MM 593 Advanced

Characterization Techniques
Shanza Rehan
Lecture # Scanning Electron Microscopy
Chapter 4, Materials Characterization by Yang Leng, Wiley-VCH
SEM Data Representation
Chemical Composition (Spot Analysis) (Line Analysis)
SEM Data Representation
Chemical Composition

(Line Scan)
(EDS
Mapping)

(X-ray
maps)
Fields of Applications Types of Samples Examined
▪ Materials identification ▪ Metals
▪ Alloys
▪ Forensic science
▪ Polymers
▪ Metallurgical and ▪ Coatings
electronic materials
failure analysis ▪ Fractured/rough surfaces
▪ Ceramics
▪ Corrosion science ▪ Rocks, Minerals
▪ Rock mineralogy ▪ Sand
▪ Polymer science ▪ Corrosion products
▪ Catalysis ▪ Catalysts, Membranes, Foils
▪ Biological Tissues
▪ Semiconductor design
▪ Cells
▪ Desalination ▪ Insects
▪ Life science ▪ Leaves
Case Study: Failure of a Weld Joint
Component
▪ Pipe and elbow joint
Material
▪ Weld between SS304 and CS
Observation
▪ Separation, weld cracks, leakage
Analysis
▪ High Hardness (HRC 60) due to C segregation in weld
zone
Mode of Failure
▪ Cracking at brittle region
Cause of Failure
▪ Improper welding procedure
Recommendations
▪ Follow proper welding procedure: low heat input,
minimum penetration, avoid H contamination. Replace
CS with SS material.
Case Study: Failure of a Cracked Gear
Component
▪ Forged helical gear in extruder assembly used
at 45 °C and 222 rpm
Observation
▪ Broken gear teeth, no fragments, sound
Analysis
▪ Fatigue striations
Mode of Failure
▪ Quasi-cleavage crack propagation
Cause of Failure
▪ Repeated bending stress leading to fatigue due
to misalignment
Recommendations
▪ Proper alignment of gear assembly
Analyzed Samples
▪ Form: Solid, bulk, thin, nanostructured, powder, pellet, organic, inorganic
▪ State: Dry, wet
▪ Sample Size: 1 mm to 15 cm (Typically 10 to 20 mm)
▪ Conductive, Non-conductive
▪ As-received or prepared (sectioned, ground, polished, etched, coated, etc)
condition.
▪ Spatial Resolution: up to 1 nm
▪ Sampling Depth: 1-5 mm (depends on sample density and electron beam
accelerating voltage)
▪ Sample Area Analyzed: <1 mm to 100 mm (Depends on electron probe size)
▪ Detection limit of elements: 0.2 wt% (depends on relative elemental content
and atomic weight)
COMPONENTS OF THE SEM
Electron column: Cylindrical body
1. Electron Gun
▪ Thermionic Emission Electron Gun
(i) Tungsten Filament Gun
(ii) Lanthanum Hexaboride (LaB6) Gun
▪ Field Emission Electron Gun
▪ Advanced SEM systems use a field emission
gun because of its high beam brightness
▪ The acceleration voltage for generating an
electron beam is in the range 1–40 kV, which
is about 1 order of magnitude less than that for
a TEM.
▪

