IRC in

Nanotechnology

AFM at Video Rate and Beyond

Mervyn Miles

H.H. Wills Physics Laboratory

IRC in Nanotechnology
University of Bristol
Tyndall Avenue
Bristol
U.K.

Frontiers in Scanning Probe Microscopy,

Purdue University, October 2006
Atomic Force Microscopy: Strengths

High-resolution 3-D imaging;

Imaging in liquid, air, & vacuum;
No staining or coating required;
No radiation damage;
Mapping of physical properties;
Modification of surfaces;
Non-scanning applications: force spectroscopy, sensors, ...
 Speed Weakness of SPM

Imaging rate too low:

to follow many processes;

to examine large areas of a specimen;

to create or manipulate structures over usefully large areas.

 Limitations of Conventional SPM

General to all SPMs

Scanning system ~ inertia and resonance problems

Feedback loop response time

Response of interaction sensor

Specific to AFM
Force-sensing cantilever has inertia and resonance
 How to go faster:

Parallel imaging with multiple cantilevers

Strobe imaging of repetitive processes

Decrease Q in AC modes

Shift the time domain using higher frequencies

Another method ....

 Solution 1

Decrease the mass of the scanning system

Increase the stiffness of the scanning system
Decrease the mass of the cantilever
Increase the stiffness of the cantilever
Decrease the Q factor of the cantilever
 A Different Solution

Instead of avoiding resonance,

use a resonating beam

for scanning in the fast direction

 Solution 2

Scan by oscillating at resonance with a high amplitude -

resonant scanning microscopy (RSM);

High Q-factor results in high scan stability;

Data are collected throughout each sweep;

Before high-speed AFM,

we first built a high-speed SNOM

 Scanning Near-field Optical Microscopy (SNOM)
Capture & Processing
Feedback Control
Electronics

Optical
Detector
Quartz Tuning Fork Optical fibre
(Drive & feedback)
Exponential decay of
Specimen evanescent field away
from the interface

scan
ADL Humphris, JK Hobbs, MJ Miles, Applied Physics Letters, 83(1), 6-8 (2003)
Melt-tapered optical fibre SNOM probe
 Scanning Near-field Optical Microscopy (SNOM)
Capture & Processing
Feedback Control
Electronics

Optical
Detector
Quartz Tuning Fork Optical fibre
(Drive & feedback)
Exponential decay of
Specimen evanescent field away
from the interface

scan
ADL Humphris, JK Hobbs, MJ Miles, Applied Physics Letters, 83(1), 6-8 (2003)
IRC in
Nanotechnology

Transverse dynamic force microscope (TDFM)

Probe

Detector
Laser
Low-amplitude (~1 nm) Oscillations
Transverse Dynamic Force Microscope, TDFM

M Antognozzi
 Surface detection via confined water layer
a b
PROBE PROBE

SAMPLE SAMPLE

0.8

0.6

0.4

0.2

0
-1 -0.5 0 0.5 1 1.5 2 2.5 3 3.5 4
tip-sample distance (nm)

M Antognozzi, ADL Humphris, MJ Miles, APPLIED PHYSICS LETTERS, 78(3), 300-302 (2001)
Low-amplitude (~1 nm) Oscillations
 For high-speed SNOM
High-amplitude (~ 5 µm) for fast axis scanning

Tip scanning in fixed plane set by average optical intensity

ADL Humphris, JK Hobbs, MJ Miles, Applied Physics Letters, 83(1), 6-8 (2003)
 Several crystals may nucleate together and grow to form
a spherical structure known as a spherulite.

Within the spherulite, the

polymer crystals grow radially
from the centre in a ribbon
morphology

These ribbon crystals often twist

as they grow with the same pitch
Spherulite
and remain in phase.

