up and initialize automatically, in other words: the automatic reset is disabled.
When the system is to be started, an initialization wizard is started in the data collector software. You must use
the data collection software to verify that all axes are in a safe position. The initialization procedure can only be
activated by the system, that occurs when a system that is configured as an in-plane diffraction system needs to
be initialized.
NOTE: Make sure that the “In-plane Diffractometer” check box is checked in the configuration that you
saved in the data collector software, otherwise you will not be able to connect with the instrument.
CAUTION
Never enable the automatic reset on a system configured for
in-plane diffraction.
During start-up of a system configured for in-plane diffraction, the psi axis of the MRD Cradle should be set
around -90º ± 2º or +90º ± 2º. When the system has been used for in-plane diffraction before switching the
system off, this will generally be the case. When the cradle is in another position, as will be the case when any
other type of measurement has been performed, the cradle has to be moved to one of these positions.
The initialization procedure allows you to (i) remove all of the incident and diffracted beam PreFIX modules
and the stage accessories, and (ii) to send the cradle to a safe ψ position, before the actual initialization procedure
is started up.
Once the initialization is complete, the system is on-line and you can proceed with your measurements.
11.2.2.4.2 Aligning the Sample for In-plane Diffraction

For in-plane diffraction measurements the sample must be aligned so that the sample is exactly positioned in the
diffraction plane, as determined by the incident and diffracted X-ray beam. The procedure for sample alignment
is described in this section. You can use the PW3132/62 Reference Samples as test samples for this procedure.
Proceed as follows:
1. Ensure that the X-ray tube is in the point focus position. If necessary change the tube to the point focus
position following the procedure given in section 1.4.7 in Chapter 1 in Part II of this User’s Guide.
07.03.27 Page 11.25

2. Mount a PW3146/60 X-ray Lens on the incident beam PreFIX position and a PW3098/27 Parallel Plate
Collimator (acceptance angle = 0.27º) and a detector on the diffracted beam PreFIX position.
Alternatively, you can use a PW3110/6x High-resolution Monochromator on the incident beam PreFIX
position and either a PW3097/60 Rocking Curve Attachment or a PW3120/60 Triple Axis and Rocking
Curve Attachment or a PW3120/65 Asymmetric Triple Axis and Rocking Curve Attachment on the
diffracted beam PreFIX position.
3. Which of the following actions you do depends on whether you have an X-ray lens fitted (step a), or a
high-resolution monochromator (step b).
a. If you are using an X-ray lens in the incident beam, insert a standard copper foil (0.2 mm) beam
attenuator into the appropriate slot in the X-ray lens. Set the HT generator to 45 kV and 40 mA.
b. If you are using a high-resolution monochromator in the incident beam, set the HT generator
according to the settings as given in the column “Direct Beam Intensity” in Table 7.1 in Chapter 7
in Part II of this User’s Guide.
4. Set the crossed slits on the X-ray lens or the high-resolution monochromator so that the X-ray beam
exiting from the X-ray lens or monochromator has a width of 5 mm and height of 5 mm or less (see
Figure 7.2 or Figure 9.3 in either Chapter 7 or Chapter 9 in Part II of this User’s Guide for details about
the crossed slits assembly).
5. Use the data collector software to move the system to the following positions:
2θ = 0º
X = 0 mm
Y = 0 mm
Z = 0 mm
ϕ = 0º
ψ = 90º
Make sure that the application offsets are all set to 0 in the data collector software.
CAUTION
It is very important that you do not forget to set ψ = 90º.
6. Move the MRD cradle to ω = -90º.

7. Mount the sample in the center of the cradle.
8. Your action here depends on whether you have a parallel plate collimator (action a) or a rocking curve
attachment (action b):
a. If you are using a parallel plate collimator: insert the special 0.2 mm in-plane mask (see Figure
11.6) into the slot for the collimator slit in the parallel plate collimator (refer to section 18.2 in
Chapter 18 in Part II of this User’s Guide).
b. If you are using a rocking curve attachment: insert a 1 mm mask into the rotatable slit holder (refer
to section 16.4.1.1.3 in Chapter 16 in Part II of this User’s Guide).
9. Make a 2θ scan from -1º to 1º. You will measure a single peak with a gaussian shape. Make sure that the
intensity does not exceed the detector’s maximum allowed count rate.
10. Set 2θ to the peak position (this should be 2θ = 0º) and make a note of the maximum intensity (Ip).
11. Move the Z-translation of the sample table with small increments until the direct beam intensity = Ip/2.
Make a note of this Z value.
Page 11.26 07.03.27

12. Make a ψ scan from 88º to 92º in order to remove possible small errors in the sample tilt. The scan must
show a triangular shaped peak with its maximum value at ψ = 90º. If the peak is at a different position,
move the psi axis to that position and repeat the procedure from step 9 on.
13. Your sample is now correctly aligned, and you can start to find a reflection. Set the angle of incidence
(α) between the incident X-ray beam and the sample surface to 0.3º; that means: move the psi axis to
the position found in step 12, and add 0.3º.
14. Move the 2theta axis to a position where you expect a reflection. If applicable, remove the attenuation
foil and the beam width mask from their slots. Set the HT generator to 45 kV and 40 mA.
15. If your sample is a randomly oriented polycrystalline sample, proceed with step 16. If your sample is
mono-crystalline, or shows preferred orientation: make a ϕ scan in order to find the reflection. If your
sample has a slight miscut, or the sample support blocks the X-ray beam, make the ϕ scan over the full
360º.
16. When you have found the reflection you can optimize the 2θ angle by making a small 2θ scan.
17. Finally, you can optimize the angle of incidence (α) by making a ψ scan. The angle of incidence
determines the penetration depth of the X-ray beam.
The choice of α is not very critical when you are measuring a bulk sample. However, if you
want to analyze a reflection from a thin layer you will find that the intensity of the reflection
strongly depends on the setting of α.
You are now ready to start with your in-plane diffraction experiments.
11.2.2.5 Using the Domed Hot Stage DHS 900 with X'Pert PRO MRD
This section describes mounting the Domed Hot Stage DHS 900 onto the MRD cradle and connecting the
compressed air supply, the gas/vacuum supply and the temperature controller. It further describes the system's
goniometer and cradle axes limitations when working with the DHS 900, and sample height alignment. For
information about sample mounting and operation of the DHS 900 in air, inert gas or vacuum, please refer to the
Anton Paar manuals: “DHS 900 Domed Hot Stage for PANalytical MRD Instruction Manual” (document
number C17IB03), “TCU 150 Temperature Control Unit” (document number B39IB16) and “General
Information Vacuum Systems (document number B34IE13).
11.2.2.5.1 Axes Limitations with DHS 900 Mounted
Using the DHS 900 on the MRD cradle changes the limits of the cradle's movements. These limitations are given
in Table 11.3. At high negative psi values the cooling gas nozzle may interfere with the incident and/or diffracted
beam. Most X-ray diffraction applications do not require high negative psi tilts, the exception being psi-stress
analysis with positive and negative tilts. For this case, we recommend that you work with positive and pseudo-
negative tilts instead.
Table 11.3: Axes Limitations with DHS 900 Mounted
All-purpose MRD MRD Cradle with

Axis
Cradle DHS 900 Mounted
X ±50 mm ±10 mm
Y ±50 mm ±10 mm
Z 0 mm to 11 mm 0 mm to 4 mm
ϕ -360º to +360° 0º to +360º
ψ -95° to 95° -95° to 95° *
* Please note that the nozzle might block the X-ray beam at high negative tilts.
07.03.27 Page 11.27

CAUTION
When working with the DHS 900 you must watch out for and
prevent collisions between the cradle and the modules mounted
onto the goniometer.
Normally, the MRD cradle automatically resets when the system is
reset procedure involves driving all movements of the cradle
through their full range which could damage the hose on the DHS
900. Therefore in order to prevent this you must disable this
automatic reset using the data collector software. This activates an
initialization wizard that guides you through the initialization
procedure. You then have the opportunity to dismount the DHS 900
and to make sure that all the goniometer and cradle axes are in a
safe position before proceeding with the procedure for (re)starting
the system as described in section 4.3 of Chapter 4 of Part I of this
User's Guide.
11.2.2.5.2 Mounting the DHS 900 onto the MRD Cradle

Mounting the DHS 900 onto the MRD cradle is performed by executing the following steps in sequence:
1. Preparing the X'Pert PRO MRD system.
2. Attaching the DHS 900 to the MRD cradle.
3. Connecting the compressed air supply.
4. Connecting the temperature controller.
5. Mounting the sample.
6. Adjusting the sample height.
11.2.2.5.2.1 Preparing the X'Pert PRO MRD System

1. Remove the sample holder currently mounted on the MRD cradle in order to gain access to the sample
mounting disk. Four holes for mounting the DHS 900 are now visible (see Figure 11.17).
2. If you are going to exceed 200º C in your experiment, you will need to have a compressed air supply
available.
3. If you are going to work in an atmosphere other than air at atmospheric pressure, ensure that the
vacuum or inert gas equipment is available.
4. Ensure that the configuration that you are going to use in data collector software includes the DHS 900.
Page 11.28 07.03.27

Dial Gauge
Holder
Holes for
mounting
the DHS 1100
Figure 11.17: MRD Cradle with Sample Holder Removed
11.2.2.5.2.2 Attaching DHS 900 to the MRD Cradle
The DHS 900 is attached to the sample mounting disk on the MRD cradle using four attachment screws. To
attach the DHS 900 to the MRD cradle, proceed as follows:
1. Go on-line using the data collector software with a configuration that includes a DHS 900.
CAUTION If you go on-line with a configuration that does NOT include the
DHS 900, BUT the DHS 900 is physically mounted onto the MRD
cradle, the axes limitations as described in section 11.2.2.5.1 are
NOT set. This means that if you were to accidentally move the cradle
out of the restricted range, you could damage the hose on the DHS
900.
2. Set ϕ to +360°.
3. Make sure that the black hose that connect the DHS 900 housing with the cooling air attachment is fully
unrolled. It will be rolled up when ϕ is set back to 0°.
4. Place the DHS 900 onto the sample mounting disk and attach it as shown in Figure 11.18 using the four
attachment M4 screws. The white arrows in Figure 11.18 show where the four mounting screws are
located.
07.03.27 Page 11.29

Figure 11.18: DHS 900 Attachment Holes
5. Mount the cooling air attachment onto the dial gauge holder on the cradle using the knurled knob, as
6. Rotate ϕ back to 0°.
7. Loosen the fixing screws holding the X-ray transparent dome in place, turn the dome slightly anti-
clockwise and lift it away.
11.2.2.5.2.3 Connecting the Compressed Air Supply to the DHS 900
The DHS 900 is cooled with cooling gas, preferably clean compressed air. A schematic representation of the
interconnections of the compressed air supply to the DHS 900 is given in Figure 11.20.
1. Connect the compressed air supply to the TCU 150 Temperature Control Unit (air inlet) using the
transparent hose.
2. Connect the black hose from the TCU 150 (air outlet) to the Cooling Air Attachment.
Page 11.30 07.03.27

Figure 11.19: 9430 500 20491 DHS 900 Domed Hot Stage Mounted onto the MRD Cradle
Figure 11.20: Schematic Representation of the Interconnections of the DHS 900
07.03.27 Page 11.31

11.2.2.5.2.4 Connecting the Temperature Controller

The temperature of the DHS 900 is controlled using the Temperature Control Unit TCU 150. The TCU 150 is
connected to the DHS 900 housing and heating plate via a connection device. This connection device can also
be connected to vacuum equipment or an inert gas supply if required. A schematic representation of the
interconnections of the TCU 150 and the connection device to the DHS 900 is given in Figure 11.20.
1. Attach the connection device for the gas/vacuum and temperature control to the ceiling of the
instrument enclosure, so that the hoses cannot be caught by any part of the goniometer.
2. Refer to Figure 11.10 and Figure 11.20 and connect the TCU 150 to the Connection Device as follows:
a. Connect the green cable (thermocouple) from the rear of the TCU 150 to the 4-pin connector on the
Connection Device.
b. Connect the grey cable (heating) from the rear of the TCU 150 to the 2-pin connector on the
Connection Device.
3. If required, connect the vacuum equipment or inert gas supply to the Connection Device.
11.2.2.5.2.5 Mounting Sample

The DHS 900 heating attachment is ideally suited for flat or flake shaped samples with a maximum diameter of
28 mm. Refer to the DHS 900 Domed Hot Stage Instruction Manual (Document number: C17IB03), Chapter 7,
for information on how to mount the sample onto the heating plate.
Solid samples of sufficient size can be clamped directly using the springs delivered with the DHS 900. Samples
that are too small to be mounted in this way should be glued to a suitable substrate material (for example: a
fragment of a monocrystalline wafer) using a heat resistant glue. A suitable glue is: Thermokitt Roth 1100 ºC.
(www.carl-roth.de).
CAUTION
X-rays that fall onto the substrate, the DHS 900 heating plate or the
springs, could cause spurious peaks in your diffractogram.
11.2.2.5.2.6 Adjusting the Sample Height

The sample height can be adjusted using the data collector Z scan or the dial gauge. To use the dial gauge,
proceed as follows:
1. Move the sample platform (with the DHS 900 mounted) to the lowest possible Z position.
2. Remove the X-ray transparent dome: loosen the fixing screws holding the X-ray transparent dome in
place, turn the dome slightly anti-clockwise and lift it away.
3. Remove the cooling air attachment from the dial gauge holder on the cradle and push it slightly to one
side to make room for the dial gauge.
4. Attach the dial gauge onto the dial gauge holder (see Figure 11.14).
dials gauge as provided by the PANalytical Service Engineer when the system was installed.
8. Remove the dial gauge from the dial gauge holder.
9. Fit the cooling air attachment back onto the dial gauge holder.
10. Fit the X-ray transparent dome.
Page 11.32 07.03.27

11.2.2.6 Using the Domed Hot Stage DHS 1100 with X'Pert PRO MRD
This section describes mounting of the Domed Hot Stage DHS 1100 onto the MRD cradle and connecting the
compressed air supply, the gas/vacuum supply and the temperature controller. It further describes the system's
goniometer and cradle axes limitations when working with the DHS 1100, and sample height alignment. For
information about sample mounting and operation of the DHS 1100 in air, inert gas or vacuum, please refer to
the “DHS 1100 Domed Hot Stage PANalytical Version Instruction Manual” (document number C58IB01),
Systems” (document number B34IE13).
11.2.2.6.1 Axes Limitations with DHS 1100 mounted

Using the DHS 1100 on the MRD cradle changes the limits of the cradle's movements. These limitations are
given in Table 11.4. At high negative psi values the cables of the DHS 1100 might interfere with the diffracted
beam optics. Most X-ray diffraction applications do not require high negative psi tilts, the exception being psi-
stress analysis with positive and negative tilts. For this case, we recommend that you work with positive and
pseudo-negative tilts instead.
Table 11.4: Axes Limitations with DHS 1100 Mounted
All-purpose MRD MRD Cradle with

Axis
Cradle DHS 1100 Mounted
X ±50 mm ±10 mm
Y ±50 mm ±10 mm
Z 0 mm to 11 mm 0 mm to 2 mm
ϕ -360º to +360° 0º to +360º
ψ -95° to 95° -95° to 95° *
* Please note that the cables of the DHS 1100 can interfere with the diffracted beam optics at
high negative tilts (psi <-70°).
CAUTION
When working with the DHS 1100 you must watch out for and prevent
collisions between the cradle and the modules mounted onto the
goniometer.
Normally, the MRD cradle automatically resets when the system is
switched on or when power is restored after a power failure. The reset
procedure involves driving all motions of the cradle through their full
range and which could damage the hose on the DHS 1100. Therefore,
you must disable this automatic reset using the data collector
software. This activates an initialization wizard that guides you
through the initialization procedure. You then have the opportunity to
dismount the DHS 1100 and to make sure that all the goniometer and
cradle axes are in a safe position before proceeding with the procedure
for (re)starting the system as described in section 4.3 of Chapter 4 of
Part I of this User's Guide.
07.03.27 Page 11.33

11.2.2.6.2 Mounting the DHS 1100 onto the MRD Cradle

Mounting the DHS 1100 onto the MRD cradle is performed by executing the following steps in sequence:
1. Preparing the X'Pert PRO MRD system.
2. Attaching the DHS 1100 to the MRD cradle.
3. Connecting the compressed air supply.
4. Connecting the temperature controller.
5. Mounting the sample.
6. Adjusting the sample height.
11.2.2.6.2.1 Preparing the X'Pert PRO MRD system

1. Remove the sample holder mounted on the MRD cradle in order to gain access to the sample mounting
disk. Four holes for mounting the DHS 1100 are now visible (see Figure 11.21).
2. If you are going to exceed 200º C in your experiment, you will need to have a compressed air supply
available.
3. If you are going to work in an atmosphere other than air at atmospheric pressure, ensure that the
vacuum or inert gas equipment is available.
4. Ensure that the configuration that you are going to use in the data collector software includes the
DHS 1100.
Dial Gauge
Holder
Holes for
mounting
the DHS 1100
Figure 11.21: MRD Cradle with Sample Holder Removed
Page 11.34 07.03.27

11.2.2.6.2.2 Attaching DHS 1100 to the MRD Cradle

The DHS 1100 is attached to the sample mounting disk on the MRD cradle with four attachment screws. Proceed
as follows to attach the DHS 1100 to the MRD cradle:
1. Go on-line using the data collector software with a configuration that contains DHS 1100.
CAUTION If you go on-line with a configuration that does NOT include the DHS
1100, BUT the DHS 1100 is physically mounted onto the MRD cradle,
the axes limitations as described in section 11.2.2.6.1 are NOT set. This
means that if you were to accidentally move the cradle out of the
restricted range, you could damage the hose on the DHS 1100.
2. Set ϕ to +360°.
3. Make sure that the black hose that connect the DHS 1100 housing with the cooling air attachment is
fully unrolled. It will be rolled up when ϕ is set back to 0°.
4. Place the DHS 1100 onto the sample mounting disk and attach it as shown in Figure 11.14 using the
four attachment M4 screws. The white arrows in Figure 11.22 show where the four mounting screws
are located.
5. Mount the cooling air attachment onto the dial gauge holder on the cradle using the knurled knob, as
Figure 11.22: 9430 500 21091 DHS 1100 Domed Hot Stage mounted onto the MRD Cradle
6. Rotate ϕ back to 0°.
7. Loosen the fixing screws holding the X-ray transparent dome in place, turn the dome slightly anti-
clockwise and lift it away.
07.03.27 Page 11.35

11.2.2.6.2.3 Connecting the Compressed Air Supply to the DHS 1100

The DHS 1100 is cooled using cooling gas, preferably clean compressed air. A schematic representation of the
interconnections of the compressed air supply to the DHS 1100 is given in Figure 11.23.
Figure 11.23: Schematic Representation of the Interconnections of the DHS 1100

1. Connect the compressed air supply to the TCU 200 Temperature Control Unit (air inlet) using the
transparent hose.
2. Connect the black hose from the TCU 200 (air outlet) to the Cooling Air Attachment.
11.2.2.6.2.4 Connecting the Temperature Controller

The temperature of the DHS 1100 is controlled using the Temperature Control Unit TCU 200. The TCU 200 is
connected with the DHS 1100 housing and heating plate via a connection device. This connection device can
also be connected to vacuum equipment or an inert gas supply if required. A schematic representation of the
interconnections of the TCU 200 and the connection device to the DHS 1100 is given in Figure 11.23.
1. Attach the connection device for the gas/vacuum and temperature control to the ceiling of the
instrument enclosure, so that the hoses cannot be caught by any part of the goniometer.
2. Refer to Figure 11.14 and Figure 11.23 and connect the TCU 200 to the Connection Device as follows:
a. Connect the green cable (thermocouple) from the rear of the TCU 200 to the 6-pin connector on the
Connection Device.
b. Connect the grey cable (heating) from the rear of the TCU 200 to the 2-pin connector on the
Connection Device.
3. If required, connect the vacuum equipment or inert gas supply to the Connection Device.
Page 11.36 07.03.27

11.2.2.6.2.5 Mounting a Sample

The DHS 1100 heating attachment is ideally suited for flat or flake shaped samples with a maximum diameter
of 28 mm. Refer to the DHS 1100 Domed Hot Stage Instruction Manual (Document number: C58IB01),
Chapter 5, for information how to mount the sample onto the heating plate.
Solid samples of sufficient size can be clamped directly using the springs delivered with the DHS 1100. Samples
that are too small to be mounted in this way should be glued onto a suitable substrate material (for example: a
fragment of a monocrystalline wafer) using a heat resistant glue. A suitable glue is Thermokitt Roth 1100º C.
(www.carl-roth.de).
CAUTION
X-rays that fall onto the substrate, the DHS 1100 heating plate or the
springs could cause spurious peaks in your diffractogram.
11.2.2.6.2.6 Adjusting the Sample Height

The sample height can be adjusted using the data collector Z-scan or the dial gauge. To use the dial gauge,
proceed as follows:
1. Move the sample platform (with the DHS 1100 mounted) to the lowest possible Z position.
2. Remove the X-ray transparent dome: loosen the fixing screws holding the X-ray transparent dome in
place, turn the dome slightly anti-clockwise and lift it away.
3. Remove the cooling air attachment from the dial gauge holder on the cradle and push it slightly to one
side to make room for the dial gauge.
4. Attach the dial gauge onto the dial gauge holder (see Figure 11.16).
5. Use the data collector software to carefully move the sample platform upwards in the z-direction. The
dials gauge as provided by the PANalytical Service Engineer when the system was installed.
8. Remove the dial gauge from the dial gauge holder.
9. Fit the cooling air attachment back onto the dial gauge holder.
10. Fit the X-ray transparent dome.
07.03.27 Page 11.37

Page 11.38 07.03.27

Chapter 12
Platforms for Horizontal & Vertical Systems
Contents
12.1 General............................................................................................................................... 12 - 5
12.1.1 Exchanging PreFIX Sample Stages..................................................................................... 12 - 6
12.2 PW3062/00 Stage for Micro-diffraction ......................................................................... 12 - 8
12.2.1 Accessories .......................................................................................................................... 12 - 8
12.2.1.1 Set of Three Sample Tables ................................................................................. 12 - 8
12.2.1.2 PW3714/20 Motor Supply ................................................................................... 12 - 9
12.2.1.3 9430 500 28351 Goniometer Head ...................................................................... 12 - 9
12.2.1.4 9430 500 28341 Alignment Microscope ............................................................. 12 - 9
12.2.2 Use ..................................................................................................................................... 12 - 10
12.2.2.1 Alignment Using an Alignment Microscope ..................................................... 12 - 10
12.3 PW3063/00 Capillary Spinner ....................................................................................... 12 - 12
12.3.1 Accessories ........................................................................................................................ 12 - 12
12.3.1.1 PW3714/20 Motor Supply ................................................................................. 12 - 12
12.3.1.2 9430 500 28351 Goniometer Head .................................................................... 12 - 13
12.3.1.3 9430 500 28341 Alignment Microscope ........................................................... 12 - 13
12.3.2 Use ..................................................................................................................................... 12 - 13
12.4 PW3064/00 Sample Spinner........................................................................................... 12 - 14
12.4.1 Accessories ........................................................................................................................ 12 - 15
12.4.1.1 Sample Holder ................................................................................................... 12 - 15
12.4.1.2 PW18xx Circular Sample Holders..................................................................... 12 - 15
12.4.1.3 PW3064/10 Beam Knife for Sample Spinner.................................................... 12 - 15
12.4.1.4 PW3065/xx PreFIX Sample Changer ................................................................ 12 - 16
12.4.2 Manually Loading a Sample.............................................................................................. 12 - 16
07.03.27 Page 12.1

12.5 PW3064/60 Reflection - transmission Spinner .............................................................12 - 17

12.5.1 Accessories ........................................................................................................................ 12 - 18
12.5.1.1 Sample Holder.................................................................................................... 12 - 18
12.5.1.2 PW18xx Circular Sample Holders ..................................................................... 12 - 18
12.5.1.3 PW3064/10 Beam Knife for Sample Spinner .................................................... 12 - 18
12.5.1.4 PW3064/20 Direct Beam Stop for Reflection-transmission Spinner................. 12 - 20
12.5.1.5 PW3065/xx PreFIX Sample Changer ................................................................ 12 - 22
12.5.1.6 PW3099/70 Large Offset Arm ........................................................................... 12 - 22
12.5.2 Use ..................................................................................................................................... 12 - 23
12.5.2.1 Manually Loading a Sample .............................................................................. 12 - 23
12.5.2.2 Changing Sample Modes ................................................................................... 12 - 23
12.6 PW3067/00 Automatic Phi Cradle ATC-1 ....................................................................12 - 25
12.6.1 Use ..................................................................................................................................... 12 - 25
12.6.1.2 Rotating the ATC-1 Cradle on its Axis.............................................................. 12 - 26
12.6.1.3 Mounting a Sample onto the ATC-1 .................................................................. 12 - 27
12.7 PW3068/00 Automatic Texture Cradle ATC-3 ............................................................12 - 28
12.7.1 Use ..................................................................................................................................... 12 - 29
12.8 PW3069/00 Open Eulerian Cradle ................................................................................12 - 30
12.8.1 Accessories ........................................................................................................................ 12 - 31
12.8.1.1 Multi-purpose Sample Holder............................................................................ 12 - 31
12.8.1.2 Wafer Holder...................................................................................................... 12 - 32
12.8.1.3 PW3069/10 Manual Z Translation Stage ........................................................... 12 - 32
12.9 PW3070/00 Open Eulerian Cradle with Motorized X-translation .............................12 - 38
12.9.1 Accessories ........................................................................................................................ 12 - 39
12.9.1.1 Wafer Holder...................................................................................................... 12 - 39
12.9.1.2 Sample Cups....................................................................................................... 12 - 40
12.9.2 Use ..................................................................................................................................... 12 - 40
12.9.2.1 Mounting Samples on the Wafer Holder ........................................................... 12 - 40
12.9.2.2 Mounting Samples on the Sample Cup .............................................................. 12 - 40
12.9.2.3 Aligning the Sample Using X-rays .................................................................... 12 - 41
12.10 PW3071/60 Stage for Solids or Powders in Flat Sample Holders...............................12 - 42
12.10.1 Accessories ........................................................................................................................ 12 - 42
12.10.1.1 PW1172/01 Set of 25 Flat Sample Holders ....................................................... 12 - 42
12.10.1.2 PW3071/65 Beam Knife for Flat Sample Stage ................................................ 12 - 42
12.10.2 Use ..................................................................................................................................... 12 - 43
12.11 PW3072/60 Stationary Stage for PW18xx Sample Holders ........................................12 - 44
12.11.1 Accessories ........................................................................................................................ 12 - 44
12.11.1.1 Sample Holder.................................................................................................... 12 - 44
12.11.1.2 PW18xx Circular Sample Holders ..................................................................... 12 - 44
12.11.1.3 PW3072/65 Beam Knife for Stationary Stage ................................................... 12 - 45
12.11.2 Use ..................................................................................................................................... 12 - 45
Page 12.2 07.03.27

Part II - Chapter 12: Platforms for Horizontal & Vertical Systems
12.12 PW3074/00 Multi-purpose Sample Stage ..................................................................... 12 - 46

12.12.1 Accessories ........................................................................................................................ 12 - 47
12.12.1.1 Sample Holder for Flat Solid Samples .............................................................. 12 - 47
12.12.1.2 Reference Plate .................................................................................................. 12 - 49
12.12.1.3 Dial Gauge ......................................................................................................... 12 - 49
12.12.1.4 Pin Key .............................................................................................................. 12 - 50
12.12.1.5 PW1172/01 Set of 25 Flat Sample Holders ....................................................... 12 - 51
12.12.1.6 PW3074/10 Beam Knife for Multi-purpose Sample Stage ............................... 12 - 51
12.12.2 Use ..................................................................................................................................... 12 - 52
12.12.2.1 Mounting a Sample onto the Sample Table....................................................... 12 - 52
12.12.2.2 Coarse Sample Height Adjustment.................................................................... 12 - 52
12.12.2.3 Fine Sample Height and Tilt Adjustment .......................................................... 12 - 54
12.13 PreFIX Positioning Stages.............................................................................................. 12 - 55
12.13.1 PW3075/61 Positioning Stage with Motorized X, Y, Z, Tilt & Phi.................................. 12 - 57
12.13.2 PW3075/62 Positioning Stage with Motorized Z, Tilt and Phi Movements ..................... 12 - 58
12.13.3 PW3075/63 Positioning Stage with Motorized X, Y and Z Movements .......................... 12 - 61
12.13.4 Accessories ........................................................................................................................ 12 - 63
12.13.4.1 PW3075/64 Control Electronics ........................................................................ 12 - 63
12.13.4.2 PW3075/65 Dial Gauge ..................................................................................... 12 - 64
12.13.4.3 PW3075/66 Beam Knife for Reflectivity Measurements .................................. 12 - 65
12.13.4.4 PW3075/67 Beam Knife for Positioning Stages................................................ 12 - 66
12.13.4.5 PW3061/21 Sample Holder for Solid Samples.................................................. 12 - 66
12.13.4.6 PW3061/22 4-inch Wafer Holder ...................................................................... 12 - 67
12.13.4.7 9430 500 20351 Magnetic Ring......................................................................... 12 - 67
12.13.4.8 9430 500 20361 Sample Platform ..................................................................... 12 - 67
12.13.5 Use ..................................................................................................................................... 12 - 68
12.13.5.1 Sample Movement Using the Remote Control .................................................. 12 - 68
12.13.5.2 Sample Height Alignment Using the Dial Gauge.............................................. 12 - 69
12.13.5.3 Aligning the Sample Using X-rays .................................................................... 12 - 70
12.14 PW3076/00 Transmission Spinner ................................................................................ 12 - 72
12.14.1 Accessories ........................................................................................................................ 12 - 72
12.14.1.1 Sample Holder ................................................................................................... 12 - 72
12.14.1.2 PW18xx Circular Sample Holders..................................................................... 12 - 73
12.14.1.3 PW3714/20 Motor Supply ................................................................................. 12 - 73
12.14.2 Use ..................................................................................................................................... 12 - 73
12.14.2.1 Manually Loading a Sample .............................................................................. 12 - 73
12.15 PW3077/00 High-throughput Attachment ................................................................... 12 - 75
12.15.1 Accessories ........................................................................................................................ 12 - 78
12.15.1.1 Dial Gauge ......................................................................................................... 12 - 78
12.15.1.2 Multiple-sample Holder for Reflection Sample Mode ...................................... 12 - 79
12.15.1.3 Well Plate Holder for Transmission Sample Mode ........................................... 12 - 79
12.15.1.4 Direct Beam Stop............................................................................................... 12 - 80
12.15.1.5 PW3099/70 Large Offset Arm........................................................................... 12 - 83
12.15.2 Use ..................................................................................................................................... 12 - 83
12.15.2.1 Mounting the PW3077/00 High-throughput Attachment onto the X'Pert PRO Theta-
Theta System...................................................................................................... 12 - 83
12.15.2.2 Dismounting the PW3077/00 High-throughput Attachment from the X'Pert PRO
Theta-Theta system............................................................................................ 12 - 87
12.15.2.3 Changing Sample Mode..................................................................................... 12 - 89
12.15.2.4 Mounting and Aligning of a Well Plate Holder for Transmission Applications12 - 89
12.15.2.5 Mechanical Sample (Stage) Height Alignment ................................................. 12 - 90
12.15.2.6 Sample Height Alignment Using X-rays ........................................................... 12 - 91
12.15.2.7 Performing Measurements ................................................................................. 12 - 91
07.03.27 Page 12.3

Page 12.4 07.03.27

12.1 GENERAL
can be measured or analyzed. The sample platforms used on X'Pert PRO systems can be divided into six groups,
they are:
• the all-purpose MRD cradle described in Chapter 11.
• PreFIX sample stages for X’Pert PRO MPD systems described in this chapter.
• PreFIX high-throughput attachment described in this chapter.
• PreFIX non-ambient sample stages described in Chapter 13.
• PreFIX temperature controlled humidity chamber described in Chapter 13.
• PreFIX cryogenic temperature controlled sample stages described in Chapter 13.
Except for the MRD cradle (which is not removable), all of the sample stages are PreFIX mounted onto the
diffractometer and can be interchanged without needing re-alignment.
This chapter describes platforms that can be PreFIX mounted onto X’Pert PRO MPD systems. The various
platforms are all listed in Table 12.1. The section in which the sample stage is described is also indicated in the
table. Information about the use of the sample stage, mounting of the samples and finally alignment is given in
each section.
Table 12.1: Sample Platforms
Type
Sample Platform Types of Sample Section
Number
PW3062/00 Stage for Micro-diffraction Small (spots on) samples 12.2

PW3063/00 Capillary Spinner Samples in glass capillaries 12.3
PW3064/00 Spinner for PW18xx Sample Holders Samples fitted in circular sample holders 12.4
PW3064/60 Reflection/transmission Spinner for PW18xx Samples fitted in circular sample holders 12.5
Sample Holders
PW3067/00 Cradle for Transmission and Reflection Foils 12.6
PW3068/00 Texture Cradle Small textured samples 12.7
PW3069/00 Open Eulerian Cradle General solid samples 12.8
PW3070/00 Open Eulerian Cradle with General solid samples 12.9
X-translation
PW3071/60 Stage for Flat Samples/Holders Flat solids or powders in flat holders 12.10
PW3072/60 Stationary Stage for PW18xx Sample Holders Samples fitted in circular sample holders 12.11
PW3074/00 Multi-purpose Sample Stage Large or unusually shaped samples, or 12.12
flat solids, or powders in flat holders
PW3075/61 Positioning Stage with Motorized X, Y, Z, Tilt Thin films and small irregularly shaped 12.13.1
and Phi Movements samples
PW3075/62 Positioning Stage with Motorized Z, Tilt and Thin films and small irregularly shaped 12.13.2
Phi Movements samples
PW3075/63 Positioning stage with Motorized X, Y and Z Small irregularly shaped samples 12.13.3
Movements
PW3076/00 Transmission Spinner Foils, fibers, pharmaceuticals and other 12.14
low-absorbing materials
PW3077/00 High-throughput Attachment Samples in well-plates 12.15
07.03.27 Page 12.5

12.1.1 Exchanging PreFIX Sample Stages

Each sample stage has a PreFIX stage interface to mount the sample stage onto the goniometer.
The procedure for exchanging the PreFIX sample stages is supported by the data collector software.
Proceed as follows to exchange the PreFIX sample stages:

1. Move the arms of the goniometer to a position where you have easy access to the screws holding the
sample stage. At this time you also have the opportunity to remove any optical modules and/or the
sample if it is necessary.
2. Go off-line with the data collector software.
3. In the data collector software select the menu item Tools - Exchange Sample Stage and follow the
instructions given by the X’Pert Wizard “Exchange Sample Stage” that then appear. Note that you can
only do this when the instrument is off-line (disconnected). The manual actions that you need to
perform are described below.
4. Go on-line with the data collector software (using the configuration containing the sample stage you
have just mounted). The sample stage is now ready for use.
In the procedure described above, the X’Pert Wizard will instruct you to dismount the sample stage and to mount
the new sample stage. We will describe the general procedure for dismounting and mounting sample stages here.
A specific procedure for mounting PW3077/00 High-throughput Attachment is given in section 12.15.2. Specific
procedures for mounting PreFIX non-ambient chambers are given in sections 13.2.1.1, 13.4.3 and 13.5.2.
1. Loosen the four securing screws (see Figure 12.1) and remove the sample stage. If you have a
PW3062/00 Stage for Micro-diffraction, a PW3063/00 Capillary Spinner, or a PW3076/00
Transmission Spinner; make sure that the spinner motor is switched off. If necessary you can now
disconnect the cable from the (motorized) sample spinner and connect to the sample spinner that you
are now going to mount onto the goniometer.
2. Bring the new sample stage into position so that it fits over the PreFIX alignment blocks on the
goniometer (see Figure 12.2). The hinged clip at the top will hold the sample stage in position, allowing
you two hands free to tighten the securing screws.
3. Tighten the four securing screws.
Page 12.6 07.03.27

Figure 12.1: Loosening the Securing Screws
Hinged
Clip PreFIX
Alignment Blocks
Figure 12.2: Bringing the Sample Stage into Position over the PreFIX Alignment Blocks
07.03.27 Page 12.7

12.2 PW3062/00 STAGE FOR MICRO-DIFFRACTION

The PW3062/00 Stage for Micro-diffraction is designed to hold a goniometer head onto which a sample table
can be placed to mount small samples. The stage is shown in Figure 12.3. It can be PreFIX mounted onto an
X’Pert PRO goniometer. The stage is commonly used in combination with a mono-capillary as incident beam
PreFIX module in order to irradiate a small area on the sample, an X’Celerator or a PIXcel with an anti-scatter
device is used on the diffracted beam side. The sample can be rotated around its vertical axis in order to bring
more crystallites into the diffraction position to reduce the influence of particle statistics. The spinner is manually
operated by pressing the On/Off switch on the PW3914/20 Motor Supply. The spinner speed is 5 revolutions per
second. A sample with a maximum sample height of 5 mm and a mass of up to 50 g can be mounted onto the
table.
Sample Table
Goniometer
Head
Connection for
PW3714/20
Motor Supply
Figure 12.3: PW3062/00 Stage for Micro-diffraction with

9430 500 28351 Goniometer Head and Sample Table Mounted
12.2.1 Accessories
12.2.1.1 Set of Three Sample Tables
A set of three brass sample tables with a table diameter of 13 mm is included with the PW3062/00 Stage for
Micro-diffraction. The shaft of these tables can be inserted into the goniometer head mounted onto the stage. The
sample to be measured can be secured with adhesive material, for example: plasticine or double-sided adhesive
tape.
We advise you to mount very small, thin or transparent samples onto a glass slide, or a PW1817/32 or
PW1819/32 Zero Background Holder in order to prevent diffraction peaks from the sample table. The sample
together with its support can then be mounted onto the sample table.
Page 12.8 07.03.27

12.2.1.2 PW3714/20 Motor Supply

The PW3714/20 Motor supply is an electrical power supply unit for the spinner motor of the micro-diffraction
spinner. The unit is shown in Figure 12.4. It is manually operated by pressing the On-Off button on the housing.
The motor supply can also be used in conjunction with the PW3063/00 Capillary Spinner and the PW3076/00
Transmission Spinner. If you have more than one of these stages, you still only need to have one power supply
unit present in your system. You can switch the power supply from one stage to another by disconnecting the
cable from the spinner that you have used and then connecting it to the spinner that you are going to use next.
For more information about exchanging PreFIX sample stages, refer to section 12.1.1.
Figure 12.4: PW3714/20 Motor Supply
12.2.1.3 9430 500 28351 Goniometer Head

The 9430 500 28351 Goniometer Head can be fitted onto the PW3062/00 Stage for Micro-diffraction to enable
small samples to be mounted. The samples can be moved in the X and Y directions by ± 10 mm and the axial
position can be adjusted up to 3 mm. The sample can be aligned with the goniometer axis by means of the tilt
angle adjustment (±20°).
12.2.1.4 9430 500 28341 Alignment Microscope

The correct alignment of the sample with respect to the X-ray beam can be determined with the use of an
alignment microscope. The alignment microscope (9430 500 28341) is attached to a PreFIX microscope
interface (PW3019/10) which can be mounted on the diffracted beam PreFIX position on the PW3050/6x X’Pert
PRO Goniometer (with a radius of 200 mm or more). The alignment microscope has a cross-hair with a division
of 50 μm. The viewing diameter is 6 mm.
07.03.27 Page 12.9

Figure 12.5: 9430 500 28341 Alignment Microscope with

PW3019/10 PreFIX Microscope Interface
12.2.2 Use
12.2.2.1 Alignment Using an Alignment Microscope
You can align a micro-diffraction sample as follows:
1. Mount the prepared sample on the brass sample table and place this onto the goniometer head. Refer to
section 12.2.1.1 for sample mounting instructions.
2. Mount the micro-diffraction stage onto the X’Pert PRO goniometer.
3. Mount the goniometer head onto the micro-diffraction stage. Make sure that the pin on the micro-
diffraction stage corresponds to the hole in the goniometer head. Rotate the securing ring clockwise
until the goniometer head is fixed onto the micro-diffraction stage.
4. Mount the mono-capillary onto the incident beam PreFIX position, check that no collisions can occur
between the sample or the sample stage and the mono-capillary.
5. Mount the alignment microscope on the diffracted beam PreFIX position. Make sure that the alignment
microscope does not touch the other diffracted beam PreFIX module when mounted (only applicable
when two diffracted beam PreFIX positions are available).
6. Move the goniometer using the data collector software to such a position that you can observe the
sample from the side in order to check the correct height and tilt (for a Theta-Theta system: 2θ = 0º,
offset = 0º; for a Omega-2Theta system: 2θ = 96º, offset = 48º; for an Alpha-1 system: 2θ = 120º, offset
= 60º). You should now be able to look through the microscope when standing in front of the enclosure.
7. Look through the microscope and focus onto the edge of the sample. Using a sheet of white paper to
reflect the light, or using a light directed onto the sample helps to enhance the contrast.
Page 12.10 07.03.27

8. You can now start to align the sample:

a. Begin with the tilt adjustment on the goniometer head closest to the base of the goniometer. Rotate
the goniometer head in such a way that the tilt axis is parallel to the microscope's optical axis.
b. Adjust the tilt until the sample surface is lined up with the cross-hair of the ocular of the
microscope.
c. Check the correct alignment by rotating the goniometer head around its axis back and forth
between 0º and 180º and comparing the position of the sample surface. If the two situations do not
correspond, it may well be that the cross-hair of the microscope is not correctly oriented.
9. Repeat the previous step with the other tilt adjustment.
10. Switch the micro-diffraction stage spinner motor on and check the sample to see if it wobbles at all. If it
does wobble, repeat steps 8 and 9. When you are satisfied, switch the spinner motor off.
11. Adjust the height of the sample until its edge matches the cross-hair of the microscope.
12. Move the goniometer (using the data collector software) to such a position that you can observe the
sample from the top in order to find the position on the sample that you want to analyze (for a Theta-
Theta system: 2θ = 90º, offset = -45º; for an Omega-2Theta system: 2θ = 96º, offset = -42º; for an
Alpha-1 system: 2θ = 120º, offset = -30º). Align the sample using the translational movements of the
goniometer head. The center of the area that will be measured corresponds to the cross-hair of the
microscope.
13. Replace the alignment microscope with the PreFIX module that you want to use for the X-ray
experiment. You are now ready to start collecting data!
CAUTION The end of the mono-capillary is close to the sample. As a result of

this, there is a chance for a collision between the sample or sample
cradle and the mono-capillary. Before collecting data, make sure
that there is no chance for such a collision at any ω angle that is
used in your program(s). Also disable the automatic reset of the
instrument in the data collector software.
07.03.27 Page 12.11

12.3 PW3063/00 CAPILLARY SPINNER

The PW3063/00 Capillary Spinner is designed to hold a goniometer head into which a capillary sample can be
placed. It is shown in Figure 12.6. It can be PreFIX mounted onto an X’Pert PRO goniometer. The purpose of
the capillary samples is to allow the accurate measurement of small amounts of powders, or powders which
should not be exposed to air, or which are dangerous to the operator’s health. The spinning rotation around the
axis of the sample is to bring more crystallites into the diffraction position in order to reduce the influence of
particle statistics on the measurements.
The capillary spinner can also be used together with the Oxford Cryosystems Cryostream Plus in order to
measure capillary samples at non-ambient temperatures. How to use the capillary spinner at non-ambient
temperatures is described in section 13.4 of Chapter 13 in Part II of this User’s Guide.
The spinner revolves at around 5 revolutions per second. The capillary spinner is manually operated by pressing
the On/Off switch on the PW3714/20 Motor Supply. We advise that the capillary sample diameters are between
0.3 mm and 0.5 mm.
Goniometer
Head
Connection for
PW3714/20
Motor Supply
Figure 12.6: PW3063/00 Capillary Spinner with 9430 500 28351 Goniometer Head
12.3.1 Accessories
The PW3714/20 Motor supply is an electrical power supply unit for the spinner motor of the micro-diffraction
spinner. The unit is shown in Figure 12.4. It is manually operated by pressing the On-Off button on the housing.
The motor supply can also be used in conjunction with the PW3062/00 Stage for Micro-diffraction and the
PW3076/00 Transmission Spinner. If you have more than one of these stages, you still only need to have one
power supply unit present in your system. You can switch the power supply from one stage to another by
disconnecting the cable from the spinner that you have used and then connecting it to the spinner that you are
going to use next. For more information about exchanging PreFIX sample stages, refer to section 12.1.1.
Page 12.12 07.03.27

12.3.1.2 9430 500 28351 Goniometer Head

The 9430 500 28351 Goniometer Head can be fitted onto the PW3063/00 Capillary Spinner to enable capillary
samples to be mounted. The samples can be moved in the X and Y directions by ± 10 mm and the axial position
can be adjusted up to 3 mm. The sample can be aligned with the goniometer axis by means of the tilt angle
adjustment (±20°).
12.3.1.3 9430 500 28341 Alignment Microscope

The correct alignment of the capillary with respect to the X-ray beam can be determined with the use of an
alignment microscope which is shown in Figure 12.5. The alignment microscope (9430 500 28341) is attached
to a PreFIX microscope interface (PW3019/10) which can be mounted on the diffracted beam PreFIX position
on the PW3050/6x X’Pert PRO Goniometer (with a radius of 200 mm or more). The alignment microscope has
a cross-hair with a division of 50 μm. The viewing diameter is 6 mm.
12.3.2 Use
This section describes the alignment of the capillary with respect to the incident X-ray beam. The preparation
of powder samples in glass capillaries is described in Appendix A of this User’s Guide.
Align a glass capillary on the capillary spinner stage as follows:
1. Mount the prepared glass capillary in the goniometer head. Adjust the shifts and tilts of the goniometer
head by visual inspection until the capillary is centered and in a vertical position using the special key
delivered with the goniometer head.
2. Mount the capillary spinner stage onto the X’Pert PRO goniometer.
3. Mount the incident beam optical module onto the incident beam PreFIX position.
4. Mount the alignment microscope on the diffracted beam PreFIX position. Make sure that the alignment
microscope does not touch the other diffracted beam PreFIX module when mounted (only applicable
when two diffracted beam PreFIX positions are available). Move the diffracted beam arm using the
data collector software to such a position that the arm points upwards (for a Theta-Theta system:
2θ = 90º; offset = -45º for an Omega-2Theta system: 2θ = 96º, offset = -42º; for an Alpha-1 system:
2θ = 120º, offset = -30º). You should now be able to look through the microscope when standing in
front of the enclosure.
5. Mount the goniometer head onto the capillary spinner stage. Make sure that the pin on the capillary
spinner stage corresponds to the hole in the goniometer head. Rotate the securing ring clockwise until
the goniometer head is fixed onto the capillary spinner stage.
6. Look through the microscope and focus onto the glass capillary. Using a sheet of white paper to reflect
the light, or using a light directed onto the glass capillary helps to enhance the contrast.
7. You can now start the alignment of the glass capillary:
a. Begin with the tilt adjustment on the goniometer closest to the base of the goniometer. Rotate the
goniometer head in such a way that the tilt axis is parallel to the microscope's optical axis.
b. Adjust the tilt until the glass capillary is lined up with the cross-hair of the ocular of the
microscope.
c. Check the correct alignment by rotating the goniometer head back and forth between 0º and 180º
and comparing the position of the glass capillary. If the two situations do not correspond, it may
well be that the cross-hair of the microscope is not correctly oriented.
d. After adjusting the tilt, adjust the corresponding shift.
8. Repeat the previous step with the other tilt and shift adjustments.
9. Switch the capillary spinner stage spinner motor on and check to see if the capillary wobbles. If it does
wobble, repeat the steps 7 and 8. When you are satisfied, switch the spinner motor off.
10. Replace the alignment microscope with the PreFIX module that you want to use for the X-ray
experiment. You are now ready to start collecting data!
07.03.27 Page 12.13
12.4 PW3064/00 SAMPLE SPINNER

The PW3064/00 Sample Spinner is designed to spin samples fitted in PW18xx sample holders about their axis.
The sample spinner is shown in Figure 12.7. It can be PreFIX mounted onto a vertical X’Pert PRO goniometer.
The purpose of spinning is to bring more crystallites into the diffraction position in order to reduce the influence
of particle statistics on the measurements. Spinning gives better results, especially in phase analysis and omega-
stress measurements compared to “static” measurements.
The spinner rotation speed can be set at 2, 1, 1/2, 1/4, 1/8 and 1/16 revolutions per second. The maximum sample
mass (including the sample holder) is 150 g.
If the spinner includes a loading handle the spinner lift is manually operated; otherwise, the spinner lift is
operated using the data collector software.
When the sample spinner is used in combination with a PW3065/xx Sample Changer, the lift operation is
motorized and can be controlled with the data collector software.
When a sample is correctly fitted into a PW18xx Sample Holder and loaded into the PW3064/00 Sample Spinner
it is automatically adjusted to the correct sample height. The reference plane of the PW18xx Sample Holder is
flush with that of the sample spinner.
Position for
Loading
a Circular
Handle
Sample Holder
Figure 12.7: PW3064/00 Sample Spinner
Page 12.14 07.03.27

12.4.1 Accessories
12.4.1.1 Sample Holder
One circular sample holder is included with the PW3064/00 Sample Spinner. The sample holder is physically
the same as the PW1813/32 Sample Holder for Circular Samples. It is used to mount filters or solid samples with
a diameter between 30 mm and 32.3 mm and a maximum thickness of 6 mm. The circular silicon pressed powder
sample delivered with the X’Pert PRO diffraction system fits into this holder. More details about this type of
sample holder are given in Appendix A of this User’s Guide (section A.2.1.4).
12.4.1.2 PW18xx Circular Sample Holders

The PW18xx Sample Holders are circular sample holders that can be loaded in the PW3064/00 Sample Spinner.
These sample holders can also be used with the PW3072/60 Stationary Sample Stage, on the PW3074/00 Multi-
purpose Sample Stage, on the PW3076/00 Transmission Spinner and on the PW3061/21 Sample Holder for
Solid Samples to be used with the PW3060/20 MRD cradle. A description of the PW18xx Sample Holders and
their applications is given in Appendix A of this User’s Guide.
12.4.1.3 PW3064/10 Beam Knife for Sample Spinner

The PW3064/10 Beam Knife for Sample Spinner can be mounted onto the PW3064/00 Sample Spinner in
order to improve the peak-to-background ratio in measurements using the PW3015/x0 X’Celerator or the
PIXcel.
The height of the beam knife above the sample can be adjusted so that the gap between the sample and the knife
is between 0.5 and 5 mm. More information about using this type of beam knife is given in section 14.3.1 in
12.4.1.3.1 Mounting the Beam Knife onto the Sample Spinner
Mount the beam knife onto the sample spinner as follows:

1. Unlock the black knurled knob at the rear of the beam knife holder and set the knife in its highest
position. Lock the black knurled knob.
2. Bring the beam knife holder into its position on the sample spinner as shown in Figure 12.8.
3. Fix the beam knife holder to the spinner using the two M3 x 10 screws with black knurled knobs
supplied.
The beam knife is now ready for use. Instructions on how to choose the optimum height of the knife above the
sample are given in section 14.3.6 in Chapter 14 in Part II of this User’s Guide.
07.03.27 Page 12.15

Figure 12.8: PW3064/10 Beam Knife Mounted onto a PW3064/00 Sample Spinner
12.4.1.4 PW3065/xx PreFIX Sample Changer

The PW3064/00 Sample Spinner can be automatically loaded and unloaded if your system includes a
PW3065/xx PreFIX Sample Changer. These sample changers contain sample magazines that can be loaded with
PW18xx Sample Holders. Using a sample changer makes it possible for the system to run batches of routine
measurements. More information about the PreFIX sample changers is given in Chapter 15 in Part II of this
User’s Guide.
12.4.2 Manually Loading a Sample

A sample fitted into a PW18xx Sample Holder can be manually loaded onto a PW3064/00 Sample Spinner as
follows:
1. Pull the loading handle on the right-hand side of the spinner towards you to bring the sample position to
the loading situation. If there isn’t a loading handle on the spinner you can move the sample lift
downwards using the data collector software.
2. Place the sample holder onto its position on the sample spinner (indicated in Figure 12.7).
3. Push the loading handle into the upright position, or use the data collector software to lift the sample
holder into its reference position. Check that the sample holder is positioned correctly so that the
reference surface of the sample holder is flush with the reference plane of the sample spinner.
If the sample holder is not inserted correctly, the sample will tilt during a spinning measurement. This will cause
a sample height displacement resulting in defocusing and thus peak broadening and a weakening of the peak
intensity.
Page 12.16 07.03.27
12.5 PW3064/60 REFLECTION - TRANSMISSION SPINNER

The PW3064/60 Reflection-transmission Spinner is a PreFIX sample stage that is designed for reflection and
transmission applications. The sample spinner is shown in Figure 12.9. It can be PreFIX mounted onto a vertical
X'Pert PRO goniometer. Samples fitted in PW18xx sample holders can be used with this spinner.
Figure 12.9: PW3064/60 Reflection-transmission Spinner
The PW3064/60 Reflection-transmission Spinner can be operated in two rotation modes:

1. The spinning mode, in which the samples are rotated around their axis. The purpose of spinning is to
bring more crystallites into the diffraction position in order to reduce the influence of particle statistics
on the measurements. Spinning gives better results, especially in phase analysis and omega-stress
measurements compared to “static” measurements. The spinner rotation speed can be set at 2, 1, 1/2,
1/4, 1/8 and 1/16 revolutions per second.
2. The phi axis mode, in which the sample can be automatically positioned or scanned along the phi axis,
that is the central axis of the spinner.
Which of the rotation modes used in a measurement is selected in the data collector software.
The PW3064/60 Reflection-transmission Spinner can be used in reflection and transmission sample modes.
1. Reflection Sample Mode: The (flat) sample is partially penetrated by the incident beam. The
diffracted beam leaves the sample on the same side as the incident beam entered. At an Omega setting
of 0°, the incident beam is parallel to the sample surface.
2. Transmission Sample Mode: The (flat) sample is completely penetrated by the incident beam. The
diffracted beam leaves the sample at the opposite side to the incident beam. At an Omega setting of 0°,
the incident beam is perpendicular (90º) to the sample surface.
Changing sample modes is described in section 12.5.2.2 below.
07.03.27 Page 12.17

The specifications of the PW3064/60 Reflection-transmission Spinner are given in Table 12.2.
Table 12.2: PW3064/60 Reflection-transmission Spinner - Specifications
Adjustable Axis Phi
Range n x (0º - 360º)
Minimum step size 0.1º
Accuracy ± 0.1º
Reproducibility ± 0.1º
The maximum sample mass (including the sample holder) is 150 g.
The spinner lift is motorized and is operated using the data collector software. Samples can be loaded when the
spinner stage is in its lower position.
The sample spinner can be used in combination with a PW3065/x1 Sample Changer.
When a sample is correctly fitted into a PW18xx Sample Holder and loaded into the PW3064/60 Sample Spinner
it is automatically adjusted to the correct sample height. The reference plane of the PW18xx Sample Holder is
flush with that of the sample spinner.
12.5.1 Accessories
A circular sample holder is included with the PW3064/60 Reflection-transmission Spinner. The sample holder
is physically the same as the PW1813/32 Sample Holder for Circular Samples. It is used to mount filters or solid
samples with a diameter between 30 mm and 32.3 mm with a maximum thickness of 6 mm. The circular silicon
pressed powder sample delivered with the X'Pert PRO diffraction system fits into this holder. More details about
this type of sample holder are given in Appendix A of this User's Guide (section A.2.1.4)

The PW18xx Sample Holders are circular sample holders that can be loaded in the PW3064/60 Reflection-
transmission Spinner. These sample holders can also be used with the PW3072/60 Stationary Sample Stage, on
the PW3074/00 Multi-purpose Sample Stage, on the PW3076/00 Transmission Spinner and on the PW3061/21
Sample Holder for Solid Samples to be used with the PW3060/20 MRD cradle. A description of the PW18xx
Sample Holders and their applications is given in Appendix A of this User's Guide.
12.5.1.3 PW3064/10 Beam Knife for Sample Spinner

The PW3064/10 Beam Knife for Sample Spinner can be mounted onto the PW3064/60 Reflection-transmission
Spinner in order to improve the peak-to-background ratio in measurements using the PW3015/x0 X'Celerator or
the PIXcel in reflection sample mode. The height of the beam knife above the sample can be adjusted so that the
gap between the sample and the knife is between 0.5 and 5 mm. More information about using this type of beam
knife is given in section 14.3.1 in Chapter 14 in Part II of this User's Guide.
Page 12.18 07.03.27

12.5.1.3.1 Mounting the Beam Knife onto the Reflection-transmission Spinner
Mount the beam knife onto the sample spinner as follows:

1. Undo the black knurled knob at the rear of the beam knife holder and set the knife in its highest position
and then tighten the black knurled knob.
2. Bring the beam knife holder into its place on the reflection-transmission spinner as shown in Figure
12.10.
supplied with the spinner.
sample are given in section 14.3.6 in Chapter 14 in Part II of this User's Guide.
Figure 12.10: PW3064/10 Beam Knife Mounted onto a PW3064/60 Reflection-transmission Spinner
CAUTION When a beam knife is mounted on the spinner you must make sure
that you do not automatically change from reflection to
transmission sample mode. This is because it is possible that
collisions between the beam knife and incident or diffracted beam
modules could occur.
07.03.27 Page 12.19

12.5.1.4 PW3064/20 Direct Beam Stop for Reflection-transmission Spinner

The PW3064/20 Direct Beam Stop can be mounted onto the reflection-transmission spinner in order to allow
transmission measurements using the PW3152/63 Focusing X-ray Mirror with a minimum 2theta angle in the
range from 1° to 2.5°. The maximum 2theta angle in the measurement is 43°. The direct beam stop, mounted
onto the PW3064/60 Reflection-transmission Spinner is shown in Figure 12.11.
Figure 12.11: PW3064/20 Direct Beam Stop Mounted onto a PW3064/60 Reflection-transmission
Spinner
12.5.1.4.1 Mounting the Direct Beam Stop onto the Reflection-transmission Spinner
Mount the direct beam stop onto the reflection-transmission spinner as follows:
1. Bring the beam stop into its position on the reflection-transmission spinner, so that the two pins on the
spinner fit into the holes on the beam stop, see Figure 12.11.
2. Fix the direct beam stop to the spinner using the M3 x 16 screw supplied.
Now you can proceed with aligning the direct beam stop.
12.5.1.4.2 Aligning the Direct Beam Stop

The height setting of the beam stop is adjustable. Align the beam stop as follows:
1. If one is present, remove the sample from the sample stage.
2. Ensure that the X-ray tube is in line focus position and that the tube height is correctly aligned. Refer to
Chapter 1 of Part II of this User's Guide.
3. Ensure that the direct X-ray beam passes through 2θ = 0°. Use a beam attenuator to protect your
detector from being saturated. Also, makes sure that the beam is not blocked by a beam stop or the
sample stage.
4. Set the high-tension generator to 45 kV, 40 mA.
5. Mount the focusing X-ray mirror onto the incident beam PreFIX position of the X'Pert PRO MPD
system.
Page 12.20 07.03.27

6. Insert a 1/2° divergence slit, a 1/2° or a 1/4° anti-scatter slit (the one that you are going to use in your
experiments) and a 0.04 rad or smaller Soller slits assembly into their appropriate positions in the
focusing X-ray mirror.
7. If you are using an X'Celerator or a PIXcel, set it to scanning mode; if you are using a PW3093/60
Programmable Receiving Slit, set it to 0.1 mm. If a programmable anti-scatter slit is mounted onto the
X'Celerator or the PIXCel or the programmable receiving slit, set it to 1/32° . If you have a fixed anti-
scatter device mounted onto the X’Celerator or the PIXcel, use the advised combination given in Table
6.12 and Table 6.13 in Chapter 6 of Part II of this User’s Guide.
8. Set ω = 0° and make a 2θ scan around 2θ = 0°, for example: from -1° to 3° 2θ. Use the same scan type
and omega-offset that you are going to use in the experiments that you are going to perform. A typical
result of this scan is shown in Figure 12.12.
Intensity [cps]
3600
1600
400
0
-0.8 -0.6 -0.4 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8
2theta [deg.]
Figure 12.12: Typical Scan Around 2θ = 0°

9. Now one of the following situations applies:
a. If your scan shows a narrow peak around 0.8º 2θ, a background intensity that is 5 to 10 times lower
than the peak height and a flat background from 1° to 3° 2θ as shown in Figure 12.12, then your
beam stop is correctly aligned. You can skip the steps given below.
b. If your scan does not show a peak (that is, the edge of the direct beam) then your beam stop is set
too high and must be lowered.
c. If your scan shows a broad line, or an irregular background around 2º 2θ, then your beam stop is
set too low and must be raised.
10. Slightly loosen the two mounting screws that fix the beam stop onto the assembly.
11. Depending on the result obtained in step 9, follow the procedure given in step a or b below:
a. In order to lower the beam stop: use a 1.5 Allen key to loosen the upper setscrew by turning it
about 45° (or less for smaller steps) and then tighten the lower setscrew by the same amount. Make
a new scan with the same settings as in step 8 and repeat this procedure until your scan looks like
the scan shown in Figure 12.12.
07.03.27 Page 12.21

b. In order to raise the beam stop: use a 1.5 Allen key to loosen the lower setscrew by turning it about
45° (or less for smaller steps) and then tighten the upper setscrew by the same amount. Make a new
scan with the same settings as in step 8 and repeat this procedure until your scan looks like the scan
12. Fix the two mounting screws.
This completes the beam stop alignment. Your system is now ready for use.
12.5.1.5 PW3065/xx PreFIX Sample Changer

The PW3064/60 Reflection-transmission Spinner can be automatically loaded and unloaded if your system
includes a PW3065/xx PreFIX Sample Changer. These sample changers contain sample magazines that can be
loaded with PW18xx Sample Holders. Using a sample changer makes it possible for the system to run batches
of routine measurements. More information about the PreFIX sample changers is given in Chapter 15 in Part II
of this User's Guide.
12.5.1.6 PW3099/70 Large Offset Arm

The PW3099/70 Large Offset Arm is an accessory that is used to support the transmission sample mode on
X'Pert PRO Theta-Theta systems equipped with a the PW3064/60 Reflection-transmission Spinner or a
PW3077/00 High-throughput Attachment. It is designed as a PreFIX module with an offset of approximately
-60° 2θ. It is mounted on the goniometer's diffracted beam PreFIX position and provides a position to mount a
diffracted beam PreFIX module The PW3099/70 Large Offset Arm is shown in Figure 12.13. The large-offset
arm mounted onto an X'Pert PRO goniometer is shown in Figure 12.14.
Figure 12.13: PW3099/70 Large Offset Arm

Page 12.22 07.03.27
12.5.2 Use
12.5.2.1 Manually Loading a Sample
A sample fitted into a PW18xx Sample Holder can be manually loaded onto a PW3064/60 Reflection-
transmission Spinner as follows:
1. Move the sample lift down using the data collector software to bring the sample position to the loading
situation.
2. Place the sample holder onto its position on the sample spinner (indicated in Figure 12.9).
3. Move the sample lift up so that the sample holder is brought into its reference position.
4. Check that the sample holder is positioned correctly so that the reference surface of the sample holder is
flush with the reference plane of the sample spinner. If the sample holder is not inserted correctly, the
sample will tilt during a spinning measurement. This will cause a sample height displacement resulting
in defocusing and thus peak shift and broadening and a weakening of the peak intensity.
12.5.2.2 Changing Sample Modes

The PW3064/60 Reflection-transmission Spinner can be used in reflection or in transmission mode. Changing
from one sample mode to another is done by setting the required sample mode in the data collector software.
The actions that are executed automatically or manually depend on the type of X'Pert PRO MPD system and on
the sample mode that you are going to use. These actions are given in Table 12.3.
Table 12.3: Overview of Actions Required on Changing the PW3064/60 Reflection-transmission Spinner
Sample Mode
X'Pert PRO Changing Sample Action Perormed by the

Manual Actions
System Mode Data Collector Software
Omega-2Theta From reflection to Rotate omega axis +90° -

or transmission
Alpha-1 From transmission to Rotate omega axis -90° -
reflection
Theta-Theta From reflection to Move incident beam arm +90°, Mount large offset arm and
transmission move 2theta arm -30° make sure that is announced
as an accessory in the
diffracted beam path in the
data collector software.
From transmission to Move incident beam arm -90°, Dismount large offset arm and
reflection move 2theta arm +30° make sure that is removed
from the diffracted beam path
in the data collector software.
NOTE: The large offset arm can also be used in reflection mode; in this case the maximum 2theta angle
obtainable is decreased by 60° 2θ.
07.03.27 Page 12.23

Figure 12.14: X'Pert PRO Theta-Theta System in Reflection Sample Mode
Figure 12.15: X'Pert PRO Theta-Theta System in Transmission Sample Mode
Page 12.24 07.03.27

12.6 PW3067/00 AUTOMATIC PHI CRADLE ATC-1

The PW3067/00 Automatic Phi Cradle ATC-1 is designed for transmission and reflection applications. The
cradle is shown in Figure 12.17. It can be PreFIX mounted onto an X’Pert PRO goniometer. Thin samples and
foils can be mounted onto this cradle. The open area in the center of the cradle has a diameter of 34 mm. The
reference plane, perpendicular to the diffraction plane containing the goniometer axis, coincides with the flat
side of the central part of the cradle.
The sample can be automatically infinitely rotated around a phi axis. The specifications of the Automatic Phi
Cradle are given in Table 12.3.
Table 12.4: PW3067/00 Automatic Phi Cradle - Specifications
Adjustable Axis Phi
Range n x (0º - 360º)

Minimum step size 0.1º
Accuracy ± 0.05º
Reproducibility ± 0.05º
Slew speed 20º per second
12.6.1 Use
Figure 12.16: PW3067/00 Automatic Phi Cradle ATC-1 in Transmission Sample Mode
- Mode Changing Screws
07.03.27 Page 12.25

The PW3067/00 Automatic Phi Cradle ATC-1 can be used in reflection or in transmission mode. Change from
one sample mode to another is performed by setting the sample mode required in the data collector software. The
actions that are executed automatically or manually depend on the type of X'Pert PRO MPD system and on the
sample mode that you are going to use. These actions are given in Table 12.5.
Table 12.5: Overview of Actions Required on Changing the Sample Mode of the PW3067/00 Automatic
Phi Cradle ATC-1
X'Pert PRO Changing Sample Action Performed by the

Manual Actions
System Mode Data Collector Software
Omega-2Theta From reflection to Rotate omega axis +90° -

or transmission
Alpha-1 From transmission to Rotate omega axis -90° -

reflection
Theta-Theta From reflection to - Rotate ATC-1 cradle on its
transmission axis 90° counter-clockwise,
move 2theta arm -30°
From transmission to - Rotate ATC-1 cradle on its

reflection axis 90° clockwise
Rotating the ATC-1 cradle on its axis is described in section 12.6.1.2.
12.6.1.2 Rotating the ATC-1 Cradle on its Axis

In order to change the ATC-1 sample mode on an X'Pert PRO Theta-Theta system you must rotate the ATC-1
cradle on its axis with respect to the PreFIX interface through 90°. You do that as follows:
1. Remove the screw marked Y in Figure 12.16.
2. Loosen the setscrew (also shown in Figure 12.16).
CAUTION
Do not touch the alignment screw (shown in Figure 12.16) as this
screw is factory aligned and will disturb the sample’s position if
moved.
3. Carefully pull the alignment block a little distance (just under 1 cm) away from the PreFIX Interface,
turn the cradle:
a. through 90º counter-clockwise when you are changing the cradle position from reflection to
transmission mode,
or
b. through 90º clockwise when you are changing the cradle position from transmission to reflection
mode;
and then push it back against the PreFIX Interface.
4. Put back the screw (Y) that you removed in step 1, and loosely tighten it.
5. Tighten the setscrew and then tighten screw Y.
Figure 12.17 shows the ATC-1 cradle in the reflection mode position.
Page 12.26 07.03.27

Figure 12.17: PW3067/00 Automatic Phi Cradle ATC-1 in Reflection Sample Mode
- Sample Mounting Screws
12.6.1.3 Mounting a Sample onto the ATC-1

