Electron Microscopy for

Materials Characterization

SMSE, NITC
 Introduction to microscopy
 Microscope - Used to ‘see’ objects not visible to the human eye (from the
Greek: μικρός, mikrós, "small“ and σκοπεῖν, skopeîn, "to look" or "see")
 Seeing is believing
 Human eye can ‘resolve’ objects ~ 0.1mm apart. For anything closer, we
need a means of magnifying
 Note : BIG difference between ‘seeing’ and ‘resolving’ Robert Hooke's
microscope
Seeing a car approaching (from its headlights)
Resolving the two headlights as separate sources of light

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 Microscope and resolution
o Resolving power is the ability of the components of an
imaging device to measure the angular separation of the
points in an object.
o The term resolution or minimum resolvable distance is
the minimum distance between distinguishable objects in
an image.
o Magnification: Image size/Object size

Eye
Optical System - Components
Radiation source – Visible light
System of lenses and apertures
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 Why microscopy?

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 Why microscopy?
Micro and nano view of gecko's toe
o Morphology: The shape and
size of the particles making
up the object; direct
relation between these
structures and Materials
properties (ductility,
strength, reactivity etc.)
o Topography: The surface
features of an object or
“how it looks” its Texture;
direct relation between
these features and Materials
properties (hardness,
reflectivity)
17-09-2021 CC BY-SA 3.0, https://en.wikipedia.org/w/index.php?curid=25482399 5
 Why microscopy?

A modern light microscope (OM) has

a magnification of about 1000x and
enables the eye to resolve objects
separated by 0.0002 mm

“Resolution limit”

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 Microscope and resolution
o Any system used to form an image uses lenses and apertures that have a
certain dimension
Limit to resolution arises from the phenomenon of diffraction

Diffraction from a single slit

Intensity at any
point ~ ((sin(a))/a)2

A big maximum surrounded by smaller maxima

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 Rayleigh Criterion
Profiles from two adjacent point will overlap
To be able to resolve two points as distinct, To increase resolution

qR = sin-1(1.22 l /d) Large d (‘Big’ lens)

Small l (small wavelength light)
This is the diffraction-limited resolution limit

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 Electrons as ‘light’ source - principle
Electrons as Waves - The particle-wave duality
Electron moving with a velocity ‘v’ has a wavelength associated with it
To increase resolution
l = h/mv = h/p
Large d (‘Big’ lens)
Ek = ½ mv2 = p2/2m = eV
Small l
l = h/p = h/(2meV)½
l (in Angstrom) ~ 12.247/(V (in volts))½
Accelerating
Typical for Scanning Electron Wavelength (nm)
Voltage (kV)
Microscopy – 5-30 kV
10 1.22
At the acceleration voltages used in
Transmission Electron Microscopy, 20 0.86
relativistic effects needs to be considered 100 0.37
200 0.25
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 Electrons as ‘light’ source

Resolution did improve!

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 Electrons as ‘light’ source - History
o In the 1920s it was discovered that accelerated electrons behave in vacuum just like light.
They travel in straight lines and have a wavelength which is about several times smaller than
that of light. Furthermore, it was found that electric and magnetic fields have the same
effect on electrons as glass lenses and mirrors have on visible light.
o Dr Ernst Ruska at the University of Berlin combined these characteristics and built the first
transmission electron microscope (TEM) in 1931 who was awarded with Nobel Prize in
Physics for 1986.
o The first published description appeared in 1935 in a paper by the German physicist Dr Max
Knoll. Although another German physicist Dr Manfred von Ardenne performed some
experiments with what could be called a scanning electron microscope (SEM) in 1937.
o In 1942 three Americans, D. Zworykin, Dr Hillier and Dr Snijder first described a true SEM
with a resolving power of 50 nm and a magnification of 8000x.

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 Electrons as ‘light’ source - History

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 Electrons as ‘light’ source - History

Modern day SEM

Old SEM

Modern day SEMs can have a resolving

power of better than 0.5 nm and can
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 Electron Microscopy - Applications
o Topography (Imaging) - The surface features of an object or "how it looks", its texture;
detectable features limited to a few nanometers
o Morphology (Imaging) - The shape, size and arrangement of the particles making up
the object that are lying on the surface of the sample or have been exposed by
grinding or chemical etching; detectable features limited to a few nanometers
o Composition (Microanalysis) - The elements and compounds the sample is composed
of and their relative ratios, in areas ~ 1 micrometer in diameter
o Crystallographic information (Diffraction) - The arrangement of atoms in the
specimen and their degree of order; only useful on single-crystal particles >20
micrometers
 Scanning Electron Microscopy (SEM)
Unlike optical microscope, SEM does not ‘project’
an image
Basics of SEM Operation
• Electron gun produces a ‘beam’
Thermionic/Field-emission guns (5-30 kV)
• Produce a ‘tight’ spot on the specimen surface
Condenser and Objective lenses (Electromagnetic
lenses converge electron beam)
• Scanning coils ‘raster’ the beam across the
specimen
Size of scan (scan area)  Magnification
• Electron-specimen interactions
Produces a wide variety of signals
• Detectors to collect the signal
Always in
Different detectors for different signals
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 The sample
Sample can be An ideal sample should be

