Characterization of Materials

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 Optical Microscopy
Microscope

Simple Compound

Magnifying Glass

Biological Metallurgical
Microscope Microscope
(Transmitted Light) (Reflected Light)

Upright Microscope Inverted Microscope

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 Upright Microscope

Inverted Microscope
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 Refractive index, refraction and reflection

 Refractive index (n): The ratio of velocity of light in vacuum to that

in another medium is called the refractive index of that medium.
 Refractive Index for Air and Gas is 1.0
 When the speed of light waves is reduced their frequency is

unaltered but their wavelength is shortened i.e. (c=νλ)

 Consequently, when a ray of light passes from one isotropic medium
to another it is refracted, i.e. bent, through an angle which is
determined by Snell's Law.

𝒔𝒊𝒏𝒊 𝒗𝟏 𝒏𝟐
= =
𝐬𝐢𝐧𝒓 𝒗𝟐 𝒏𝟏
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 Rules of rays tracing for a Simple Len

A light ray passing through the A light ray parallel with the optic axis will, after
center of a len is not deviated refraction, pass through the rear focal point

The intersection of any two of the

A ray passing through the front
three key rays just described identifies
focal point will be refracted in a
the location of the image plane 9
direction parallel to the axis
Image formation by single lens

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Image Magnification by single lens

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 Lens formula and magnification

Thin lens equation

1 1 1
 
f u v

Magnification M

v
M
u
f v f
M 
u f f

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 Two-stage projection microscope

Light rays from the object firstly converge at the objective lens and are then focused

at position B to form a magnified inverted image.

The light rays from the image are further converged by the second lens (projector

lens) to form a final magnified image of an object at C.

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 When we examine microstructure with our eyes,

the light path in a microscope goes through an eyepiece instead of

projector lens to form a virtual image on the human eye retina

 Object (O) placed just outside focal point of objective lens

 A real inverted (intermediate) image (I1) forms at or close to focal point of

eyepiece.

 The eyepiece produces a further magnified virtual inverted image (I214)

 Magnification of Optical Microscope

𝒕𝑫
𝑴 = 𝑴𝒐 𝑴𝒆 = t=optical tube length
𝒇𝒐 𝒇𝒆 15
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 Optical system

Transmission
Illumination

Reflected
Illumination

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Diffraction of light

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Airy Disc

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Airy Disc

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Diffraction of light

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Diffraction Mechanism for Image formation in
optical Microscopy

Abbe's theory of the microscope

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 Mechanism for Image formation in optical Microscopy

Direct and first-order diffracted beams are collected by the objective.

Detail in the image is resolved.

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Mechanism for Image formation in optical Microscopy

Only the direct beam is collected by the objective.

Detail in the image is not resolved.
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 Mechanism for Image formation in optical Microscopy

The direct and several orders of diffracted beams arc collected by the
objective.

Detail is resolved accurately.

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 Mechanism for Image formation in optical Microscopy

the objective collects the direct beam and a diffracted beam.

Resolution of detail in the image is restored.

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 Mechanism for Image formation in optical Microscopy

The direct beam is so oblique that it no longer enters the objective. but two
diffracted beams are collected by the objective.

Detail in the image is resolved, but with reversed contrast, i.e. a dark-ground
image is formed.
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Other Mechanism for Image formation in optical Microscopy

 Diffraction is the essential mechanism of image formation in the

microscope
 Some other mechanisms may also be involved for the image
formation
 Reflection,
 Absorption,
 Refraction,
 Fluorescence, and
 Polarization.

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 Image formation in optical Microscopy by Reflection

 Reflection: An essential mechanism in the formation of images of metallic and

other opaque specimens

 It occurs at interfaces at which there is a large difference in the refractive indices

of the media, as between air and metal

 In the metallurgical microscope the specimen may be illuminated either

 vertically, (i.e. normal to the surface of the specimen along the optic axis of
the microscope) producing bright-field illumination or

 very obliquely, producing dark-field illumination

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 Bright-field and Dark field image formation in optical
Microscopy by Reflection
 In the bright-field illumination,
 light from the surfaces of grains that are perpendicular to the incident beam is
reflected back into the objective,
 while light from features in the microstructure (such as grain boundaries and
tilted areas of the surface) is reflected away from the objective.
 Hence, they appear dark.
 In the dark-field illumination,
 light reflected from surfaces which are almost perpendicular to the optic axis
of the microscope is reflected away from the objective,
 while light from features in the microstructure is reflected into it.
 Reflection also occurs in transparent materials at interfaces between constituents
of different refractive index, e.g. grain boundaries. 30
 Ni-based super alloys

Bright-field image Dark-field image

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Brightfield Phase contrast

DIC Darkfield

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 Objective and its Properties
 The image formed by a microscope is produced by the action of both the
objective and the eyepiece.
 Of the two lenses, the objective is most important
 it determines the detail that can be seen in the final image and the optimum
useful magnification.
 The eyepiece enlarges the image formed by the objective to the optimum
overall magnification and corrects residual aberrations in the primary image,
 But it cannot improve the detail in the image formed by the objective.