There are three different options for mounting a sample onto the PW3067/00 Automatic Phi Cradle ATC-1, they
are:
Option 1:
Put the sample (with sample holder) on the sample mounting area in the central part of the cradle.
Clamp the sample by tightening the two setscrews (M2 x 4) at the side of the sample holder. The
position of the setscrews is shown in Figure 12.17. The maximum sample (holder) diameter is 34 mm.
The sample holder must be 3.0 mm thick.
Option 2:
Put the sample (with sample holder) on the sample mounting area in the central part of the cradle and
clamp it with two screws (M2 x 6) and washers using the screw holes just outside the sample mounting
area. These screw holes are indicated in Figure 12.17. The sample holder must have a diameter of 34
mm and be 3.0 mm thick.
Option 3:
Put the sample (with sample holder) on the sample mounting area in the central part of the cradle and
clamp it with two screws (M2 x 6) and washers using the screw holes in the sample mounting area.
These screw holes are indicated in Figure 12.17. This option requires a circular sample holder with a
diameter of 34 mm and a maximum thickness of 3.0 mm which has two (diametrically opposite) holes
drilled in it. These holes must be 27 mm ± 0.1 mm apart and have a diameter of 2.4 mm ± 0.1 mm.
07.03.27 Page 12.27

12.7 PW3068/00 AUTOMATIC TEXTURE CRADLE ATC-3

The PW3068/00 Automatic Texture Cradle ATC-3 is designed for general texture analysis in the Schulz
reflection geometry. It is shown in Figure 12.18. It can be PreFIX mounted onto an X’Pert PRO goniometer.
Samples that have a maximum diameter of 32 mm (42 mm when not translated or oscillated), a maximum height
of 10 mm and a maximum mass of 30 g can be analyzed using this cradle.
The samples can be mounted onto a circular table which can then be mounted into a phi rotation table. Both the
sample table and the phi rotation table have an alignment mark that allows you to align the sample to be analyzed
in a specific direction. The reference plane for sample height adjustment is indicated by a height adjustment pin
(see Figure 12.18).
The sample can be rotated over 360° around a phi axis, tilted around a psi axis from -90° to +90º and translated
over a maximum distance of 10 mm in the Y direction (along the goniometer axis). It is also possible to oscillate
over 5 or 10 mm in the Y direction in order to bring more crystallites into the diffraction position during a
measurement. An overview of the specifications of the axes is provided in Table 12.5.
Table 12.6: Specifications of the Adjustable Axes on the ATC-3 Cradle
Axis Phi Psi Y Z
Adjustable Automatic Automatic Automatic Manual
Range 0º to 360º -90º to +90º Oscillation over 5 mm 0 to 10 mm

or 10 mm
Minimum step size 0.1º 0.1º - -
Accuracy ± 0.05º ± 0.05º - ± 50 μm

Reproducibility ± 0.05º ± 0.05º - ± 50 μm
Slew speed 20º per second 10º per second - -
Height
Adjustment
Pin Sample
Table
Figure 12.18: PW3068/00 Automatic Texture Cradle ATC-3
Page 12.28 07.03.27

12.7.1 Use
The procedure for mounting and adjusting the height of the sample is as follows:
1. Move the diffracted beam optics out of the way, using the data collector software, to provide more
working space.
NOTE: This step is optional but advised. Moving the secondary beam optics allows more working space.
2. Mount the sample onto the sample table and secure it with plasticine or double-sided adhesive tape. If
the sample is very light in weight it can be secured with an acid free grease. If the sample cannot be
secured by these methods experiment with other ways of fixing the sample to the sample table.
3. Place the sample table, with sample already mounted, in the hole in the center of the phi rotation table,
see Figure 12.19.
4. Make sure that the sample is pushed far enough down to allow the height adjustment pin to be moved to
the vertical position.
5. Move the height adjustment pin to the vertical position so that the sample table shaft and the height
adjustment pin are in line.
6. Pull the sample table up until the sample surface just touches the height adjustment pin.
NOTE: The sample table and the phi rotation table are both marked to allow you to align the sample in a
specific direction. We advise you to mount the sample with its reference direction (RD) oriented
towards the alignment mark on the sample table. When the alignment on the sample table is then
aligned with the alignment mark on the phi rotation table, the reference direction (RD) on a pole
figure is along the ϕ = 0º direction.
7. Turn the height adjustment pin clear of the sample, ensuring that the pin does not scrape the sample
surface and does not touch the inner cylinder of the ATC-3.
The sample is now aligned and ready for measurement.
Height
Adjustment
Pin
Sample Table
Alignment Mark on
the Sample Table
Alignment Mark
on the Phi
Rotation Table
Hole for Sample

Table Pin
Figure 12.19: Adjusting Sample Height

07.03.27 Page 12.29
12.8 PW3069/00 OPEN EULERIAN CRADLE

The PW3069/00 Open Eulerian Cradle is a sample stage used for texture, omega-stress analysis and parallel
beam applications. The cradle is shown in Figure 12.20. It can be PreFIX mounted onto an X’Pert PRO
goniometer. Samples with a maximum diameter of 100 mm, a maximum height of 25 mm, and a maximum mass
of 150 g can be mounted onto this cradle. Several sample mounting platforms are available for the open Eulerian
cradle.
The type of sample mounting platform to be used depends on the sample to be analyzed. Details about the sample
mounting platforms and their specific reference planes for sample height alignment are given in section 12.8.1.
When a sample is mounted onto the cradle it can be rotated over ϕ range of n x 360° and tilted over a ψ range
from -5° to +95°. A manual Z translation is available as an accessory; it is described in section 12.8.1.3.
An overview of the specifications of the axes on the PW3069/00 Open Eulerian Cradle is given in .
Open Eulerian
Cradle
Phi-ring
Dial Gauge Holder

(Optional)
Double Knife
Edge
Alignment Tool
Wafer Holder
Multi-purpose
Sample Holder
Figure 12.20: PW3069/00 Open Eulerian Cradle and Sample Holders
Page 12.30 07.03.27

Table 12.7: Specifications of the Adjustable Axes on the Open Eulerian Cradle
Axis Phi Psi Z*
Adjustable Automatic Automatic Manual
Range n x (0º - 360º) -5º to +95º 0 - 12 mm
Minimum step size 0.01º 0.01º -

Accuracy ± 0.05º ± 0.05º ± 10 μm
Reproducibility ± 0.05º ± 0.05º ± 5 μm
Slew speed 10º per second 5º per second -
* = The Z translation is optional
12.8.1 Accessories
12.8.1.1 Multi-purpose Sample Holder
A multi-purpose sample holder is delivered as an accessory to the open Eulerian cradle. It is shown in Figure
12.20. It is used to mount unusually shaped samples onto the open Eulerian cradle. The maximum sample
diameter is 55 mm; the maximum sample height is 25 mm. The reference plane for sample height adjustment is
given by the top surface of the three metal rods attached to the sample holder.
12.8.1.1.1 Mounting a Sample onto the Multi-purpose Sample Holder
To mount a sample in the Multi-purpose Sample Holder lay the sample face down on a flat surface, extend the
three spring loaded fingers to the rim of the holder and then move the fingers inward to grab the sample.
Spring-loaded
Finger
Metal Rod
Figure 12.21: Mounting a Sample onto the Multi-purpose Sample Holder
07.03.27 Page 12.31

12.8.1.1.2 Mounting the Multi-purpose Sample Holder
The multi-purpose sample holder can be mounted onto the PW3069/00 Open Eulerian Cradle as follows:
1. Place the multi-purpose sample holder in position on the phi ring of the Open Eulerian Cradle.
2. Apply enough pressure onto the sample stage to click it into place.
The sample stage is now ready for use.
12.8.1.2 Wafer Holder

The Wafer Holder is included with the open Eulerian cradle. It is shown in Figure 12.20. It is used to mount
wafers with a thickness of 0.35 mm and a maximum diameter of 100 mm (4 inch). Wafers can be mounted onto
the wafer holder with an adhesive, for example: double-sided adhesive tape or plasticine.
The wafer holder is designed so that when a 0.35 mm thick wafer is mounted it is automatically aligned for the
correct sample height.
12.8.1.2.1 Mounting the Wafer Holder
The wafer holder can be mounted onto the PW3069/00 Open Eulerian Cradle as follows:
1. Place the wafer holder in its position on the phi ring of the Open Eulerian Cradle.
2. Apply enough pressure onto the sample stage to click it into place.
12.8.1.3 PW3069/10 Manual Z Translation Stage

In addition the cradle can have an option called a manual Z translation stage that will allow you to adjust the
sample height relative to the diffractometer axis (diffraction plane). Translating the sample also in Z direction
over 10 mm allows you to easily adjust the sample height to the diffractometer axis (diffraction plane).
The manual Z translation stage mounted onto an open Eulerian cradle is shown in Figure 12.22. A dial gauge
used for accurate reading of the sample height is included with the Z translation stage, it can be mounted onto
the dial gauge holder which is factory mounted onto the open Eulerian cradle. The Z translation stage itself can
be mounted onto the open Eulerian cradle. Mounting instructions are given in section 12.8.1.3.1. Specifications
of the Z translation stage are included in . The Z translation stage can hold samples with maximum dimensions
of 10 mm thickness and 160 mm diameter. The maximum sample mass is 75 g. The samples can be mounted
onto the stage with an adhesive, for example: double-sided adhesive tape or plasticine. If your sample is more
than 10 mm thick, you can remove the central disk from the Z translation stage to create more space to mount
your sample. How to remove the central disk is described in section 12.8.1.3.2.
Page 12.32 07.03.27

Dial Gauge
Sample
Platform
Dial Gauge
Holder
Central Disk’s
Fixing Screws
(3x)
Figure 12.22: Sample Height Adjustment on Z Translation Stage
12.8.1.3.1 Mounting the Z Translation Stage
You can mount the Z translation stage onto the PW3069/00 Open Eulerian Cradle as follows:
1. Mount the open Eulerian cradle onto the PreFIX interface on the goniometer and report this to the data
collector software. Use the X’Pert Wizard: “Exchange Sample Stage” and follow its instructions for the
correct procedures (see section 12.1.1 for a description of the procedures).
2. Dismount the open Eulerian cradle from the goniometer. Do not disconnect the electrical connecting
cable.
3. If mounted, remove the multi-purpose sample holder or wafer holder from the open Eulerian cradle.
4. Before you mount the Z translation stage, look at its bottom, you will see three threaded screw holes
which will match the three holes on the securing ring (indicated in Figure 12.23) when they are
correctly lined up. In steps 7 to 9 you will be inserting three screws into these holes.
5. Place the Z translation stage into the open Eulerian cradle, make sure that it distinctly clicks into place.
6. Turn the cradle upside down and place the securing ring over the Z translation stage’s base so that the
holes in the securing ring line up with those in the base (you will only be able to see one or two holes at
the same time). Make sure that the countersink in the holes on the securing ring are on the surface
facing you, not facing the base (see Figure 12.23).
7. Insert one of the supplied screws (M3 x 10) and tighten it.
8. Use the Phi movement of the data collector software to rotate the open Eulerian cradle (make sure that
the cradle rotation is not obstructed) until you can gain access to the next screw hole. Insert the next
screw and tighten it.
07.03.27 Page 12.33

Securing Ring
Fixing Screw
Figure 12.23: PW3069/00 Open Eulerian Cradle Viewed from Bottom

9. Repeat step 8 for the final screw.
10. Re-mount the open Eulerian cradle.
The Z translation stage is now ready for use.
12.8.1.3.2 Removing the Z Translation Stage’s Central Disk
You can create more space to mount your sample on the Z translation stage by removing the central disk. You
do that as follows:
1. If the Open Eulerian Cradle is mounted on the X’Pert PRO goniometer, remove it from the PreFIX
stage interface. See section 12.1.1 for this procedure.
2. Loosen the central disk’s three fixing screws (see Figure 12.22).
3. Hold one hand under the cradle and carefully turn it upside-down. The three screws and the central disk
should now fall into your hand.
4. Turn the cradle the right way up and mount it on the goniometer.
The cradle is now ready for use.
Page 12.34 07.03.27

Figure 12.24: Central Disk Removed from Z Translation Stage
12.8.1.3.3 Mechanical Sample Height Adjustment with the Z Translation Stage
In order to achieve accurate measurements the sample surface must be positioned in the reference plane for the
sample height. When the sample is mounted onto the Z translation stage sample height adjustment is performed
with the use of a dial gauge. To align the sample proceed as follows:
1. Mount the dial gauge onto the dial gauge holder as shown in Figure 12.22.
2. Rotate the upper part of the Z translation stage so that the reading on the dial gauge corresponds to the
Z = 0 position as provided by the PANalytical Service Engineer when the system was installed.
The sample is now adjusted to the correct height position.
is known to within a few micrometers. Do not therefore pull on the
long arm of the dial gauge assembly, rotate the outer rim of the
gauge or drop the gauge as these actions are likely to cause the
gauge to lose calibration.
for the delicate sample. Alternatively, you can use the procedure for sample height adjustment with the use of
X-rays as described in section 12.8.1.3.4. Alignment of a sample for micro-diffraction experiments using an
alignment microscope is described in section 10.4.1 in Chapter 10 in Part II of this User’s Guide.
07.03.27 Page 12.35

12.8.1.3.4 Aligning the Sample Using X-rays

When mechanical contact with the sample surface should be avoided, or when measurements are to be made at
very low angles; the sample must be positioned so that it exactly intersects the incident beam when set parallel
to it. A procedure for sample alignment using X-rays is described in this section. Mechanical alignment using a
dial gauge is described in section 12.8.1.3.3. Sample alignment for micro-diffraction experiments is described in
section 10.4.1 in Chapter 10 in Part II of this User’s Guide.
In order to align a sample on the Z translation stage using X-rays the sample must be large and flat. The alignment
procedure is as follows:
slit) and report this to the data collector software.
center.
3. Set all of the axes 2theta, omega, phi and psi to 0º; rotate the upper part of the Z translation stage to its
lowest position and make sure that the X-ray beam is not obstructed by the sample or the open Eulerian
cradle.
4. Insert a 0.2 mm copper attenuation foil into the incident beam path in order to protect the detector.
5. Use a small receiving slit or the X’Celerator or the PIXcel in the scanning mode to find the peak
position of the direct X-ray beam by performing a 2θ scan through the 2θ = 0º position. Make a note of
the exact 2θ peak position.
the direct beam.
c. If you are using an X’Celerator, rotate it 90º (see section 21.4 in Chapter 21 of Part II of this User’s
Guide) and set it to the receiving slit mode. Use the maximum length of 9 mm. Do not insert a slit
into the the fixed anti-scatter slits holder.
d. If you are using a PIXcel, set it to the receiving slit mode and use the maximum length. Do not
insert a slit into the the fixed anti-scatter slits holder.
(Ip).
9. Set 2θ = 0º and rotate the upper part of the Z translation stage until the direct beam intensity is equal to
Ip/2.
11. The next action depends on whether Im > Ip/2 (step a), or Im < Ip/2 (step b).
a. If Im > Ip/2, move the sample forward with small increments of Z until the maximum intensity
b. If Im < Ip/2, move the sample backwards with small increments of Z until the maximum intensity
12. Move the goniometer to the peak position of the ω scan where Im equals Ip/2 and make a note of the Full
Width at Half Maximum (FWHM) of the peak.
Page 12.36 07.03.27

14. Set the ψ angle at the value that produces the minimum FWHM.
Alternatively you can automatically optimize the ψ setting in a series of ω scans using the optimize
program in the data collector software.
sample is now aligned at optimal 2θ, ω, ψ and Z settings.
NOTE: If you are using an X’Celerator, rotate it back to its normal position before starting the
measurement.
12.8.1.3.5 Dismounting the Z Translation Stage
You can dismount the Z translation stage as follows:

1. Dismount the open Eulerian cradle from the goniometer.
2. Turn the cradle upside down.
3. Use the Phi movement of the data collector software to rotate the open Eulerian cradle (make sure that
the cradle rotation is not obstructed) until you can gain access to the securing screws. Undo and remove
all three fixing screws.
4. Remove the securing ring. Turn the open Eulerian cradle the right way up and pull the Z translation
stage out.
5. Re-mount the open Eulerian cradle.
The open Eulerian cradle is now ready for use with a multi-purpose sample holder or a wafer holder.
07.03.27 Page 12.37

12.9 PW3070/00 OPEN EULERIAN CRADLE WITH MOTORIZED X-TRANSLATION

The PW3070/00 Open Eulerian Cradle with motorized X-translation is a sample stage used for texture, omega-
stress analysis, wafer mapping and parallel beam applications. The cradle is shown in Figure 12.25. It can be
PreFIX mounted onto an X'Pert PRO goniometer.
Figure 12.25: PW3070/00 Open Eulerian Cradle with Motorized X-translation

With a Wafer Holder Mounted on the Cradle
Samples with a maximum diameter of 70 mm (100 mm if not translated), a maximum height of 4 mm, and a
maximum mass of 150 g can be mounted onto this cradle. Several sample mounting platforms are available for
the open Eulerian cradle. The type of sample mounting platform to be mounted depends on the sample to be
analyzed. Details about the sample mounting platforms and their specific reference planes for sample height
alignment are given in section 12.9.1.
When a sample is mounted onto the cradle it can be rotated over phi range of n x 360° and tilted over a psi range
from -5° to +95°. The samples can be automatically positioned in the X direction over a total range of 50 mm.
Samples can be translated manually in the Y direction. An overview of the specifications of the axes on the
PW3070/00 Open Eulerian Cradle is given in Table 12.8.
Page 12.38 07.03.27

Table 12.8: Specifications of the Adjustable Axes on the PW3070/00 Open Eulerian Cradle
Axis Phi Psi X Y
Adjustable Automatic Automatic Automatic Manual
Range n x (0º - 360º) -5º to +95º -25 mm to 25 mm -25 mm to 25 mm
Minimum step size 0.01º 0.01º 0.01 mm -

Accuracy ±0.05º ±0.05º ±0.5 mm ±0.5 mm
Reproducibility ±0.05º ±0.05º ±0.5 mm ±0.5 mm
Slew speed 10º per second 5º per second 10 mm/s -
12.9.1 Accessories
12.9.1.1 Wafer Holder
A Wafer Holder is included with the PW3070/00 Open Eulerian Cradle. It is shown in Figure 12.26. It is used
to mount wafers with a thickness of 0.35 mm and a maximum diameter of up to 100 mm (4 inch). The wafer
holder is designed such that when a 0.35 mm thick wafer is mounted it is automatically aligned for the correct
sample height.
Figure 12.26: Wafer Holder for PW3070/00 Open Eulerian Cradle
12.9.1.1.1 Mounting the Wafer Holder
The wafer holder can be mounted onto the PW3070/00 Open Eulerian Cradle as follows:
1. Place the wafer holder in its position on the phi ring of the Open Eulerian Cradle.
2. Apply enough pressure onto the wafer holder to click it into place.
07.03.27 Page 12.39

12.9.1.2 Sample Cups

Two sample cups are included with the PW3070/00 Open Eulerian Cradle. The sample cup is shown in Figure
12.27. The inner diameter of the cup is 74 mm, the depth is 4 mm. The sample cup must be placed on the sample
stage so that its reference plane is exactly level with the goniometer’s reference plane.
Figure 12.27: Sample Cup for PW3070/00 Open Eulerian Cradle
12.9.1.2.1 Mounting the Sample Cups
The sample cup can be mounted onto the PW3070/00 Open Eulerian Cradle as follows:
1. Place the sample cup in its position on the phi ring of the Open Eulerian Cradle.
2. Apply enough pressure onto the sample cup to click it into place.
12.9.2 Use
12.9.2.1 Mounting Samples on the Wafer Holder
There are clips provided on the wafer holder which can be used to gently and securely hold full wafers or large
pieces of wafers. Alternatively some form of adhesive tape or plasticine may be used. Care should be taken to
avoid straining the sample as this will alter the diffraction profile. The footprint of the incident beam should be
well away from the mounting area if there is any doubt about the strain-free nature of the mounting. When
measurements at low angles are being used, care should be taken to avoid obstructing the X-ray beam path with
12.9.2.2 Mounting Samples on the Sample Cup

Adhesive tape or plasticine may be used to fix the sample to the sample cup. Care should be taken to avoid
straining the sample as this will alter the diffraction profile. The footprint of the incident beam should be well
away from the mounting area if there is any doubt about the strain-free nature of the mounting. When
measurements at low angles are being used, care should be taken to avoid obstructing the X-ray beam path with
Page 12.40 07.03.27


When mechanical contact with the sample surface must be avoided, or when measurements are to be made at
very low angles; the sample must be positioned so that it exactly intersects the incident beam when set parallel
to it. A procedure for sample alignment using X-rays is described in this section.
In order to align a sample using X-rays the sample must be large and flat. The alignment procedure is as follows:
slit) and report this to the data collector software.
2. Center the sample in the heart of the goniometer.
3. Set all of the axes 2theta, omega, psi and phi to 0º.
4. Remove the wafer holder or the sample cup from the sample stage.
5. Use a small receiving slit or the X'Celerator or the PIXcel in the scanning mode to find the peak
position of the direct X-ray beam by performing a 2θ scan through the 2θ = 0º position. Make a note of
the exact 2θ peak position.
the direct beam.
7. Depending on the diffracted beam optics being used, perform one of the following actions:
c. If you are using an X'Celerator, rotate it 90º (see section 21.4 in Chapter 21 of Part II of this User's
Guide) and set it to the receiving slit mode. Use the maximum length of 9 mm. Do not insert a slit
into the the fixed anti-scatter slits holder.
(Ip).
9. Set 2θ = 0º and mount the wafer holder with the wafer mounted or the sample cup.
11. Move the goniometer to the peak position of the ω scan and make a note of the Full Width at Half
Maximum (FWHM) of the peak.
13. Set the ψ angle at the value that produces the minimum FWHM. Alternatively you can automatically
optimize the ψ setting in a series of ω scans using the optimize program in the data collector software.
sample is now aligned at optimal 2θ, ω and ψ settings.
NOTES: If you are using an X'Celerator, rotate it back to its normal position before starting the
measurement.
07.03.27 Page 12.41

12.10 PW3071/60 STAGE FOR SOLIDS OR POWDERS IN FLAT SAMPLE HOLDERS

The PW3071/60 is a spring loaded sample holder for accurate and reproducible mounting of flat solid samples
or samples in flat sample holders, it is shown in Figure 12.28. This sample stage is included as a standard
accessory with X’Pert PRO MPD systems to be used as an alignment shaft in the tube height alignment
procedure (see section 1.4.9 in Chapter 1 in Part II of this User’s Guide). It can be PreFIX mounted onto an
X’Pert PRO goniometer. The reference plane for the correct sample height is situated on the bottom surface of
the sample clamp. The sample height positioning accuracy is ± 10 μm. A vertical reference line on the sample
clamp indicates the symmetry plane of the sample stage.
Solid samples with a minimum width of 40 mm and a maximum thickness of 5 mm can be mounted. The
maximum sample mass is 50 g. A PW1172/01 Flat Sample Holder can be used for smaller solid samples or
powder samples.
Using this sample holder together with the single knife edge in the tube height fine check and adjustment
procedure is described in section 1.4.9.2 of Chapter 1 in Part II of this User’s Guide.
Reference Line
Sample Clamp
Spring
Figure 12.28: PW3071/60 Sample Stage
12.10.1 Accessories
12.10.1.1 PW1172/01 Set of 25 Flat Sample Holders
PW1172/01 is a set of 25 rectangular sample holders for powder samples or small solid samples. The maximum
sample volume is 15 mm width x 20 mm length x 2 mm thickness. A sample holder consists of a metal holder
plate and a metal back plate. It can be used to prepare samples using the back-loading technique. More
information about this type of sample holder and its applications is given in Appendix A of this User’s Guide.
12.10.1.2 PW3071/65 Beam Knife for Flat Sample Stage

The PW3071/65 Beam Knife for Flat Sample Stage can be mounted onto the PW3071/60 Flat Sample Stage in
order to improve the peak-to-background ratio in measurements using the PW3015/x0 X’Celerator or a
PW3018/00 PIXcel.
Page 12.42 07.03.27

Figure 12.29: PW3071/65 Beam Knife Mounted onto a PW3071/60 Sample Stage
12.10.1.2.1 Mounting the Beam Knife onto the Flat Sample Stage
Mount the beam knife onto the flat sample stage as follows:
1. Unlock the black knurled knob on the rear side of the beam knife holder and set the knife in its highest
position. Lock the black knurled knob.
2. Slide the beam knife holder into its position on the flat sample stage as shown in Figure 12.29, making
sure that the beam knife is parallel to the reference line on the flat sample stage.
supplied.
12.10.2 Use
To mount a flat sample onto the sample holder proceed as follows:
1. Fit the sample onto the sample holder between the sample clamp and the spring against the back edge
of the holder.
2. Check that the sample surface is flush with the reference plane.
NOTE: We recommend that you use a mask opening on the incident beam PreFIX that irradiates 10 mm or
less of the sample width in order to prevent some of the sample stage itself being irradiated by the
incident X-ray beam.
07.03.27 Page 12.43

12.11 PW3072/60 STATIONARY STAGE FOR PW18XX SAMPLE HOLDERS

PW3072/60 is a stationary platform to mount samples fitted in a PW18xx type of circular sample holders. The
stationary stage is shown in Figure 12.30, it can be PreFIX mounted onto an X’Pert PRO goniometer. It is
suitable for all applications except for texture, psi-stress and non-ambient analysis. The sample platform is used
to clamp a sample holder accurately against a reference surface which ensures that the sample surface coincides
with the goniometer axis, height positioning accuracy is ± 10 μm. The maximum sample mass (including the
sample holder) is 150 g.
Figure 12.30: PW3072/60 Stationary Stage for PW18xx Sample Holders with Sample Holder Mounted
12.11.1 Accessories
One circular sample holder is included with the PW3072/60 Stationary Stage. The sample holder is physically
the same as the PW1813/32 Sample Holders for Circular Solid Samples. It is used to mount filters or solid
samples with a diameter between 30 mm and 32.3 mm and a maximum thickness of 6 mm. The circular silicon
pressed powder sample delivered with the X’Pert PRO diffraction system fits into this holder. More details about
this type of sample holder are given in Appendix A of this User’s Guide (section A.2.1.4).

The PW18xx Sample Holders are circular sample holders that can be loaded in the PW3072/60 Stationary Stage.
The sample holders can also be used with the PW3064/00 Sample Spinner, the PW3074/00 Multi-purpose
Sample Stage and on the PW3061/21 Sample Holder for Solid Samples to be used with the PW3060/20 MRD
cradle. A description of the PW18xx Sample Holders and their applications is given in Appendix A of this User’s
Guide.
Page 12.44 07.03.27
12.11.1.3 PW3072/65 Beam Knife for Stationary Stage

The PW3072/65 Beam Knife for Stationary Stage can be mounted onto the PW3072/60 Stationary Stage in
order to improve the peak-to-background ratio in measurements using the PW3015/x0 X’Celerator or a
PW3018/00 PIXcel.
Figure 12.31: PW3072/65 Beam Knife Mounted onto a PW3072/60 Stationary Stage
12.11.1.3.1 Mounting the Beam Knife onto the Stationary Stage
Mount the beam knife onto the stationary stage as follows:

1. Unlock the black knurled knob on the beam knife and set the knife in its highest position. Lock the
black knurled knob.
2. Bring the beam knife holder into its position on the stationary stage as shown in Figure 12.31.
3. Fix the beam knife holder to the spinner using the M3 x 10 screw with the black knurled knob supplied.
12.11.2 Use
To mount a sample in the platform:
1. Press the spring loaded lever down with one hand and insert the sample until it is firmly against the far
surface so that the spring can press it securely into the reference plane.
If the sample is not inserted so that the top holders (bars or clamps) are in contact with the sample, the sample
will tilt causing a sample height displacement and thus a peak shift. This also causes defocusing and thus peak
broadening and a weakening of intensity.
07.03.27 Page 12.45

12.12 PW3074/00 MULTI-PURPOSE SAMPLE STAGE

The PW3074/00 Multi-purpose Sample Stage is designed to mount and accurately position large and irregularly
shaped samples for phase analysis and omega-stress measurements.
The multi-purpose sample stage basically consists of a sample mounting table that can be PreFIX mounted onto
an X’Pert PRO goniometer. It is shown in Figure 12.32. A sample holder for mounting flat samples is included
as an accessory. The sample mounting has a number of threaded holes which are used to secure samples by
means of screws and clamps. The position of these holes is such, that third party micro-positioning devices can
be mounted. The height of the sample table can be chosen from one of three basic positions with steps of 25 mm.
When the sample stage is used in combination with an X’Pert PRO Theta-Theta diffraction system the sample
mounting table can be completely removed to allow measurements on extremely large samples positioned on the
base plate of the X’Pert PRO enclosure. Refer to section 12.12.2 for sample mounting and height alignment
procedures.
The PW3074/00 Multi-purpose Sample Stage can only be fitted to an X’Pert PRO vertical goniometer. Samples
with maximum dimensions of 10 cm diameter and 10 cm height, weighing no more than 1 kg can be mounted
on this sample stage.
The sample stage has three axes that can be manually adjusted: phi, Z and a tilt axis.
The sample can be manually rotated (φ) through 360°, and tilted through ± 3°. Sample height (Z) can be adjusted
very accurately using the dial gauge supplied with the sample stage. The reference plane for sample height
adjustment is indicated with the use of a reference plate that can be inserted into a holder for flat samples. The
reference plate and the dial gauge are described in sections 12.12.1.2 and 12.12.1.3. An overview of the
specifications of the adjustable axes is given in Table 12.9.
Figure 12.32: PW3074/00 Multi-purpose Sample Stage with Tools

Page 12.46 07.03.27
Table 12.9: Specifications of the Adjustable Axes on the Multi-purpose Sample Stage
Axis Phi Tilt * Z*
Range Infinite ± 3º 0 to 100 mm
Accuracy ± 1º 0.3º ± 15 μm
Reproducibility ± 1º 0.3º ± 15 μm
* = With the use of a dial gauge
12.12.1 Accessories
The PW3074/00 Multi-purpose Sample Stage can be used together with a dial gauge and a variety of sample
holders. These are described in this section. You can also, taking into account the specifications given above,
mount your own sample holder onto this sample platform. To help you in designing sample holders for the
Multi-purpose Sample Stage, a schematic diagram of the mounting platform is shown in Figure 12.33.
Figure 12.33: Schematic Diagram of the Sample Mounting Platform of the PW3074/00 Multi-purpose
Sample Stage
12.12.1.1 Sample Holder for Flat Solid Samples

A spring loaded sample holder for accurate and reproducible mounting of flat solid samples or samples in flat
sample holders is included with the PW3074/00 Multi-purpose Sample Stage. Flat samples with a maximum
surface of 60 mm x 60 mm, can be mounted onto this sample holder. The maximum sample mass is 50 g.
Alternatively, PW1172/01 Sample Holders can be mounted onto the sample holder. PW1172/01 Sample Holders
can contain powder samples or solid materials with a maximum volume of 15 mm width x 20 mm length x 2
mm thickness. The reference plane for the correct sample height alignment is situated on the bottom surface of
the sample holder for flat solid samples.
07.03.27 Page 12.47
12.12.1.1.1 Mounting the Sample Holder onto the Multi-purpose Sample Stage
Figure 12.34: Mounting a Sample onto the PW3074/00 Multi-purpose Sample Stage
Mount the sample holder for flat samples onto the PW3074/00 Multi-purpose Sample Stage as follows:
Insert the sample holder into the multi-purpose sample stage in the position indicated in Figure 12.32
until it clicks into place. It is not necessary to remove the sample mounting table in order to fit the sam-
ple holder, but it may be necessary to lower the sample table prior to inserting the sample holder for flat
samples.
12.12.1.1.2 Mounting a Flat Sample onto the Sample Holder
Mount a flat solid sample or a powder sample in a PW1172/01 Sample Holder as follows:
1. Fit the sample between the metal plate and the spring of the sample holder (see Figure 12.32) against
the back edge of the holder.
2. Check that the surface is flush with the reference plane.
NOTE: If you are using the flat sample holder we recommend that you use a mask opening on the incident
beam PreFIX that irradiates 10 mm or less of the sample width in order to prevent some of the
sample stage itself being irradiated by the incident X-ray beam. If part of the sample holder is
irradiated it may result in spurious peaks or a high background on the diffractogram.
Page 12.48 07.03.27

12.12.1.2 Reference Plate

A metal reference plate is included with the PW3074/00 Multi-purpose Sample Stage. This reference plate can
be inserted into the sample holder for flat solid samples (see section 12.12.1.1 and Figure 12.35). When this plate
is placed in position its top surface indicates the reference plane for sample height adjustment. The reference
plate can then be used for the calibration of the dial gauge, as described in section 12.12.1.3.1.
12.12.1.3 Dial Gauge

A dial gauge for sample height alignment purposes is supplied with the PW3074/00 Multi-purpose Sample
Stage. It can be mounted onto the sample stage with the use of a dial gauge holder, see Figure 12.35. The
calibration of the dial gauge is described below, use of the dial gauge for sample height alignment is described
in section 12.12.2.
Figure 12.35: PW3074/00 (Dial Gauge Calibration)
12.12.1.3.1 Calibration of the Dial Gauge
The following procedures are used to calibrate the dial gauge.

1. Insert the reference plate into the sample holder between the spring and the reference plane (bottom
surface of the sample holder) until it cannot be pushed in any further (see Figure 12.32).
2. Mount the sample holder onto the goniometer.
07.03.27 Page 12.49

3. Push the two dial gauge holder arms into position on the multi-purpose sample stage until they are
locked into position (clicks into the deep grooves). The dial gauge measuring pin now should point to
the center of the reference plate (see Figure 12.35).
4. Loosen the dial gauge fixing screw shown in Figure 12.35. Rotate the dial gauge in its holder until you
can comfortably read its scale. Firmly tighten the dial gauge fixing screw.
5. Turn the knurled ring of the dial gauge until the 0.002 mm scale reads zero.
6. Read and record the exact 0.2 mm scale value for later use when mounting and aligning the sample.
7. Remove the dial gauge holder and the sample shaft.
NOTE: Take care not to turn the dial gauge scale accidentally when removing the holder. If the scale is
turned accidentally repeat the complete calibration procedure.
After calibration the dial gauge is used to align the height of the sample, mounted on the sample mounting table.
12.12.1.4 Pin Key

A pin key is included with the PW3074/00 Multi-purpose Sample Stage. This pin key is used to rotate the sample
mounting table around the phi axis. The sample can be rotated infinitely. This facility can be used to align the
sample optimally with respect to the incident X-ray beam. Rotation of the sample is required for biaxial residual
stress analysis.
Figure 12.36: Pin Key
You rotate the sample table by inserting the two locating pins on the pin key into the holes on the sample rotating
table as shown in Figure 12.36 and then pulling slowly in a circular movement to rotate the sample table.
Page 12.50 07.03.27

12.12.1.5 PW1172/01 Set of 25 Flat Sample Holders

PW1172/01 is a set of 25 rectangular sample holders for powder samples or small solid samples. The maximum
sample volume is 15 mm width x 20 mm length x 2 mm thickness. A sample holder consists of a metal holder
plate and a metal back plate. It can be used to prepare samples using the back-loading technique. More
information about this type of sample holder and its applications is given in Appendix A of this User’s Guide.
12.12.1.6 PW3074/10 Beam Knife for Multi-purpose Sample Stage

The PW3074/10 Beam Knife for Multi-purpose Sample Stage can be mounted onto the
PW3074/00 Multi-purpose Sample Stage in order to improve the peak-to-background ratio in measurements
using the PW3015/x0 X’Celerator or a PW3018/00 PIXcel.
Figure 12.37: PW3074/10 Beam Knife Mounted onto a PW3074/00 Multi-purpose Sample Stage
12.12.1.6.1 Mounting the Beam Knife onto the Multi-purpose Sample Stage
Mount the beam knife onto the multi-purpose sample stage as follows:
black knurled knob.
2. Push the two arms of the beam knife holder into their position on the multi-purpose sample stage until
they are locked into position (clicked into the deep grooves) as shown in Figure 12.8. The beam knife
should now be above the center of the sample mounting table.
07.03.27 Page 12.51

You can also use the beam knife in combination with the sample holder for flat solid samples. To mount the
sample holder and the beam knife onto the multi-purpose sample stage, proceed as follows:
1. Insert the flat sample holder in position as described in section 12.12.1.1.1.
black knurled knob.
3. Push the two arms of the beam knife holder into their position on the multi-purpose sample stage until
they are locked into position (clicked into the shallow grooves).
12.12.2 Use
There are two methods of mounting a sample on the PW3074/00 Multi-purpose Sample Stage:
• on the sample holder
• on the sample mounting table.
Both of these mounting methods are determined by the weight, shape and volume of the sample. Mounting of
flat samples with the sample holder is described in section 12.12.1.1. This section describes mounting of samples
onto the sample mounting table, coarse and fine sample height adjustment and sample tilt adjustment.
12.12.2.1 Mounting a Sample onto the Sample Table

Samples with a maximum height of 100 mm, a maximum diameter of 100 mm and 1 kg maximum mass can be
mounted onto the sample mounting table.
The sample must be attached and positioned accurately before measuring the sample. There are several ways of
attaching samples to the mounting table: screws and clamps, the M4 threaded holes in the mounting plate of the
table, plasticine, or adhesive tape (see Figure 12.36).
The spot on the sample that is to be analyzed has to be mounted in the center of the sample mounting table; there
are no X and Y direction translation possibilities on the multi-purpose sample stage.
CAUTION
Care must be taken that clamps, samples or mounting materials do
not obstruct the movements of the goniometer arms.
Suitable clamps or supports should be obtained locally as samples are of various shapes, dimensions and weights.
Fixing screws that protrude more than 1 or 2 mm will limit the levelling range of the sample mounting table.
12.12.2.2 Coarse Sample Height Adjustment

The sample mounting table is secured to the height adjustment mechanism, see Figure 12.38, using two screws
(tightened with an M10 spanner), in one of the three available positions:
• sample height maximum 50 mm - use the upper set of fixing holes
• sample height from 25 to 75 mm - use the middle set of fixing holes
• sample height from 50 to 100 mm - use the lower set of fixing holes.
Select one of these three positions so that the area to be analyzed can be accurately positioned, in height, to
coincide with the omega axis. The sample mounting table can be completely removed so that extremely large
samples can be measured on an X’Pert PRO Theta-Theta diffraction system. Sample height adjustment
procedures are given in section 12.12.2.3.
Page 12.52 07.03.27
Figure 12.38: PW3074/00 (Bottom View)
The following procedure is used to align a sample using the sample mounting table:
1. Move the diffracted beam optics out of the way, to 160° 2θ if possible (or the highest value allowed),
using the software, to obtain more working space. Alternatively, you can remove (all of) the diffracted
beam PreFIX modules.
2. Remove the sample mounting table from the height adjustment mechanism by loosening the two fixing
screws at the bottom of the sample stage, using the M10 spanner, see Figure 12.38.
3. Mount the sample on the sample mounting table plate.
CAUTION
Care must be taken that the clamps or mounting materials do not
obstruct the movement of the goniometer arms.
4. Mount the sample mounting table at one of the three height positions. Make sure that you can fit the
dial gauge holder. Tighten the two fixing screws using the M10 spanner.
This procedure adjusts the sample height coarsely. Follow the instructions given in 12.12.2.3 to finely adjust the
sample height.
07.03.27 Page 12.53

12.12.2.3 Fine Sample Height and Tilt Adjustment

Fine adjustment of the sample height can be obtained by rotating the height adjusting screw, shown in Figure
12.39. One complete rotation of the screw corresponds to a change in height of 0.35 mm. The total range of the
fine adjustment mechanism is approximately 50 mm. Proceed as follows to finely adjust the sample height:
Figure 12.39: PW3074/00 (Height Adjustment)

1. Push the two arms of the dial gauge holder (with the dial gauge mounted) into position on the multi-
purpose sample stage until they are locked into the deep grooves in the arms. In this position, the dial
gauge measuring pin is in the center of the sample analysis surface, see Figure 12.39.
2. Loosen the height locking screw, shown in Figure 12.39.
3. Adjust the height of the sample mounting table by turning the height adjusting screw with the small
hexagonal screwdriver (M4), until the dial gauge shows a reading.
4. Tighten the height locking screw and remove the hexagonal screwdriver.
5. Pull both of the arms of the dial gauge holder (with the dial gauge mounted) until it clicks into the
shallow grooves. In this position, the dial gauge measuring pin is 5 mm from the center of the analysis
surface.
Page 12.54 07.03.27

6.Using the pin key, rotate the mounting plate through 120°, and then through 240° (the rotation
procedure is given in section 12.12.1.4). If the reading of the dial gauge changes after each rotation, tilt
the sample using the three levelling screws underneath the sample stage, see Figure 12.38. Keep on
repeating this step until you read approximately the same value on the dial gauge through the complete
rotation. The sample surface for analysis is now levelled.
NOTE: This levelling of the sample surface is very important, especially when measuring in focusing
geometry. If the sample surface is tilted, a defocusing effect occurs leading to peak broadening and
weakening.
7. Reposition the dial gauge holder with the dial gauge mounted, by pushing it into the multi-purpose
sample stage until it clicks into the deep grooves in the arms shown in Figure 12.39. When the dial
gauge holder is in this position the measuring pin is in the center of the sample analysis surface.
8. Loosen the height locking screw.
9. Adjust the height of the sample mounting table by turning the height adjusting screw using the small
hexagonal screwdriver until the dial gauge shows exactly the same 0.2 mm calibration reading recorded
in step 6 of 12.12.1.3.1 “Calibration of the dial gauge”.
10. Tighten the Height Locking Screw, ensuring that the reading of the dial gauge does not change.
11. Remove hexagonal screwdriver and the dial gauge holder.
The sample is now aligned and ready for measurement.
NOTE: Take care not to turn the dial gauge scale accidentally when removing the holder. If the scale is
turned accidentally repeat the complete calibration procedure.
12.13 PREFIX POSITIONING STAGES

PreFIX Positioning Stages provide motor-assisted sample positioning and alignment on vertical X'Pert PRO
MPD systems. These stages are used to accurately position thin films and small samples with respect to the
X-ray beam. The motors are controlled using an infrared (IR) remote control unit. The IR radiation can be
transmitted through the windows of the PW3040/60 Enclosure doors, which means that the sample can be
moved while the X-ray beam shutter is opened. This allows the intensity of the direct or the diffracted X-ray
beam to be monitored directly during sample positioning and alignment.
Three types of positioning stage are available:

• PW3075/61 Positioning stage with motorized X, Y, Z, Tilt and Phi movements, described in section
12.13.1.
• PW3075/62 Positioning stage with motorized Z, Tilt and Phi movements, described in section 12.13.2.
• PW3075/63 Positioning stage with motorized X, Y and Z movements, described in section 12.13.3.
These PW3075/6x Positioning Stages can be PreFIX mounted onto a vertical X'Pert PRO MPD goniometer.
Exchanging PreFIX sample stages is described in section 12.1.
The general specifications of the PW3075/6x Positioning Stages are listed in Table 12.10.
07.03.27 Page 12.55

Table 12.10: PW3075/6x Positioning Stages - Specifications
Stage X Y Z Tilt Phi
PW3075/61 Positioning Stage with Motorized X, Y, Z, Tilt and Phi Movements
Range 75 mm 50 mm 75 mm 20° n * 360°

Min. step size Ca. 0.05 mm Ca. 0.05 mm Ca. 0.002 mm Ca. 0.01° Ca. 0.01°
Max. speed 40 mm / min 40 mm / min 40 mm / min 20° / min 180° / min
PW3075/62 Positioning Stage with Motorized Z, Tilt and Phi Movements

Range - - 75 mm 20° n * 360°
Min. step size - - Ca. 0.002 mm Ca. 0.01° Ca. 0.01°
Max. speed - - 40 mm / min 20° / min 180° / min

PW3075/63 Positioning Stage with Motorized X, Y and Z Movements
Range 75 mm 50 mm 75 mm - -
Min. step size Ca. 0.05 mm Ca. 0.05 mm Ca. 0.002 mm - -

Max. speed 40 mm / min 40 mm / min 40 mm / min - -
The PW3075/6x Positioning Stages are controlled using PW3075/64 Control Electronics. It is possible to use
more than one of these stages sequentially on an X'Pert PRO system. The same PW3075/64 Control Electronics
can be used for each stage. These electronics and other accessories for the sample stages, including beam knives
and sample holders, are described in section 12.13.4.
Sample positioning and alignment using the positioning stages is described in section 12.13.5.
CAUTION
Be very careful to avoid collisions between the optics and oversize
samples when large angular movements are requested.
WARNING
IT IS POSSIBLE TO MOVE THE POSITIONING STAGES WITH THE DOORS
OF THE INSTRUMENT ENCLOSURE OPENED. MAKE SURE THAT YOU
KEEP CLEAR WHILE MOVING THE SAMPLE STAGE.
Page 12.56 07.03.27

12.13.1 PW3075/61 Positioning Stage with Motorized X, Y, Z, Tilt & Phi

The PW3075/61 Positioning Stage is a sample stage with motorized X, Y, Z, Tilt and Phi movements. It is
designed to enable you to mount and accurately position thin films and small irregularly shaped samples. This
positioning stage is shown in Figure 12.41. Typical applications for this stage are reflectometry, measurements
of rocking curves, micro-diffraction and omega-stress analysis. The sample table can be moved over 75 mm in
the X and Z directions and over 50 mm in the Y direction, tilted over 20° and rotated over n x 360°. General
specifications of the PW3075/61 Positioning Stage are given in Table 12.10.
NOTES: 1. The tilt axis of the PW3075/61 Positioning Stage is beneath the sample surface. Therefore
changing the tilt position of the sample induces a change in the height (Z) position of the sample.
2. The position of the phi axis changes when the X and Y axes are moved.
The sample stage is equipped with a PreFIX U-block to mount a dial gauge or a beam knife. These accessories
are described in section 12.13.4.
Indications of the ϕ angle set are shown at the sample table. The distance between the lines is 5°. These lines are
meant for accurate ϕ angle setting for omega-stress measurements.
The phi rotation can be set continuously during the measurements, so that the sample acts as a slowly rotating
spinner. At the highest speed one revolution takes about 2 minutes.
Samples can be mounted onto the phi rotation table with adhesive material, for example plasticine or double-
sided adhesive tape. The maximum volume of the samples to be measured is a truncated cone with a base
diameter of 70 mm, a top diameter of 50 mm and a height of 75 mm. The maximum sample mass (including the
sample holder) is 300 g when used in combination with an X'Pert PRO MPD Omega-2Theta system; the
maximum sample mass (including the sample holder) is 1 kg in combination with an X'Pert PRO MPD Theta-
Theta system.
Accessories for this sample stage, including sample holders, are described in section 12.13.4. You can also
mount your own sample holder onto this sample platform, taking into account the specifications given above.
To help you in designing sample holders for the PW3075/61 Positioning Stage, a schematic diagram of the
mounting platform is shown in Figure 12.40.
Figure 12.40: Schematic Diagram of the PW3075/61 Positioning Stage’s Sample Mounting Platform
Sample height adjustment with respect to the reference plane can be performed using the PW3075/65 Dial
Gauge (see section 12.13.4.2). Sample height alignment procedures are described in section 12.13.5.
07.03.27 Page 12.57

PreFIX
Mounting
Position
Phi Rotation +
Reference Line +
- - Z
+ -
Y
ϕ Angle Marking
-
Tilt
- +
X
Figure 12.41: PW3075/61 Positioning Stage with X, Y, Z, Tilt and Phi Movements
12.13.2 PW3075/62 Positioning Stage with Motorized Z, Tilt and Phi

Movements
The PW3075/62 Positioning Stage is a sample stage with motorized Z, Tilt and Phi movements. It is designed
to allow you to mount and accurately position thin films and small or irregularly shaped samples. The positioning
stage is shown in Figure 12.42. Typical applications for this stage are reflectometry, measurements of rocking
curves and omega-stress analysis. The sample table can be moved over 75 mm in the Z direction, tilted over 20°
and rotated over n x 360°. General specifications of the PW3075/62 Positioning Stage are given in Table 12.10.
NOTE: The tilt axis of the PW3075/62 Positioning Stage is beneath the sample surface. Therefore changing
the tilt position of the sample induces a change in the height (Z) position of the sample.
Indications of the ϕ angle set are shown at the sample table. The distance between the lines is 5°. These lines are
meant for accurate ϕ angle setting for omega-stress measurements.
Page 12.58 07.03.27

The phi rotation can be set continuously during the measurements, so that the sample acts as a slowly rotating
spinner. At the highest speed one revolution takes about 2 minutes.
Samples can be mounted onto the phi rotation table with adhesive material, for example plasticine or double-
sided adhesive tape. Alternatively, they can be mounted onto a sample holder that can then be mounted onto the
phi rotation table. Sample holders for the PW3075/62 Positioning Stage are described in Section 12.13.5.
The maximum volume of the samples to be measured (including the sample holder) is a truncated cone with a
base diameter of 135 mm, a top diameter of 150 mm and a height of 75 mm. The maximum sample mass
(including the sample holder) is 300 g when used in combination with an X'Pert PRO MPD Omega-2Theta
system; the maximum sample mass (including the sample holder) is 1 kg in combination with an X'Pert PRO
MPD Theta-Theta system.
Figure 12.42: Schematic Diagram of the PW3075/62 Positioning Stage’s Sample Mounting Platform
07.03.27 Page 12.59

Sample height adjustment with respect to the reference plane can be performed using the PW3075/65 Dial Gauge
(see section 12.13.4.2). Sample height alignment procedures are described in section 12.13.5.
PreFIX
Mounting
Position
+
Z
Phi Rotation +
Holes for Sample
- Holder Mounting
Screws (6x)
-
ϕ Angle Marking
Tilt
Reference Line
Figure 12.43: PW3075/62 Positioning Stage with Z, Tilt and Phi Movements
Page 12.60 07.03.27

12.13.3 PW3075/63 Positioning Stage with Motorized X, Y and Z

Movements
The PW3075/63 Positioning Stage is a sample stage with motorized X, Y and Z movements. It is designed to
allow you to mount and accurately position small or irregularly shaped samples. The positioning stage is shown
in Figure 12.45. Typical applications for this stage are micro-diffraction and omega-stress analysis. The sample
table can be moved over 75 mm in the X and Z directions and over 50 mm in the Y direction. General
specifications of the PW3075/63 Positioning Stage are given in Table 12.10.
Samples can be mounted onto the sample table with adhesive material, for example plasticine or double-sided
adhesive tape. The maximum volume of the samples to be measured is a box with a footprint of 70 mm x 70 mm
and a height of 75 mm. The maximum sample mass (including the sample holder) is 1 kg.
Figure 12.44: Schematic diagram of the PW3075/63 Positioning Stage’s Sample Mounting Platform
Sample height adjustment with respect to the reference plane can be performed using the PW3075/65 Dial
Gauge (see section 12.13.4.2). Sample height alignment procedures are described in section 12.13.5.
07.03.27 Page 12.61

PreFIX
Mounting
Position
+
Z
+ -
Y
- +
X
Figure 12.45: PW3075/63 Positioning Stage with X, Y and Z Movements
Page 12.62 07.03.27

12.13.4 Accessories
12.13.4.1 PW3075/64 Control Electronics
The motorized movements of the PW3075/6x Positioning Stages are controlled by the PW3075/64 Positioning
Stage Control Electronics. The type number consists of an IR Stage Control electronics box mounted in the
PW3040/60 Instrument Enclosure and an IR remote control unit. They are shown in Figure 12.46, the remote
control shown is just an example (it could be slightly different in your system). Use of the control electronics
for sample positioning and alignment is described in section 12.13.5.
Figure 12.46: PW3075/64 Positioning Stage Control Electronics: IR Stage Control Unit
The Control electronics are connected with the PW3075/6x Positioning Stage with a cable. The cable can only
be disconnected from the PW3075/6x sample stage when the X'Pert PRO system is switched off. The procedure
for exchange of PW3075/6x sample stages (including disconnecting the cable) is described in section 12.1.
CAUTION
Do not disconnect the cable from the PW3075/6x Positioning Stages
when the X'Pert PRO system is switched on.
07.03.27 Page 12.63

12.13.4.2 PW3075/65 Dial Gauge

A dial gauge for sample height alignment purposes is available for the PW3075/6x Positioning Stages. The dial
gauge can be PreFIX mounted onto the PreFIX U-block on the sample stage as is shown in Figure 12.47. Use of
the dial gauge for sample height (Z position) alignment is described in section 12.13.5.2. The dial gauge is
factory-aligned for the sample stage on which it is used. The sample is at the correct height when the reading of
the dial gauge corresponds to the Z = 0 position provided by the PANalytical Service Engineer.
Figure 12.47: PW3075/65 Dial Gauge Mounted onto a PW3075/61 Positioning Stage
CAUTION
Do not turn the adjustment screw as this is used for calibration
purposes.
Page 12.64 07.03.27

12.13.4.3 PW3075/66 Beam Knife for Reflectivity Measurements

The PW3075/66 Beam Knife is an adjustable “De Wolff's” knife used in reflectivity measurements with the
PW3075/6x Positioning Stages to reduce the reflecting area on the sample. It is shown in Figure 12.48. The beam
knife can be mounted onto the PW3075/6x sample stage at the PreFIX U-block. The alignment and use of this
beam knife for reflectivity measurements are described in section 14.2.2 in Chapter 14 in Part II of this User's
Guide.
Figure 12.48: PW3075/66 Beam Knife for Reflectivity Measurements Mounted onto a PW3075/61
Positioning Stage
07.03.27 Page 12.65

12.13.4.4 PW3075/67 Beam Knife for Positioning Stages

The PW3075/67 Beam knife for Positioning Stages is used with the PW3075/6x Positioning Stages in order to
improve the peak-to-background ratio in measurements using the PW3015/x0 X'Celerator or the PW3018/00
PIXcel. The beam knife can be mounted onto PreFIX U-block on the PW3075/6x Sample Stages, as is shown in
Figure 12.49.
The height of the beam knife above the sample can be adjusted such that the gap between the knife and the
sample is between 0.5 and 5 mm. Instructions how to choose the optimum height of the knife above the sample
are given in section 14.3.6 of Chapter 14 in Part II of this User's Guide.
Figure 12.49: PW3075/67 Beam Knife Mounted onto a PW3075/61 Positioning Stage
12.13.4.5 PW3061/21 Sample Holder for Solid Samples

The PW3061/21 Sample Holder for Solid Samples is used to hold irregularly shaped samples securely in position
on the sample stage. It can be mounted onto the phi rotation table of the PW3075/62 Positioning Stage with
Motorized Z, Tilt and Phi movements. The PW3061/21 Sample Holder comprises a V-block and clamping block
as shown in Figure 11.7. The positions of these blocks can be changed to accommodate a wide variety of sample
shapes as well as samples mounted in PW18xx sample holders (see Appendix A of this User's Guide).
Page 12.66 07.03.27

12.13.4.5.1 Mounting the Sample Holder on the PW3075/62 Positioning Stage

The sample holder can be secured to the phi rotation table of the PW3075/62 Sample stage using the three screws
supplied.
12.13.4.5.2 Mounting Irregularly Shaped Samples

Irregularly shaped samples can be clamped between the V-block and the clamping block as shown in Figure
11.7. Proceed as follows to mount a sample:
1. Secure the V-block at one of its five specific positions on the sample holder, refer to Figure 11.7
2. Position the sample against the V-block.
3. Loosen the clamping screw on the clamping block and slide the block along its groove until it is firmly
up against the sample.
4. Tighten the clamping screw to lock the sample in position.
If measurements at low angles are required, take care that the mounting blocks (or any other material used to
secure the sample) do not obstruct the X-ray beam path.
12.13.4.6 PW3061/22 4-inch Wafer Holder

The PW3061/22 4-Inch Wafer Holder is a 100 mm (4 inch) diameter wafer mounting plate for semiconductor
wafers and other thin parallel-sided samples. It is fitted onto the phi rotation table of the PW3075/62 Positioning
Stage with Motorized Z, Tilt and Phi movements by six screws. The wafer holder is shown in Figure 11.8.
Clips are provided on the wafer holder, these clips can be used to securely (and gently) hold full wafers or large
pieces of wafer. Alternatively some form of adhesive tape or plasticine may be used. Care should be taken to
avoid straining the sample, as this will alter the diffraction profile. The footprint of the incident beam should be
well away from the mounting area if there is any doubt about the strain-free nature of the mounting. When
measurements at low angles are required, care should be taken to avoid obstructing the X-ray beam path with
12.13.4.7 9430 500 20351 Magnetic Ring

The magnetic ring can be fitted onto the PW3075/62 Positioning Stage in order to enable the 9430 500 20361
Sample Platform to be magnetically mounted. It is shown in Figure 11.9.
The magnetic ring is secured to the PW3075/62 Positioning Stage using the six screws supplied with the
magnetic ring.
12.13.4.8 9430 500 20361 Sample Platform

The 9430 500 20361 Sample Platform is used to mount thin parallel sided samples (for example: pieces of a
semiconductor wafer) onto the PW3075/62 Positioning Stage. It is shown in Figure 11.9.
The 9430 500 20351 Magnetic Ring must be mounted onto the PW3075/62 Positioning Stage and then the
sample platform (with the samples already fixed onto it) can be magnetically attached to it.
Adhesive tape or plasticine can be used to affix the samples onto the sample holder. Alternatively, you can use
the magnetic strips delivered with the sample platform. Care should be taken to avoid straining the sample, as
this will alter the diffraction profile. The footprint of the incident beam should be well away from the mounting
area if there is any doubt about the strain-free nature of the mounting. When measurements at low angles are
required, care should be taken to avoid obstructing the X-ray beam path with the mounting material.
07.03.27 Page 12.67

12.13.5 Use
12.13.5.1 Sample Movement Using the Remote Control
The motorized movements of the PW3075/6x Positioning Stages are controlled by the PW3075/64 Control
Electronics using an IR Remote Control Unit. The functionality of the buttons on the remote control unit and of
the various LEDs (Light Emitting Diodes) on the IR Stage Control box are given in the Table 12.11. The buttons
on the IR Remote Control Unit that are not described in the table are not used to control the sample stage
movements. Please note that the LED switches on after selection, even when the corresponding movement is not
available on the positioning stage that is being used.
Table 12.11: Functionality of the IR Remote Control Buttons on the

PW3075/64 Control Electronics
IR Remote
Control Functionality Additional Remarks
Button
0 Stop movement. Either the + or - LED switches off

Disable all motors. Either the X, Y, Z, Psi or Phi LED
switches off
1 Activate motor for movement in X direction. X- LED switches on
and and
Stop movement in any direction. Either the + or - LED switches off
2 Activate motor for movement in Y direction. Y-LED switches on

and and
3 Activate motor for movement in Z direction. Z- LED switches on

and and
4 Activate motor for movement in tilt direction. Tilt- LED switches on.
and and
Stop movement in any direction. Either the + or - led switches off.
5 Activate motor for movement in phi direction. Phi-LED switches on.

and and
Stop movement in any direction. Either the + or - LED switches off.
9 Toggle between fast and normal mode. Fast-LED switches on when fast
Fast mode indicates the velocity increments / mode is selected.
decrements and movement steps are approx-
imately 10 times larger than in normal mode.
Volume (+) Increase velocity of selected motor in positive

direction or decrease velocity of selected motor
in negative direction.
Volume (-) Increase velocity of selected motor in negative

direction or decrease velocity of selected motor
in positive direction.
Channel One step movement in positive direction of the Size of the step depends on the
(+) selected motor. selected motor
Channel (-) One step movement in negative direction of Size of the step depends on the
the selected motor. selected motor
Page 12.68 07.03.27

Table 12.12: Meaning of the Indicator Lamps on the IR Stage Control Unit of the PW3075/64 Control
Electronics
LED Meaning When Lit Additional Remarks
- Velocity of the selected motor is negative

+ Velocity of the selected motor is positive
Limit The limit (factory settings) for the selected motor Velocity applied to the selected motor
has been reached is switched off when limit is reached,
for example: when positioning stage
runs into the end stops.
Fast Fast mode is selected
Signal Signal sent from the IR remote control unit has

reached the IR stage control
X Motor for movement in X direction is enabled
Y Motor for movement in Y direction is enabled
Z Motor for movement in Z direction is enabled
Tilt Motor for movement in tilt direction is enabled
Phi Motor for movement in phi direction is enabled
12.13.5.2 Sample Height Alignment Using the Dial Gauge

The sample should be positioned on the diffractometer axis using the Z movement of the
PW3075/6x Positioning Stage. For most applications this can be done mechanically using the dial gauge (see
Figure 12.47). The reading corresponding to the Z = 0 position (that is, the correct sample height) is provided by
the PANalytical Service Engineer when the system is installed. Where the application requires data collection
at very low angles of incidence, the sample will need to be positioned so that it exactly intercepts the incident
beam when set parallel to it. This procedure is described in section 12.13.5.3.
is known to within a few micrometers. Therefore do not turn the
adjustment screw, rotate the outer rim of the gauge or drop the
gauge as these actions are likely to cause the gauge to become
uncalibrated.
for the delicate sample. Alternatively delicate samples can be aligned using the X-ray method described in
section 12.13.5.3.
Alignment of a sample for micro-diffraction experiments using an alignment microscope is described in section
10.4.1 in Chapter 10 in Part II of this User's Guide.
07.03.27 Page 12.69

Proceed as follows to align the sample height position mechanically:

1. Move the sample platform (with the sample mounted) to the lowest Z position.
2. Mount the dial gauge onto PreFIX U-block on the PW3075/6x Positioning Stage.
3. Carefully move the sample platform upwards in the Z direction using the data collector software. The
sample is at the correct height position when the reading of the dial gauge corresponds to the reference
value of the dial gauge provided.
4. Carefully remove the dial gauge from the positioning stage. In order not to scratch the sample or
otherwise damage it, you can lift the shaft of the dial gauge by lifting the black knurled knob at the top
of the dial gauge, while removing the dial gauge.
The sample is now adjusted at the correct height position.

When mechanical contact with the surface of the sample should be avoided, or when measurements are to be
performed at very low angles, the sample must be positioned so that it exactly intersects the incident beam when
set parallel to it. This section describes the procedure for standard experiments. Alignment of a sample for micro-
diffraction experiments using an alignment microscope is described in section 10.4.1 in Chapter 10 in Part II of
this User's Guide.
In order to align the sample using X-rays, the sample must be large and flat. The alignment procedure is as
follows:
slit) and report this to the data collector software. Use the smallest available opening, e.g. 1/32°
divergence slit.
center.
3. Set the goniometer axes 2theta and omega to 0° and move the sample platform on the positioning stage
to such a position that the direct X-ray beam is not obstructed by the sample or the positioning stage.
4. Insert a 0.2 mm Cu attenuation foil into the incident beam path in order to protect the detector.
5. Use a small receiving slit or the X'Celerator or the PIXcel in scanning mode to perform a 2θ scan
through the 2θ = 0° position using a small receiving slit to find the peak position of the direct X-ray
beam. Make a note of the 2θ-peak position.
6. Use the data collector software to recalibrate the 2θ = 0° position to coincide with the peak position of
the direct beam.
a. If you are using the PW3093/60 Programming Receiving Slit, set it to 3 mm.
b. If a programmable of fixed anti-scatter slit assembly is mounted onto the programmable receiving
slit, set it to 4°.
c. If you are using the X'Celerator, rotate it 90° (see section 21.4 in Chapter 21 of Part II of this User's
Guide) and set it to the receiving slit mode. Use the maximum length of 9 mm. Use the maximum
length of 9 mm. Do not insert a slit into the the fixed anti-scatter slits holder.
(Ip).
9. Move the sample, incrementing Z, until the direct beam intensity is between 50% and 60% of Ip.
Page 12.70 07.03.27
10. Make a small ω scan and move ω to the position at the peak intensity.
a. If no maximum is visible in the range, increase the ω range and rescan.
b. If a maximal intensity is achieved over this larger ω range, move ω to the center of this range and
repeat steps 9 and 10.
Legend:-0.5 (full red line),

-0.25 (dotted line),
0 (dashed line),
0.25 (dash-dotted line),
0.5 (full blue line) times the height of the direct beam.
Figure 12.50: Relative Intensity as a Function of the Tilt Angle
11. Move the sample with small increments of Z until the intensity is between 50% and 60% of Ip.
12. Adjust the Tilt of the sample, using small increments or decrements, until a maximum intensity is
reached.
a. If the intensity is more than or equal to Ip/2, the Tilt of the sample is correct. Continue with step 13.
b. If the intensity is less than Ip/2, decrease the Z position of the sample until the direct beam intensity
is between 50% and 60% of Ip and repeat step 12.
The relative intensity of the direct beam as a function of the tilt angle at different height positions of
the positioning stage is shown in Figure 12.50.
13. Move Z, using small increments, until the intensity equals Ip/2.
The sample is now aligned at optimal ω, Tilt and Z positions.
NOTES: If you are using an X’Celerator, rotate it back to its normal position before starting the
measurement.
07.03.27 Page 12.71

12.14 PW3076/00 TRANSMISSION SPINNER

The PW3076/00 Transmission Spinner is designed to rotate samples fitted in PW18xx sample holders about their
axis in transmission and reflection applications. The transmission spinner is shown in Figure 12.51, it can be Pre-
FIX mounted onto a vertical X'Pert PRO goniometer. The purpose of spinning is to bring more crystallites into
the diffraction position in order to reduce the influence of particle statistics on the measurements. Spinning gives
better results, especially in phase analysis and omega-stress measurements compared to “static” measurements.
The maximum sample mass (including the sample holder) is 150 g.
When a sample is correctly fitted into a PW18xx Sample Holder and loaded into the PW3076/00 Transmission
Spinner it is automatically adjusted to the correct sample height. The reference plane of the PW18xx Sample
Holder is flush with that of the sample spinner. Mounting samples is described in section 12.14.2.1.
The PW3076/00 Transmission Spinner can be used in reflection and transmission sample modes.
1. Transmission Mode: The (flat) sample is completely penetrated by the incident beam. The diffracted
beam leaves the sample at the other side. At an Omega setting of 0°, the incident beam is perpendicular
to the sample surface.
2. Reflection Sample Mode: The (flat) sample is partly penetrated by the incident beam. The diffracted
beam leaves the sample at the same side as the incident beam entered. At an Omega setting of 0°, the
incident beam is parallel to the sample surface.
Changing sample modes is described in section 12.14.2.2 below.
Figure 12.51: PW3076/00 Transmission Spinner in Transmission Sample Mode
12.14.1 Accessories
One circular sample holder is included with the PW3064/00 Sample Spinner. The sample holder is physically
the same as the PW1813/32 Sample Holder for Circular Samples. It is used to mount filters or solid samples with
a diameter between 30 mm and 32.3 mm and a maximum thickness of 6 mm. The circular silicon pressed powder
sample delivered with the X'Pert PRO diffraction system fits into this holder. More details about this type of
sample holder are given in Appendix A of this User's Guide (section A.2.1.5).
Page 12.72 07.03.27

The PW18xx Sample Holders are circular sample holders that can be loaded in the PW3076/00 Transmission
Spinner. These sample holders can also be used with the PW3064/x0 Sample Spinner, with the PW3072/60
Stationary Sample Stage, on the PW3074/00 Multi-purpose Sample Stage and on the PW3061/21 Sample
Holder for Solid Samples to be used with the PW3060/20 MRD cradle. A description of the PW18xx Sample
Holders and their applications is given in Appendix A of this User's Guide.

The PW3714/20 Motor supply is an electrical power supply unit for the spinner motor of the transmission
spinner. The unit is shown in Figure 12.4. It is manually operated by pressing the On-off button on the housing.
The motor supply can also be used in conjunction with the PW3062/00 Stage for Micro-diffraction and the
PW3063/00 Capillary Spinner. When you have more than one of these stages, you only need to have one power
supply unit present in your system. You can switch the power supply from one stage to another by disconnecting
the cable from the spinner that you have been using and then connecting it to the spinner that you are going to
use next. For more information about exchanging PreFIX sample stages, refer to section 12.1.1.
12.14.2 Use
12.14.2.1 Manually Loading a Sample
A sample fitted into a PW18xx Sample Holder can be manually loaded onto a PW3076/00 Transmission Spinner
as follows:
1. Place the sample holder onto its position on the sample spinner (see in Figure 12.51).
2. Click the sample holder into the stage so that it is brought into its reference position.
3. Check that the sample holder is positioned correctly so that the reference surface of the sample holder is
flush with the reference plane of the sample spinner. If the sample holder is not inserted correctly, the
sample will tilt during a spinning measurement. This will cause a sample height displacement resulting
in peak shift and defocusing and thus peak broadening and a weakening of the peak intensity.