In a thin film, the spherulite is a disk-like structure in which the

coherent twisting of the ribbon crystals results in concentric rings
with the ribbons alternately flat on and edge.
Crystallization of poly(hydroxybutyrate-co-valerate) (PHB/V)

Topography Phase

5 µm 5 µm

AFM
Quality factor has been reduced from 270 to 90.
Tip velocity was 403µm/s, line rate 8Hz
High Amplitude Oscillations
 Birefringent PSTM
Slow scanning - 20 minutes/image
assisted with active Q

Detector

Analyser
2 µm Height

Polariser

Shear-force controlled
via tuning fork 2 µm Optical
ADL Humphris/JK Hobbs
see, e.g., RL Williamson, MJ Miles, JOURNAL OF VACUUM SCIENCE & TECHNOLOGY B, 14(2), 809-811 (1996
High Amplitude Oscillations
 Comparison:
Conventional SNOM & RSM SNOM
Conventional SNOM RSM SNOM
1 frame in 1000 sec 120 frames/sec

200 nm

> 100,000 Faster than existing SNOM

PHB spherulite between crossed polars
ADL Humphris, JK Hobbs, MJ Miles, Applied Physics Letters, 83(1), 6-8 (2003)
High-speed SNOM of collagen

Intensity related to height -

67 nm repeat of collagen visible
A Major (Uni Wien, ), L Bozec, MA Horton, Miles
 Scanning Near-field Optical Microscopy (SNOM)
Capture & Processing
Feedback Control
Electronics

Optical
Detector
Analyzer
Quartz Tuning Fork
(Drive & feedback)
Optical fibre
Specimen
scan

transmission Polarizer

A. Ulcinas, M Antognozzi
 Flexure Stage for high-speed SPM

sample stage

` flexures

piezo drivers operating in tandem

This flexure stage provides the high-speed scan

of up to 40kHz with about 3 µm amplitude
Picco, Engledew
High-speed SNOM of polymer spherulite of PHB

Flexure stage scanner - 3 µm x 3 µm image

Transmission SNOM with crossed polars
A. Ulcinas, M Antognozzi, Picco, Engledew
High-speed AFM
 Resonant scanning AFM
side Resonant sample scan stage (x)
Piezo stack for ‘slow’ scan (y)

conventional No electronic feedback

scan tube Mechanical feedback
super lubricity
QCR (x) water in confined geometry
cantilever
piezo stack (y)

ADL Humphris, MJ Miles, JK Hobbs,

top Applied Physics Letters, 86(3), Art.No.
034106 (2005)
 High-speed AFM of Chitosan Film
- tuning-fork resonance scanning

> 3000 Faster than conventional AFM

Conventional AFM

30 frames/s
1µm x 1µm (Infinitesima vAFM)
Ulcinas, Payne, Heppenstall-Butler
 Flexure Stage for high-speed SPM

sample stage

` flexures

piezo drivers operating in tandem

This flexure stage provides the high-speed scan

of up to 40kHz with about 3 µm amplitude
Picco, Engledew
 PEO Spherulite video AFM
- flexure stage (non-resonance) scanning

30 frames/second
1.5 µm x 1.5 µm
Engledew, Picco, Miles
 PEO Spherulite video AFM

30 frames/second

- flexure stage (non-resonance) scanning Engledew, Picco, Miles

PEO Spherulite video AFM

30 frames/second
1.5 µm x 1.5 µm Engledew, Picco, Miles
 PEO video AFM 30 f/s - image reproducibility

0 mins 3 mins
0 frames ~ 6000
frames

7 mins 10 mins
13,000 18,000
frames frames
High-speed AFM of ‘large’ objects
Air Set of human chromosomes c AFM

Picco, Miles, Komatsubara, Hoshi, Ushiki

Human Chromosome No. 2

Picco, Miles, Komatsubara, Hoshi, Ushiki

Picco, Miles, Komatsubara, Hoshi, Ushiki
High-speed AFM of parts of human chromosomes

