19-Feb-15

Scanning Electron Microscopy Scanning Electron Microscopy

(SEM) (SEM)
Contents
Dr. Mohsin Ali Raza • Introduction (What is SEM used for?)
• Resolution
• Interaction of Electrons with samples
• Secondary Electrons
• Backscattered Electrons
• Characteristic X-rays
• Other Electrons
• Component of SEM
• Depth of field
• Image formation
• Magnification
• Specimen preparation
• Selective SEM images

What is SEM used for? How SEM works?

A tiny beam of high energy electron is scanned on the surface of the specimen
XRD for crystal structure analysis and SEM for analysis of microstructures

We can study
• Topography and morphology
• Orientation of grains SEM offers high
resolution, magnification,
• Elemental composition/mapping/contrast
easy sample preparation.
• Fracture surfaces In situ experiments at
(high temperature or in
• Electronic devices/circuits
controlled atmosphere)
• Fibres, particles, coatings
can also be performed
• Defects, porosity
Electrons in
Electrons out
or: x-rays out
Interaction of electrons
with the specimen surface
produces electrons signals
• Secondary electrons
• Backscattered electrons
These electrons are
detected by suitable
detector and converted into
image

Topography and morphology Depth of focus

• High depth of focus Optical microscopy vs SEM

Screw length: ~ 0.6 cm

• 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

MENA3100

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Elemental mapping In-situ imaging

Ce • A modern SEM can be equipped with various
accessories, e.g. a hot stage

Fe Sr

In-situ imaging: oxidation of steel at high Optical Micrscopy vs SEM

temperatures OM SEM
Light source Electrons
• 800 °C, pH2O = 667 Pa
Limit of resolution ~ 2000 Å ~ 5 nm
• Formation of Cr2O3

Useful Magnification 1000-2000x 15-200,000x

2 min 10 min 90 min (limited by power of optical lens) (magnetic lens)

Surface topography, microstructure, Elemental mapping, orientation of

phase analysis grains (visualise structures normally not
possible with optical microscope)
Short depth of field Greater depth of field

Can Show original colour of image Image black and white

Optical Micrscopy vs SEM Optical Microscopy vs SEM

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Resolution Resolution

The minimum distance by which two structures can be

separated and still appear as two distinct objects is
called “Resolution”

Resolution is limited by the

“Wavelength of the illumination source”

“When the centre of two peaks are separated by a distance equal to

radius of Airy disk, the two objects can be distinguished”

Abbe’s Equation Interactions of Electrons with Samples

Elastic Scattering
Abbe’s Equation describes resolution in perfect optical system
• Incident electrons deflected by specimen atomic nucleus or by outer
electrons

• No energy loss

• Electrons elastically scattered through an angle of more than 90° are

called Backscattered Electrons (BSE)

Inelastic Scattering

• Occurs in various ways in which incident electrons transfer their energy to

the specimen atoms
First Transmission Electron microscope was constructed in 1930 by
replacing illumination source with electrons and condenser lens with • Secondary electrons generated due to ionisation of specimen atoms (50
electromagnetic coils in light microscopes eV energy used for imaging)

• Emission of characteristics x-rays, Auger Electron and

Cathodoluminescence

Interactions of Electrons with Samples Interactions of Electrons with Samples

Energetic electrons penetrate into the sample for some distance
and produce a “Region of primary excitation”
• RPE produces variety of signals
• Size and shape of the zone depends on the electron energy (voltage), atomic
number and density
• The volume and depth of penetration increase with increase of beam energy
and decrease with increase of atomic number

Images taken at 3KV

give better surface
information than at
20KV

Interaction volume
Interaction volume
is like hemisphere
is like Tear drop

Use of a high accelerating voltage will result in deep penetration length and a
large primary excitation region resulting in loss of detailed surface information
of sample

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Secondary Electrons Secondary Electrons

• Emission of loosely bound electron from the sample surface upon Effect of surface topography and position of detector on the secondary
interaction of energetic electrons (ionisation). electron detection

• SE have low energy 3-5 eV, escape only from a region within few
nanometers of the material surface.

• SE gives topographic information with good resolution (for visualisation

of surface texture and roughness).

• SE can resolve surface structures down to 10 nm or better.

• SE reaching detector will generate image.

The Edge Effect
• SE prevented from reaching detector will generate shadows or be darker
in contrast than those regions that have unobstructed electron path to the More secondary electrons leave
detector. the sample at edges leading to
increased brightness
• Low voltage incident electrons will generate secondary electrons from
the very surface region, which will generate detailed structure information
on the sample surface.