The PW3076/00 Transmission Spinner can be used in transmission or in reflection mode. Changing from one
sample mode to another is performed by setting the required sample mode in the data collector software. The
actions that are executed automatically or manually depend on the type of X'Pert PRO MPD system and on the
sample mode that you are going to use. These actions are given in Table 12.13.
Table 12.13: Overview of Actions Required On Changing the PW3076/00 Transmission Spinner’s
Sample Mode
X'Pert PRO Action Performed by the

Changing Sample mode Manual Actions
System Data Collector Software
Theta- 2Theta From transmission to reflection Rotate omega axis -90° -

or
Alpha-1 From reflection to transmission Rotate omega axis +90° -
Theta-Theta From transmission to reflection - Rotate transmission spinner on
its axis 90° clockwise
From reflection to transmission - Rotate transmission spinner on

its axis 90° counter-clockwise
Rotating the transmission spinner on its axis is described in section 12.14.2.2.1.
07.03.27 Page 12.73

12.14.2.2.1 Rotating the Transmission Spinner on its Axis
In order to change the transmission spinner sample mode on an X'Pert PRO Theta-Theta system you must rotate
the transmission spinner on its axis with respect to the PreFIX interface through 90°. You do that as follows:
1. Loosen the setscrew (refer to Figure 12.51).
2. Carefully pull the alignment block a little distance (this distance must be less than 1 cm) away from
the PreFIX Interface, turn the cradle:
a. through 90º counter-clockwise when you are changing the cradle position from reflection to
transmission mode,
or
b. through 90º clockwise when you are changing the cradle position from transmission to reflection
mode.
3. Make sure that the alignment pins on the interface fit into the holes on the cradle and push the cradle
back against the PreFIX Interface.
4. Tighten the setscrew Y.
The transmission spinner is now ready for use. No alignment is required. Figure 12.52 shows the transmission
spinner in the reflection mode position.
Figure 12.52: PW3076/00 Transmission Spinner in reflection sample mode
Page 12.74 07.03.27

12.15 PW3077/00 HIGH-THROUGHPUT ATTACHMENT

The PW3077/00 High-throughput Attachment is a sample stage with motorized X, Y and Z movements,
controlled by the data collector. It allows the mapping of larger samples, or to measure several different samples
without the need to (dis)mount between the measurements. In combination with the X'Pert Operator Interface
software, the system is optimized for measurements on sample arrays where the samples are arranged in a grid
(for example: well plates). These well plates are commonly used in combinatorial chemistry, drug discovery,
polymorph screening or catalyst development. The high-throughput attachment can be PreFIX mounted onto an
X'Pert PRO Theta-Theta system. A special mounting procedure is described in section 12.15.2.1.
The high-throughput attachment can be used in two sample modes:

1. Reflection Sample Mode (refer to Figure 12.53): The (flat) sample is partially penetrated by the
incident beam. The diffracted beam leaves the sample at the same side as the incident beam entered. At
an Omega setting of 0°, the incident beam is parallel to the sample surface.
In the reflection geometry, the following optics are advised:
- Incident beam side: Programmable divergence slit with fixed anti-scatter slit, beam mask and Soller
slits. The slit and mask size should be chosen according to the well diameter to ensure that the
maximum area of the well is irradiated without irradiating the neighboring wells.
- Diffracted beam side: X'Celerator or PIXcel detector with programmable anti-scatter slit, Ni filter
and Soller slits
2. Transmission Sample Mode (refer to Figure 12.54): The (flat) sample is completely penetrated by the
incident beam. The diffracted beam leaves the sample on the other side. At an Omega setting of 0°, the
incident beam is perpendicular to the sample surface. For this sample mode, a PW3099/70 Large Offset
Arm must be mounted onto the diffracted beam arm to allow the detector to move underneath the
sample holder. A direct beam stop enabling measurements at low angles (down to 1° 2θ) is available.
We advise you to use the following optical configuration is for the transmission geometry:
- Incident beam side: Focusing X-ray mirror with fixed anti-scatter slit, beam mask and Soller slits.
The slit and mask size should be chosen according to the well diameter to ensure that the maximum
area of the well is irradiated without irradiating the neighboring wells.
- Diffracted beam side: X'Celerator detector with PW3494/30 Fixed Anti-scatter Slits Holder and
PW3494/35 Extension, Soller slits or the PIXcel detector with PW3490/00 Fixed Anti-scatter Slits
Holder and PW3494/35 Extension and Soller slits.
NOTES: Different optics may be advisable for other applications (please refer to Chapter 3 in Part I of this
User's Guide).
In the data collector software the PW3077/00 High-throughput Attachment is known as
“Programmable Stage (X,Y,Z)” for reflection sample mode and as “High-throughput Stage” for
transmission sample mode.
There are two PreFIX positions on the goniometer's stage interface associated with these two
sample modes. The high-throughput attachment must be mounted onto the relevant position as
described in section 12.15.2.3 below.
07.03.27 Page 12.75

Figure 12.53: X'Pert PRO Theta-Theta system with PW3077/00 High-throughput Attachment in
Reflection Sample Mode
Page 12.76 07.03.27

Figure 12.54: X'Pert PRO Theta-Theta system with PW3077/00 High-throughput Attachment in
Transmission Sample Mode
The specifications of the motorized movements of the PW3077/00 High-throughput Attachment are given in
Table 12.14.
Table 12.14: PW3077/00 High-throughput Attachment - Specifications
Adjustable Axis X Y Z
Range 100 mm 100 mm 11 mm
Minimum step size 0.01 mm 0.01 mm 0.001 mm
Reproducibility 0.1 mm 0.1 mm 0.001 mm

Slew speed 20 mm/s 20 mm/s 1 mm/s
NOTE: The optical configuration used may limit the ranges of the X, Y and Z movements. Use the option
in the data collector software to set more stringent limits for the motorized movements in order to
prevent collisions between the sample stage and the optical modules in your configuration.
The sample stage can be oscillated in the X and Y directions to decrease the effect of particle statistics.
Oscillation ranges depend on the sample mode used. Information about oscillation ranges is given in Table 12.15
below. Oscillations can be combined with wobbling of the sample orientation during measurements.
07.03.27 Page 12.77

Table 12.15: PW3077/00 High-throughput Attachment - Oscillation Ranges
Sample Mode Range Step
Reflection 5 mm - 100 mm 5 mm
Transmission 1 mm - 20 mm 1 mm
The reference plane of the PW3077/00 in reflection sample mode can be determined mechanically using a dial
gauge.
In transmission sample mode, samples are often inserted into well plates. In order to mount well plates onto the
high-throughput attachment, special well plate holders must be designed for the type of well plates that you are
going to use in the high-throughput screening applications.
In reflection sample mode samples (including their sample holders) can have a maximum diameter of 120 mm
(X movement range can be limited depending on sample size and configuration used), a maximum height of 24
mm, and a maximum mass of 0.5 kg. A multiple-sample holder for reflection applications is available and
described in section 12.15.2. Well plates can also be used as sample holders for reflection applications.
Mounting of sample holders onto the high-throughput attachment is described in section 12.15.2.
12.15.1 Accessories
12.15.1.1 Dial Gauge
A dial gauge for sample height alignment purposes in reflection sample mode is supplied with the PW3077/00
High-throughput Attachment. It is shown in Figure 12.55. It can be mounted onto the dial gauge holder as
indicated in Figure 12.53. The use of the dial gauge for mechanical alignment of the height (Z position) of the
sample mounted onto the high-throughput attachment is described in section 12.15.2.5.
Figure 12.55: Dial gauge for High-throughput Attachment
Page 12.78 07.03.27

12.15.1.2 Multiple-sample Holder for Reflection Sample Mode

A multiple-sample holder for reflection applications is supplied with the PW3077/00 High-throughput
Attachment. It is mounted and factory aligned onto the sample stage. It provides space for 12 samples or sample
holders with a diameter of 25 mm such as the PW1819/25 Zero-background Holders. This type of sample hloder
is described in Appendx A of this User’s Guide (section A.3.2). The multiple sample holder can also be used as
a mounting platform for well plate holders for transmission applications.
Figure 12.56: Multiple Sample Holder for Reflection Sample Mode
12.15.1.3 Well Plate Holder for Transmission Sample Mode

Well plates used as sample holders for transmission applications can be mounted into special well plate holders.
These holders are mounted onto the PW3077/00 High-throughput Attachment, such that they are flush with the
diffraction plane. The well plate holders are specifically designed for the type of well plate you are using in high-
throughput screening applications. An example is shown in Figure 12.57. Mounting of well plate holders onto
the high-throughput attachment is described in section 12.15.2.4. Sample height adjustment is described in
section 12.15.2.6.
Figure 12.57: Example of Well-plate Holder for High-throughput Screening Applications
07.03.27 Page 12.79

12.15.1.4 Direct Beam Stop

A direct beam stop can be mounted onto the high-throughput attachment mounted in transmission sample mode.
Using the beam stop allows transmission measurements with the focusing X-ray mirror with a minimum 2θ angle
in the range between 1° and 2.5°. The direct beam stop is shown in Figure 12.58.
Figure 12.58: Direct Beam Stop for Transmission Measurements with the
PW3077/00 High-throughput Attachment
12.15.1.4.1 Mounting the Direct Beam Stop onto the High-throughput Attachment
Mount the direct beam stop onto the PW3077/00 High-throughput Attachment as follows:
1. Make sure that the high-throughput attachment is mounted in transmission sample mode; the procedure
to change the sample mode is given in section 12.15.2.3.
2. Bring the direct beam stop into its position on the high-throughput stage interface, so that the mounting
pins fit into the holes, see Figure 12.59.
3. Fasten the direct beam stop to the attachment using the M3 x 16 screws supplied.
Now you can proceed with aligning the direct beam stop.
Page 12.80 07.03.27

Figure 12.59: Direct Beam Stop Mounted onto the High-throughput Stage Interface
The height setting of the beam stop is adjustable. Align the beam stop as follows:
1. If there is a sample present, remove it from the sample stage.
Chapter 1 in Part II of this User's Guide.
3. Ensure that the direct X-ray beam passes through 2θ = 0°. Use a beam attenuator to protect your your
detector from saturation; make sure that the X-ray beam is not blocked by a beam stop or the sample
stage.
5. Mount the focusing X-ray mirror with the PW3086/70 Incident Beam Anti-scatter Device (without
beam stop assembly) onto the incident beam PreFIX position of the X'Pert PRO MPD system.
6. Insert a 1/2° divergence slit, a 1/2° or 1/4° anti-scatter slit (the one that you are going to use in your
experiments) and a 0.04 rad or smaller Soller slits assembly into their appropriate positions in the
focusing X-ray mirror.
7. If you are using an X'Celerator or PIXcel, set it to scanning mode; if you are using a PW3093/60
Programmable Receiving Slit, set it to 0.1 mm. If a Programmable Anti-scatter Slit is mounted onto the
X'Celerator or the PIXcell or the Programmable Receiving Slit, set it to 1/32°. If you have a fixed anti-
scatter device mounted onto the X’Celerator or the PIXcel, use the advised combination as given in
Table 6.12 or Table 6.13 in Chapter 6 of Part II of this User’s Guide.
8. Set ω = 0° and make a 2θ scan around 2θ = 0°, for example: from -1° to 3° 2θ. Use the same scan type
and omega-offset as used in the experiments that you are going to perform. A typical result of this scan
is shown in Figure 12.60.
07.03.27 Page 12.81

Intensity [cps]
3600
1600
400
0
-0.8 -0.6 -0.4 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8
2theta [deg.]
Figure 12.60: Typical Scan Around 2θ = 0°

a. If your scan shows a narrow peak around 0.7º 2θ, a flat background from 1° 2θ upwards (the
minimum 2θ from where you can start your measurement) as shown in Figure 12.60, then your
beam stop is correctly aligned. You can skip the steps given below.
c. If your scan shows a broad line, or an irregular background around 2º 2θ, then your beam stop is set
too low and must be raised.
11. Depending on the result obtained in step 9, follow the procedure given in either step a or b below:
a. In order to lower the beam stop: loosen the upper setscrew by turning it (using a 1.5 Allen key)
about 45° (or less for smaller steps) and then tighten the lower setscrew by the same amount. Make
b. In order to raise the beam stop: loosen the lower setscrew by turning it (using a 1.5 Allen key)
about 45° (or less for smaller steps) and then tighten the upper setscrew by the same amount. Make
Page 12.82 07.03.27

12.15.1.5 PW3099/70 Large Offset Arm

The PW3099/70 Large Offset Arm is an accessory that is used to support the transmission sample mode on
X'Pert PRO Theta-Theta systems equipped with a PW3064/60 Reflection-transmission Spinner or a PW3077/
00 High-throughput Attachment. It is designed as a PreFIX module with an offset of approximately -60º 2theta.
It is mounted on the goniometer's diffracted beam PreFIX position and provides a position to mount a diffracted
beam PreFIX module. The PW3099/70 Large Offset Arm is shown in Figure 12.61. The large-offset arm
mounted onto an X'Pert PRO goniometer is shown in Figure 12.67.
Figure 12.61: PW3099/70 Large Offset Arm
12.15.2 Use
The PW3077/00 High-throughput Attachment can be PreFIX mounted onto an X'Pert PRO Theta-Theta system
and removed from it. It can be used in reflection and transmission sample modes. A special PreFIX mounting
procedure and sample mode changing procedure, as well as sample (holder) alignment are described in this
section.
12.15.2.1 Mounting the PW3077/00 High-throughput Attachment onto the X'Pert

PRO Theta-Theta System
This section describes the mounting procedure for the PW3077/00 High-throughput Attachment onto the X'Pert
PRO Theta-Theta X-ray diffraction system. This procedure is supported by the data collector software.
Mounting of other PreFIX sample stages is described in section 12.1.1.
Proceed as follows to exchange a PreFIX sample stage with a High-throughput attachment:

sample stage. Also, you can now, if necessary, remove the optical modules and the sample.
2. Go off-line with the data collector software (Disconnect).
07.03.27 Page 12.83

instructions given by the X'Pert Wizard ‘Exchange Sample Stage” that then appear. Note that you can
only do that when the instrument is off-line (disconnected). The manual actions that you need to
perform are described below.
4. Go on-line with the data collector software using the configuration containing the PW3077/00 High-
throughput Attachment in the sample mode that you just have mounted.
NOTE: The High-throughput Attachment is called “Programmable Stage (X,Y,Z)” in the data collector
software, when it is used in reflection sample mode, and “High Throughput Stage”, when it is used
in transmission sample mode.
5. Mount the optical modules required for your measurements. The system is now ready for use.
In the procedure described above, the X'Pert Wizard will instruct you to dismount the PreFIX sample stage and
mount the High-throughput Attachment. We will describe here the manual actions required for this procedure.
1. Loosen the four securing screws (see Figure 12.1) and remove the PreFIX sample stage.
Figure 12.62: X'Pert PRO MPD Theta-Theta System after Removal of Sample Stage and Optical
Modules
2. Loosen the four interface securing screws (see Figure 12.62) and remove the PreFIX stage interface
from the goniometer (see Figure 12.63). Make sure that you hold it so that it doesn’t fall down.
Page 12.84 07.03.27

Figure 12.63: PreFIX Stage Interface Dismounted from the X'Pert PRO Goniometer
3. Carefully mount the High-throughput Attachment interface onto the X'Pert PRO goniometer (see
Figure 12.64) and secure it with the four screws supplied. Ensure that the interface fits properly on the
locating pins. When the interface is mounted correctly, the right-hand side edge of the interface is flush
with the metal squares on the goniometer.
07.03.27 Page 12.85

Figure 12.64: Mounting the High-throughput Stage Interface onto the X'Pert PRO Goniometer
4. The High-throughput stage interface has two PreFIX mounting positions to mount the PW3077/00
High-throughput Attachment (see Figure 12.64). The PreFIX mounting position nearest to you is used
for mounting the High-throughput Attachment in transmission sample mode. The PreFIX mounting
position closest to the goniometer is used for mounting the High-throughput Attachment in reflection
sample mode. Install the High-throughput Attachment on the PreFIX mounting positions required (see
Figure 12.65).
Page 12.86 07.03.27

Figure 12.65: High-throughput Attachment Mounted onto the X'Pert PRO Goniometer
5. If you have mounted the High-throughput Attachment in transmission sample mode, you must mount
the PW3099/70 Large Offset Arm onto the diffracted beam PreFIX position (see Figure 12.54) to allow
the movement of the detector underneath the stage.
This concludes the manual actions required in the X'Pert Wizard’s instructions.
12.15.2.2 Dismounting the PW3077/00 High-throughput Attachment from the

X'Pert PRO Theta-Theta system
This section describes the dismounting procedure for the PW3077/00 High-throughput Attachment from the
X'Pert PRO Theta-Theta X-ray diffraction system. This procedure is supported by the data collector software.
Mounting of other PreFIX sample stages is described in section 12.1.1.
Proceed as follows to exchange the High-throughput attachment with a PreFIX sample stage:
sample stage. You can now, if necessary, remove the optical modules (including, if present, the large
offset arm) and the sample.
instructions given by the X'Pert Wizard “Exchange Sample Stage” that then appear. Note that you only
can do that when the instrument is off-line (disconnected). The manual actions that you need to perform
are described below.
4. Go on-line with the data collector software using the configuration containing the PreFIX sample stage
that you just have mounted.
5. Mount the optical modules required for your measurements. The system is now ready for use.
In the procedure described above, the X'Pert Wizard will instruct you to dismount the High-throughput
Attachment and mount a PreFIX sample stage. We will describe here the manual actions required for this
procedure.
07.03.27 Page 12.87

1. Loosen the PreFIX screw and remove the High-throughput Attachment from the X'Pert PRO
goniometer (see Figure 12.64).
2. Loosen the four interface securing screws and remove the High-throughput stage interface from the
X'Pert PRO goniometer (see Figure 12.66).
Figure 12.66: Dismounting the High-throughput Stage Interface from the X'Pert PRO Goniometer
3. Mount the PreFIX stage interface and secure the four interface securing screws (see Figure 12.62).
Ensure that the stage interface fits properly on the locating pins. When the interface is mounted
correctly, the right hand side edge of the interface is flush with goniometer.
4. Bring the new PreFIX sample stage into position so that it fits over the PreFIX alignment blocks on the
goniometer (see Figure 12.2). The hinged clip at the top will hold the sample stage in position, allowing
you two hands free to tighten the securing screws.
5. Tighten the four securing screws.
This concludes the manual actions required in the X'Pert Wizard’s instructions.
Page 12.88 07.03.27

12.15.2.3 Changing Sample Mode

This section describes the switching procedure for the PW3077/00 High-throughput Attachment from reflection
to transmission sample mode and vice versa. This procedure is supported by the data collector software. To
change the sample mode, proceed as follows:
1. Move the arms of the goniometer to a position where you have easy access to the PreFIX screw holding
the sample stage. You can now, if necessary, remove the optical modules (including, if present, the
large offset arm) and the sample holder.
3. In the data collector software select the menu item Tools - Exchange Sample Stage.
4. Follow the instructions given by the X'Pert Wizard “Exchange Sample Stage” that then appear. Select
the sample stage that you are going to use.
NOTE: The High-throughput attachment is called “Programmable Stage (X,Y,Z)” in the data collector
software, when it is used in reflection sample mode, and “High Throughput Stage”, when it is used
in transmission sample mode.
5. Loosen the PreFIX screw and remove the High-throughput attachment from its PreFIX position on the
high-throughput stage interface (see Figure 12.64). Mount the high-throughput attachment onto the
other PreFIX position on the stage interface and tighten the PreFIX screw.
6. Go on-line with the data collector software using the configuration containing the high-throughput
attachment in the sample mode that you just have installed.
7. If you have mounted the high-throughput attachment in transmission sample mode, you must mount the
PW3099/70 Large Offset Arm onto the diffracted beam PreFIX position (see Figure 12.67) to allow the
movement of the detector underneath the stage. The large offset arm must be removed for reflection
applications.
8. Mount the optical modules required for your measurements. You can now mount the sample holder
onto the sample stage. If you are using reflection sample mode, you can mount the sample holder
directly on the stage's sample platform. If you are using transmission sample mode, first you must
mount a well plate holder onto the sample platform. This procedure is described in section 12.15.2.4.
12.15.2.4 Mounting and Aligning of a Well Plate Holder for Transmission

Applications
In transmission sample mode, samples are often placed in well plates. Before you can mount a well plate onto
the high-throughput attachment, you must mount a special well plate holder, designed for the type of well plates
that you are using in high-throughput screening applications, onto the sample platform.
To mount the well plate holder onto the sample platform, proceed as follows:
1. Ensure that the High-throughput Attachment is configured for transmission applications. See also
section 12.15.2.3.
2. Bring the well plate holder into position on the sample platform, as is shown in Figure 12.67 and fix the
holder to the platform with the two securing screws supplied. There are marker lines for the well plate
holder on the sample platform.
3. Now you can put your well plate into its position on the well plate holder.
Height alignment of sample holders is described in section 12.15.2.5.
07.03.27 Page 12.89

Figure 12.67: Mounting the Well Plate Holder onto the Sample Platform
12.15.2.5 Mechanical Sample (Stage) Height Alignment

The sample holder should be positioned using the Z movement of the High-throughput Attachment such that the
holder's reference plane is on the diffractometer axis. For most reflection applications this can be done
mechanically using the dial gauge supplied (see Figure 12.55). The reading corresponding to the Z = 0 position
(that is, the correct sample height) is provided by the PANalytical Service Engineer when the system is installed.
Where it is undesirable to make mechanical contact with the top surface of a sample, a sample of identical
thickness should be aligned and the same Z setting used for the delicate sample. Alternatively delicate samples
can be aligned using the X-ray method describe in section 12.15.2.6.
Proceed as follows to mechanically align the sample height position:

1. Move the sample platform (with the sample mounted) to the lowest possible Z position.
2. If necessary, move the sample platform to a position in X and Y where the dial gauge can touch the
surface without damaging it.
3. Mount the dial gauge onto the dial gauge holder on the high-throughput attachment.
dial gauge as provided by the PANalytical Service Engineer when the system was installed.
Page 12.90 07.03.27

is known to within a few micrometers. Do not therefore turn the
adjustment screw, pull on the long arm of the dial gauge assembly,
rotate the outer rim of the gauge or drop the gauge as these
actions are likely to cause the gauge to lose calibration.
7. Remove the dial gauge from the dial gauge holder on the high-throughput attachment.
12.15.2.6 Sample Height Alignment Using X-rays

For most accurate height adjustment in transmission and reflection sample modes, we recommended that you
make use of a reflection of a known reference material. A low absorbing material, such a silicon or aluminium
oxide powder, is preferred for transmission applications. To perform a height alignment of the sample holder
using X-rays, proceed as follows:
1. Make sure that the tube height is correctly aligned (refer to Chapter 1 of Part II of this User's Guide and
that the direct beam is at 2θ = 0° position of the detector.
2. Mount the sample holder with the reference sample onto the high-throughput attachment.
3. Mount the optical modules that you are going to use in your experiments onto the incident and
diffracted beam PreFIX positions.
center.
5. Perform a small 2θ-θ scan (gonioscan) on a reflection of the known reference material. If you use
silicon powder, we recommend you to use the Si(111) reflection at 2θ = 28.440°.
6. If the reflection is not found at the required 2θ position, move the sample stage over a small distance in
the Z direction and perform the small scan again. Keep repeating this step until you have found the
reflection at the known 2θ position.
The sample holder is now at the correct Z-height position.
12.15.2.7 Performing Measurements

The PW3077/00 High-throughput Attachment is controlled by the X'Pert Data Collector. You can use the data
collector software to define all the measurements you need to perform on your samples. For measurements on
sample arrays arranged in a grid, such as in well plates, you can use the X'Pert Operator Interface. This software
program is specifically designed to automate measurements in fixed grids. For setting up measurements on
samples in fixed grids in batch mode, refer to the X'Pert Data Collector Quick Start Guide (4022 339 07601) or
the X'Pert Operator Interface Quick Start Guide (4022 339 07901).
07.03.27 Page 12.91

Page 12.92 07.03.27

Chapter 13
Non-ambient Chambers
Contents
13.1 General............................................................................................................................... 13 - 3
13.2 PreFIX Non-ambient Chambers ..................................................................................... 13 - 3
13.2.1 Use ....................................................................................................................................... 13 - 5
13.2.1.1 Mounting Non-ambient Chambers ...................................................................... 13 - 5
13.2.1.2 Adjusting the Sample Height in a Non-ambient Sample Chamber ..................... 13 - 6
13.2.1.3 Adjusting the Sample Height using the PC-controllable Alignment Stage ......... 13 - 7
13.2.2 9430 500 27841 TTK 450 Low Temperature Attachment ................................................ 13 - 12
13.2.2.1 Accessories ........................................................................................................ 13 - 12
13.2.2.2 Use ..................................................................................................................... 13 - 16
13.2.3 9430 500 20711 HTK 1200N High Temperature Oven-chamber, Rigid System ............. 13 - 20
13.2.3.1 Accessories ........................................................................................................ 13 - 21
13.2.4 9430 500 20721 HTK 1200N High Temperature Oven-chamber, Spinner System.......... 13 - 22
13.2.4.1 Accessories ........................................................................................................ 13 - 22
13.2.5 9430 500 27761 HTK 16 High Temperature Chamber..................................................... 13 - 23
13.2.5.1 Accessories ........................................................................................................ 13 - 23
13.2.6 9430 500 28271 HTK 2000 High Temperature Attachment............................................. 13 - 24
13.2.6.1 Accessories ........................................................................................................ 13 - 25
13.2.7 9430 500 21021 XRK 900 Reactor Chamber.................................................................... 13 - 26
13.2.7.1 Accessories ........................................................................................................ 13 - 26
13.2.8 9430 500 21031 XRK 900 Reactor Chamber Spinner ...................................................... 13 - 27
13.2.8.1 Accessories ........................................................................................................ 13 - 27
13.3 9430 500 20371 Temperature Controlled Humidity Chamber................................... 13 - 28
13.3.1 Accessories ........................................................................................................................ 13 - 30
13.3.1.1 9430 500 20121 Vacuum Equipment ................................................................ 13 - 30
13.3.1.2 9430 500 20381 Humidity Generator ................................................................ 13 - 30
13.3.1.3 Temperature Bath .............................................................................................. 13 - 31
13.3.1.4 9430 500 28361 Adaptor TTK-PW3050/6x ...................................................... 13 - 32
13.3.1.5 9430 500 21161 PC-controllable Alignment Stage ........................................... 13 - 32
07.03.27 Page 13.1

13.3.2 Use ..................................................................................................................................... 13 - 33

13.3.2.1 Experimental Set-up of the Temperature Controlled Humidity System ............ 13 - 33
13.3.2.2 Mounting the Temperature Controlled Humidity Chamber............................... 13 - 33
13.3.2.3 Adjusting the Sample Height of a Humidity Chamber ...................................... 13 - 34
13.3.2.4 Adjusting the Sample Height Using the PC-controllable Alignment Stage ...... 13 - 35
13.3.2.5 Operation............................................................................................................ 13 - 40
13.3.2.6 Switching Off the Temperature Controlled Humidity System .......................... 13 - 43
13.3.2.7 Dismounting the Temperature Controlled Humidity Chamber ......................... 13 - 43
13.3.2.8 References .......................................................................................................... 13 - 43
13.4 Cryostream Plus ................................................................................................................1 - 44
13.4.1 Accessories ........................................................................................................................ 13 - 45
13.4.1.1 Capillary Spinner with PreFIX Mounting Position............................................ 13 - 45
13.4.1.2 Screening Plate for Goniometer Head................................................................ 13 - 46
13.4.1.3 Dewar Vessel ..................................................................................................... 13 - 46
13.4.1.4 Direct Beam Stop for Focusing X-ray Mirror.................................................... 13 - 46
13.4.1.5 Cryostream Controller........................................................................................ 13 - 47
13.4.1.6 Nitrogen Gas Pump Unit .................................................................................... 13 - 48
13.4.1.7 Dry Air Unit ....................................................................................................... 13 - 49
13.4.1.8 Auto-refill Unit................................................................................................... 13 - 50
13.4.2 Use ..................................................................................................................................... 13 - 51
13.4.2.1 Experimental Set-up of the Non-ambient Capillary Measurement System ....... 13 - 51
13.4.2.2 Setting up the Non-ambient Capillary Measurement System ............................ 13 - 52
13.5 PheniX Helium Powder Cryostat.....................................................................................1 - 54
13.5.1 Accessories ........................................................................................................................ 13 - 55
13.5.1.1 Temperature Control Unit .................................................................................. 13 - 55
13.5.1.2 Vacuum System ................................................................................................. 13 - 55
13.5.1.3 Cryodrive Compressor ....................................................................................... 13 - 56
13.5.1.4 PC-controllable Alignment Stage ...................................................................... 13 - 56
13.5.2 Use ..................................................................................................................................... 13 - 56
13.5.2.1 Experimental Set-up........................................................................................... 13 - 56
13.5.2.2 Setting up the Cryostat System for Low Temperature Measurements .............. 13 - 57
13.5.2.3 Mounting a Sample onto the Sample Position ................................................... 13 - 58
13.5.2.4 Switching the system on and cooling down ....................................................... 13 - 59
13.5.2.5 Adjusting the Sample Height Using the PheniX Height Controller .................. 13 - 61
13.5.2.6 Switching Off the Vacuum System and Releasing the Vacuum in the PheniX. 13 - 64
Page 13.2 07.03.27

Part II - Chapter 13: Non-ambient Chambers
13.1 GENERAL
can be measured or analyzed. The sample platforms used on X'Pert PRO systems.
s can be divided into six groups, they are:

• the all-purpose MRD cradle described chapter 11.
• PreFIX sample stages for X’Pert PRO MPD systems described in chapter 12.
• PreFIX high-throughput attachment described in chapter 12.
• PreFIX non-ambient sample stages described in this chapter.
• PreFIX temperature controlled humidity chamber described in section 13.2.
• PreFIX cryogenic temperature controlled sample stages described in sections 13.4 and 13.5.
In this chapter we will provide you with information about the non-ambient chambers.
13.2 PREFIX NON-AMBIENT CHAMBERS

Non-ambient chambers are used to analyze samples at high or low temperatures in various atmospheric
conditions or in a vacuum. The non-ambient chambers described in this section are manufactured by Anton Paar
GmbH, Graz, Austria. An overview of the available types of non-ambient chambers with references to the
sections in which they are described is given in Table 13.2. The temperature controlled humidity chamber is
described in section 13.3.
Separate manuals for the non-ambient chambers and their control units are delivered together with the chambers
themselves, please refer to these manuals for correct operation of the non-ambient chambers. This section
provides an overview of the non-ambient chambers that are available for X’Pert PRO and their accessories.
The non-ambient chambers are designed to be used on vertical X’Pert PRO MPD diffraction systems. They are
mounted onto a PreFIX sample stage interface and can be interchanged with other (non-ambient) sample stages
without needing realignment. Mounting instructions are given in section 13.2.1.
07.03.27 Page 13.3

Table 13.1: Overview of Available Non-ambient Chambers

Type Temperature Temperature Pressure
Item Atmosphere Section
Number Control Unit Range range
9430 500 TTK 450 TCU 100 -193 ºC to 450 ºC Under vacuum Vacuum 13.2.2
27841 to 1.3 bar
RT to 450 °C In inert gas
RT to 300 °C In air
9430 500 HTK 1200N TCU 1000N RT to 1200 ºC In air, inert gas or Vacuum 13.2.3
20711 Rigid System under vacuum to 2.0 bar
9430 500 HTK 1200N TCU 1000N RT to 1200 ºC In air, inert gas or Vacuum 13.2.4
20721 Spinner under vacuum to 2.0 bar
System
9430 500 HTK 16 TCU 2000 RT to 1450 ºC In air, inert gas or Vacuum 13.2.5
27761 under vacuum, to 1.0 bar
with use of Pt
filament
(permanent
operation)
RT to 1600 ºC In air, inert gas or

under vacuum,
with use of Pt
filament (short-
term operation;
max. 3 hours)
RT to 1500 °C Under vacuum

with use of
Ta filament
RT to 400 °C In air, inert gas
with use of
Ta filament
9430 500 HTK 2000 TCU 2000/20 RT to 2300 ºC Under vacuum Vacuum 13.2.6
28271 with use of
W filament
RT to 1450 °C In air, inert gas Vacuum

with use of Pt fila- to 1.0 bar
ment (permanent
operation)
RT to 1600 ºC In air, inert gas Vacuum

with use of Pt to 1.0 bar
filament (short-
term operation;
max. 3 hours)
9430 500 XRK 900 TCU 750 RT to 900 ºC Reducing, inert or 1 mbar to 13.2.7
21021 Rigid System oxidizing 10 bar
atmosphere
RT to 750 °C In helium 1 mbar to

10 bar
9430 500 XRK 900 TCU 750 RT to 900 ºC In air, inert gas or 1 mbar to 13.2.8
21031 Spinner under vacuum 10 bar
System
RT to 750 °C In helium 1 mbar to
10 bar
Page 13.4 07.03.27

13.2.1 Use
13.2.1.1 Mounting Non-ambient Chambers
This section describes how to mount non-ambient chambers onto an X’Pert PRO MPD system.
1. Make sure that you do not have any other stage mounted.
2. Make sure that you have available to you the four securing screws with hexagonal heads (M6 x 20) that
are delivered with the system.
3. Very loosely (about 3 turns) put the four screws into the outer holes on the sample stage PreFIX mount
(see Figure 13.1).
Figure 13.1: X’Pert PRO Goniometer with Hexagonal Head Securing Screws
Figure 13.2: Putting the Banana Shaped Securing Clip into Position
07.03.27 Page 13.5
4. Place the non-ambient chamber over the four screws and locate it into position using the three
positioning lugs and the hinged clip at the top.
5. Put the securing clips (one on each side) between the washers on the screws and the non-ambient
chamber as shown in Figure 13.2.
6. Tighten the screws using an M10 wrench. The non-ambient chamber is now ready for further actions.
Figure 13.3: Non-ambient Chamber fitted onto an X’Pert PRO MPD System
13.2.1.2 Adjusting the Sample Height in a Non-ambient Sample Chamber

This section describes the adjustment of the sample height using a reference sample.
1. Place a reference sample (for example: a silicon or aluminium oxide powder sample) into the non-
ambient chamber.
2. You can, if you wish, mount the dial gauge so that you can note the optimum sample height for future
use.
3. Use the data collector software to make a measurement as follows:
a. Set 2θ to the required angle according to the characteristic radiation of the X-ray tube and the
offset to 0º in order to measure a known reflection of your reference sample by making a short
2θ - θ scan. Data for the Si(111) reflection are given in Table 13.2.
b. Open the shutter and monitor the intensity while you use the Anton Paar PC-controllable
alignment stage in manual operation mode to move the chamber up and down until you reach
a maximum.
If you do not have a motorized chamber you will have to: close the shutter, open the enclosure
doors, adjust the height according to the procedure for height alignment given in the non-ambient
chamber’s instruction manual, close the doors, open the shutter, measure again, and so on.
Page 13.6 07.03.27

Table 13.2: 2θ Angle of the Si(111) and Si(311) Reflections for Different Types of Characteristic
Radiation
Characteristic
Si(111) Si(311)
Radiation
Mo Kα1 12.979º 25.009º
Cu Kα1 28.420º 56.103º
Co Kα1 33.124º 66.199º
Fe Kα1 35.937º 72.455º
Cr Kα1 42.796º 88.686º
CAUTION
Ensure that you do not exceed the maximum allowed count rate for
the detector used.
4. Set 2θ to another of your reference sample’s known reflections. Data about the angle for the Si(311)
reflection are given in Table 13.2.
Make a short 2θ - θ scan over about 1º, around this angle and check that the resulting peak is within
0.02º.
If this is not the case, check that the four screws holding the non-ambient chamber in position are tight,
check that you have reported the correct PreFIX optical modules to the data collector software, and start
this procedure again at step 3.
5. When you have completed the height adjustment, make a note of the height indication on the dial gauge
(if mounted) and remove the dial gauge.
6. Remove the reference sample and mount the sample that you want to measure. If the sample is correctly
mounted, the sample height is automatically correct.
13.2.1.3 Adjusting the Sample Height using the PC-controllable Alignment Stage
If your non-ambient chamber is mounted onto a PC-controllable alignment stage (9430 500 21161 for TTK 450,
9430 500 21171 for HTK 1200N, HTK 16 and HTK 2000 or 9430 500 21181 for XRK 900), you then have the
option to automatically correct the sample height position for temperature effects. The PC-controllable
alignment stage is shown in Figure 13.4.
Proceed as follows to use the PC-controllable alignment stage:

1. Switch the alignment stage controller on. Normally the alignment stage controller is built into the
instrument enclosure in such a way that the controller is switched on when the X'Pert PRO system is
switched on. If it is not built in, you can switch on the alignment stage controller using the main switch
at the rear of the alignment stage controller (see Figure 13.6). The green LED at the front side of the
controller indicates that the controller is switched on.
07.03.27 Page 13.7

Figure 13.4: PC-controllable Alignment Stage
Figure 13.5: Alignment Stage Controller - Front
Page 13.8 07.03.27

Figure 13.6: Alignment Stage Controller - Rear

2. Connect the data collector software to the X'Pert PRO system with a configuration that contains the
non-ambient chamber that you are going to use.
3. Start the AP Stage Mover program from the PC that controls your X'Pert PRO system.
Figure 13.7: Opening AP Stage Mover

4. When you are using the AP Stage Mover for the first time, open the menu item: Tools - Options and
insert the following information:
a. Insert the folder and file names of the Temperature File. Normally the Temperature File is stored
under the name D:\temperature.txt.
b. Select the correct COM port for the communication between the PC and the alignment stage
controller.
07.03.27 Page 13.9

Figure 13.8: AP Stage Mover - Options Menu
NOTE: The Temperature File contains the current temperature value of the non-ambient chamber, stored
by the data collector software. This file is read by the AP Stage Mover to automatically adjust the
sample height position as a function of temperature. The file name and location must also be
specified in the data collector software's initialization file “xpert.ini”. After a default installation
this file can be found in the folder:
C:\Program Files\PANalytical\X'Pert Data Collector.
To specify the temperature file name and location, add the following line in the xpert.ini file under
the section header “[Diffractometer communication]”: “NALogFile=<path><file name>.<file
extension>”, for example:
...
[Diffractometer communication]
NALogFile=d:\Temperature.txt
...
5. Initialize the system using the menu item: Tools - Initialize.
NOTE: The Initialize command has to be executed after every start of the AP Stage Mover program.
If the alignment stage controller is not initialized, a hardware initialization procedure is started
automatically, the procedure involves the following steps:
- The alignment stage moves downwards until it reaches the lower limit switch, indicated by a
yellow LED.
- The alignment stage moves upwards until the switch opens. This position is defined as the
“mechanical” zero position of the alignment stage. The reproducibility of the mechanical zero
position after initialization is ±2 μm.
- The alignment stage moves upwards 100 μm.
Now you can use the AP Stage Mover in two modes of operation, displayed in the user interface as tabs:
Manual mode
In the manual mode the alignment stage can be moved relative to the present position or as an absolute movement
with respect to the defined zero position. This mode is used in the sample stage alignment procedure (refer to
section 13.2.1.2) or when no temperature data are available for automated adjustment. After you have adjusted
the sample to the correct sample height at room temperature in the manual mode, you can use Tools - Define Zero
to calibrate it for automatic sample height alignment as a function of temperature in the automatic mode.
Page 13.10 07.03.27

Figure 13.9: AP Stage Mover - Manual Operation Mode
Automatic mode
In the automatic mode the AP Stage Mover reads the temperature value stored by the data collector in the
temperature file and adjusts the sample height position automatically according to a pre-selected adjustment
table. A set of Anton Paar defined tables is available in the program; user-defined tables can be created. Select
the table that you are going to use from the table drop-down box.
Use the and buttons in order to switch on and off the automatic height adjustment.
Figure 13.10: AP Stage Mover - Automatic Operation Mode
Refer to the Anton Paar manual “PC-controllable alignment stage Instruction Manual” (document number
B08IB03) and the data collector's software help for further details about the use of the PC-controllable alignment
stage.
07.03.27 Page 13.11

13.2.2 9430 500 27841 TTK 450 Low Temperature Attachment

The TTK 450 low temperature attachment allows temperature studies by X-ray methods at temperatures from
approximately -193 ºC to 450 ºC under vacuum or from room temperature to 300 ºC in air, or to 450 ºC in inert
gas. The delivery includes the complete chamber TTK 450 (AP70056), the temperature control unit TCU 100
(AP70057) and a simple water control device (AP70067). When the product is delivered the TTK 450 is factory
mounted onto a PreFIX adaptor (9430 500 28361 or 9430 500 21161). Vacuum equipment (9430 500 20121),
low temperature equipment (9430 500 27851) and Dewar vessels (9430 500 20141 and 9430 500 20341) can be
ordered as accessories.
Please refer to the Anton Paar manuals “TTK 450 Low Temperature Chamber Instruction Manual” (document
number A31IB02) and “TCU 100 Temperature Control Unit Instruction Manual” (document number B39IB06)
for further details.
13.2.2.1 Accessories
13.2.2.1.1 9430 500 20121 Vacuum Equipment TTK
The vacuum equipment (AP58974) for TTK 450 (9430 500 27841) includes a pre-vacuum pump; vacuum
measuring devices and parts for installation.
NOTES: a) If both an HTK and TTK are present, the high vacuum equipment (9430 500 20101;
9430 500 28291) can also be used for the TTK.
b) The vacuum equipment is required for operation at temperatures below room temperature.
Vacuum (ca. 10-2 mbar) prevents the formation of ice at temperatures below 0 ºC (273 K)
inside the low temperature chamber. Please refer to the Anton Paar manual “Vacuum Systems”
(document number B34IE13) for further details.
13.2.2.1.2 9430 500 27851 Low Temperature Equipment for TTK 450
The low temperature equipment for TTK 450 low temperature attachment includes the Liquid Nitrogen
Controller (AP58320) for the suction of liquid nitrogen, with built-in diaphragm pump for manual or automatic
dosage of the nitrogen flow, and the connector to the TTK 450 chamber for the supply of liquid nitrogen
(AP58972). Parts for installation are also included.
The liquid nitrogen flow can be controlled automatically by the TCU 100 Temperature Control Unit. Please refer
to the Anton Paar manual “LNC Liquid Nitrogen Controller Instruction Manual” (document number B39IB08)
13.2.2.1.3 9430 500 20141 Dewar Vessel 10 l
The dewar vessel with a 10 l capacity is used for the supply of liquid nitrogen to the TTK 450 (9430 500 27841).
13.2.2.1.4 9430 500 20341 Dewar Vessel 5 l
The dewar vessel with a 5 l capacity is used for the supply of liquid nitrogen to the TTK 450 (9430 500 27841).
13.2.2.1.5 9430 500 28361 Adaptor TTK-PW3050/6x
The adaptor TTK-PW3050/6x is used to install the low temperature chamber TTK 450 on an X’Pert PRO MPD
system. When this adaptor is mounted onto the TTK 450 the sample height adjustment is performed manually.
Page 13.12 07.03.27

13.2.2.1.6 9430 500 21161 PC-controllable Alignment Stage
The PC-controllable alignment stage (9430 500 21161) is an adaptor for mounting a non-ambient chamber onto
an X'Pert PRO MPD system. It includes a stepper motor-driven precision stage that allows height alignment of
the chamber via PC control and a software program “AP Stage Mover”. This program reads temperature data as
stored by the data collector software in a temperature log file and uses these data to correct the sample position
automatically for temperature-induced height variations, based on (user-definable) calibration data.
Please refer to the Anton Paar manual “PC-controllable alignment stage with alignment stage controller
Instruction Manual” (document number B08IB03) and the data collector software's help for further details.
Use of the alignment stage is described in section 13.2.1.3.
13.2.2.1.7 9430 500 20411 Lid for Humidity Chamber
The 9430 500 20411 Lid for Humidity Chamber (together with the 9430 500 20381 Relative Humidity
Generator) can be used together with the TTK 450 low temperature attachment on the X’Pert PRO goniometer.
With the use of the lid, you can vary the relative humidity in the low temperature chamber at room temperature
between 5% and approximately 70%, or to 90% in combination with the double walled gas hose
(9430 500 21041).
13.2.2.1.7.1 Mounting the Lid onto the TTK 450
You mount the lid for the humidity chamber onto the TTK 450 Low Temperature Chamber as follows:
1. Mount the TTK 450 according to the instructions given in section 13.2.1.1.
1. Remove the existing front cover from the TTK 450.
2. Mount the lid for the humidity chamber onto the remaining part of the TTK 450, being careful to ensure
that the gas nozzle is at the top pointing down onto the sample. Push the front part securely into place
so that the two chromium securing clips click into place and then tighten the two black knurled knobs
(marked A on Figure 13.11).
3. Connect the gas transfer hose between the lid and the humidity generator. The TTK 450 can now be
used as a humidity chamber at room temperature.
Operation instructions for the humidity generator are given in section 13.3.2.5. Please note that you can only
measure at room temperature.
07.03.27 Page 13.13

Mylar
Window
Connector for
Humidified Gas
from the Gas
Transfer Hose
Chromium Securing Black Knurled

Clip Knob A
Figure 13.11: 9430 500 2041 Lid for Humidity Chamber

Mounted onto a TTK 450 Low Temperature Chamber
13.2.2.1.8 9430 500 21041 Double Walled Gas Hose
The 9430 500 21041 Double Walled Gas Hose is used to transfer the humidified gas from the humidity generator
to the TTK 450 with Lid for Humidity Chamber. A water bath is required to heat the water circulating in the
hose. Using this double walled gas hose increases the humidity range at room temperature to 90%.
13.2.2.1.9 9430 500 20381 Humidity Generator
If your TTK450 is equipped with a lid for humidity chamber, you use the 9430 500 20381 Humidity Generator
to provide a specified constant flow of gas at a given level of relative humidity. The instrument is shown in
Figure 13.19. The relative humidity can be set between 5% and 95%. The maximum flow rate of the humidified
gas is 500 cc/min.
Page 13.14 07.03.27

Temperature
Display
Flap
Water Level
Indicator Pipe
Gas Pressure
Meter
Flow Rate
Meter
Pressure
Regulator
Figure 13.12: Humidity Generator
The delivery includes a NI-DAQ (National Instruments Data Acquisition Driver Software) interface card which
is installed in your PC; and RH Generator software from VTI Corporation to automate the control of relative
humidity.
Depending on the requested value of the total gas flow, the relative humidity at the sample surface and the
sample temperature, the software steers the flow of a dry and a water saturated (wet) gas stream. These gas
streams are mixed to achieve the required dew point by using a calibrated dew point analyzer (chilled mirror).
Please refer to the VTI Corporation manuals “Relative Humidity Generator RH-200 Operation Manual” and
“RH Generator Software User Manual” for further details about the operation and maintenance of the humidity
generator.
13.2.2.1.10 Temperature Bath
The temperature bath is used in a closed heating circuit that heats the (double-walled) gas transfer hose. This
prevents condensation in the system because the humidified gas cannot come into contact with parts of the
system at a temperature below (or near) the dew point of the gas. The temperature bath is shown in Figure 13.13.
There are two types of temperature bath; the one that you have in your system depends on the local power supply.
The 9430 500 20391 Temperature Bath is used with an electrical supply providing 110 V at 60 Hz.
The 9430 500 20431 Temperature Bath is used with an electrical supply providing 220 - 240 V at 50 Hz.
Please refer to the NESLAB manual “GP Series Constant Temperature Bath and Circulator Instruction and
Operation Manual” (Neslab Manual P/N U00222) for further details.
07.03.27 Page 13.15

Temperature
Display
Coarse Temperature
Setting Knob
Fine Temperature
Setting Knob Button to Display
Set Temperature
Water Heater
Cover
Figure 13.13: Temperature Bath
13.2.2.2 Use
This section describes the use of the TTK 450 equipped with a lid for humidity chamber for measurements at a
relative humidity between 5% and 90% at ambient temperature.
Use of the TTK 450 Low Temperature Chamber, the TCU 100 Temperature Control Unit and the LNC Liquid
Nitrogen Controller is described in the Anton Paar Instruction Manuals.
Mounting of the TTK 450 onto the X'Pert PRO goniometer and sample height adjustment are described in
section 13.2.1 of this chapter.
13.2.2.2.1 Experimental Set-up of the TTK 450 with Lid for Humidity Chamber
The measurements under controlled humidity conditions are performed at ambient temperature. Therefore
switch off the heater by pressing the heater button on the front of the TCU 100 Temperature Control Unit and
let the TTK 450 stabilize at environmental conditions, refer to section 4.2 in Chapter 4 of Part I of this User’s
Guide.
The relative humidity in the humidity chamber is controlled by the RH-200 Humidity Generator. The specified
gas flow with a given dew point is transported from the humidity generator to the humidity chamber through a
(double-walled) gas transfer hose.
In order to prevent condensation (or absorption of water molecules) in the system, the humidified gas must not
be allowed to come into contact with parts at a temperature below (or close to) the dew point of the gas.
Page 13.16 07.03.27
If you have a double-walled gas transfer hose it is water heated by means of a closed heating circuit. The
NESLAB GP-100 Constant Temperature Bath and Circulator controls the water temperature and the water flow
in the closed circuit.
NOTE: If you want to make low humidity measurements at room temperature, you may need to remove the
humidity generator’s internal insulation (refer to the RH-200 manual).
13.2.2.2.2 Operation of the TTK 450 with Lid for Humidity Chamber
Before you start a measurement using the TTK 450 with Lid for Humidity Chamber you must make several
decisions about the measurement that you wish to make and how to ensure that the timing is correct. These
decisions are:
a. The humidity at which the sample is to be measured.
b. The measuring steps to be made. This entails combining your data collector program with the
settings in the RH Generator software in order to make sure that there is plenty of time for the
chamber to stabilize before each measurement is made (we recommend 30 minutes).
NOTE: Depending on the sample, additional time may be necessary in order to let the sample stabilize
under the new conditions.
In general you should remember that condensation is detrimental to accurate humidity measurements, so you
should make sure that you do not cause any condensation to be created. When you have made all these decisions
you are ready to start:
1. Make sure that there is enough water in the Neslab water heater's temperature bath and then switch the
temperature bath on.
NOTE: During normal operation, you should regularly and often check the water level in the Neslab water
heater.
2. Set the required water temperature; in general 5 ºC higher than the sample temperature, to prevent
condensation in the gas hose or the humidity chamber itself. Press the Display button on the water
heater front panel (see Figure 13.13) and use the Coarse and Fine knobs until the required temperature
is displayed.
3. Switch the RH-200 Relative Humidity Generator on and set the internal temperature to approximately
5 ºC higher than the temperature at which you will be measuring the sample.
You set the internal temperature as follows:

a. Drop the flap underneath the display (see Figure 13.12) and press the middle black knob.
b. Observe which digit flashes on the display and press the middle knob again to step through to the
digit you wish to change.
c. Set the required value of the digit by pressing the ∧ and ∨ buttons.
d. When you have the required setting press the left-hand knob (MD) and close the flap again.
During use you must occasionally check that the internal water level is between the two marks on the WATER
LEVEL indicator pipe on the relative humidity generator's front panel (see Figure 13.12).
4. Set the gas pressure on the humidity generator to 11 psi - 12 psi (758 - 827 mbar) on the pressure meter.
5. Set the required humidities for the complete X-ray diffraction experiment:
a. Start the RH Generator software.
b. Click on Experiment and the screen as shown in Figure 13.14 will be displayed.
07.03.27 Page 13.17

Figure 13.14: Relative Humidity Generator Experiment Definition

c. You must enter at least the following information on this window:
- Expt ID: (the identification name of the experiment that you are performing).
- The correct Sample Temperature (the one that you can read on the temperature control unit's
front panel).
- The correct Humidifier Temperature (the one that you just set on the humidity generator in step
3 above).
- Flow Rate. We recommend 500 cc/min, you should only reduce this value if your sample is
made of loose powder.
- The required Data Logging Interval.
- A data file with the name given in the “Expt ID:” box with the extension .RLO will be saved
when you run an experiment. This data file contains the humidity data as a function of time.
- The measuring Steps that you want:
Set RH to the required relative humidity.
Set the required Time for this step. This time must include both the time needed for the sample
to stabilize according to the specified conditions, and the measurement time.
NOTE: This time does not include the 5 to 15 minutes that the humidity generator (not the sample) takes to
stabilize. This means that the actual time per step is longer, so make sure that you enter generous
times in the data collector batch program to allow for this generator stabilization.
For instance, step 3 as shown in Figure 13.14 will take, in total 85 - 90 minutes, and not the 80
minutes net time as entered in this window.
Press ADD and repeat as many times as you need to. An experiment with three steps: one for 70
minutes at 45% humidity, followed by 80 minutes at 50% humidity, and finally 80 minutes at
85% humidity is shown in Figure 13.14.
Page 13.18 07.03.27

d. You can if you wish add other information, like Sample Name, for your own reference purposes.
e. You can also, if you wish, save the information as entered in this window for future use by
pressing the Save Template button. The template will be saved with the name entered in the “Expt
ID:” box with the extension .RTM.
Figure 13.15: Data Collector Batch Program

6. Prepare your batch program in the data collector software. The example shown in Figure 13.15 when
combined with the RH Generator experiment program shown in Figure 13.14 will result in:
a. 45 minutes wait (10 minutes setting the humidity and 35 minutes stabilizing the sample) at 45%
humidity,
b. 30 minutes measuring at 45% humidity,
c. 60 minutes wait (10 minutes setting the humidity and 50 minutes stabilizing the sample) at 50%
humidity,
d. 30 minutes measuring at 50% humidity,
e. 60 minutes wait (10 minutes setting the humidity and 50 minutes stabilizing the sample) at 85%
humidity,
f. 30 minutes measuring at 85% humidity.
Note that the first waiting step is slightly shorter than the others, in order to make sure that the
measurement is finished before the relative humidity generator software starts to change the humidity
to the next value.
7. Press Run Experiment (in RH Generator software) and select Measure - Start (in the data collector
software) to start the measurement.
When the experiment, as performed by the humidity generator is finished; the generator automatically stops the
flow of humidified gas. The gas system is then purged with a dry gas flow for approximately ten minutes.
07.03.27 Page 13.19

13.2.2.2.3 Switching the TTK450 with Lid for Humidity Chamber Off
When the measurements are finished you can switch the humidity system off as follows:
1. In order to prevent condensation in the humidity chamber, make sure that you have purged the system
for a period (we recommend at least 30 minutes) before the system cools down.
2. Switch off: the water bath and the relative humidity generator.
13.2.2.2.4 Dismounting the TTK450 with Lid for Humidity Chamber
Before you start to dismount the temperature controlled humidity chamber from the goniometer; make sure that
you have switched the humidity system off as described in section 13.2.2.2.3 and proceed with the following
steps.
1. Loosen the two black knurled knobs (see Figure 13.11) enough to allow the securing clips to be
released.
2. Take the front part of the humidity chamber off and take the sample out of the chamber.
3. Loosen the four hexagonal headed securing screws and remove the banana shaped securing clamps (see
Figure 13.12) and remove the chamber. Put the front part of the humidity chamber back on in order to
keep dust out of the chamber.
CAUTION
Be very careful NOT to damage the chamber's Mylar windows with
the Torx key (especially if you are using a right-angle Torx key)
when you are loosening the securing screws.
13.2.2.2.5 References
Please refer to the manuals supplied with the component parts of the system for further details, they are:
Anton Paar: “THC Temperature Humidity Chamber Instruction Manual” (document number
B91IB01),
“TCU 50 Temperature Chamber Instruction Manual” (document number B91IB02).
VTI Corporation: “Relative Humidity Generator RH-200 Operational Manual”.
“RH Generator Software User Manual”.
NESLAB: “GP Series Constant Temperature Bath and Circulator, Instruction and Operation
Manual (Neslab Manual P/N U00222)”.
13.2.3 9430 500 20711 HTK 1200N High Temperature Oven-chamber, Rigid
System
The HTK 1200N High Temperature Oven-chamber with rigid sample holder is designed for non-ambient X-ray
studies. Measurements can be performed from room temperature up to 1200 ºC, in air, inert gas, or under
vacuum. The oven-chamber offers a high temperature uniformity. The delivery includes the complete oven-
chamber HTK 1200N (AP16407), two sample holders (AP15913) the temperature control unit TCU 1000N
(AP16413) and a simple water control device (AP70067). When delivered the HTK 1200N is factory mounted
onto a PreFIX adaptor (9430 500 28381 or 9430 500 21171). Vacuum equipment can be ordered as an accessory.
Please refer to the Anton Paar manuals “HTK 1200N High Temperature Oven-chamber Instruction Manual”
(document number B40IB04) and “TCU 1000N Temperature Control Unit Instruction Manual” (document
number B39IB19) for further details.
Page 13.20 07.03.27

13.2.3.1.1 9430 500 20101 High Vacuum Equipment
The high vacuum equipment (AP58963) for HTK 1200N (9430 500 20711; 9430 500 20721), for HTK 16
(9430 500 27761) and for HTK 2000 (9430 500 28271) includes a pre-vacuum pump; a turbo molecular high
vacuum pump; vacuum measuring devices and parts for installation.
NOTE: If both an HTK and TTK or XRK are present, the vacuum equipment for HTK (9430 500 20101)
can also be used with the TTK or XRK.
Please refer to the Anton Paar manual “Vacuum Systems Instruction Manual” (document number B34IB13) for
further details.
13.2.3.1.2 9430 500 28381 Adaptor HTK-PW3050/6x
The adaptor HTK-PW3050/6x is used to install the high temperature chambers HTK 16, HTK 1200N and
HTK 2000 on an X’Pert PRO MPD system. When this adaptor is mounted on an HTK the sample height
adjustment is performed manually.
the X'Pert PRO MPD system. It includes a stepper motor-driven precision stage that allows height alignment of
the chamber under PC control using a software program “AP Stage Mover”. This program reads temperature
data as stored by the data collector software in a temperature log file and uses this information to correct the
sample position automatically for temperature-induced height variations, based on (user-definable) calibration
data.
13.2.3.1.4 9430 500 20731 HTK 1200N Sample Carrier - 0.8 mm deep
The Sample Carrier (9430 500 20731) is an alumina cup the cavity of which has an inner diameter of 16 mm
and a depth of 0.8 mm. Alumina provides a high corrosion resistance. The sample carrier can be taken from the
HTK 1200N's sample holder flange in order to load it with sample material at a separate location. Two of these
sample holders are included in the delivery of the HTK 1200N High-temperature Oven-chamber.
The Sample Carrier (9430 500 20741) is an alumina cup with a cavity with an inner diameter of 16 mm and a
depth of 0.4 mm. Alumina provides a high corrosion resistance. The sample carrier can be taken from the
HTK 1200N's sample holder flange in order to load it with sample material at a separate location.
13.2.3.1.6 9430 500 20751 HTK 1200N Sample Carrier - Flat
The Sample Carrier (9430 500 20751) is an alumina sample holder with a diameter of 16 mm without a cavity.
Alumina provides a high corrosion resistance. The sample carrier can be taken from the HTK 1200N's sample
holder flange in order to load it with sample material at a separate location.
07.03.27 Page 13.21

13.2.4 9430 500 20721 HTK 1200N High Temperature Oven-chamber,

Spinner System
The HTK 1200N High Temperature Oven-chamber with spinning sample holder is designed for non-ambient
X-ray studies. Spinning improves the statistics of the measurement by bringing more particles into the diffraction
condition. Measurements can be performed from room temperature up to 1200 ºC, in air, inert gas, or under
vacuum. The oven-chamber offers a high temperature uniformity. The delivery includes the complete oven-
chamber HTK 1200N (AP16408), two sample holders (AP15913), the temperature control unit TCU 1000N
(AP16413) and a simple water control device (AP70067). When the product is delivered the HTK 1200N is
factory mounted onto a PreFIX adaptor (9430 500 28381 or 9430 500 21171). Vacuum equipment can be ordered
as an accessory.
Please refer to the Anton Paar manuals “HTK 1200N High Temperature Oven-chamber Instruction Manual”
(document number B40IB04) and “TCU 1000N Temperature Control Unit Instruction Manual” (document
number B39IB19) for further details.
13.2.4.1.1 9430 500 20101 Vacuum Equipment
further details.
13.2.4.1.2 9430 500 28381 Adaptor HTK-PW3050/6x
data.
Use of the alignment stage is described in section 13.2.1.3
The Sample Carrier (9430 500 20731) is an alumina cup with a cavity which has an inner diameter of 16 mm
and a depth of 0.8 mm. Alumina provides a high corrosion resistance. The sample carrier can be taken away from
the HTK 1200N's sample holder flange in order to load it with sample material at a separate location. Two of
these sample holders are included in the delivery of the HTK 1200N High-temperature Oven-chamber.
Page 13.22 07.03.27

The Sample Carrier (9430 500 20741) is an alumina cup with a cavity with an inner diameter of 16 mm and a
depth of 0.4 mm. Alumina provides a high corrosion resistance. The sample carrier can be taken off from the
HTK 1200N's sample holder flange to load it with sample material on a separate location.
13.2.4.1.6 9430 500 20751 HTK 1200N Sample Carrier - Flat
The Sample Carrier (9430 500 20751) is an alumina sample holder with a diameter of 16 mm without a cavity.
Alumina provides a high corrosion resistance. The sample carrier can be taken from the HTK 1200N's sample
holder flange in order to load it with sample material at a separate location.
13.2.5 9430 500 27761 HTK 16 High Temperature Chamber

The HTK 16 High Temperature chamber is designed for non-ambient X-ray studies with direct sample heating.
Measurements can be performed from room temperature up to 1600 ºC, in air, inert gas, or vacuum with the use
of a platinum filament for short-term operation; or up to 1450 ºC permanently. A tantalum filament enables the
HTK 16 to be permanently used at a temperatures between room temperature and 1500 ºC under vacuum, or up
to 400 ºC in air or inert gas. For a detailed overview of the specifications please refer to Table 13.2.
The delivery includes the complete chamber HTK 16 (AP70236), the temperature control unit TCU 2000
(AP70059) and a simple water control device (AP70067). When the product is delivered the HTK 16 is factory
mounted onto a PreFIX adaptor (9430 500 28381 or 9430 500 21171). Vacuum equipment can be ordered as an
accessory.
Please refer to the Anton Paar manuals “HTK 16 High Temperature Chamber Instruction Manual” (document
number B34IB02) and “TCU 2000 Temperature Control Unit Instruction Manual” (document number B39IB02)
13.2.5.1.1 9430 500 27771 Heating Strip, Pt 1.0 mm for HTK 16 and HTK 2000
The heating strip made of platinum with dimensions 102 mm x 10 mm x 1 mm, it includes a welded-on
thermocouple Pt/10%RhPt. It is designed for use with HTK 16 and HTK 2000 chambers.
Please refer to the Anton Paar manual “HTK 16 High Temperature Chamber Instruction Manual” (document
number B34IB02) for further details about the use of platinum heating strips.
13.2.5.1.2 9430 500 27781 Heating Strip, Pt 0.5 mm for HTK 16

The heating strip made of platinum with dimensions of: 102 mm x 10 mm x 0.5 mm, it includes a welded-on
thermocouple Pt/10%RhPt. It is designed for use with HTK 16 only.
13.2.5.1.3 9430 500 27791 Heating Strip, Pt 1x0.2 mm for HTK 16

The heating strip made of platinum with dimensions of: 102 mm x 10 mm x 1.0 mm, it includes a welded-on
thermocouple Pt/10%RhPt. The strip is provided with a cavity 20 mm x 8 mm x 0.2 mm as a sample preparation
facility. It is designed for use with HTK 16 only.
Please refer to the Anton Paar manual “HTK 16 High Temperature Camera Instruction Manual” (document
07.03.27 Page 13.23

13.2.5.1.4 9430 500 27801 Heating strip, Ta 1.0 mm for HTK 16

The heating strip made of tantalum with dimensions of 102 mm x 10 mm x 1 mm, it includes a welded-on
thermocouple Pt/10%RhPt. It is designed for use with HTK 16 only.