Air

Picco, Miles, Komatsubara, Hoshi, Ushiki

Montage of high-speed AFM images of part of human
chromosome No. 2

Picco, Miles, Komatsubara, Hoshi, Ushiki

Air

Picco, Miles, Komatsubara, Hoshi, Ushiki

2M NaCl

Picco, Miles, Komatsubara, Hoshi, Ushiki

 Human chromosomes in liquid

2M NaCl

Height range: ~0.5 µm

Picco, Miles, Komatsubara, Hoshi, Ushiki
Conventional AFM Image of Collagen Specimen
Collagen Fibres

Banding
periodicity: 67 nm

30 fps Picco, Bozec, Horton Engledew

 Linear Collage of High-speed AFM Images
of Collagen Fibre
Conventional AFM

High-speed AFM

All the high-speed images were taken in 0.7 s

Single frame from collagen movie

Image acquired in 17 ms
Picco, Bozec, Horton Engledew
 High-speed AFM Collagen Collage

12 images involved - acquired in 200 ms

Picco, Bozec, Horton Engledew, Miles
Large area collagen collage

103 images acquired in 1.7 s

 Non-imaging:

High-speed writing

Electrochemical oxidation of passived silicon

 Local AFM electrochemical oxidation

Can be used to pattern surface -

conventional AFM too slow to pattern large areas
 James Vicary
Ti Oxidation

250 nm

10 ms; -12 V Si tip;

conventional AFM
non-contact
 Oxidation of Silicon with high-speed AFM
100 µs 5 µs

50 µs 1 µs

10 µs 500 ns

Topographic AFM images of oxide nanostructures created with

a -12 V tip bias for pulse times. Height range: 2 nm.
Picco,Vicary
 High-speed AFM
Simultaneous writing (oxidation) and imaging

30 fps

Read-Write

3 voltage pulses synchronized to fast line scan

Picco,Vicary
Conventional AFM of oxidized lines on Si
 High-speed AFM of Collagen
Bimorph Tuning fork Flexure

9 fps 15 fps 30 fps

How fast can this system image?

>1000
1000
750
500
250
100
30 fps
75
50

AFM images in less than 1 ms

Scanner Arrangement for kilohertz AFM

piezo drivers operating in tandem

tuning fork scanning

 Collagen Collagen
Frame banding
Rate: 67 nm
1300 fps
Playback
Line Rate:
Rate: 25 fps
64,000 lps

500 nm x 500 nm

Each frame acquired in: 750 µs

Playback slowed down by > 40 times!
1 Million Images generated in ~15 minutes!
Picco, Ulcinas, Antognozzi, Engledew, Horton, Bozec, Miles
 Collagen
Frame
Rate:
1200 fps Playback
Rate:
Line 25 fps
Rate:
64,000 lps
500 nm x 500 nm

Specimen being oscillate by 50 nm

Collagen banding = 67 nm
Picco, Ulcinas, Antognozzi, Engledew, Horton, Bozec, Miles
Composite image from 1000 fps AFM of Collagen

200 nm
 So far, the movies were rather pixellated ....

... this can be fixed by increasing the line rate further ....
Frame Rate:
1000 fps
Playback
Line Rate:
Rate: 25 fps
200,000 lps

200 x 100 pixels; ~ 25 ns/pixel (on average)

Picco, Ulcinas, Antognozzi, Engledew, Horton, Bozec, Miles

 Nanoscience and QI Centre, Bristol
Infinit
esima Thanks to...

(Andras Major)
Peter Dunton Sheila Morris
Massimo Antognozzi Niigata University:
Loren Picco
Monica Berry Tatsuo Ushiki
Andy Round
Debra Brayshaw Osamu Hoshi
i Mark Szczelkun
David Engledew Nae Komatsubara
Arturas Ulcinas
Simon Haward James Vicary
Jon Hayes UCL, London : Craig Williams
(Jamie Hobbs) Michael Horton Alex Wotherspoon
(Andy Humphris*) Laurent Bozec
Terry McMaster
Thank you for your attention
*www.infinitesima.com