Secondary Electrons Secondary Electrons

Effect of Accelerating voltage Effect of Accelerating voltage

Secondary Electrons Secondary Electrons

Effect of Accelerating voltage and Atomic number on yield of SE and BSE Intensity of Secondary Electrons decreases as the distance
increases from incident beam
The number of SE and BSE emitted from the specimen for each incident electron are
known as the secondary coefficient (δ) and the backscattered electron coefficient (η),
respectively.

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Back Scattered Electrons Back Scattered Electrons

• Another way of imaging in SEM is use of BSEs
Comparison of Secondary electron signal and backscattering electron signal
• BSEs provide both compositional and topographic information

• A BSE is one which has undergone single or multiple scattering events and which
escapes from the surface with an energy greater than 50 eV.

• Roughly 10-50% of the beam electrons are backscattered toward their source,
and on average these retain 60-80 % of their initial energy.

• Higher the atomic number, higher will be the yield of BSEs .

• BSEs produce atomic number contrast in the SEM images.

• BSEs yield ~6% of light element carbon (dark will be image) but ~50% for heavier
element like gold or tungsten (brighter will be image as more electrons are
deflected).

• Lateral resolution of BSEs image is worse (1.0 μm) than SEs (10 nm)

• BSEs carry information about features that are deep beneath the surface.

Detecting Secondary Electrons Detecting Secondary Electrons

Everhart-Thornley Detector Everhart-Thornley Detector
A Scintillator-photomultiplier system known as ETD is used for SE detection

• Scintillator is biased with a voltage of ~+10 kV

• Metal grid prevents the high voltage of the scintillator affecting the incident
electron beam
• Improves the efficiency by attracting secondary electrons, and thus collecting
even those which were initially not moving towards the detector
ETD is very efficient, and for flat specimens almost all the secondary electrons are collected

Detecting Backscattered Electrons Detecting Backscattered Electrons

Old Method Robinson Type Scintillator Detector
• Signal received on ETD detector is not only due to secondary • Specially designed to increase solid angle of collection
electrons
• Can be used with rapid scan rates
• Some BSE are also entering the detector
• Bulky and may restrict the working distance of the microscope
• By switching off scintillator bias or by giving small negative
potential will exclude SE entering the detector and the
backscattered signal will be obtained.

• Only those BSE will reach detector which are travelling along the
direct line of sight towards the detector , resulting in lower yield.

• Method is now rarely used.

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Detecting Backscattered Electrons SEM Optics

Solid State Detector SEM purpose is to produce a fine beam of electrons incident on the specimen
• High-energy beam hits semiconductor, it produces electron-hole pair.

• By applying voltage to the detector, electron-hole pair will not recombine and can
be separated, thus producing current which can be amplified.

• The detector is a thin flat plate which is mounted on the objective pole piece, and
thus does not interfere with normal operation of the instrument.

• Slow response rate, unsuitable for rapid scan rates.

Ray Diagram of two Lens SEM

SEM Optics SEM Optics

Condenser Lens

The condenser lens of focal length (fc) produces demagnified image of the filament. Spherical Aberration

The diameter of the intermediate image (d 1) is given by

𝑣1
𝑑1 = 𝑑𝑜 ×
𝑢1
do diameter of the filament

Objective lens

The objective lens of focal length (fo) further demagnify the filament image, producing a probe
of diameter d on the surface of the specimen.

The diameter of the final probe (d) on the specimen is given by

𝑣2 𝑤𝑑
𝑑 = 𝑑1 × = 𝑑1 × The probe size can be
𝑢2 𝑢2
controlled by altering
wd or 𝑣2 is the working distance of the mircoscope. the strength of the
condenser lens.

SEM Optics Electromagnetic Lens

The rays entry is restricted by an aperture of diameter A, not all of the An electromagnetic lens are comprised of
electron beam which passes through the condenser lens can enter the windings of wire through which electric field is
objective lens. applied. This creates strong magnetic field
through which negatively-charged electrons
must pass.
The current in the final probe is given by

2
𝛼1
𝐼1 = 𝐼𝑜 ×
𝛼𝑜

The current decreases as the strength of the condenser lens increases

(probe becomes smaller), and also decreases as the aperture
diameter is reduced.

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Condenser Lens Aperture

Condenser lens converges the cone of electron beam to a spot. The closer the
spot to the condenser lens smaller the spot diameter. Condenser lens current The objective aperture arm fits above the objective lens in the SEM.
control initial spot size and is referred to as the spot size control.

The diameter of initial The aperture stops the

convergence affects electrons that are off-
the final diameter of the axis from progressing
spot on the specimen down the column. It
also narrow the beam
below aperture
depending on the size
of the hole selected.