(9430 500 27761) and for HTK 2000 (9430 500 28271), it includes a pre-vacuum pump; a turbo molecular high
further details.
13.2.5.1.6 9430 500 28381 Adaptor HTK-PW3050/6x


data.
13.2.6 9430 500 28271 HTK 2000 High Temperature Attachment

The HTK 2000 High Temperature Attachment is designed for non-ambient X-ray studies with direct sample
heating. Measurements can be performed from room temperature up to 1600 ºC, in air, inert gas, or vacuum with
the use of a platinum filament for short-term operation; or up to 1450 ºC permanently. A tungsten filament
enables the HTK 2000 to be permanently used at a temperatures between room temperature and 2300 ºC under
vacuum. For a detailed overview of the specifications of the HTK 2000 please refer to Table 13.2.
The delivery includes the complete chamber HTK 2000 (AP75726), the temperature control unit TCU 2000/20
(AP75731) and a simple water control device (AP70067). When the product is delivered the HTK 2000 is factory
mounted onto a PreFIX adaptor (9430 500 28381 or 9430 500 21171). Vacuum equipment and heating strips can
be ordered as accessories.
Please refer to the Anton Paar manuals “HTK 2000 High Temperature Camera Instruction Manual” (document
number B41IB02) and “TCU 2000/20 Temperature Control Unit Instruction Handbook” (document number
B39IB12) for further details.
Page 13.24 07.03.27

13.2.6.1.1 9430 500 27771 Heating Strip, Pt 1.0 mm for HTK 16 and HTK 2000
The heating strip made of platinum with dimensions 102 mm x 10 mm x 1 mm includes a welded-on
thermocouple Pt/10%RhPt. It is designed for use with the HTK 16 and HTK 2000.
13.2.6.1.2 9430 500 28281 Heating Strip, W 0.5 mm for HTK 2000
The heating strip made of tungsten with dimensions 102 mm x 9 mm x 0.5 mm includes a welded-on
thermocouple W3%Re/W25%Re. It is designed for use with an HTK 2000.

further details.
13.2.6.1.4 9430 500 28381 Adaptor HTK-PW3050/6x

The adaptor HTK-PW3050/6x is used to install the high temperature chambers HTK 16, HTK 1200 and

data.
07.03.27 Page 13.25

13.2.7 9430 500 21021 XRK 900 Reactor Chamber

The XRK 900 X-ray Reactor Chamber permits studies of solid state and solid state-gas reactions at temperatures
from room temperature to 900 ºC. Experiments may be carried out in reduced (low vacuum), inert or oxidizing
atmospheres. The delivery includes the complete chamber (AP17157), a temperature control unit TCU 750
(AP70058) with connectors for gas supply and parts for installation and alignment. When the product is
delivered the XRK 900 is factory mounted onto a PreFIX adaptor (9430 500 28401 or 9430 500 21181). Sample
holders are available as accessories.
A water flow control device is not required.
Please refer to the Anton Paar manuals “XRK 900 Reactor Chamber Instruction Manual” (document number
A98IB02) and “TCU 750 Temperature Control Unit Instruction Manual” (document number B39IB04) for
further details.
13.2.7.1.1 9430 500 27951 Sample Holder Closed Steel
The closed sample holder for the XRK 900 reactor chamber makes it possible to operate the XRK in vacuum.
Consequently, the reaction gas cannot flow through the sample. The sample holder is made of stainless steel.
13.2.7.1.2 9430 500 27961 Sample Holder Closed Glass Ceramic
The closed sample holder for the XRK 900 reactor chamber makes it possible to operate the XRK in vacuum.
Consequently, the reaction gas cannot flow through the sample. The sample holder is made of glass ceramics.
13.2.7.1.3 9430 500 27971 Sample Holder Open Steel
The open sample holder for the XRK 900 reactor chamber has a sieve-like bottom so that the reaction gas can
flow through the sample. With this type of holder the XRK chamber cannot be used in vacuum. The sample
holder is made of stainless steel.
13.2.7.1.4 9430 500 27981 Sample Holder Open Glass Ceramic
The open sample holder for the XRK 900 reactor chamber has a sieve-like bottom so that the reaction gas can
flow through the sample. With this type of holder the XRK chamber cannot be used in vacuum. The sample
holder is made of glass ceramics.
The vacuum equipment (AP58974) for TTK 450 (9430 500 27841) can also be used with X-ray reactor chamber
type XRK 900. It includes a pre-vacuum pump; vacuum measuring devices and parts for installation.
NOTE: If both an HTK and XRK are present, the high vacuum equipment (9430 500 20101) can also be
used with the XRK.
further details.
13.2.7.1.6 9430 500 28401 Adaptor XRK-PW3050/6x
The adaptor XRK-PW3050/6x is used to install the X-ray reactor chambers XRK 900 on an X’Pert PRO MPD
system. When this adaptor is mounted onto an XRK the sample height adjustment is performed manually.
Page 13.26 07.03.27

data.
13.2.8 9430 500 21031 XRK 900 Reactor Chamber Spinner

The XRK 900 X-ray Reactor Chamber with sample spinner permits studies of solid state and solid state-gas
reactions at temperatures from room temperature to 900 ºC. Spinning improves the statistics of the measurement
by bringing more particles into the diffraction condition. Experiments may be carried out in reduced (low
vacuum), inert or oxidizing atmospheres. The delivery includes the complete chamber (AP17159), a temperature
control unit TCU 750 (AP70058) with connectors for gas supply and parts for installation and alignment. When
the product is delivered the XRK 900 spinner is factory mounted onto a PreFIX adaptor (9430 500 28401 or
9430 500 21181). Sample holders can be ordered as accessories.
A water flow control device is not required.
Please refer to the Anton Paar manuals “XRK 900 Reactor Chamber Instruction Manual” (document number
A98IB02) and “TCU 750 Temperature Control Unit Instruction Handbook” (document number B39IB04) for
further details.
13.2.8.1.1 9430 500 28231 Spinner Sample Holder Closed Steel
The closed spinning sample holder for the XRK 900 Reactor Chamber Spinner makes it possible to operate the
XRK in vacuum. Consequently, the reaction gas cannot flow through the sample. The sample holder is made of
stainless steel.
13.2.8.1.2 9430 500 28241 Spinner Sample Holder Closed Ceramic
The closed spinning sample holder for the XRK 900 Reactor Chamber Spinner makes it possible to operate the
XRK in vacuum. Consequently, the reaction gas cannot flow through the sample. The sample holder is made of
glass ceramics.
13.2.8.1.3 9430 500 28251 Spinner Sample Holder Open Steel
The open spinning sample holder for the XRK 900 Reactor Chamber Spinner, has a sieve-like bottom so that
the reaction gas can flow through the sample. With this type of holder the XRK chamber cannot be used in
vacuum. The sample holder is made of stainless steel.
13.2.8.1.4 9430 500 28261 Spinner Sample Holder Open Ceramic
The open spinning sample holder for the XRK 900 Reactor Chamber Spinner, has a sieve-like bottom so that
the reaction gas can flow through the sample. With this type of holder the XRK chamber cannot be used in
vacuum. The sample holder is made of glass ceramics.
07.03.27 Page 13.27

The vacuum equipment (AP58974) for TTK 450 (9430 500 27841) can also be used with X-ray reactor chamber
XRK 900. It includes a pre-vacuum pump; vacuum measuring devices and parts for installation.
NOTE: If both an HTK and XRK are present, the high vacuum equipment (9430 500 20101) can also be
used with the XRK.
further details.
13.2.8.1.6 9430 500 28401 Adaptor XRK-PW3050/6x
The adaptor XRK-PW3050/6x is used to install the X-ray reactor chamber XRK 900 on an X’Pert PRO MPD
system. When this adaptor is mounted onto an XRK the sample height adjustment is performed manually.
data.
13.3 9430 500 20371 TEMPERATURE CONTROLLED HUMIDITY CHAMBER

The 9430 500 20371 Temperature Controlled Humidity Chamber (THC) is designed for X-ray diffraction studies
under temperature and humidity controlled conditions. The THC is shown in Figure 13.16. It can be PreFIX
mounted onto an X’Pert PRO MPD system.
Samples can be measured between room temperature and 50 ºC (323 K) with relative humidity between 5% and
95%. The relative humidity range is limited at higher temperatures. In a vacuum or in dry gas the temperature
range is from 0 ºC (273 K) to 150 ºC (423 K). An overview of the available temperature and humidity range can
be seen in Figure 13.17. The relative humidities can be set with an accuracy of ± 3%. The sample temperature is
controlled using a Peltier element with a control accuracy of ± 0.1 ºC. The maximum volume of the sample is 14
mm length x 10 mm width x 0.8 mm thickness.
The 9430 500 20371 Temperature Controlled Humidity Chamber comprises: a humidity chamber, a TCU 50
Temperature Control Unit (shown in Figure 13.18) and a double-walled gas transfer hose. When the temperature
controlled humidity chamber is delivered it is factory mounted onto a PreFIX adaptor. A temperature bath and
a humidity generator are required for the operation. Use of vacuum equipment is optional.
Please refer to the Anton Paar manuals “THC Temperature Controlled Humidity Chamber Instruction Manual”
(document number B91IB01) and “TCU 50 Temperature Control Unit for Temperature Controlled Humidity
Chamber Instruction Manual” (document number B91IB02) for further details.
Page 13.28 07.03.27

Mylar
Window
Connector for
Humidified Gas
from the Gas
Transfer Hose
Chromium Securing Black Knurled

Clip Knob A
Connector for Water from

the Gas Transfer Hose
Figure 13.16: Temperature Controlled Humidity Chamber
Figure 13.17: Accessible Temperature and Humidity Range of the Temperature Controlled Humidity
Chamber
07.03.27 Page 13.29

Temperature Display
Lamp Indicating
Active Heating
Actual Temperature
Indicator Lamp
Set Temperature
Indicator Lamp
Temperature Control
On Indicator Lamp
Temperature Control
Start/Stop Button
Temperature Setting Toggle Button for
Buttons Temperature Display
13.3.1 Accessories
13.3.1.1 9430 500 20121 Vacuum Equipment
The vacuum equipment (AP58974) for TTK 450 (9430 500 27841) can also be used with the temperature
controlled humidity chamber. It includes a pre-vacuum pump; vacuum measuring devices and parts for
installation.
NOTE: If both an HTK and THC are present, the vacuum equipment for HTK (9430 500 20101;
9430 500 28291) can also be used for the THC.
further details.
13.3.1.2 9430 500 20381 Humidity Generator

The 9430 500 20381 Humidity Generator is an automated bench top instrument that can provide a specified
constant flow of a gas at a given level of relative humidity. The instrument is shown in Figure 13.19. The relative
humidity can be set between 5% and 95%. The maximum flow rate of the humidified gas is 500 cc/min.
Page 13.30 07.03.27

Temperature
Display
Flap
Water Level
Indicator Pipe
Gas Pressure
Meter
Flow Rate
Meter
Pressure
Regulator
Figure 13.19: Humidity Generator
The delivery includes a NI-DAQ (National Instruments Data Acquisition Driver Software) interface card which
is installed in your PC; and RH Generator software from VTI Corporation to automate the control of relative
humidity.
Depending on the requested value of the total gas flow, the relative humidity at the sample surface and the
sample temperature, the software steers the flow of a dry and a water saturated (wet) gas stream. These gas
streams are mixed to achieve the required dew point by using a calibrated dew point analyzer (chilled mirror).
Please refer to the VTI Corporation manuals “Relative Humidity Generator RH-200 Operation Manual” and
“RH Generator Software User Manual” for further details about the operation and maintenance of the humidity
generator.
13.3.1.3 Temperature Bath

The temperature bath is used in a closed heating circuit that heats the (double-walled) gas transfer hose as well
as the walls of the humidity chamber. This prevents condensation in the system because the humidified gas
cannot come into contact with parts of the system at a temperature below (or near) the dew point of the gas. The
temperature bath is shown in Figure 13.20.
There are two types of temperature bath; the one that you have in your system depends on the local power supply.
The 9430 500 20391 Temperature Bath is used with an electrical supply providing 110 V at 60 Hz.
The 9430 500 20431 Temperature Bath is used with an electrical supply providing 220 - 240 V at 50 Hz.
Please refer to the NESLAB manual “GP Series Constant Temperature Bath and Circulator Instruction and
Operation Manual” (Neslab Manual P/N U00222) for further details.
07.03.27 Page 13.31

Temperature
Display
Coarse Temperature
Setting Knob
Fine Temperature
Setting Knob Button to Display
Set Temperature
Water Heater
Cover
Figure 13.20: Temperature Bath
13.3.1.4 9430 500 28361 Adaptor TTK-PW3050/6x

The adaptor TTK-PW3050/6x is used to install the humidity chamber THC on an X’Pert PRO MPD system.
When this adaptor is mounted onto the THC the sample height adjustment is performed manually.
13.3.1.5 9430 500 21161 PC-controllable Alignment Stage

data.
Page 13.32 07.03.27

13.3.2 Use
13.3.2.1 Experimental Set-up of the Temperature Controlled Humidity System
A schematic representation of the temperature controlled humidity chamber and its accessories is shown in
Figure 13.21. These systems are installed by PANalytical Service Engineers.
The temperature of the sample in the humidity chamber that is to be measured is controlled by the TCU 50
Temperature Control Unit which can either be controlled by the data collector software or manually by the
operator.
The relative humidity in the humidity chamber is controlled by the RH-200 Humidity Generator. The specified
gas flow with a given dew point is transported from the humidity generator to the humidity chamber through a
double-walled gas transfer hose.
In order to prevent condensation (or absorption of water molecules) in the system, the humidified gas must not
be allowed to come into contact with parts at a temperature below (or close to) the dew point of the gas.
Therefore the gas transfer hose and the walls of the humidity chamber are water heated by means of a closed
heating circuit. The NESLAB GP-100 Constant Temperature Bath and Circulator controls the water temperature
and the water flow in the closed circuit.
13.3.2.2 Mounting the Temperature Controlled Humidity Chamber

This section describes how to mount the temperature controlled humidity chamber onto an X’Pert PRO MPD
system.
1. Make sure that you do not have any other stage mounted.
2. Check that you have available to you the four securing screws with hexagonal heads (M6 x 20) that are
delivered with the system.
3. Make sure that the temperature control unit (TCU 50) and the relative humidity generator are switched
off (refer to the instruments’ Operation Manuals).
4. Locate the humidity chamber into position using the three positioning lugs and the hinged clip at the
top, insert and tighten the four securing screws - see caution below.
CAUTION
Be very careful NOT to damage the chamber’s Mylar windows with
when you are tightening the screws.
5. Remove the lid from the humidity chamber and mount the sample (refer to the “THC Temperature
Controlled Humidity Chamber Instruction Handbook” for further details.
6. Mount the front part of the humidity chamber onto the part that you just mounted (in step 4) being
careful to ensure that the gas nozzle is at the top pointing down onto the sample. Push the front part
securely into place so that the two chromium securing clips click into place and then tighten the two
black knurled knobs (marked A on Figure 13.16).
07.03.27 Page 13.33

Figure 13.21: Temperature Controlled Humidity System - Schematic Representation
13.3.2.3 Adjusting the Sample Height of a Humidity Chamber

This section describes the adjustment of the sample height using a reference sample.
1. Place a reference sample (for instance, a silicon or alumina powder sample) into the humidity chamber.
2. You can, if you wish, mount the dial gauge so that you can note the optimum sample height for future
use.
3. Use the data collector software to make a measurement as follows:
a. Set 2θ to the required angle according to the characteristic radiation of the X-ray tube and the
offset to 0º in order to measure the a known reflection of your reference sample by making a
short 2θ - θ scan.
Information about the Si(111) reflection is given in Table 13.3.
Page 13.34 07.03.27

b. Open the shutter and monitor the intensity while you use the Anton Paar PC-controllable
alignment stage in the manual operation mode to move the chamber up and down until you
reach a maximum.
If you do not have a motorized chamber you will have to: close the shutter, open the enclosure doors,
adjust the height according to the instructions provided in the temperature controlled humidity
chamber’s instruction manual, close the doors, measure again, and so on.
Table 13.3: 2θ Angle of the Si(111) and Si(311) Reflections for Different Types of Characteristic
Radiation
Characteristic
Si(111) Si(311)
Radiation
Mo Kα1 12.979 25.09º
Cu Kα1 28.420º 56.103º
Co Kα1 33.124º 66.199º
Fe Kα1 35.937º 72.455º
Cr Kα1 42.796º 88.686º
CAUTION
Ensure that you do not exceed the maximum allowed count rate for
the detector used.
4. Set 2θ to the angle of another known reflection on your reference sample. Table 13.3 shows the angles
of the Si(311) reflection.
Make a short 2θ - θ scan over about 1º, around this angle and check that the resulting peak is within 0.02º.
If this is not the case, check that the four screws holding the non-ambient chamber in position are tight,
check that you have reported the correct PreFIX optical modules to the data collector software, and start
this procedure again at step 3.
5. When you have completed the height adjustment, make a note of the height indication on the dial gauge
(if mounted) and remove the dial gauge.
6. Remove the silicon reference sample and mount the sample that you want to measure. If the sample is
correctly mounted, the sample height is automatically correct.
13.3.2.4 Adjusting the Sample Height Using the PC-controllable Alignment Stage
If your temperature-controlled humidity chamber is mounted onto a PC-controllable alignment stage
(9430 500 21161), you then have the option to automatically correct the sample height position for temperature
effects. The PC-controllable alignment stage is shown in Figure 13.22.
07.03.27 Page 13.35

Figure 13.22: PC-controllable Alignment Stage
Proceed as follows to use the PC-controllable alignment stage:

1. Switch the alignment stage controller on. Normally the alignment stage controller is built in the
instrument enclosure, such that the controller is switched on when the X'Pert PRO system is switched
on. If it is not built in, you can switch on the alignment stage controller using the main switch at the rear
side of the alignment stage controller (see Figure 13.24). The green LED at the front side of the
controller indicates that the controller is switched on.
Figure 13.23: Alignment Stage Controller - Front
Page 13.36 07.03.27

Figure 13.24: Alignment Stage Controller - Rear

2. Connect the data collector software to the X'Pert PRO system with a configuration that contains the
non-ambient chamber that you are going to use.
3. Start the AP Stage Mover program on the PC that is controlling your X'Pert PRO system.
Figure 13.25: Opening AP Stage Mover

4. When you are using the AP Stage Mover for the first time, open the menu window Tools - Options and
insert the following information:
a. Insert the folder and file names of the Temperature File. Normally the Temperature File is stored
under the name D:\temperature.txt.
b. Select the correct COM port for the communication between the PC and the alignment stage
controller.
07.03.27 Page 13.37

Figure 13.26: AP Stage Mover - Options Menu
NOTE: The Temperature File contains the current temperature value of the non-ambient chamber stored by
the data collector software. This file is read by the AP Stage Mover in order to automatically adjust
the sample height position as a function of temperature. The file name and location must also be
specified in the data collector software's initialization file “xpert.ini”. After a default installation
this file can be found in the folder:
the section header “[Diffractometer communication]”: “NALogFile=<path><file name>.<file
extension>”, for example:
5. Initialize the system by selecting Tools - Initialize.
NOTE: The Initialize command has to be executed after every start of the AP Stage Mover program.
If the alignment stage controller is not initialized, a hardware initialization procedure is started
automatically, which involves the following steps:
- The alignment stage moves downwards until it reaches the lower limit switch, indicated by the
yellow LED on the front of the alignment stage controller LED lighting.
- The alignment stage moves upwards until the switch opens, indicated by the yellow LED on the
front of the alignment stage controller going out. This position is defined as the “mechanical”
zero position of the alignment stage. The reproducibility of the mechanical zero position after
initialization is ±2 μm.
- The alignment stage moves upwards 100 μm.
Now you can use the AP Stage Mover in two modes of operation, displayed in the user interface as tabs:
Manual mode
In the manual mode the alignment stage can be moved relative to the present position or absolutely with respect
to the defined zero position. This mode is used in the sample stage alignment procedure (refer to section 13.3.2.3)
or when no temperature data are available for automated adjustment. After you have adjusted the sample to the
correct sample height at room temperature in the manual mode, you can select Tools - Define Zero to calibrate
it for automatic sample height alignment as a function of temperature in the automatic mode.
Page 13.38 07.03.27

Figure 13.27: AP Stage Mover - Manual Operation Mode
Automatic mode
In the automatic mode the AP Stage Mover reads the temperature value stored by the data collector in the
temperature log file and adjusts the sample height position automatically according to a pre-selected adjustment
table. A set of Anton Paar defined tables is available in the program; it is also possible to create user-defined
tables.
Select the table that you are going to use from the Table drop-down box.
Use the and buttons in order to switch on and off the automatic height adjustment.
Figure 13.28: AP Stage Mover - Automatic Operation Mode
Refer to the Anton Paar manual “PC-controllable alignment stage Instruction Manual” (document number
B08IB03) and the data collector software's help for further details about the use of the PC-controllable alignment
stage.
07.03.27 Page 13.39

13.3.2.5 Operation
Before you start a measurement using the temperature controlled humidity chamber you must make several
decisions about the measurement that you wish to make and how to ensure that the timing is correct. These
decisions are:
1. The temperature at which the sample is to be measured.
2. The humidity at which the sample is to be measured.
In practical terms it is best if you either choose a set temperature and vary the humidity; or perform a dry
measurement (5% humidity, or a vacuum) and vary the temperature.
NOTE: If you want to make low humidity measurements at the lower end of the temperature range (below
26 ºC) you may need to remove the relative humidity generator’s internal insulation (refer to the
RH-200 manual).
3. The measuring steps to be made. This entails combining your data collector program with the settings in
the RH Generator software in order to make sure that there is plenty of time for the chamber to stabilize
before each measurement is made (we recommend 30 minutes).
NOTE: Depending on the sample, additional time may be necessary in order to let the sample stabilize in
the new conditions.
In general you should remember that condensation is detrimental to accurate humidity measurements, so you
should make sure that you do not cause any condensation to be created. You do that by ensuring that you always
reduce the relative humidity (we recommend, for 30 minutes) before you reduce the temperature.
When you have made all these decisions you are ready to start:
1. Make sure that there is enough water in the Neslab water heater’s temperature bath and then switch the
temperature bath on.
NOTE: During normal operation, you should regularly and often check the water level in the Neslab water
heater.
2. Set the required water temperature; in general 10 ºC higher than the sample temperature, to prevent
condensation in the gas hose or the humidity chamber itself. Press the Display button on the water
heater front panel (see Figure 13.20) and use the Coarse and Fine knobs until the required temperature
is displayed.
3. Switch the TCU 50 on and set the required sample measuring temperature; either on the TCU 50 front
panel (see Figure 13.18), or in the data collector software. When you use the TCU 50 to set the sample
temperature, proceed as follows: Press the Toggle button to display set temperature. Use the
Temperature Setting buttons to set the required temperature. Press the Toggle button again to display
the actual temperature. Press the Start/Stop button to start the sample heating process.
4. Switch the RH-200 Relative Humidity Generator on and set the internal temperature to approximately
10 ºC higher than the temperature at which you will be measuring the sample.
You set the internal temperature as follows:
a. Drop the flap underneath the display (see Figure 13.19) and press the middle black knob.
b. Observe which digit flashes on the display and press the middle knob again and step through
to the digit you wish to change.
c. Set the required value of the digit by pressing the ∧ and ∨ buttons.
d. When you have the required setting press the left-hand knob (MD) and close the flap again.
During use you must occasionally check that the internal water level is between the two marks on the
WATER LEVEL indicator pipe on the relative humidity generator’s front panel (see Figure 13.19).
Page 13.40 07.03.27
5. Set the gas pressure on the humidity generator to 11 psi - 12 psi (758 - 827 mbar) on the pressure meter.
6. Set the required humidities for the complete X-ray diffraction experiment:
a. Start the RH Generator software.
b. Click on Experiment and the screen as shown in Figure 13.29 will be displayed:
Figure 13.29: RH Generator Experiment Definition

c. You must enter at least the following information on this window:
- Expt ID: (the identification name of the experiment that you are performing)
- The correct Sample Temperature (the one that you just set either in the data collector software
or on the temperature control unit’s front panel in step 3 above).
- The correct Humidifier Temperature (the one that you just set on the humidity generator in step
4 above).
- Flow Rate. We recommend 500 cc/min, you should only reduce this value if your sample is
made of loose powder.
- The required Data Logging Interval.
A data file with the name given in the “Expt ID:” box with the extension .RLO will be saved
when you run an experiment. This data file contains the humidity data as a function of time.
- The measuring Steps that you want:
Set RH to the required relative humidity.
Set the required Time for this step. This time must include both the time needed for the
sample to stabilize according to the specified conditions, and the measurement time.
NOTE: This time does not include the 5 to 15 minutes that the humidity generator (not the sample) takes
to stabilize. The actual time per step is longer. Make sure that you enter generous times in the data
collector batch program to allow for this generator stabilization.
For instance, step 3 as shown in Figure 13.29 will take in total 85 - 90 minutes, and not the 80
minutes net time as entered in this window.
07.03.27 Page 13.41

Press ADD and repeat as many times as you need to. An experiment with three steps: one for
70 minutes at 45% humidity, followed by 80 minutes at 50% humidity, and finally 80
minutes at 85% humidity is shown in Figure 13.29.
d. You can if you wish add other information, like Sample Name, for your own reference pur-
poses.
e. You can, if you wish, save the information as entered in this window for future use by pressing
the Save Template button. The template will be saved with the name entered in the “Expt ID:”
box with the extension .RTM.
Figure 13.30: Data Collector Batch Program

7. Prepare your batch program in the data collector software. The example shown in Figure 13.30 when
combined with the RH Generator experiment program shown in Figure 13.29 will result in:
45 minutes wait (10 minutes setting the humidity and 35 minutes stabilizing the sample) at 50 ºC
and 45% humidity,
30 minutes measuring at 50 ºC and 45% humidity,
and 50% humidity,
30 minutes measuring at 50 ºC and 50% humidity,
and 85% humidity,
30 minutes measuring at 50 ºC and 85% humidity.
Note that the first waiting step is slightly shorter than the others, in order to make sure that the measure-
ment is finished before the relative humidity generator software starts to change the humidity to the
next value.
8. Press Run Experiment (in RH Generator software) and Measure - Start (in the data collector software)
to start the measurement.
When the experiment, as performed by the humidity generator is finished; the generator automatically stops the
flow of humidified gas. The gas system is then purged with a dry gas flow for approximately ten minutes.
Page 13.42 07.03.27

13.3.2.6 Switching Off the Temperature Controlled Humidity System

When the measurements are finished you can switch the humidity system off as follows:
1. In order to prevent condensation in the humidity chamber, make sure that you have purged the system
for a period (we recommend at least 30 minutes) before the system cools down.
2. Switch off: the TCU 50 Temperature Control Unit, the water bath and the relative humidity generator.
13.3.2.7 Dismounting the Temperature Controlled Humidity Chamber

Before you start to dismount the temperature controlled humidity chamber from the goniometer; make sure that
you have switched the humidity system off as described in section 13.3.2.6 and proceed with the following steps.
1. Loosen the two black knurled knobs (see Figure 13.16) enough to allow the securing clips to be
released.
2. Take the front part of the humidity chamber off and take the sample out of the chamber.
3. Loosen the four hexagonal head securing screws, and remove the banana shaped securing clips (see
Figure 13.2) and then remove the chamber. Replace the front part to keep dust out of the chamber.
CAUTION
Be very careful NOT to damage the chamber’s Mylar windows with
when you are loosening the securing screws.
13.3.2.8 References
Please refer to the manuals supplied with the component parts of the system for further details, they are:
Anton Paar: “THC Temperature Humidity Chamber Instruction Manual” (document number B91IB01),
“TCU 50 Temperature Chamber Instruction Manual” (document number B91IB02).
VTI Corporation: “Relative Humidity Generator RH-200 Operational Manual”.
“RH Generator Software User Manual”.
NESLAB: “GP Series Constant Temperature Bath and Circulator, Instruction and Operation Manual
(Neslab Manual P/N U00222)”.
07.03.27 Page 13.43

13.4 CRYOSTREAM PLUS

The Cryostream Plus (9430 500 21071 or 9430 500 21341) is a PreFIX attachment for X'Pert PRO MPD systems
that allows temperature studies on samples in glass capillaries at temperatures from 227 °C (500 K) down to
-193 °C (80 K), with a gas temperature stability of 0.1 K. Liquid nitrogen is used to cool the sample with an
economic consumption of 0.6 liters per hour at a nitrogen gas flow of 5 liters per minute. The liquid nitrogen is
supplied from an unpressurized Dewar vessel.
Figure 13.31: Oxford Cryosystems Cryostream Plus Coldhead
The delivery includes the Cryostream Plus Coldhead, mounted on a PreFIX support, a flexible stainless steel
transfer line, the 700 Series Cryostream Controller, a nitrogen gas pump unit and a Dewar vessel. A dry air unit
and an auto-refill unit are available as optional accessories.
NOTE: Before you start using the Cryostream Plus, please read the safety information provided in section
2.2.7 of Chapter 2 of Part I of this User's Guide and the section “Liquid and Gaseous Nitrogen
Safety Sheet” in the Oxford Cryosystems manual “700 Series Cryostream Plus Operation &
Instruction Guide”.
Please refer to the Oxford Cryosystems manual “700 Series Cryostream Plus Operation & Instruction Guide” for
further details.
Page 13.44 07.03.27

13.4.1 Accessories
13.4.1.1 Capillary Spinner with PreFIX Mounting Position
In order to use to perform capillary measurements with the Cryostream Plus, the capillary spinner has to be
mounted onto the special stage interface that is delivered as an accessory. This stage interface contains a PreFIX
mounting position onto which the Cryostream Plus can be mounted. The capillary spinner with this stage
interface is shown in Figure 13.32.
Figure 13.32: PW3063/00 Capillary Spinner Mounted onto the Special Stage Interface
How to mount and align a capillary sample on the capillary spinner is described in section 12.3.2 of Chapter 12
in Part II of this User's Guide.
07.03.27 Page 13.45

13.4.1.2 Screening Plate for Goniometer Head

A ring-shaped white screening plate for the capillary spinner's goniometer head is provided with the Cryostream
Plus. This plate is used to prevent condensation of water and the formation of ice on the goniometer head.
To mount the plate onto the goniometer head:

1. Slide the plate carefully over the goniometer head such that the screw fits into the screw hole on the
upper part of the goniometer head.
2. Fix the plate by tightening the screw using a T6 screwdriver.
Figure 13.33: Screening Plate Mounted onto Goniometer Head
13.4.1.3 Dewar Vessel

The Dewar vessel is used to supply liquid nitrogen to the Cryostream Plus. Its capacity of 30 liters of liquid
nitrogen is sufficient for 48 hours of operation of the Cryostream Plus at a nitrogen gas flow rate of 5 l/min or
24 hours at a flow rate of 10 l/min. The Dewar vessel is placed inside the X'Pert PRO enclosure.
13.4.1.4 Direct Beam Stop for Focusing X-ray Mirror

The special direct beam stop delivered with the Cryostream Plus is used in combination with the PW3152/63
Focusing X-ray Mirror equipped with PW3086/70 Incident Beam Anti-scatter Device. It is shown in Figure
13.34. Mounting and alignment instructions are given in section 20.2.4.2 of Chapter 20 of Part II of this User's
Guide.
Page 13.46 07.03.27

Figure 13.34: Direct Beam Stop for Focusing X-ray Mirror
13.4.1.5 Cryostream Controller

The Cryostream Controller is used to control the temperature of the capillary sample and the flow of the nitrogen
gas. The controller is shown in Figure 13.35. It is integrated in X'Pert PRO MPD systems in such a way that it
can be operated using the data collector software.
Further information about the Cryostream Controller and its use is given in the Oxford Cryosystems manual
“700 Series Cryostream Plus Operation and Instruction Guide”
Use of the Cryostream Controller with X'Pert PRO MPD systems is described in section 13.4.2.
Figure 13.35: Cryostream Plus Controller

07.03.27 Page 13.47
13.4.1.6 Nitrogen Gas Pump Unit

The Nitrogen Gas Pump Unit is a diaphragm pump that draws up the liquid nitrogen from the Dewar vessel into
the gas flow circuit. The pump is controlled (switched on and off) by the Cryostream controller. The nitrogen
flow rate is controlled by a flow controller inside the Cryostream controller.
Further information about the nitrogen gas pump unit and its use is given in the Oxford Cryosystems manual
“700 Series Cryostream Plus Operation and Instruction Guide”.
Use of the nitrogen gas pump with the Cryostream Plus in X'Pert PRO MPD systems is described in section
13.4.2.
Figure 13.36: Nitrogen Gas Pump Unit
Page 13.48 07.03.27

13.4.1.7 Dry Air Unit

The Oxford Cryosystems AD51 Dry Air Unit (9430 500 21331 or 9430 500 21351) is a stand-alone unit that
draws in atmospheric air and converts it to dry air. The dry air has a dew point lower than -60 °C (213 K) and a
variable flow rate up to 25 l/min. You can control the output flow rate with a built-in needle valve and flow
meter. The dry air unit is connected with the Cryostream Plus Coldhead with a red tube with a right-angled
connector.
NOTE: If the AD51 Dry Air Unit has not been used for some time it is advisable to run the unit overnight
to establish the correct moisture gradient within the drying columns.
Please refer to the Oxford Cryosystems manual “AD51 Dry Air Unit Operation & Instruction Guide” for further
details.
Use of the Dry Air Unit with X'Pert PRO MPD systems is described in section 13.4.2.
Figure 13.37: AD51 Dry Air Unit
07.03.27 Page 13.49

13.4.1.8 Auto-refill Unit

The Auto-refill Unit (9430 500 21081 or 9430 500 21381) is an AMI 186 Liquid Level Instrument that monitors
and controls the level of the liquid nitrogen in the Dewar vessel inside the X'Pert PRO enclosure. It is available
as an optional accessory for the Cryostream Plus to allow measurements for an extended time period, without
interrupting the experiment. The instrument is connected to a sensor inserted in the Dewar vessel that monitors
the liquid nitrogen level and to an electronic valve that controls the flow from a liquid nitrogen storage vessel
outside the X'Pert PRO enclosure to the Dewar vessel.
Figure 13.38: AMI 186 Liquid Level Instrument
NOTE: Before you start using the Auto-refill unit, please read the safety information provided in section
2.2.7 of Chapter 2 of Part I of this User's Guide and the “General Precautions” about safety in the
AMI manual “Model 185/186 Liquid Level Instrument -Installation, Operation and Maintenance
Instructions”.
Use of the auto-refill unit with X'Pert PRO MPD systems is described in section 13.4.2.
Page 13.50 07.03.27

13.4.2 Use
13.4.2.1 Experimental Set-up of the Non-ambient Capillary Measurement System
A schematic representation of the X'Pert PRO MPD system set up for measurements on capillary samples at non-
ambient temperatures using the Cryostream Plus is shown in Figure 13.39. This set-up is installed by
PANalytical Service Engineers.
Figure 13.39: Schematic Representation of the Set-up for Non-ambient Capillary Measurements
The principle of operation of the Cryostream Plus is as follows: Liquid nitrogen is drawn up from the vessel into
the Cryostream Plus Coldhead, inside of which it evaporates. The nitrogen gas then flows outward along one
path of a heat exchange, through the Cryostream Plus Temperature Controller, to arrive at the inlet of the
nitrogen gas pump unit at a temperature of approximately 10 K below room temperature. The nitrogen gas then
passes a line drier unit and flows back via the Cryostream Plus Temperature Controller into the second path of
the heat exchanger in the Cryostream Plus Coldhead, where it is re-cooled. The flow rate is regulated by a flow
controller in the Cryostream Plus Temperature Controller. The gas temperature is regulated by a heater and
sensor before it flows along a nozzle out over the sample. The temperature regulation is set such that the
temperature indicated is the temperature at 5 mm from the end of the nozzle. Therefore you obtain the most
accurate temperatures in your sample when you install the nozzle between 5 mm and 10 mm from the sample
position.
In order to prevent condensation of water or formation of ice at low temperatures, the nitrogen gas stream req-
uires a shroud gas as it exits the nozzle. This gas can be dry air with a maximum dew point of -60 °C (213 K),
a maximum pressure of 10 bar and free from particles. Alternatively you can use an inert gas such as nitrogen.
The AD51 Dry Air Unit is available as an optional device that provides a constant stream of clean dry air.
For measurements are running more than 24 hours an auto-refill unit is available. This device controls the level
of the liquid nitrogen in the Dewar and regulates the flow of liquid nitrogen from a storage vessel into the Dewar.
07.03.27 Page 13.51
13.4.2.2 Setting up the Non-ambient Capillary Measurement System

This section describes how to set-up the X'Pert PRO MPD system for measurements on glass capillaries at non-
ambient temperatures with the use of the Cryostream Plus.
1. Make sure that you do not have any optical modules or stages mounted.
2. Mount the capillary spinner with PreFIX mounting position (see Figure 13.32) according to the
procedure described in section 12.1.1 of Chapter 12 in Part II of this User's Guide. At the end of the
procedure, do not connect to the instrument again with the data collector.
3. Mount the PW3086/70 Anti-scatter Device onto the focusing X-ray mirror according to the procedure
described in section 6.3.3.6.1 of Chapter 6 in Part II of this User's Guide).
4. Mount the special beam stop onto the PW3086/70 Anti-scatter Device (see section 20.2.4.2 in Chapter
20 in Part II of this User's Guide).
5. Mount the focusing X-ray mirror onto the goniometer's incident beam PreFIX position.
6. Mount the Cryostream Plus Coldhead onto the PreFIX mounting position of the capillary spinner (see
Figure 13.40).
7. Connect the red tube with right-angled connector of the dry air supply, the Teflon tubes Coldhead
FLOW and Coldhead SUCT and the black Coldhead cable to the Cryostream Plus Coldhead.
8. Fill the Dewar vessel with liquid nitrogen by subsequently performing the following steps in sequence:
a. Move the liquid nitrogen storage vessel close to the X'Pert PRO enclosure.
b. Put on safety glasses and safety gloves.
c. Connect the liquid nitrogen storage vessel to the Dewar vessel in the X'Pert PRO enclosure.
d. Fill the Dewar vessel with liquid nitrogen.
e. Disconnect the liquid nitrogen storage vessel.
9. If your system contains an auto-refill unit:
a. Switch on the AMI 186 Liquid Level Controller. The LED display will blink and then indicate the
liquid level. The yellow ACTIVITY LED will begin blinking.
NOTE: If the displayed level reading is below the LO SETPOINT level or exceeds the HI SETPOINT, an
audible alarm will sound. To silence the alarm, rotate the control mode rotary switch on the front
panel to the SILENCE position.
b. Set the fill toggle switch on the front panel to the position AUTO. When the switch is in this
position, the instrument is capable of automatically initiating and terminating liquid fill via the
control valve, maintaining the level between selected A and B set points.
c. Connect the liquid nitrogen storage vessel to the tube of the auto-refill unit.
10. Switch on the Cryostream Plus Controller and let the controller initialize itself. The nitrogen gas pump
unit is connected with the Cryostream Plus Controller and will switch on automatically, when it is in
use.
11. Make sure that the goniometer head that you are going to use is equipped with the white screening plate.
Mount the capillary sample onto the goniometer head (see section B.4 in Appendix B of this User's
Guide).
12. Go on-line (Connect) using the data collector software.
13. Mount and align the capillary sample that you are going to measure onto the capillary spinner. This
procedure is described in section 12.3.2 in Chapter 12 of Part II of this User's Guide.
14. Mount the required diffracted beam fixed anti-scatter devices onto the X'Celerator or PIXcel detector as
given in Table 6.12 and Table 6.13 in Chapter 6 of Part II of this User's Guide respectively.
15. Mount the X'Celerator or PIXcel onto the goniometer' s diffracted beam PreFIX position.
16. Slide the Coldhead forward to the sample by turning the black knob underneath the Coldhead.
The distance between the Coldhead's nozzle and the measurement position on the sample must be
Page 13.52 07.03.27
between 5 mm and 10 mm for optimum temperature control. If necessary you can also translate and
rotate the Coldhead to the correct position aligned with the capillary by turning the black knobs at the
right-hand side of the Coldhead.
Figure 13.40: X'Pert PRO MPD System with Cryostream Plus
NOTE: If the data collector software indicates that the temperature controller is not responding, you should
now disconnect and connect again in the data collector in order to be able to control the Cryostream
Plus with the data collector.
17. Switch on the AD51 Dry Air Unit. The POWER lamp of the unit should light as soon as the electrical
supply is connected. Set the black switch from “0” to “1”; the RUN lamp will flash for 4 seconds after
which you will hear the compressor start and the RUN lamp continuously light.
18. Set the required dry air flow rate with the needle valve on the flow meter on the front panel of the AD51
Dry Air Unit between 10 l/min and 15 l/min.
19. Press the “START” button on the Cryostream Controller. The LED above the button will light.
This completes the experimental set-up procedure for the non-ambient capillary measurement. You can start
your experiments now.
07.03.27 Page 13.53

13.5 PHENIX HELIUM POWDER CRYOSTAT

The PheniX Helium Powder Cryostat (9430 500 21391 or 9430 500 21571) is a PreFIX attachment for X'Pert
PRO MPD systems that allows temperature studies on flat plate powder samples and thin films from room
temperature down to 11 K (-262 °C), with a temperature stability of 0.1 K. Cooling is performed using
compressed helium gas provided by a water-cooled compressor. It can cool down from room temperature to
20 K in 35 minutes and to 11 K in a further 25 minutes. It takes 40 minutes for the sample to return to room
temperature.
Measurements can be performed over the full 2theta range on both X'Pert PRO Theta-Theta and Omega-2Theta
systems.
Solid samples with a maximum diameter of 20 mm can be mounted onto a chromium-plated copper or anodized
aluminium flat sample holder. Sample holders with a raised edge (with a height of 1 mm) are available for
powder samples. The z-adjustment range is 9 mm.
The sample stage is mounted onto a PC-controllable alignment stage. This option allows the sample position to
be automatically corrected for temperature-induced height variations, based on (user-definable) calibration data.
Figure 13.41: PheniX Helium Powder Cryostat
The delivery includes the PheniX Sample Stage and Coldhead, mounted onto a PreFIX support, a 730 series
temperature controller, a height controller and a vacuum system, including a sealed membrane (pre-vacuum)
pump and a turbomolecular (high vacuum) pump, and a compressor.
Please refer to the Oxford Cryosystems manual "Oxford PheniX Operation & Instruction Guide" for further
details. Use of the PheniX cryostat with X'Pert PRO MPD systems is described in section 13.5.2.
Page 13.54 07.03.27

13.5.1 Accessories
13.5.1.1 Temperature Control Unit
The 730 Series Temperature Controller is used to control the temperature of the flat plate or powder sample. The
controller is shown in Figure 13.42. It is integrated in X'Pert PRO MPD systems in such a way that it can be
operated using the data collector software.
Further information about the 730 Series Temperature Controller and its use is given in the Oxford Cryosystems
manual "Oxford PheniX Operation & Instruction Guide". Use of the 730 Series Temperature Controller with
X'Pert PRO MPD systems is described in section 13.5.2.
Figure 13.42: PheniX Temperature Controller, Cryodrive and Vacuum Trolley
13.5.1.2 Vacuum System

The PheniX cryostat’s vacuum system comprises a trolley with a Seal Vac diaphragm pump, a Cryo Vac Turbo
Station with integrated diaphragm pump along with a wide range gauge and a display and operating unit. It is
shown in Figure 13.42. The Cryo Vac Turbo Station is used to pump the main body of the PheniX cryostat. The
Seal Vac diaphragm pump evacuates the rotating seal of the PheniX to ensure that when the seal moves, the main
body vacuum is not affected.
Further information about the vacuum system and its use is given in the Oxford Cryosystems manual "Oxford
PheniX Operation and Instruction Guide" and the manuals supplied with the vacuum system. Use of the vacuum
system with the PheniX cryostat in X'Pert PRO MPD systems is described in section 13.5.2.
07.03.27 Page 13.55

13.5.1.3 Cryodrive Compressor

The Cryodrive is a compressor that supplies compressed helium gas in a closed circuit. It is shown in Figure
13.42. The Cryodrive is supplied fully charged with helium. There are two pressurized helium lines (one supply
line and one return line) connecting it to the PheniX coldhead.
The Cryodrive is water-cooled. The cooling water supply has a typical flow rate of 5.0 l/min; the minimum flow
rate is 1.5 l/min and the maximum flow rate is 7.0 l/min. The water supply pressure must be between 2.0 bar and
7.0 bar; the water temperature must be between 4 °C (277 K) and 26 °C (299 K).
The cooling power of the Cryodrive is controlled by the PheniX temperature controller.
Use of the Cryodrive together the PheniX cryostat on X'Pert PRO MPD systems is described in section 13.5.2.
Please refer to the Cryodrive Instruction Manual for more information.
13.5.1.4 PC-controllable Alignment Stage

The PC-controllable alignment stage onto which the PheniX Cryostat is mounted includes a stepper motor-
driven precision stage that allows height alignment of the chamber under PC control using the software program
"PheniX Height Controller". The program reads temperature data as stored by the data collector software in a
temperature log file and uses this information to correct the sample position for temperature-induced height
variations, based on (user-definable) calibration data.
Please refer to the Oxford Cryosystems manual "Oxford PheniX Operation and Instruction Guide" and the data
collector software's help for further details.
Adjusting the sample height using the PC-controllable alignment stage is described in section 13.5.2.6.
13.5.2 Use
13.5.2.1 Experimental Set-up
A schematic representation of the X'Pert PRO MPD system set up for measurements at cryogenic temperatures
using the Oxford PheniX is shown in Figure 13.43. This set-up is installed by PANalytical Service Engineers.
The principle of operation of the PheniX is as follows: Compressed helium gas is transported from the Cryodrive
compressor to the coldhead of the PheniX sample stage, where the gas is expanded, the gas then flows back into
the compressor in a closed cycle. The sample stage is cooled by the conduction of heat between the sample stage
and the coldhead. The temperature of the sample stage and the cooling power of the Cryodrive are controlled by
the temperature controller. The compressor is water-cooled. There is no helium gas consumption in the system;
the helium gas closed cycle circuit is sealed.
A vacuum system with a turbomolecular vacuum pump is used to continuously pump the vacuum space inside
the PheniX to minimize heat leaks. It is important to maintain a good vacuum (<10-4 mbar); otherwise it is not
possible to achieve extremely low sample temperatures.
Page 13.56 07.03.27

Figure 13.43: Helium Powder Cryostat XRD Measurement System - Schematic Representation
13.5.2.2 Setting up the Cryostat System for Low Temperature Measurements

This section describes how to set the X'Pert PRO MPD system up for measurements at cryogenic temperatures.
1. Make sure that you do not have any optical module mounted on the X'Pert PRO MPD system.
2. Mount the PheniX sample stage to the X'Pert PRO goniometer according to the procedure described in
section 12.1.1 of Chapter 12 of Part II of this User's Guide. At the end of the procedure, do not connect
the instrument to the data collector.
3. Open the lower front panel of the Cryodrive compressor and check the helium charge pressure. The
charge pressure gauge should read 16.5 bar ± 1.0 bar in inactive state. If the pressure is less than 15.5
bar, contact your local PANalytical Service Engineer.
NOTE: Under normal operating conditions the helium charge pressure is about 22 bar and will noticeably
oscillate by around 0.5 bar.
A schematic diagram showing the connections between the PheniX cryostat and its accessories is shown in
Figure 13.43. Follow the next steps to connect the PheniX system.
07.03.27 Page 13.57

4. Connect the two pressurized helium lines between the PheniX coldhead and the Cryodrive compressor.
The helium supply line has a red band at both ends and the helium return line has a green band at both
ends.
NOTES: a) When tightening the nut connections on the pressurized helium lines, hold the line in alignment
with the fixed coupling to prevent loss of helium gas.
b. 2. Do NOT allow the fitting to rotate.
Figure 13.44: X'Pert PRO MPD System with Phenix Cryostat Sample Stage Mounted
5. Connect the signal cable from the Cryodrive to the PheniX coldhead.
6. Connect the vacuum lines between the PheniX coldhead and the vacuum pumps.
7. Connect the ColdHead cable from the PheniX temperature controller to the PheniX coldhead.
This completes the experimental set-up procedure of the PheniX Cryostat. You can now mount your sample onto
the sample stage and switch the system on according to procedures described in sections 13.5.2.3 and 13.5.2.4
respectively.
13.5.2.3 Mounting a Sample onto the Sample Position

The PheniX cryostat is ideally suited for flat plate samples with a maximum diameter of 20 mm. The sample
holder with the raised edge can be used if you want to measure powder samples. Mount the sample onto the
sample position as follows:
1. Open the sample stage by opening the four clips at the side of the sample stage and removing the outer
cover.
2. Undo the four screws at the side of the inner cover and remove it. Now you have access to the sample
holder.
Page 13.58 07.03.27
3. Mount the sample holder onto its position on the sample stage.
4. Mount the sample:
a. If you have a flat plate sample, mount it on the flat sample holder. You can, if required, use a small
droplet of Zapon lacquer to ensure a good thermal contact.
b. If you have a powder sample, use the sample holder with a cavity in the center. Use a spatula to
press the powder into the cavity of the sample holder and smooth the surface, for example: by
pressing it with a glass platelet.
Alternatively, you can mix the powder with a small quantity of diluted Zapon lacquer solution. Use
a spatula to apply the slurry into the cavity. Allow sufficient time to let the sample dry and become
an adhesive and solid substance.
Figure 13.45: Removing the Outer and Inner Cover from the PheniX Cryostat
5. Put the inner cover over the sample holder and fix the four screws.
6. Put the outer cover on the PheniX cryostat and fix the four clips.
The sample is now mounted onto the sample stage. You can start to switch the system on.
13.5.2.4 Switching the system on and cooling down

When the sample has been mounted and the PheniX cryostat has been closed, you can continue with switching
the system on and cooling down.
07.03.27 Page 13.59

Figure 13.46: Vacuum Trolley seen from the Rear

1. Switch on the Seal Vac diaphragm pump (located on the vacuum trolley behind the turbomolecular
pump) with the green switch, refer to Figure 13.46.
2. To ensure a good vacuum, open the gas ballast valve on the diaphragm pump for ten minutes to remove
residual water vapor and air from the lines and the PheniX cryostat. To open the valve, push (twist) the
knurled sleeve down.
3. Wait for ten minutes and close the ballast valve by pushing the knurled sleeve up.
4. Switch on the Cryo Vac Turbo Station with the power switch indicated in Figure 13.42. The display
unit then goes through an initialization process.
5. Press the left or right arrow keys on the display unit to scroll through the menu options and select '309:
Act rotspd' to observe the rotation speed of the turbomolecular pump when being used. The rotation
speed of the turbomolecular pump will reach 1500 Hz.
NOTE: We recommend that you to leave the display unit on this menu item when the system is running.
6. If the vacuum reading begins to rise (or does not drop) during the early stages of pumping down, open
the gas ballast valve on the diaphragm backing pump to ensure a good vacuum. The position of the gas
ballast valve is indicated in Figure 13.46.
7. Wait for 10 to 20 seconds or until the vacuum pressure drops again, and close the gas ballast valve.
Page 13.60 07.03.27
When the vacuum pressure is less than 10-4 mbar, the PheniX is ready to be used.
NOTE: Always remember to close the ballast valve.

8. Switch on the PheniX temperature controller by pressing the START button on the front panel, refer to
Figure 13.42. The LED above the button will light.
9. Turn on the water supply of the Cryodrive compressor and set a flow rate of 5.0 l/min.
10. Use the rocker switch on the front panel to switch the Cryodrive compressor on. The Cryodrive then
goes through an initialization procedure. The Cryodrive is ready for use after the green
"COMPRESSOR ON" LED has flashed for 3 seconds.
11. Check that the helium charge pressure gauge on the Cryodrive compressor now reads approximately 21
bar.
12. Go on-line (Connect) using the data collector software with a configuration that contains the PheniX
cryostat.
This completes the experimental set-up procedure for the low temperature measurements. You can start now
start to adjust the sample height.
13.5.2.5 Adjusting the Sample Height Using the PheniX Height Controller
The PheniX cryostat is mounted onto a PC-controllable alignment stage so that the sample height can be adjusted
automatically to correct the sample position for temperature effects.
Before you start your measurements, make sure that the sample height is correctly adjusted as described here:
1. Mount the incident beam PreFIX module that you are going to use in your experiments.
2. Mount a programmable receiving slit, or an X'Celerator, rotated through 90° (see section 21.4 in
Chapter 21 of Part II of this User's Guide) or a PIXcel, or a rocking curve attachment onto the diffracted
beam PreFIX position.
3. Insert a copper (0.2 mm) attenuation foil into the incident beam PreFIX module in order to protect the
detector from being saturated.
5. Insert a beam mask 10 into the incident beam PreFIX module.
6. Depending on your diffracted beam path components:
a. If you are using a programmable receiving slit, set it to 3 mm.
b. If a programmable or a fixed anti-scatter slit assembly is mounted onto the programmable
receiving slit, set it to 4º.
c. If you are using an X'Celerator, set it into receiving slit mode and use the maximum active length
d. If you are using a PIXcel, set it into receiving slit mode and use the maximum active length (14
mm). Do not insert a slit into the fixed anti-scatter slit holder.
e. If you are using a rocking curve attachment, do not insert a slit.
7. Set ω and 2θ to 0°.
8. Set the high tension generator to 30 kV, 40 mA (if you have the ceramic X-ray tube with an iron anode
set the generator to 30 kV, 30 mA).
9. Start the PheniX Height Controller program on the PC that is controlling your X'Pert PRO system.
10. When you are using the PheniX Height Controller for the first time, open the menu window “Settings”
07.03.27 Page 13.61
and insert the following information:

a. Insert the folder and file names of the Temperatures File. Normally the Temperatures File is stored
under the name “D:\Temperature.txt”.
b. Select the correct Serial Port for the communication between the PC and the alignment stage
controller.
Figure 13.47: PheniX Height Controller - Settings Menu
NOTE: The Temperatures File contains the current temperature value of the non-ambient chamber, as
stored by the data collector software. This file is read by the PheniX Height Controller to
automatically adjust the sample height position as a function of temperature. The file name and
location must also be specified in the data collector software's initialization file "xpert.ini". After a
default installation this file can be found in the folder:
the section header "[Diffractometer communication]": "NALogFile=<path><file name>.<file
extension>", for example:
...
...
Press Apply to activate the changes.

11. Check that the "Temperature File Mode" check box on the "Settings" tab is unchecked. In this situation
you can directly change the height of the PheniX cryostat by entering a command on the "Commands"
tab (see Figure 13.48).
Page 13.62 07.03.27

Figure 13.48: PheniX Height Controller - Commands Menu

12. Open the shutter and use the "Move down" command to move the sample stage down so that the
sample does not block the direct beam anymore and the direct beam no longer increases. Make a note of
the direct beam intensity (Ip).
13. Move the sample stage up with small increments using the "Move up" command until the direct beam
intensity is equal to Ip/2.
15. The next action depends on whether Im > Ip/2 (step a), or Im < Ip/2 (step b):
a. If Im > Ip/2, move the sample up with small increments until the maximum intensity measured in
an ω scan (Im) equals Ip/2.
b. If Im < Ip/2, move the sample down with small increments until the maximum intensity measured
in an ω scan (Im) equals Ip/2.
16. Check the "Temperature File Mode" check box on the "Settings" tab. The sample height is now
automatically adjusted with temperature. You can display the current sample temperature and position
on the "Display" tab (see Figure 13.49).
07.03.27 Page 13.63

Figure 13.49: PheniX Height Controller - Display Menu
This completes the sample height adjustment procedure. You can now start to perform your experiments.
13.5.2.6 Switching Off the Vacuum System and Releasing the Vacuum in the PheniX
After you have performed your measurements, let the sample stage warm up to room temperature. This will take
about 40 minutes. You then can switch the vacuum system off and release the vacuum. In order to release the
vacuum in a controlled way, follow the procedure given below.
1. Press the Turbo Station Start / Stop key on the display of the vacuum trolley to switch the vacuum
system off.
2. Wait until the rotation speed of the turbomolecular pump has slowed down to less than 200 Hz.
3. Slowly open the vent valve on the back of the turbomolecular pump on the Cryo Vac Turbo Station.
4. Switch the Seal Vac diaphragm pump off.
5. Now you can open the PheniX Cryostat sample stage. Do not forget to close the vent valve on the
turbomolecular pump.
Page 13.64 07.03.27

Chapter 14
Beam Knives
Contents
14.1 General............................................................................................................................... 14 - 3
14.2 Beam Knives for Reflectivity Measurements ................................................................. 14 - 3
14.2.1 PW3061/25 Adjustable “de Wolff’s” Knife......................................................................... 14 - 3
14.2.1.1 Use ....................................................................................................................... 14 - 4
14.2.2 PW3075/66 Beam Knife for Positioning Stages .................................................................. 14 - 7
14.2.2.1 Use ....................................................................................................................... 14 - 8
14.3 Beam Knives Used with the X’Celerator or PIXcel..................................................... 14 - 10
14.3.1 PW3064/10 Beam Knife for Sample Spinner .................................................................... 14 - 11
14.3.2 PW3071/65 Beam Knife for Stage for Flat Samples/Holders............................................ 14 - 11
14.3.3 PW3072/65 Beam Knife for Stationary Sample Stage ...................................................... 14 - 12
14.3.4 PW3074/10 Beam Knife for Multi-purpose Sample Stage ................................................ 14 - 13
14.3.5 PW3075/67 Beam Knife for Positioning Stage.................................................................. 14 - 13
14.3.6 Use...................................................................................................................................... 14 - 15
07.03.27 Page 14.1

Page 14.2 07.03.27

Part II - Chapter 14: Beam Knives
14.1 GENERAL
Beam knives are inserted into the X-ray beam path in X-ray diffraction in order to improve the resolution of a
reflectivity measurement or to increase the peak-to-background ratio in measurements with line (1-dimensional)
detectors.
Two types of beam knife are available for use on X’Pert PRO systems:
• Adjustable “De Wolff’s” knives which are used for reflectivity measurements on small samples or on
samples with bent or undulating surfaces. This type of beam knife is described in section 14.2.
• Beam knives used for measurements with the X’Celerator and PIXcel detectors. This type of beam knife
is described in section 14.3.
14.2 BEAM KNIVES FOR REFLECTIVITY MEASUREMENTS

X-ray reflectivity measurements require extremely flat sample surfaces, for sample alignment and for an
accurate determination of intensity changes, especially near the critical angle. However, in practice the sample
surface is not always perfectly flat; it may be bent or undulating due to manufacturing or production processes.
In these cases a beam knife is necessary in order to reduce the effective reflecting area of the sample. The beam
knife can also be used to limit the beam size in measurements on small samples.
A beam knife is placed just above the sample surface in the center of the goniometer. A pictorial representation
of the beam path when a beam knife is used is shown in Figure 14.1. The beam knife works by blocking a part
of the incident beam and a part of the reflected beam, only allowing the X-ray beams to pass between the knife
edge and the sample surface. This means that only those X-rays reflected from a very small area of the sample
surface are available for the measurement. This small sample area is assumed to be flat enough for accurate
determination of the reflectivity curve.
This section describes the adjustable De Wolff’s knives that are used with X’Pert PRO systems, and their
adjustment, they are:
• PW3061/25 for X’Pert PRO MRD Systems, described in section 14.2.1.
• PW3075/66 for PW3075/6x Positioning Stages on X’Pert PRO MPD Systems, described in section
14.2.2.
Figure 14.1: The Beam Path without and with a Beam Knife
14.2.1 PW3061/25 Adjustable “de Wolff’s” Knife

The adjustable “De Wolff’s” knife is a beam knife designed for use in X’Pert PRO systems and is shown in
Figure 14.2. It can be mounted on the dial gauge holder on the MRD Sample Cradle (PW3060/20), refer to
Figure 11.16 in Chapter 11 in Part II of this User’s Guide.
When delivered with a factory aligned X’Pert PRO MRD system the beam knife is factory adjusted with respect
to a flat glass sample coated with a thin chromium film (part of PW3132/62).
Use of the beam knife and how to adjust it for a reflectivity measurement is described in section 14.2.1.1.2.
07.03.27 Page 14.3

Figure 14.2: PW3061/25 Beam Knife for Reflectivity Measurements
14.2.1.1 Use
This section describes how to adjust the De Wolff’s knife prior to X-ray reflectivity measurements. If your beam
knife has been delivered as a separate item you have to adjust it for use on your system before it is used for the
first time. This procedure is given in section 14.2.1.1.1. When the beam knife is adjusted, either by yourself
before first time use following section 14.2.1.1.1, or in the factory together with the rest of your system, you can
continue with the procedure to adjust the beam knife for reflectivity measurements as described in section
14.2.1.1.2.
14.2.1.1.1 Adjustment of the Beam Knife before First Time Use

When the beam knife assembly is delivered as a separate unit then the following procedure should be followed
to adjust the unit for use before it is used for the first time. Before you start to adjust the beam knife, check that
the height of the tube’s line focus is correct (see also: section 1.4.9.2 in Chapter 1 in Part II of this User’s Guide).
1. Use the data collector software to set all the MRD cradle positions (X, Y, Z, ψ, and ϕ) to 0. Make sure
that all of the application offsets are set to 0 in the data collector software.
2. Install the 4-inch wafer holder table on the mounting disk (see Figure 11.1).
3. Install the dial gauge assembly on the MRD cradle.
4. Move X and Y to 30 mm and set Z to the reference height as indicated on the dial housing (usually 1.0).
Make a note of Z.
5. Remove the dial gauge assembly.
6. Move the knife edge to its highest position using the height adjustment knob. See Figure 14.2.
7. Carefully install and secure the beam knife assembly by tightening the mounting/locking knob on the
MRD cradle on the dial gauge assembly holder.
8. Check if any play can be detected by carefully moving the beam knife sideways. If play is evident then
carefully tighten the unit with the setscrew (see Figure 14.2). The clamping force should be adjusted
such that the assembly can be removed and installed with only a fractional play.
Page 14.4 07.03.27

9. Set the knife tilt using the tilt adjustment knob (fine) such that it is centered, visible by observing both
gaps “G” (see Figure 14.3) at the side of the dial holder. Both gaps must have the same opening.
10. Lower the knife edge towards the sample table using the height adjustment knob, see Figure 14.2, until
the edge just touches the sample table.
11. Align the tilt of the knife edge such that it is parallel with the sample table surface. This can be done by
loosening the three screws at the back that secure the dial holder assembly and adjusting the holder
assembly using the tilt adjustment screws (coarse).
12. After completion secure the holder assembly by tightening the three screws.
13. Check if the tilt of the knife edge is still correct. If necessary adjust the tilt finely using the tilt
adjustment knob (fine).
14. Check if the dial indicates approximately 1.0 (same as the dial gauge assembly of the MRD cradle). If
this is not the case, loosen the dial gauge clamp screw (see Figure 14.2), adjust the dial gauge itself
until it indicates 1.0 and then tighten the clamp screw again. Make sure that you do not tighten the
clamp screw too much as this may result in the dial shaft sticking.
15. Move the knife edge to its highest position using the height adjustment knob. Dismount the beam knife.
16. Check if the dial indicator has a range from 0.5 to 2.5 mm by using the height adjustment knob. If not
then loosen the dial gauge clamp screw underneath the dial and adjust until correct. Mount the beam
knife on the dial gauge assembly holder and repeat from step 14.
This completes the mechanical adjustment of the beam knife assembly. You can now continue with the
procedure given in section 14.2.1.1.2 to adjust the beam knife for reflectivity measurements.
14.2.1.1.2 Adjustment of the Beam Knife for Reflectivity Measurements
NOTE: The sample has to be optimized for a reflectivity measurement before the beam knife assembly is
installed (refer to section 11.2.2.2 in Chapter 11 in Part II of this User’s Guide).
1. If necessary, calibrate the ψ position of the MRD cradle to 0° (typical for the sample in use).
2. Make a note of the optimal, current sample position (X, Y and Z).
3. Move X, Y or Z such that the sample is protected from damaging when installing the beam knife.
4. Set the beam knife to the highest possible position using the small, knurled height adjustment knob. Do
NOT use this knob as a rotating handle!
5. Install the beam knife assembly on the dial gauge assembly holder on the MRD cradle and secure it by
tightening the mounting/locking knob.
6. Check if any play can be detected by carefully moving the beam knife sideways. If play is evident then
carefully tighten the unit with the setscrew (See Figure 14.2) until the play is removed.
7. Set the sample back to the positions as noted in step 2.
8. Close the enclosure doors, open the shutter. Make a note of the direct beam intensity with the sample
adjusted to the correct height (Z) and its surface parallel to the beam. Use the appropriate generator
setting and attenuation foils to reduce the direct beam intensity!
9. Carefully move the beam knife towards the sample using the height adjustment knob until a thin gap is
visible between the sample surface and the knife edge.
Tip: Use a piece of paper as background and monitor the gap from the side.
10. Adjust the tilt of the knife edge such that it is parallel with the sample surface using the tilt adjustment
knob (fine) (see Figure 14.3). The tilt setting is visible at the two gaps “G”.
NOTE: For larger tilt changes the dial gauge head can be loosened by undoing the three screws and then
setting the dial gauge holder to the required tilt setting with the tilt adjustment screws (coarse). The
zero position of the dial gauge is changed by loosening the coarse tilt adjustment screws. After that
small tilt adjustments can be done with the tilt adjustment knob (fine).
07.03.27 Page 14.5

Figure 14.3: Detail of the Beam Knife Controls

11. Move the knife edge away from the sample surface to its highest position using the height adjustment
knob.
12. Close the shutter and lower the knife edge towards the sample until a small gap is visible.
13. Open the shutter and observe the intensity; the intensity must be reduced about 30% compared to the
intensity without a beam knife (as noted in step 8) by adjusting the knife edge with the height
adjustment knob. For example, a typical direct beam intensity is ~200 000 cps using the appropriate
attenuation foil. With the sample correctly adjusted in the beam it is then ~100 000 cps, the beam
intensity with the knife edge must be then ~70 000 cps. For strongly curved samples the beam knife can
be put even further into the X-ray beam.
NOTE: If a concave sample has to be measured, the optimal sample height can differ from the adjusted
height using the normal procedure (setting the sample to 50% of the direct beam intensity). For
these type of samples the height should be also checked, for at least two scans, using two different
2θ-θ values (rocking curves for example: on a fringe position or below the critical angle). For a
correct Z value of the sample at both angle settings, the position of ω, at maximum found intensity,
has to be half 2θ.
At this stage the system can be used to carry out a reflectivity measurement.
CAUTION
Remove the beam knife assembly before increasing the Z position
or moving X, Y or φ.
Page 14.6 07.03.27

14.2.2 PW3075/66 Beam Knife for Positioning Stages

The PW3075/66 Beam Knife is an adjustable “De Wolff’s” knife. It is designed for use with reflectivity
measurements on samples mounted on PW3075/6x Positioning Stages on vertical X’Pert PRO MPD systems
and is shown in Figure 14.4. It can be PreFIX mounted onto the PreFIX U-block on the PW3075/6x Positioning
Stage, refer to Figure 12.41, Figure 12.43 and Figure 12.45 in Chapter 12 in Part II of this User’s Guide.
When delivered with a factory aligned X’Pert PRO MPD system the beam knife is factory adjusted with respect
to a flat glass sample coated with a thin chromium film (part of PW3132/62). The alignment of a beam knife is
positioning stage specific. Adjustment of the beam knife before first time use is described in section 14.2.2.1.1.
Adjustment of the beam knife prior to reflectivity measurements is described in section 14.2.2.1.2.
Figure 14.4: PW3075/66 Beam Knife for Reflectivity Measurements
07.03.27 Page 14.7

14.2.2.1 Use
This section describes how to adjust the De Wolff’s knife prior to X-ray reflectivity measurements. If your beam
knife has been delivered as a separate item you have to adjust it for use on your system before it is used for the
first time. This procedure is given in section 14.2.2.1.1. When the beam knife is adjusted, either by yourself
before first time use following section 14.2.2.1.1, or in the factory together with the rest of your system, you can
continue with the procedure to adjust the beam knife for reflectivity measurements as described in section
14.2.1.1.2.
14.2.2.1.1 Adjustment of the Beam Knife before First Time Use

When the beam knife assembly is delivered as a separate unit then the following procedure should be followed
to adjust the unit for use before it is used for the first time. Before you start to adjust the beam knife, check that
the height of the tube’s line focus is correct (see also: section 1.4.9.2 in Chapter 1 in Part II of this User’s Guide).
1. Install the PW3075/65 Dial Gauge Assembly on the PreFIX position on the PW3075/6x Positioning
Stage.
2. Move X and Y (if present) so that the center of the sample platform is below the dial gauge’s shaft. Set Z
to the reference height as indicated on the dial housing (usually 1.0).
3. Remove the dial gauge assembly.
4. Move the knife edge to its highest position using the height adjustment knob. See Figure 14.4.
5. Carefully install and secure the beam knife assembly on the PreFIX position of the PW3075/6x
Positioning Stage.
6. Set the knife tilt using the tilt adjustment knob (fine) such that it is centered, visible by observing both
gaps “G” (see Figure 14.5) at the side of the dial holder. Both gaps must have the same opening.
7. Check that the edge of the dial gauge clamp is parallel to the edge of the block (dial gauge holder
assembly) onto which the dial gauge is mounted (see Figure 14.4). If this is not the case, loosen the
three screws at the back that secure the dial gauge holder and adjust the holder using the tilt adjustment
screws (coarse). Tighten the three screws to secure the holder into position.
8. Lower the knife edge towards the sample table using the height adjustment knob (coarse), see Figure
14.4, until the edge just touches the sample table.
9. Align the sample table using the tilt movement such that it is parallel with the knife edge.
10. Check if the dial indicates approximately 1.0 (same as the PW3075/65 Dial Gauge Assembly). If this is
not the case, loosen the dial gauge clamp screw (see Figure 14.4), adjust the dial gauge itself until it
indicates 1.0 and then tighten the clamp screw again. Make sure that you do not tighten the clamp screw
too much as this may result in the dial shaft sticking.
11. Move the knife edge to its highest position using the height adjustment knob. Dismount the beam knife.
12. Check if the dial indicator has a range from 0.5 to 2.5 mm by using the height adjustment knob. If not
then loosen the dial gauge clamp screw underneath the dial and adjust until correct. Mount the beam
knife on the dial gauge assembly holder and repeat from step 4.
This completes the mechanical adjustment of the beam knife assembly. You can now continue with the
procedure given in section 14.2.2.1.2 to adjust the beam knife for reflectivity measurements.
14.2.2.1.2 Adjustment of the Beam Knife for Reflectivity Measurements

NOTE: The sample has to be optimized for a reflectivity measurement before the beam knife assembly is
installed (refer to section 12.13.5.3 in Chapter 12 in Part II of this User’s Guide).
1. Set the beam knife to the highest possible position using the small, knurled height adjustment knob. Do
NOT use this knob as a rotating handle!
2. Install the PW3075/66 Beam Knife Assembly on the PreFIX position of the PW3075/6x Positioning
Stage. Be very careful not to damage the sample during this operation.
3. Carefully move the beam knife towards the sample using the height adjustment knob until a thin gap is
visible between the sample surface and the knife edge.
Tip: Use a piece of paper as background and monitor the gap from the side.
Page 14.8 07.03.27

4. Adjust the tilt of the knife edge such that it is parallel with the sample surface using the tilt adjustment
knob (fine) (see Figure 14.3). The tilt setting is visible at the two gaps “G”.
NOTE: For larger tilt changes the dial gauge head can be loosened by undoing the three screws and then
setting the dial gauge holder to the required tilt setting with the tilt adjustment screws (coarse). The
zero position of the dial gauge is changed by loosening the coarse tilt adjustment screws. After that
small tilt adjustments can be done with the tilt adjustment knob (fine).
Figure 14.5: Detail of the Beam Knife Controls

5. Move the knife edge away from the sample surface to its highest position using the height adjustment
knob.
6. Close the enclosure doors, open the shutter. Make a note of the direct beam intensity with the sample
adjusted to the correct height (Z) and its surface parallel to the beam. Use the appropriate generator
setting and attenuation foils to reduce the direct beam intensity!
7. Close the shutter and lower the knife edge towards the sample until a small gap is visible.
8. Open the shutter and observe the intensity; the intensity must be reduced about 30% compared to the
intensity without a beam knife by adjusting the knife edge with the height adjustment knob. For
example, a typical direct beam intensity is ~200 000 cps using the appropriate attenuation foil. With the
sample correctly adjusted in the beam it is then ~100 000 cps, the beam intensity with the knife edge
must be then ~70 000 cps. For strongly curved samples the beam knife can be put even further into the
X-ray beam.
NOTE: If a concave sample has to be measured, the optimal sample height can differ from the adjusted
height using the normal procedure (setting the sample to 50% of the direct beam intensity). For
these type of samples the height should be also checked, for at least two scans, using two different
θ/2θ values (rocking curves for example: on a fringe position or below the critical angle). For a
correct Z value of the sample at both angle settings, the position of ω, at maximum found intensity,
has to be half 2θ.
07.03.27 Page 14.9

At this stage the system can be used to carry out a reflectivity measurement.
CAUTION
Remove the beam knife assembly before increasing the Z position
or moving X, Y or ϕ.
14.3 BEAM KNIVES USED WITH THE X’CELERATOR OR PIXCEL

In X-ray diffraction experiments, X-rays are not only diffracted by the sample, but may also be scattered by the
air, by parts of the diffractometer, or by the sample holder. Scattered radiation gathered by the detector may give
rise to an increased background in the diffractogram. A beam knife can be inserted into the X-ray beam path in
X-ray diffraction experiments that utilize an X’Celerator or PIXcel to reduce the background to a low level. This
ensures a good signal-to-background ratio. For standard detectors, the task of reducing the background intensity
is performed by incident beam and diffracted beam anti-scatter slits.
Several types of beam knife can be used with the X’Celerator or PIXcel. These beam knives are specific to the
sample stage which they are to be used with. They are listed in Table 14.1.
Optimizing the height of the beam knife with respect to the sample surface for a measurement is described in
section 14.3.6.
Table 14.1: Sample Stages and their Corresponding Beam Knife
Sample Stage Beam Knife