Required Characteristics of Electron Source

▪ For high performance, high spatial resolution, rapid data acquisition, and reliable
operation, an electron microscope requires an electron source with the following ideal
properties:
▪ Small source size, low electron emission energy spread, high brightness (beam current per solid
angle), low short-term noise and long-term stability.
COMPONENTS OF THE SEM
2. Electromagnetic Lenses
▪ Lenses in SEM are for electron probe formation, not for
image formation directly as in a TEM.
▪ Condenser Lenses
▪ reduce the crossover diameter of the electron beam;
▪ Objective lens
▪ focuses the electron beam as a probe with a diameter on
the nanometer scale
▪ demagnifies the cross section of the electron beam; (In
TEM objective lens magnifies the electron beam)
3. Scan Coils
▪ The electron beam is scanned from left to right pixel by
pixel across the surface of the specimen (raster scanning)
▪ This scan across the specimen surface is accomplished
through 2 pairs of electromagnetic deflection coils
located within objective lens assembly in the electron
column.
COMPONENTS OF THE SEM
4. Specimen Chamber
▪ It is kept under a vacuum during SEM operation, and has
▪ specimen stage, specimen holder, CCD camera and several detectors for
imaging as well as microchemical analysis.
CCD Camera
▪ Modern SEMs are fitted with an Infra-red CCD camera inside the
specimen chamber. The picture from this camera is displayed on the
computer monitor.
SEM Detectors
▪ Detector is a device that is used to collect and convert the radiation of
interest that leaves the specimen into an electrical signal
▪ The electron signals from each pixel of the raster are collected by a
detector in order to generate a corresponding point-to-point image on a
display screen
▪ Located inside chamber close to the specimen and faces the sample surface at an
angle
▪ Everhart-Thornley detector (ETD) is the most commonly used detector in the
SEMs➔ Capable of detecting
both secondary and backscattered electrons emanating from the specimen.
▪ Permanent, mountable, retractable
COMPONENTS OF THE SEM: SEM Detectors
Everhart–Thornley (E–T) detector
▪ ETD is built in the form of a tube with its front end covered by Faraday cage (F) which protects the beam from unwanted
deflection and distortion by this large (+10-12kV) potential in the specimen chamber. The scintillator is surrounded by a
Faraday cage which is insulated from the scintillator bias.
▪ The electrons pass through the cage and strike the Scintillator and are converted into light (e.g. Cathodoluminescence)
▪ The light then passes through total internal reflection in plastic or glass pipe (light guide: LG) to reach a photomultiplier
tube which converts the light into an electric signal that is amplified to levels suitable for the formation of an image
which is converted into a digital signal and viewed on a computer monitor.
▪ The pulse which is translated into image pixel, carries information about the energy of the original incident radiation on
the scintillator. Thus both intensity and energy of the radiation can be measured.
Signal Collection Efficiency of Detectors
The strength of the signal depends on the number of electrons reaching the detector
▪ Take-off Angle: The position of the detector is described by the take-off angle (ψ -psi) which is defined as the angle
from the surface of the specimen to the line connecting centre of the detector face. Usually around 30°.
▪ Size: The size of the detector is described by the solid angle (Ω–omega) which is the ratio of the area of the face of the
detector to the square of the radial distance to the beam impact point, Ω= A/r2.The unit of measure of solid angle is the
steradian(sr).

PM = Photomultiplier, B =
Backscattered electrons, LG = Light
Guide, SE = Secondary Electrons, F =
Faraday’s Cage, S = Scintillator
COMPONENTS OF THE SEM: Probe size and current
▪ The resolution of SEM imaging is determined by the cross-sectional diameter of the
scanning probe.
▪ Thus, the size of the probe limits the size of features on the specimen surface to be resolved.
▪ To obtain high resolution, we should know how to minimize probe size. The probe
diameter is approximately expressed as dp
▪ ip is the probe current, β is the beam brightness, which is
controlled by the electron source, and αf is the convergence
angle of the probe, which is determined by the final aperture
diameter and the distance between aperture and specimen
surfaces (called the working distance) The brightness of
electron illumination or beam brightness (β) depends on the
type of electron gun used.
▪ a field emission gun is 1000× brighter than a tungsten thermionic gun
and 100× brighter than a LaB6 thermionic gun.
▪ the brightness is proportional to the acceleration voltage (Vo)
of the gun
▪ β ∝ e Vo where e is the charge of an electron.
COMPONENTS OF THE SEM: Probe size and current
▪ To obtain a minimal probe size, we should increase
the brightness as well as the convergence angle, On
the other hand, a large αf likely introduces other
optical problems (spherical aberration). Thus, αf
must be optimized, not simply increased.