Apertures help to
minimise spherical
aberrations.

Aperture Aperture
The objective aperture arm fits above the objective lens in the SEM. Decreasing the aperture size will reduce the beam angle α for the same WD,
resulting in an enhancement of the depth of field

The appropriate choice

of lens demagnification
and aperture size
results in a reduction of
the diameter of electron
beam on the specimen
surface (spot size), and
enhances the image
resolution.

Aperture Aperture

Effect of aperture on depth of field Effect of Working Distance on depth of field

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Aperture Astigmatism

• The imperfection on the electromagnetic lens is called

Effect of Working Distance on depth of field
astigmatism.

• An Elliptical cross section is formed instead of circular one (the

image will stretch out at underfocus and overfocus conditions).

• A series of coils surrounding the electron beam (stigmator), can be

used to correct astigmatism and achieve an image with higher
resolution.

• Astigmatism is common at high magnification but less at low

magnification and hence is performed at the increased
magnification.

Astigmatism Astigmatism

The image in the centre shows a correctly focused image that has also been corrected for
astigmatism. At left and right are examples of poorly corrected astigmatism, seen as
streaking of the image.

Objective Lens Designs Objective Lens Designs

The Asymmetric pinhole lens

Pros: Offers a field-free
region above the specimen
for detecting secondary
electrons
Cons: Large lens aberration

The Symmetric immersion

lens

Pros: Specimen in the lens, The Snorkel lens

reduces focal length Pros: Snorkel lens produces
significantly (lowest lens strong magnetic field extending
aberration) to specimen.
Cons: Specimen size cannot Low lens aberration and allows
exceed 5 mm large specimen.
Two SE detectors (conventional
and in-lens can be used)

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GEMINI-The Principle of In-Lens Detection Advantage of In-Lens Detection

The electron optical column possesses a

positively biased booster that shifts the
energy of the primary electrons Topographic information

Compositional contrast, supresses

charging and edge effects allowing
accurate metrology to be performed

Advantage of In-Lens Detection Scanning Coils

• Scanner coils or pair of deflector plates (small coils of wire carrying the
Image of graphite electrode controlling current) in the electron column , typically , in the final lens, deflect
the beam in x and y axes so that it scans in a raster fashion over a rectangular
Conventional Secondary electron detector In-lens Detector area of sample surface.

• The beam is scanned over the specimen in a series of lines and frames called
a raster. A raster can be thought of as arrays of picture points or pixels.

• In order to study more than a single location and eventually construct an

image, the beam must be moved from place to place by means of scanning
coils system.

• Scanning action is usually accomplished by energizing electromagnetic coils

arranged in sets consisting of two pairs, one pair each for deflection X and Y
directions.
(LEO 1530 Gemini, operated at 1 keV)
• Scanning action is produced by altering the strength of the current in the scan
coils as a function of time, so that the beam is moved through a sequence of
Homogeneous contrast Bright Contrast (low work
positions on the specimen (e.g., locations 1, 2, 3, 4, etc. in Fig. 4.1).
Topographic information is function), polymer fibres appears
dominant black (high work functions, no
• Slower scan rates allow more electrons to be collected at each point along the
electrons leaving the surface)
line of beam scan. This produces better quality image.

Scanning Coils Image Formation in SEM

Image quality can be improved

by increasing signal to noise
ratio (S/N). S/N increases as the
total number of electrons
recorded per picture point
increases

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Image Formation in SEM Image Formation in SEM

• In SEM image is built up successively during the scan.

• The amplified signal from the detector is output to a high quality cathode ray
tube (CRT), and the minimum size of spot which may be obtained on such a
CRT is about 0.1 mm.

• A 100 mm 2 CRT contain 1000 x 1000 discrete picture elements or pixels.

• To resolve two features A and B, each should have separate pixels.

• The working resolution of the instrument can not be better than pixel size which
is given by • If probe larger than specimen pixel, the signal from adjacent pixels is merged,
100 𝜇𝑚
𝑝= and the resolution degraded.
𝑀
• If probe is smaller than pixel size, the signal would be weak.
Scanned 10 μm x 10 μm
on the specimen, then on • If probe size is exactly same as the diameter of the pixels, high resolution
100 mm x 100 mm CRT achieves (required for optimum performance)
screen, the linear
magnification will be
10,000x.