Section
Type Type
Description Description
Number Number
PW3064/00 Spinner for PW18xx Sample PW3064/10 Beam Knife for Sample Spinner 14.3.1
Holders
PW3064/60 Reflection-transmission Spinner PW3064/10 Beam Knife for Sample Spinner 14.3.1
for PW18xx Sample Holders
PW3071/60 Stage for Flat Samples/Holders PW3071/65 Beam Knife Stage for Flat 14.3.2
Samples/Holders
PW3072/60 Stationary Stage for PW18xx PW3072/65 Beam Knife for Stationary 14.3.3
Sample Holders Sample Stage
PW3074/00 Multi-purpose Sample Stage PW3074/10 Beam Knife for Multi-purpose 14.3.4
Sample Stage
PW3075/6x Positioning Stage PW3075/67 Beam Knife for Positioning 14.3.5

Sample Stage
Page 14.10 07.03.27

14.3.1 PW3064/10 Beam Knife for Sample Spinner

The PW3064/10 Beam Knife for Sample Spinner can be mounted onto the PW3064/x0 Sample Spinner for
X-ray diffraction experiments using the PW3015/x0 X’Celerator or the PW3018/00 PIXcel. The beam knife is
shown in Figure 14.6. Instructions on how to mount this beam knife are given in sections 12.4.1.3.1 and
12.5.1.3.1 in Chapter 12 in Part II of this User’s Guide.
The height of the beam knife above the sample can be adjusted so that the gap between the knife and the sample
surface is between 0.5 mm and 5 mm. When the beam knife is in its lowest position (the upper line of the
millimeter scale is opposite the reference line), the gap between the sample reference plane and the knife edge
is 0.5 mm. Selecting the optimum height of the beam knife above the sample surface is described in section
14.3.6.
Setting
Screw
(Not Visible
on this view)
Figure 14.6: PW3064/10 Beam Knife for Sample Spinner
14.3.2 PW3071/65 Beam Knife for Stage for Flat Samples/Holders

The PW3071/65 Beam Knife can be mounted onto the PW3071/60 Stage for Flat Samples or Samples in Flat
Holders for X-ray diffraction experiments using the PW3015/x0 X’Celerator or the PW3018/00 PIXcel. The
beam knife is shown in Figure 14.7. Instructions on how to mount this beam knife are given in section
12.10.1.2.1 in Chapter 12 in Part II of this User’s Guide.
14.3.6.
07.03.27 Page 14.11

Setting
Screw
(Not Visible
on this view)
Figure 14.7: PW3071/65 Beam Knife for Stage for Flat Samples/Holders
14.3.3 PW3072/65 Beam Knife for Stationary Sample Stage

The PW3072/65 Beam Knife can be mounted onto the PW3072/60 Stationary Stage for PW18xx Sample
Holders for X-ray diffraction experiments using the PW3015/x0 X’Celerator or the PW3018/00 PIXcel. The
beam knife is shown in Figure 14.7. Instructions on how to mount this beam knife are given in section 12.11.1.3.1
14.3.6.
Setting
Screw
Figure 14.8: PW3072/65 Beam Knife for Stationary Stage for PW18xx Sample Holders
Page 14.12 07.03.27

14.3.4 PW3074/10 Beam Knife for Multi-purpose Sample Stage

The PW3074/10 Beam Knife can be mounted onto the PW3074/00 Multi-purpose Sample Stage for X-ray
diffraction experiments using the PW3015/x0 X’Celerator or the PW3018/00 PIXcel. The beam knife is shown
in Figure 14.9. Instructions on how to mount this beam knife are given in section 12.12.1.6.1 in Chapter 12 in
surface is between 0.5 mm and 5 mm. Selecting the optimum height of the beam knife above the sample surface
is described in section 14.3.6.
Setting
Screw
Figure 14.9: PW3074/10 Beam Knife for Multi-purpose Sample Stage
14.3.5 PW3075/67 Beam Knife for Positioning Stage

The PW3075/67 Beam Knife can be mounted onto the PW3075/6x Positioning Stage for X-ray diffraction
experiments using the PW3015/x0 X’Celerator or the PW3018/00 PIXcel. The beam knife is shown in Figure
14.10 it can be PreFIX mounted onto the PreFIX U-block on the PW3075/6x Positioning Stage. The alignment
of the beam knife is specific for the sample stage that it is delivered with; it cannot be used with any other
positioning stage.
14.3.6.
07.03.27 Page 14.13

Setting
Screw
Figure 14.10: PW3075/67 Beam Knife for the Positioning Stage

Mounted onto a PW3075/61 Positioning Stage
Page 14.14 07.03.27

14.3.6 Use
The gap between the beam knife and the sample surface should be as small as possible without obstructing the
incident and diffracted X-ray beams. Figure 14.11 shows a graphical representation of the optimum setting of
the beam knife with respect to the sample surface.
In order to calculate the optimum setting the following variables must be calculated:
R
L 1 = ------------------------------------------------------------------
sin ( 2θ – ω )-
---------------------------- + cos ( 2θ – ω )
tan ( δ ⁄ 2 )
P = R sin ( 2θ – ω )
S = R cos ( 2θ – ω )
a
T = ---------------------------------
2 cos ( 2θ – ω )
Figure 14.11: Beam Knife Setting
07.03.27 Page 14.15

The optimum setting of the beam knife above the sample surface is then given by:
( P + T )L 1
h = ------------------------
( L1 + S )
in which h = the optimum height of the beam knife with respect to the diffracted X-ray beam
δ = the divergence angle of the divergence slit used
ω = the angle between the incident beam and the sample surface
2θ−ω = the angle between the diffracted beam and the sample surface
a = the active length of the X’Celerator or the PIXcel (set in the data collector software)
R = the radius of the goniometer
Note that in symmetrical geometries, ω = 2θ/2.
Proceed as follows to set the height of the beam knife above the sample surface:
1. Calculate the optimum height of the beam knife by choosing the maximum values of ω and (2θ − ω) in
the scan.
2. Loosen the black knurled knob on the beam knife and carefully bring the knife to the correct height
above the sample.
3. Tighten the black knurled knob.
The beam knife is now ready for use.
The exact position of the beam knife above the sample is not critical. In most normal situations, a setting of
between 0.5 mm and 1 mm above the minimum calculated height will not significantly influence the results of
the measurement. However, if you are performing a scan with a long 2θ range (for example: for Rietveld
analysis) you must be very careful not to block the X-ray beam.
If you are performing measurements at high 2θ angles, such as in residual stress analysis using the omega-offset
method, we recommend that you completely remove the beam knife from the sample stage.
Page 14.16 07.03.27

Chapter 15
Sample Changers
Contents
15.1 General............................................................................................................................... 15 - 3
15.2 PreFIX Sample Changers ................................................................................................ 15 - 3
15.2.1 PW3065/01 15 Position Sample Changer ............................................................................ 15 - 4
15.2.2 PW3065/12 3 x 15 Position Sample Changer ...................................................................... 15 - 4
15.2.3 Accessories........................................................................................................................... 15 - 5
15.2.3.1 PW3066/01 Sample Magazine............................................................................. 15 - 5
15.2.3.2 PW18xx Circular Sample Holders....................................................................... 15 - 5
15.3 Use ...................................................................................................................................... 15 - 6
15.3.1 Installing the Sample Changer in the Instrument Enclosure ................................................ 15 - 6
15.3.2 Removing the Sample Changer from the Instrument Enclosure.......................................... 15 - 7
15.3.3 Moving the PW3065/xx Sample Changer in Front of the Sample Spinner ......................... 15 - 8
15.3.4 Moving the PW3065/xx Sample Changer to the Parking Position ...................................... 15 - 9
07.03.27 Page 15.1

Page 15.2 07.03.27

Part II - Chapter 15: Sample Changers
15.1 GENERAL
Sample changers are used in X-ray diffraction systems to automatically load and unload samples onto a sample
stage. This makes it possible for the system, even when unattended, to run batches of routine measurements.
Two types of sample changer are available in X’Pert PRO. Both sample changers work with 15 position sample
magazines (for PW18xx sample holders); the PW3065/01 has a mounting position for one magazine, the
PW3065/12 has mounting positions for three magazines. These sample changers and their operation in X’Pert
PRO systems are described in this chapter.
15.2 PREFIX SAMPLE CHANGERS

PreFIX sample changers are constructed to work in combination with the PW3064/x0 Sample Spinner mounted
onto a vertical X’Pert PRO diffractometer. When a sample changer is used together with a Theta-Theta
diffractometer the samples remain horizontal during the entire measurement process.
The sample changers utilize removable magazines, each magazine containing 15 sample positions. There is also
a position available underneath the magazine mounting position for a monitor sample for drift correction
purposes, for instance in quantitative phase analysis.
Sample changers are PreFIX mounted onto the floor of the PW3040/60 Enclosure. When they are not in use they
can be removed from their position in front of the goniometer and shifted to a parking position or removed from
the instrument enclosure. They can be easily returned to the PreFIX measuring position and remounted without
the need for re-alignment when required.
The method of operation is that a sample arm moves into position to pick up the selected sample from the
magazine, lifts and rotates the sample, then the arm moves up to a height to travel over the top of the magazine
and finally moves the sample into position in the sample spinner. These operations are controlled by the data
collector software.
Position for
Monitor Sample
Sample Magazine
Plug for
D-connector
Locating Ring
for Locking
Base Plate
Black Knobs
Knurled Metal
Knob
Figure 15.1: PW3065/01 15 Position Sample Changer
07.03.27 Page 15.3

15.2.1 PW3065/01 15 Position Sample Changer

The PW3065/01 Sample Changer has a mounting position for one 15 position sample magazine and a monitor
sample position just underneath the magazine, it is shown in Figure 15.1. The sample changer can be easily
unlocked from its working position and moved aside to the parking position to allow easy access to the
goniometer for the exchange of sample stages. When the sample changer is needed again, it is unlocked from its
parking position, moved back to its position in front of the goniometer, and locked into place again. Alignment
of the sample changer with respect to the goniometer is not necessary. The procedures for moving the sample
changer to its parking position at the left-hand side of the instrument enclosure and back again are given in
section 15.3.
The sample changer can also be taken out of the enclosure if required. It can be put back into its position in front
of the PW3064/x0 Sample Spinner without the need for alignment. The procedures for removing and placing the
sample changer are given in section 15.3.
15.2.2 PW3065/12 3 x 15 Position Sample Changer

The PW3065/12 Sample Changer is in all respects the same as the PW3065/01 Sample Changer with the
difference that this sample changer has mounting positions for three 15 position sample magazines and three
monitor sample positions underneath the magazines. The sample changer is shown in Figure 15.2.
The sample changer can be easily unlocked from its working position and moved aside to the parking position
to allow easy access to the goniometer for the exchange of sample stages. When the sample changer is needed
again, it is unlocked from its parking position, moved back to its position in front of the goniometer, and locked
into place again. Alignment of the sample changer with respect to the goniometer is not necessary. The
procedures for moving the sample changer to its parking position at the left-hand side of the instrument enclosure
and back again are given in section 15.3.
The sample changer can also be taken out of the enclosure if required. It can be put back into its position in front
of the PW3064/x0 Sample Spinner without the need for alignment. The procedures for removing and placing the
sample changer are given in section 15.3.
Figure 15.2: PW3065/12 3 x 15 Position Sample Changer

Page 15.4 07.03.27
15.2.3 Accessories
15.2.3.1 PW3066/01 Sample Magazine
The PW3066/01 Sample Magazine is delivered with the sample changer (one with the PW3065/01, and three
with the PW3065/12). It can also be ordered as an accessory to be used as a spare magazine.
The PW3066/01 Magazine can accommodate up to 15 PW18xx Circular Sample Holders. The magazine can be
taken out of the sample changer and remotely loaded. There is no requirement to tilt the magazine when loading
it into the sample changer, thus making it suitable for loading/unloading samples that comprise loose powder.

The PW18xx Sample Holders are circular sample holders that can be loaded in the PW3064/x0 Sample Spinner
and the PW3066/01 Sample Magazines. These sample holders can also be mounted in the PW3072/60
Stationary Sample Stage, the PW3074/00 Multi-purpose Sample Stage, or the PW3076/00 Transmission
Spinner, and on the PW3061/21 Sample Holder for Solid Samples to be used with the PW3060/20 MRD Cradle.
A description of the PW18xx Sample Holders and their applications is given in Appendix A of this manual.
Figure 15.3: PW3066/01 15 Position Sample Magazine
07.03.27 Page 15.5

15.3 USE
The PW3065/xx Sample Changer can be taken out of the enclosure if required. It can be put back into its position
in front of the PW3064/x0 Sample Spinner without additional alignment. These operations are described in
sections 15.3.1 and 15.3.2.
The PW3065/xx Sample Changer can also be moved from the parking position to the working position and back
without the need for additional alignment. The procedures for these operations are given in sections 15.3.3 and
15.3.4.
15.3.1 Installing the Sample Changer in the Instrument Enclosure

Proceed as follows to install the PW3065/xx Sample Changer in the instrument enclosure:
1. If it is not already mounted, mount the PW3064/x0 Sample Spinner making use of the X’Pert wizard
“Exchange Sample Stages”. Refer to section 12.1.1 of Chapter 12 in Part II of this User’s Guide for
more details about changing PreFIX sample stages.
2. Switch the system off according to the procedure given in Chapter 4 in Part I of this User’s Guide.
3. Place the sample changer over the base plate (shown in Figure 15.1 and Figure 15.2) in front of the
goniometer, so that it is symmetrical with respect to the goniometer.
4. Plug the large (37-pin) D-connector end of the spinner/changer cable into the sample changer.
5. If it is present, remove the fixing screw (indicated in Figure 15.4) that fixes the sample changer arm to
the reset position.
Figure 15.4: Location of Fixing Screw on Sample Changer Arm in Reset Position
6. Rotate the black knobs (indicated in Figure 15.5) to let the alignment pins click into place (the
alignment pins determine the position of the sample changer in the enclosure). Try to move the sample
changer slightly to ensure that both of the pins have clicked into place.
Page 15.6 07.03.27

Black Knobs
Base Plate
Knurled Metal
Knob
Figure 15.5: Location of the Sample Changer Locking and Locating knobs
7. Use the two knurled metal knobs to fix the sample changer to the enclosure. One of the two knurled
metal knobs is indicated on Figure 15.5, the other knurled metal knob can be seen from the left-hand
side of the sample changer.
8. Place the sample magazine(s) on the sample changer.
9. Switch the system on according to the procedure given in Chapter 4 in Part I of this User’s Guide, and
use the data collector software to go on-line with a configuration that includes a sample changer.
15.3.2 Removing the Sample Changer from the Instrument Enclosure

In some situations, for instance: when you want to work with a non-ambient chamber with vacuum equipment,
you may need to create space in front of the goniometer. Removing the sample changer is then a useful option.
In order to remove a PW3065/xx Sample Changer from its position in front of the goniometer and take it out of
the enclosure, proceed as follows:
1. Check to see if the sample spinner still contains a sample. If it does, use the data collector software to
unload the sample.
2. Use the data collector software to reset the sample changer, this will send the sample changer to a safe
(reset) position.
3. If necessary, remove any PreFIX modules that may restrict your easy access to the sample changer.
4. Switch the system off according to the procedure given in Chapter 4 in Part I of this User’s Guide.
5. Remove the sample magazine(s) from the sample changer.
6. Fix the sample changer arm to its reset position using a (M5 x 20) screw (see Figure 15.4).
7. Undo the two knurled metal knobs located on the base plate of the sample changer. You can see one of
these knobs from the right-hand side of the sample changer (see Figure 15.5), and the other from the
left.
8. Lift the two black knobs (see Figure 15.5) and rotate them by about 90º to lock the alignment pins up.
These knobs can be found on the right-hand side of the sample changer base plate. The sample changer
can now be moved.
07.03.27 Page 15.7

9. Unplug the large (37-pin) D-connector end of the spinner/changer cable from the sample changer.
10. Lift the sample changer out of the enclosure and store it in a safe place. The sample changer is mounted
on roller balls, therefore make sure that it cannot roll off any surface that you put it on, for instance: a
table. You can if required, lay the sample changer on its side.
11. Switch the system on according to the procedure given in Chapter 4 in Part I of this User’s Guide, and
use the data collector software to go on-line with a configuration that does not include a sample
changer.
15.3.3 Moving the PW3065/xx Sample Changer in Front of the Sample

Spinner
The PW3065/xx Sample Changer can be located on a parking position inside the instrument enclosure. This
procedure tells you how to move the sample changer from the parking position into its position in front of the
PW3064/x0 Sample Spinner.
1. If it is not already mounted, mount the PW3064/x0 Sample Spinner. Refer to section 12.1.1 of Chapter
12 in Part II of this User’s Guide for more details about changing PreFIX sample stages.
2. Lift the two black knobs (see Figure 15.5) and rotate them by about 90º to lock the alignment pins up.
The black knob nearest you is used to secure the sample changer in its parking position by locking the
alignment pin into place in the locating/locking ring on the instrument enclosure floor.
3. Roll the sample changer to the operating position in front of the goniometer (see Figure 15.1).
4. Place the sample changer so that it is symmetrical with respect to the goniometer.
5. Rotate the black knobs as indicated in Figure 15.5 to let the alignment pins click into place (the
alignment pins determine the position of the sample changer in the enclosure). Try to move the sample
changer slightly to ensure that both of the pins have clicked into place.
6. Use the two knurled metal knobs (see Figure 15.5) to fix the changer to the enclosure.
7. If it is present, remove the screw that fixes the sample changer arm to the reset position (see Figure
15.4).
8. Place a sample magazine on the sample changer.
9. Use the data collector software to go on-line with a configuration that includes a sample changer.
The sample changer is now ready for operation.
Page 15.8 07.03.27

15.3.4 Moving the PW3065/xx Sample Changer to the Parking Position

The PW3065/xx Sample Changer can be moved to a parking position inside the instrument enclosure. This
procedure tells you how to move the sample changer from its position in front of the PW3064/x0 Sample Spinner
to its parking position.
1. Check to see if the sample spinner still contains a sample. If it does, use the data collector software to
unload the sample.
2. Use the data collector software to reset the sample changer, this will send the sample changer to a safe
(reset) position.
3. If necessary, remove any PreFIX modules that may restrict your easy access to the sample changer.
4. Remove the sample magazine from the sample changer.
5. Fix the sample changer arm to its reset position using a (M5 x 20) screw. This screw is indicated in
Figure 15.4.
6. Undo the two knurled metal knobs located on the base plate of the sample changer. You can see one of
these knobs from the right-hand side of the sample changer (see Figure 15.5), and the other from the
left.
7. Lift the two black knobs (indicated in Figure 15.5) and rotate them by about 90º to lock the alignment
pins up. These knobs can be found on the right-hand side of the sample changer base plate. The sample
changer can now be moved.
8. Roll the sample changer to its parking position in the instrument enclosure. For single diffraction
systems this position is normally in the left-hand corner of the enclosure (see Figure 15.6).
a. If you have a PW3065/01 Sample Changer, rotate the sample changer 90º and move it to the left so
that the long edge of its base plate is touching the front wall of the enclosure and the sample
magazine is towards you.
b. If you have a PW3065/12 Sample Changer, move it to the left so that the long edge is touching the
front wall of the enclosure.
You can now secure the sample changer in this position using the black knob nearest to you, allowing
the alignment pin to lock into place into the locating/locking ring on the instrument enclosure floor, as
indicated in Figure 15.1.
07.03.27 Page 15.9

Base Plate
Figure 15.6: PW3065/01 15 Position Sample Changer in its Parking Position

Now you can use the sample spinner without the sample changer, or exchange it for another sample stage.
Exchanging sample stages is described in section 12.1.1 of Chapter 12 in Part II of this User’s Guide.
Page 15.10 07.03.27

Chapter 16
Diffracted Beam Slits
Contents
16.1 General............................................................................................................................... 16 - 3
16.2 Anti-scatter Slits................................................................................................................ 16 - 3
16.2.1 Applications.......................................................................................................................... 16 - 3
16.2.1.1 Phase Analysis and Omega-stress Analysis......................................................... 16 - 3
16.2.1.2 Reflectivity and Thin-film Phase Analysis .......................................................... 16 - 3
16.2.2 PW3091/x0 Programmable Anti-scatter Slit........................................................................ 16 - 4
16.2.2.1 Accessories .......................................................................................................... 16 - 5
16.2.2.2 Using Programmable Anti-scatter Slits ............................................................... 16 - 7
16.2.3 PW3092/00 Fixed Anti-scatter Slit Assembly ..................................................................... 16 - 9
16.2.3.1 Accessories .......................................................................................................... 16 - 9
16.2.3.2 Using Fixed Anti-scatter Slits.............................................................................. 16 - 9
16.3 Receiving Slits ................................................................................................................. 16 - 10
16.3.1 Applications........................................................................................................................ 16 - 10
16.3.1.1 Phase Analysis and Omega-stress Analysis....................................................... 16 - 10
16.3.1.2 Thin-film Phase Analysis and Reflectivity ........................................................ 16 - 10
16.3.1.3 Phase Analysis on Loosely Prepared Powder Samples ..................................... 16 - 10
16.3.1.4 Texture and Psi-stress Analysis ......................................................................... 16 - 11
16.3.2 PW3093/60 Programmable Receiving Slit......................................................................... 16 - 11
16.3.2.1 Accessories ........................................................................................................ 16 - 12
16.3.2.2 Using Programmable Receiving Slits ................................................................ 16 - 18
16.4 High Resolution Diffracted Beam Optics ..................................................................... 16 - 19
16.4.1 PW3097/60 Rocking Curve Attachment............................................................................ 16 - 19
16.4.1.1 Accessories ........................................................................................................ 16 - 20
16.4.1.2 Use ..................................................................................................................... 16 - 22
16.4.2 PW3120/60 Triple Axis and Rocking Curve Attachment.................................................. 16 - 23
16.4.3 PW3120/65 Asymmetrical Triple Axis and Rocking Curve Attachment .......................... 16 - 25
07.03.27 Page 16.1

Page 16.2 07.03.27

Part II - Chapter 16: Diffracted Beam Slits
16.1 GENERAL
Slits used in the diffracted beam path of X’Pert PRO systems can be divided into three groups:
• Anti-scatter slits
Anti-scatter slits are fitted in the diffracted beam path to control the acceptance in the equatorial plane
of the X-ray beam received by the detector. These slits also reduce the level of background radiation
due to scatter. Alternatively, anti-scatter slits can be used in combination with a receiving slit to form a
“beam tunnel” for parallel beam applications. The anti-scatter slits are described in section 16.2.
Anti-scatter slits devices in combination with the X’Celerator or PIXcel detector are described in
• Receiving slits
Receiving slits are placed in the diffracted beam path on the diffractometer circle; for para-focusing
applications this position forms the natural focusing point of the diffracted X-ray beam. In these
applications the receiving slits define the resolution of the measurements.
As described above, the receiving slit can be used in combination with an anti-scatter slit to form a
“beam tunnel” for parallel beam applications. The receiving slits are described in section 16.3.
• Receiving slits for high resolution diffraction
In high resolution rocking curve measurements the resolution is determined by the incident beam high-
resolution monochromator and the sample. In these applications the receiving slit is used to reduce the
background radiation or to reduce the acceptance of the detector in the 2θ direction. High resolution
receiving optics are described in section 16.4.
16.2 ANTI-SCATTER SLITS

Anti-scatter slits are fitted into the diffracted beam path to control the amount of the diffracted X-ray beam (in
the equatorial plane) that is accepted by the detector. Related to this, the anti-scatter slit defines the length of the
sample that is “seen” by the receiving slit. Another function is to block the scattered radiation and therefore
reduce the level of background radiation.
In the parallel beam geometry, the combination of an anti-scatter slit and a receiving slit can be used as an
alternative to the parallel plate collimator. The opening of the anti-scatter slit must then be set equal to that of
the receiving slit to create a “beam tunnel”.
Two types of anti-scatter slit are available on X’Pert PRO systems, they are: Programmable Anti-Scatter Slits
(PASS) and Fixed Anti-Scatter Slits (FASS).
16.2.1 Applications
Typical applications in which anti-scatter slits are used are: phase analysis, omega-stress analysis, reflectivity
and thin-film phase analysis.
16.2.1.1 Phase Analysis and Omega-stress Analysis

In Bragg-Brentano geometry for phase analysis, anti-scatter slits are used to control the acceptance of the
diffracted X-ray beam. The size of the anti-scatter slit is chosen to equal the size of the divergence slit in the
incident beam path. Omega-stress analysis uses the same optical configuration; however, here the sample is
inclined in the equatorial plane.
16.2.1.2 Reflectivity and Thin-film Phase Analysis

An anti-scatter slit used together with a receiving slit (both must have the same aperture) forms a “beam tunnel”.
This beam tunnel can be used in quasi-parallel beam applications like reflectivity and thin-film phase analysis.
07.03.27 Page 16.3

16.2.2 PW3091/x0 Programmable Anti-scatter Slit

PW3091/x0 is a diffracted beam optical module with a programmable anti-scatter slit.
The programmable anti-scatter slit is shown in Figure 16.1.
Holes for the Automatic Beam

Interface Attenuator Mounting Screws
Mounting Screws
Holes for
Mounting Screws
Mounting
Interface
Adjustment
Screw
Figure 16.1: PW3091/60 Programmable Anti-scatter Slit

Two types of programmable anti-scatter slit exist:
• PW3091/60 can be used in combination with the PW3093/60 Programmable Receiving Slit, and on
X'Pert PRO MPD systems also with the PW3015/x0 X'Celerator.
• PW3091/70 can be used in combination with the PW3093/60 Programmable Receiving Slit, and on
X'Pert PRO MPD systems also with the PW3015/x0 X'Celerator and the PW3018/00 PIXcel detector.
If required, the programmable anti-scatter slit can be mounted onto or dismounted from the programmable
receiving slit or the detector interface. Mounting instructions are given in section: 16.3.2.1.5.
The distance between the anti-scatter slit and the receiving slit is 63 mm.
Alternatively, the programmable anti-scatter slit can be used in combination with the X’Celerator or the PIXcel
and the PW3094/40 Interface on X’Pert PRO MPD systems. Mounting instructions for this are given in sections
21.4.3.5.1 and 21.5.3.5.1 in Chapter 21 of this User’s Guide.
The distance between the anti-scatter slit and the X’Celerator detector or the PIXcel is 109 mm.
The programmable anti-scatter slit is software controlled to operate in one of three modes:
• The fixed anti scatter slit mode, to provide a defined acceptance of 4°, 2°, 1°, 1/2°, 1/4°, 1/8°, 1/16°, and
1/32°.
• The automatic mode, to provide a defined observed length on the sample of 0.5 to 20 mm in 0.1 mm
steps, with the acceptance changing automatically as a function of the angle between the diffracted beam
and the sample surface (2θ - ω).
The observed area can also be offset from the goniometer axis in order to asymmetrically select the area
on the sample to be observed. The offset distance can be applied using the data collector software.
• The beam tunnel mode, with the aperture of the programmable anti-scatter slit set at the same value as
the receiving slit height, or the active length of the X’Celerator or the PIXcel in receiving slit mode; this
yields an appropriate optical path for quasi-parallel beam applications.
More information about using programmable anti-scatter slits is given in section 16.2.2.2.
Page 16.4 07.03.27


The PW3087/6x Automatic Beam Attenuator can be mounted on the front of the programmable anti-scatter slit.
The attenuation factor shown on the Acceptance Test Form is entered in the data collector software and is used
to automatically adjust the measured intensity values.
The automatic beam attenuator window size is 25 mm in the axial direction and 6 mm in the equatorial plane.
When you use the automatic beam attenuator together with the programmable anti-scatter slit you must ensure
that the diffracted beam is not obstructed by the beam attenuator.
CAUTION The maximum 2θ angle of the diffracted beam arm is limited when
an automatic beam attenuator is mounted. Use the data collector
software to set a lower maximum value of 2θ in order to avoid
collision between the X-ray tube shield and the automatic beam
attenuator
When you use a maximum acceptance angle setting of 2º on the programmable anti-scatter slit, you can use the
full range of aperture settings on the programmable receiving slit of 0.01 mm to 3.0 mm.
16.2.2.1.1.1 Mounting the Automatic Beam Attenuator onto a PASS
Proceed as follows to mount the automatic beam attenuator onto the programmable anti-scatter slit:
1. Remove the three screws marked A in Figure 2.2 (in Chapter 2 of Part II of this User’s Guide).
3. Place the brass fill plate onto the programmable anti-scatter slit and fit the metal part (NOT the side
with the alignment pins) of the automatic beam attenuator onto the programmable anti-scatter slit;
using the four screws supplied with the automatic beam attenuator into the four holes on the front of the
PASS and secure it into place. Ensure that the automatic beam attenuator is correctly orientated.
07.03.27 Page 16.5

Figure 16.2: PW3087/6x Automatic Beam Attenuator Mounted

onto a Programmable Anti-scatter Slit
16.2.2.1.2 PW3094/40 Interface PASS to X’Celerator or PIXcel

The PW3094/40 is an interface enabling the PW3091/x0 Programmable Anti-scatter Slit to be mounted onto the
X’Celerator detector or the PIXcel detector for use on an X’Pert PRO MPD system. It is shown in Figure 16.3.
When the programmable anti-scatter slit is used in combination with the X’Celerator or the PIXcel detector it
controls the detector’s acceptance and reduces the level of background radiation due to scatter.
Instructions for mounting the programmable anti-scatter slit onto the X’Celerator or the PIXcel using the
PW3094/40 Interface are given respectively in sections 21.4.3.5.1 and 21.5.3.6.1 of Chapter 21 in Part II of this
User’s Guide.
Information about using the programmable anti-scatter slit in combination with the X’Celerator or the PIXcel is
Page 16.6 07.03.27

Figure 16.3: PW3091/x0 Programmable Anti-scatter Slit Mounted onto the X’Celerator with a
PW3094/40 Interface
16.2.2.2 Using Programmable Anti-scatter Slits

This section describes the operating modes and the determination of the observed area as a function of the
sample position and the size of the acceptance angle.
16.2.2.2.1 Operating Modes

The programmable anti-scatter slit can be programmed using the data collector software to operate in three
modes: fixed, automatic or follow (beam tunnel). These modes are described in Table 16.1.
NOTES: When the programmable anti-scatter slit is used in fixed mode, optimal results for goniometer
(2θ - θ) scans are attainable when the size of the fixed anti-scatter slit matches that of the
programmable divergence slit, used in fixed mode. In this case the aperture of the receiving slit
must not be larger than 0.3 mm. For other scan types you should take care that the observed length
does not become smaller than the irradiated length.
When the programmable anti-scatter slit is used in automatic mode, optimal results for goniometer
(2θ - θ) scans are attainable when the size of the automatic anti-scatter slit matches that of the
automatic divergence slit, except for reflectivity measurements.
07.03.27 Page 16.7

Table 16.1: PASS Operating Modes and their Applications
Mode Size Application
4º, 2º, 1º, 1/2º, 1/4º, 1/8º, 1/ The size of the acceptance slit can be set to one of these fixed
Fixed 16º, 1/32º values. We advise you to use the same setting as is used for the
programmable divergence slit, set in the fixed mode.
0.5 to 20 mm in steps of 0.5 The observed length of the sample can be defined.
mm Depending on the measured (2θ - ω) angle the acceptance is
Automatic automatically changed to ensure that the observed length of the
sample remains constant over full measured angular range.
Offset: When the programmable anti-scatter slit is used in the automatic

0 to minimum value of: mode, the observed length on the sample can be offset by
(observed length/2) and defining an offset in the data collector software. When the
((20 - obsd. length)/2) mm offset is set to 0 mm (standard), the sample is observed
in steps of 0.25 mm. asymmetrically with respect to the goniometer axis. When a
The offset can be set either negative offset is given, the observed area on the sample is
positive or negative moved towards the X-ray tube; entering a positive offset value
moves the irradiated area towards the detector. You should set
the offset value for the programmable anti-scatter slit to the
same value as that used for the programmable divergence slit in
the incident beam path.
Match PRS size: In combination with programmable receiving slit, the anti-scatter
0.01 to 3.0 mm in steps of slit size will follow the receiving slit height appropriate for quasi-
Follow 0.01 mm parallel beam applications, for instance: reflectivity.
(Beam
Tunnel) Match X’Celerator or PIXcel: In combination with X’Celerator or PIXcel in receiving slit mode,
0.01 to 3.0 mm in steps of the detector’s active length is matched.
0.01 mm
16.2.2.2.2 Determination of the Observed Length in the Fixed Anti-scatter Mode

The length of the observed area on the sample is dependent on the acceptance angle of the diffracted beam as
seen by the detector and the position of the sample with respect to the beam. In the automatic anti-scatter slit
mode the observed length of the sample is fixed; the acceptance angle is automatically changed as the (2θ - ω)
angle changes. In the fixed anti-scatter slit mode the observed length is a function of the anti-scatter slit angle
set in the data collector software. It can be calculated as follows:
R sin δ sin ( 2θ – ω )
L = --------------------------------------------------------------
sin2 ( 2θ – ω ) – sin2 ( δ ⁄ 2 )
where L = observed length on the sample,

δ = acceptance angle of the programmable anti-scatter slit,
2θ -ω = angle between diffracted beam and sample surface.
Page 16.8 07.03.27

16.2.3 PW3092/00 Fixed Anti-scatter Slit Assembly

The PW3092/00 Fixed Anti-Scatter Slit assembly (FASS) consists of a holder for exchangeable fixed anti-
scatter slits as shown in Figure 16.4.
Figure 16.4: PW3092/00 Fixed Anti-scatter Slit Assembly

The fixed anti-scatter slit holder is fitted onto the PW3093/60 Programmable Receiving Slit (see 16.3.2), the slits
can be inserted into the holder to provide a defined diffracted beam acceptance angle as “seen” by the detector.
Fixed anti-scatter slits used in combination with the X’Celerator or the PIXcel are described in Chapter 20 in
Fixed anti-scatter slits come in two size ranges:
4º, 2º, 1º, 1/2º, and 1/4º used for standard applications
1/8º, 1/16º and 1/32º used for measurements where there is a small angle between the sample sur-
face and the diffracted beam
The distance between the anti-scatter slit and the receiving slit is 34 mm.
NOTE: The actual acceptance angle as set by the fixed anti-scatter slits is 2.58 times the size (marking) on
the slits.
16.2.3.1.1 Fixed Anti-scatter Slits
Five anti-scatter slits marked 4°, 2°, 1º, 1/2° and 1/4° are supplied together with the PW3092/00 Fixed Anti-
scatter Slit Assembly. These slits are used to control the acceptance of the diffracted beam by the detector, and
thus the observed length on the sample. The fixed anti-scatter slits must be inserted into the slot in the fixed anti-
scatter slit assembly.
16.2.3.1.2 PW3083/00 Fixed Slits for Low Angle Measurements

PW3083/00 is a set of fixed slits for low angle measurements, as in thin-film phase analysis or reflectivity
applications. It consists of three slits marked: 1/8º, 1/16º and 1/32º. These slits must be inserted into the slot on
the fixed anti-scatter slit assembly.
16.2.3.2 Using Fixed Anti-scatter Slits

16.2.3.2.1 Selecting the Slit Size
Optimal results for goniometer (2θ - θ) scans are attainable when the size of the fixed anti-scatter slit matches
that of the fixed divergence slit. In this case the aperture of the receiving slit must not be larger than 0.3 mm. For
other scan types you should take care that the observed length does not become smaller than the irradiated
length.
07.03.27 Page 16.9
16.2.3.2.2 Determination of the Observed Length

This section describes the operating modes and the determination of the observed area as a function of the sample
position and the size of the acceptance angle.
The length of the observed length on the sample is dependent on the acceptance angle of the diffracted beam as
seen by the detector and the position of the sample with respect to the beam. The observed length can be
calculated as follows:
R sin ( A × δ ) sin ( 2θ – ω ) -
L = ----------------------------------------------------------------------------
sin2 ( 2θ – ω ) – sin2 ( ( A × δ ) ⁄ 2 )
where A = a correction factor with a value of 2.58,

L = observed length on the sample,
δ = acceptance angle as engraved on the fixed anti-scatter slit used,
2θ - ω = angle between diffracted beam and sample surface.
16.3 RECEIVING SLITS

In Bragg-Brentano geometry the incident X-ray beam diverges from the tube focus until it irradiates the sample.
The diffracted X-ray beam converges from the sample until it reaches its natural focusing point.
Receiving slits are fitted on the diffractometer circle at the focal point of the diffracted beam to control the
resolution of the measurement.
In the parallel beam geometry, receiving slits can be used in combination with an anti-scatter slit to form a “beam
tunnel”. The opening of the anti-scatter slit must then be set equal to that of the receiving slit. This beam tunnel
is an alternative to the use of a parallel plate collimator in the diffracted beam path.
16.3.1 Applications
Receiving slits are commonly used in phase analysis, omega-stress, thin-film phase analysis with the line focus
of the X-ray tube; and in texture and psi-stress analysis with the point focus of the X-ray tube.

In Bragg-Brentano geometry, receiving slits are placed in the focusing point of the diffracted X-ray beam. The
opening of the slit determines the accuracy of the measurement. The receiving slit is used in combination with
an anti-scatter slit. Omega-stress analysis uses the same optical configuration, during the measurement the
sample is inclined in the equatorial plane.
16.3.1.2 Thin-film Phase Analysis and Reflectivity

A receiving slit in combination with an anti-scatter slit set with equal apertures forms a “beam tunnel”. This beam
tunnel can be used in quasi-parallel beam geometries to replace a parallel plate collimator.
16.3.1.3 Phase Analysis on Loosely Prepared Powder Samples

The receiving slit can be used in combination with an X-ray mirror on the diffracted beam side, and an X-ray
mirror (or hybrid monochromator) as the incident beam module. This configuration is called the mirror - mirror
(or hybrid monochromator - mirror) geometry. It is especially suited for measurements on loosely prepared
powder samples. The parallel beam geometry ensures that the peak positions are insensitive to sample height
misalignment and sample surface roughness.
Page 16.10 07.03.27

16.3.1.4 Texture and Psi-stress Analysis

The receiving slit is used in combination with the point focus of the X-ray tube in the Schulz geometry for texture
analysis, as well as in psi-stress analysis where the sample is inclined around the psi axis.
16.3.2 PW3093/60 Programmable Receiving Slit

The PW3093/60 PreFIX Programmable Receiving Slit consists of a receiving slit unit as shown in Figure 16.5
which is fitted onto the diffracted beam arm. It includes:
• a slot for a beta-filter or attenuation foil
• a slot for diffracted beam Soller slits or a diffracted beam mask holder.
Figure 16.5: PW3093/60 Programmable Receiving Slit with PW3011/20 Proportional Detector
Mounted
It is possible to mount a fixed or programmable anti-scatter slit on the sample side of the programmable
receiving slit. A detector (or a curved crystal monochromator with detector) is mounted on the detector side of
the programmable receiving slit.
The programmable receiving slit is software controlled to provide a defined receiving slit height which can be
varied between 0.01 mm and 3.0 mm in steps of 0.01 mm.
07.03.27 Page 16.11

16.3.2.1.1 Beta-filters
There are four beta-filters that can be used with the programmable receiving slit, they are:
Zr filter (part of set PW3151/00) for Mo Kα radiation.
16.3.2.1.2 Attenuation Foil

A 0.1 mm and a 0.2 mm copper foil are delivered with the X’Pert PRO diffraction system. This foil can be
can be damaged by higher count rates. Please refer to Chapter 21 in Part II of this User’s Guide for more
information about the detectors used in X’Pert PRO.

beta-filter slot on the programmable receiving slit in order to
attenuate the beam whenever the measured intensity is expected
to exceed maximum count rate of the detector used.

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
on the attenuation foil itself and on the Acceptance Test Form for the system, which is supplied when the system
is delivered. This value can be entered in the data collector software and is used to automatically adjust the
measured intensity values. For more information about the use of a copper attenuation foil refer to Chapter 2
(section 2.2) in Part II of this User’s Guide.

Soller slits are used together with the programmable receiving slit to control the axial acceptance of the X-ray
beam by the detector. The slot for the Soller slits is shown in Figure 16.5.
Four Soller slits are available, their sizes are:
Soller slits are mounted into the slot for Soller slits on the PreFIX module as shown in Figure 16.5. Insert the
Soller slits into the slot until it clicks into place.
Page 16.12 07.03.27

16.3.2.1.4 X-ray Mirrors

An X-ray mirror can be used in combination with a programmable receiving slit in the diffracted beam path. The
PW3088/6x X-ray Mirror is used in X’Pert PRO MRD systems and the PW3148/6x X-ray Mirror is used in
X’Pert PRO MPD systems. The combination of an X-ray mirror and a programmable receiving slit acts as an
analyzer module with a variable resolution in the parallel beam geometry. An X-ray mirror or a hybrid
monochromator (for pure Kα1 radiation) is used at the incident beam PreFIX position.
In order to mount an X-ray mirror in the diffracted beam path you must have a PW3099/60 PreFIX Interface for
Diffracted Beam X-ray Mirror. Mounting instructions can be found in section 16.3.2.1.4.1. When you have
mounted the mirror you must then inform the data collector software of the diffracted beam X-ray mirror’s
2theta offset; measuring this offset is described in section 16.3.2.1.4.2.
Figure 16.6: X-ray Mirror Mounted onto a PW3099/60 PreFIX Interface

in the Diffracted Beam Path
16.3.2.1.4.1 Mounting the X-ray Mirror in the Diffracted Beam Path
Proceed as follows to mount an X-ray mirror and a programmable receiving slit at the diffracted beam PreFIX
position:
1. If there is a diffracted beam PreFIX module present on the 2theta arm of the goniometer, remove it.
2. Mount the PW3099/60 PreFIX Interface for Diffracted Beam X-ray Mirror at the diffracted beam
PreFIX position (refer to Figure 16.6).
3. If present, remove the programmable or fixed anti-scatter slit from the programmable receiving slit.
07.03.27 Page 16.13

4. Mount the X-ray mirror on the diffracted beam PreFIX position with its divergence slit nearest the
detector.
5. Mount the programmable receiving slit on the PreFIX position furthest away from the goniometer axis.
A diffracted beam monochromator is not required.
6. You can now insert a Soller slits assembly into the Soller slits holder on the X-ray mirror.
7. Use a 1/2º divergence slit at the divergence slit position of the X-ray mirror module.
8. Report the X-ray mirror and the programmable receiving slit to the data collector software and enter the
diffracted beam mirror 2theta offset.
16.3.2.1.4.2 Measuring the Diffracted Beam X-ray Mirror’s 2Theta Offset
When you mount an X-ray mirror at the diffracted beam PreFIX position you have to introduce its 2theta offset
into the data collector software. This section describes how you measure that offset.
1. Install the incident beam PreFIX module that you are going to use in the next measurements (an X-ray
mirror or a hybrid monochromator) in the mirror-mirror geometry. Report the incident beam module to
the data collector software.
2. Insert an attenuation foil into the incident beam PreFIX module:
if you are using Cu radiation: the combined copper/nickel attenuation foil,
if you are using Co radiation: the 0.2 mm iron attenuation foil.
3. Mount the PW3093/60 Programmable Receiving Slit onto the diffracted beam PreFIX position and
report this to the data collector software.
4. Set ω = 0º and make sure that the direct X-ray beam is not obstructed by the sample or the sample stage.
5. Make a 2θ scan around 2θ = 0º to find the peak position of the direct X-ray beam. Note this position as
2θA.
6. Mount the diffracted beam X-ray mirror and the programmable receiving slit in the diffracted beam
path as described in section 16.3.2.1.4.1. Note that you DO NOT report this to the data collector
software.
7. Make a 2θ scan over a range of 5º around 2θ = 0º to find the peak position of the direct X-ray beam now
that you have the mirror-mirror geometry. Note this position as 2θB.
8. The offset is calculated by subtracting 2θA from 2θB (2θB - 2θA).
9. Enter the reverse of the offset value into the data collector software, so that the 2theta axis is
automatically offset when you select the X-ray mirror together with the programmable receiving slit as
diffracted beam PreFIX modules. This means, for example: if your calculation of the offset results in
-1.1º you actually enter 1.1º, whereas if your calculation resulted in +1.1º you enter -1.1º.
16.3.2.1.5 PW3091/x0 Programmable Anti-scatter Slit

A PW3091/x0 Programmable Anti-scatter Slit can be mounted on the front of the programmable receiving slit
as advised in Bragg-Brentano geometry or the quasi-parallel beam geometry. Proceed as follows to mount the
programmable anti-scatter slit:
1. In the data collector software, include the PRS PreFIX module with PASS in the configuration that you
currently have open.
2. If necessary, mount the PASS onto its interface using the interface mounting screws as shown in Figure
16.1.
3. Make sure to switch the system off according to the procedure described in Chapter 4 in Part I of this
User’s Guide before connecting or disconnecting cables. Close the data collector software.
4. Position the programmable anti-scatter slit so that the four holes on the interface line up with the four
holes on the programmable receiving slit as is shown in Figure 16.5.
Page 16.14 07.03.27

CAUTION
Do not turn the adjustment screw (shown in Figure 16.1) as it is
ONLY to be used for module alignment.
5. Secure the programmable anti-scatter slit with four screws supplied.

6. Switch the system on according to the procedure described in Chapter 4 in Part I of this User’s Guide.
Open the data collector and go on-line (Connect) with the configuration that you were using before you
switched the system off.
Figure 16.7: PW3091/x0 Programmable Anti-scatter Slit Mounted onto a Programmable Receiving
Slit with Curved Crystal Monochromator and Proportional Detector
16.3.2.1.6 PW3092/00 Fixed Anti-scatter Slit Assembly

A PW3092/00 Fixed Anti-scatter Slit Assembly can be mounted on the front of the programmable receiving slit
as advised in Bragg-Brentano geometry. Proceed as follows to mount the fixed anti-scatter slit:
1. Position the fixed anti-scatter slit so that the four holes on the interface line up with the four holes on
the programmable receiving slit.
2. Secure the fixed anti-scatter slit with four screws supplied.
07.03.27 Page 16.15

CAUTION
Do not turn the adjustment screw (shown in Figure 16.4) as it is
Figure 16.8: PW3092/00 Fixed Anti-scatter Slit Mounted onto a

Programmable Receiving Slit
Page 16.16 07.03.27

16.3.2.1.7 PW3094/20 Diffracted Beam Mask Set

Diffracted beam masks can be inserted into the programmable receiving slit module to control the width of the
diffracted beam accepted by the detector. The diffracted beam mask set comprises a beam mask holder and two
metal strips with beam mask apertures marked 20, 10, 4 and 2 mm.
Mount the beam masks as follows:
1. If a Soller slits assembly is mounted, remove it.
2. Insert the beam mask holder into the slot with the mask slot facing the detector until it clicks into place.
3. Insert the required mask into the slot in the beam mask holder.
16.3.2.1.8 PW3121/00 Flat Crystal Monochromator

A PW3121/00 Flat Crystal Monochromator can be added to the programmable receiving slit when it is used in
the beam tunnel mode in combination with an anti-scatter slit.
16.3.2.1.8.1 Mounting a Flat Crystal Monochromator
CAUTION
Do not turn the alignment screw (indicated in Figure 19.1) as it is
Mount the diffracted beam flat crystal monochromator onto the programmable receiving slit as follows:
1. Remove the detector from the PW3093/60 Programmable Receiving Slit by sliding it out of the
detector interface and place it carefully to one side.
2. Undo the two screws that secure the detector interface and remove the interface.
3. Hold the flat crystal monochromator in place and carefully align the holes on the monochromator with
the screw holes where you removed the screws in step 2. Insert two screws into the holes you just lined
up and tighten them.
4. Re-mount the detector onto the detector interface on the flat crystal monochromator.
Aligning the flat crystal monochromator is described in Chapter 19 (section 19.2.1.2.1) of Part II of this User’s
Guide.
16.3.2.1.9 PW312x/10 Curved Crystal Monochromators

Curved crystal monochromators are used together with programmable receiving slits in focusing geometries.
The X-ray tube’s characteristic wavelength determines which monochromator has to be used. Curved crystal
monochromators are described in Chapter 19 in Part II of this User’s Guide.
The curved crystal monochromator mounted onto a programmable receiving slit is shown in Figure 16.7.
16.3.2.1.9.1 Mounting a Curved Crystal Monochromator
CAUTION
Do not turn the alignment screw (indicated in Figure 19.4) as it is
Mount the diffracted beam curved crystal monochromator onto the programmable receiving slit as follows:
07.03.27 Page 16.17

1. Remove the detector from the PW3093/60 Programmable Receiving Slit by sliding it out of the detector
interface and place it carefully to one side.
2. Undo the two screws that secure the detector interface and remove the interface.
3. Hold the curved crystal monochromator in place and carefully align the holes on the monochromator
with the screw holes where you removed the screws in step 2. Insert two screws into the holes you just
lined up and tighten them.
4. Re-mount the detector onto the detector interface on the curved crystal monochromator.
No further alignment is required.
16.3.2.1.10 PW3011/20 Proportional Detector

A PW3011/20 Proportional Detector can be mounted behind the programmable receiving slit in the detector
interface which holds the detector in place by means of two spring-loaded balls. To mount the detector, slide it
into the interface until it clicks into position. A detector mounted onto a programmable receiving slit is shown
in Figure 16.5.
If a diffracted beam monochromator is mounted, the detector is then fitted into the detector interface on the
monochromator. This is shown in Figure 16.7.
16.3.2.1.11 PW1964/96 Scintillation Detector

A PW1964/96 Scintillation Detector can be mounted behind the programmable receiving slit in the detector
interface which holds the detector in place by means of two spring-loaded balls. To mount the detector, slide it
into the interface until it clicks into position.
monochromator.
16.3.2.1.12 PW3018/00 PIXcel Detector

A PW3018/00 PIXcel detector, equipped with a PW3017/60 Interface, can be mounted behind the programmable
receiving slit in the detector interface which holds the detector in place by means of two spring-loaded balls. To
mount the detector, slide it into the interface until it clicks into position.
16.3.2.2 Using Programmable Receiving Slits

In order to obtain an optimum resolution, the size of the receiving slit in the Bragg-Brentano geometry should
be as large as (or slightly larger than) the height of the diffracted beam at the receiving slit position. Using a
smaller slit size will have no (or very little) effect on the resolution, whereas the intensity of the measured peak
decreases proportionally to the reduction in slit size. Using a larger slit will cause a deterioration in the shape of
the diffracted peak, the increase in intensity that you gain will be less than the proportional increase of the
receiving slit aperture.
When you use the programmable receiving slit together with the programmable anti-scatter slit in the beam
tunnel mode, we recommend that you use an aperture of at least 0.05 mm.
Page 16.18 07.03.27

16.4 HIGH RESOLUTION DIFFRACTED BEAM OPTICS

There are two types of high resolution diffracted beam optics, they are:
• Rocking curve attachment to enable rocking curves to be measured.
• Triple axis and rocking curve attachment for rocking curve measurements, reciprocal space mapping,
and high resolution X-ray topography.
16.4.1 PW3097/60 Rocking Curve Attachment

The PW3097/60 Rocking Curve Attachment shown in Figure 16.9 is a diffracted beam PreFIX module used to
mount a proportional detector on the diffracted beam optics arm. This module is used for recording conventional
rocking curves and medium resolution reciprocal space maps using one of the high-resolution monochromators
as incident beam PreFIX module. The slit holder has a 6 mm aperture. There is a slit holder for mounting slits
in front of the detector to reduce the accepted beam height, it can be rotated with respect to the diffraction plane.
This rotation can be used when the physical surface of a single crystal sample is inclined with respect to the
diffractometer axis when lattice planes are aligned parallel to the diffractometer axis. In this case the slit rotation
can be used to make the slit parallel to the rectangular dimensions of the diffracted beam shape [8]. The slit can
also be rotated 90º in order to increase the acceptance angle to about 3.5º. The rotation mechanism is described
in section 16.4.1.2.1.
The PreFIX rocking curve attachment incorporates a rotatable slit holder and a detector mounting plate.
Figure 16.9: PW3097/60 Rocking Curve Attachment with

PW3011/20 Proportional Detector Mounted
07.03.27 Page 16.19

16.4.1.1.1 Fixed Slits
A set of three fixed receiving slits marked 1/4º (opening 0.38 mm), 1º (opening 1.5 mm), and 1 mm (shown in
Figure 16.10) are supplied as part of the rocking curve attachment. They can be fitted into the rotatable slit
holder. These slits are used to control the height of the diffracted beam as seen by the detector, and to reduce the
background intensity.
Figure 16.10: 1 mm Fixed Slit

PW3083/00 is a set of fixed slits marked 1/32º (opening 0.05 mm), 1/16º (opening 0.1 mm) and 1/8º (opening
0.19 mm). These slits can be fitted into the rotatable slit holder. These slits are used to control the height of the
diffracted beam as seen by the detector, and to reduce the background intensity.
16.4.1.1.3 Beam Width Mask

A beam width mask with a 1 mm opening (shown in Figure 16.11) is supplied as part of the rocking curve
attachment. It can be fitted into the rotatable slit holder.
Figure 16.11: 1 mm Beam Mask
16.4.1.1.4 Metal Rod

A metal rod is supplied with the rocking curve attachment to rotate the receiving slits through small angles. How
to use this rod is described in section 16.4.1.2.

A PW3011/20 Proportional Detector can be mounted behind the rocking curve attachment in the detector
interface which holds the detector in place by means of two spring-loaded balls. This is shown in Figure 16.9.
Page 16.20 07.03.27


The PW3087/6x Automatic Beam Attenuator can be mounted on the front of the rocking curve attachment (see
Figure 16.12). The attenuation factor is entered in the data collector software and is used to automatically adjust
the measured intensity values. More information about the automatic beam attenuator is given in Part II -
Chapter 2, section 2.2.2.
16.4.1.1.6.1 Mounting the Automatic Beam Attenuator onto the Rocking Curve Attachment
1. Remove the three screws (see Figure 2.2) at the back (metal part) of the PW3087/6x Automatic Beam
Attenuator.
3. Fit the metal part (NOT the side with the alignment pins) onto the rocking curve attachment; line it up
with the slit of the automatic beam attenuator to the slit on the rocking curve attachment and ensure that
the four screw holes line up. Use the four screws supplied with the automatic beam attenuator and
Replace the painted part of the automatic beam attenuator and use the three screws you removed in step 1 to

Rocking Curve Attachment
CAUTION When an automatic beam attenuator is mounted onto a rocking

curve attachment the maximum 2θ angle of the diffracted beam
arm is limited. Use the data collector software to set a lower
maximum value of 2θ in order to avoid collision between the X-ray
shield and the automatic beam attenuator
07.03.27 Page 16.21


A PW3018/00 PIXcel detector, equipped with a PW3017/60 Interface, can be mounted behind the rocking curve
attachment in the detector interface which holds the detector in place by means of two spring-loaded balls. To
16.4.1.2 Use
16.4.1.2.1 Rotating the Slit Holder
Figure 16.13: Rotatable Slit Holder with Rod Inserted

To rotate the slit holder on the rocking curve attachment, proceed as follows:
1. Slide the slit into position.
2. Unlock the rotatable slit holder by loosening the locking screw (see Figure 16.9).
3. Insert the metal rod into the slot at the top of the rotatable slit holder (see Figure 16.13).
4. Rotate the holder using the rod. The amount of rotation can be seen on the engraved scale.
5. Tighten the locking screw and remove the rod.
Page 16.22 07.03.27

16.4.1.2.2 Recording Rocking Curves

Rocking curves can be recorded on an X’Pert PRO system as follows:
Focus: point or line, depending on the incident beam monochromator used
Incident beam optics: PreFIX high-resolution monochromator, or PreFIX hybrid monochromator
Diffracted beam optics: PreFIX rocking curve attachment (open receiving slit)
Variations:
Add receiving slits to reduce background intensity.
When studying small lattice parameter differences (<0.01%) use a Ge(440) four-crystal
monochromator.
General experimental procedure:
1. Find reflection using the reciprocal space map option in the data collector software.
2. Set the reflecting plane normal perpendicular to the diffractometer axis using ϕ or ψ optimization.
3. Collect intensity data using an ω or ω-2θ scan.
16.4.1.2.3 Recording Medium Resolution Reciprocal Space Maps

Medium resolution reciprocal space maps can be recorded on an X’Pert PRO system as follows:
Focus: point or line, depending on the incident beam monochromator used
Incident beam optics: PreFIX high-resolution monochromator, or PreFIX hybrid monochromator
Diffracted beam optics: PreFIX rocking curve attachment with rotatable slit
1. Choose a reflection for which the diffracted beam is narrower than the incident beam - this requires
reflection from a plane inclined to the sample surface using a beam path where ω is greater than 2θ/2.
Calculate the expected diffracted beam width Wd.
2. Find and optimize the reflection (Steps 1 and 2 of section 16.4.1.2.2) using an open receiving slit.
3. Set ω on the peak position.
4. Fit a slit with a width close to Wd into the rotatable slit holder.
5. Adjust 2θ to give a maximum intensity.
6. Rotate the slit by small amounts and repeat step 5.
7. Rotate the slit to the position which gave the highest maximum intensity.
8. Record an area map using a 2-axes scan program (omega-2theta and omega).
16.4.2 PW3120/60 Triple Axis and Rocking Curve Attachment

PW3120/60 is a diffracted beam PreFIX module combining a triple axis and rocking curve attachment designed
for rocking curve measurements, reciprocal space mapping, and high resolution X-ray topography. It is intended
for use with X’Pert PRO MRD systems. It provides two different diffracted beam path options.
One beam path is identical to the PW3097/60 Rocking Curve Attachment. The second path carries an analyzer
crystal to convert the diffractometer to triple axis mode. The analyzer crystal is a channel cut germanium crystal.
The diffracted beam undergoes three (022) reflections within the groove before entering the detector. The
acceptance angle of the analyzer crystal is 12 arc seconds. The offset angle between the beam paths is 6°.
The attachment can be supplied with one or two detectors. If two detectors are available it is possible to record
rocking curves and diffraction space maps using the batch mode of the data collector software. If only one
detector is available it must be moved to the analyzer arm when operating the diffractometer in triple axis mode.
The detectors can be mounted in the detector interface which holds the detector in place by means of two spring-
loaded balls.
Refer to section 16.4.1 for a description of the rocking curve part of the attachment. The triple axis part of the
attachment is described in Chapter 19 (section 19.5.1) in Part II of this User’s Guide.
07.03.27 Page 16.23
Slot for Detector Interface

Metal Rod Scale for (Triple Axis Arm)
Rotatable Slit
Detector Interface Locking Screw
(Rocking Curve Arm) (not visible)
Analyzer
Crystal
Housing
Holes for Automatic

Beam Attenuator
Mounting Screws
Figure 16.14: PW3120/60 Triple Axis and Rocking Curve Attachment
Page 16.24 07.03.27

16.4.3 PW3120/65 Asymmetrical Triple Axis and Rocking Curve

Attachment
for rocking curve measurements, reciprocal space mapping, and high resolution X-ray topography. It is intended
for use with X’Pert PRO MRD systems. It provides two different diffracted beam path options.
The diffracted beam undergoes two (022) reflections within the groove before entering the detector. The
rocking curves and diffraction space maps using the batch mode of the data collector software. If only one
loaded balls.
Refer to section 16.4.1 for a description of the rocking curve part of the attachment. The triple axis part of the
attachment is described in section 19.5.2 in Chapter 19 in Part II of this User’s Guide.
Figure 16.15: PW3120/65 Asymmetrical Triple Axis and Rocking Curve Attachment
07.03.27 Page 16.25

Page 16.26 07.03.27

Chapter 17
Diffracted Beam Masks
Contents
17.1 General............................................................................................................................... 17 - 3
17.1.1 Applications.......................................................................................................................... 17 - 3
17.1.1.1 Texture and Psi-stress Analysis ........................................................................... 17 - 3
17.1.1.2 Parallel Beam Applications with Line Focus ...................................................... 17 - 3
17.2 PW3094/20 Diffracted Beam Mask Set........................................................................... 17 - 3
17.3 Choice of Beam Mask ....................................................................................................... 17 - 4
07.03.27 Page 17.1

Page 17.2 07.03.27

Part II - Chapter 17: Diffracted Beam Masks
17.1 GENERAL
Beam masks are fitted in the diffracted beam path to control the axial width and acceptance of the diffracted
beam, thus defining the amount (width) of the sample that is observed by the detector. Normally, beam masks
are used for point focus applications, for example: texture and psi-stress analysis. Soller slits are used to control
the axial acceptance of the diffracted beam in line focus applications.
Diffracted beam masks are also used in the parallel beam geometry, with line focus applications. Here they can
be used to define the axial size and acceptance of the diffracted X-ray beam as an alternative to Soller slits.
17.1.1 Applications
Beam masks are used in the Schulz and the parallel beam geometry of point focus applications, such as texture
and psi-stress analysis, to control the axial width of the diffracted X-ray beam. The beam mask opening must be
selected such that the complete part of the sample contributing to the diffracted intensity (that is, irradiated by
the incident beam) is “seen” by the detector. However, no more than that, in order to avoid scattered radiation
giving rise to high background intensities in the measurement.
17.1.1.2 Parallel Beam Applications with Line Focus

Soller slits are usually used to control the axial acceptance of the diffracted beam in parallel beam applications
employing the line focus of an X-ray tube. However, when Soller slits are already inserted in the incident beam
path to control the axial divergence, it is sometimes useful to limit the observed width of the sample. Diffracted
beam masks are set such that the irradiated part of the sample, determined by the incident beam mask is “seen”
by the detector. However, no more than that, in order to avoid scattered radiation giving rise to high background
intensities in the measurement.
17.2 PW3094/20 DIFFRACTED BEAM MASK SET

The PW3094/20 Diffracted Beam Mask Set comprises a beam mask holder and two metal strips each with two
openings for the diffracted beam to pass through. The sizes of the openings are marked on the strips, they are
20, 10, 4, and 2 mm. The complete set is shown in Figure 17.1.
The holder is mounted onto a PW3093/60 Programmable Receiving Slit or a PW3098/xx Parallel Plate
Collimator and the selected strip can then be inserted into the holder. Mounting the beam mask holder onto the
programmable receiving slit or the parallel plate collimator is described in Chapter 16 (section 16.3.2.1.7) or
Chapter 18 (section 18.3.3) in Part II of this User’s Guide.
07.03.27 Page 17.3

Figure 17.1: PW3094/20 Diffracted Beam Mask Set
17.3 CHOICE OF BEAM MASK

Which beam mask you use depends on the irradiated width of the sample, the axial divergence of the diffracted
beam and the distance between the beam mask and the center of the goniometer. The width of the X-ray beam
at the position of the beam mask can be estimated by:
M = d tan α + W
in which:
M = the width of the X-ray beam at the position of the diffracted beam mask,
d = the distance between the center of the goniometer and the diffracted beam mask position,
α = the axial divergence of the X-ray beam, as determined by the incident beam module,
W = the irradiated width on the sample at ψ = 0º.
Select a beam mask with an opening larger than the width of the X-ray beam.
Page 17.4 07.03.27

Chapter 18
Diffracted Beam Collimators
Contents
18.1 General............................................................................................................................... 18 - 3
18.1.1 Applications.......................................................................................................................... 18 - 3
18.1.1.1 Thin-film Phase Analysis and Reflectivity .......................................................... 18 - 3
18.1.1.2 Phase Analysis and Omega-stress Analysis......................................................... 18 - 3
18.1.1.3 Texture and Psi-stress Analysis ........................................................................... 18 - 3
18.1.1.4 In-plane Diffraction ............................................................................................. 18 - 3
18.2 PW3098/xx Parallel Plate Collimator ............................................................................. 18 - 4
18.3 Accessories ......................................................................................................................... 18 - 5
18.3.1 Collimator Slit (0.1 mm) ...................................................................................................... 18 - 5
18.3.2 PW3085/x0 Soller Slits ........................................................................................................ 18 - 5
18.3.3 PW3094/20 Diffracted Beam Mask Set ............................................................................... 18 - 5
18.3.4 PW3121/00 Diffracted Beam Flat Crystal Monochromator ................................................ 18 - 6
18.3.4.1 Mounting a Flat Crystal Monochromator ............................................................ 18 - 6
18.3.5 Large Beta-filters.................................................................................................................. 18 - 7
18.3.6 PW3011/20 Proportional Detector ....................................................................................... 18 - 7
18.3.7 PW1964/96 Scintillation Detector........................................................................................ 18 - 7
18.3.8 PW3018/00 PIXcel Detector ................................................................................................ 18 - 7
07.03.27 Page 18.1

Page 18.2 07.03.27

Part II - Chapter 18: Diffracted Beam Collimators
18.1 GENERAL
A diffracted beam collimator is an optical module used in the quasi-parallel beam geometry to define the
acceptance angle of the diffracted beam as seen by the detector. This collimator is used with parallel beam
modules, such as an X-ray mirror, an X-ray lens, and a mono-capillary in the incident beam path. It is also used
in thin-film phase analysis and reflectivity, using a small angle divergence slit at a low angle of incidence. A
diffracted beam collimator does not control the axial acceptance of the X-ray beam, Soller slits are used in the
diffracted beam path to control the axial acceptance.
Two types of diffracted beam collimator are available on X’Pert PRO systems:
• One type consists of a set of parallel plates perpendicular to the diffraction plane, these are called parallel
plate collimators. The distance between the plates inside the collimator defines the acceptance angle; the
total height (the size of the opening perpendicular to the plates) of the collimator and the angle between
the diffracted beam and the sample surface define the length of the sample that is observed.
• The other type of diffracted beam collimator is called a beam tunnel. This collimator is formed by
combining an anti-scatter slit and a receiving slit. The aperture of the anti-scatter slit is set to match the
aperture of the receiving slit.
Parallel plate collimators are described in this chapter. The beam tunnel is described in Chapter 16 in Part II of
18.1.1 Applications
Diffracted beam collimators are commonly used in thin-film phase analysis and reflectivity applications, and in
parallel beam applications; both of which use the line focus and the point focus of the X-ray tube.
18.1.1.1 Thin-film Phase Analysis and Reflectivity

In thin-film phase analysis and reflectivity studies a diffracted beam collimator is used in combination with an
incident beam optical module providing an X-ray beam with a very low divergence, for instance: an X-ray
mirror, a hybrid monochromator or a divergence slit with a small opening (divergence angle smaller than 1/4º).
In this configuration the angle of incidence of the X-ray beam is fixed at a very low angle with respect to the
sample surface. During the measurement only the 2θ angle changes.

Diffracted beam collimators are used in line focus applications in the parallel beam geometry such as phase
analysis and omega-stress analysis. The parallel beam geometry ensures that the measured peak positions are
insensitive to sample height misalignment and roughness. This also means that there are no defocusing effects
in omega-stress measurements over a wide range of ω tilts. However, the highly parallel beam leads to a reduced
number of crystallites from a random powder contributing to the diffracted intensity, and particle statistics may
become a problem.

