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IMPERFECTIONS IN
SOLIDS(Ⅱ)
Dr. Aneela Wakeel
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Characteristics of dislocations
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Twins in microstructure of steel

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OPTICAL AND
ELECTRON
MICROSCOPY
Dr. Aneela Wakeel
What is a microscope?
Light Microscopy
• Light or optical microscopy is the primary means for scientists
and engineers to examine the microstructure of materials.
• The history of using a light microscope for microstructural
examination of materials can be traced back to the 1880s. Since
then, light microscopy has been widely used by metallurgists to
examine metallic materials.
• Light microscopy for metallurgists became a special field named
metallography. The basic techniques developed in metallography
are not only used for examining metals, but also are used for
examining ceramics and polymers.
Optical images
 Basic components
and their functions

(1) Eyepiece (ocular lens)

(2) Revolving nose piece (to hold
multiple objective lenses)
(3) Objective lenses
(4) And (5) Focus knobs
(4) Coarse adjustment
(5) Fine adjustment
(6) Stage (to hold the specimen)
(7) Light source (lamp)
(8) Condenser lens and
diaphragm
(9) Mechanical stage (move the
specimen on two horizontal axes
for positioning the specimen)
Functions of the Major Parts of a Optical
Microscope

Lamp and Condenser: project a parallel beam

of light onto the sample for illumination
Sample stage with X-Y movement: sample is
placed on the stage and different part of the
sample can be viewed due to the X-Y movement
capability
Focusing knobs: since the distance between
objective and eyepiece is fixed, focusing is
achieved by moving the sample relative to the
objective lens
Functions of the Major Parts of a Optical
Microscope

Objective: does the main part of

magnification and resolves the fine
details on the samples (mo ~ 10 – 100)
Eyepiece: forms a further magnified
virtual image which can be observed
directly with eyes (me ~ 10)
Beam splitter and camera: allow a
permanent record of the real image from
the objective be made on film (for
modern research microscope)
camera

Beam
splitter Reflected light

Olympus
BX51
Research
Microscope
Cutaway
Diagram

Transmitted light
http://micro.magnet.fsu.edu/primer/java/microassembly/index.html
 Objective Lens
dmin = 0.61l/NA
Objective specifications Anatomy of an objective

rical
ture

DIC-differential interference contrast

Objectives are the most important components of a

light microscope: image formation, magnification, the
quality of images and the resolution of the microscope
http://www.youtube.com/watch?v=P0Z4H2O_Stg Objectives to~5:26
http://www.youtube.com/watch?v=H8PQ9RMUoA8 Grades of objectives to~2:30 & 3:25-4:50
https://www.youtube.com/watch?v=FwBjpi8ck1Y Alignment of OM
 Eyepiece Lens

(Diaphragm)

M=(L/fo)(25/fe)
Eyepieces (Oculars) work in combination with microscope
objectives to further magnify the intermediate image
http://micro.magnet.fsu.edu/primer/anatomy/oculars.html
http://www.birdwatching.com/optics/diopter_set.html
 Common Modes of Analysis
Depending on the nature of samples, different illumination
methods must be used
• Transmitted OM - transparent specimens
thin section of rocks, minerals and single crystals
• Reflected OM - opaque specimens
most metals, ceramics, semiconductors
Specialized Microscopy Techniques
• Polarized LM - specimens with anisotropic optical
character http://www.youtube.com/watch?v=ulNZ3u7_J5I to ~1:05

Characteristics of materials can be determined

morphology (shape and size), phase distribution
(amorphous or crystalline), transparency or opacity,
color, refractive indices, dispersion of refractive
indices, crystal system, birefringence, degree of
crystallinity, polymorphism and etc.
http://www.youtube.com/watch?v=Iw734z1e6wQ to~1:30
Modes of OM
 Optical principles- 1.Image formation
The optical principles of microscopes include image formation, magnification, and
resolution.
A specimen(object) is placed at position
A where it is between one and two focal
lengths from an objective lens. Light
rays from the object first 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.
The light path shown in Figure 1.1
generates the real image at C on a screen
or camera film, which is not what we see
with our eyes. Only a real image can be
formed on a screen and photographed.
Image formation
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, as shown in Figure 1.2.
The virtual image is inverted with respect to the object. The virtual image is often
adjusted to be located as the minimum distance of eye focus, which is conventionally
taken as 250 mm from the eyepiece.