 Objective has three important characteristics

 Magnifying power,
 Resolving power, i.e. ability to separate fine detail in the image, and
 Its ability to gather light from the object.
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 Objective Specifications

Magnification power of Objective

Optical Tube Length (t)

M=
Focal Length of Objective (f)
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 Numerical Aperture of Objective

The numerical aperture (N.A.) of an optical system such as an objective lens is defined
by
N.A. = nSinθ

where n is the refractive index the medium between lens and specimen, and
θ is the half-angle of the maximum cone of light that can enter or exit the lens

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 Light-gathering Power and Numerical
Aperture of Objective
 The light-gathering power of the objective (or light grasp) is determined
 by the angle of the cone of rays that the objective can accept,
 thus it is related to the NA.

 The angle of the cone depends on the relationship between the diameter of the
front lens of the objective and its focal length;

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 Light-gathering Power and Numerical
Aperture of Objective
 For a given diameter,
 the shorter the focal length the greater will be the angle and the NA.
 NA increases as focal length decreases
 The precise combination of the two depends on the lens design and the
need for eyepiece magnification

 Objective should receive as wide a cone of rays from the object as possible,
because the angle of the cone of rays affects the brightness of image as well as
the resolution.

 For greatest image brightness the objective must be completely filled with light,
 if the come of rays has a semi angle less than alpha then the image is less
bright
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 Resolution

 Resolution is defined as minimum resolvable distance or it is the smallest

separating distance (d) that can be discerned between two lines in the image
 The unaided eye: resolution is 0.1 mm
 The limit of resolution is a measure of the ability of the objective to separate
in the image individual, adjacent details that are present in the object;
 it is the distance between two points in the object that are just resolved.
 The resolving power is the reciprocal of the limit of resolution

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 Resolution (or resolving power)
Closest spacing of two points which can be clearly seen through
the microscope to be separate entities

Actual What We Might See

Even if we magnify an image of two objects, we can not distinguish them
unless we have adequate resolution.
The resolution of a microscope is controlled by the diffraction of
light.
Light with short wavelength is diffracted at a smaller angle. Diffraction of light
plays a paramount role in limiting the resolving power of any optical
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instrument.
 Resolution

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Higher resolution Lower resolution
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 Resolution
 Path difference =λ, hence 𝒅𝐬𝐢𝐧𝒊 + 𝒅𝐬𝐢𝐧𝜶 = 𝝀

 Since the two beams are just collected by the objective i is equal to α,
thus the limit of resolution, dmin

𝝀
𝒅𝐦𝐢𝐧 =
𝟐𝐬𝐢𝐧𝜶

 if the object space is filled with a medium of refractive

index n, the wavelength of the light in the medium, λn
𝜆
𝜆𝑛 =
𝑛
𝝀𝒏 𝝀 𝝀
𝒅𝐦𝐢𝐧 = = =
𝟐𝐬𝐢𝐧𝜶 𝟐𝒏𝐬𝐢𝐧𝜶 𝟐𝑵𝑨
 For circular aperture

𝟏. 𝟐𝟐𝝀 𝟎. 𝟔𝟏𝝀
𝒅𝐦𝐢𝐧 = =
𝟐𝒏𝐬𝐢𝐧𝜶 𝟐𝑵𝑨
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 Depth of Field and Depth of Focus
 Depth of field in the object plane refers to the
thickness of the optical section along the z-axis within
which objects in the specimen are in focus;
 The range of distances over which points appear in
acceptable focus is called the depth of field.

 Depth of focus is the thickness of the image plane

itself.
 This also refers to the range of position at which the
image can be viewed without appearing out of focus
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for a fixed position of object.
 Sample Preparation for
Metallographic Examination

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 Introduction
 Metallography is basically the study of the structures and
constitution of metals and alloys, using metallurgical microscopes
and magnifications, so that the physical and mechanical properties
of an alloy can be related to its observed microstructure.

 It provides information about the specimen under investigation,

including the size and shape of the grains, the presence of micro
defects (such as segregation, hair cracks, and nonmetallic
inclusions), and the nature and distribution of secondary phases.

