PH 516 Materials Characterization

Electron microscopy in the study of materials

Lesson 4 - Scanning Electron Microscopy

(Working principle and basic design)

Professor BSB Karunaratne

• A scanning electron microscope (SEM) scans a focused

electron beam over a surface to create an image.

• The electrons in the beam interact with the sample,

producing various signals that can be used to obtain
information about the surface topography and composition.

• As a powerful technique, SEM has been extensively used for

imaging materials, especially at micro and nanoscales. 1
 Scanning Electron Microscope (SEM)
• Unlike in the TEM, the SEM produces
images by scanning the electron
beam across the surface of the
sample.

• The image is built up point by point

in a way similar to that in a TV.

• However, in a TV- A light beam is

used.

• In SEM- An electron beam is used for

high resolution required for resolving
atomic scale structures.
2
Scanning Electron Microscope

Schematic of a Scanning Electron Microscope 3

Electron Beam and Specimen Interactions

(1-50 keV)

Electron Beam Induced Current (EBIC) 4

1. A fine (7-10 nm) high energy beam of The image formation
electrons(typically 20 kV) is focused to a point on in the SEM.
the specimen.
2. This causes the emission of Secondary Electrons
(SE), Back Scattered Electrons BSE), etc.
3. The emitted electrons (for example consider
Secondary electrons) are collected and amplified
to give an electrical current (i). Display CRT
4. This current (i) is used to modulate the intensity of
the beam of electrons in the display CRT ( I+i) to
produce one point of the image. (I is the current
through the CRT filament to produce electron
beam in the CRT).
5. To built up the complete image of the sample the i
electron beam in the SEM and the electron beam I
in the display CRT are scanned synchronously by
a scan generator. 5
The image formation in the SEM • As discussed, the SEM image is formed by a fine
beam of electrons focused to a very small area of
the specimen and the beam is swept across the
surface of the sample in a series of fixed rows, until
a complete two dimensional pattern is formed.
• As shown below, the beam sweeps horizontally
left-to-right at a steady rate, then blanks and
rapidly moves back to the left, where it turns back
on and sweeps out the next line. During this time,
the vertical position is also steadily increasing
(downward), but much more slowly.
• To built up the image the
electron beam in the display CRT
is also scanned synchronously
with the SEM electron beam by
the scan generator. Scanning process
6
 Scanning process and Image Formation
1 µm
• The synchronous scanned process is performed as follows: a b
c d
• From a to b on the specimen surface and then simultaneously,
from A to B on the display and so on (from c to d on the specimen
and then C to D on the display) to complete all the scan lines.

• The raster is normally a square, and has scan lines up to 1000. Specimen raster
Changing the specimen raster size one can change the magnification (Area scanned over
of the image. the specimen)

• As the beam strikes specimen, electrons are emitted from the 10 cm

specimen and those are collected to form an image. If the A B
collected electrons are secondary electrons the image is C D
therefore called a secondary electron image. If the collected
electrons are BSE the image is therefore called a BSE image.

Question 1: How many scan lines are on the screen of a normal TV set?

Question 2: Comparing the specimen raster and the display raster

shown above, find the magnification of the image.
Display raster7
 Specimen Raster1 µm
a a

b b
C c
d d
e e
f f
g g
Display Raster10 cm
A A
B B
C C
D D
E E
F F
G G
8
Answer:
Magnification = Display raster/Specimen raster
= 10 cm/ 1 µm
= 10 x10-2 / 1 x 10-6
= 10 4
= 10000
Note that the display raster dimensions are kept constant. We change the specimen
raster (Area scanned over the specimen) by adjusting the scanned amplitude, to
obtain required magnification.

Question: What are the raster dimensions scanned over the specimen to obtain
a magnification of 100x and 10-6 x of the image?
SEM of a Female dengue
Colour encoded SEM of the
mosquito head (Aedes
Female dengue mosquito head.
aegypti). Yellow fever and
dengue fever carrier.