Figure 1.2 Schematic path of light in a

microscope with an eyepiece. The virtual
image is reviewed by a human eye composed
of the eye lens and retina.
Magnification
 http://micro.magnet.fsu.edu/primer/java/microscopy/immersion/index.html

Resolution (Lateral)
The smallest distance between two specimen points
that can still be distinguished as two separate entities
To achieve high
resolution, We
should use dmin = 0.61l/NA NA=nsin()
Shortest wavelength
Larger numerical
aperture

λ – illumination wavelength (light)

NA – numerical aperture
-one half of the objective angular aperture
n-imaging medium refractive index

The N.A. is a measure of the light gathering

capabilities of an objective Lens.

https://www.youtube.com/watch?v=n2asdncMYMo at~5:35-6:00
 What is resolution?
Resolution describes the minimal distance of two points that can be distinguished.

Picture taken from http://microscopy.fsu.edu/primer/anatomy/numaperture.html

 What is the numerical aperture?
NA is an estimate of how much light from the sample is collected by the objective

α2
α1

Objective lens
Oil (n = 1.5)
Air (n = 1.0)
Coverslip (n = 1.5)
Glass slide (n = 1.5)

NA = n sin  n = refractive index

α = angle of incident illumination
 Numerical aperture, NOT
magnification determines resolution!

Resolution of 0.175µ Bead Pair

1.1
1.0
0.9
Normalized Intensity

0.8 1.4 NA
0.7
0.6
0.5
0.4
0.7 NA
0.3
0.2
0.1
0.0
-1.10
-0.96
-0.81
-0.66
-0.51
-0.37
-0.22
-0.07

0.37

0.66

0.96
0.07
0.22

0.51

0.81

1.10

Microns

Increasing NA

A lens with a larger NA will be able to

visualize finer details and will also collect
more light and give a brighter image than
a lens with lower NA.
 light

Light is electromagnetic radiation.

What we usually describe as light is
only the visible spectrum of this
radiation with wavelengths between
400nm and 700nm.
The elementary particle that defines
light is the photon.

b) a)

There are 3 basic dimensions of light

a) Intensity (amplitude) which is related to the perception of brightness
b) Frequency (wavelength), perceived as colour
c) Polarization (angle of vibration) which is not or weakly perceptible to humans
Axial resolution – Depth of Field
Depth of focus (f mm) Depth of Field Ranges
(F (F
mm)m)

NA f F
0.1 0.13 15.5
0.4 3.8 5.8
.95 80.0 0.19

The distance above and below The axial range through which
geometric image plane within an object can be focused without
which the image is in focus any appreciable change in image
sharpness
M NA f F
F is determined by NA.
M NA f F
http://www.matter.org.uk/tem/depth_of_field.htm
http://www.youtube.com/watch?v=FvC2WLUqEug at~3:40
 Brightness
Brightness refers to the intensity of light.
In a transmission light microscope the brightness is related to
the numerical aperture (NA) and magnification (M).
 http://micro.magnet.fsu.edu/primer/techniques/contrast.html

Contrast
Contrast is defined as the difference in light intensity
between the specimen and the adjacent background
relative to the overall background intensity.

Image contrast, C is defined by

Sspecimen-Sbackgroud S
C= =
Sspecimen SA

Sspecimen (Smax) and Sbackgroud (Smin)

are intensities measured from
specimen and background, e.g., A and
B, in the scanned area.

