3/2/2024

Scanning Electron Microscopy

(SEM)
Dr. Mohsin Ali Raza

Scanning Electron Microscopy

(SEM)
Contents
• 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

1
 3/2/2024

What is SEM used for?

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

How SEM works?

A tiny beam of high energy electron is scanned on the surface of the specimen

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

2
 3/2/2024

Topography and morphology

• High depth of focus

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

3
 3/2/2024

Elemental mapping
Ce

Fe Sr

In-situ imaging
• A modern SEM can be equipped with various
accessories, e.g. a hot stage

4
 3/2/2024

In-situ imaging: oxidation of steel at high

temperatures

• 800 °C, pH2O = 667 Pa

• Formation of Cr2O3

2 min 10 min 90 min

Optical Micrscopy vs SEM

OM SEM
Light source Electrons

Limit of resolution ~ 2000 Å ~ 3 nm

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

(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

5
 3/2/2024

Optical Micrscopy vs SEM

Optical Microscopy vs SEM

6
 3/2/2024

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”

Resolution

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

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

7
 3/2/2024

Abbe’s Equation
Abbe’s Equation describes resolution in perfect optical system

First Transmission Electron microscope was constructed in 1930 by

replacing illumination source with electrons and condenser lens with
electromagnetic coils in light microscopes

8
 3/2/2024

Interactions of Electrons with Samples

Elastic Scattering

• 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

• Secondary electrons generated due to ionisation of specimen atoms (50

eV energy used for imaging)

• Emission of characteristics x-rays, Auger Electron and

Cathodoluminescence

Interactions of Electrons with Samples

9
 3/2/2024

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

Secondary Electrons
• Emission of loosely bound electron from the sample surface upon
interaction of energetic electrons (ionisation).

• 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.

• SE prevented from reaching detector will generate shadows or be darker

in contrast than those regions that have unobstructed electron path to the
detector.

• Low voltage incident electrons will generate secondary electrons from

the very surface region, which will generate detailed structure information
on the sample surface.

10
 3/2/2024

Secondary Electrons
Effect of surface topography and position of detector on the secondary
electron detection

The Edge Effect

More secondary electrons leave

the sample at edges leading to
increased brightness

Secondary Electrons
Effect of Accelerating voltage

11
 3/2/2024

Secondary Electrons
Effect of Accelerating voltage

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

12
 3/2/2024

Secondary Electrons
Intensity of Secondary Electrons decreases as the distance
increases from incident beam

Back Scattered Electrons

• Another way of imaging in SEM is use of BSEs

• 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.

13
 3/2/2024

Back Scattered Electrons

Comparison of Secondary electron signal and backscattering electron signal

Detecting Secondary Electrons

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

14
 3/2/2024

Detecting Secondary Electrons

Everhart-Thornley Detector

Detecting Backscattered Electrons

Old Method
• Signal received on ETD detector is not only due to secondary
electrons

• Some BSE are also entering the detector

• 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.

15
 3/2/2024

Detecting Backscattered Electrons

Robinson Type Scintillator Detector
• Specially designed to increase solid angle of collection

• Can be used with rapid scan rates

• Bulky and may restrict the working distance of the microscope

Detecting Backscattered Electrons

Solid State Detector
• 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.

16
 3/2/2024

SEM Optics
SEM purpose is to produce a fine beam of electrons incident on the specimen

Ray Diagram of two Lens SEM

SEM Optics
Condenser Lens

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

The diameter of the intermediate image (d1) 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.

17
 3/2/2024

SEM Optics

The rays entry is restricted by an aperture of diameter A, not all of the

electron beam which passes through the condenser lens can enter the
objective lens.

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.

SEM Optics

Spherical Aberration

18
 3/2/2024

Electromagnetic Lens

An electromagnetic lens are comprised of

windings of wire through which electric field is
applied. This creates strong magnetic field
through which negatively-charged electrons
must pass.

Condenser Lens
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
control initial spot size and is referred to as the spot size control.

The diameter of initial

convergence affects
the final diameter of the
spot on the specimen

19
 3/2/2024

Aperture
The objective aperture arm fits above the objective lens in the SEM.

The aperture stops the

electrons that are off-
axis from progressing
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
The objective aperture arm fits above the objective lens in the SEM.

The distance h over which the specimen will remain in

focus, the depth of field, is given by
0.1
ℎ= mm
𝑀∝

The convergence angle α of the beam is given by

𝐴
∝=
2𝑊𝐷

0.2 𝑊𝐷
𝐷𝑒𝑝𝑡ℎ 𝑜𝑓 𝐹𝑖𝑒𝑙𝑑 = mm
𝐴𝑀

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.

20
 3/2/2024

Aperture
Decreasing the aperture size will reduce the beam angle α for the same WD,
resulting in an enhancement of the depth of field

Aperture

Effect of aperture on depth of field

21
 3/2/2024

Aperture

Effect of Working Distance on depth of field

Aperture

Effect of Working Distance on depth of field

22
 3/2/2024

Astigmatism

• The imperfection on the electromagnetic lens is called

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

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.