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Sample preparation
• SEM samples have to be small enough to fit on the specimen stage, and may need special
preparation to increase their electrical conductivity and to stabilize them, so that they can
withstand the high vacuum conditions and the high energy beam of electrons.
• Samples are generally mounted rigidly on a specimen holder or stub using a conductive
adhesive. Many SEMs have chambers that can tilt the specimen to 45° and provide
continuous 360° rotation.
• As mentioned in the TEM specimen preparation, nonconductive specimens collect
charge when scanned by the electron beam, and this causes scanning faults and other
image artifacts.
• For conventional imaging in the SEM, specimens must be electrically conductive, at least
at the surface, and electrically grounded to prevent the accumulation of electrostatic
charge.
• Metal objects require little special preparation for SEM except for cleaning and
conductively mounting to a specimen stub. Non-conducting materials are usually coated
with an ultrathin coating of electrically conducting material ( e.g. gold), deposited on the
sample either by low-vacuum sputter coating or by high-vacuum evaporation.
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Sample preparation – Continued……

Specimen mounting stubs

Sputter coater for gold coating .

SEM with opened sample chamber 12

 Depth of focus (DOF)
• The depth of focus (DOF) or the focal
depth is the range of distances for which
the specimen (object) is imaged with an
acceptable sharpness on the image
plane. DOF is larger as the opening
(aperture) angle of the incident probe is
smaller.
• However, DOF is smaller as the
magnification of the image is higher.

• The opening angle of the incident electron probe of the SEM is about 100 times smaller
than that of the optical microscope. Figure schematically shows the change in DOF when
the diameter of the objective lens aperture is changed.

Question: Out of these two microscopes (SEM and Optical), which has a larger
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depth of focus (DOF)?
 Depth of Focus (DOF)- Examples
Answer: Since the incident electron probe of
the SEM is about 100 times smaller than that of Optical SEM
the optical microscope the DOF of the SEM is
about 100 times larger than that of the optical
microscope.

The DOF is the distance between the two

extreme axial points appeared to be in
focus. Compare the images. We can see that
the DOF is larger for he SEM images.

• The higher magnification, lower the

depth of focus.
• The aperture diameter and the electron
column in SEM play important roles in
relation to DOF.
• SEM images show the characteristic
depth of field.
Comparison- Optical microscopy vs SEM
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Secondary Electrons (SE)
or Emissive electrons
Primary

Inelastic interactions

SE1 is used to form a secondary electron image, which

possesses information on the specimen shape (angle of the
specimen surface against the incident electron beam)

• SEs are produced by inelastic interactions of incident electrons with valence

electrons of atoms in the specimen.
• This causes the ejection of the loosely bound electrons from the atoms.
• These ejected electrons with energy less than 50 eV are termed secondary
electrons or emissive electrons.
• Due to their low energy, only SE that are very near the surface (<10nm) can come
15
out of the surface.
Backscattered Electrons (BSE) or Reflected electrons
• BSE are produced by elastic
interactions of incident
Primary electrons with nuclei of atoms in
the specimen and they have
high energy close to the
incident energies.

• The angle of scattering can

range from 0-180 degrees

• Sometimes the angle is such

that the electron comes back out
of the sample. These are
backscattered electrons.
• Similar to a comet interaction
with a planet. 16
Energy spectrum of the emitted electrons from a specimen
surface for a primary electron beam of 20 keV.
• A large peak at the left is due
to the secondary electrons,
extending to about 50 eV.
• The electrons with more than
50 eV are backscattered
electrons (reflected electrons)
existing over a wide energy
range.
• Small peaks seen in the range
of backscattered electrons are
attributed to the Auger
electrons.

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 Specimen Interaction Volume
Interaction volumes is the depth range probed by the various types of scattered electrons
and x-rays, where imaging resolution is dependent on the volume generated by the
emission type.
• Secondary electrons originate from
within a few nm from the surface. They
are therefore very sensitive to surface
structure, and provide topographic
information.
• Backscattered electrons originate from
much deeper within the sample (a few
m below the surface), and interact
much more strongly with the sample.
They therefore provide compositional
information as well as topographic
information, but give lower resolution
images. 18
 Secondary electrons (SE) Detector System

Both SE and BS electrons can be detected, but the geometric collection

efficiency for BS electrons is low, about 1-10%, while for SE electrons it is
high, often 50% or more.
19
• The detection of BSEs is often BSE Detector
carried out by solid state (or
semiconductor) detectors.
These consist of a doped
semiconductor material
(typically silicon) and are placed
directly above the sample and
below the objective lens.