Image Formation in SEM Electron Guns

Requirements
Resolution
• Produces a stable electron beam with high current

• Small spot size

• Adjustable energy

• Small energy dispersion

• Life of emitter is important consideration

Conventional SEM used “hairpin” or Lanthanum hexaboride (LaB6) cathodes

(based on thermionic emission i.e., high temperature is required to
overcome the work function of the metal so that electrons can escape from
cathode)

Modern SEM use “Field Emission” source which produces high current and low
energy dispersion

Tungsten Electron Guns Tungsten Electron Guns

Tungsten Electron guns are composed of three parts:
(0.1-30 kV)
• V-shaped hairpin tungsten filament (the cathode) (100 μm in dia)
• Wehnelt Cylinder
• Anode

Filament is heated to 2,800 K by

applying a filament current so
that electrons can escape from
the surface of the filament tip.

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Tungsten Electron Guns Lanthanum Hexaboride Electron Guns

• LaB6 produces stronger emission of electrons at same heating temperature as
Electron Emission depends on filament current that of tungsten due to its low work function (2.4 eV) than tungsten (4.5 eV).

Advantage
Low cost, suitable for low
magnification imaging and for
microanalysis
The highest electron • 5 to 10x greater brightness and longer life time compared with conventional
emission is obtained by least tungsten guns
amount of current called
saturation current. • LaB6 single crystal 100–200 μm in diameter and 0.5 mm long and is mounted on
Electrons are emitted from graphite which act as the resistive heater to elevate the temperature of the
the tip of the filament and crystal.
focused in tight bundle by
the negative accelerating
voltage.
Advantage Disadvantage
-Smaller emission Readily
area reduces spot oxidised at
size. high
-Smaller energy temperature.
spread resulting in
At false peak, life of filament high resolution and To increase life
increases but beam stability smaller chromatic time high
decreases aberration vacuum (10-8
Life influenced by vacuum -Can be replaced Torr) required
status and cleanliness of gun easily in conventional
SEM

Field Emission Guns Types of Field Emission Guns

• In the FEG, a single crystal tungsten wire with very sharp tip, generally prepared
• Cold Field Emission
by electrolytic etching, is used as the electron source.
Operates at room temperature, high brightness due to small diameter of electron
beam and emission area
• V1 is the of few kilovolts provided to emit electrons and Vo is used for
accelerating electrons
• Thermal Field Emission
Operates at elevated temperature, flashing (2000 K for few seconds), high
• Extracting electrons from a material by applying a very large electric field. By
temperature cleans the gas adsorbed on the tip, stable beam even if vacuum
drawing tungsten wire to a very fine point (<100 nm , application of a potential of
degrades
1 kV gives an electric field of 1010 A m -1 which is large enough to allow electrons
to tunnel out of the sample. This is called field emission). • Schottky Emitters
To get emission from the source it is
• FEG offer higher brightness, longer life, high resolution. operated at an elevated K) in a
vacuum of ~10-9 mbar and the
electric field at the tip end is
of the order of ½-1 V/nm.

SE and CFE have superior performance in terms of brightness, source size and life
time. SE has 100 x larger area than CFE and is capable of delivering more than 50x
higher emission current than CFE. Probes smaller than 2 nm can be obtained which
provides higher resolution for SEM image. Field emitters must operate under
ultrahigh vacuum (10-9 Torr) to stabilise emission and to prevent contamination.

Vacuum Systems Vacuum Systems

• Ultrahigh vacuum is must for SEM (10-6 Torr or better)

• UHV increases electron mean free path and decreases scattering

Vacuum beter than 5 x 10-5 Torr
• Contamination of guns and other components can be prevented.
Longer pump down times
• Mechanical pump and diffusion pumps are employed to pump down the
chamber from atmospheric pressure.

Vacuum better than 5 x 10-5 Torr

Longer pump down times

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Specimen preparation Sputtering

• A technique used to deposit thin films of a material onto a surface ( “substrate").
• Any conducting or non-conducting sample • First a gaseous plasma is created and ions are accelerated from this plasma into
can be imaged. some source material ("target").
• The source material is eroded by the arriving ions via energy transfer and is ejected
• Nanoparticles, carbon nanotubes, in the form of neutral particles - either individual atoms, clusters of atoms or
nanowires, nanostructured materials, etc. molecules.
can be observed by loading them on carbon • As these neutral particles are ejected they will travel in a straight line unless they
tape. come into contact with something - other particles or a nearby surface. If a
"substrate" such as a Si wafer (Sample to be imagined) is placed in the path of these
• Conducting sample need no or little sample ejected particles it will be coated by a thin film of the source material.
preparation. Directly mount on the stub.
May need to provide conductive path with
Ag paint.