▪ The reduction of probe size alone is not sufficient to

obtain a high-resolution image in an SEM.
▪ For obtaining a high-resolution image, there must
be sufficient signal electrons generated by the probe
for each pixel of an image in order to distinguish
the signals from the background noise of electrons.
▪ Background noise in an SEM system is generated by
fluctuation of the electron beam current and signal
amplification in the detector, and cannot be totally
eliminated
BEAM-SPECIMEN INTERACTION-Elastic Scattering Elastic Scattering
▪ Dependence on Z
▪ The probability of elastic scattering is greater in specimens with large atoms electrons are deflected into a new
(roughly proportional to Z2) due to their stronger positive charge direction by the atomic nuclei without
losing kinetic energy
▪ Dependence on Beam Energy
▪ Tendency of electron beam to scatter elastically decreases as its energy is increased
(proportional to 1/E2) since the beam can now more effectively overcome the
positive charge of atomic nuclei of the specimen.
▪ Extent of backscattering in a specimen is expressed in the form of
backscatter coefficient (η) which is the fraction of incident electrons that
leave the specimen surface:
η = backscatter coefficient η = η(BSE) / η(B)
electron trajectory changes, but its kinetic
▪ η(BSE)= number of backscattered electrons energy and velocity remain essentially
▪ η(B)= number of incident beam electrons constant backscattering

▪ Backscatter coefficient increases with atomic number

▪ atomic number or compositional or Z contrast ➔ the phase with a high
atomic number will appear relatively brighter (due to larger number of
backscatter electrons ejecting out of this phase) while phase with a low
atomic number will appear relatively dark.
▪ Backscatter coefficient changes only slightly with a change in incident
electron beam energy of 5-30 kV
BEAM-SPECIMEN INTERACTION-Inelastic Scattering
▪ In inelastic scattering, the trajectory of the incident electron is only slightly perturbed, but energy is lost through
interactions with the orbital electrons of the atoms in the specimen.
▪ Inelastic interactions produce diverse effect including:
▪ Secondary electrons, phonon excitation (heating), cathodoluminescence(visible light fluorescence), characteristic
x-ray radiation , Plasmon production (secondary electrons), Auger electron production
▪ Dependence on distance
▪ The rate at which this energy is lost depends on the distance travelled. Greater the distance already traversed by
the beam within the material, the greater the energy loss
▪ Dependence on atomic number
▪ The electron energy is reduced approximately by 1-10 eV per nm of distance travelled within the specimen
depending on its Z
Secondary Electrons (SE)
▪ Are loosely bound outer shell electrons of the specimen, that are struck by the electrons of the incident beam in an
inelastic manner are ejected out of the specimen and are known as secondary electrons
▪ They are differentiated from backscattered electrons purely on the basis of their energy i.e. electrons emitted from
the specimen with less than 50 eV kinetic energy are classified as secondary electrons
▪ SE that are generated within a few nm of specimen surface can eject out of the specimen. SE that are generated away
from the surface cannot escape the specimen as they lack enough energy to propagate through the solid to reach the
surface and are lost within the specimen
BEAM-SPECIMEN INTERACTION
▪ Extent of secondary electron generation in a specimen is expressed in the form of
secondary electron coefficient (d) which is defined as the ratio of the number of
secondary electrons emitted from a specimen to the number of incident beam electrons
that enter the specimen, The probability of escape
of secondary electrons as
d= n(SE)/ n(B) a function of specimen
▪ d= total secondary electron coefficient depth Z is shown above
▪ n(SE)= number of secondary electrons
▪ n(B)= number of incident beam electrons

▪ d is higher at lower incident beam energy since any increase in beam energy will
produce secondary electrons at greater depths which cannot escape to the surface.
▪ There is a significant increase in secondary electron emission below 5 keV.
▪ The escape depth of SE in metals is approximately 1nm while its around 10 nm in
insulators.
▪ In metals due to the presence of large number of electrons SE generated within greater depths of
metals cannot escape the surface
▪ In insulators due to lack of electrons, inelastic scattering of generated SE is not significant thus
allowing them to reach and escape the specimen surface from greater depths.
BEAM-SPECIMEN INTERACTION
Secondary electrons
▪ Secondary electrons that are produced within the narrow escape depth of
the specimen are called SE1. These electrons make up the high
resolution image that encompasses lateral spatial resolution as well as
shallow sampling depth of the signal.
▪ Backscattered electrons can also inelastically scatter secondary electrons
which in turn can emanate from the surface if present within the escape
depth of the specimen. These secondary electrons are known as SE2. and
possess lateral and depth characteristics of the BSE signal that generates
such signal. It is a low resolution signal that carries different information
than SE1
▪ The contribution of SE1 signal in secondary electron emission is greater Sample surface
than SE2 signal in light elements. This is due to the fact that
backscattering is low in light elements due to their small atomic size.
Therefore, the main component of the total SE signal is generated by the
primary beam incident on the specimen surface.
▪ In heavy elements, SE2 signal dominates since backscattering is
prominent due to large atomic size.
▪ Generation of secondary electrons increases with an increase in the tilt
of the specimen
BEAM-SPECIMEN INTERACTION

BSE image

Comparison between: (a) a secondary electron image; and

(b) a backscattered electron image for the same area of
nickel alloy.
Topographical information is obtained from secondary
electron image while compositional information is SE image
obtained from the backscattered image.