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 Metallography
Cutting
Grounding using emery papers (110, 220, 300, 400, 600, 800,
1000, 2000, 5000)
Cloth Polishing: Using Alumina Suspension (0.5, 0.1, 0.05μm) or
Diamond paste (0.5, 0.1, 0.05μm)
Etching: Etching agents (like Nital/ Kellers Solution)
Microscopy
 Grounding
Grinding is a subset of cutting, as grinding is a true metal
cutting process.
Abrasive :The use of Premium SiC abrasive paper is the
most efficient and practical technique for grinding metallic
metallographic specimens. Although many qualities of
silicon carbide are readily available, only the premium
grade SiC powder provides the most consistent results and
highest grinding rates.
 Grinding Soft non-ferrous metals
Soft non-ferrous metals - Initial grinding is recommended with
320 grit SiC
 Abrasive paper followed by 320 400, 600 and, 800 grit SiC
paper. because These materials are relatively soft they do
not easily break down the SiC paper.

The initial grinding with 320 grit is generally sufficient for

minimizing initial deformation and yet maintaining adequate
removal rates.

 For extremely soft materials such as tin, lead and zinc it is

also recommended that the abrasive paper be lightly coated
with a paraffin wax. The wax reduces the tendency of the
SiC abrasive to embed into the soft specimen.
 Grinding Ferrous metals
• Ferrous metals - are relatively easy to grind with the depth
of deformation being a major consideration.110 grit SiC
abrasives provide a good initial start with subsequent use
of 220 or 300, 400, 600 and 800 grit SiC.

• Super alloys - are generally of moderate hardness but have

extremely stable elevated temperature characteristics and
corrosion resistance.

• The procedures for preparing super alloys is very similar to

that for most non-ferrous metals.
 Sample Preparation
• The purpose of this practice is to understand how to prepare
and interpret metallographic samples systematically.

• Gather information about chemical composition, heat

treatment, processing, phase diagram.
• Cut representative sample.
• Mount sample, grind and polish.
• Examine unetched sample.
• Etch lightly and examine again.
• Etch further if necessary.
• Compare with microstructure expected from equilibrium
phase diagram
Surface Finish and Surface Roughness (Original Magnification 50x)
Metallographical etching
Etching:
 Grain Size Examination

Objective Lens

x100
 Phase contrast
Principle: Incident light [Io] is out of phase with transmitted light [I] as it
was slowed down while passing through different parts of the sample
and when the phases of the light are synchronized by an interference
lens, a new image with greater contrast is seen.
Phase ring

not aligned aligned

I0 Phase stops

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 Phase contrast
Application: Phase contrast is the most commonly used contrasting
technique in this institute. All tissue culture microscopes and the
time-lapse microscopes are set up for phase.

BUT: MOST OF YOU ARE USING IT IN THE WRONG WAY!! Because you do not use
the right phase stop with the corresponding objective!

wrong phase stop

brightfield

right phase stop

 Polarization Contrast
Principle: Polarized light is used for illumination. Only when the vibration direction of the
polarized light is altered by a sample placed into the light path, light can pass through the analyser
The sample appears light against a black background. A lambda plate can be used to convert this
contrast into colours.
Application: Polarization contrast is used to look at
materials with birefringent properties, in which the
refractive index depends on the vibration direction of the
incident light, e.g. crystals or polymers.

Analyzer

Lambda
plate

Brightfield Polarization Polarization contrast

contrast with Lambda plate

Polarizer
Optical Microscopy vs Scanning Electron Microscopy

25mm
radiolarian
OM SEM

Small depth of field Large depth of field

Low resolution High resolution
Fe-C Phase Diagram

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 Steel

 Low Carbon Steel or Mild Steel (0.05-0.3 wt% C)

 Medium Carbon Steel (0.3-0.6 wt% C)

 High Carbon Steel (0.6-1.0 wt% C)

 Ultra High Carbon Steel (1.0-2.0 wt% C)

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Pure Iron

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Steel

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Steel

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Steel

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Martensite

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 Stainless Steel (Fe-Cr-Ni-0.15% max C alloys)

 Ferritic Stainless Steel (14-27% Cr)

 Austenitic Stainless Steel

(at least 23% Cr+Ni, 18 Cr and 8% Ni)

 Matensitic Stainless Steel (11.5-18% Cr)

 Precipitation-Hardening Stainless Steel

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Stainless Steel

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 Cast Iron

 White Cast Iron

 Grey Cast Iron

 Malleable Cast Iron

 Nodular/ ductile/ Cast Iron

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White Cast Iron

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Grey Cast Iron

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Malleable Cast Iron

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Nodular Cast Iron

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