• Non-conductive samples need metal

coatings (sputter coating of gold, silver,
platinum, palladium)

• Fractured surfaces of polymer and

composites give better results.

Coating thickness 5-10 nm depending on the sample nature

Selective SEM images Selective SEM images

SEM image of Emiliania huxleyi Cells SEM image of virus (T4 Bacteriophage)
Mag: 25,000X

SEM of nitrogen pearlite surrounded by SEM of granular nitrogen pearlite

proeutectoid ferrite (etching with HF)

SEM image of Mosquito Head

Selective SEM images Selective SEM images

SEM of Stress corrosion cracking in 300 Pitting corrosion in 300 series stainless SEM of Ductile fracture in 300 SS Cleavage fracture
series steel steel backscattered SEM image

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Selective SEM images Selective SEM images

SEM micrographs for the Fe-10Ni-15Al alloy aged at 750°C for (a) 75, (b) 250, and (c) 500 h,
and at 920°C for (d) 25, (e) 100 and (f) 200 h.

http://www.intechopen.com/books/scanning-electron-microscopy/sem-
analysis-of-precipitation-process-in-alloys

Selective SEM images

Transmission Electron Microscope

Fig. Cross section SEM images of a
304SS/Ni/Au sample with thick, 70
μm, Au layer electroplated, (a) at
low magnification (2000 x),
showing the entire Au layer, (b ) at
medium magnification (5000 x),
displaying SS/Ni/Au assembly at a
closer view,(c ) at high
magnification (10000 x), showing
that Ni/Au bonds well to SS
substrate

Interaction of Electrons with Materials Resolution of TEM

The distance between two details just separable from one another
is called “Resolution”.

For electron beam

0.61𝜆
𝑑= (Rayleigh Criterion)
sin 𝛼

𝜆 is wavelength of light, and α is the maximum angle between

incident and deflected beam in the limit of lens aberration.

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Resolution of TEM Definition of major angles in TEM

• In a TEM, the electrons are accelerated at high voltage (100-1000 kV) to

a velocity approaching the speed of light ; they must therefore be
considered as relativistic particles.
• Angle of incidence/convergence
• The associated wavelength is five orders of magnitude smaller than the angle of beam is α,
light wavelength (0.04-0.008 Å). The vacuum requirement is much
higher for TEM than SEM. • Collection angle is β

• The magnetic lens aberrations limit the convergence angle of the • Scattering angles are θ
electron beam to 0.5° (instead of 70° for the glass lens used in optics),
and reduce the TEM resolution to the Å order. • All angles are measured from the
optic axis, an imaginary line along
• This resolution enables material imaging and structure determination at the length of TEM Column
the atomic level.

• TEM is used for imaging defects (dislocations), nanoparticles/coatings,

average structure (lattice parameter), chemical composition analysis.

Ray Diagram of TEM TEM Structure

• Electron source

• Ist condenser lens

• 2nd condenser lens

• Objective lens

• Projection lens

• Screen

TEM Structure TEM Structure

• Ist Condenser lens

The Ist condenser lens

demagnetises the source,
either to increase
brightness or decrease the
area of the specimen that is
illuminate.

• 2nd Condenser lens

It controls convergence
angle of the beam on the
specimen.

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TEM Structure TEM Structure

Ray Diagram of TEM Imaging in TEM

• Electrons from condenser lens

are scattered by the sample
situated in the object plane of
the objective lens.

• Electrons scattered in same

direction are focused in back
focal plane, and, as a result
diffraction pattern is formed
there.

• Electrons coming from the

same point of the object are
focused in the image plane

The first intermediate image is magnified by further lenses

Bright Field Imaging Dark Field Imaging

• In BF mode, an aperture is
placed in the back focal plane
of the objective lens which
allows only the direct beam to
pass. • In DF mode, the direct beam
is blocked by the aperture
• Image result due to weakening while one or more diffracted
of the direct beam by its beam are allowed to pass the
interaction with the sample. objective aperture.

• Thickness of the sample and • Diffracted beam interact

diffraction contrast contribute strongly with the atoms.
to image formation.

• Image interpretation is
sometimes tricky

Thick areas, areas in which heavy atoms are enriched and crystalline areas Useful information about stacking faults, planar defects, or particle size can
appear dark be obtained.

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Examples of Bright Field Imaging Examples of Bright Field Imaging

Figure : Bright field TEM images of benzylthiol-gold nanoparticles prepared

with Au/S molar ratio 15:1 (A4) taken with different magnification. The particle
agglomeration is well pronounced (a) and only very few isolated particles can
be observed (b, c). The average particle size is about 9 nm (c).