Image formed by SEs should have a better spatial

resolution than that formed by BSEs
BEAM-SPECIMEN INTERACTION
Effect of Electron Scattering
▪ Electrons penetrate into the depth and breadth of the specimen forming a relatively large
micrometer scaled 3D volume from within all imaging and micro-chemical information is
extracted. This is called ‘Interaction Volume’
▪ The total volume of the specimen material that is affected by the incident electron beam is known as
interaction volume
▪ It is much larger compared to the size of the incident probe
Effect of Electron Scattering
▪ SEs (inelastically scattered e-) have an energy level of several eV can escape only from a depth of top 5–50 nm, even
though they are generated in the whole pear-shaped zone.
▪ BSEs (elastically scattered e-) have energy level close to that of incident electrons. Their high energy enables them to
escape from a much deeper level in the interaction zone, from depths of about 50–300 nm.
The interaction volume is influenced by:
a) the beam energy
b) the atomic number of the solid depth of electron penetration(x)
c) surface tilt and
d) Density of the solid

width of the excited volume(y)

BEAM-SPECIMEN INTERACTION
Monte Carlo Electron Trajectory Simulation
1. Influence of beam energy on the interaction volume:
▪ As the beam energy is increased, the electron beam can penetrate to greater depths.
▪ There is no significant change in the shape of the interaction volume with beam 0˚ tilt
energy
2. Influence of the atomic number of the solid in the interaction volume:
▪ In specimens of high atomic number the electrons undergo more elastic scattering
per unit distance and the average scattering angle is greater.
▪ The electron trajectory in the high atomic number materials, tends to deviate out of 45˚ tilt
the initial direction of travel more quickly.
▪ The shape of the interaction volume is greatly affected by the atomic number of the
specimen.
3. Influence of tilt on the interaction volume
▪ As the angle of tilt of the specimen surface increases the interaction volume 60˚ tilt
becomes smaller and asymmetric
Less dense denser
IMAGE FORMATION IN THE SEM
▪ An electron beam is raster scanned (operated by a beam-
deflection system incorporated within the objective lens) across
the specimen surface resulting in the generation of
▪ secondary and backscattered electrons which are used to form images
▪ X-rays are used to obtain elemental constitution of the specimen
material.
▪ The beam is positioned in a particular location remains there for
a fixed time, called dwell time, and then it is moved to the next
point
▪ The signal electrons emitted from the specimen are collected by
a detector, amplified, and used to reconstruct an image,
according to a one-to-one correlation between scanning points
on the specimen and picture points on a screen of a cathode ray
tube (CRT) or liquid crystal display.
▪ The SEM image is a 2D intensity map in the analog or digital
domain. Unlike optical or transmission electron microscopes no
true image exists in the SEM. The image is generated and
displayed electronically.
IMAGE FORMATION IN THE SEM
Magnification
▪ The magnification of an SEM is determined by the ratio of the linear size of the display screen to the linear
size of the specimen area being scanned
Magnification = CRT Scan Length / Specimen Scan Length
▪ Since the maximum length of CRT is fixed, magnification is increased by decreasing the length of
specimen scan. Magnifications of up to 1 million times can be produced in microscopes in use today.
Resolution
▪ The resolution of the SEM depends on the diameter of the electron probe. The smaller the probe size, the greater the
achievable resolution. Probe size should be comparable to the dimensions of the feature that is being imaged in order
to be able to resolve it.
▪ Contrast Formation
1. Topographic➔ SEs are the primary source
2. Compositional ➔ BSEs are the primary source
Signal to Noise Ratio
▪ Image noise means the random or undesired pixel values that is inherent in the process which produces
signal and damage the quality of the image.
▪ Signal to noise ratio (S/N) determines the quality of image. In order to detect an object against a
background of random noise, signal strength should be at least 5X the noise level
▪ i.e. sufficient signal electrons generated by the probe for each pixel of an image in order to distinguish the