• Powder, thin film or bulk pieces • Clean

• Conducting/non conducting • Small (Easily fits on the stub for signal collection)

• Biological, polymer, metallic, ceramic • Conducting

• Does not outgas
• Non-magnetic

Sample storage and handling

• Protect from dust and humidity
• Powder free gloves and tweezers
• Cleaning with compressed air, solvent, ultra sonication
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 Sample preparation

o Sample mounted on aluminium stubs and sticked to

conducting C or Cu tape, Ag or C paint/paste
o Specimen stage is grounded
o Non conducting samples can be imaged either at
low kV or can be coated with C or Au to avoid
overcharging and related sample damage

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 Scanning and Magnification

More signal appears

Whitish in the image

Small signal appears

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 Electron - specimen interactions
Elastic and inelastic scattering of electrons with the sample produces many signals including
photon and electron signals

Based on the signals and detectors used various information can be obtained
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 Interaction volume and escape depth

Ref. Kelsall
 X-rays
2 Types of X-rays
Characteristic x-rays
Elemental identification 1.5406 Å
Quantitative analysis
Continuum x-rays
Background radiation
must be subtracted for
quantitative analysis

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 Example SE micrograph
Polymer sample on a carbon tape Polycrystalline CrNbO4 on Al2O3

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 SE and BSE micrograph comparison

https://www.gla.ac.uk/schools/ges/research/researchfacilities/isaac/services/scanning
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 Example BSE image and composition analysis

Si dispersed Al
doped β-FeSi2

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 SEM - Advantages
SEM is the most widely used of all electron beam instruments.
o It is versatile of its various modes of imaging (Z contrast, topography contrast etc.)
o Excellent spatial resolution (up to 0.5 nm with FEG SEM)
o Magnification as low as 5 X to 10,00,000 X, i.e. from naked eye to nanometer dimensions.
o Very modest requirement on sample preparation and condition
o Relatively straightforward interpretation of the acquired images
o Accessibility of associated spectroscopy and diffraction techniques
o User friendly
o High level of automation and high throughput
o Biological and non-conducting samples can be used
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 Specimen damage by electron beam
The loss of electron beam energy in the specimen occurs mostly
in the form of heat generation at the irradiated point.
The temperature increase at an irradiated point is dependent on:
1. The electron beam accelerating voltage and dosage
2. Scanning area
3. Scanning time
4. Heat conductivity of the specimen.
Polymer materials and biological specimens, which are generally
not resistant to heat are easily damaged by the electron beam,
because of their low heat conductivity
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 Contamination
When the electron probe is irradiated on a specimen portion for a long time, its image may
lose sharpness and become dark.

This is caused by the residual gas in the vicinity of the

specimen being struck by the electron probe. This
phenomenon is called specimen contamination.
This may be the:
Gases caused from the instrument itself
Gas that specimens bring into the instrument
Gas that the specimen itself gives off.
Specimen: ITO
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 Charging artefacts
Abnormal contrast Formation of strips

Dust Toner
particle powder Avoided by
coating the
sample with
metal film

Calcite
crystal

Bee hive

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 Transmission Electron Microscopy
TEM is a “great” instrument capable of
Imaging
Diffraction from the same area on the specimen
Chemical Analysis
Electron energy 100s of keV
Thin ‘electron-transparent’ specimen (~100 nm)

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 The instrument
Optical & Electron Microscopes Comparison

Cu grid

Sample holder
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 Diffraction and imaging

The changes in a uniform, parallel beam of electrons after passing through an

electron-transparent specimen. The spatial variation in the intensity of the beam
constitutes the image, while the angular variation after passing through the specimen
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Example micrograph Example diffraction pattern

HRTEM

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 Drawbacks
• Can take a lot of time to make sample thin enough to be transparent to electrons
• The composition of the sample can also be damaged during preparation
• Viewing area only shows a small section of the sample being analysed, which can differ
from the rest of the sample
• The sample can be damaged by the electrons, especially when dealing with biological
samples

Beware of projection
artifacts!
No depth sensitivity
Averaged through the thickness

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 References and further information
1.https://www.youtube.com/watch?v=eOyfoMRHfgE&ab_channel=TheKavliNanoscienceInstituteatCaltech
A superb video on basic concepts of SEM.
2. https://myscope.training/#/SEMlevel_3_1
This is an excellent site by Microscopy Australia which provides an online learning environment for those who
want to learn about microscopy. The platform provides insights into the fundamental science behind different
microscopes, explores what can and cannot be measured by different systems and provides a realistic
operating experience on high end microscopes.
You can experience the SEM operation using the simulator!

3. http://cleanenergywiki.org/index.php?title=Scanning_Electron_Microscope
An excellent set of 6 videos about the practical sample preparation and operation of an SEM. Please note that
some of the details mentioned in the video (for example the graphical user interface) is specific to the SEM
system (company and model) they are using. So, please don’t use this video to use an SEM by your own!

4. David B. Williams and C. Barry Carter, Transmission Electron Microscopy: A Textbook for Materials Science

5. Joseph l. Goldstein et al., Scanning electron Microscopy and X-ray microanalysis, Kluwer Academic /
Plenum Publishers

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