Typical point focus applications in the parallel beam geometry employing a diffracted beam collimator are
texture and psi-stress analysis. The X-ray lens or a mono-capillary for analysis on small spots, can be used as
incident beam modules. Alternatively, an incident beam collimator with a low divergence can be used. The
advantage of this configuration is that it is insensitive to sample height misalignment. This also means that no
defocusing effects occur over a wide range of ψ tilts during a psi-stress or texture measurement.
18.1.1.4 In-plane Diffraction

The parallel plate collimator can be used in the diffracted beam path for diffraction experiments on specially
equipped X’Pert PRO MRD systems. The X-ray lens is then used as an incident beam module.
In-plane diffraction is used to measure the lattice spacings between the crystal planes perpendicular to the
sample’s surface in very thin films.
Using X’Pert PRO MRD for in-plane diffraction is described in section 11.2.2.4 in Chapter 11 in Part II of this
User’s Guide.
07.03.27 Page 18.3
18.2 PW3098/XX PARALLEL PLATE COLLIMATOR

The PW3098/xx Parallel Plate Collimator is a diffracted beam PreFIX module that consists of a set of parallel
plates which define the equatorial acceptance angle as seen by the detector. The parallel plate collimator is shown
in Figure 18.1.
Three different parallel plate collimators are available on X’Pert PRO systems; they differ in the distance
between their plates, and thus by the equatorial acceptance angle. The relationship between the type number of
the parallel plate collimator and the equatorial acceptance (half opening angle) is shown in Table 18.1.
Table 18.1: Parallel Plate Collimator Type Numbers and their Equatorial Acceptance
Type Number Equatorial Acceptance
PW3098/09 0.09º
PW3098/18 0.18º
PW3098/27 0.27º
Figure 18.1: PW3098/xx Parallel Plate Collimator with PW3011/20 Proportional Detector Mounted
The PreFIX parallel plate module incorporates:
• a slot for a collimator slit
• a slot for Soller slits or a diffracted beam mask holder
• an interface to mount a detector.
The detector interface can be removed in order to mount a flat crystal monochromator with detector.
The height (equatorial aperture) of the parallel plate collimator is 20 mm, the width (axial aperture) is 23 mm.
Page 18.4 07.03.27

18.3 ACCESSORIES
The accessories described in this section are common to all three of the above mentioned parallel plate
collimators.
18.3.1 Collimator Slit (0.1 mm)

A collimator slit with an equatorial aperture of 0.1 mm is supplied together with the parallel plate collimator.
This slit is used during reflectivity measurements to enhance the resolution at very low 2θ angles (<4º). It is
placed in the slot for the collimator slit which is located behind the parallel plates.
Figure 18.2: Collimator Slit
18.3.2 PW3085/x0 Soller Slits

Parallel plate collimators only control the equatorial acceptance, Soller slits are used to control the axial
acceptance of the diffracted beam. Four sizes of Soller slits are available for X’Pert PRO systems, they are:
PW3085/80 0.08 rad Soller Slits.
Soller slits are mounted into the slot for Soller slits on the PreFIX module as shown in Figure 18.1. To do this,
insert the Soller slits into the slot until it clicks into place.
18.3.3 PW3094/20 Diffracted Beam Mask Set

Diffracted beam masks can be inserted into the parallel plate collimator to control the axial width of the
diffracted X-ray beam. The diffracted beam mask set consists of a beam mask holder and four beam masks with
openings of 20, 10, 4 and 2 mm. The masks are used in texture and psi-stress measurements.
The beam mask holder is inserted into the slot on the PreFIX module as indicated in Figure 18.1. To mount the
beam masks proceed as follows:
1. If Soller slits are mounted, remove them.
2. Insert the beam mask holder into the slot with the mask slot facing the detector until it clicks into place.
3. Insert the required mask into the slot in the beam mask holder.
07.03.27 Page 18.5

18.3.4 PW3121/00 Diffracted Beam Flat Crystal Monochromator

The PW3121/00 Diffracted Beam Flat Crystal Monochromator is designed for use in parallel beam applications.
It can be mounted on the detector side of the parallel plate collimator as shown in Figure 18.3. Mounting
instructions are given in section 18.3.4.1. Information about adjusting the flat crystal monochromator to the
characteristic wavelength of the X-ray tube being used is given in Chapter 19 in Part II of this User’s Guide.
If a diffracted beam flat crystal monochromator is used, a detector slit must be inserted into the slot for the
collimator slit (see Figure 18.1). This detector slit is used to make sure that only the monochromized X-ray beam
is collected by the detector.
Figure 18.3: PW3121/00 Diffracted Beam Flat Crystal Monochromator with

Detector Mounted onto a Parallel Plate Collimator
18.3.4.1 Mounting a Flat Crystal Monochromator
CAUTION
Do not turn the alignment screw marked X in Figure 19.1 as it is
used to adjust the module alignment.
Mount the diffracted beam flat crystal monochromator as follows:

1. Remove the detector by sliding it out of the detector interface and place it carefully to one side.
2. Undo the two screws that secure the detector interface and then remove it.
3. Hold the flat crystal monochromator in place and carefully align the holes on the monochromator with
the screw holes where you removed the screws in step 2. Insert two screws into the holes you just lined
up and tighten them.
4. Re-mount the detector onto the detector interface on the flat crystal monochromator.
5. Insert the detector slit (part of the PW3121/00) with the chemical symbol corresponding to the X-ray
tube’s anode material into the slot for the collimator slit. The chemical symbol marked on the slit must
face towards the detector.
Aligning the flat crystal monochromator for a specific wavelength is described in section 19.2.1.2.1.
Page 18.6 07.03.27
18.3.5 Large Beta-filters

There are four large beta-filters that can be used with the parallel plate collimator, they are:
Fe filter (part of PW3158/00) for Co Kα radiation
V filter (part of PW3158/00) for Cr Kα radiation
Zr filter (part of PW3158/00) for Mo Kα radiation
The filter must be installed (mounted) in the slot for collimator slit as shown in Figure 18.1.
18.3.6 PW3011/20 Proportional Detector

A PW3011/20 Proportional Detector can be mounted behind the parallel plate collimator in the detector interface
which holds the detector in place by means of two spring-loaded balls. This is shown in Figure 18.1.
monochromator (see Figure 18.3). It should be mounted such that it is rotated 90º with respect to its position
when mounted directly behind the parallel plate collimator.
18.3.7 PW1964/96 Scintillation Detector

A PW1964/96 Scintillation Detector can be mounted behind the parallel plate collimator in the detector interface
which holds the detector in place by means of two spring-loaded balls.
monochromator.
18.3.8 PW3018/00 PIXcel Detector

A PW3018/00 PIXcel detector, equipped with a PW3017/60 Interface, can be mounted behind the parallel plate
collimator in the detector interface which holds the detector in place by means of two spring-loaded balls. To
07.03.27 Page 18.7

Page 18.8 07.03.27

Chapter 19
Diffracted Beam Monochromators
Contents
19.1 General............................................................................................................................... 19 - 3
19.2 Flat Crystal Monochromators ......................................................................................... 19 - 3
19.2.1 PW3121/00 Diffracted Beam Flat Crystal Monochromator ................................................ 19 - 3
19.2.1.1 Detector Slits........................................................................................................ 19 - 3
19.2.1.2 Use ....................................................................................................................... 19 - 3
19.3 Curved Crystal Monochromators ................................................................................... 19 - 6
19.3.1 PW312x/10 Diffracted Beam Curved Crystal Monochromators ......................................... 19 - 6
19.3.1.1 Use ....................................................................................................................... 19 - 7
19.4 Monochromators for Line Detectors............................................................................... 19 - 7
19.4.1 PW3122/00 Diffracted Beam Monochromator for X’Celerator .......................................... 19 - 8
19.4.1.1 PW3094/50 Fixed Anti-scatter Slit for Monochromator for X'Celerator ............ 19 - 8
19.4.1.2 Use ....................................................................................................................... 19 - 9
19.4.2 PW3124/00 Diffracted Beam Monochromator for PIXcel .................................................. 19 - 9
19.4.2.1 PW3490/50 Fixed Anti-scatter Slit for Monochromator for PIXcel ................... 19 - 9
19.4.2.2 Use ..................................................................................................................... 19 - 11
19.5 Triple Axis Monochromator .......................................................................................... 19 - 12
19.5.1 PW3120/60 Triple Axis and Rocking Curve Attachment.................................................. 19 - 12
19.5.1.1 Accessories ........................................................................................................ 19 - 13
19.5.1.2 Use ..................................................................................................................... 19 - 16
19.5.2 PW3120/65 Asymmetric Triple Axis and Rocking Curve Attachment ............................. 19 - 17
19.5.2.1 Accessories ........................................................................................................ 19 - 18
19.5.2.2 Use ..................................................................................................................... 19 - 20
07.03.27 Page 19.1

Page 19.2 07.03.27

Part II - Chapter 19: Diffracted Beam Monochromators
19.1 GENERAL
Diffracted beam monochromators are situated between the receiving optics and the detector. They are used to
reduce the background radiation efficiently, eliminate unwanted lines, such as the Kβ line almost completely,
and reduce the effect of sample fluorescence.
The diffracted beam monochromator consists of crystalline material which diffracts the radiation accepted by
the receiving optics on which the monochromator is mounted. The detector slit is set at an angle so that only the
wavelength of interest is collected by the detector.
There are four types of diffracted beam monochromator associated with X’Pert PRO, they are:
Flat crystal monochromator for parallel beam applications.
Curved crystal monochromator for focusing beam applications.
Diffracted Beam monochromator for use with line detectors, X’Celerator and PIXcel.
Triple axis monochromator for reciprocal space maps.
19.2 FLAT CRYSTAL MONOCHROMATORS

Diffracted beam flat crystal monochromators consist of a flat pyrolytic graphite crystal in a housing, for use in
parallel beam applications. They can be adjusted to diffract a specific wavelength.
19.2.1 PW3121/00 Diffracted Beam Flat Crystal Monochromator

The PW3121/00 Diffracted Beam Flat Crystal Monochromator is designed to be used with PW3098/xx Parallel
Plate Collimators and the PW3093/60 Programmable Receiving Slit when used together with a PW3091/x0
Programmable Anti-Scatter Slit in the beam tunnel mode for parallel beam applications. The monochromator is
shown in Figure 19.1. The monochromator can be dismounted from the diffracted beam module and mounted
again without the need of additional alignment. It can be used for the characteristic wavelength of molybdenum,
iron, cobalt, copper and chromium tubes. The reflectivity for Cu Kα radiation is between 14% and 20%. The
rocking width of the crystal is 0.4º.
19.2.1.1 Detector Slits

A set of five detector slits each with a different chemical symbol engraved on it (Mo, Cu, Co, Fe and Cr) is
delivered with the PW3121/00 Flat Crystal Monochromator. The slits can be inserted into the slot for the
collimator slit on the PW3098/xx Parallel Plate Collimator, they are used to prevent the X-ray beam coming off
the parallel plate collimator being accepted by the detector without having been diffracted by the
monochromator.
The chemical symbol on the slit used should correspond to the anode material of the X-ray tube being used.
19.2.1.2 Use
Mounting instructions for the flat crystal monochromator are given in the chapters describing diffracted beam
collimators (Chapter 18) and receiving slits (Chapter 16) in Part II of this User’s Guide. This section describes
the alignment of the monochromator for a specific wavelength.
When the flat crystal monochromator is mounted onto a programmable receiving slit used in the beam tunnel
mode, the receiving slit can be opened over its full range of slit settings (0 to 3 mm).
07.03.27 Page 19.3

Detector
Interface Alignment Screw Y
Alignment Screw X (Not visible)
(Not visible)
Holes for
Mounting Screws
Locking Screw
Shaft
Figure 19.1: PW3121/00 Flat Crystal Monochromator
Figure 19.2: Detector Slits

19.2.1.2.1 Adjusting Wavelengths
Proceed as follows to adjust the flat crystal monochromator for the characteristic wavelength used:
1. Mount the flat crystal monochromator onto the diffracted beam PreFIX module that you are going to
use. Refer to section 16.3.2.1.8.1 for the programmable receiving slit or to section 18.3.4.1 for parallel
plate collimators.
2. Mount the pressed powder silicon reference sample supplied with your X’Pert PRO system onto the
sample stage.
Page 19.4 07.03.27

3. Mount a fixed or programmable divergence slit with a fixed slit aperture of 1º.
4. a. If you are using the flat crystal monochromator with a parallel plate collimator, insert the detector slit
that has the chemical symbol of the anode material of the X-ray tube being used.
b. If you are using the flat crystal monochromator with a programmable divergence slit and a
programmable anti-scatter slit, use the “beam tunnel” mode and set the aperture to 3 mm.
5. Set the goniometer to ω = 2º and 2θ to the value for the Si(311) reflection corresponding to the
characteristic radiation used, refer to Table 19.1.
Table 19.1: 2θ Angle of the Si(311) Reflection for

Different Types of Characteristic Radiation
Characteristic
2θ
Radiation
Mo Kα 25.07º
Cu Kα 56.17º
Co Kα 66.27º
Fe Kα 72.53º
Cr Kα 88.78º
Locking Screw
Shaft
Alignment Screw Y
Figure 19.3: Position of the Alignment Screw Y on the

PW3121/00 Flat Crystal Monochromator
6. You must first do a coarse alignment of the monochromator crystal to the characteristic radiation. The
alignment screw has four rings engraved on it to help you do this. Release the locking screw and then
turn the alignment screw (marked Y in Figure 19.3) so that the line corresponding to the characteristic
radiation being used is flush with the surface of the monochromator housing. The lines for the
characteristic radiation are distributed from the screw head downwards as follows:
Cr Kα, Fe Kα, Co Kα, and then Cu Kα / Mo Kα.
Note that the line for Mo Kα is the same line as for Cu Kα. The reason for this is that for coarse
alignment purposes, the graphite (004) reflection with Mo Kα radiation has the same setting as the
(002) reflection with Cu Kα radiation.
07.03.27 Page 19.5

7. Fine adjustment is performed by maximizing the measured intensity of the Si(311) reflection. Open the
shutter and measure the intensity of the reflection. Close the shutter and carefully adjust the alignment
screw. Open the shutter and measure the intensity again. Keep repeating this procedure until you have
found the maximum intensity. This fine adjustment should not need very much adjustment.
8. Tighten the locking screw to lock the monochromator into its position.
The flat crystal monochromator is now aligned for the characteristic of the wavelength being used.
19.3 CURVED CRYSTAL MONOCHROMATORS

Diffracted beam curved crystal monochromators are used in Bragg-Brentano geometry. They consist of a curved
(Johann) pyrolytic graphite crystal in a housing with a built-in 0.8 mm detector slit.
The curvature of the crystal is such that the crystal surface, the receiving slit and the detector slit all lie on the
focusing circle of the monochromator. The monochromator is aligned in a way that ensures that only the required
wavelength passes the detector slit to be collected by the detector.
19.3.1 PW312x/10 Diffracted Beam Curved Crystal Monochromators

The PW312x/10 Diffracted Beam Curved Crystal Monochromators are all designed as single wavelength
monochromators. The relationship between the type number and the relevant characteristic radiation is shown in
Table 19.2. The monochromator is shown in Figure 19.4. The reflectivity for Cu Kα radiation is between 25%
and 40%. The rocking width of the crystals is 0.4º.
Detector
Interface
Alignment Screw X
(Not visible)
Holes for
Mounting Screws
Figure 19.4: PW312x/10 Curved Crystal Monochromator
Page 19.6 07.03.27

Table 19.2: Monochromator Type numbers

and Characteristic Radiation
Type Characteristic
Number Radiation
PW3123/10 Cu Kα
PW3125/10 Mo Kα
PW3126/10 Co Kα
PW3127/10 Fe Kα
PW3128/10 Cr Kα
19.3.1.1 Use
The curved crystal monochromator can only be mounted onto the PW3093/60 Programmable Receiving Slit. No
further alignment is required after mounting. Mounting instructions are given in section 16.3.2.1.9.1 in Chapter
16 in Part II of this User’s Guide.
19.4 MONOCHROMATORS FOR LINE DETECTORS

Fast X-ray detectors require a special kind of diffracted beam monochromator. This section describes the
monochromator for the RTMS detector, the X’Celerator and for the PIXcel detector.
X’Celerator
Soller Slits
Assembly
Detector
Interface
Monochromator
Housing
Knurled Knob
Figure 19.5: PW3122/00 Diffracted Beam Monochromator for X’Celerator

with the X’Celerator Mounted
07.03.27 Page 19.7

19.4.1 PW3122/00 Diffracted Beam Monochromator for X’Celerator

The PW3122/00 Diffracted Beam Monochromator is designed for use with the PW3015/x0 X’Celerator. The
monochromator with an X’Celerator mounted is shown in Figure 19.5. The type number comprises a
monochromator housing mounted onto a PreFIX interface, a detector interface to fit the X’Celerator and an
integrated Soller slits assembly. The monochromator is factory aligned for the characteristic Kα radiation. The
acceptance angle of the Soller slits assembly is 0.017 rad.
The intensity of an X-ray beam coming out of the PW3122/00 Diffracted Beam Monochromator is between 14%
to 20% compared to the intensity detected by an X’Celerator with a nickel filter and a 0.04 rad Soller slits
assembly. The intensity of the Cu Kβ line is less than 1% of the intensity of the Cu Kα1 line.
19.4.1.1 PW3094/50 Fixed Anti-scatter Slit for Monochromator for X'Celerator

PW3094/50 is a set of fixed anti-scatter slits marked 0.2 mm, 3.9 mm, 4.6 mm, 5.9 mm and 8.6 mm for use with
the PW3122/00 Diffracted Beam Monochromator. They can be inserted in the slit holder supplied as part of the
set. These slits are used to reduce the amount of scattered radiation entering the X'Celerator detector equipped
with the PW3122/00 Monochromator. Instructions on how to mount the slit holder onto the monochromator are
given in section 19.4.1.1.1 below. Information about how to use these fixed anti-scatter slits including the
selection of slit size is given in section 20.3.4 in Chapter 20 of Part II of this User's Guide.
Figure 19.6: Mounting the PW3094/50 Fixed Anti-scatter Slits Holder

onto the PW3122/00 Monochromator
Page 19.8 07.03.27

19.4.1.1.1 Mounting the Fixed Anti-scatter Slits Holder onto the Diffracted Beam
Monochromator
Mount the fixed anti-scatter slits holder onto the PW3122/00 Diffracted Beam Monochromator as follows:
1. Bring the fixed anti-scatter slit holder into position on the entrance of the Soller slits assembly of the
monochromator, as is shown in Figure 19.6.
2. Tighten the Allen screw to fix the holder into position.
Now you can insert one of the fixed anti-scatter slits into the holder, pressing it home in such a way that it clicks
into place. No alignment is required.
19.4.1.2 Use
The PW3122/00 Diffracted Beam Monochromator can only be used with the PW3015/x0 X’Celerator and Cu
Kα radiation. No further alignment is necessary when the X’Celerator is mounted onto the detector interface.
Mounting instructions are given in section 21.4 of Chapter 21 of Part II of this User’s Guide.
For further information about the best choice of modules to suppress unwanted lines in measurements using the
X’Celerator refer to section 21.4 of Chapter 21 of Part II of this User’s Guide.
19.4.2 PW3124/00 Diffracted Beam Monochromator for PIXcel

The PW3124/00 Diffracted Beam Monochromator is designed for use with the PW3018/00 PIXcel. The
monochromator with a PIXcel detector mounted is shown in Figure 19.7. The type number comprises a
monochromator housing mounted onto a PreFIX interface, a detector interface to fit the PIXcel and an integrated
Soller slits assembly. The monochromator is factory aligned for the characteristic Kα radiation. The acceptance
angle of the Soller slits assembly is 0.017 rad.
The intensity of an X-ray beam coming out of the PW3124/00 Diffracted Beam Monochromator is between 14%
and 20% compared to the intensity detected by a PIXcel with a nickel filter and a 0.04 rad Soller slits assembly.
The intensity of the Cu Kβ line is less than 1% of the intensity of the Cu Kα1 line.
19.4.2.1 PW3490/50 Fixed Anti-scatter Slit for Monochromator for PIXcel

PW3490/50 is a set of fixed anti-scatter slits marked 15.8 mm, 10.4 mm, 7.7 mm, 6.4 mm, 5.7 mm and 0.2 mm
for use with the PW3124/00 Diffracted Beam Monochromator. They can be inserted into the slit holder supplied
as part of the set. These slits are used to reduce the amount of scattered radiation entering the PIXcel detector
equipped with the PW3124/00 Monochromator. Instructions on how to mount the slit holder onto the
monochromator are given in section 19.4.2.1.1 below. Information about how to use these fixed anti-scatter slits
including selection of slit sizes is given in section 20.3.7 in Chapter 20 of Part II of this User's Guide.
19.4.2.1.1 Mounting the Fixed Anti-scatter Slits Holder onto the Diffracted Beam
Monochromator
Mount the fixed anti-scatter slits holder onto the PW3124/00 Diffracted Beam Monochromator as follows:
1. Bring the fixed anti-scatter slit holder into position on the entrance of the Soller slits assembly of the
monochromator, as is shown in Figure 19.8.
2. Tighten the Allen screw to fix the holder into position.
Now you can insert one of the fixed anti-scatter slits into the holder, pressing it home in such a way that it clicks
into place. No alignment is required.
07.03.27 Page 19.9

Figure 19.7: PW3124/00 Diffracted Beam Monochromator for PIXcel with the PIXcel Mounted
Page 19.10 07.03.27

Figure 19.8: Mounting the PW3490/50 Fixed Anti-scatter Slits Holder onto the
PW3124/00 Monochromator
19.4.2.2 Use
The PW3124/00 Diffracted Beam Monochromator can only be used with the PW3018/00 PIXcel and Cu Kα
radiation. No further alignment is necessary when the PIXcel is mounted onto the detector interface.
Mounting instructions are given in section 21.5.3.10.1 in Chapter 21 of Part II of this User's Guide.
For further information about the best choice of modules to suppress unwanted lines in measurements using the
PIXcel refer to section 21.5.4.4 in Chapter 21 of Part II of this User's Guide.
07.03.27 Page 19.11

19.5 TRIPLE AXIS MONOCHROMATOR

19.5.1 PW3120/60 Triple Axis and Rocking Curve Attachment
for rocking curve measurements, reciprocal space mapping, and high resolution X-ray topography. It provides
two different diffracted beam path options. It is shown in Figure 19.9. It is intended for use with X’Pert PRO
MRD systems.
The diffracted beam undergoes three (220) reflections within the groove before entering the detector. The
rocking curves and diffraction space maps using the batch mode of the data collection software. If only one
loaded balls.
Refer to Chapter 16 (section 16.4.1) of Part II of this User’s Guide for a description of the rocking curve part of
the attachment. This section describes the use of the triple axis part.
Slot for Scale for

Adjustment Rod Rotatable Slit Detector
Interface
Locking
Screw
Analyzer
Crystal
Housing
Scale for
Topography
B Holder
A
Figure 19.9: PW3120/60 Triple Axis and Rocking Curve Attachment
Page 19.12 07.03.27

A set of three fixed receiving slits marked 1/4º (opening 0.38 mm), 1º (opening 1.5 mm) and 1 mm are supplied
as part of the rocking curve attachment. They can be fitted into both the rotatable slit holders. These slits are
used to control the height of the diffracted beam as seen by the detector and to reduce the background intensity.

0.19 mm). These slits can be fitted into both the rotatable slit holders.

A beam width mask with a 1 mm opening is supplied as part of the triple axis and rocking curve attachment. It
can be fitted into both the rotatable slit holders. This mask is used to control the width of the diffracted beam as
seen by the detector.

A metal rod is supplied with the triple axis and rocking curve attachment to rotate the receiving slits through
small angles. How to use this rod is described in Chapter 16 (section 16.4.1.2.1) in Part II of this User’s Guide.

A PW3011/20 Proportional Detector can be mounted behind both the rocking curve and the triple axis beam
paths in the detector interfaces which hold the detector in place by means of two spring-loaded balls.
We advise you to use the triple axis and rocking curve attachment with two PW3011/20 Detectors mounted.
19.5.1.1.6 PW3018/00 PIXcel detector

A PW3018/00 PIXcel detector, equipped with a PW3017/60 Interface, can be mounted behind both the triple-
axis and rocking curve beam paths in the detector interface which holds the detector in place by means of two
spring-loaded balls. To mount the detector, slide it into the interface until it clicks into position.

The PW3087/6x Automatic Beam Attenuator can be mounted on the front of the triple axis and rocking curve
attachment and used in place of the foil described in section 2.2.1 in Chapter 2 of Part II of this User’s Guide.
The attenuation factor is entered in the data collector software and is used to automatically adjust the measured
intensity values. More information about the automatic beam attenuator is given in Part II - Chapter 2, section
2.2.2.
CAUTION When an automatic beam attenuator is mounted onto a triple axis

and rocking curve attachment, the maximum 2θ angle of the
diffracted beam arm is restricted. Use the data collector software to
set a lower maximum 2θ angle in order to avoid a collision between
the automatic beam attenuator and the tube shield.
07.03.27 Page 19.13

19.5.1.1.7.1 Mounting the Automatic Beam Attenuator onto the Triple Axis and Rocking Curve
Attachment

Triple Axis and Rocking Curve Attachment
1. Remove the three screws at the back (metal part) of the PW3087/6x Automatic Beam Attenuator (see
Figure 2.2).
3. Fit the metal part (NOT the side with the alignment pins) onto the triple axis and rocking curve
attachment; line it up with the slit of the automatic beam attenuator to the slit in one of the beam paths
and ensure that the four screw holes line up. Use the four screws supplied with the automatic beam
attenuator and secure it into place.
19.5.1.1.8 PW3142/20 Topography Film Holder
A topography film holder can be mounted behind the analyzer crystal, it is designed for X-ray film pieces
measuring 25 mm x 40 mm. The topography film holder is shown in Figure 19.11.
X-ray topographs recorded after the analyzer crystal can be used to identify defects present in the irradiated part
of a (nearly) perfect sample.
X-ray topography is explained in more detail in Appendix C of this User’s Guide. How to record a topograph is
described in section 19.5.1.2.2.
Page 19.14 07.03.27

Figure 19.11: PW3142/20 Topography Film Holder
19.5.1.1.8.1 Loading a Film into the Holder
Loading film into the holder is described in Appendix C to this User’s Guide in section C.7.3.
19.5.1.1.8.2 Mounting the Holder onto the Triple Axis and Rocking Curve Attachment
The topography film holder mounted onto the triple axis and rocking curve attachment is shown in Figure 19.12.
Mount the topography film holder as follows:
1. Slide the topography film holder into the slot on the triple axis and rocking curve attachment with the
knurled ring on the detector side. Slide the holder in until the leading edge is at the 7th of the shorter
lines marked on the attachment (see A in Figure 19.9).
2. Slide the locking bar into the slot in the holder until it lines up with the two holes for the securing
screws (the left-hand screw hole is marked B in Figure 19.9). Insert and tighten the two securing screws
using the washers and spring washers provided.
19.5.1.1.8.3 Moving the Topography Film Holder
You can move the topography film holder to the next exposure position by loosening the two securing screws,
sliding the holder to the next mark and then tightening the screws.
07.03.27 Page 19.15

Figure 19.12: PW3142/20 Topography Film Holder Mounted on the Triple Axis
and Rocking Curve Attachment
19.5.1.2 Use
19.5.1.2.1 High Resolution Reciprocal Space Maps
High resolution reciprocal space maps can be recorded on an X’Pert PRO MRD system as follows:
Hardware configuration:
Focus: point or line, depending on the incident beam monochromator used.
Incident beam optics: a PW3110/6x High-resolution Monochromator or a PW3147/x0 Hybrid
Monochromator.
Diffracted beam optics: PW3120/60 Triple Axis and Rocking Curve Attachment.
1. Using the rocking curve beam path find a reflection using the Reciprocal Space Map option in the data
collector software.
3. Move ω to the peak position.
4. Move 2θ to the peak position using the triple axis beam path (change detector position if necessary).
5. Record an area map in using a 2-axes scan program (omega-2theta and omega).
Page 19.16 07.03.27

19.5.1.2.2 X-ray Topography

X-ray topographs can be recorded on an X’Pert PRO MRD system as follows:
Monochromator.
Diffracted beam optics: PW3120/60 Triple Axis and Rocking Curve Attachment.
1. Record a high resolution reciprocal space map as described in section 19.5.1.2.1.
2. Select a feature on the map for investigation and find the ω and 2θ values.
3. Move diffractometer to the ω and 2θ values found in step 2.
4. Load a film into the topography holder.
5. Mount the topography film holder onto the triple axis and rocking curve attachment as described in
section 19.5.1.1.8.2.
6. Make an exposure as described in Appendix C.
7. Process the film, instructions are given in Appendix C.
The topograph will provide an image of the area of sample irradiated by the incident beam. A detailed
description of the interpretation, recording and processing of topographs is given in Appendix C.
19.5.2 PW3120/65 Asymmetric Triple Axis and Rocking Curve Attachment

for rocking curve measurements, reciprocal space mapping, and high resolution X-ray topography. It provides
two different diffracted beam path options. It is shown in Figure 19.9. It is intended for use with X’Pert PRO
MRD systems.
The diffracted beam undergoes two (220) reflections within the groove before entering the detector. The
rocking curves and diffraction space maps using the batch mode of the data collection software. If only one
loaded balls.
Refer to Chapter 16 (section 16.4.1) of Part II of this User’s Guide for a description of the rocking curve part of
the attachment. This section describes the use of the triple axis part.
07.03.27 Page 19.17

Figure 19.13: PW3120/65 Asymmetric Triple Axis and Rocking Curve Attachment
A set of three fixed receiving slits marked 1/4º (opening 0.38 mm), 1º (opening 1.5 mm) and 1 mm are supplied
as part of the rocking curve attachment. They can be fitted into both the rotatable slit holders. These slits are used
to control the height of the diffracted beam as seen by the detector and to reduce the background intensity.

0.19 mm). These slits can be fitted into both the rotatable slit holders.

A beam width mask with a 1 mm opening is supplied as part of the triple axis and rocking curve attachment. It
can be fitted into both the rotatable slit holders. This mask is used to control the width of the diffracted beam as
seen by the detector.

A metal rod is supplied with the triple axis and rocking curve attachment to rotate the receiving slits through
small angles. How to use this rod is described in Chapter 16 (section 16.4.1.2.1) in Part II of this User’s Guide.
Page 19.18 07.03.27

A PW3011/20 Proportional Detector can be mounted behind both the rocking curve and the triple axis beam
paths in the detector interfaces which hold the detector in place by means of two spring-loaded balls.
We advise you to use the triple axis and rocking curve attachment with two PW3011/20 Detectors mounted.

A PW3018/00 PIXcel detector, equipped with a PW3017/60 Interface, can be mounted behind both the triple-
axis and rocking curve beam paths in the detector interface which holds the detector in place by means of two
spring-loaded balls. To mount the detector, slide it into the interface until it clicks into position.

The PW3087/6x Automatic Beam Attenuator can be mounted on the front of the triple axis and rocking curve
attachment and used in place of the foil described in section 2.2.1 in Chapter 2 of Part II of this User’s Guide.
The attenuation factor is entered in the data collector software and is used to automatically adjust the measured
intensity values. More information about the automatic beam attenuator is given in Part II - Chapter 2, section
2.2.2.
CAUTION When an automatic beam attenuator is mounted onto a triple axis and
rocking curve attachment, the maximum 2θ angle of the diffracted beam
arm is restricted. Use the data collector software to set a lower maximum
2θ angle in order to avoid a collision between the automatic beam
attenuator and the tube shield.
19.5.2.1.7.1 Mounting the Automatic Beam Attenuator onto the Triple Axis and Rocking Curve
Attachment
1. Remove the three screws at the back (metal part) of the PW3087/6x Automatic Beam Attenuator (see
Figure 2.2).
2. Split the automatic beam attenuator apart, the metal part from the painted part. This can be quite difficult
to do, persevere.
3. Fit the metal part (NOT the side with the alignment pins) onto the triple axis and rocking curve
attachment; line it up with the slit of the automatic beam attenuator to the slit in one of the beam paths
and ensure that the four screw holes line up. Use the four screws supplied with the automatic beam
attenuator and secure it into place.
07.03.27 Page 19.19

Figure 19.14: PW3087/6x Automatic Beam Attenuator Mounted onto an Asymmetric

Triple Axis and Rocking Curve Attachment
19.5.2.2 Use
19.5.2.2.1 High Resolution Reciprocal Space Maps
High resolution reciprocal space maps can be recorded on an X’Pert PRO MRD system as follows:
Monochromator.
Diffracted beam optics: PW3120/65 Asymmetric Triple Axis and Rocking Curve Attachment.

1. Using the rocking curve beam path find a reflection using the Reciprocal Space Map option in the data
collector software.
3. Move ω to the peak position.
4. Move 2θ to the peak position using the triple axis beam path (change detector position if necessary).
5. Record an area map in using a 2-axes scan program (omega-2theta and omega).
Page 19.20 07.03.27

Chapter 20
Anti-scatter Devices
Contents
20.1 General............................................................................................................................... 20 - 3
20.1.1 Applications......................................................................................................................... 20 - 3
20.1.1.1 Para-focusing Geometries.................................................................................... 20 - 3
20.1.1.2 Capillary Samples ................................................................................................ 20 - 3
20.1.1.3 Transmission Diffraction and High-throughput Applications ............................. 20 - 3
20.1.1.4 Microdiffraction................................................................................................... 20 - 3
20.2 Incident Beam Anti-scatter Devices ................................................................................ 20 - 4
20.2.1 PW3086/00 Incident Beam Anti-scatter Slit Holder for Divergence Slit ........................... 20 - 4
20.2.1.1 Accessories .......................................................................................................... 20 - 5
20.2.2 PW3086/60 Incident Beam Anti-scatter Slit Holder for X-ray Mirror ............................... 20 - 6
20.2.2.1 Accessories .......................................................................................................... 20 - 7
20.2.2.2 Use ....................................................................................................................... 20 - 7
20.2.3 PW3086/65 Incident Beam Anti-scatter Slit Holder for Hybrid Monochromator .............. 20 - 8
20.2.3.1 Accessories .......................................................................................................... 20 - 8
20.2.3.2 Use ....................................................................................................................... 20 - 9
20.2.4 PW3086/70 Incident Beam Anti-scatter Device for Focusing Mirror ................................ 20 - 9
20.2.4.1 Accessories ........................................................................................................ 20 - 11
20.2.4.2 Use ..................................................................................................................... 20 - 12
20.2.5 PW3086/75 Incident Beam Anti-scatter Device for Focusing X-ray Mirror .................... 20 - 16
20.2.5.1 Accessories ........................................................................................................ 20 - 16
20.3 Diffracted Beam Anti-scatter Devices........................................................................... 20 - 18
20.3.1 PW3x94/30 Fixed Anti-scatter Slits for X'Celerator......................................................... 20 - 18
20.3.1.1 Accessories ........................................................................................................ 20 - 19
20.3.1.2 Use ..................................................................................................................... 20 - 21
20.3.2 PW3x94/32 Fixed Anti-scatter Slit for Non-ambient Chambers and MRD...................... 20 - 22
20.3.3 PW3x94/35 Fixed Anti-scatter Slit for Capillary and Transmission Applications ........... 20 - 23
20.3.3.1 Replacing the Mylar Foil ................................................................................... 20 - 24
20.3.4 PW3094/50 Fixed Anti-scatter Slits for X'Celerator Monochromator.............................. 20 - 25
20.3.4.1 Use ..................................................................................................................... 20 - 26
20.3.5 PW3490/00 Fixed Anti-scatter Slits for PIXcel ................................................................ 20 - 27
20.3.5.1 Accessories ........................................................................................................ 20 - 28
20.3.5.2 Use ..................................................................................................................... 20 - 30
20.3.6 PW3490/32 Anti-scatter Slit Holder Extension for Non-Ambient and MRD................... 20 - 31
20.3.7 PW3490/50 Fixed Anti-scatter Slit for Monochromator for PIXcel ................................. 20 - 31
20.3.7.1 Use ..................................................................................................................... 20 - 32
07.03.27 Page 20.1

Page 20.2 07.03.27

Part II - Chapter 20: Anti-scatter Devices
20.1 GENERAL
In diffraction experiments X-rays are not only diffracted by the sample but may also be scattered by air, by parts
of the diffractometer, or by the sample holder. When scattered radiation is collected by the detector it may give
rise to an increased background in the diffractogram.
Anti-scatter devices are used in diffraction measurements which utilize an X’Celerator or a PIXcel. They reduce
the intensity of background radiation to a low level. Together with a beam knife just above the sample surface
this ensures that good signal-to-background ratios are obtained in these experiments. If a different type of
detector is used, the task of reducing the background contribution is performed by anti-scatter slits.
Two types of anti-scatter devices are used in X’Pert PRO systems, incident beam and diffracted beam anti-
scatter devices:
• Incident beam anti-scatter devices are mounted directly onto the incident beam PreFIX module that they
are used with. They are described in section 20.2.
• The diffracted beam anti-scatter devices are mounted onto the line detectors (the X’Celerator or the
PIXcel). They are described in section 20.3.
20.1.1 Applications
20.1.1.1 Para-focusing Geometries
In experiments in which measurements must be performed very quickly, for example: recording a phase
transition in non-ambient studies, an X’Celerator or a PIXcel can be used to obtain a diffraction pattern in a
limited amount of time. Anti-scatter devices can be mounted at the divergence slit holder in the incident beam
path.
20.1.1.2 Capillary Samples

Anti-scatter devices are used in capillary sample measurements in which the diffracted intensities are often very
low. An X’Celerator detector or a PIXcel is used in order to have acceptable measurement times for these
measurements. In order to reduce the amount of scattered radiation as much as possible, anti-scatter devices are
mounted onto the incident beam module and on the X’Celerator detector or on the PIXcel. Anti-scatter devices
can also be used to reduce the incident beam size, such that only the sample is irradiated. This is extremely useful
when your capillary is partly filled, or inhomogeneously filled.
20.1.1.3 Transmission Diffraction and High-throughput Applications

In transmission experiments or in high-throughput applications performed in transmission mode, samples,
including tablets, are often mounted between foils or in well-plates covered by foils. These foils contribute to
the amount of background radiation detected due to the X-rays being scattered by the foil material. Anti-scatter
devices in the incident and diffracted beam paths reduce the scattered radiation entering the detector.
They can also be used to reduce the incident beam size so that only the sample is irradiated and not the well-
plate or sample holder.
20.1.1.4 Microdiffraction
In microdiffraction experiments only a small part on the sample is irradiated. Because of the resulting low
intensity of the diffracted beam, an X’Celerator detector or a PIXcel is used to collect the data. In this geometry,
the scattered radiation is reduced by the use of an anti-scatter device mounted onto the detector.
07.03.27 Page 20.3

20.2 INCIDENT BEAM ANTI-SCATTER DEVICES

Three sorts of incident beam anti-scatter device are available in X’Pert PRO systems. Which of the three is used
depends on the incident beam PreFIX module present in the configuration. The relationship between the anti-
scatter device and the PreFIX module on which it can be mounted is given in Table 20.1. Information on their
use is given in the chapters as listed in the table.
Table 20.1: Incident Beam PreFIX Modules that Incident Beam Anti-scatter
Devices can be used with
Type
Anti-scatter Device Used With Chapter
Number
PW3086/00 Anti-scatter Slit Holder for PW3081/60 Programmable Divergence II - 3

Divergence Slit Slit
PW3082/60 Fixed Divergence Slit II - 3
PW3086/60 Anti-scatter Slit Holder for PW3148/6x X-ray Mirror II - 6

X-ray Mirror
PW3086/65 Anti-scatter Slit Holder for PW3149/63 Hybrid Monochromator 2X II - 7

PW3086/7x Anti-scatter Device for PW3152/63 Focusing X-ray Mirror II - 6

Focusing X-ray Mirror
20.2.1 PW3086/00 Incident Beam Anti-scatter Slit Holder for Divergence

Slit
PW3086/00 is an incident beam anti-scatter device for mounting onto a PW3081/60 Programmable Divergence
Slit or onto a PW3082/00 Fixed Divergence Slit. It comprises two incident beam anti-scatter slit holders for
divergence slits, a short one and a long one. The short one is shown in Figure 20.1. These holders incorporate:
• a slot for an incident beam anti-scatter slit
• a beam mask holder.
The PreFIX modules onto which this holder can be mounted are listed in Table 20.1. This table also refers to the
chapter where the mounting instructions are given. We advise you to use the long holder unless it will not
(because of geometric reasons) fit into your diffractometer configuration.
The distance to the X-ray tube’s focus depends on what kind of divergence slit is mounted, and whether you have
a long holder or a short holder mounted, these distances are given in Table 20.2.
Table 20.2: Anti-scatter Slit and Beam Mask Focus Distances
Distance to the X-ray Short Long

Divergence Slit
Tube’s Focus Holder Holder
PW3081/60 Programmable Anti-scatter slit holder 137 mm 155 mm

Divergence Slit
Beam mask 115 mm 115 mm
PW3082/60 Fixed Anti-scatter slit holder 124 mm 143 mm

Divergence Slit
Beam mask 96 mm 96 mm
Page 20.4 07.03.27

20.2.1.1.1 Anti-scatter Slits
A set of eight slits are delivered together with the PW3086/00 Incident Beam Anti-scatter Slit Holder. They are
marked 4º (opening 6.0 mm), 2º (opening 3.0 mm), 1º (opening 1.5 mm), 1/2º (opening 0.75 mm), 1/4º (opening
0.38 mm), 1/8º (opening 0.19 mm), 1/16º (opening 0.1 mm), and 1/32º (opening 0.05 mm). These slits can be
inserted into the slot for anti-scatter slits.
The choice of the anti-scatter slit size to be used during a diffraction experiment is determined by the size of the
divergence slit on the programmable or fixed divergence slit holder. The optimal anti-scatter slit size is twice
that of the divergence slit.
NOTE: If you are using a programmable divergence slit in the automatic mode, make sure that the
maximum slit opening during a measurement is maximum half the size of the anti-scatter slit used.
Figure 20.1: PW3086/00 Incident beam Anti-scatter Holder for Divergence Slits
20.2.1.1.2 Beam Masks
Four beam masks, supplied together with the PW3081/60 Programmable Divergence Slit and the PW3082/60
Fixed Divergence Slit Holder, can be inserted into the beam mask holder on the PW3086/00 Incident Beam Anti-
scatter Slit Holder. They are used to control the axial width of the incident beam, and thus the amount (width)
of the sample irradiated by the X-ray beam.
The four beam mask are marked 5, 10, 15 and 20. The relationship between the marking on the mask (5, 10, 15
and 20) and the irradiated width on the sample is given in Chapter 4 in Part II of this User’s Guide.
07.03.27 Page 20.5

20.2.2 PW3086/60 Incident Beam Anti-scatter Slit Holder for X-ray Mirror
PW3086/60 is an incident beam anti-scatter slit holder for the PW3148/6x X-ray Mirror. It is shown in Figure
20.2. This holder incorporates:
• a metal plate with a lip to block scattered radiation
• a direct beam stop.
The incident beam anti-scatter slit holder is intended for use on X’Pert PRO MPD systems with a goniometer
radius of 240 mm, equipped with a PW3063/00 Capillary Spinner.
Mounting instructions are given in Chapter 6 in Part II of this User’s Guide.
The beam stop is fitted to ensure that it is possible to measure from 3º 2θ onwards without exposing the detector
to the direct beam.
Slot for
Soller Slits
Direct Beam
Stop
Incident Beam
Anti-scatter Slit
Metal Plate Black

with Lip Knurled Knob
Figure 20.2: PW3086/60 Anti-scatter Slit Holder for X-ray Mirror
CAUTION
The beam stop is factory aligned and must not be moved or
removed.
Page 20.6 07.03.27

Two slits, marked 1/2º and 1/4º, are supplied together with the PW3086/60 Incident Beam Anti-scatter Slit
Holder for X-ray mirror. These slits can be inserted into the slot for anti-scatter slits. They are used to control
the irradiated height on the capillary sample.
The choice of the anti-scatter slit to be used during a measurement depends on the diameter of the glass capillary.
The relationship between the diameter of the capillary sample and the anti-scatter slit to be used is given in Table
20.3.
Table 20.3: Relationship between Capillary Diameter

and Anti-scatter Slit Size
Capillary
Anti-scatter
Diameter
Slit Size
(mm)
0.3 1/4º
0.5 1/2º
Soller slits are used together with the X-ray mirror in order to control the axial acceptance of the incident beam
emerging from the mirror. Four sizes of Soller slits are available for X’Pert PRO systems, they are:
• PW3085/10 0.01 rad Soller Slits
• PW3085/80 0.08 rad Soller Slits.
Soller slits must be inserted into the slot for Soller slits on the anti-scatter slit holder (Figure 20.2). To do this,
insert the Soller slits assembly into the slot until it clicks into place. For more information about Soller slits refer
to Chapter 5 in Part II of this User’s Guide.
20.2.2.2 Use
The metal plate with a lip (Figure 20.2) can be shifted back and forth along the incident beam. Its optimum
position is when it blocks the scattered radiation as much as possible but does not block the diffracted beam.
When the maximum 2θ angle in the scan is low (<90º) the metal plate can be shifted towards, or even over the
capillary sample as much as possible. For high maximum 2θ angles the plate must be shifted back towards the
X-ray tube in order to avoid blocking the diffracted beam.
To shift the metal plate, proceed as follows:

1. Unscrew the two screws with the black knurled knobs.
2. Shift the metal plate to the required position.
3. Lock the metal plate into position by tightening the two screws loosened in step 1.
07.03.27 Page 20.7

20.2.3 PW3086/65 Incident Beam Anti-scatter Slit Holder for Hybrid

Monochromator
PW3086/65 is an incident beam anti-scatter slit holder for the PW3149/63 Hybrid Monochromator 2X or the
PW3150/63 Hybrid Monochromator 4X. It is shown in Figure 20.3. This holder incorporates:
• a direct beam stop.
The incident beam anti-scatter slit holder is intended for use on X’Pert PRO MPD systems with a goniometer
radius of 240 mm, equipped with a PW3063/00 Capillary Spinner.
Mounting instructions are given in Chapter 7 in Part II of this User’s Guide.
The beam stop is fitted to ensure that it is possible to measure from 3º 2θ onwards without exposing the detector
to the direct beam.
CAUTION
The beam stop is factory aligned and must not be moved or
removed.
Two slits, with sizes 1/4º and 1/2º, are supplied together with the PW3086/65 Incident Beam Anti-scatter Slit
Holder for Hybrid Monochromator. These slits can be inserted into the slot for anti-scatter slits. They are used
to control the irradiated height on the capillary sample.
The choice of the anti-scatter slit to be used during a measurement depends on the diameter of the glass capillary.
The relationship between the diameter of the capillary sample and the anti-scatter slit to be used is given in Table
20.3.
Soller slits are used together with the hybrid monochromator in order to control the axial divergence of the
incident beam emerging from the monochromator. Four sizes of Soller slits are available for X’Pert PRO
systems, they are:
Soller slits must be inserted into the slot for Soller slits on the anti-scatter slit holder (Figure 20.3). To do this,
insert the Soller slits assembly into the slot until it clicks into place. For more information about Soller slits refer
to Chapter 5 in Part II of this User’s Guide.
Page 20.8 07.03.27

20.2.3.2 Use
When the maximum 2θ angle in the scan is low (<90º) the metal plate can be shifted towards, or even over the
capillary sample as much as possible. For high maximum 2θ angles the plate must be shifted back towards the
X-ray tube in order to avoid blocking the diffracted beam.
To shift the metal plate, proceed as follows:

2. Shift the metal plate to the required position.
Slot for Soller

Slits
Direct
Beam Stop
Incident Beam
Anti-scatter Slit
Metal Plate Black
with Lip Knurled Knob
Figure 20.3: PW3086/65 Incident Beam Anti-scatter Slit Holder for Hybrid Monochromator
20.2.4 PW3086/70 Incident Beam Anti-scatter Device for Focusing Mirror

PW3086/70 is an incident beam anti-scatter slit holder for the PW3152/63 Focusing X-ray Mirror. It is shown
in Figure 20.4. This holder incorporates:
• a slot for a beam mask
• a direct beam stop assembly.
The incident beam anti-scatter slit holder is intended for use on X'Pert PRO MPD systems with a goniometer
radius of 240 mm, equipped with a PW3063/00 Capillary Spinner, a PW3076/00 Transmission Spinner or a
PW3077/00 High-throughput Attachment.
Mounting instructions and use of the PW3086/70 Anti-scatter Device are given in Chapter 6 in Part II of this
User's Guide.
07.03.27 Page 20.9

Figure 20.4: PW3086/70 Incident Beam Anti-scatter Device for Focusing X-ray Mirror
The beam stop is adjustable in height to allow an optimal blocking of the direct beam so that the minimum 2theta
angle in a diffractogram can be as low as possible. The beam stop assembly can be mounted in either of two
positions onto the anti-scatter device:
• One position is for use when the focusing X-ray mirror is used in combination with the PW3063/00
Capillary Spinner. It allows measurements from 1º 2θ onwards without exposing the detector to the
direct beam.
• The other position is for use with the PW3076/00 Transmission Spinner. In this case, the beam stop is
only used if you want to perform measurements with the lowest 2θ angles being between 1° and 2.5°. If
the beam stop is not mounted, the lowest 2θ angle in a measurement is 2.5°.
A special direct beam stop is delivered with the Oxford Cryosystems Cryostream Plus. This beam stop is used
with the focusing X-ray mirror for measurements on capillary samples at non-ambient temperatures, see also:
section 13.4.1.4 in Chapter 13 of Part II of this User’s Guide.
Mounting of the beam stop onto the anti-scatter device and alignment instructions are given in section 20.2.4.2.
Page 20.10 07.03.27

Two slits, marked 1/2º and 1/4º, are supplied together with the PW3086/70 Incident Beam Anti-scatter Device
for Focusing X-ray mirror. These slits can be inserted into the slot for anti-scatter slits. They are used to control
the irradiated height on the capillary sample. If you want to make use of the full beam coming off the focusing
X-ray mirror, you must use the 1/2° slit. You use the 1/4° slit when you are working with thin capillaries or if
you want to measure at very low angles, close to 1° 2theta. In this case it is also advisable to insert a 1/4° slit
into the slot for the equatorial slit on the focusing X-ray mirror module. The relationship between the diameter
of the capillary sample and the anti-scatter slit to be used is given in Table 20.4.
Table 20.4: Relationship between Capillary Diameter and Anti-scatter Slit Size
Capillary
Anti-scatter
Diameter
Slit Size
(mm)
0.3 1
/4º
0.5 1/ º
2

emerging from the mirror. Three sizes of Soller slits are available for focusing X-ray mirrors, they are:
Soller slits must be inserted into the slot for Soller slits on the anti-scatter device (Figure 20.4). To do this, insert
the Soller slits assembly into the slot until it clicks into place. For more information about Soller slits refer to
20.2.4.1.3 PW3089/00 Beam Mask Set

The distance between the X-ray tube's focus and the beam mask is 204 mm. Table 20.5 shows the relationship
between the various masks positioned in the slot for the mask in the Soller slits holder and the amount of the
sample irradiated, when used in combination with 0.04 rad, 0.02 rad and 0.01 rad Soller slits. The beam mask
must be installed into the slot for beam masks or in the anti-scatter device (see Figure 20.4).
Table 20.5: Relationship between Beam Masks and Irradiated Width
0.04 rad 0.02 rad 0.01 rad

Mask
Soller Slits Soller Slits Soller Slits
20 22.9 mm 12.9 mm 20.7 mm
10 12.9 mm 11.4 mm 10.7 mm
4 6.9 mm 5.4 mm 4.7 mm
2 4.9 mm 3.4 mm 2.7 mm
07.03.27 Page 20.11

20.2.4.2 Use
20.2.4.2.1 Mounting the Beam Stop Assembly
The beam stop assembly can be mounted in two different positions onto the PW3086/70 Anti-scatter Device.
The position onto which the beam stop needs to be mounted depends on the sample stage that the focusing
X-ray mirror is being used with.
• When the anti-scatter device is used in combination with the PW3063/00 Capillary Spinner, the beam
stop must be mounted in the position nearest to the X-ray tube (see Figure 20.5). A special direct beam
stop must be mounted when the capillary spinner is used in combination with the Cryostream Plus for
non-ambient experiments (see Figure 20.6).
• When the anti-scatter device is used in combination with the PW3076/00 Transmission Spinner, the
beam stop must be mounted in the position farthest away from the X-ray tube (see Figure 20.7).
Proceed as follows to mount the beam stop onto the PW3086/70 Anti-scatter Device:
1. Bring the beam stop assembly into the required position on the anti-scatter device, such that the screw
holes in the anti-scatter device are visible through the holes in the beam stop assembly. Refer to Figure
20.5 and Figure 20.7 for the two positions that the beam stop can be mounted onto.
2. Fix the beam stop assembly to the anti-scatter device using the two M3x10 screws supplied.
Figure 20.5: Focusing X-ray Mirror and PW3086/70 Incident Beam Anti-scatter Device with
Beam Stop Assembly Mounted for use with PW3063/00 Capillary Spinner
Page 20.12 07.03.27

Beam Stop Assembly Mounted for use with PW3063/00 Capillary Spinner in combination with the
Cryostream Plus
Beam Stop Assembly Mounted for use with PW3076/00 Transmission Spinner
07.03.27 Page 20.13


The beam stop is adjustable in height and should be aligned as follows:
1. If there is a sample mounted, remove it from the sample stage.
3. Ensure that the direct X-ray beam passes through 2θ = 0°. Use a beam attentuator to protect your
detector from saturation; also make sure that the X-ray beam is not blocked (even partially) by a beam
stop or the sample stage.
5. Mount the anti-scatter device including the beam stop assembly onto the focusing X-ray mirror.
6. Mount the focusing X-ray mirror onto the incident beam PreFIX position of the X'Pert PRO MPD
system.
7. Insert a 1/2° divergence slit, a 1/2° or 1/4° anti-scatter slit that you are going to use in your experiments,
and a 0.04 rad or smaller Soller slits assembly into their appropriate positions in the focusing X-ray
mirror.
8. If you are using an X'Celerator or PIXcel, set it to scanning mode; if you are using a PW3093/60
Programmable Receiving Slit, set it to 0.1 mm. If a programmable anti-scatter slit is mounted onto the
X'Celerator, the PIXcel or the programmable receiving slit, set it to 1/32°. If you have a fixed anti-scatter
device mounted onto the X’Celerator or PIXcel, use the advised combinations as given in Table 6.12
and Table 6.13 respectively.
9. Set ω = 0° and make a 2θ scan around 2θ = 0°, for example: from -1° to 3° 2θ use the same scan type
and omega-offset as used in the experiments that you are going to perform. A typical result of this scan
is shown in Figure 20.8.
Intensity [cps]
3600
1600
400
0
-0.8 -0.6 -0.4 -0.2 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0 2.2 2.4 2.6 2.8
2theta [deg.]
Figure 20.8: Typical scan around 2θ = 0°
Page 20.14 07.03.27


a. If your scan shows a narrow peak around 0.7° 2θ and a flat background from 1° 2θ upwards (the
minimum 2θ from where you can start your measurement) as is shown in Figure 20.8 your beam
stop is correctly aligned and you can skip steps 11 to 13 below.
c. If your scan shows a broad line or an irregular background around 2° 2θ then your beam stop is set
too low and must be raised.
12. Depending on the result obtained in step 10, select one of the situations below:
a. In order to lower the beam stop: Loosen the upper setscrew by turning it with a 1.5 Allen key about
45° (or less for smaller steps) and tighten the lower setscrew by the same amount. Make a new scan
with the same settings as in step 9 and repeat this procedure until your scan looks like the scan
b. In order to raise the beam stop: Loosen the lower setscrew by turning it with a 1.5 Allen key about
45° (or less for smaller steps) and tighten the upper setscrew by the same amount. Make a new scan
with the same settings as in step 9 and repeat this procedure until your scan looks like the scan
20.2.4.2.3 Positioning of the Metal Plate with Lip

When the maximum 2θ angle in the scan is low (<90º) the metal plate can be shifted towards or even over the
capillary sample as much as possible. For high 2θ angles the plate must be shifted back towards the X-ray tube
in order to avoid blocking the diffracted beam.
Proceed as follows to move the metal plate:

2. Slide the metal plate to the required position.
Proceed as follows to remove the metal plate:

2. Remove the metal plate.
07.03.27 Page 20.15

20.2.5 PW3086/75 Incident Beam Anti-scatter Device for Focusing X-ray

Mirror
PW3086/75 is an incident beam anti-scatter slit holder for the PW3152/63 Focusing X-ray Mirror. It is shown
in Figure 20.9. This holder incorporates:
• a slot for a beam mask.
The incident beam anti-scatter slit holder is intended for use on X'Pert PRO MPD systems with a goniometer
radius of 240 mm, equipped with a PW3064/60 Reflection-transmission Spinner used in transmission mode.
Mounting instructions and use of the PW3086/75 Anti-scatter Device are given in Chapter 6 in Part II of this
User's Guide.
Figure 20.9: PW3086/75 Incident beam Anti-scatter Device for Focusing X-ray Mirror
A direct beam stop is not included. Measurements can be performed with a lowest 2θ angle of 2.5°. If a 2θ angle
below 2.5° (to a minimum of 1°) is required in a measurement, the PW3064/20 Direct Beam Stop must be
mounted onto the reflection-transmission spinner. More information about this beam stop is given in Chapter 12
of Part II of this User's Guide.
Two slits, marked 1/2º and 1/4º, are supplied together with the PW3086/75 Incident Beam Anti-scatter Device
for Focusing X-ray mirror. These slits can be inserted into the slot for anti-scatter slits. They are used to control
the irradiated height on the sample. If you want to make use of (almost) the full beam coming from the focusing
X-ray mirror, you must use the 1/2° slit. You can use the 1/4° slit when you are working with thin capillaries or
when you want to measure at very low angles, close to 1° 2θ. In this case it is also advisable to insert a 1/4° slit
in the slot for the equatorial slit on the focusing X-ray mirror module.
Page 20.16 07.03.27

The relationship between the anti-scatter slit size and the irradiated height on the sample is given in Table 20.6.
Table 20.6: Relationship between Anti-scatter Slit Size and Irradiated Height on the Sample
Anti-scatter Irradiated
Slit Size Height (mm)
1/ ° 0.7
2
1 °
/4 0.4
emerging from the mirror. Three sizes of Soller slits are available for focusing X-ray mirrors, they are:
Soller slits must be inserted into the slot for Soller slits on the anti-scatter device (Figure 20.9). To do this, insert
the Soller slits assembly into the slot until it clicks into place. For more information about Soller slits refer to
20.2.5.1.3 PW3089/00 Beam Mask Set
The distance between the X-ray tube's focus and the beam mask is 167 mm. Table 20.7 shows the relationship
between the various masks positioned in the slot for the mask in the Soller slits holder and the amount of the
sample irradiated, when used in combination with 0.04 rad, 0.02 rad and 0.01 rad Soller slits. The beam mask
must be installed into the slot for beam masks in the anti-scatter device (see Figure 20.9).
Table 20.7: Relation between Beam Masks and Irradiated Width
0.04 rad 0.02 rad 0.01 rad

Mask
Soller Slits Soller Slits Soller Slits
20 25.8 mm 22.9 mm 21.5 mm

10 15.8 mm 12.9 mm 11.5 mm
4 9.8 mm 6.9 mm 5.5 mm
2 7.8 mm 4.9 mm 3.5 mm
07.03.27 Page 20.17

20.3 DIFFRACTED BEAM ANTI-SCATTER DEVICES

Seven types of diffracted beam anti-scatter device are available for X'Pert PRO systems. They are:
• PW3x94/30 Fixed Anti-scatter Slits for the X'Celerator. This is described in section 20.3.1.
• PW3x94/32 Fixed Anti-scatter Slit for X'Celerator used in combination with Anton Paar non-ambient
chambers or the MRD cradle. This is described in section 20.3.2.
• PW3x94/35 Fixed Anti-scatter Slit for X'Celerator or the PIXcel used in combination with the
PW3063/00 Capillary Spinner, the PW3064/60 Reflection-transmission Spinner, the PW3076/00
Transmission Spinner or the PW3077/00 High-throughput Attachment. This is described in section
20.3.3.
• PW3094/50 Fixed Anti-scatter Slits for the X'Celerator used in combination with the PW3122/00
Monochromator. This is described in section 20.3.4.
• PW3490/00 Fixed Anti-scatter Slits for the PIXcel. This is described in section 20.3.5.
• PW3490/32 Fixed Anti-scatter Extension for the PIXcel used in combination with Anton Paar
non-ambient chambers or the MRD cradle. This is described in section 20.3.6.
• PW3490/50 Fixed Anti-scatter Slits for the PIXcel used in combination with the
PW3124/00 Monochromator. This is described in section 20.3.7.
The PW3091/x0 Programmable Anti-scatter Slit and its use in combination with the PW3093/60 Programmable
Receiving Slit and with the X'Celerator is described in section 16.2.2 of Chapter 16 of this User's Guide.
20.3.1 PW3x94/30 Fixed Anti-scatter Slits for X'Celerator

The PW3x94/30 Fixed Anti-scatter Slits are inserted into the diffracted beam path in order to reduce the
influence of X-rays that are scattered by air along the beam path. Six anti-scatter slits marked 13, 8.7, 6.6, 5.5, 5
and 0.2 are delivered with the PW3x94/30 Fixed Anti-scatter Slits. This set of slits and the slit holder are shown
in Figure 20.10. The anti-scatter slit holder can be mounted onto the PW3014/00 Interface for X'Celerator as is
shown in Figure 21.5. The mounting of this holder is described in section 21.4.3.6.1 in Chapter 21 in Part II of
this User's Guide. For use on an X’Pert PRO MRD system or with Anton Paar non-ambient chambers, the fixed
anti-scatter slits holder must be extended with the PW3x94/32 Fixed Anti-scatter Slits Holder Extension.
Selection of anti-scatter slit size related to the divergence slit setting for symmetrical scan conditions is given in
section 20.3.1.2.1.
NOTE: The Fixed Anti-scatter Slits for X'Celerator are available in two versions: PW3094/30 and
PW3494/30. If you have a PW3064/60 Reflection-transmission Spinner or a PW3077/00
High-throughput Attachment mounted on your goniometer you must use the PW3494/30
Fixed Anti-scatter Slits. If you are using another sample stage, you can either use PW3094/30 or
PW3494/30 Fixed Anti-scatter Slits.
Page 20.18 07.03.27

CAUTIONS 1. If you have mounted a diffracted beam anti-scatter slit holder onto
the X'Celerator, be careful to avoid collisions between the diffracted
beam anti-scatter slit holder and the sample stage or the sample itself.
2. The X'Pert PRO system automatically resets when the system is
switched on or when power is restored after a power failure. The reset
procedure involves driving the goniometer back to its hardware zero
points, which may cause collisions between the sample or the sample
stage and the diffracted beam anti-scatter slit holder. You should
disable this automatic reset using the data collector software in cases
where collisions are possible. This activates an initialization wizard
that guides you through the initialization procedure. You then have
the opportunity to remove the diffracted beam anti-scatter slit holder
before resetting the system.
Figure 20.10: PW3x94/30 Fixed Anti-scatter Slits for X'Celerator and Slit Holder
20.3.1.1.1 PW3x94/32 Anti-scatter Slit for Non-ambient Chambers and MRD
The PW3x94/32 Anti-scatter Slit must be mounted in the diffracted beam path when the X'Celerator is used in
the combination with Anton Paar non-ambient chambers or an X’Pert PRO MRD system, in order to reduce the
amount of scattered radiation entering the detector. The slits delivered with the fixed anti-scatter slits holder can
also be into the slot on the extension block. Information about this anti-scatter slit is given in section 20.3.2.
07.03.27 Page 20.19

20.3.1.1.1.1 Mounting the PW3x94/32 Anti-scatter Slit
The Anti-scatter slit must be mounted onto the fixed anti-scatter slits holder for the X'Celerator. Proceed as
follow to mount the anti-scatter slit:
1. Bring the PW3x94/32 Anti-scatter Slit into position, so that the two pins on this device fit into the
corresponding holes at the front of the anti-scatter slit holder.
2. Insert and tighten the two M3 x 8 screws supplied, as shown in Figure 20.11.
3. You can now insert the 3.4 mm slit supplied in the slot at the front of the PW3x94/32 Anti-scatter Slit.
Figure 20.11: PW3x94/32 Fixed Anti-scatter Slit mounted onto PW3x94/30 Fixed Anti-scatter Slits
Holder for X'Celerator
20.3.1.1.2 PW3x94/35 Fixed Anti-scatter Slit for Capillary and Transmission Applications
The PW3x94/35 Fixed Anti-scatter Slit must be mounted in the diffracted beam path when the X'Celerator is
used in the combination with the PW3063/00 Capillary Spinner, the PW3064/60 Reflection-transmission
Spinner, the PW3076/00 Transmission Spinner or the PW3077/00 High-throughput Attachment, in order to
reduce the amount of scattered radiation entering the detector. Information about this anti-scatter slit is given in
section 20.3.3.
Page 20.20 07.03.27

20.3.1.1.2.1 Mounting the PW3x94/35 Fixed Anti-scatter Slit
The Fixed Anti-scatter slit must be mounted onto the Fixed Anti-scatter Slits Holder for the X'Celerator. Proceed
as follows to mount the anti-scatter slit:
1. Bring the PW3x94/35 Anti-scatter Slit into position, so that the two pins on this device fit into the
Figure 20.12: PW3x94/35 Fixed Anti-scatter Slit mounted onto PW3x94/30 Fixed Anti-scatter Slits
Holder for X'Celerator
20.3.1.2 Use
20.3.1.2.1 Reflection mode
When the diffractometer is to be used to record data about flat polycrystalline samples under symmetrical scan
conditions in reflection mode (a gonio scan), in other words: omega = 2theta/2, you should choose a diffracted
beam anti-scatter slit that matches the chosen divergence slit size. Symmetrical scan conditions are used for most
powder applications: phase identification, quantification and crystallography. The optimum combinations of
divergence slits and anti-scatter slits related to the X’Pert PRO system use are given in Table 20.8.
If asymmetrical scan conditions are used on a flat powder sample, we advise you to use the PW3x94/30 Fixed
Anti- scatter Slits Holder without a slit inserted. A typical example of this would be residual stress analysis using
the omega-offset method.
07.03.27 Page 20.21

Table 20.8: Relationship between X'Pert PRO system, Anti-scatter Slit Holder, Divergence Slit Size and
Anti-scatter Slit Size for Symmetrical Scan Conditions
X'Pert PRO MPD

X'Pert PRO with non-
X'Pert PRO system X'Pert PRO MRD
MPD ambient
chamber
PW3x94/30 with PW3x94/30 with

Anti-scatter Slit Holder PW3x94/30
PW3x94/32 PW3x94/32
Anti-scatter Anti-scatter Slit Anti-scatter Slit

Divergence Slit Size (°)
Slit Size (mm) Size (mm) Size (mm)
4 13 No slit inserted No slit inserted

2 8.7 8.7 13
1 6.6 6.6 8.7

1/ 5.5 5.0 6.6
2
1/ 5.0 5.0 5.5

4
1
/8 and smaller 5.0 3.4 5.0
For alignment purposes 0.2 0.2 0.2
NOTE: The 3.4 mm slit is part of PW3x94/32 Fixed Anti-scatter Slit. It is used in combination with a 1/8°
divergence slit and Anton Paar non-ambient chambers to measure at 2theta angles below 10°. More
information is given in section 20.3.2.
20.3.1.2.2 Transmission Mode
When you are using the diffractometer in transmission mode and employing a focusing X-ray mirror, you should
choose a diffracted beam anti-scatter slit of 6.6 mm or smaller. If you are working with the PW3015/20
X'Celerator Scientific in static mode, we advise you to use the 6.6 mm slit.
20.3.2 PW3x94/32 Fixed Anti-scatter Slit for Non-ambient Chambers

and MRD
The PW3x94/32 is a diffracted beam anti-scatter slit for the X'Celerator with PW3x94/30 Fixed Anti-scatter Slits
used in combination with one of the following Anton Paar non-ambient chambers: HTK 1200N, TTK 450, THC
and XRK 900. It is used to suppress the peak around 6° 2theta, resulting from scatter of the incident X-ray beam
at the window of the non-ambient chamber. The delivery comprises a slit holder and a 3.4 mm slit. The holder
and its slit are shown in Figure 20.13. The slit size corresponds to an anti-scatter slit of 1/8° when it is inserted
in the slot at the entrance of the slit holder. The slit holder has to be mounted onto the PW3x94/30 Fixed Anti-
scatter Slit Holder for the X'Celerator.
NOTE: The Fixed Anti-scatter Slits for Non-ambient Chambers are available in two versions: PW3094/32
and PW3494/32. Depending on the type of Fixed Anti-scatter Slit for X'Celerator that you have
(PW3094/30 or PW3494/30), you must use PW3094/32 or PW3494/32 respectively.
Page 20.22 07.03.27

Instructions on how to mount the PW3x94/32 Fixed Anti-scatter Slit onto the X'Celerator's anti-scatter slit
holder are given in section 20.3.1.1.1.1. Information about the use of the anti-scatter slit with the X'Celerator is
Figure 20.13: PW3x94/32 Fixed Anti-scatter Slit for Non-ambient Chambers
20.3.3 PW3x94/35 Fixed Anti-scatter Slit for Capillary and Transmission

Applications
The PW3x94/35 Fixed Anti-scatter Slit for Capillary and Transmission Applications is a diffracted beam anti-
scatter slit for the X'Celerator with PW3x94/30 Fixed Anti-scatter Slits or the PIXcel with fixed anti-scatter slits
used in combination with one of the following stages: PW3063/00 Capillary Spinner, the PW3064/60
Reflection-transmission Spinner, the PW3076/00 Transmission Spinner and the PW3077/00 High-throughput
Attachment. It is used to reduce the amount of scattered radiation entering the detector in measurements on
samples in glass capillaries or between foils.
The delivery consists of a slit holder onto which a slit with a slit opening of 2.5 mm (height) x 30 mm (width)
is mounted. The slit holder and the slit are shown in Figure 20.14. The entrance of the slit is covered by a
removable Mylar foil (6 µm thick). It can be replaced with a new one when necessary. The Mylar foil is to be
used when the PW3063/00 Capillary Spinner is equipped with a Huber capillary heater.
NOTE: The Fixed Anti-scatter Slits for Capillary and Transmission Applications are available in two
versions: PW3094/35 and PW3494/35. Depending on the type of Fixed Anti-scatter Slit for
X'Celerator that you have (PW3094/30 or PW3494/30), you must use PW3094/35 or PW3494/35
respectively.
07.03.27 Page 20.23