Cminimum ~ 2% for human eye to

distinguish differences between the
specimen (image) and its
http://www.youtube.com/watch?v=SVK4OkUK0Yw background.
at~1:47-3:04
 Grain Size Examination

Objective Lens

x100

Reflected OM
 Grain Growth - Reflected OM

5m 30mm
m

Polycrystalline CaF2 Large grains in polycrystalline

illustrating normal grain spinel (MgAl2O4) growing by
growth. Better grain size secondary recrystallization
distribution. from a fine-grained matrix
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Scanning electron
microscopy (SEM)
Dr Aneela Wakeel
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The most versatile instrument for a materials

scientist?
What can we study in a SEM?
• Topography and morphology
• Chemistry
• Crystallography “Easy” sample
• Orientation of grains preparation!!
• In-situ experiments:
• Reactions with atmosphere “Big” samples!
• Effects of temperature
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How do we get an image?

Electrons in
Electrons out

or: x-rays out

• In brief: we shoot high-energy electrons and

analyze the outcoming electrons/x-rays
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Components of the instrument

• electron gun (filament)
• electromagnetic optics
• scan coils
• sample stage
• detectors
• vacuum system
• computer hardware and
software
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Probe scanning
• Probe scanning is operated by a beam deflection system incorporated within
the objective lens in an SEM. The deflection system moves the probe over
the specimen surface along a line and then displaces the probe to a position
on the next line for scanning, so that a rectangular raster is generated on the
specimen surface.
• The signal electrons emitted from the specimen are collected by a detector,
amplified, and used to reconstruct an image, according to one-to-one
correlation between scanning points on the specimen and picture points on a
screen of a cathode ray tube(CRT) or liquid crystal display.
• The deflection system of the electron probe is controlled by two pairs of
electromagnetic coils (scan coils). The first pair of coils bends the beam off
the optical axis of the microscope. The second pair of coils bends the beam
back onto the axis at the pivot point of a scan.
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How do we get an image?

Electron gun
156 electrons!
288

Detector

Image
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Electron guns
• We want many electrons per time unit per
area (high current density) and as small
electron spot as possible
• Traditional guns: thermionic electron gun
(electrons are emitted when a solid is
heated)
• W-wire, LaB6-crystal

• Modern: field emission guns (FEG) (cold

guns, a strong electric field is used to
extract electrons)
• Single crystal of W, etched to a thin tip
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Electron guns
• A field emission gun is 1000×brighter than a tungsten thermionic gun and
100×brighter than a LaB6 thermionic gun. The brightness is proportional to
the acceleration voltage (Vo) of the gun.
• With field emission guns we get a smaller spot and higher current densities
compared to thermionic guns
• Vacuum requirements are tougher for a field emission guns

Single crystal of LaB6 Tungsten wire Field emission tip

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Signal detection
When high energy electrons strike a specimen, they produce either elastic or
inelastic scattering.
Elastic scattering produces the backscattered electrons (BSEs), which are
incident electrons scattered by atoms in the specimen. BSEs are typically
deflected from the specimen at large angles and with little energy loss; they
typically retain 60–80% of the energy of incident electrons.

Inelastic scattering produces secondary electrons(SEs), which are electrons

ejected from atoms in the specimen. SEs are typically deflected at small angles
and show considerably low energy compared with incident electrons. During
inelastic scattering, an incident electron transfers kinetic energy to an electron
in a specimen atom. Any electron in atoms in the specimen with sufficient
kinetic energy will leave its orbital to become a secondary electron. The SE
energy is usually in the range of about 3–5 eV.

In terms of usefulness, SEs are the primary signals for

achieving topographic contrast, while BSEs are useful for
formation of elemental composition contrast.
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• Secondary electrons: Everhart-Thornley Detector
• Backscattered electrons: Solid State Detector

Detectors • X-rays: Energy dispersive spectrometer (EDS)

Backscattered electron
detector:
(Solid-State Detector)

Secondary electron detector:

(Everhart-Thornley)

Image: Anders W. B. Skilbred, UiO

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Why do we need vacuum?