• The principle of semiconductor detectors is based on the

generation of electron-hole pairs in a semiconductor by the
incident BSE electrons.

• To form an electron-hole pair in silicon, an energy of 3.6 eV is required and the

number of electron-hole pairs that are generated is proportional to the energy of
the incident electrons. Moreover, semiconductor detectors are only sensitive to
electrons with high energy, which is the reason why they are only used for the
detection of backscattered electrons. 20
 Contrast Mechanisms in SEM
• In order to obtain an image in the SEM, we must have some variation in the
signal strength from different parts of the specimen. This is called image
contrast and is always related to some properties of the specimen.

• Understanding the concept of contrast and its meaning is of great importance in

scanning electron microscopy.

• Various contrast mechanisms obtainable in SEM. However the common types

include topographic contrast and compositional/elemental contrast which
apply for virtually all specimens and provide the foundation of SEM image
formation.

• Additionally, some special contrast mechanisms, such as electric field contrast,

magnetic contrast, and crystallographic contrast, exist for certain types of
materials and are related closely to their special properties. We shall now
discuss the two main contest mechanisms. 21
Topographical Contrast
• Number of SEs entering the detector
Detector is sensitive to the roughness of the
surface of the sample.

Dark Bright • This is called “topographic contrast”.

• Topographic tilt contrast occurs when surface

features in a homogeneous material are larger
than the excitation volume of the primary beam
in the specimen.

Growth • The yield of secondary electrons is at a minimum

-steps when the surface of the specimen is perpendicular
in to the electron beam. The SE yield, δ, and the BSE
BaTiO3 coefficient, η, dependent on the surface inclination
2 m angle. 22
 Secondary emission images of Fracture surface

Undulation (or rough) surfaces show greater contrast

(topographic).
Polished (Smooth or flatter) surfaces show a dull
appearance in SE mode due to low contrast.

SEM, SE micrographs of (a) the polished Inter-granular Fracture surfaces Trans-granular cleavage fracture
surface- dull appearance), (b) and fracture (Greater topographic contrast) (Lesser topographic contrast)
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surface of a ceramic sample.
Backscattered Electrons (BSE)
Yield of BSEs is sensitive to the topography of the specimen surface,
as well as the atomic number, Z of the specimen. Therefore, to detect
compositional contrast or atomic number contras, one has to
remove the topography of the sample by polishing it.
η

An alloy-Al and Cu Z

Question: Identify Al and Cu Sensitivity of BSE with atomic number, Z

24
Answer:

An alloy-Al (Z=13) and Cu (Z=29)

BSE images show characteristics of atomic number contrast, i.e., high average
Z appear brighter than those of low average Z.
Copper atoms (higher atomic number) scatter more electrons back towards the
detector than the lighter aluminum. Thus, Cu shows light (white) and Al shows
dark (black) contrast. 25
Examples: Secondary Electrons (SE) micrographs of SEM

Copper oxide crystals Scales in hair

SEM of a Polycrystalline material 26

Surface of a kidney stone
More Examples of SE - SEM micrographs

YBa2Cu3O7 superconductor

Raw powders used in the fabrication of materials

for various applications (cathodes, solar cells, Micrographs showing dislocation
structural, etc.) pile up at a grin boundary 27
More Examples of SE - SEM micrographs Composite materials
Study of creep Study of fatigue
cavitation in alloys in alloys

Striation (fatigue)
SiC fibres in glass ceramics –
Longitudinal and Transverse
directions respectively

Creep cavities at grain boundaries

(a) steady-state growth of cavities Fracture surface
Incremental growth of a fatigue crack 28
(b) interlinkage of cavities
More Examples of SE SEM micrographs

Scanning electron micrograph

reveals zinc powder after ultrasonic
irradiation. The neck formation
from localized melting or plastic
deformation was caused by high-
velocity collisions of the zinc
The textured surface of the silicon solar cell is made using
particles.
micromachining technology. in order to obtain the lowest possible
reflectance and a maximum surface area.