Examples of Bright Field Imaging Examples of Bright Field Imaging

Au nanoparticles
under BF microscope Bright field imaging of Perovskite nanoparticles

Examples of Bright Field Imaging Examples of Bright Field Imaging

Bright field imaging of Carbon black nanoparticles

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Examples of Dark Field Imaging Examples of Dark Field Imaging

TEM images of a thermoplastic vulcanized (TPV) specimen imaged in different

Dark field image of precipitates (S’(S)) in a AlCuMg alloy (or 2024). modes: bright field conventional TEM of (A) unstained specimens; (B) high-angle
annular dark field scanning TEM image of the same area as imaged in A (arrows
indicate same specimen features)

Examples of Dark Field Imaging Schematic illustration of BF and DF imaging

TEM BF and DF images of the same area of microcrystalline ZrO 2. In the BF image (left), some
crystals appear with dark contrast since they are oriented (almost) parallel to a zone axis (Bragg
contrast). In addition, thickness contrast occurs: areas close to the edge are thinner and thus
appear brighter (lower right side) than those far of the edge (upper left side). In the DF image
(right), some of the microcrystals appear with bright contrast, namely such whose diffracted
beams partly pass the objective aperture.

Lattice Images-High Resolution TEM Examples of HRTEM images

• In Lattice imaging mode, a

large objective aperture has to
be selected that allows many
beams including direct beams
to pass.

• The image is formed due to

phase contrast.

• If the point of resolution of

microscope is sufficiently high
and a suitable crystalline
sample is oriented along a
zone axis, then high resolution
TEM (HRTEM) images are HRTEM image showing a dislocation and Burgers vector b
obtained.

The lattice fringes, one dimensional or 2-D lattice images of a specimen can
directly be investigated by HRTEM. Simulation of the lattices can be used to
find atomic positions.

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Examples of HRTEM images TEM Specimens

• For best resolution, specimen must
be extremely thin (a few
nanometers).

• Specimen diameter 3 mm.

• Align specimen very accurately with

the electron beam to achieve the
required images. Specimen Holder

• Nanoparticles can be imaged

High resolution TEM image of a HRTEM image of Carbon black nanoparticles without any preparation.
graphite shell abandoned by a Ni
core. The arrow indicates the • Metallurgical samples require
outflow channel of the Ni. Graphite special sample preparation
lattice fringes are also visible on the
plane substrate.

Electron Diffraction in TEM EWALD SPHERE

Electrons can produce diffraction patterns in the same way as a beam of X-ray
does.
When beam hits a crystal, Ewald Sphere shows sets of planes at (or close
to) their Bragg’s angles for diffraction to occur.

Difference between Electron diffraction and X-rays

• Electrons have much smaller wavelengths than x-rays

• Sample is very thin in the direction of electron beam (of the order of 100 nm or
less). It has to be thin so that enough electrons can be transmitted without
being absorbed by the sample

EWALD SPHERE EWALD SPHERE

When beam hits a crystal, Ewald Sphere shows which sets of planes at (or
close to) their Bragg’s angles for diffraction to occur.

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EWALD SPHERE EWALD SPHERE

• The small wavelength of electron beam makes the Ewald Sphere very large.

• The diffraction angle θ is very small (1-2°)

The diffraction pattern recorded for any particular k vector and lattice orientation is
The Ewald sphere diagram look like this so that whole layers of the reciprocal lattice end up usually seen as projection onto a 2-D film.
projected onto film or screen.

Differences between Electron Diffraction and XRD Electron diffraction patterns

• Due to large size of Ewald Sphere more reflections appear by Electron Electron diffraction patterns of Single crystal
diffraction than XRD.

• Diffraction angles are very small in ED than XRD.

• Electrons interaction with matter is much (106-107×) stronger than that of X-

rays. This has the advantage that the diffracted electron beams have a high
intensity and exposure times are in the order of a few seconds. ED patterns
can directly be observed on the viewing screen of the electron microscope.
Thus, orienting a crystal along a direction can be easily achieved by tilting
while observing changes of the ED pattern simultaneously. Furthermore,
diffraction patterns can be obtained from very small crystals selected with a
diffracted aperture (Selected Area Electron Diffraction SAED) and by a
focused electron beam even from nm-sized regions. Electron diffraction patterns of Ta97Te60 along two perpendicular
directions. The parameters of the tetragonal unit cell can be determined
• The disadvantage of the strong interaction is that multiple scattering plays from these SAED patterns: a = 27.6, c= 20.6 Å.
an important role, and the intensities of the reflections are much influenced
by this dynamical effect. This makes structure determination from ED more
difficult and less reliable than that from XRD data.