• Chemical and thermal stability is necessary for a well-
functioning filament (gun pressure)
• A field emission gun requires ~ 10-10 Torr
• LaB6: ~ 10-6 Torr
• The signal electrons must travel from the sample to the
detector (chamber pressure)
• Vacuum requirements is dependant of the type of detector
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Contrast formation

• There are two types of contrast in SEM images:

topographic and compositional. The secondary electrons
are the primary source for surface topographic images,
while backscattered electrons are mainly used for
compositional images.
• Knowledge about the interaction between the high energy
electron probe and the specimen is necessary for
understanding these mechanisms of contrast formation.
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Electron beam-sample interactions

• The incident electron beam is scattered in the sample,
both elastically and inelastically.
• Interaction volume increases with increasing acceleration
voltage and decreases with increasing atomic number

Images: Smith College Northampton, Massachusetts

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Signals from the sample

Incoming electrons
Secondary electrons
Auger electrons
Backscattered Cathodo-
electrons luminescence (light)

X-rays

Sample
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Where does the signals come from?

• Diameter of the interaction

volume is larger than the
electron spot
 resolution is poorer than the
size of the electron spot

Image: Department of Geology and

Geophysics, Louisiana State University
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Secondary electrons (SE)

• Generated from the collision
between the incoming electrons
and the loosely bonded outer
electrons
• Low energy electrons (~10-50
eV)
• Only SE generated close to
surface escape (topographic
information is obtained)
• Number of SE is greater than the
number of incoming electrons
• We differentiate between SE1
and SE2
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Backscattered electrons (BSE)

• A fraction of the incident
electrons is retarded by the
electro-magnetic field of the
nucleus and if the scattering
angle is greater than 180 ° the
electron can escape from the
surface

• High energy electrons

(elastic scattering)
• Fewer BSE than SE
• We differentiate between
BSE1 and BSE2
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BSE vs SE

Images: Greg Meeker, USGS

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X-rays
• Photons not electrons
• Each element has a fingerprint X-ray
signal
• Relatively few X-ray signals are
emitted and the detector is inefficient
 relatively long signal collecting times are
needed

• Most common spectrometer: EDS (energy-dispersive spectrometer)

• Signal overlap can be a problem
• We can analyze our sample in different modes
• spot analysis
• line scan
• chemical concentration map (elemental mapping)
 MENA3100 57

Topography and morphology

• High depth of focus

Image: Christian Kjølseth, UiO Image: Camilla Kongshaug, UiO

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Depth of focus
Optical microscopy vs SEM

Screw length: ~ 0.6 cm

Images: the A to Z of Materials

• A SEM typically has orders of magnitude better

depth of focus than a optical microscope making
SEM suitable for studying rough surfaces
• The higher magnification, the lower depth of focus
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Topographic contrast
Topographic contrast in an SEM refers to variation in signal levels that corresponds
to variation in geometric features on the specimen surface. An SEM image with
topographic contrast often has the stereoscopic appearance of a rough specimen
surface.
Topographic contrast occurs because signal electrons arise from two effects: the
trajectory effect and the electron number effect.
The trajectory effect arises from variations in how the specimen surface is
oriented with respect to the detector.
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Topographic contrast
In an SEM image, the electron number effect will create bright areas in the image
that do not correspond to surface contours on the specimen. Figure 4.13 illustrates
the electron number effect. When the electron probe hits a surface at an angle,
more electrons can escape from the specimen than when the probe hits a flat
surface directly. Thus, certain areas of the specimen (such as edges of spherical
particles, raised areas and cavities) will appear bright in an SEM image. Figure 4.14
shows the example of topographic contrast from the electron number effect

Commonly, a topographic image is obtained

by operating an SEM in the SE mode.
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Compositional Contrast
Compositional contrast refers to the variation in gray levels in an SEM image that
correspond to variation in chemical composition in a specimen.
An image formed by BSEs exhibits very useful compositional contrast if the
specimen consists of more than one chemical element.
The origin of compositional contrast arises because the capability of BSEs to
escape from the specimen depends on the atomic numbers of the specimen atoms

The backscatter coefficient (η) characterizes such capability.