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More Examples of SE - SEM micrographs

Spray-painted lithium-ion re-chargeable battery

developed at Rice University shows its five-layer
Bone Fracture Study
structure.(Anode-Lithium titanate; Cathode-LiCoO2 30
More Examples of SE SEM micrographs- Bio-Materials

Comparison: Optical and SEM

Micrographs of e. coli

SEM of Dengue virus infected

Cholera bacteria-SEM Hookworm -SEM mosquito cell culture. 31
More Examples of SE SEM micrographs

SEM image of a butterfly wing scale (x 11,000). Microscopic

ridges on these scales can give the insect it's colour by
reflecting the diffracted light in a certain way. The colours are (SEM) image showing the smaller units making up the
produced because the scales on the butterfly's wing behave as compound eye of a blowfly.
diffraction gratings. Spacing is about 700 nm and comparable
with the wavelength of light. 32
More Examples of SE SEM micrographs Nano Structured materials

Comparison :TEM of nano barium

SEM micrographs of β-SiAlON SEM of nano barium titanate powder titanate powder
nanostructure whiskers

SEM-nano rod in the composite Comparison :TEM of nano rod

SEM images of Ag nanoprisms
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 Back-Scattered Electron Images- Examples

In silicate rocks, for example, quartz(SiO2) and feldspars (KAlSi3O8 – NaAlSi3O8 –

CaAl2Si2O8) will appear dark or nearly black, Fe-Mg silicates will be brighter, and Fe-Ti brightest.
BSE images can also be converted to false colour, which often helps the human eye distinguish
subtle variations.
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 Back-Scattered Electron Images- Examples

. Lead-tin solder. Niobium-rich intermetallic phase

dispersed in an alumina matrix.
Z (Pb) = 82, and Z(Sn) =50
Z (Nb) = 41, Z (Al) = 13 and Z(O) = 8
Alumina-Al2O3

Questions: Identify Lead and Alumina in the above micrographs.

35
 Back-Scattered Electron Images- Examples

The back scattered electron micrograph of 10 wt. % Fe containing Yb doped

sialon sample.
-sialon grains
SiAlON

- sialon grains
Yb-SiAlON

10 wt. % Fe

Questions: Identify -sialon grains, - sialon grains and Fe-silicide inclusions.

36
Applications of BSE images

The distribution and the chemical composition of

Suspended Particulate Matter (SPM)I water
37
Comparison of SE and BSE images-
Question: Identify the SE and BSE images. One of the two images below is SE
and the other is BSE image. Differentiate them with explanation. Samples are iron
oxide particles.

38
 X-ray microanalysis in the SEM
• We know that characteristic X-rays
produced when the electron beam hit the X-rays can be analyzed in two ways
specimen and can be used for analytical
purposes in the SEM.
Energy dispersive (ED) Wavelength dispersive (WD)
• We have already studied this under TEM.
However, we discuss some important
points concerned with SEM.
A solid state detector A crystal spectrometer
Resolution about 100 eV. Geometrical arrangement
ED X-ray is somewhat complicated.
spectrometer
However, the resolution is
ED is the popular X-ray good. About 10 eV.
analytical technique and
available in many electron
microscopes (TEM & SEM)
and is quite easy to use.
(EDX, EDS, EDAX, etc.) 39
 X-ray microanalysis

YBa2Cu3O7-δ

40
X-ray microanalysis

Spot analysis

Copper-29 Silver-47 Bismuth-83

41
 X-ray microanalysis

Sialon simple

Iron silicide

BES micrograph

Spot analysis of iron silicide inclusions in sialon simple

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X-ray microanalysis

Example image shows

EDS spectrum of
phosphorous-rich granules
in a plant EDS spectrum of the mineral
crust of Rimicaris exoculata
(Deep Sea Shrimp)
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X-ray Mapping
• Production of images showing elemental distributions on a fine scale is an
important contribution of electron microscopy to scientific investigations. X-ray
maps are formed by collecting characteristic X rays from elements in the specimen
as a focused electron beam is scanned in a raster across the specimen.

• Computer control of the electron beam and computer storage of digital images
dramatically changed X-ray mapping to the point that digital methods are standard
in all commercial systems.

• X-ray mapping provides images of elemental distributions in a sample.