Figure 20.14: PW3x94/35 Fixed Anti-scatter Slit for Capillary and Transmission Applications
The slit holder has to be mounted onto the PW3x94/30 Anti-scatter Slit Holder for the X'Celerator or onto the
PW3490/00 Anti-scatter Slit Holder for the PIXcel. Instructions on how to mount the PW3x94/35 Anti-scatter
Slit onto the anti-scatter slit holder are given in sections 20.3.1.1.2.1 for the X’Celerator, or 20.3.5.1.2.1 for the
PIXcel. Information about the use of the anti-scatter slit in combination with the X'Celerator or PIXcel are given
in Chapter 21 of this User's Guide in sections 21.4 and 21.5 respectively.
NOTE: When you are using the PW3076/00 Transmission Spinner, the PW3x94/35 Fixed Anti-scatter Slit
cannot be used in combination with the direct beam stop of the PW3086/70 Anti-scatter Slit Holder
for Focusing X-ray Mirror.
20.3.3.1 Replacing the Mylar Foil

The Mylar foil at the slit holder's entrance can be replaced when necessary. Proceed as follows to do so:
1. Unscrew the two screws that hold the slit onto the slit holder (see Figure 20.15).
2. Replace the Mylar foil with a new one.
Put the slit back into its position in front of the slit holder and secure it into place with the two screws.
Page 20.24 07.03.27

Figure 20.15: Replacing the Mylar foil of the PW3x94/35 Fixed Anti-scatter Slit
20.3.4 PW3094/50 Fixed Anti-scatter Slits for X'Celerator Monochromator

The PW3094/50 Fixed Anti-scatter Slits used with the Monochromator for X'Celerator are inserted in the
diffracted beam path in order to reduce the influence of X-rays that are scattered by air along the beam path. Five
anti-scatter slits marked: 8.6 mm, 5.9 mm, 4.6 mm, 3.9 mm and 0.2 mm are delivered with the PW3094/50 Fixed
Anti-scatter Slits. This set of slits and the slit holder are shown in Figure 20.16. The anti-scatter slit holder can
be mounted onto the PW3122/00 Monochromator for X'Celerator. Mounting instructions are given in section
19.4.1.1.1 in Chapter 19 of Part II of this User's Guide. Selection of the anti-scatter slit sizes related to the
divergence slit setting for asymmetric scan conditions is given in section 20.3.4.1.
07.03.27 Page 20.25

Figure 20.16: PW3094/50 Fixed Anti-scatter Slits for Monochromator for X'Celerator and Slit Holder
the X'Celerator, be careful to avoid collisions between the diffracted
beam anti-scatter slit holder and the sample stage or the sample itself.
reset procedure involves driving the goniometer back to its hardware
zero points, which may cause collisions between the sample or the
sample stage and the diffracted beam anti-scatter slit holder. You
should disable this automatic reset using the data collector software
in cases where collisions are possible. This activates an initialization
wizard that guides you through the initialization procedure. You then
have the opportunity to remove the diffracted beam anti-scatter slit
holder before resetting the system.
20.3.4.1 Use
20.3.4.1.1 Reflection Mode
When the diffractometer is used to record data about flat polycrystalline samples under symmetrical scan
powder applications: phase identification, quantification and crystallography. The optimum combination of
divergence slits and anti-scatter slits mounted on the monochromator for X’Celerator are given in Table 20.9.
If asymmetrical scan conditions are used on a flat powder sample, we advise you to use the PW3094/50 Fixed
Page 20.26 07.03.27
Table 20.9: Relationship between Divergence Slit Size and Diffracted Beam Anti-scatter Slit Size for
Symmetrical Scan Conditions
X'Pert PRO system X'Pert PRO MPD X'Pert PRO MRD
Anti-scatter Slit Anti-scatter Slit

Divergence Slit Size (º)
Size (mm) Size (mm)
2 8.6 No slit inserted
1 5.9 8.6
1
/2 4.6 5.9
1
/4 and smaller 3.9 5.9
For alignment purposes 0.2 0.2

When you are using the diffractometer in transmission mode, employing a focusing X-ray mirror, you should
choose a diffracted beam anti-scatter slit of 5.9 mm or smaller. If you are working with the PW3015/20
X'Celerator Scientific in static mode, we advise you to use the 5.9 mm slit.
20.3.5 PW3490/00 Fixed Anti-scatter Slits for PIXcel

The PW3490/00 Fixed Anti-scatter Slits are inserted into the diffracted beam path in order to reduce the
influence of X-rays that are scattered by air along the beam path. Six anti-scatter slits marked P15.4, P11.2, P9.1,
P8, P7.5 and one not marked at all are delivered with the PW3490/00 Fixed Anti-scatter Slits for PIXcel. This
set of slits and the slit holder are shown in Figure 20.17. The anti-scatter slit holder can be mounted onto the
PW3017/00 Interface for PIXcel as is shown in Figure 21.11. The mounting of this holder is described in section
21.5.3.6 in Chapter 21 in Part II of this User's Guide. When it is to be used on X’Pert PRO MRD systems or with
Anton Paar non-ambient chambers the fixed anti-scatter slit holder must be extended with the PW3490/32 Anti-
scatter Slit Holder Extension (see section 20.3.5.1.1). Selection of anti-scatter slit sizes relative to the divergence
slit setting for symmetrical scan conditions is given in section 20.3.5.2.
the PIXcel, be careful to avoid collisions between the diffracted beam
anti-scatter slit holder and the sample stage or the sample itself.
wizard that guides you through the initialization procedure. You
then have the opportunity to remove the diffracted beam anti-
scatter slit holder before resetting the system.
07.03.27 Page 20.27

Figure 20.17: PW3490/00 Fixed Anti-scatter Slits and Slit Holder for PIXcel
20.3.5.1.1 PW3490/32 Anti-scatter Slit Holder Extension for Non-Ambient Chambers & MRD
The PW3490/32 Anti-scatter Slit Holder Extension must be mounted onto the PW3490/00 Fixed Anti-scatter
Slits Holder in the diffracted beam path when the PIXcel is used in combination with Anton Paar non-ambient
chambers or an X’Pert PRO MRD system, in order to reduce the amount of scattered radiation entering the
detector. One slit, marked 5.0, is supplied in the delivery. The slits delivered with the fixed anti-scatter slits
holder can also be inserted into the slot of the extension block. Information about this anti-scatter slit holder
extension is given in section 20.3.6.
Figure 20.18: PW3490/32 Fixed Anti-scatter Slit Holder Extension mounted onto
PW3490/00 Fixed Anti-scatter Slits Holder for PIXcel
Page 20.28 07.03.27
20.3.5.1.1.1 Mounting the PW3490/32 Anti-scatter Slit Holder Extension
The anti-scatter slit holder extension must be mounted onto the fixed anti-scatter slits holder for the PIXcel.
Proceed as follows to mount the anti-scatter slit:
1. Bring the PW3490/32 Anti-scatter Slit into position, so that the two pins on this device fit into the
3. You can now insert a fixed slit in the slot at the front of the PW3490/32 Anti-scatter Slit.
20.3.5.1.2 PW3494/35 Fixed Anti-scatter Slit for Capillary and Transmission Applications
The PW3494/35 Fixed Anti-scatter Slit must be mounted in the diffracted beam path when the PIXcel is used in
the combination with the PW3063/00 Capillary Spinner, the PW3064/60 Reflection-transmission spinner, the
PW3076/00 Transmission Spinner or the PW3077/00 High-throughput Attachment, in order to reduce the
amount of scattered radiation entering the detector. Information about this anti-scatter slit is given in section
20.3.4.
20.3.5.1.2.1 Mounting the PW3494/35 Fixed Anti-scatter Slit
The Fixed Anti-scatter slit must be mounted onto the Fixed Anti-scatter Slits Holder for the PIXcel. Proceed as
follows to mount the anti-scatter slit:
1. Bring the PW3494/35 Anti-scatter Slit into position, so that the two pins on this device fit into the
Figure 20.19: PW3494/35 Fixed Anti-scatter Slit mounted onto PW3490/00 Fixed Anti-scatter Slits
Holder for PIXcel
07.03.27 Page 20.29

20.3.5.2 Use
When the diffractometer is to be used to record data about flat polycrystalline samples under symmetrical scan
conditions in reflection mode (a gonio scan, in other words: omega = 2theta/2, you should choose a diffracted
powder applications: phase identification, quantification and crystallography. The optimum combinations of
divergence slits and anti-scatter slits related to the X’Pert PRO system being used are given in Table 20.10. If
asymmetrical scan conditions are used on a flat powder sample, we advise you to use the PW3490/00 Fixed Anti-
scatter Slits Holder without a slit inserted. A typical example of this would be residual stress analysis using the
omega-offset method.
Table 20.10: Relationship between X'Pert PRO system, Anti-scatter Slit Holder, Divergence Slit Size and
Anti-scatter Slit Size for Symmetrical Scan Conditions
X'Pert PRO MPD

X'Pert PRO X'Pert PRO with non-
X'Pert PRO MRD
system MPD ambient
chamber
Anti-scatter PW3490/00 with PW3490/00 with

PW3490/00
Slit Holder PW3490/32 PW3490/32
Divergence Slit Anti-scatter Anti-scatter Slit Anti-scatter Slit

Size (º) Slit Size (mm) Size (mm) Size (mm)
4 15.4 No slit inserted No slit inserted
2 11.2 11.2 15.4
1 9.1 7.5 11.2

1/ 8.0 7.5 9.1
2
1/ 7.5 7.5 8.0

4
1/
and smaller 7.5 5.0 7.5
8
For alignment 0.2 0.2 0.2

purposes
NOTE: The 5.0 mm slit is part of PW3490/32 Fixed Anti-scatter Slit. It is used in combination with a 1/8°
divergence slit and Anton Paar non-ambient chambers to measure at 2theta angles below 10°. More
information is given in section 20.3.6.
When you are using the diffractometer in transmission mode and employing a focusing X-ray mirror, you should
choose a diffracted beam anti-scatter slit of 9.1 mm or smaller. If you are working with the PIXcel in static mode,
we advise you to use the 9.1 mm slit.
Page 20.30 07.03.27

20.3.6 PW3490/32 Anti-scatter Slit Holder Extension for Non-Ambient

and MRD
The PW3490/32 is an extension for the PW3490/00 Fixed Anti-scatter Slit Holder for the PIXcel to insert the
fixed anti-scatter slit at the correct position in the diffracted beam path. The delivery comprises a slit holder and
a 5.0 mm slit. The holder and its slit are shown in Figure 20.20.
Instructions on how to mount the PW3490/32 Fixed Anti-scatter Slit Holder Extension onto the PIXcel's fixed
anti-scatter slit holder are given in section 20.3.5.1.1.1. Information about the use of the anti-scatter slit with the
PIXcel is given in section 20.3.5.2.
Figure 20.20: PW3490/32 Fixed Anti-scatter Slit Holder Extension for Non-ambient and MRD with
Slit inserted
20.3.7 PW3490/50 Fixed Anti-scatter Slit for Monochromator for PIXcel

The PW3490/50 Fixed Anti-scatter Slits used with the Monochromator for PIXcel are inserted in the diffracted
beam path in order to reduce the influence of X-rays that are scattered by air along the beam path. Six anti-scatter
slits marked: PM15.8, PM10.4, PM7.7, PM6.4, PM5.7 and 0.2 mm are delivered with the PW3490/50 Fixed
Anti-scatter Slits. This set of slits and the slit holder are shown in Figure 20.21. The anti-scatter slit holder can
be mounted onto the PW3124/00 Monochromator for PIXcel. Mounting instructions are given in section
19.4.2.1.1 in Chapter 19 of Part II of this User's Guide. Selection of the anti-scatter slit sizes relative to the
divergence slit setting for asymmetrical scan conditions is given in section 20.3.7.1.
07.03.27 Page 20.31

Figure 20.21: PW3490/50 Fixed Anti-scatter Slits for Monochromator for PIXcel and Slit Holder
the PIXcel, be careful to avoid collisions between the diffracted beam
anti-scatter slit holder and the sample stage or the sample itself.
wizard that guides you through the initialization procedure. You
then have the opportunity to remove the diffracted beam anti-
scatter slit holder before resetting the system.
20.3.7.1 Use
When the diffractometer is used to record data about flat polycrystalline samples under symmetrical scan
powder applications: phase identification, quantification and crystallography. The optimum combination of
divergence slits and anti-scatter slits mounted onto the monochromator for PIXcel are given in Table 20.11.
If asymmetrical scan conditions are used on a flat powder sample, we advise you to use the PW3094/50 Fixed
Page 20.32 07.03.27

Table 20.11: Relationship between X'Pert PRO System, Divergence Slit Size and Anti-scatter Slit Size for
Symmetrical Scan Conditions
X'Pert PRO system X'Pert PRO MPD X'Pert PRO MRD
Anti-scatter Slit Anti-scatter Slit

Divergence Slit Size (º)
Size (mm) Size (mm)
2 10.4 15.8
1 7.7 10.4
1
/2 6.4 10.4
1
/4 5.7 10.4
1/ and smaller 5.7 7.7

8
For alignment purposes 0.2 0.2
When you are using the diffractometer in transmission mode, employing a focusing X-ray mirror, you should
choose a diffracted beam anti-scatter slit of 7.7 mm or smaller. If you are working with the PIXcel in static mode,
we advise you to use the 7.7 mm slit.
07.03.27 Page 20.33

Page 20.34 07.03.27

Chapter 21
Detectors
Contents
21.1 General............................................................................................................................... 21 - 3
21.1.1 Pulse Height Distribution Determination ............................................................................. 21 - 4
21.1.2 Selecting PHD Levels .......................................................................................................... 21 - 5
21.1.3 Escape Peaks ........................................................................................................................ 21 - 5
21.1.3.1 Escape Peaks in a PHD Determination Scan ....................................................... 21 - 5
21.1.3.2 Escape Peaks in the Low Angle Regions of Diffractograms............................... 21 - 6
21.2 Sealed Proportional Detectors ......................................................................................... 21 - 7
21.2.1 PW3011/20 Proportional Detector ....................................................................................... 21 - 8
21.2.1.1 Use ....................................................................................................................... 21 - 8
21.3 Scintillation Detectors....................................................................................................... 21 - 9
21.3.1 PW1964/96 Scintillation Detector........................................................................................ 21 - 9
21.3.1.1 Use ..................................................................................................................... 21 - 10
21.4 RTMS Detector X’Celerator.......................................................................................... 21 - 10
21.4.1 Applications........................................................................................................................ 21 - 10
21.4.1.1 Phase Analysis on Flat Powder Samples ........................................................... 21 - 10
21.4.1.2 Analysis of Samples in Glass Capillaries .......................................................... 21 - 11
21.4.1.3 Micro-diffraction ............................................................................................... 21 - 11
21.4.2 PW3015/x0 X’Celerator..................................................................................................... 21 - 11
21.4.3 Accessories......................................................................................................................... 21 - 13
21.4.3.1 PW3014/00 PreFIX Interface ............................................................................ 21 - 13
21.4.3.2 Beta-filters ......................................................................................................... 21 - 15
21.4.3.3 Attenuation Foil ................................................................................................. 21 - 15
21.4.3.4 PW3085/x1 Soller Slits...................................................................................... 21 - 15
21.4.3.5 PW3091/x0 Programmable Anti-scatter Slit ..................................................... 21 - 16
21.4.3.6 PW3x94/30 Fixed Anti-scatter Slit for X’Celerator .......................................... 21 - 18
21.4.3.7 PW3x94/32 Anti-scatter Slit .............................................................................. 21 - 18
21.4.3.8 PW3x94/35 Anti-scatter Slit .............................................................................. 21 - 18
21.4.3.9 PW3094/50 Fixed Anti-scatter Slit for X’Celerator Monochromator ............... 21 - 19
21.4.3.10 PW3122/00 Diffracted Beam Monochromator for X’Celerator........................ 21 - 19
21.4.4 Use...................................................................................................................................... 21 - 19
21.4.4.1 Selecting PHD Levels ........................................................................................ 21 - 19
21.4.4.2 Operating Modes................................................................................................ 21 - 20
21.4.4.3 Optimizing Measurements with the X'Celerator ............................................... 21 - 20
21.4.4.4 Suppression of Unwanted Radiation.................................................................. 21 - 21
07.12.04 Page 21.1

21.5 Medipix2 Detector PIXcel ..............................................................................................21 - 22

21.5.1 Applications........................................................................................................................ 21 - 22
21.5.1.1 Phase Analysis on Flat Powder Samples ........................................................... 21 - 22
21.5.1.2 Analysis of Samples in Glass Capillaries........................................................... 21 - 22
21.5.1.3 Texture Measurements ....................................................................................... 21 - 22
21.5.1.4 Parallel Beam Measurements ............................................................................. 21 - 22
21.5.1.5 Micro-diffraction................................................................................................ 21 - 23
21.5.1.6 High-resolution Rocking Curves and Reciprocal Space Mapping .................... 21 - 23
21.5.1.7 Reflectivity ......................................................................................................... 21 - 23
21.5.3 Accessories ......................................................................................................................... 21 - 25
21.5.3.1 PW3017/00 PreFIX Interface for PIXcel Used as a Line Detector ................... 21 - 25
21.5.3.2 PW3017/60 Interface for PIXcel Used as a Point Detector ............................... 21 - 26
21.5.3.3 Beta-filters.......................................................................................................... 21 - 27
21.5.3.4 PW3085/x1 Soller Slits ...................................................................................... 21 - 27
21.5.3.5 PW3091/70 Programmable Anti-scatter Slit...................................................... 21 - 27
21.5.3.6 PW3490/00 Fixed Anti-scatter Slit for PIXcel .................................................. 21 - 29
21.5.3.7 PW3490/32 Anti-scatter Slit .............................................................................. 21 - 30
21.5.3.8 PW3494/35 Anti-scatter Slit .............................................................................. 21 - 30
21.5.3.9 PW3490/50 Fixed Anti-scatter Slit for PIXcel Monochromator ....................... 21 - 30
21.5.3.10 PW3124/00 Diffracted Beam Monochromator for PIXcel ................................ 21 - 30
21.5.4 Use ...................................................................................................................................... 21 - 31
21.5.4.1 Selecting PHD Levels ........................................................................................ 21 - 31
21.5.4.2 Operating Modes ................................................................................................ 21 - 31
21.5.4.3 Optimizing Measurements with the PIXcel ....................................................... 21 - 32
21.5.4.4 Suppression of Unwanted Radiation .................................................................. 21 - 32
Page 21.2 07.12.04

Part II - Chapter 21: Detectors
21.1 GENERAL
The X-ray detector is the last item in the X-ray beam path. It is used to count the number of photons, that is, the
intensity of the diffracted beam at a certain 2θ position of the goniometer.
Basically, a detector consists of two parts, a transducer and a pulse forming circuit. The transducer collects the
X-ray photons entering the detector through a window and converts the energies into an electric current. This
current is then converted by the pulse forming circuit into electrical pulses which are counted by the counting
electronics for further processing.
Important characteristics of a detector that are relevant to XRD measurements are: quantum-counting efficiency,
linearity, energy proportionality, energy resolution and sensitivity.
• Quantum-counting efficiency is the ratio of the number of photons detected by the detector to the
number of photons entering the detector.
• Linearity is the ability of the detector to provide an output that is in direct proportion to the intensity of
the X-ray beam, that is the number of X-ray photons entering the detector.
• Energy proportionality is the ability of the detector to produce a pulse with a height proportional to the
energy of the X-ray photon detected.
• Energy resolution is the ability of the detector to distinguish between energies. When an X-ray photon
with a certain energy is detected, it produces an electrical pulse with a certain average voltage. The
spread around this average is related to the energy resolution.
• Sensitivity is the ability of the detector to detect low intensity levels.
There are four types of detector that can be used in X’Pert PRO systems:
• Sealed proportional detectors; sealed chambers filled with a counting gas
• Scintillation detectors; scintillation crystal with a photo multiplier tube
• RTMS detectors; fast X-ray detection system based on Real Time Multiple Strip (RTMS) technology
• Medipix2 detector; fast X-ray detection system with high spatial resolution and a high contrast.
The choice of a detector depends on the wavelength of the radiation of interest, the required speed of the
measurements, the maximum intensity to be measured, and on the acceptable background intensities.
A summary of the properties of the detectors available in X’Pert PRO systems is shown in Table 21.1. The 99%
linearity range as given in this table is defined as the range within which the deviation from the linear
relationship between the incoming and counted X-ray photons is less than 1%. The energy resolution is
determined by the ratio of the Full Width at Half Maximum and the peak position of the pulse height distribution.
More information about the pulse height distribution is given in section 21.1.1.
The energy proportionality is realized by the high voltage control for all detectors.
The maximum count rate defines the maximum intensity of the X-ray beam to which the detector may be
exposed. X-ray beams with a higher intensity than the maximum count rate can easily saturate the detector,
resulting in wrong intensity readouts.
CAUTION
An attenuation foil MUST be mounted into the incident beam or
diffracted beam PreFIX module used in order to attenuate the beam
07.12.04 Page 21.3

Table 21.1: Summary of Detectors
Detector PW3011/20 PW1964/96 PW3015/x0 PW3018/00
Sealed
Scintillation X’Celerator PIXcel
Type Proportional
Detector RTMS Detector Medipix2 Detector
Detector
Window size 20 mm x 24 mm 30 mm diameter 9 mm x 15 mm 14 mm x 14 mm
Efficiency Cu Kα 84% 93% > 94% >94%
Efficiency Mo Kα 36% 99% - -
99% Linearity range 0 - 1000 kcps 0 - 500 kcps 0 - 900 kcps - Overall 0 - 1.3 x 109 cps - Overall
0 - 7000 cps - Local
0 - 5 x 106 cps - Column
Energy resolution 19% 45% 25% 25%

around Cu Kα
Maximum count 1000 kcps 1000 kcps 5000 kcps - Overall >10 x 109 cps - Overall
rate 250 kcps - Local
>50 x 106 cps - Column
Maximum 2 cps 8 cps < 0.1 cps <1 cps - Overall

background <0.01 cps - Column
Active length - - 9 mm 14 mm
Smallest step size - - 0.0021º 2θ at 240 mm 0.0016º 2θ at 240 mm

goniometer radius goniometer radius
0.0016º 2θ at 320 mm 0.0012º 2θ at 320 mm
goniometer radius goniometer radius
21.1.1 Pulse Height Distribution Determination

Fluctuations in the primary conversion from X-ray photons of a certain energy into electrical current result in the
fact that the height of the pulse, produced by the pulse forming circuit, is not constant. These fluctuations result
in a distribution of pulse height, approximating a Gaussian curve. The energy resolution of the detector can be
determined from this distribution.
This pulse height distribution can be determined with the use of the data collector software:
NOTE: A PHD determination scan cannot be performed in conjunction with an X’Celerator or a PIXcel
detector.
1. Start the data collector software.
2. Perform a gonio scan (easiest is a manual scan) in order to obtain some measurement data.
3. When you have measured a peak, move to a position on that peak where the count rate is below
3 000 cps (preferably above 1 000 cps) and use the data collector software to perform “PHD
Determination”.
The pulse height determination is centered around a relative level of 50% of the maximum pulse height,
corresponding to a certain maximum X-ray photon energy.
Page 21.4 07.12.04

21.1.2 Selecting PHD Levels

To select the energy range of the X-ray photons to be detected, you can set the lower and upper detection levels
in the data collector software. Typical PHD levels for a proportional detector are 35% for the lower level and
80% for the upper. Typical PHD levels for the PIXcel detector are 25% for the lower level and 70% for the upper.
Generally, we recommend setting the PHD levels to the factory levels in the data collector software. If the
sample shows strong fluorescence, we recommend that you set the levels to 45% and 80%If the sample shows
strong fluorescence, we recommend that you set the levels to 45% and 80%, but please note that better ways of
reducing the sample fluorescence are either to use a monochromator, or an X-ray tube with a different anode
material.
NOTE: When you replace an X-ray tube with one with a different anode material, the X’Pert PRO system
detector electronics are automatically adjusted to detect the characteristic radiation of the new tube.
This adjustment is performed in such a way that the peak position of the PHD remains at the relative
level of 50%.
21.1.3 Escape Peaks

The photons entering the detector may interact with the detector gas or the scintillation crystal and create
fluorescence radiation via interaction between the photons and the detecting media. This fluorescence is
apparent as a peak either in a PHD determination scan or in a diffractogram (2θ - θ scan). These peaks are often
referred to as escape peaks.
21.1.3.1 Escape Peaks in a PHD Determination Scan

An escape peak in a PHD determination scan is observed at the lower energy side. It is produced as follows:
When an X-ray photon enters the detector it has sufficient energy to remove an electron from an inner
orbit of an atom of the counting gas or the scintillation crystal. The removed electron may be replaced
by an electron from a higher orbit, thereby releasing an X-ray photon. This process is called X-ray
fluorescence. The energy of the initial photon is reduced by an amount equal to the ionization
procedure.
Both photons may create ion-electron pairs in the gas or be absorbed in the scintillation crystal to
produce an output pulse with a height proportional to the energy of the X-ray photon that entered the
detector. However, since the detecting medium has a very low absorption coefficient for its own
fluorescence radiation, the fluorescence photon may “escape” from the detector chamber to be
absorbed by the detector wall. The remaining photon will now produce a pulse with a much lower
height which is visible at the low energy side in a PHD determination scan.
For example: a Cu Kα photon of 8.04 keV may produce Xe Lα radiation which has an energy of 4.1
keV. When the Xe Lα photon escapes from the detector chamber, only the energy of the remaining
photon, somewhat less than 4 keV, is detected.
In the PHD determination scan the escape peak is around 25%, where the Cu Kα peak is centered around 50%
as is shown in Figure 21.1.
This effect is not restricted to the combination of Cu radiation and Xe gas, it can occur with other combinations
of radiation and detection mediums.
07.12.04 Page 21.5

Pulse rate (cps)
Pulse height
Cu Kα = 8.04 keV
Figure 21.1: Pulse Height Distribution Curve for Cu Kα Radiation
21.1.3.2 Escape Peaks in the Low Angle Regions of Diffractograms

The low angle part of diffractograms may contain different types of spurious peaks; peaks not caused by the
normal Bragg diffraction of the tube anode’s Kα X-rays at lattice planes in the sample. These peaks are caused
by the occurrence of escape peaks in the detector; they are created in the following way:
High energy X-rays from the tube’s continuum (‘white radiation’) scattered from (strongly) diffracting
lattice planes in the sample are generally eliminated by a crystal monochromator and/or by pulse height
discrimination.
However, the high energy X-rays entering the detector may produce some fluorescence radiation, some
of which will escape from the detector without being absorbed (detected). The remaining energy of the
original photons can contribute to the detector signal if the energy falls within the PHD ‘window’.
For example: when X-rays with an energy around 38 keV are diffracted by a crystalline sample and
enter a detector chamber filled with Xe gas, they may produce Xe Kα fluorescence radiation with a pho-
ton energy of 29.67 keV. As the Xe gas absorbs its own fluorescence radiation very inefficiently Xe Kα
will escape from the detector. The remaining energy, around 8 keV, will be detected radiation as if it
were Cu Kα radiation.
In the diffractogram, peaks caused by the 38 keV (corresponding to a wavelength around 0.33 Å) may
occur in the low angle region, will be detected as if they were Cu Kα radiation.
This effect is not restricted to the combination of Cu radiation and Xe gas, it can occur with other combinations
of radiation and detection mediums.
These escape peaks must not be confused with low angle diffraction peaks. Production of escape peaks can be
avoided in two ways:
1. Place an incident beam or a diffracted beam monochromator in the X-ray beam path so that only the
characteristic radiation used in the experiment will be detected.
2. Set the generator voltage at a level lower than the absorption edge of the element giving rise to the
X-ray fluorescence.
Figure 21.2 shows an example of escape peaks due to Xe Kα and Xe Lα fluorescence radiation measured on a
Si (004) single crystal wafer at two different generator settings. The detector was a PW3011/20 Proportional
Detector filled with xenon counting gas. A beta-filter was inserted into the X-ray beam path. Note that the
intensity scale is logarithmic. The escape peaks due to Xe Kα fluorescence could be eliminated by selecting a
lower generator high voltage setting.
Page 21.6 07.12.04

Figure 21.2: Escape Peaks Showing in a Diffractogram
21.2 SEALED PROPORTIONAL DETECTORS

Sealed proportional detectors consist of a sealed chamber with a beryllium detection window. This chamber is
filled with a counting gas, typically xenon; and a quenching gas, typically methane.
An anode wire is positioned in the axial center of the cylinder. The detection process in this kind of detector can
be described as follows:
When an X-ray photon enters the detector and collides with an inert gas atom, it may ionize the atom by
removing an electron from the outer shell of the atom. A primary electron ion-pair is formed in this
way. The total number of primary electron ion-pairs produced by an X-ray photon is defined by the
ratio of the energy of the X-ray photon and the ionization energy of the inert gas atom. The electrons
from the electron ion-pair are then accelerated towards the anode wire by its high potential. On its way
to the anode wire the accelerating electron can produce another electron ion-pair.
Each primary electron may give rise to many secondary electrons which in turn are accelerated towards
the anode wire. This process is called gas amplification.
The electrons (primary and secondary) create an electrical current in the wire, this electrical current is
then converted into an electrical pulse by the pulse forming circuit. The height of the pulse is
proportional to the energy of the detected (incoming) X-ray photon.
The positively charged ions are attracted towards the grounded casing. The inert gas is mixed with a
quenching gas to prevent ions from creating an avalanche. This quenching gas neutralizes the positive
ions without any other reactions.
07.12.04 Page 21.7

21.2.1 PW3011/20 Proportional Detector

PW3011/20 is a proportional detector consisting of a cylindrical chamber filled with a xenon/methane gas
mixture, it is shown in Figure 21.3. The beryllium detector window is 20 mm x 24 mm.
The detector is most efficient for Cu Kα radiation, it can also be used for radiation with longer wavelengths. We
do not advise its use with Mo Kα radiation, as the efficiency with this radiation is as low as 36%. General
properties of the PW3011/20 Proportional Detector are given in Table 21.1.
Figure 21.3: PW3011/20 Proportional Detector
21.2.1.1 Use
This section describes the diffracted beam modules onto which the PW3011/20 Detector can be mounted. The
procedure for determining the pulse height distribution and setting PHD levels is described in 21.1.1.
21.2.1.1.1 Mounting
This detector can be mounted on the following diffracted beam optical components:
Table 21.2: Devices onto which Detectors can be Mounted
Type Number Item Chapter
PW3093/60 Programmable Receiving Slit II - 16
PW3093/60 & PW312x/10 Programmable Receiving Slit & Curved II - 19

Crystal Monochromator
PW3091/x0 & PW3093/60 & Programmable Anti-scatter Slit & II - 19

PW3121/00 Programmable Receiving Slit & Flat
Crystal Monochromator
PW3098/xx Parallel Plate Collimator II - 18
PW3098/xx & PW3121/00 Parallel Plate Collimator & Flat Crystal II - 19

Monochromator
PW3097/60 Rocking Curve Attachment II - 16
PW3120/60 Triple Axis and Rocking Curve II - 16 / 19

Attachment (2 detector positions)
PW3120/65 Asymmetric Triple Axis and Rocking II - 16 / 19

Curve Attachment (2 detector positions)
Page 21.8 07.12.04

Detector mounting instructions are given in the chapter describing the device onto which the detector is
mounted, as shown in the third column in Table 21.2.
The detector is standardly mounted in such a way that the window opening is 20 mm in the diffraction plane
(height) and 24 mm perpendicular to the diffraction plane (width). When the detector is mounted behind a
PW3121/00 Flat Crystal Monochromator it is mounted so that the window opening is 24 mm in the diffraction
plane and 20 mm perpendicular to the diffraction plane.
21.3 SCINTILLATION DETECTORS

A scintillation detector basically consists of two parts: a scintillation crystal, and a photo-multiplier tube.
Conversion of incoming X-ray photons onto electrical pulses is performed in two stages:
The X-ray photons are absorbed by the scintillation crystal. The absorbed energy is then re-emitted by
the crystal in the form of photons with much lower energy.
In the second stage the photons emitted by the scintillation crystal are transformed into electrical pulses
by the photo-multiplier tube. The output pulse is proportional to the number of photons entering the
photo-multiplier tube and in its turn, the number of photons is proportional to the energy of the detected
X-ray photon. Thus, the height of the pulse produced by the photo-multiplier tube is proportional to the
energy of the X-ray photon.
21.3.1 PW1964/96 Scintillation Detector

The PW1964/96 Scintillation Detector contains a thallium activated sodium iodide crystal (NaI:Tl). This crystal
is hygroscopic and is hermetically sealed in a holder with a circular beryllium detection window with a diameter
of 30 mm at the front and a glass plate to transmit the emitted photons to the photo-multiplier at the back. The
NaI:Tl crystal produces photons in the visible light region (average wavelength 410 nm).
The detector is shown in Figure 21.4. The module consists of a detector housing, a scintillation tube containing
the sodium iodide crystal and the photo-multiplier, and the detector mounting interface.
This scintillation detector is most efficient for Mo Kα radiation, it can be used for the detection of characteristic
radiation with longer wavelengths. General properties of the PW1964/96 Scintillation Detector are given in
Table 21.1.
Figure 21.4: PW1964/96 Scintillation Detector
07.12.04 Page 21.9

21.3.1.1 Use
This section describes the diffracted beam optical modules onto which the PW1964/96 can be mounted. The
procedure for determining the pulse height distribution and setting the PHD levels is described in 21.1.1.
21.3.1.1.1 Mounting
This detector can be mounted on the diffracted beam optical components as listed in Table 21.2. Detector
mounting instructions are given in the chapter describing the device onto which the detector is mounted, as
shown in Table 21.2.
NOTES: 1. Although the PW1964/96 Scintillation Detector can be physically mounted onto high resolution
attachments (PW3097/60, PW3120/60 and PW3120/65) we advise that you use the PW3011/20
Proportional Detector with these attachments as the proportional detectors have a lower background
noise.
2. For mechanical reasons, the PW1964/96 Scintillation Detector cannot be used on an X’Pert PRO
MRD system onto which a diffracted beam PreFIX module is mounted with a diffracted beam
monochromator.
21.4 RTMS DETECTOR X’CELERATOR

The X’Celerator is an ultra-fast X-ray detector based on RTMS (Real Time Multiple Strip) technology. This
technology operates as if there were an array of over a hundred detectors at work simultaneously in an X-ray
diffraction system. Unlike other detection technologies that rely on the delayed response of gas ionization,
RTMS technology offers direct detection of diffracted X-rays, and the ability to efficiently process high count
rates without any compromise on resolution.
Together, all these benefits lead to a reduction in measurement time for a normal powder diffraction
diffractogram with a factor of up to 100, compared to a system with focusing optics.
21.4.1 Applications
The X’Celerator can be used in a number of powder diffraction applications. Typical examples of applications
are:
• Phase identification, standardless quantification, crystallography, and non-ambient studies on flat powder
samples.
• Analysis of samples in glass capillaries.
• Micro-diffraction.
These applications are all described in detail in the following sections.
21.4.1.1 Phase Analysis on Flat Powder Samples

The X’Celerator can be used in phase analysis applications like: phase identification, standardless quantification,
crystallography, and non-ambient studies on flat powder samples. The ultra-fast data acquisition based on RTMS
technology makes it possible to optimize on resolution but still have reasonable total measurement times.
A (fixed or programmable) divergence slit with an incident beam anti-scatter slit mounted is used in the incident
beam path. An anti-scatter shield is mounted onto the X’Celerator.
A beam knife is placed above the sample in order to improve the peak-to-background ratio in the diffractograms.
Page 21.10 07.12.04


The X’Celerator can also be used for the analysis of samples in glass capillaries mounted onto a capillary
spinner. In this case, the time to record a reasonable measurement can be reduced significantly with respect to a
standard proportional detector. The capillary is irradiated by a small beam emitted by a focusing X-ray mirror
or a hybrid monochromator. An additional anti-scatter device is mounted onto the X’Celerator’s anti-scatter
shield in order to optimize the data quality.
21.4.1.3 Micro-diffraction
When small samples, or small parts of a larger sample need to be analyzed, a mono-capillary is used in the
incident beam path to collimate the X-ray beam to a small diameter. Using an X’Celerator in the diffracted beam
path reduces the measurement time considerably, and improves the counting statistics in comparison to a
proportional detector.
21.4.2 PW3015/x0 X’Celerator

The PW3015/x0 X’Celerator is an X-ray detection system based on RTMS technology. The detector itself is
mounted into a rectangular housing with a beryllium entrance window and a cooling fan. Two types of
X’Celerator are available:
• PW3015/00 X’Celerator Scientific
The X’Celerator Scientific can be used in scanning mode, receiving slit mode and static mode.
• PW3015/20 X’Celerator
The X’Celerator can be used in scanning mode and receiving slit mode.
Figure 21.5: PW3015/x0 X’Celerator with PW3094/30 Anti-scatter Slit Holder Mounted onto a
PW3014/00 PreFIX Interface
07.12.04 Page 21.11

The X’Celerator is mounted onto a PW3014/00 PreFIX Interface to allow it to be mounted onto the 2theta arm
of the X’Pert PRO goniometer as shown in Figure 21.5. The PreFIX interface and the mounting procedure are
described in sections 21.4.3.1 and 21.4.3.1.1 respectively.
The PW3014/00 PreFIX Interface includes a slot to insert Soller slits and a slot for a beta-filter or a beam
attenuator.
Alternatively, when monochromatic radiation is required, the X’Celerator can be mounted onto the PW3122/00
Diffracted Beam Monochromator. This is shown in Figure 21.6. Mounting instructions are given in section
21.4.3.10.1. The monochromator is described in more detail in section 19.4 of Chapter 19 in Part II of this User’s
Guide.
The opening of the detector window measures 9 mm in the diffraction plane and 15 mm perpendicular to the
diffraction plane. The active length is 9 mm. The smallest step size that can be set in the data collector software
is 0.0021º 2θ at a goniometer radius of 240 mm and 0.0016º 2θ at a goniometer radius of 320 mm.
The X’Celerator is optimized for use with Cu Kα radiation with an efficiency higher than 94%. It can be used
with other characteristic radiation, however the efficiency will be reduced.
The general properties of the X’Celerator are given in Table 21.1.
Mounting
Screws
Detector
Interface
Mounting
Screw
Black Knurled
Knob
Figure 21.6: PW3015/x0 X’Celerator Mounted onto a PW3122/00 Diffracted Beam Monochromator
for X’Celerator
Page 21.12 07.12.04

21.4.3 Accessories
21.4.3.1 PW3014/00 PreFIX Interface
PW3014/00 consists of a PreFIX interface to mount the X’Celerator onto the 2theta arm of an X’Pert PRO
goniometer. The PreFIX interface with an X’Celerator with an anti-scatter slit mounted onto it is shown in
Figure 21.5. The PreFIX interface contains a slot for Soller slits and a slot for a beta-filter or a beam attenuator.
The X’Celerator can be mounted in one of two ways onto the interface; the standard orientation used for
diffraction experiments, or rotated through 90º which is used for tube height alignment purposes. Mounting
instructions are given in the following section.
21.4.3.1.1 Mounting the X’Celerator onto the PreFIX Interface

Proceed as follows to mount the X’Celerator onto the PreFIX interface in the standard position for diffraction
experiments:
1. Make sure that the diffracted beam anti-scatter shield, the Soller slits and the beta-filter or the beam
attenuator are removed from the interface.
2. Loosely mount the X’Celerator onto the PreFIX interface using the three M3 x 8 screws provided.
Refer also to Figure 21.7.
3. Tighten the small black knurled knob on the interface.
4. Tighten the three screws (see step 2) to securely attach the X’Celerator to the interface.
5. If required, you can now mount the diffracted beam anti-scatter shield (see section 21.4.3.6), or insert
Soller slits, a beta-filter or a beam attenuator.
Figure 21.7: PW3015/x0 X’Celerator Mounted onto a PW3014/00 PreFIX Interface
07.12.04 Page 21.13

21.4.3.1.2 Removing the X’Celerator from the PreFIX Interface

The X’Celerator can be removed from the PreFIX interface in order to make it possible to rotate it 90º for
alignment purposes, or to mount it onto the PW3122/00 Diffracted Beam Monochromator. To remove it from
the PreFIX interface, proceed as follows:
1. If present, remove the Soller slits, the beta-filter or the beam attenuator from their slots on the PreFIX
interface.
2. Remove the diffracted beam anti-scatter device by undoing the two screws.
3. Loosen the small black knurled knob on the interface.
4. Undo the three screws holding the detector onto the interface.
Now you can rotate the X’Celerator through 90º, or mount it onto the diffracted beam monochromator.
CAUTION
If you perform these actions with the X’Celerator connected to the
X’Pert PRO system and the system is switched on, be careful not to
touch the spinning fan.
21.4.3.1.3 Mounting the X’Celerator 90º Rotated onto the PreFIX Interface
You can mount the X’Celerator 90º rotated with respect to the standard position for alignment purposes. Proceed
as follows:
1. Bring the X’Celerator into position on the PreFIX interface as shown in Figure 21.8.
2. Fix the M3 x 8 screw (see Figure 21.8).
When the X’Celerator is mounted 90º rotated it is not possible to insert Soller slits.
Figure 21.8: PW3015/x0 X’Celerator Mounted 90º rotated onto a PW3014/00 PreFIX Interface
Page 21.14 07.12.04

There are three types of beta-filter that can be used together with the X’Celerator, they are:
Ni Filter (PW3151/03) for Cu Kα radiation
Fe Filter (part of set PW3151/00) for Co Kα radiation
Zr Filter (part of set PW3151/00) for Mo Kα radiation
The filter must be installed in the slot for attenuator foil or beta-filter as shown in Figure 21.5. Beta-filters and
their use are described in Chapter 2 of Part II of this User’s Guide.

A 0.1 mm and a 0.2 mm copper foil are delivered with the X’Pert PRO diffraction system. This foil can be
1 000 000 cps.

beta-filter slot on the X’Celerator in order to attenuate the beam
whenever the measured intensity is expected to exceed maximum
count rate of the X’Celerator.

Copper (0.1 mm): ≈ 100
Copper (0.2 mm): ≈ 10 000
on the attenuation foil itself and on the Acceptance Test Form for the system, which is supplied when the system
is delivered. This value can be entered in the data collector software and is used to automatically adjust the
measured intensity values. For more information about the use of a copper attenuation foil refer to Chapter 2
(section 2.2) in Part II of this User’s Guide.

Soller slits are used in the diffracted beam path to control the axial acceptance of the detector. Four Soller slits
are available for use with the X’Celerator (see Figure 21.5), they are:
The Soller slits must be inserted into the slot for Soller slits on the X’Celerator. To do this, insert the Soller slits
assembly into the slot until it clicks into place. For more information about Soller slits refer to Chapter 5 in Part
NOTE: Be careful not to interchange the PW3085/x1 Soller Slits with the PW3085/x0 Soller Slits, as they
are mechanically different.
07.12.04 Page 21.15

21.4.3.5 PW3091/x0 Programmable Anti-scatter Slit

The PW3091/x0 Programmable Anti-scatter Slit (PASS) is used in combination with the X'Celerator in order to
reduce the intensity of the background radiation to a low level. The programmable anti-scatter slit mounted onto
the PreFIX interface with the use of a PW3094/40 Mounting interface is shown in Figure 21.9.
Mounting instructions for the programmable anti-scatter slit are given in section 21.4.3.5.1 below.
CAUTIONS 1. If you have mounted a programmable anti-scatter slit onto the

X'Celerator, be careful to avoid collisions between the anti-
scatter slit and the sample stage or the sample itself.
2. Normally the X'Pert PRO system automatically resets when the

system is switched on or when power is restored after a power
failure. The reset procedure involves driving the goniometer
back to its hardware zero points, which may cause collisions
between the sample or the sample stage and the anti-scatter slit.
You should disable this automatic reset using the data collector
software in cases where collisions are possible. You then have
the possibility to remove the anti-scatter slit before resetting the
system.
Figure 21.9: PW3091/x0 Programmable Anti-scatter Slit with PW3094/40 Interface Mounted onto the
X’Celerator
Page 21.16 07.12.04

21.4.3.5.1 Mounting the Programmable Anti-scatter Slit onto the X'Celerator

Mount the programmable anti-scatter slit onto the X'Celerator as follows:
1. Select the X'Celerator PreFIX module with PASS in your configuration in the data collector software.
2. Make sure to switch the X'Pert PRO system off according to the procedure described in Chapter 4 in
Part I of this User's Guide. This is necessary because the distance between the slit and the sample has
been changed. Close the data collector software.
3. Bring the PW3094/40 Interface into position so that the two holes on this device fit into the
corresponding pins on the PW3014/00 PreFIX Interface for the X'Celerator, refer to Figure 21.9.
4. Insert and tighten the two M3 x 8 screws supplied.
5. Remove the programmable anti-scatter slit assembly from its interface by removing the interface
mounting screws indicated in Figure 16.1.
6. Bring the programmable anti-scatter slit assembly into position on the PW3094/40 Interface, so that the
two pins on this device fit into the corresponding holes in the PW3094/40 Interface, refer to Figure
21.10.
7. Tighten the interface mounting screws of the programmable anti-scatter slit so that it is secured to the
interface.
8. Switch the X'Pert PRO system on according to the procedure described in Chapter 4 in Part I of this
User's Guide. Start up the data collector software and go on-line with the configuration that you are
going to use.
Figure 21.10: Mounting the PW3091/x0 Programmable Anti-scatter Slit onto the X’Celerator
07.12.04 Page 21.17

21.4.3.6 PW3x94/30 Fixed Anti-scatter Slit for X’Celerator

A fixed anti-scatter slit mounted onto the X’Celerator is used to reduce the intensity of the background radiation
to a low level. The fixed anti-scatter slit holder mounted onto the X’Celerator is shown in Figure 21.5. When the
X’Celerator is used for measurements on samples in glass capillaries or in combination with Anton Paar
chambers or on the MRD, additional anti-scatter devices must be mounted onto the fixed anti-scatter slit holder.
Mounting instructions for the fixed anti-scatter slit holder are given in section 21.4.3.6.1 below. Mounting the
PW3x94/32 and PW3x94/35 Anti-scatter Slits onto the fixed anti-scatter slit holder is described in sections
20.3.1.1.1.1 and 20.3.1.1.2.1 in Chapter 20 in Part II of this User’s Guide. More information about the
PW3x94/30 Fixed Anti-scatter Slits and their use is given in section 20.3.1 in Chapter 20 of Part II of this User’s
Guide.
CAUTIONS 1. If you have mounted a fixed anti-scatter slit holder onto the
X’Celerator, be careful to avoid collisions between the anti-scatter
slit holder and the sample stage or the sample itself.
2. Normally the X’Pert PRO system automatically resets when the

failure. The reset procedure involves driving the goniometer back
to its hardware zero points, which may cause collisions between
the sample or the sample stage and the anti-scatter slit holder.
You should disable this automatic reset using the data collector
software in cases where collisions are possible. You then have the
opportunity to remove the anti-scatter slit holder before resetting
the system.
21.4.3.6.1 Mounting the Fixed Anti-scatter Slit Holder onto the X’Celerator
Mount the fixed anti-scatter slit holder onto the X’Celerator as follows:
1. Bring the fixed anti-scatter slit holder into position so that the two holes on this device fit into the
corresponding pins on the X’Celerator, refer to Figure 21.5.
21.4.3.7 PW3x94/32 Anti-scatter Slit

The PW3x94/32 Anti-scatter Slit for the X’Celerator must be mounted onto PW3x94/30 Fixed Anti-scatter Slit
Holder when the X’Celerator is used for measurements in combination with Anton Paar non-ambient chambers.
It is used to reduce the amount of scattered radiation that enters the detector. The PW3x94/32 Fixed Anti-scatter
Slit is described in detail in section 20.3.2 in Chapter 20 in Part II of this User’s Guide. Mounting the anti-scatter
slit onto the fixed anti-scatter slit holder is described in section 20.3.1.1.1.1 in Chapter 20 in Part II of this User’s
Guide.
21.4.3.8 PW3x94/35 Anti-scatter Slit

The PW3x94/35 Anti-scatter Slit must be mounted in the diffracted beam path onto PW3x94/30 Fixed Anti-
scatter Slit Holder when the X’Celerator is used in combination with a PW3063/00 Capillary Spinner in order to
reduce the amount of scattered radiation entering the detector. Information about the PW3x94/35 Fixed Anti-
scatter Slit is given in section 20.3.3 in Chapter 20 in Part II of this User’s Guide. Mounting the anti-scatter slit
onto the fixed anti-scatter slit holder is described in section 20.3.1.1.2.1 in Chapter 20 in Part II of this User’s
Guide.
Page 21.18 07.12.04

21.4.3.9 PW3094/50 Fixed Anti-scatter Slit for X’Celerator Monochromator

PW3094/50 is a set of fixed anti-scatter slits marked 0.2 mm, 3.9 mm, 4.6 mm, 5.9 mm and 8.6 mm for use with
the PW3122/00 Diffracted Beam Monochromator and X'Celerator detector. They can be inserted in the slit
holder supplied. These slits are used to reduce the amount of scattered radiation entering the X'Celerator detector
equipped with the PW3122/00 Monochromator. Mounting instructions are given in section 19.4.1.1.1 of Chapter
19 of Part II of this User's Guide. Information about how to use these fixed anti-scatter slits is given in section
20.3.5 of Chapter 20 of Part II of this User's Guide.
21.4.3.10 PW3122/00 Diffracted Beam Monochromator for X’Celerator

The X’Celerator can be used together with a PW3122/00 Diffracted Beam Monochromator for X’Celerator and
copper radiation to reduce the background radiation and sample fluorescence, and to eliminate unwanted lines.
It is shown in Figure 21.6.
The monochromator comprises a PreFIX T-block to mount it onto the diffracted beam arm of the goniometer,
and a detector interface to mount the X’Celerator. Mounting instructions are given below. If necessary you can
mount a fixed anti-scatter slit holder onto the monochromator. More information can be found in section
19.4.1.1.1 of Chapter 19 in Part II of this User’s Guide.
21.4.3.10.1 Mounting the X’Celerator onto the PW3122/00 Diffracted Beam Monochromator
Proceed as follows to mount the X’Celerator onto the PW3122/00 Diffracted Beam Monochromator:
1. If necessary, remove the X’Celerator from its PreFIX interface, refer to section 21.4.3.1.2.
2. Bring the X’Celerator into position on the detector interface on the diffracted beam monochromator as
3. Insert and loosely tighten the three M3 x 8 screws supplied to attach the X’Celerator to the interface.
4. Tighten the small black knurled knob on the interface.
5. Tighten the three screws (see step 3) to securely attach the X’Celerator to the interface.
The X’Celerator with its monochromator is now ready for use. No further alignment is required.
21.4.4 Use
The X’Celerator does not use counting gas or cooling liquids, so no additional system maintenance is required.
The use of the X’Celerator in alignment procedures is given in the appropriate sections throughout this User’s
Guide. In some situations the X’Celerator must be rotated 90º on its interface; the procedure for this is given in
section 21.4.3.1.3.
This section describes:
• Selecting the X’Celerator’s PHD levels
• The operating modes of the X’Celerator
• How to optimize measurements with the X’Celerator
• Suppression of background radiation and unwanted lines in diffractograms.
21.4.4.1 Selecting PHD Levels

You can set the lower and upper detection levels to select the energy range of the X-ray photons to be detected.
Typical PHD levels for the X'Celerator are 35% and 80% for the lower and upper level respectively. We
recommend setting the PHD levels to the factory levels in the data collector software.
If the sample shows strong fluorescence, you may reduce this effect by choosing the lower level closer to the
50% level of the main energy peak, for example: 45%. However, remember that you also discard part of the
diffraction signal when you do that. Better ways of reducing sample fluorescence are either to use a
monochromator, or an X-ray tube with a different anode material.
07.12.04 Page 21.19

The X’Celerator can be used in three distinctive modes:
• Scanning mode
In the scanning mode, the X’Celerator is moved over the 2θ range-of-interest at each step along the
scan; the intensity at that particular 2θ position (data point) is measured and then summed, until the data
point is no longer in range. When the X’Celerator is used over its total active length (9 mm) its opening
(height) is slightly larger than 2º 2θ on an X’Pert PRO system with a radius of 240 mm.
It is possible to reduce the active length using the data collector software. When extremely well-defined
powders are measured, such a reduction can lead to sharper peaks in the diffractogram. However, for
the vast majority of powder samples, you do not need this option.
Scans measured in the scanning mode are continuous scans. Their axis can be: gonio, 2theta,
2theta-omega and omega-2theta.
In the scanning mode the only 2-axes measurements that are allowed are those in which a gonio scan, a
2θ scan or a 2θ - ω scan is one of the directions.
• Receiving slit mode
In the receiving slit mode, the intensity of the radiation entering the detector is added together over its
complete active length. This option is used for alignment of system components, such as the tube height
or the sample surface. For optimum sensitivity we advise you to rotate the X’Celerator 90º on its
interface (see section 21.4.3.1.3). Alternatively, you can use the receiving slit mode to record pole
figures or for stationary measurements.
In the Receiving slit mode, all 2-axes measurements are allowed.
• Static mode
NOTE: This mode is only available for the PW3015/00 X’Celerator Scientific.
In the static mode, the X’Celerator does not move along the 2θ circle. Each of the X’Celerator’s
channels corresponds to a unique 2θ value. Scans measured in the static mode are stepped scans with a
2theta scan axis. You cannot perform a stationary measurement in this mode.
NOTE: When you are setting up a measurement program in the data collector software you must explicitly
specify the X’Celerator’s operating mode in the measurement conditions. If you leave this at
“Actual”, the X’Celerator will be automatically set into the Scanning mode with maximum active
length.
21.4.4.3 Optimizing Measurements with the X'Celerator

The resolution of a measurement on a flat powder sample using the X'Celerator can be optimized by selecting
the appropriate divergence slit size, its active length, anti-scatter device and beam knife.
• Divergence slit size
To optimize the resolution of a measurement with the X'Celerator, you should use a very narrow
divergence slit in the incident beam path. For normal applications you can use a 1°, a ½°, or a ¼°
divergence slit. For measurements at low angles of incidence or measurements on small samples, we
advise you to use a narrower divergence slit: 1/8°, 1/16° or 1/32° in order to prevent over-irradiation of
the sample.
• Active length
It is possible to reduce the active length of the X'Celerator, in this way only a part of the X'Celerator is
activated. X-ray photons falling outside the active length are collected but are filtered out electronically.
Reducing the active length can lead to a better peak shape of the reflections observed. However, this
can only be observed in diffractograms measured on extremely well-defined powder samples. In all
other cases, you should use the X'Celerator over its complete length.
Page 21.20 07.12.04

• Anti-scatter devices
Anti-scatter devices can be mounted in the incident and the diffracted X-ray beam path in order to
reduce the intensity of the background radiation caused by scattered X-rays.
An incident beam anti-scatter slit holder can be mounted onto the (fixed or programmable) divergence
slit module. This type of anti-scatter device is described in section 20.2.1 of Chapter 20 of Part II of this
User's Guide. The choice of the anti-scatter slit size to be used during the diffraction experiment is
determined by the size of the divergence slit selected. The optimal anti-scatter slit size is twice that of
the size of the divergence slit.
Special incident beam anti-scatter devices can be used with X-ray mirrors or hybrid monochromators in
measurements on samples in glass capillaries in transmission measurements or in high-throughput
applications. These types of anti-scatter device are described in sections 20.2.2 to 20.2.5 in Chapter 20
The PW3091/x0 Programmable Anti-scatter Slit can be mounted onto the X'Celerator (refer to section
21.4.3.6). The choice of the anti-scatter slit size to be used during the diffraction experiment is
determined by the divergence slit size selected. Information about operating modes of the
programmable anti-scatter slit is given in section 16.2.2.2.1 in Chapter 16 of Part II of this User's
Guide.
The PW3x94/30 Fixed Anti-scatter Slit Holder is used in the diffracted beam path. This holder has a
slot to accommodate a fixed anti-scatter slit. Selecting the correct slit size for the task in hand is
described in section 20.3.1.2 in Chapter 20 of Part II of this User's Guide. For measurements on sam-
ples in glass capillaries or in combination with Anton Paar non-ambient chambers, special anti-scatter
slits can be mounted onto this fixed anti-scatter slit holder. Diffracted beam anti-scatter devices for use
with the X'Celerator are described in detail in section 20.3.1 to 20.3.4 in Chapter 20 of Part II of this
User's Guide.
• Beam knife
In addition to the anti-scatter devices, a beam knife can be inserted in the X-ray beam path to reduce the
background intensity due to scattered radiation to a low level. Several types of beam knife can be used;
they are specific to the sample stage used. An overview of the available types is given in section 14.3 of
Chapter 14 of Part II of this User's Guide. For optimum use of the beam knife the gap between the beam
knife and the sample surface should be as small as possible without obstructing the incident and the
diffracted X-ray beam. A procedure for calculation of the optimum height is given in section 14.3.6 of
21.4.4.4 Suppression of Unwanted Radiation

The energy resolution of the X'Celerator is around 25%, which is comparable with a proportional detector. This
means that additional X-ray optical components needs to be inserted in the X-ray beam path to reduce the
intensity of unwanted radiation, such as Cu Kβ or white radiation. The intensity of unwanted radiation can be
reduced in the following ways:
• Beta-filter
For most powder samples, a beta-filter is sufficient to reduce Kβ radiation. For example, with a
PW3151/03 Ni filter inserted into the X'Celerator, the intensity of the Cu Kβ peak is reduced to less
than 1% of the Cu Kα peak. If you need better suppression of the Cu Kβ peak, we recommend that you
use an additional Ni filter, so that one is inserted in the incident beam optical module, and the other is
inserted in the X'Celerator.
• Diffracted Beam Monochromator
For samples yielding fluorescent radiation (a well-known example is that of samples containing iron
when copper radiation is being used) we advise using a PW3122/00 Diffracted Beam Monochromator
in combination with Cu Kα radiation. With a diffracted beam monochromator the fluorescence is
almost completely eliminated. If required, it is possible to use this monochromator in combination with
a Ni filter in order to reduce the intensity of the Cu Kβ peaks to a very low level.
07.12.04 Page 21.21

21.5 MEDIPIX2 DETECTOR PIXCEL

The PIXcel is an ultra-fast X-ray detector based on Medipix2 technology, a solid-state technology providing for
counting photons with a high spatial resolution and a high dynamic range. The PIXcel comprises more than
65,000 pixels, each 55 mm x 55 mm in size. Each pixel has its own counting circuitry, giving rapid readout, a
high counting linearity combined with a high dynamic range. The PIXcel can be used as a line detector or as a
point detector for static and scanning applications. The PIXcel is designed for use with Cu Kα radiation; it can
also be used with other types of radiation.
21.5.1 Applications
The PIXcel can be used in a wide range of diffraction applications. Typical examples of applications are:
• Phase analysis on powder samples.
• Analysis of samples in glass capillaries.
• Texture measurements.
• Parallel beam measurements on thin films and rough samples.
• Micro-diffraction.
• High-resolution rocking curves and reciprocal space mapping.
• Reflectivity.
These applications are all described in detail in the following sections.
21.5.1.1 Phase Analysis on Flat Powder Samples

The PIXcel can be used in powder diffraction applications like: phase identification, standardless quantification,
crystallography, and non-ambient studies on flat powder samples. The ultra-fast data acquisition makes it
possible to optimize on resolution but still have reasonable total measurement times.
A (fixed or programmable) divergence slit with an incident beam anti-scatter slit mounted is used in the incident
beam path. An anti-scatter shield is mounted onto the PIXcel.
A beam knife is placed above the sample in order to improve the peak-to-background ratio in the diffractograms.

The PIXcel can also be used for the analysis of samples in glass capillaries mounted onto a capillary spinner. In
this case, the time to record a reasonable measurement can be reduced significantly with respect to a standard
proportional detector. The capillary is irradiated by a small beam emitted by a focusing X-ray mirror or a hybrid
monochromator. An additional anti-scatter device is mounted onto the PIXcel's anti-scatter shield in order to
optimize the data quality.
21.5.1.3 Texture Measurements

The PIXcel can be used as a point detector in quantitative texture analysis. The active length of the PIXcel can
be set and used as a programmable receiving slit in the Schultz geometry. Alternatively, the PIXcel can be
mounted onto a parallel plate collimator for texture measurements in the parallel beam geometry.
21.5.1.4 Parallel Beam Measurements

In parallel beam applications, such as thin film phase identification, the PIXcel can be used as a point detector
mounted onto a parallel plate collimator.
Page 21.22 07.12.04

21.5.1.5 Micro-diffraction
When small samples, or small parts of a larger sample need to be analyzed, a mono-capillary is used in the
incident beam path to collimate the X-ray beam to a small diameter. Using a PIXcel in the diffracted beam path
reduces the measurement time considerably, and improves the counting statistics in comparison to a proportional
detector.
21.5.1.6 High-resolution Rocking Curves and Reciprocal Space Mapping

The high dynamic range of the PIXcel makes it a very useful detector for high-resolution applications such as
rocking curve analysis and reciprocal space mapping. A manual or programmable beam attenuator is not needed
during the measurements. When the PIXcel is used as a point detector, it can be mounted onto a rocking curve
attachment or onto a triple-axis analyzer; the variable active length can act as a programmable receiving slit.
Used as a line detector, the PIXcel provides ultra fast analysis.
21.5.1.7 Reflectivity
For reflectivity analysis, the PIXcel can be combined with a parallel plate collimator to be used as a point
detector, or it can be used in combination with an anti-scatter slit fixed or programmable) in order to create a
beam tunnel. Depending on the intensity of the incident X-ray beam, a beam attenuator may be required, for
instance when you are working with an X-ray mirror. For other optical modules, such as a divergence slit or a
hybrid monochromator, a beam attenuator is generally not required during the measurements.
21.5.2 PW3018/00 PIXcel

The PW3018/00 PIXcel is a fast X-ray detection system based on Medipix2 technology. The detector itself is
mounted into a rectangular housing with a beryllium entrance window. The PIXcel can be used in scanning
mode, receiving slit mode and static mode.
The PIXcel is mounted onto a PW3017/00 PreFIX Interface to allow it to be mounted onto the 2theta arm of the
X'Pert PRO goniometer as shown in Figure 21.11. The PreFIX interface and the mounting procedure are
described in sections 21.5.3.1 and 21.5.3.1.1 respectively. The PW3017/00 PreFIX Interface includes a slot to
insert Soller slits and a slot for a beta-filter.
Alternatively, the PIXcel can be mounted onto a PW3017/60 Interface to allow it to be used as a point detector
mounted onto a diffracted beam PreFIX module. This interface and its mounting procedure are described in
sections 21.5.3.2 and 21.5.3.2.1 respectively.
When monochromatic radiation is required, the PIXcel can be mounted onto the PW3124/00 Diffracted Beam
Monochromator. This is shown in Figure 21.12. Mounting instructions are given in section 21.5.3.10.1. The
monochromator is described in more detail in section 19.4.2 of Chapter 19 in Part II of this User's Guide.
The opening of the detector window measures 14 mm in the diffraction plane and 14 mm perpendicular to the
diffraction plane. The active length is 14 mm. The smallest step size that can be set in the data collector software
is 0.0016º 2θ at a goniometer radius of 240 mm and 0.0012º 2θ at a goniometer radius of 320 mm.
The PIXcel is optimized for use with Cu Kα radiation with an efficiency higher than 94%. It can be used with
other characteristic radiation, however the efficiency will be reduced.
The general properties of the PIXcel are given in Table 21.1.
07.12.04 Page 21.23

Figure 21.11: PW3018/00 PIXcel with PW3490/00 Fixed Anti-scatter Slit Mounted onto a
PW3017/00 PreFIX Interface
Page 21.24 07.12.04

Figure 21.12: PW3018/00 PIXcel Mounted onto a

PW3124/00 Diffracted Beam Monochromator for PIXcel
21.5.3 Accessories
21.5.3.1 PW3017/00 PreFIX Interface for PIXcel Used as a Line Detector
PW3017/00 is an interface to mount the PIXcel onto the 2theta arm of an X'Pert PRO goniometer for 1-D
applications. The PreFIX interface with a PIXcel with an anti-scatter slit mounted onto it is shown in Figure
21.11. The PreFIX interface contains a slot for Soller slits and a slot for a beta-filter.
21.5.3.1.1 Mounting the PIXcel onto the PreFIX Interface

Proceed as follows to mount the PIXcel onto the PreFIX interface:
1. Make sure that the diffracted beam anti-scatter shield, the Soller slits and the beta-filter are removed
from the interface.
2. Loosely mount the PIXcel onto the PreFIX interface using the two M3 x 8 screws provided (refer to
Figure 21.11).
3. Tighten the two screws to securely attach the PIXcel to the interface.
4. If required, you can now mount a diffracted beam anti-scatter device (see section 21.5.3), or insert
Soller slits or a beta-filter.
07.12.04 Page 21.25

21.5.3.1.2 Removing the PIXcel from the PreFIX Interface

You can remove the PIXcel from the PreFIX interface in order to mount it onto a PW3017/60 PreFIX interface
or onto the PW3124/00 Diffracted Beam Monochromator. To remove it from the PreFIX interface, proceed as
follows:
1. If present, remove the Soller slits and the beta-filter from their slots on the PreFIX interface.
2. Remove the diffracted beam anti-scatter device by undoing the two screws.
3. Undo the two screws holding the detector onto the interface.
Now you can remove the PIXcel from the interface and mount it onto the other interface or the diffracted beam
monochromator.
21.5.3.2 PW3017/60 Interface for PIXcel Used as a Point Detector

PW3017/60 is an interface to mount the PIXcel onto a diffracted beam PreFIX module, such as a parallel plate
collimator for 0-D applications. The PreFIX interface with a PIXcel mounted is shown in Figure 21.13. The
detector interface at the front is similar to the front of the proportional and scintillation detectors. The diffracted
beam PreFIX modules onto which the PIXcel can be mounted as a point detector is given in Table 21.2.
Figure 21.13: PIXcel with PW3017/60 Interface Mounted
Page 21.26 07.12.04

21.5.3.2.1 Mounting the PIXcel onto the Interface

Proceed as follows to mount the PIXcel onto the interface:
1. Loosely mount the PIXcel onto the PreFIX interface using the two M4 x 10 screws provided (refer to
Figure 21.13).
3. You can now insert the detector into its position in the detector interface of the diffracted beam PreFIX
module you are going to use. Detector mounting instructions are given in the chapter describing the
device onto which the detector is mounted, as shown in the third column in Table 21.2.
There are four types of beta-filter that can be used together with the PIXcel, they are:
Large Ni Filter (PW3158/03) for Cu Kα radiation.
Large Zr Filter (part of set PW3158/00) for Mo Kα radiation.
Large Fe Filter (part of set PW3158/00) for Co Kα radiation.
Large V Filter (part of set PW3158/00) for Cr Kα radiation.
The filter must be installed in the slot for beta-filter as shown in Figure 21.11.
Beta-filters and their use are described in Chapter 2 in Part II of this User's Guide.