Η is the ratio of the number of BSEs escaping from the

specimen (nBSE) to the number of incident electrons (ni).
It increases monotonically with the atomic number as
shown in Figure 4.15.
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Compositional contrast
Thus, any area in a specimen containing chemical elements with higher atomic
number will generate more BSEs. The difference in the number of BSEs collected
by a detector will appear as differences in gray levels in a black and white image;
that is, an area with atoms of higher atomic numbers will appear brighter. Thus, a
BSE image shows the atomic number contrast or compositional contrast as
demonstrated in Figure 4.16
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In-situ imaging
• A modern SEM can be equipped with various
accessories, e.g. a hot stage
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Some comments on resolution

• Best resolution that can be obtained: size of the
electron spot on the sample surface
• The introduction of FEG has dramatically improved the
resolution of SEM’s
• The volume from which the signal electrons are
formed defines the resolution
• SE image has higher resolution than a BSE image
• Scanning speed:
• a weak signal requires slow speed to improve signal-to-
noise ratio
• when doing a slow scan drift in the electron beam can
affect the accuracy of the analysis
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Summary
• The scanning electron microscope is a versatile
instrument that can be used for many purposes
and can be equipped with various accessories
• An electron probe is scanned across the surface
of the sample and detectors interpret the signal
as a function of time
• A resolution of 1 – 2 nm can be obtained when
operated in a high resolution setup
• The introduction of ESEM and the field emission
gun have simplified the imaging of challenging
samples
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Summary
Signals:
•
• Secondary electrons (SE): mainly topography
• Low energy electrons, high resolution
• Surface signal dependent on curvature
• Backscattered electrons (BSE): mainly chemistry
• High energy electrons
• “Bulk” signal dependent on atomic number
• X-rays: chemistry
• Longer recording times are needed
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Electron Back
Scattered Diffraction
 Introduction to EBSD
EBSD = Electron Backscatter Diffraction
EBSD is a technique that allows:

• Crystallographic Orientations
• Misorientations
• Texture trends
• Grain size and boundary types
• Phases

To be characterised and quantified on a sub-micron scale

 Visualization of Data
General
Micro-
structure

Deformed silica
(quartz)

=100 µm; BC+GB+DT+E1-3; Step=1 µm; Grid297x227

Pixel map of pattern quality + crystal orientation +

grain boundary location and character
Introduction to EBSD - FSE Examples

• Nickel

• Austenitic
Stainless
Steel
Introduction to EBSD - Color Key for COMs
• COM with
Inverse Pole
Figure color key
for cubic
material
• Red = 100
• Green = 110
• Blue = 111
planes parallel
to the surface
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Difference between OM,EM

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TEM
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SCANNING PROBE MICROSCOPY

Background
• First scanning probe microscope invented in 1981 by
Binning and Roher
• Wide range of applications
• Topography/Atomic Structure
• Magnetic/Electric fields
• Surface temperatures
 Branches of Scanning Probe Microscopy

http://spm.phy.bris.ac.uk/
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Operation

• Scanning probe
microscopes operate
by detecting the
deflection in the
cantilever
• Modern scanning
probe microscopes
use a split photo
diode to detect the
deflection http://spm.phy.bris.ac.uk/
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• Scanning probe microscopes employ a tiny probe with a very

sharp tip that is brought into very close proximity (i.e., to
within on the order of a nanometer) of the specimen surface.
• This probe is then raster-scanned across the plane of the
surface. During scanning, the probe experiences deflections
perpendicular to this plane, in response to electronic or other
interactions between the probe and specimen surface.
• The in-surface-plane and out-of-plane motions of the probe
are controlled by piezoelectric ceramic components that have
nanometer resolutions.
• Furthermore, these probe movements are monitored
electronically and transferred to and stored in a computer,
which then generates the three dimensional surface image.