• An image is generated by converting the number of X-ray photons of specified

energy detected at each point into a brightness value for a pixel on the screen or
digital image. 44
X-ray Mapping -Continued

SEM imaging, EDS analysis of single-walled carbon nanotubes (SWCNT) and X-ray mapping

Digital elemental distribution maps can be collected simultaneously with SEM electron image acquisition thus
giving a visual representation of the chemical distribution in the sample. This can be done in SEM as well as in
TEM.
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X-ray Mapping - Continued

Backscattered electron (BSE, left) and secondary electron (SE, right) SEM images and EDX maps (Ti, Ni, and Sn
respectively) for TiNi 1.02 Sn. The elemental maps cover the same area as the BSE and SE images. 46
Special Contrast Mechanisms

Magnetic and
Electric Field
Contrasts

• SE Electron trajectories are

affected by both electric and
magnetic fields and as a result
contrast effects are observed.

• Very little effect is obtained with

BSE Magnetic Field Contrast-
Magnetic domains in
Fe-Si alloy- 5 µm
47
 Semiconductor p-n junction (Voltage contrast).

Line scans taken across a vertical junction of a diode at different reverse bias
voltages (0, 5, 10 and 15 V). Depletion region expands with increased bias.

The shape of the contrast can be treated mathematically to determine the minority carrier
properties of the semiconductor, such as diffusion length, lifetime, mobility, etc.

Question: Estimate the width of the depletion region of the above p-n junction,
for 10 V reverse bias voltage.
48
In-situ intrinsic resistivity test - Four-probe tips on a ZnO Nano Wire

(a) Nano Wire lying flat on insulating SiO2 .

(b) Shows a good fit of the Ohm’s law.

The intrinsic resistivity of the NW can be obtained from the gradient.

Mechanical characterization at the nano-scale can also be performed.

Question: Estimate the diameter of the nano wire and calculate the resistivity of
the ZnO Nano Wire. 49
EBIC / EBAC/RCI Techniques for Semiconductor Failure Analysis
• When the electron beam of the SEM strikes a semiconductor, electron-hole pairs
are generated and separated in depletion region due to the built-in electric field.

• The resulting current flow can be measured and used to develop an image.

Electron Beam Induced Current (EBIC) and Electron Beam Absorbed

Current (EBAC), Resistive Contrast Imaging (RCI). 50
EBIC showing
defects in a diode

Comparison of SE and EBIC

images as well as the resulting
mixed images

Areas with good

crystal quality will
show bright contrast,
and areas containing
defects will show dark
EBIC contrast.
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Experimental setup - Resistive Contrast Imaging (RCI)

Integrated Circuits mounted

Inside the SEM sample chamber
SEM sample chamber

52
 Integrated Circuit (IC) Failure Analysis

Production faults Metal Oxide Bridge

Logic failure analysis 65/45nm device

using RCI & nano scale probe Metal bridge 53
 Experimental setup for in situ nano-indentation in a SEM

Quantitative measurement of nano-mechanical properties such as: Hardness,

Stiffness, Modulus, Fracture onset characterisation, Crack propagation, etc. Nano
(grain to grain) properties are different to the bulk properties. 54
 In situ SEM nanoindentation

Images of the indentation imprints for a maximum load of 0.9 mN on the

following coatings: (a) TiN, (b) TiN/NbN, (c) NbN, (d) TiN/CrN, (e) CrN,
and (f) NbN/CrN.
55
Hot stage microscopy is a thermal analysis technique that combines the best
properties of thermal analysis and microscopy at very fine scale.

(a) Hot stage (b) Hot tension/compression stage integrated into an

SEM (Kammrath & Weiss Co.) (After Biallas & Maier, 2007 ; Gorkaya
et al., 2010).
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Applications in Research and Industry (Nano-materials)

Representative SEM images of asbestiform minerals

Medical applications,
Drug delivery
systems, diagnostics
applications,
Catalysis and
adsorbents, filters
etc.

Nanoporous silica material. Nanofibers- 4000x

Fiber Analysis – Using SEM for the Quality Analysis of Fibers 57
 Applications in fabric Industry

SEM analysis of fabrics before and

after the deposition of mud:
(a) white cotton;
(b) patterned cotton;
(c) black polyester;
(d) black nylon/lycra

Electrospun nylon
nanofibres, coated
with antibacterial
silver nanoparticles

58
Before After
Applications in Cement
and Paper Industry

SEM images of a
strip of paper
being stretched
using the tensile
testing machine.