Soller slits are used in the diffracted beam path to control the axial acceptance of the detector. Four Soller slits
are available for use with the PIXcel (see Figure 21.5), they are:
The Soller slits must be inserted into the slot for Soller slits on the PIXcel. To do this, insert the Soller slits
assembly into the slot until it clicks into place. For more information about Soller slits refer to Chapter 5 in Part
II of this User's Guide.
NOTE: Be careful not to interchange the PW3085/x1 Soller Slits with the PW3085/x0 Soller Slits, as they
are mechanically different.
21.5.3.5 PW3091/70 Programmable Anti-scatter Slit

The PW3091/70 Programmable Anti-scatter Slit (PASS) is used in combination with the PIXcel in order to
reduce the intensity of the background radiation to a low level. The programmable anti-scatter slit mounted onto
the PreFIX interface with the use of a PW3094/40 Mounting interface is shown in Figure 21.14.
Mounting instructions for the programmable anti-scatter slit are given in section 21.5.3.5.1 below.
07.12.04 Page 21.27

CAUTIONS 1. If you have mounted a programmable anti-scatter slit onto the

PIXcel, be careful to avoid collisions between the anti-scatter slit
and the sample stage or the sample itself.

the sample or the sample stage and the anti-scatter slit. You should
disable this automatic reset using the data collector software in
cases where collisions are possible. You then have the possibility to
remove the anti-scatter slit before resetting the system.
Figure 21.14: PW3091/70 Programmable Anti-scatter Slit with PW3094/40 Interface

Mounted onto the PIXcel
Page 21.28 07.12.04

21.5.3.5.1 Mounting the Programmable Anti-scatter Slit onto the PIXcel

Mount the programmable anti-scatter slit onto the PIXcel as follows:
1. Select the PIXcel PreFIX module with PASS in your configuration in the data collector software.
2. Make sure to switch the X'Pert PRO system off according to the procedure described in Chapter 4 in
Part I of this User's Guide. This is necessary because the distance between the slit and the sample has
been changed. Close the data collector software.
3. Bring the PW3094/40 Interface into position so that the two holes on this device fit into the
corresponding pins on the PW3017/00 PreFIX Interface for the PIXcel, refer to Figure 21.14.
5. Remove the programmable anti-scatter slit assembly from its interface by removing the interface
mounting screws indicated in Figure 16.1.
6. Bring the programmable anti-scatter slit assembly into position on the PW3094/40 Interface, so that the
two pins on this device fit into the corresponding holes in the PW3094/40 Interface, see Figure 21.10.
7. Tighten the programmable anti-scatter slit’s interface mounting screws so that it is secured to the
interface.
8. Switch the X'Pert PRO system on according to the procedure described in Chapter 4 in Part I of this
User's Guide. Start up the data collector software and go on-line with the configuration that you are
going to use.
21.5.3.6 PW3490/00 Fixed Anti-scatter Slit for PIXcel

A fixed anti-scatter slit is mounted onto the PIXcel to reduce the intensity of the background radiation to a low
level. The fixed anti-scatter slit holder mounted onto the PIXcel is shown in Figure 21.11. When the PIXcel is
used for measurements on samples in glass capillaries or in combination with Anton Paar chambers or on the
MRD additional anti-scatter devices must be mounted onto the fixed anti-scatter slit holder. Mounting
instructions for the fixed anti-scatter slit holder are given in section 21.5.3.6.1 below. Mounting the PW3490/32
and PW3494/35 Anti-scatter Slits onto the fixed anti-scatter slit holder is described in sections 20.3.5.1.1.1 and
20.3.5.1.2.1 in Chapter 20 in Part II of this User's Guide.
More information about the PW3490/00 and its use is given in section 20.3.5 of Chapter 20 in Part II of this
User's Guide.
CAUTIONS 1. If you have mounted a fixed anti-scatter slit holder onto the PIXcel,
be careful to avoid collisions between the anti-scatter slit holder
and the sample stage or the sample itself.

the sample or the sample stage and the anti-scatter slit holder. You
should disable this automatic reset using the data collector
software in cases where collisions are possible. You then have the
opportunity to remove the anti-scatter slit holder before resetting
the system.
07.12.04 Page 21.29

21.5.3.6.1 Mounting the Fixed Anti-scatter Slit Holder onto the PIXcel
Mount the fixed anti-scatter slit holder onto the PIXcel as follows:
1. Bring the fixed anti-scatter slit holder into position so that the two holes on this device fit into the
corresponding pins on the PIXcel, refer to Figure 21.11.
21.5.3.7 PW3490/32 Anti-scatter Slit

The PW3490/32 Anti-scatter Slit for the PIXcel must be mounted onto PW3490/00 Fixed Anti-scatter Slit
Holder when the PIXcel is used for measurements in combination with Anton Paar non-ambient chambers or
with the X'Pert PRO MRD. It is used to reduce the amount of scattered radiation that enters the detector. The
PW3490/32 Fixed Anti-scatter Slit is described in detail in section 20.3.6 of Chapter 20 in Part II of this User's
Guide. Mounting the anti-scatter slit onto the fixed anti-scatter slit holder is described in section 20.3.5.1.1.1 of
21.5.3.8 PW3494/35 Anti-scatter Slit

The PW3494/35 Anti-scatter Slit must be mounted in the diffracted beam path onto PW3490/00 Fixed Anti-
scatter Slit Holder when the PIXcel is used in combination with a PW3063/00 Capillary Spinner in order to
reduce the amount of scattered radiation entering the detector. Information about the PW3494/35 Fixed Anti-
scatter Slit is given in section 20.3.7 of Chapter 20 in Part II of this User's Guide. Mounting the anti-scatter slit
onto the fixed anti-scatter slit holder is described in section 20.3.5.1.2.1 of Chapter 20 in Part II of this User's
Guide.
21.5.3.9 PW3490/50 Fixed Anti-scatter Slit for PIXcel Monochromator

PW3490/50 is a set of fixed anti-scatter slits marked 15.8 mm, 10.4 mm, 7.7 mm, 6.4 mm, 5.7 mm and 0.2 mm
for use with the PW3124/00 Diffracted Beam Monochromator and PIXcel detector. They can be inserted into
the slit holder supplied. These slits are used to reduce the amount of scattered radiation entering the PIXcel
detector equipped with the PW3124/00 Monochromator. Mounting instructions are given in section 19.4.2.1.1
of Chapter 19 of Part II of this User's Guide. Information about how to use these fixed anti-scatter slits is given
in section 20.3.7 of Chapter 20 of Part II of this User's Guide.
21.5.3.10 PW3124/00 Diffracted Beam Monochromator for PIXcel

The PIXcel can be used together with a PW3124/00 Diffracted Beam Monochromator for PIXcel and copper
radiation to reduce the background radiation and sample fluorescence, and to eliminate unwanted lines. It is
The monochromator comprises a PreFIX T-block to mount it onto the diffracted beam arm of the goniometer,
and a detector interface to mount the PIXcel. Mounting instructions are given below. If necessary you can mount
a fixed anti-scatter slit holder onto the monochromator.
More information about the monochromator can be found in section 19.4.2 of Chapter 19 in part II of this User's
Guide.
21.5.3.10.1 Mounting the PIXcel onto the PW3124/00 Diffracted Beam Monochromator
Proceed as follows to mount the PIXcel onto the PW3124/00 Diffracted Beam Monochromator:
1. If necessary, remove the PIXcel from its PreFIX interface, refer to section 21.5.3.1.2.
2. Bring the PIXcel into position on the detector interface on the diffracted beam monochromator as
3. Insert and loosely tighten the two M3 x 8 screws supplied to attach the PIXcel to the interface.
The PIXcel with its monochromator is now ready for use. No further alignment is required.
Page 21.30 07.12.04
21.5.4 Use
The PIXcel does not use counting gas or cooling liquids, so no additional system maintenance is required.
The use of the PIXcel in alignment procedures is given in the appropriate sections throughout this User's Guide.
This section describes:
• Selecting the PIXcel’s PHD levels.
• The operating modes of the PIXcel.
• How to optimize measurements with the PIXcel.
• Suppression of background radiation and unwanted lines in diffractograms.
21.5.4.1 Selecting PHD Levels

You can set the lower and upper detection levels to select the energy range of the X-ray photons to be detected.
Typical PHD levels for the PIXcel are 25% and 70% for the lower and upper level respectively. We recommend
setting the PHD levels to the factory levels in the data collector software.
If the sample shows strong fluorescence, you may reduce this effect by choosing the lower level closer to the
50% level of the main energy peak, for example: 45%. However, remember that you also discard part of the
diffraction signal when you do that. Better ways of reducing sample fluorescence are either to use a
monochromator, or an X-ray tube with a different anode material.

The PIXcel can be used in three distinctive modes:
• Scanning mode
In the scanning mode, the PIXcel is moved over the 2θ range-of-interest at each step along the scan; the
intensity at that particular 2θ position (data point) is measured and then summed, until the data point is
no longer in range. When the PIXcel is used over its total active length (14 mm) its opening (height) is
about 3.3º 2θ on an X'Pert PRO system with a radius of 240 mm or about 2.5° 2θ on an X'Pert PRO
MRD system. It is possible to reduce the active length using the data collector software. When
extremely well-defined powders are measured, such a reduction can lead to sharper peaks in the diffrac-
togram. However, for the vast majority of powder samples, you do not need this option.
Scans measured in the scanning mode are continuous scans. Their axis can be: gonio, 2theta, 2theta-
omega and omega-2theta.
In the scanning mode, the only 2-axes measurements that are allowed are those in which a gonio scan, a
2θ scan or a 2θ - ω scan is one of the directions.
• Receiving slit mode
In the receiving slit mode, the intensity of the radiation entering the detector is added together over its
complete active length. This option is used for alignment of system components, such as the tube height
or the sample surface. You can use the receiving slit mode to record pole figures or for stationary
measurements.
All 2-axes measurements are allowed in the Receiving slit mode.
• Static mode
In the static mode, the PIXcel does not move along the 2θ circle. Each of the PIXcel's channels corre-
sponds to a unique 2θ value. Scans measured in the static mode are stepped scans with a 2theta scan
axis. You cannot perform a stationary measurement in this mode.
NOTE: When you are setting up a measurement program in the data collector software you must explicitly
specify the PIXcel's operating mode in the measurement conditions. If you leave this at “Actual”,
the PIXcel will be automatically set into the Scanning mode with maximum active length.
07.12.04 Page 21.31

21.5.4.3 Optimizing Measurements with the PIXcel

The resolution of a measurement on a flat powder sample using the PIXcel can be optimized by selecting the
appropriate divergence slit size, its active length, anti-scatter device and beam knife.
• Divergence slit size
To optimize the resolution of a measurement with the PIXcel, you should use a very narrow divergence
slit in the incident beam path. For normal applications you can use a 1°, a ½°, or a ¼° divergence slit.
For measurements at low angles of incidence or measurements on small samples, we advise you to use
a narrower divergence slit: 1/8°, 1/16° or 1/32° in order to prevent over-irradiation of the sample.
• Active length
It is possible to reduce the active length of the PIXcel; in this way only a part of the PIXcel is activated.
X-ray photons falling outside the active length are collected but are filtered out electronically.
Reducing the active length can lead to a better peak shape of the reflections observed. However, this
can only be observed in diffractograms measured on extremely well-defined powder samples. In all
other cases, you should use the PIXcel over its complete length.
• Anti-scatter devices
Anti-scatter devices can be mounted in the incident and the diffracted X-ray beam path in order to
reduce the intensity of the background radiation caused by scattered X-rays.
An incident beam anti-scatter slit holder can be mounted onto the (fixed or programmable) divergence
slit module. This type of anti-scatter device is described in section 20.2.1 of Chapter 20 in Part II of this
User's Guide. The choice of the anti-scatter slit size to be used during the diffraction experiment is
determined by the size of the divergence slit selected. The optimal anti-scatter slit size is twice that of
the size of the divergence slit.
Special incident beam anti-scatter devices can be used with X-ray mirrors or hybrid monochromators in
measurements on samples in glass capillaries in transmission measurements or in high-throughput
applications. These types of anti-scatter device are described in sections 20.2.2 to 20.2.5 in Chapter 20
The PW3091/70 Programmable Anti-scatter Slit can be mounted onto the PIXcel (refer to section
21.4.3.6). The choice of the anti-scatter slit size to be used during the diffraction experiment is
determined by the divergence slit size selected. Information about operating modes of the
programmable anti-scatter slit is given in section 16.2.2.2.1 in Chapter 16 of Part II of this User's Guide.
The PW3490/00 Fixed Anti-scatter Slit Holder is used in the diffracted beam path. This holder has a
slot to accommodate a fixed anti-scatter slit. Selecting the correct slit size fir the task in hand is
described in section 20.3.1.2 in Chapter 20 of Part II of this User's Guide. For measurements on samples
in glass capillaries or in combination with Anton Paar non-ambient chambers, special anti-scatter slits
can be mounted onto this fixed anti-scatter slit holder. Diffracted beam anti-scatter devices for use with
the PIXcel are described in detail in section 20.3.4 to 20.3.7 in Chapter 20 of Part II of this User's
Guide.
• Beam knife
In addition to the anti-scatter devices, a beam knife can be inserted in the X-ray beam path to reduce the
background intensity due to scattered radiation to a low level. Several types of beam knife can be used;
they are specific to the sample stage used. An overview of the available types is given in section 14.3 of
Chapter 14 of Part II of this User's Guide. For optimum use of the beam knife the gap between the beam
knife and the sample surface should be as small as possible without obstructing the incident and the dif-
fracted X-ray beams. A procedure for calculation of the optimum height is given in section 14.3.6 of
21.5.4.4 Suppression of Unwanted Radiation

The energy resolution of the PIXcel is around 25%, which is comparable with a proportional detector. This
Page 21.32 07.12.04
means that additional X-ray optical components need to be inserted in the X-ray beam path to reduce the
intensity of unwanted radiation, such as Cu Kβ or white radiation. The intensity of unwanted radiation can be
reduced in the following ways:
• Beta-filter
For most powder samples, a beta-filter is sufficient to reduce Kβ radiation. For example, with a
PW3158/03 Ni filter inserted into the PIXcel, the intensity of the Cu Kβ peak is reduced to less than 1%
of the Cu Kα peak. If you need better suppression of the Cu Kβ peak, we recommend that you use an
additional Ni filter, so that one is inserted in the incident beam optical module, and the other is inserted
in the PIXcel.
• Diffracted Beam Monochromator
For samples yielding fluorescent radiation (a well-known example is that of samples containing iron
when copper radiation is being used) we advise using a PW3124/00 Diffracted Beam Monochromator
in combination with Cu Kα radiation. Fluorescence is almost completely eliminated when you use a
diffracted beam monochromator. If required, it is possible to use this monochromator in combination
with a Ni filter in order to reduce the intensity of the Cu Kβ peaks to a very low level.
07.12.04 Page 21.33

Page 21.34 07.12.04

Appendices
Appendix A
Sample Holders
Contents
A.1 General...............................................................................................................................A - 3
A.2 Sample Holders for Spinner.............................................................................................A - 3
A.2.1 PW18xx Series Holders .......................................................................................................A - 3
A.2.1.1 PW1811/xx Sample Holders for Manually Prepared Powder Samples...............A - 3
A.2.1.2 PW1812/00 Sample Holders for Non-standard Sample Sizes and Shapes..........A - 5
A.2.1.3 PW1812/35 Sample Holders for Automatically Prepared Powder Samples .......A - 5
A.2.1.4 PW1813/xx Sample Holders for Circular Shaped Solid Samples .......................A - 6
A.2.1.5 PW1814/32 Sample Holders for Clay Samples and Paste Materials...................A - 7
A.2.1.6 PW1815/40 Insert for Air Sensitive Samples ......................................................A - 7
A.2.1.7 PW1816/32 Porous Ceramic Filter Plate .............................................................A - 8
A.2.1.8 PW1817/32 or PW1819/32 Zero Background Holder.........................................A - 8
A.2.1.9 PW1818/xx Sample Holders for Transmission Measurements ...........................A - 9
A.2.1.10 Accessories ........................................................................................................A - 10
A.3 Stationary Sample Holders ............................................................................................A - 12
A.3.1 PW1172/01 Rectangular Sample Holders..........................................................................A - 12
A.3.2 PW1819/25 Set of 15 Zero Background Holders...............................................................A - 13
A.4 Capillary Samples ...........................................................................................................A - 13
A.5 References........................................................................................................................A - 13
07.03.29 Page A.1

Page A.2 07.03.29

Appendix A: Sample Holders
A.1 GENERAL
This chapter gives a description of the sample holders used with the X’Pert PRO system:
- the PW18xx range of sample holders (section A.2)
- the stationary sample holder PW1172/01 (section A.3)
- the capillary sample holder (section A.4)
A.2 SAMPLE HOLDERS FOR SPINNER

This section describes the PW18xx range of sample holders for use with the PW3064/x0 Sample Spinner and
the PW3076/00 Sample Spinner for Transmission and Reflection Geometries. These sample holders can also be
mounted in the PW3072/60 Stationary Sample Stage, on the PW3074/00 Multi-purpose Sample Stage and on
the PW3061/21 Sample Holder for solid samples to be used with the PW3060/20 MRD Cradle or with the
PW3075/62 Positioning Stage with motorized Z, Tilt and Phi movements.
A.2.1 PW18xx Series Holders

A description of the sample holders in the PW18xx series, and their applications, is contained within this section.
The sample holders described in this section are all listed in Table A.1.
A.2.1.1 PW1811/xx Sample Holders for Manually Prepared Powder Samples
Figure A.1: PW1811/xx Sample Holder

The PW1811/16 and PW1811/27 Sample Holders are designed for the manual or semi-automatic preparation of
powder samples which can be either back-loaded or front-loaded.
The common bottom plate for both rings is the PW1811/00, which supports the powder and enables loading into
the PW3064/x0 Sample Spinner. The diameters of the cavities to be filled are 16 mm and 27 mm, respectively.
Note that the powder volume of the PW1811/16 is little more than one third that of the
PW1811/27. The ring is 2.4 mm thick.
Applications: General powder analysis. Powders with a maximum particle size of 25 μm, and of
low or average density, can be applied without a binder in most cases.
Measurement range: From 0° 2θ upwards, without obscuring the sample surface.
07.03.29 Page A.3

Table A.1: Sample Holder Selection
Number Material and

Type Number Outline Use
Supplied Treatment
PW1811/00 3 Steel (nickel finish) Common bottom plate
PW1811/16 3 Steel (nickel finish) Back-loading or

front-loading of
PW1811/27 3 powders
PW1812/00 3 Steel (nickel finish) Odd shapes, fixed with

wax or plasticine
PW1812/35 25 Tempered stainless Press ring for powders

steel (cement etc.)
PW1813/26 3 Steel (nickel finish) Metal plates, mem-

brane filters, pressed
pellets, etc.
PW1817/32,
PW1813/32 3 PW1819/32
PW1813/40 3
PW1814/32 3 Steel (nickel finish) PW1816/32 Holder for

clays.
Paste-like materials on
aluminium plate.
PW1817/32 or
PW1819/32 can be
used as an alternative.
PW1815/40 & 3 Stainless steel (bot- Samples sensitive to

9430 500 21011 500 tom plate), poly- air. To be used with
oxymethylene (ring) PW1813/40.
and kapton (foil)
PW1816/32 25 Ceramic With PW1814/32 for

clays
PW1817/32 2 Silicon (single crystal) Small amounts of

PW1819/32 15 powder, with
PW1813/32 or
PW1812/00.
Paste materials with
PW1814/32.
PW1818/40 & 3 Steel, nickel finish Fibers or (samples

PW1818/25 3 and spring steel between) foils to be
(upper part). measured in
Stainless steel and transmission mode.
polyoxymethylene
(lower part)
Page A.4 07.03.29

A.2.1.2 PW1812/00 Sample Holders for Non-standard Sample Sizes and Shapes
Figure A.2: PW1812/00 Sample Holder with Sample
The PW1812/00 can be used to analyze solid samples with a maximum diameter of 45 mm and a maximum
thickness of 6.5 mm, or powder samples pressed into a collapsible aluminium cup (PW1526/50). The sample
can be mounted with wax or plasticine.
Applications: Irregularly shaped solid objects, metal parts, ceramic test pieces, pieces of rock,
pressed pellets, and mounting plates (for example PW1817/32 or PW1819/32)
with powder samples.
A.2.1.3 PW1812/35 Sample Holders for Automatically Prepared Powder Samples
Figure A.3: PW1812/35 Sample Holder

The PW1812/35 Sample Pressing Ring is designed for use with (semi-)automatic hydraulic sample presses with
cylindrical pistons of 35 mm. The external shape is compatible with automatic/robotic sample handling
equipment.
Applications: Automatic cement analysis, and other industrial process control applications.
07.03.29 Page A.5

A.2.1.4 PW1813/xx Sample Holders for Circular Shaped Solid Samples
Figure A.4: PW1813/xx Sample Holder
The PW1813/26, PW1813/32 and PW1813/40 range of sample holders are designed for mounting dust filters,
sample mounting plates (for example, PW1816/32 and PW1817/32 or PW1819/32), metal plates, pressed pellets
and so on. The PW1813/40 can also be used to hold powder samples pressed into a collapsible aluminium cup
(PW1526/50) or samples sensitive to air that are prepared in a PW1815/40 Sample Holder.
The minimum and maximum sample diameters that can be accommodated by this range of holders are as
follows:
PW1813/26: 24 mm to 26.3 mm
PW1813/32: 30 mm to 32.3 mm
PW1813/40: 37.5 mm to 40.3 mm
Maximum sample thickness that can be accommodated is 6 mm.
Applications: Used in the analysis of air filters for occupational and environmental dust. The filter
sizes that can be accommodated by this range of holders are 25 mm (1 inch), 32 mm
(1.25 inch), and 38 mm (1.5 inch). Also, metal plates, pressed pellets, and other
solid objects, as long as they fit between the minimum and maximum dimensions
that can be accommodated.
The PW1813/32 can be used in conjunction with the PW1817/32 or PW1819/32
Zero Background Holders. The latter, with their low background, are ideally suited
for extremely small amounts of powder and for fiber analysis.
The PW1813/40 can be used in conjunction with samples prepared in a
PW1526/50 Collapsible Aluminium Cup using a powder press. The PW1813/40
can also be used with the PW1815/40 for measurements of (powder) samples that
are sensitive to air, oxygen or humidity. The sample material is covered by a thin
X-ray transparent foil. If there is only a small amount of sample material the
PW1817/32 or PW1819/32 Zero Background Holders can be inserted into the
PW1815/40 as a sample support.
Measurement range: Minimum 2θ angle for each type is dependent on the divergence slit and mask
dimensions used together with the PW1813/xx Sample Holder. The incident beam
is partly obscured by the sample holder at low angles of incidence.
Page A.6 07.03.29

A.2.1.5 PW1814/32 Sample Holders for Clay Samples and Paste Materials

The PW1814/32 Sample Holder is designed for use with the PW1816/32 Ceramic Filter Plate for the analysis of
clay minerals. Additionally, it can be used for all types of paste-like materials applied to the aluminium support
plate.
Maximum diameter of clay sample which can accommodated is 29 mm with a thickness between 0.4 mm and
0.5 mm.
Applications: Clay minerals can be applied using the suction method [A.1], taking the clay
sample dimensions into account.
Grease, margarine, and other paste-like materials may be spread onto the support
plate with a spatula or knife. In such applications, the PW1817/32 or PW1819/32
will offer a low background alternative to the support plate.
A.2.1.6 PW1815/40 Insert for Air Sensitive Samples

PW1815/40 consists of a set of three inserts designed for use with the PW1813/40 Sample Holder for the
measurement of samples that are sensitive to air, oxygen or humidity. Alternatively, these inserts can be
combined with the PW1818/40 Sample Holder. 9430 500 21011 X-ray Transparent Foils are used to cover the
sample to shield it from the environment.
The insert consists of a steel bottom plate with a ring into which the sample material can be inserted. The sample
is covered by Kapton foil that is clamped onto the bottom plate using a polyoxymethylene ring. The inner
diameter of the insert is 35 mm and the height is 2 mm. A PW1817/32 or PW1819/32 Zero Background Holder
can be inserted to support the sample if there is not very much sample material.
Figure A.6: PW1815/40 Insert for Air Sensitive Samples

Preparation of samples in a PW1815/40 Insert is described in section B.2.4 of Appendix B of this User's Guide.
07.03.29 Page A.7

Applications: Measurements of powders, paste-like materials, and so on, that are sensitive to air.
The PW1815/40 can be used in conjunction with the PW1817/32 or PW1819/32
Zero Background Holders. Because of their low background intensity, the
PW1817/32 and PW1819/32 are ideally suited for extremely small amounts of
sample material.
Measurement range: Minimum 2θ angle for each type is dependent on the divergence slit and mask
dimensions used together with the PW1813/40 or PW1818/40 Sample Holder. The
incident beam is partly obscured by the sample holder at low angles of incidence.
A.2.1.7 PW1816/32 Porous Ceramic Filter Plate
Figure A.7: PW1816/32 Porous Ceramic Filter Plate

The PW1816/32 Sample Holder is a ceramic filter plate to be used with the PW1814/32 for clay mineral samples.
Diameter range of the disk is between 31.8 mm and 32.2 mm, with thicknesses between 3.3 mm and 3.7 mm.
Material: Porous aluminium oxide, mean pore size 3.5 μm.
Applications: Clay minerals applied using the suction method (refer to the PW1814/32
description). In designing the suction device, consideration should be given to the
dimensions given in the previous paragraph.
Measurement range: Depends on the holder in which it has been mounted.
A.2.1.8 PW1817/32 or PW1819/32 Zero Background Holder
Figure A.8: PW1817/32 Zero Background Holder

The zero background holder is an obliquely cut silicon crystal with a 32 mm diameter and 2 mm thickness, this
holder can be used together with PW1813/32 and PW1812/00 Sample Holders. It is supplied in sets of 2 pieces
(PW1817/32) and 15 pieces (PW1819/32).
Both sides of the sample holders can be used; one side is flat and can be used to mount very small amounts of
powder (<1 mg), glass capillaries and fibers according to the zero background holder sample mounting method
[A.2]. The other side contains a cavity with diameter of 16 mm and a depth of 0.2 mm, which can be filled with
sample material.
Page A.8 07.03.29

These sample holders are suitable for those applications where a low background factor is critical.
The zero background holder can also be used in PW1814/32 Sample Holders as a support plate for paste
materials. It is an alternative to the metal support plate when the background intensity must be low.
Applications: To obtain the lowest background, apply a drop of alcohol or a smear of petroleum
jelly, and sprinkle the powder sample onto it. Glass capillaries can be attached by
applying minute amounts of petroleum jelly at the tips. Short fibers can be attached
in the same way. Long fibers can be wound around the plate.
Measurement range: Depends on the holder in which the sample has been mounted.
A.2.1.9 PW1818/xx Sample Holders for Transmission Measurements

PW1818/xx Sample holders are designed for measuring samples in transmission geometries.
PW1818/25 consists of three sets of inserts, as is shown in Figure A.9. The inserts can be used to clamp a variety
of samples, such as thin foils, fibers or powder or paste-like samples between Kapton foils for analysis in
transmission. The inner ring diameter is 25 mm.
Powder or paste-like samples are prepared between two Kapton foils that are clamped onto the insert ring with
the two polyoxymethylene rings.
Figure A.9: PW1818/25 Sample Holder Insert for Transmission Measurements

The PW1818/40 Sample Holder Ring supports inserts with a thickness of 6 mm and a diameter of 40 mm (such
as the PW1818/25 Insert) to enable loading into the PW3064/60 or the PW3076/00 Sample Spinners for
transmission and reflection geometries. It is shown in Figure A.10. Inserts are clamped into the ring using the
circular spring.
Figure A.10: PW1818/40 Sample Holder Ring for Transmission Measurements
07.03.29 Page A.9

Preparation of samples in a PW1818/25 and PW1818/40 Sample Holders is described in section B.2.3 of
Appendix B of this User's Guide.
Applications: Powder or paste-like samples can be prepared between two foils for the analysis in
transmission mode. Thin polymeric foils or fibers can be clamped onto the sample
holder between the two inner rings.
Measurement range: From 0° 2θ onwards. The maximum measurement angle in a symmetrical scan in
transmission mode is 90° 2θ with the PW3064/60 Sample Spinner and 120° 2θ with
the PW3076/00 Transmission Spinner.
A.2.1.10 Accessories
A.2.1.10.1 PW1526/50 Set of Collapsible Aluminium Cups
Figure A.11: PW1526/50 Aluminium Cup
Figure A.12: PW1526/50 Aluminium Cup after Sample Preparation

PW1526/50 is a set of 2400 collapsible aluminium cups. These cups are used for the preparation of pressed
powder samples, utilizing a powder sample press like the 9430 500 70821 TP Laboratory Press with the
9430 500 70831 Press Tool. When pressed, the samples fit in the PW1813/40 Sample Holder for Circular Shaped
Samples. Alternatively, they can be mounted into a PW1812/00 Sample Holder with the use of wax or plasticine.
Page A.10 07.03.29

A.2.1.10.2 9430 500 21011 X-ray Transparent Foils

9430 500 21011 is a set of 500 X-ray transparent foils, made from Kapton (polyimide). The foils are circular in
shape with a diameter of 63.5 mm and a thickness of 7.5 µm. The foils are used in combination with:
• PW1815/40 Insert for air sensitive samples to protect sample from air during X-ray diffraction
experiments.
• PW1818/25 Sample holder for transmission measurements for the preparation of powder samples,
paste-like materials, and so on.
NOTE: When Kapton foils are used to mount the sample into the sample holder, it is possible that a
reflection around 5° 2θ is visible in the diffractogram.
Figure A.13: 9430 500 21011 X-ray Transparent Foils
07.03.29 Page A.11

A.3 STATIONARY SAMPLE HOLDERS

A.3.1 PW1172/01 Rectangular Sample Holders
The PW1172/01 Sample Holders (sets of 25) are aluminium holders for powder samples with a volume of
15 mm x 20 mm x 1.8 mm available for use with X’Pert PRO MPD systems, with a PW3071/60 Stage for Flat
Solids or Powders in Flat Holders or a PW3074/00 Multi-purpose Sample Stage.
One back plate per sample holder is included, this allows the back-loading technique to be employed in this type
of sample holders.
Page A.12 07.03.29

A.3.2 PW1819/25 Set of 15 Zero Background Holders
Figure A.15: PW1819/25 Zero Background Holder

PW1819/25 Set of Zero Background Holders consists of 15 obliquely cut silicon single crystals with a diameter
of 25 mm and 2 mm thickness. The zero background holder is shown in Figure A.15.
Both sides of the sample holders can be used; one side is flat and can be used to mount very small amounts of
powder (<1 mg), glass capillaries and fibers according to the zero background holder sample mounting method
[A.2]. The other side contains a cavity with diameter of 10 mm and a depth of 0.2 mm, which can be filled with
sample material.
These sample holders are suitable for those applications where a low background factor is critical.
The zero background holders can be used together with the multiple sample holder, supplied with the
PW3077/00 High-throughput Attachment for X'Pert PRO MPD systems.
A.4 CAPILLARY SAMPLES

When substances under investigation are sensitive to humidity or oxygen, or could be dangerous to the operator's
health, small amounts of the substance can be put into a glass capillary. Once filled, the capillary is sealed and
mounted onto a PW3063/00 Capillary Spinner Sample Stage. This sample stage spins the glass capillary to
improve particle statistics. A goniometer head is used to align the glass capillary with respect to the heart of the
goniometer.
A.5 REFERENCES
A.1 E.G. Kinter, S. Diamond, (1956) “A new method for preparation and treatment of oriented-aggregate
specimens of soil clays for X-ray diffraction analysis”, Soil Sci. 81, 111-120.
A.2 H. P. Klug, L. E. Alexander, “X-ray Diffractometry Procedures for Polycrystalline & Amorphous
Materials”, J. Wiley & Sons Inc. (New York) 1974. ISBN 0-471-49369-4.
07.03.29 Page A.13

Page A.14 07.03.29

Appendix B
Sample Preparation
Contents
B.1 General............................................................................................................................... B - 3
B.1.1 Grinding................................................................................................................................B - 3
B.1.2 Mechanical Pelletizing .........................................................................................................B - 4
B.2 Sample Preparation for PW18xx Sample Holders ........................................................ B - 4
B.2.1 PW1770/10 Powder Sample Preparation Kit .......................................................................B - 4
B.2.2 Standard Sample Preparation ...............................................................................................B - 5
B.2.3 Sample Preparation for Transmission ..................................................................................B - 9
B.2.4 Preparation of Air Sensitive Samples.................................................................................B - 11
B.2.5 Non-standard Sample Preparation......................................................................................B - 14
B.3 Sample Preparation For Stationary Sample Holders.................................................. B - 16
B.3.1 Sample Preparation Equipment ..........................................................................................B - 16
B.3.2 Standard Sample Preparation .............................................................................................B - 16
B.3.3 Non-standard Sample Preparation......................................................................................B - 19
B.4 Sample Preparation for Samples in Glass capillaries.................................................. B - 21
B.4.1 General ...............................................................................................................................B - 21
B.4.2 Capillary Sample Preparation.............................................................................................B - 21
B.4.2.1 Sample Preparation Equipment .........................................................................B - 21
B.4.2.2 Preparing a Capillary Sample ............................................................................B - 22
B.5 References........................................................................................................................ B - 26
07.03.29 Page B.1

Page B.2 07.03.29

Appendix B: Sample Preparation
B.1 GENERAL
The preparation of samples for analysis is of critical importance if accurate and fast results are to be obtained,
and the procedures detailed in this section should be carefully followed.
Additionally, the introduction of errors, such as contamination, material loss, alteration of composition,
especially of the sample surface, and change of lattice type, during the course of sample preparation, and
afterwards, should be avoided.
Contamination of the sample can be caused by dust, material from a previous sample which remained in the
sample preparation equipment, or by material from the sample preparation equipment resulting from abrasion.
Material loss is attributed to non-quantitative transfer in concentration determining operations (dilution, binder
addition), loss of a small fraction of particle size as dust, and material remaining in the sample preparation
equipment.
Alteration of composition is attributed to losses of material particles which are of different composition to the
average composition. For example, magnetic particles, fine dust, and volatile substances. Also, physical or
chemical alteration; that is, by decomposition during preparation, such as oxidation, loss of combined water or
carbon dioxide by overheating and pick-up of water or carbon dioxide from the air, or by the addition of
materials of different composition such as by contamination.
Change of lattice type; that is, transition to another phase, is attributed to pressure, temperature, humidity, or a
combination of these.
The sample surface is only measured up to a depth of 1 or 2 mm in some cases, but in most cases only a hundred
micrometers or even less. Typical examples of errors which can occur here are non-representativeness (sample
surface has different composition than the average composition) caused by segregation, adhering particles or
extracted particles, smearing and bad particle statistics, non-uniformity (sample surface is not equal for all
samples) such as non-flat samples (concave or convex), or differences in surface roughness.
Most of the errors can be avoided if samples are prepared carefully with cleaned equipment in a clean room.
Once samples have been prepared they must be stored in a dust-free environment such as desiccators sometimes
under vacuum or filled with moisture absorbers like Silica gel. If samples are difficult to handle, use pincers or
gloves.
Samples for X-ray analysis should be, in effect, infinitely thick, depending on the energy of the X-ray line and
the matrix of the samples. Usually a 2 to 3 mm thickness seems to be sufficient. Once the sample has been
prepared, care should be taken that it fits into the holder properly.
To achieve a sufficient sample strength during sample preparation, the sample must be ground very fine,
achieving an average grain size of 5 μm, with a maximum grain size of 25 μm. If both hard and soft materials
are present together, the required size reduction of particles might be achieved by pressing the sample instead
of grinding. This may prevent the softer material being ground by the harder one.
General information on sample preparation can be found in [B.1, B.2].
B.1.1 Grinding
The penetration of the X-ray beam (Cu Kα) is in the order of 100 μm, so the grain size should be between 5 and
10 μm in order to ensure that sufficient grains of the various compounds contribute to the reflection of the beam.
However, this requirement is difficult to meet due to the time required for grinding. Also, the heat produced by
prolonged motorized grinding can introduce changes in the sample. Therefore, a grain size of 25 μm must
sometimes be accepted. A grinding agent such as alcohol or water, can be used to prevent heating of the sample
and to reduce grinding time.
07.03.29 Page B.3

B.1.2 Mechanical Pelletizing

A uniform amount of material, under constant pressure, for a set period of time, will ensure a sample of constant
and uniform density. Using a powder press will also ensure that the height of the sample is reproducible, thus
avoiding shifts in the 2θ angle.
Ideally, mechanical pelletizing should be carried out using a powder sample press with an adjustable pelletizing
pressure, which can be applied for a pre-determined time. If small numbers of samples are going to be analyzed,
a hand operated powder sample press can be used (for example: a PW4020 MiniPress). For even more uniformity
and/or larger numbers of samples, an automated pressing machine can be used (for example: a Herzog HTP40).
The sample surface should be flat and flush with the sample holder. Therefore, “back-filling” against a flat plate
is recommended.
B.2 SAMPLE PREPARATION FOR PW18XX SAMPLE HOLDERS

B.2.1 PW1770/10 Powder Sample Preparation Kit
The PW1770/10 Powder Sample Preparation Kit is designed for powder samples in the PW18xx Sample Holder
series.
The kit, illustrated in Figure B.1, comprises a sample preparation table onto which the sample holder ring is
clamped, a powder press block (or piston), a dusting brush, and a Stanley knife blade. Figure B.2 shows the
sample holder ring clamped onto the preparation table.
Figure B.1: PW1771/10 Powder Sample Preparation Kit
Page B.4 07.03.29

Figure B.2: Sample Holder Ring on Sample Preparation Table
B.2.2 Standard Sample Preparation

The sample preparation method described in this section makes use of the PW1770/10 Powder Sample
Preparation Kit. Refer to section B.2.1 and Figure B.1 for a description of this kit.
When the sample material has been prepared, proceed as follows:
1. Ensure that the sample holder ring is securely clamped to the preparation table (Figure B.2).
2. Spread the powder sample in the holder ring, so that the powder is heaped up into a conical shape inside
the holder ring (see Figure B.3). Alternatively, you can use a sieve to sift an excess of powder into the
cavity.
3. Press the powder down firmly in the holder ring using the powder press block. Ensure that a firm and
even pressure is applied by hand to the press block (see Figure B.4).
4. Using the knife blade, scrape any powder that flows out during the above pressing operation back into
the holder ring (see Figure B.5). If required, you can spread or sift a new layer of powder on top of the
surface, and press down again using the powder press block. Keep repeating this step until you have a
nice densely packed powder specimen.
5. Remove all surplus powder above the rim of the holder ring using the knife blade and then the dusting
brush to make the sample as shown in Figure B.6.
6. Place the bottom plate onto the holder ring, and clamp in position (see Figure B.7), make sure not to
click it into place too harshly as the powder sample could become loose or even damaged.
7. Remove the complete sample holder from the preparation table by turning the sample preparation table
upside down and pressing the spring loaded knob, Figure B.8 shows the sample holder separated from
the preparation table.
NOTE: When using sample holders in the X’Pert PRO system, the reference plane of the holder must
always be kept very clean, and any spilled powder must be removed before loading a sample. The
reference plane is the outer rim of the holder, where it is in contact with the three ball bearings of
the sample spinner in the measuring position.
07.03.29 Page B.5

Figure B.3: Spreading Powder in Sample Holder Ring
Figure B.4: Pressing Powder with Powder Press Block
Page B.6 07.03.29

Figure B.5: Removing Surplus Powder from Holder Ring
Figure B.6: Holder Ring with Surplus Powder Removed
07.03.29 Page B.7

Figure B.7: Bottom Plate Clamped onto Holder Ring
Figure B.8: Complete Sample Holder Removed from Preparation Table
Page B.8 07.03.29

B.2.3 Sample Preparation for Transmission

This section describes sample preparation for transmission experiments. This procedure makes use of the
PW1818/25 and PW1818/40 sample holders and the 9430 500 21011 Kapton foils.
1. Ensure that you have the complete set of the PW1818/xx Sample Holders and rings and two Kapton
foils as is shown in Figure B.9.
Figure B.9: PW1818/25 Transmission Insert, PW1818/40 Sample Holder Ring and Two Kapton Foils
2. Place one Kapton foil over the insert (see Figure B.10) and clamp it with the smaller white ring. Now
you can spread a small amount of sample material, for instance a powder or a paste-like substance onto
the Kapton foil.
Figure B.10: Spreading the Powder onto the Sample Holder

3. Cover the sample with the second Kapton foil and clamp it onto the insert using the larger white ring
(see Figure B.11).
07.03.29 Page B.9

Figure B.11: Clamping the Second Kapton Foil

4. Use a scalpel or a pair of scissors to cut the parts of the foil that are outside the insert ring. Now you can
bring the insert into its position in the PW1818/40 Sample Holder Ring and fix it using the circular steel
spring (see Figure B.12).
Figure B.12: Insert the Prepared Sample into the PW1818/40 Sample Holder Ring
The sample is now ready for use with a PW3064/60 or PW3076/00 Sample Spinner (see Figure B.13).
Figure B.13: The Sample Prepared for Transmission Diffraction
Page B.10 07.03.29

B.2.4 Preparation of Air Sensitive Samples

Samples that are sensitive to air, humidity or oxygen, or that are a danger to the operator's health, must be
prepared in a PW1815/40 Sample holder insert. If needed, you can prepare the sample in a glove box.
1. Ensure that you have the complete set of the PW1815/40 Sample Holders and Rings and two Kapton
foils as is shown in Figure B.14 If you have only a small amount of material available, you can use the
PW1817/32 or PW1819/32 Zero Background Holder as a sample support.
Figure B.14: PW1815/40 Sample Holder Insert for Air Sensitive Samples,
Zero Background Holder and Kapton Foil
2. Spread the sample material in the cavity or, if applicable, onto the zero background holder (see Figure
B.15). The sample surface must be flush with the rim of the cavity, which is the reference surface for
sample height alignment.
07.03.29 Page B.11

Figure B.15: Spreading the Sample Material onto the Sample Holder
3. Cover the sample with the Kapton foil and clamp it with the white ring onto the sample holder, as
shown in Figure B.16.
Figure B.16: Clamping the Foil onto the Sample Holder

4. Use a scalpel or a pair of scissors to cutaway the parts of the foil that are outside the sample holder (see
Figure B.17).
Page B.12 07.03.29

Figure B.17: Cutting Away the Foil outside the Sample Holder
5. Bring the sample holder into its position in the PW1813/40 Sample Holder Ring and fix it in place
using the spring (see Figure B.18).
Figure B.18: Inserting the Sample Holder into the PW1813/40 Sample Holder Ring
The sample is now ready for use with a PW3064/x0 or PW3076/00 Sample Spinner (see Figure B.19).
07.03.29 Page B.13

Figure B.19: Sample Prepared in the PW1815/40 Air Sensitive Sample Holder and
PW1813/40 Sample Holder Ring
B.2.5 Non-standard Sample Preparation

Odd or irregularly shaped samples can be mounted in the PW1812/00, using wax or Plasticine. The sample must
be in a polycrystalline state, with a flat surface that corresponds to the reference plane of the sample holder.
Glass capillaries can be attached to a PW1817/32 or PW1819/32 Zero Background Holder, which is mounted in
the PW1813/32, with minute amounts of grease or modelling wax at the tips (see Figure B.20). This is an
alternative to using the capillary sample spinner. The amount of wax must be enough to fix the sample to the
wafer, but small enough not to obstruct the X-ray beam at low angles.
Small amounts of powder sample, in the order of 0.5 milligrams, can be mounted on a PW1817/32 or
PW1819/32 Zero Background Holder, using alcohol, grease, or petroleum jelly (Vaseline). See section B.3.3.
NOTE: Silicon (zero background holder) supports must be cleaned carefully before use, preferably using
an ultrasonic bath.
Page B.14 07.03.29

Figure B.20: Glass Capillary on a Zero Background Holder

Polymeric foil samples to be measured in transmission mode can be clamped into the PW1818/25 Sample
Holder in the same way as is described for the Kapton foils in section B.2.3. Smaller pieces of foils can be
mounted into the PW1818/25 Sample Holder using small pieces of adhesive tape, for example: Scotch tape, as
is shown in Figure B.21.
Figure B.21: Polymeric Foils Mounted onto the PW1818/25 and PW1818/40 Sample Holders
07.03.29 Page B.15

B.3 SAMPLE PREPARATION FOR STATIONARY SAMPLE HOLDERS

B.3.1 Sample Preparation Equipment
The ideal powder sample should be homogeneous, with a grain size between 1 and 25 μm. There should be no
preferred orientation, or any micro or macro-crystalline strain. Reference should be made to section B.1 of this
chapter for details of the errors that should be avoided, and precautions that should be taken, in the preparation
of samples. Details of the methods for grinding and pelletizing samples, where necessary, can be found in
sections B.1.1 and B.1.2, respectively.
Figure B.22 shows the items which comprise the sample preparation equipment, as follows:
1. Cover glass
2. Mortar and pestle
3. PW1172/01 Sample Holder with back plate
4. Stanley knife blade
5. Adhesive tape
Figure B.22: Sample Preparation Equipment
B.3.2 Standard Sample Preparation

When preparing a standard sample, the following procedure should be adopted:
1. Using self-adhesive tape; for example, Sellotape, secure a glass plate to the front side of the sample
holder (see Figure B.23).
2. Put the powder into the holder (see Figure B.24).
3. Use a piece of glass (or a flat plate) to press in the powder (see Figure B.25).
4. Remove the surplus with a Stanley knife or glass plate (see Figure B.26).
5. Secure the back cover to the holder (see Figure B.27).
6. Turn the sample holder upside down and carefully remove the glass cover. You should now have a
smooth, flat sample surface, flush with the sample holder surface (Figure B.28).
7. The sample is now ready for use.
Page B.16 07.03.29

NOTES: a. To protect the sample, the front glass plate should not be removed before measuring.
b. Insert the sample into the sample stage (PW3071/60 or PW3074/00) only until the sample
material is just free from the reference plane of the sample stage. If you push it any further the
sample material could become contaminated with that of previous samples and Al lines from
the sample holder may appear in your diffractogram.
Figure B.23: Glass Plate Secured to Holder
Figure B.24: Putting the Powder into the Holder
07.03.29 Page B.17

Figure B.25: Pressing the Powder into the Holder
Figure B.26: Removing the Surplus Powder
Page B.18 07.03.29

Figure B.27: The Back Cover Secured to the Holder
Figure B.28: Powder Sample Ready for Use
B.3.3 Non-standard Sample Preparation

It is possible that powder samples may not be suitable for loading into the PW1172/01 Sample Holder; for
example, if very little material is available. In this case, non-PANalytical supply items can be made up locally,
or purchased from specialist suppliers.
If only a small amount of sample material is available, a glass plate or PW1817/32 or PW1819/32 Zero
Background Holder can be used (see Figure B.29). The amount of powder can be very small; in order to obtain
a reproducible surface structure the powder can be very lightly pressed. The powder is mounted on the substrate
using a drop of alcohol. The problem of preferred orientation is minimized by sprinkling the powder onto a
smear of petroleum jelly. Use as little as possible of the petroleum jelly in order to keep the contribution to the
background as small as possible.
07.03.29 Page B.19

Figure B.29: Small Amount of Powder on Zero Background Holder

To obtain preferred orientation for materials such as clays, samples can be prepared by spreading onto a porous
tile (1), or onto a glass slide (2).
To prepare a drug tablet, or other small solid sample, for analysis with a sample holder, a small amount of
modelling wax (Plasticine) can be used to hold the sample in place (see Figure B.30).
Figure B.30: Solid Sample
Page B.20 07.03.29

B.4 SAMPLE PREPARATION FOR SAMPLES IN GLASS CAPILLARIES

B.4.1 General
When substances under investigation are sensitive to humidity or oxygen, or could be dangerous to the operator's
health, small amounts of the substance can be put into a glass capillary. Once filled, the capillary is sealed and
mounted onto a PW3063/00 Capillary Spinner Sample Stage. This sample stage spins the glass capillary to
improve particle statistics. A goniometer head is used to align the glass capillary with respect to the heart of the
goniometer. This section describes a method of filling and mounting of glass capillaries. The alignment of the
capillaries is described in Chapter 12 (section 12.3.2) in Part II of the X’Pert PRO User’s Guide.
B.4.2 Capillary Sample Preparation

The powder used to prepare a capillary sample should be homogeneous, with a grain size between 1 and 25 µm.
Refer to section B.1 for details of the errors that should be avoided, and the precautions that should be taken, in
the preparation of the samples. Details of grinding of powders are given in section B.1.1. We advise you to use
capillary samples with a diameter between 0.3 mm and 0.5 mm. Finer capillaries give a better resolution (smaller
Full Width at Half Maximum of the peaks recorded in a scan), but using fine capillaries requires: very fine
powder, extra care during sample preparation, and longer measurement times.
B.4.2.1 Sample Preparation Equipment

The following items are used when preparing capillary samples:
Glass capillaries, inner diameter 0.3 - 0.5 mm
Wax tablets
A dusting brush
A spatula
A night light (alternatively a candle can be used)
A lighter
A plastic coffee cup
These items, together with a goniometer head, a set of capillary holders and a screw driver for alignment purpose
are also shown in Figure B.31.
Figure B.31: Sample Preparation Equipment
07.03.29 Page B.21

B.4.2.2 Preparing a Capillary Sample

You can use a plastic coffee cup as a capillary sample “preparation table”. To this end you must cut a strip out
of the cup as shown in Figure B.32 and make a hole in the bottom for the capillary as shown in Figure B.33.
Figure B.32: Preparing the Plastic Cup - 1
Figure B.33: Preparing the Plastic Cup - 2
Place a glass capillary into the hole as shown in Figure B.34.
Page B.22 07.03.29

Figure B.34: Inserting the Capillary
Use a spatula to pick up small amounts of powder and put the powder carefully into the capillary (see Figure
B.35). Do not try to put too much powder into the capillary at one go, as that is likely to cause a blockage where
the capillary narrows.
Figure B.35: Inserting the Powder - 1
You can see how the powder is filling the capillary through the gap in the cup (Figure B.36). Tap the cup gently
to ensure that the powder sinks to the bottom end of the capillary.
07.03.29 Page B.23

Figure B.36: Inserting the Powder - 2
When the capillary is full, take it out of the cup and seal the open end using a small flame from a night light or
candle (Figure B.37).
Figure B.37: Sealing the Capillary
Fill the capillary holder (the part that you will use to mount the capillary onto the goniometer head) with molten
wax from the night light or candle (Figure B.38).
Page B.24 07.03.29

Figure B.38: Filling the Capillary Holder with Candle Wax
Fix the capillary into the capillary holder. Be very careful to ensure that the capillary is mounted in such a way
that it is aligned with the capillary holder (this makes alignment with respect to the X-ray beam easier). When
the candle wax solidifies the capillary is ready for use (Figure B.39).
Figure B.39: Capillary Mounted into its Holder
You can now mount the capillary sample into the goniometer head as shown in Figure B.40. The head fits onto
the PW3063/00 Capillary Spinner Sample Stage. Alignment with respect to the X-ray beam is done on the
goniometer using an alignment microscope (see section 12.3.2 in Chapter 12 in Part II of the X’Pert PRO User’s
Guide).
07.03.29 Page B.25

Figure B.40: Capillary Sample Mounted onto the Goniometer Head
B.5 REFERENCES
1. R. Jenkins, R. L. Snyder, “Introduction to X-ray Powder Diffractometry”, J. Wiley & Sons Inc. (New
York) 1996. ISBN 0-471-51339-3.
2. H. P. Klug, L. E. Alexander, “X-ray Diffractometry Procedures for Polycrystalline & Amorphous
Materials”, J. Wiley & Sons Inc. (New York) 1974. ISBN 0-471-49369-4.
Page B.26 07.03.29

Appendix C
X-ray Topography
Contents
C.1 Introduction.......................................................................................................................C - 3
C.2 What is Topography? .......................................................................................................C - 3
C.3 Applications of Topography ............................................................................................C - 3
C.4 Defects Revealed by Topography ....................................................................................C - 4
C.5 Resolution in Topographs ................................................................................................C - 5
C.6 Contrast in Topographs ...................................................................................................C - 5
C.7 Setting up an Exposure.....................................................................................................C - 6
C.7.1 Selection of Diffraction Angles............................................................................................C - 6
C.7.2 Exposure Time .....................................................................................................................C - 6
C.7.3 Loading the Film ..................................................................................................................C - 6
C.8 Photographic Supplies and Processing ...........................................................................C - 7
C.8.1 Film Supplies and Storage....................................................................................................C - 7
C.8.2 Film Processing ....................................................................................................................C - 7
C.8.3 Processing Procedure ...........................................................................................................C - 7
C.9 Examples............................................................................................................................C - 8
C.10 References........................................................................................................................C - 10
07.03.29 Page C.1

Page C.2 07.03.29

Appendix C: X-ray Topography
C.1 INTRODUCTION
This appendix describes the use of the X-ray topography film holder supplied with X'Pert PRO MRD. The
information available from X-ray topographs is explained and the procedure for recording topographs is given.
The appendix is illustrated with examples supplied by Prof. Paul Fewster of PANalytical Research Centre. For
more information about X-ray topography we suggest that you refer to “X-ray and Neutron Dynamical
Scattering: Theory and Practice” [C.1].
C.2 WHAT IS TOPOGRAPHY?

An X-ray topograph is an image of a sample produced by Bragg diffracted radiation. Consider a monochromatic
beam with a low angular divergence incident on a perfect single crystal at the Bragg angle for the (hkl) planes.
As the crystal is assumed to be perfect all planes are parallel and will be at the Bragg condition simultaneously.
If a film is positioned to record the diffracted beam the image shape will be related to the area of the crystal
intercepting the incident beam and the geometry of the reflection.
In an imperfect crystal there can be local distortions in the planes causing changes in the Bragg condition
because of changes in plane tilts or plane spacings. The diffracted beam image coming from distorted parts of
the crystal will show a different intensity to the image from those parts of the crystal where the planes are
undistorted.
It is possible to characterize different types of defect (for example: edge and screw dislocations) by observing
how the distortions affect the topographs recorded using different reflections.
C.3 APPLICATIONS OF TOPOGRAPHY

Topography can be used to identify defects present within that part of a (nearly) perfect sample which is being
irradiated by the incident beam coming out of a Ge monochromator. Recording of X-ray topographs can be done
either with or without an analyzer:
Topographs recorded immediately after the sample (that is without a secondary monochromator)
indicate the distribution of major defects in the sample, for example: dislocations, scratches.
Topographs recorded after an analyzer crystal can be used to determine what parts of the irradiated area
of the sample are diffracting the intensity measured in an area of a diffraction space map.
The PW3142/20 Topography Film Holder is designed for use in this position.
NOTE: A topograph recorded when the sample is set on one peak from a multilayer sample will show the
defects associated with that particular peak. However care is required in determining the position
of defects as the strain fields of defects in one layer usually extend into adjacent layers.
X-ray topography is a non-destructive technique which is suitable for observing low dislocation densities
(typically of the order of 103 - 106 cm-2), this is therefore complementary to Transmission Electron Microscopy
(TEM) which is a destructive analytical technique suitable for observing high defect densities (> 108 cm-2).
X-ray topography can also be used to reveal dislocation structures, even when the dislocation density is too high
to reveal the individual dislocations. This is because dislocations are rarely evenly spaced and frequently a
mosaic type structure of dislocations forms where regions with below average dislocation density are separated
by regions of above average dislocations density. This variable distribution will be resolved in X-ray topographs
provided the average size of the mosaic blocks is more than a few micrometers.
When the dislocation separations for semiconductor materials are in the order of a few tens of micrometers it
becomes possible to reveal the dislocations on an X-ray topograph. The percentage of defective material will
however, be too low to have a marked influence on the X-ray rocking curve. The dynamic theory of diffraction
can still be applied. This means that X-ray topography is more sensitive to the onset of relaxation than X-ray
rocking curve measurements. As the defect separation approaches one micrometer the X-ray rocking curve
deviates from the shape predicted by dynamic theory. In this situation the dislocation density is too high to reveal
the individual dislocations on X-ray topographs.
07.03.29 Page C.3

C.4 DEFECTS REVEALED BY TOPOGRAPHY

This section summarizes the characteristics of defects which can be observed using X-ray topography.
• Dislocations
Dislocations are one dimensional defects characterized by a core of material where the atoms are
significantly displaced from the positions in the perfect crystal. The effective core radius for a
dislocation can be defined as the distance from the dislocation where the plane distortion causes a
deviation from the Bragg angle which is greater than the incident beam divergence. Where dislocations
are widely spaced in bulk material core radii are typically a few micrometers. The effective radius is
less for closely spaced dislocations or near surface dislocations.
A dislocation does not cause distortions in every lattice plane in the crystal structure. For instance there
is no distortion in the planes normal to a pure edge dislocation. Dislocations will appear in a topograph
where they distort the reflecting planes. Only a percentage of the dislocations are imaged for most
reflections.
• Surface damage
A single crystal may have surface scratches as a result of insufficient polishing after cutting or due to
subsequent handling. These scratches consist of closely spaced arrays of very short dislocations and
micro cracks. Again the local distortions in the lattice planes leads to contrast in the topograph.
• Stacking faults
Stacking faults are two dimensional defects where there is an abrupt change of stacking sequence of the
planes in the crystal. These defects are often bounded by partial dislocations. These dislocations are the
major source of distortion of the Bragg planes.
• Twins
Twins are two dimensional defects where there is a reversal of stacking of the planes within the crystal.
Some reflecting planes will not be continuous across the twin. Topographs recorded using these
reflections will image part of the sample. The twin is bounded by partial dislocations.
• Small angle grain boundaries
Small angle grain boundaries are two dimensional defects consisting of arrays of dislocations. The
orientation of the parts of the crystal either side of the boundary are tilted with respect to each other.
Mosaic crystals consist of volumes of crystal with relatively low dislocation densities separated by
small angle grain boundaries.
• Edges of thin films
When a crystal is partially covered with a thin film (for example: a patterned amorphous oxide or
nitride film on a silicon wafer, or a partially etched heteroepitaxial layer on a III-V semiconductor
substrate) the underlying crystal can be distorted along the edge of the film due to the difference in
either the expansion coefficient or the lattice parameter between film and substrate.
• Magnetic domain walls
The domain walls occurring in magnetic crystals give a small distortion in the lattice planes and this can
also be sufficient to cause an observable change in the diffracted intensity.
• Precipitates and point defects
Lattice planes will be distorted when precipitates or single atoms of another material are present. In the
case of single atoms the distortion will be very small. If there is a large variation in the point defect
density across the imaged area a difference in overall diffracted intensity can occur. Individual
precipitates will be imaged if the size of the associated strain field extends over several micrometers.
Page C.4 07.03.29

C.5 RESOLUTION IN TOPOGRAPHS

Three major factors influence the resolution of an X-ray topograph: the beam divergence, the film and the
diffraction angle.
• Beam divergence
When topographs are taken with the high resolution optics of the X'Pert PRO MRD the divergence of
the incident beam in the equatorial plane (containing the incident and diffracted beams) is always very
low (refer to Chapter 7 in Part II of this User’s Guide). This means resolution is always good in this
plane. Perpendicular to this plane the axial divergence is determined by the width of the X-ray beam
(X). The vertical resolution is given by FX/D where F is the sample to film distance and D is the X-ray
source to sample distance. F and D are of similar size when topographs are recorded with the X'Pert
PRO MRD system. Thus the vertical resolution is of the order of the width of the X-ray beam.
• Choice of Film
The choice of the X-ray film is based on the following considerations:
- In order to obtain high resolution images the film must be finely grained.
- In order to absorb the diffracted X-ray beam sufficiently to give reasonable exposure times, the film
must have a high silver content and a thick (25 to 50 μm) emulsion.
The best available choice is a nuclear emulsion film with a sub micron grain size. When a single Cu Kα
X-ray photon is absorbed the resulting electron cascade causes grain development over at least one
micron, which sets the minimum resolution of the film.
• Diffraction Angle
As the X-ray topography attachment is mounted on the PreFIX module, the diffracted X-ray beam
passes through the emulsion, normal to the plate. This prevents any loss of image resolution. However,
it should be noted that the image is foreshortened by a factor of sin α, in which α is the angle between
the sample surface and the diffracted beam, that is (2θ - ω).
C.6 CONTRAST IN TOPOGRAPHS

The perfect regions will be imaged with maximum intensity if a topograph is recorded exactly on a Bragg peak
for the sample. Imperfect regions will correspond to a deviation from the Bragg condition and will give weaker
images.
Defects will appear with greater contrast as the sample is moved from the Bragg condition and the perfect
regions diffract less strongly.
With X’Pert PRO, topographs can be recorded to investigate the defects associated with features observed in 2D
intensity map. If the sample angles are set at the values corresponding to a feature in the 2D intensity map then
strong features in the topograph will correspond to parts of the sample which give rise to the diffraction feature.
07.03.29 Page C.5

C.7 SETTING UP AN EXPOSURE

C.7.1 Selection of Diffraction Angles
The image size of the photograph is limited by a combination of the size of the incident beam and the maximum
size of the beam that can pass through the analyzer. The imaged area can be increased by using an asymmetric
reflection with a low angle of incidence. A high resolution image with minimum distortion will be obtained if
the beam exit angle (2θ - ω) is chosen to be close to 90º.
C.7.2 Exposure Time

The exposure time should be calculated on the basis of the intensity reading immediately before inserting the
topography cassette. As a rough guide the exposure time for Ilford L4 film with emulsion 50 μm thick is given
by: t x C = 400 000, where t is the exposure time in minutes and C is the intensity in counts per second.
C.7.3 Loading the Film

The film holder is designed to take pieces of film measuring approximately 25 mm x 40 mm. The film can be
moved in increments of 5 mm to give up to 9 exposures on a single film using the engraved lines on the base of
the holder. How to mount and how to move the film holder on the PW3120/6x Triple Axis and Rocking Curve
Attachment behind the analyzer crystal is described in Chapter 19 in Part II of this User’s Guide.
An exploded view of the film holder is shown in Figure C.1. The film is placed between the inner two disks.
Nuclear emulsion plates are supplied coated on one side only, this side must be directed towards the X-ray
source. When viewed under darkroom conditions the emulsion side is less shiny. The notches in the disks fit over
pegs in the frame which set the long edge of the film horizontal. The outer disk is screwed into the frame to hold
the film securely in position.
Figure C.1: Exploded View of Topography Holder

Two or three exposures of the same topograph can be made using times of t/2, t and 2t to ensure a good exposure
is achieved.
Page C.6 07.03.29

C.8 PHOTOGRAPHIC SUPPLIES AND PROCESSING

C.8.1 Film Supplies and Storage
Nuclear emulsion films are available by special order from The Scientific Product Business Department of Ilford
Ltd, Mabberley, Knutsford, Cheshire, UK.
The topography cassette has been designed to accommodate plates of 25 mm x 40 mm. A variety of emulsion
types and emulsion thicknesses are available - 50 μm thick Ilford L4 emulsion is recommended for work with
Cu Kα radiation.
The emulsion will melt if the unprocessed emulsion is left in a warm place. The plates should be stored in a
(domestic type) refrigerator. To prevent image deterioration during processing all processing solutions should
be stored in the refrigerator immediately before use.
C.8.2 Film Processing

Processing should be done in a darkroom using a Kodak 6BR safelight filter.
Nuclear emulsion is very soft. Handling marks can be revealed by the chemical development process. Such
marks can be reduced if the emulsion is gently stroked with a finger between the development stage and fixing
stage.
C.8.3 Processing Procedure

The recommended processing procedure is:
1. Development: about 5 minutes in Kodak D-19 developer at 15 °C. The developing film can be viewed
under the recommended safe light and development can be terminated when the image is
seen to be dark enough.
D-19 is supplied in sealed 800 g tins. The tin should be stored in a desiccator once opened.
Make up as required by heating up 200 ml of water to 39 °C and adding 32 g of D-19. Stir
until dissolved. Development time is increased for lower temperatures. Discard after use.
2. Stop Bath: 1 minute in Ilford IN-1 Stop Bath. This is just water + 1% acetic acid.
3. Fixing: about 20 minutes in Ilford Amfix diluted 1:3. Fixing should continue for approximately
double the time the emulsion takes to clear.
NOTE: Dilute Amfix can be reused if kept in a closed container.
4. Washing: 1 hour in cold running water.

5. Dry: at room temperature in a dust free atmosphere.
Ensure that the plate is dry before viewing under a microscope to avoid any risk of melting the emulsion.
07.03.29 Page C.7

C.9 EXAMPLES
Examples provided by Prof. Paul Fewster of PANalytical Research Centre, Brighton, United Kingdom.
Figure C.2: Topograph of Gallium Arsenide Substrate plus a Gallium Indium Arsenide Layer
Sample 1: GaAs substrate with a GaInAs layer
Figure C.2 is a topograph of a gallium arsenide substrate plus a gallium indium arsenide layer showing a
mismatch dislocation network.
The topograph was recorded using the (004) reflection immediately after the sample. The sample was mounted
with [100] parallel to the diffraction plane. The diffractometer was set on the top of the layer peak. A 1 mm wide
stripe of the sample is imaged.
The sample is relaxed, the two sets of inclined lines being the mismatch dislocation network. The dislocations
are not resolved individually but are seen to pile-up in bands parallel to the {111} slip planes.
The image is foreshortened due to the diffraction geometry. The diffracted beam is at an angle of about 33° to
the sample which foreshortens the image by a factor of sin 33° (≈ 0.55). This foreshortening distorts the angle
between the two <110> directions from 90° to 122°.
Sample 2: Si-doped (001) GaAs substrate
Figure C.3 shows the (004) diffraction space map recorded from the sample using a triple axis monochromator.
There are weaker lobes either side of the strong substrate diffraction peak indicating there is a high defect
density.
Page C.8 07.03.29

Figure C.3: Silicon Doped Gallium Arsenide Substrate (004) Diffraction Space Map
Figure C.4 shows the topograph taken after the analyzer crystal with the diffractometer set at the maximum count
rate. Again the image shows a strip of the sample approximately 1 mm wide. Many defects are seen in low
contrast.
Figure C.4: Silicon Doped Gallium Arsenide Substrate -

Topograph Recorded at the (004) Peak Maximum
Figure C.5 shows a topograph recorded after the analyzer crystal when the diffractometer was set 30 arc seconds
from the maximum (at the point B marked in Figure C.3). This topograph shows a smaller number of defects
with much higher contrast. The wide straight lines are surface scratches (broadened due to the poorer vertical
resolution of the topograph) while the smaller features are mainly individual dislocations.
The defects appear with high contrast because the intensity is being diffracted from the distorted planes close to
the defects rather than the matrix of more perfect material surrounding them.
07.03.29 Page C.9

Figure C.5: Silicon Doped Gallium Arsenide Substrate -

Topograph recorded at Position B in Figure C.3
C.10 REFERENCES
C.1. Authier et al., “X-ray and Neutron Dynamical Scattering: Theory and Practice” NATO ASI Series vol.
357, Plenum (New York) 1996. ISBN 0-306-45501.
Page C.10 07.03.29

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X’PERT PRO

The Analytical X-ray Company

EDITION NOTICE: This is the Sixth Edition of this publication.

07.03.27 Page iii

Introduction to X’Pert PRO

continued on next page

1.5 PW3050/6x X’Pert PRO Goniometer..............................................................................1 - 15

Page 1.2 07.03.27

1.2 HOW TO READ THIS GUIDE

07.03.27 Page 1.3

1.3 BASICS OF THE X’PERT PRO X-RAY DIFFRACTION SYSTEM

Figure 1.1: PW3040/60 X’Pert PRO Instrument Enclosure

Page 1.4 07.03.27

1.3.1 The PreFIX Concept

1.4 PW3040/60 X’PERT PRO INSTRUMENT ENCLOSURE

Table 1.1: PW3040/60 X’Pert PRO Instrument Enclosure - Technical Specifications

Mains supply 200 - 240 V, single phase, 50 or 60 Hz

System dimensions 1975 mm x 1132 mm x 1371 mm

System weight 11000 N to 12500 N, depending on the system configuration

1.4.1 Working Environment

Page 1.6 07.03.27

1.4.2 X-rays ON Lamp

1.4.3 Instrument Enclosure Lower Part

1.4.4 Control and Display Panel

Figure 1.2: Control and Display Panel

07.03.27 Page 1.7

Table 1.2: Control Panel Switches and their Functions

Power on To turn the power on. Yes

Light To switch the interior inspection lights on and off. No

Table 1.3: The LED Displays and their Functions

LED Display Function

1.4.5 High Tension Generator

1.4.6.1 Tube Shield

Page 1.8 07.03.27

1.4.6.2 High Tension Cable

Figure 1.3: Tube High Tension Cable Plug

1.4.6.3 Cooling System

1.4.6.4 Tube Support Stand

Figure 1.4: X’Pert PRO General Accessories

1.4.6.5 Filter Slit Puller

Page 1.10 07.03.27

1.4.6.7 Tube of Silicon Grease

1.4.6.8 Silicon Disk

1.4.6.9 Fluorescence Disk

1.4.6.10 Single Knife Edge

07.03.27 Page 1.11

Figure 1.7: Single Knife Edge

1.4.6.11 Copper Attenuation Foils

1.4.6.12 Bottle of Oil

1.4.6.13 Chamois Leather

1.4.6.14 Set of Tools

1.4.6.15 PW3096/60 Second Diffracted Beam PreFIX Carrier

Page 1.12 07.03.27

Figure 1.8: PW3096/60 Second Diffracted Beam PreFIX Carrier

1.4.6.16 PW3132/61 Reference Samples for Stress and Texture Measurements

07.03.27 Page 1.13

1.4.6.17 PW3132/62 Reference Samples for High Resolution and Reflectivity

1.4.6.18 PW3719/10 Display Unit