23
 3/2/2024

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

Objective Lens Designs

24
 3/2/2024

Scanning Coils
• Scanner coils or pair of deflector plates (small coils of wire carrying the
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
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.

• 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
positions on the specimen (e.g., locations 1, 2, 3, 4, etc. in Fig. 4.1).

• Slower scan rates allow more electrons to be collected at each point along the
line of beam scan. This produces better quality image.

Scanning Coils

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

25
 3/2/2024

Image Formation in SEM

• Signal detection
• Signal processing (amplification, filtering, and digitization of the signals
to improve signal-to-noise ratio and enhance image quality.)
• Image Reconstruction (mapping the detected signals to corresponding
pixels on the screen, where each pixel represents a specific point on the
specimen surface).
• Display on Computer Screen

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 mm2 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
100 𝜇𝑚
𝑝=
𝑀

Scanned 10 μm x 10 μm
on the specimen, then on
100 mm x 100 mm CRT
screen, the linear
magnification will be
10,000x.

26
 3/2/2024

Image Formation in SEM

• If probe larger than specimen pixel, the signal from adjacent pixels is merged,
and the resolution degraded.

• If probe is smaller than pixel size, the signal would be weak.

• If probe size is exactly same as the diameter of the pixels, high resolution
achieves (required for optimum performance)

Image Formation in SEM

Resolution

27
 3/2/2024

Electron Guns
Requirements

• 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 are composed of three parts:

• 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.

28
 3/2/2024

Tungsten Electron Guns

(0.1-30 kV)

Tungsten Electron Guns

Electron Emission depends on filament current

The highest electron

emission is obtained by least
amount of current called
saturation current.
Electrons are emitted from
the tip of the filament and
focused in tight bundle by
the negative accelerating
voltage.

At false peak, life of filament

Advantage increases but beam stability
Low cost, suitable for low decreases
magnification imaging and for Life influenced by vacuum
microanalysis status and cleanliness of gun

29
 3/2/2024

Lanthanum Hexaboride Electron Guns

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

• 5 to 10x greater brightness and longer life time compared with conventional
tungsten guns

• LaB6 single crystal 100–200 μm in diameter and 0.5 mm long and is mounted on
graphite which act as the resistive heater to elevate the temperature of the
crystal.

Advantage Disadvantage
-Smaller emission Readily
area reduces spot oxidised at
size. high
-Smaller energy temperature.
spread resulting in
high resolution and To increase life
smaller chromatic time high
aberration vacuum (10-8
-Can be replaced Torr) required
easily in conventional
SEM

Field Emission Guns

• In the FEG, a single crystal tungsten wire with very sharp tip, generally prepared
by electrolytic etching, is used as the electron source.

• V1 is the of few kilovolts provided to emit electrons and Vo is used for

accelerating electrons

• Extracting electrons from a material by applying a very large electric field. By

drawing tungsten wire to a very fine point (<100 nm , application of a potential of
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).

• FEG offer higher brightness, longer life, high resolution.

30
 3/2/2024

Types of Field Emission Guns

• Cold Field Emission
Operates at room temperature, high brightness due to small diameter of electron
beam and emission area

• Thermal Field Emission

Operates at elevated temperature, flashing (2000 K for few seconds), high
temperature cleans the gas adsorbed on the tip, stable beam even if vacuum
degrades

• Schottky Emitters
To get emission from the source it is
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
• Ultrahigh vacuum is must for SEM (10-6 Torr or better)

• UHV increases electron mean free path and decreases scattering

• Contamination of guns and other components can be prevented.

• 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

31
 3/2/2024

Vacuum Systems

Vacuum beter than 5 x 10-5 Torr

Longer pump down times

Specimen preparation

• Any conducting or non-conducting sample

can be imaged.

• Nanoparticles, carbon nanotubes,

nanowires, nanostructured materials, etc.
can be observed by loading them on carbon
tape.

• Conducting sample need no or little sample

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

32
 3/2/2024

Sputtering
• A technique used to deposit thin films of a material onto a surface ( “substrate").
• First a gaseous plasma is created and ions are accelerated from this plasma into
some source material ("target").
• The source material is eroded by the arriving ions via energy transfer and is ejected
in the form of neutral particles - either individual atoms, clusters of atoms or
molecules.
• As these neutral particles are ejected they will travel in a straight line unless they
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
ejected particles it will be coated by a thin film of the source material.

Selective SEM images

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

SEM image of Mosquito Head

33
 3/2/2024

Selective SEM images

SEM of nitrogen pearlite surrounded by SEM of granular nitrogen pearlite

proeutectoid ferrite (etching with HF)

Selective SEM images

SEM of Stress corrosion cracking in 300 Pitting corrosion in 300 series stainless
series steel steel backscattered SEM image

34
 3/2/2024

Selective SEM images

SEM of Ductile fracture in 300 SS Cleavage fracture

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

35
 3/2/2024

Selective SEM images

Selective SEM images

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

36