59
Applications in Criminal and other forensic investigations
• analysis of gunshot residue
• jewellery examination
• bullet marking comparison
• handwriting and print analysis
• examination of banknote authenticity.
• paint particle and fibre analysis
• filament bulb analysis in traffic incidents

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What can we study in a SEM?
• Topography and morphology
• Chemistry
• Crystallography
• Orientation of grains
• In-situ experiments:
• Reactions with atmosphere
• Effects of temperature
• Effects of stress (Mechanical Deformation)
• Effects of temperature

61
 Environmental Scanning Electron Microscope(ESEM)

• The environmental scanning

electron microscope (ESEM) is
a scanning electron
microscope, that allows for
the option of imaging of
specimens that are wet,
uncoated, or both including
biological samples, by
allowing for a gaseous
environment in the specimen
chamber.
Schematic of an ESEM.

• This is achieved in the ESEM by using a specially design differential pumping system.
This, allows the transfer of the electron beam from the high vacuum in the gun area
to the gaseous environment area in its specimen chamber. This makes it possible to
image specimens in their natural state. 62
 Environmental Scanning Electron Microscope(ESEM)
For Wet, uncoated, or live specimens
• The specimen chamber sustaining somewhat high-
pressure gaseous environment is separated from the high
vacuum of the electron optics column with at least two
small orifices customarily referred to as pressure-limiting
apertures (PLA).
• The gas leaking through the first aperture (PLA1) is quickly
removed from the system with a pump that maintains a
much lower pressure in the downstream region (i.e.
immediately above the aperture). This is called differential
pumping.
• Some gas escapes further from the low pressure region
(stage 1) through a second pressure limiting aperture
(PLA2) into the vacuum region of the column above, which
constitutes a second stage differential pumping (stage 2).

63
 ESEM micrographs of live specimens

Observation of a live
ESEM micrograph showing part Threadworm mite in an ~ESEM!.
of the eye of a live fruit fly.
64
 Scanning Transmission Electron Microscope (STEM)
A scanning transmission electron microscope is another type of mode
available for electron microscopy. We shall discuss it briefly.
• A scanning transmission electron microscope (STEM) is a type of
transmission electron microscope.
• As with a conventional transmission electron microscope (CTEM), images
are formed by electrons passing through a sufficiently thin specimen.
• In the STEM mode microscope lenses are adjusted to create a focused
convergent electron beam or spot on the sample surface. This focused
probe is then scanned across the sample and various signals are collected
point-by-point to form an image in a similar manner to SEM. (combines the
principles of TEM and SEM)
• The transmitted electrons at a high scattering angle form high-resolution
images, revealing the materials' atomic number (Z-) and chemical
composition.
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SEM has a variety of applications in a number of scientific and industry-related
fields.
(1) SEM is an essential tool for materials science and engineering. The development
of nanotechnology is heavily dependent on the application of SEM.
(2) In life sciences and research, SEM has become an integral technology. Recent
development of biocompatible materials, tissue engineering research, microbiology
and many have close relationship with SEM imaging technique.
(3) SEM, is an ideal technique in semiconductor industry by offering analytical
capabilities with high levels of precision.
(4) Equipped with an Energy Dispersion X-ray analyzer (EDX), SEM can reveal
spatial variation in chemical composition, provide chemical analysis and identify
crystalline structure of samples.
(5) SEM sample preparation is easier compared to TEM samples, and big samples
can be investigated.
(6) However, electron microscopes are expensive to buy and maintain and a
significant amount of training is required in order to operate an electron microscope
successfully.
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The difference between SEM and TEM
• The main difference between SEM and TEM is that SEM creates an
image by detecting reflected or knocked-off electrons, while TEM uses
transmitted electrons (electrons that are passing through the sample) to
create an image.
• The resolution of modern SEMs is of the order of 2 nm. This compares with a
resolution of about 1 m for a conventional optical microscope. The transmission
electron microscope (TEM), in which electrons pass through a very thin sample,
has a higher resolution than the SEM (~ 0.1 nm). Individual atoms can be imaged
in the TEM but not the SEM.

• The magnifications that TEMs offer are also much higher compared to SEMs. TEM
users can magnify their samples by more than 50 million times, while for the SEM,
this is limited to 1–2 million times.

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Thank You
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