Electron diffraction patterns Electron diffraction patterns

Electron diffraction patterns of Single crystal Electron diffraction patterns of Polycrystalline sample

Shadow of direct
beam stop

Electron diffraction pattern of YbSi1.41 along [001]. The reflection

condition h+k=2n for hkl (C face centering) is fulfilled. ED pattern of polycrystalline platinum. The indices are assigned to the
diffraction rings in accordance of the face-centered cubic lattice of Pt
(reflection condition: h,k,l all even or all odd).

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Electron diffraction patterns Relationship of the spots with d-spacing

Electron diffraction patterns of Nanocrystalline Diamond

The distance rhkl on the pattern between the spot hkl and the spot 000 is
related to the interplanar spacing between hkl planes of atoms, dhkl by the
following equation:

Bright spot is the due 𝝀𝑳

to incident beam 𝒓=
𝒅𝒉𝒌𝒍

L is the distance between the sample and the film/screen

(λL is called Camera Constant).
How to index such patterns?

(i) Measuring ring diameters D1, D2, D3 …….

(ii) Calculation of the dhkl (using the expression: rdhkl=Lλ)
(iii) Use some structure database to index each ring.

Relationship of the spots with d-spacing Relationship between spots

Derivation Diffraction pattern is a projection of the reciprocal lattice on the screen. The
angle between the lines joining spots h1k1l1 and h2k2l2 to spot 000 is the same
𝒓𝒉𝒌𝒍 𝒅𝒉𝒌𝒍 = 𝝀𝑳 as the angle between the reciprocal lattice vectors [h1k1l1]* and [h2k2l2]*

From Fig.,
𝑟
= tan 2𝜃
𝐿

From Bragg’s Law (condition for diffraction)

𝜆 = 2𝑑ℎ𝑘𝑙 𝑠𝑖𝑛𝜃

Since in electron diffraction, angle is very small

tan 2𝜃 ≃ 2𝜃
𝑠𝑖𝑛𝜃 ≃ 𝜃 ( θ is in radian)

This follows:

𝑟ℎ𝑘𝑙 𝜆
𝐿
= 2𝜃 = 𝑑
ℎ𝑘𝑙

Hence, 𝒓𝒉𝒌𝒍 𝒅𝒉𝒌𝒍 = 𝝀𝑳

Indexing Electron diffraction pattern with known

Zone axis and Electron beam Electron beam orientation
[uvw]
Material : Copper
• The planes
parallel to electron Copper: Cubic (FCC)
beam will diffract.
Lattice parameter: 0.361 nm
• The incident
electron beam is Beam direction: [211]
the zone axis of
the reflecting sets Planes which will give reflections are those which
of lattice planes. have higher spacings (smallest rhkl values)

Planes which will give reflections belong to {111},

{200},{220}, {311},{222}, etc.

Weis Zone law is obeyed for (111) and (022)

Screen hu+kv+lw=0

For unknown beam direction consult table of angles and distance ratios

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Indexing Electron diffraction pattern with unknown Indexing Electron diffraction pattern with unknown
Electron beam orientation Electron beam orientation
Below is a schematic diagram (Fig. 1) of a selected area electron diffraction (SAED) Since copper is FCC, the allowed diffraction spots (based on structure factor) are
pattern from a phase within a microstructure, the camera constant at 200 keV is λL= hkl all even or all odd
8.092 nm mm. Analysis of this phase using a small probe and an energy dispersive X-
ray (EDX) spectrometer showed characteristic Kα, Kβ rays from Cu. 1 ℎ2 +𝑘 2+𝑙 2
= (a)
𝑑2 𝑎2

Using the lattice constant of copper 0.361 nm calculate values of d for various
hkl
38.8 mm Table 1

63.4 mm hkl d (Angstroms)

44.8 mm 111 2.087
002 1.808
022 1.278
113 1.09
222 1.044
Fig. 1 004 0.904

Indexing Electron diffraction pattern with unknown Indexing Electron diffraction pattern with unknown
Electron beam orientation Electron beam orientation
Measure (or read ) the values of r in mm from Fig. 1 and using formula
Now label planes in figure 1.
𝒓𝒉𝒌𝒍 𝒅𝒉𝒌𝒍 = 𝝀𝑳 002 222 Smallest
222 parallelogram
Calculate the values of d in Angstroms 111
111
r (mm) d calculated (Angstroms) hkl assigned on the 38.8 mm
basis of Table 1 220 220
000 63.4 mm
38.8 2.09 {111}
111 44.8 mm
44.8 1.81 {002} 111
63.4 1.28 {022}
222 002 222

Fig. 1

Fully indexed diffraction pattern

Curly brackets are for family of planes, specific (hkl) plane is indicated by (). The Now index rest of the diffraction spots (planes) by simple vector addition
previous equation (a) does not tell us which specific plane has given us spot.
Specific (hkl) planes are constructed by vector
addition and angles

Indexing Electron diffraction pattern with unknown Indexing Electron diffraction pattern with unknown
Electron beam orientation Electron beam orientation

What is the direction of Electron beam? What is the direction of Electron beam?

Beam is perpendicular to vectors (111) and (002) Alternatively [uvw] beam direction can be find by following equation for (h 1k1l1)
and (h2k2l2)
[uvw] (111) = 0 and [uvw] (002) = 0
u= k1l2-k2L1
u+v+w = 0 and 2w = 0, w = 0
v= l1h2-l2h1
u+v = 0 so u = -v w= h1k2-h2k1
So beam direction [UVW] = [110]

All the planes indexed in Fig. 1 should obey Weis zone law otherwise they
are not indexed correctly.

So check out for (222) and beam direction [110]

hu+kw+vl=0, (2x-1)+(-2x-1)+(-2x0)=0

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IndexIndexing Selected Area Electron diffraction pattern Alternative method for indexing when lattice parameter
pattern (spot pattern):
the SAED pattern
1)
(spot pattern):
Choose a parallelogram with smallest
as well as beam direction is is unknown
R1, R2, R3. The spots R1 and R2 choosen Any 2-D section of a reciprocal lattice can be defined by two vectors so
should not be collinear to origin or to we only need to index 2 spots. All others can be deduced by vector
each other.
h1k1l1 2) Measure distances R1, R2, R3 and angles addition.
h3k3l3 1, 2.
R3 If the crystal structure is known, the ratio procedure for indexing is:
R1 2 3) Calculate d1,d2,d3 (using the rule rd=L).
1 • Choose one spot to be the origin. Note: it does not matter which
4) Correlate the measured d-values with
R2 dhkl taken from the list of standard spot you choose.
h2k2l2 interplanar distances for the given
structure and ascribe h1k1l1 and h2k2l2 • Measure the spacing of one prominent spot, r1. Note: for greater
and h3k3l3 indices for the chosen three accuracy measure across several spots in a line and average their
spots. spacings.
5) Check the condition that h1+h2=h3;
k1+k2=k3; l1+l2=l3. (check it on Fig. 1) • Measure the spacing of a second spot, r2. Note: the second spot
6) Compare the measured angles (both 1 must not be collinear with the first spot and the origin.
and 2) with the calculated angles. • Measure the angle between the spots, φ.

IndexIndexing Selected Area Electron diffraction pattern when IndexIndexing Selected Area Electron diffraction pattern when
Beam direction is not known Beam direction is not known
the SAED pattern (spot pattern):
• Prepare a table giving the ratios of the spacings of permitted the SAED pattern (spot pattern):
diffraction planes in the known structure. Hint: start with the widest
spaced plane (smallest r). You only ever need to do this once for
each structure.

• Take the measured ratio r1/r2 and locate a value close to this in the table.
Assign the more widely-spaced plane (usually with lower indices) to the
shorter r value.
• Calculate the angle between pair of planes of the type you have indexed
using equations given in next slides. If the experimental angle,φ, agrees
with one of the possible values - accept the indexing. If not, revisit the table
and select another possible pair of planes.
• Finish indexing the pattern by vector addition.

IndexIndexing Selected Area Electron diffraction pattern when IndexIndexing Selected Area Electron diffraction pattern when
Beam direction is not known Beam direction is not known
the SAED pattern (spot pattern): the SAED pattern (spot pattern):

22
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Index Following SAED patterns of Cubic materials

Drawbacks of TEM and also find Beam direction or Zone axis

• High skills required to interpret images

• Operating is more difficult.

• 2D image of 3D things.

• Sample preparation of metallic materials or film is very complicated. 99 mm 45°

000
71 mm
71 mm

Pattern : FCC

Index Following SAED patterns of Cubic materials Index Following SAED patterns of Cubic materials
and also find Beam direction or Zone axis and also find Beam direction or Zone axis

61 mm
52.3 mm 45°
000 145° 35°
70 mm 61 mm
000 100 mm
73 mm

Pattern : BCC Pattern : FCC

Index Following SAED patterns of Cubic materials

and also find Beam direction or Zone axis

49.7 mm
59.8°
000 50 mm

88 mm

Pattern : BCC

23