signal from the background noise of electrons. The signal electrons are proportional to the amount of
incident electrons in the probe. So, the probe current must be larger than a minimum value so that
microscopic features are visible in the SEM image.
▪ Alternatively, scan rate can be reduced to improve signal to noise ratio.
INFLUENCE OF VARIOUS FACTORS ON IMAGING
Influence of Charge-up on Image Quality
▪ When a nonconductive specimen (such as ceramics, polymers, and
biological substances) is directly illuminated with an e- beam, e- collect
locally (specimen charge-up), cause many artifacts
▪ charged regions deflect the incident electron probe in an irregular
▪ charging alters SE emission, and
▪ charging causes the instability of signal electrons.
▪ Charging is higher at higher accelerating voltages, (above 5 kV)
▪ This charge-up causes some unusual phenomena such as, unexpected
brightening/darkening in images, image deformation and shift incident
beam is actually displaced by the charge on the specimen resulting in
complete degradation of the SEM image
Reducing Charge-up
1. Reducing the probe current,
2. Lowering the accelerating voltage,
3. Coating the sample with conductive metal
4. Using low vacuum mode and
5. Tilting the specimen.
INFLUENCE OF VARIOUS FACTORS ON IMAGING
Specimen Damage by Electron Beam
▪ Heat generation occurs at the irradiated point. Its value
depends 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 are easily
damaged by the electron beam because of their low heat
conductivity.
▪ To avoid this damage:
1. Use low accelerating voltage.
2. Decrease electron beam intensity.
3. Shorten exposure time, even though this reduces image
smoothness.
4. Image large scanning areas with low magnifications.
5. To control the thickness of coating metal on the specimen surface.
INFLUENCE OF VARIOUS FACTORS ON IMAGING
Electromagnetic Interference
▪ External electromagnetic interference in the vicinity of SEM
produces image distortion. Such an effect is more visible at
higher magnification. Also, the lower the accelerating voltage the
greater the interference effect observed.
▪ Causes
▪ Leakage Magnet field from distribution board
▪ High-tension line located too close to the instrument
▪ Improper grounding
▪ Electrical equipment such as cabling, transformers, etc.
▪ Remedy
▪ Improve installation conditions by removing above stated issues
▪ Install cancellation units
Floor Vibrations
▪ Low floor strength or upper floors might have floor vibrations
▪ Remedy
▪ Anti-Vibration Platform
Site selected for installation of the microscope needs to meet strict
specifications concerning vibration
OPERATIONAL VARIABLES SUMMARY TABLE
Microscopy Conditions Effects

Misaligned microscope Images lack sharpness and focus

Coated specimen Eliminates charge build-up, Better contrast, Coating grains visible at magnifications > x100,000, Not suitable for
low voltage microscopy
Uncoated specimen Specimen charging, Low contrast, Suitable for low voltage microscopy
High Accelerating Voltage High resolution, Good for bulk surfaces, Required for EDS microchemical analysis, Lacks surface details due to
(keV) high beam penetration and large interaction volume, Specimen prone to charging, Specimen prone to beam
damage, Specimen prone to contamination, Pronounced edge effects
Low Accelerating Voltage Low resolution, Good for surface morphology examination due to less beam penetration and small interaction
(keV) volume, Not adequate to measure chemistry of heavy elements, Less charge build-up, Less edge effects, Less
specimen damage
Large objective aperture Low resolution, Small depth of field, Smooth image, Suited to microchemical analysis

Small objective aperture High resolution, High depth of field, Grainy image, Not suited for microchemical analysis

Secondary electron Suitable for surface morphology examination, High resolution, Prone to specimen charging
imaging
Backscattered electron Suitable for contrast based on composition, Low resolution, Less prone to charging
imaging
Energy Dispersive X-ray Qualitative and quantitative microchemical analysis, Spot (point analysis), area analysis, line profile, 2D area
Detector (EDS) profile
STRENGTHS AND LIMITATIONS OF SEM
Strengths
▪ Wide variety of specimens can be examined
▪ Relatively easy and quick sample preparation
▪ Easy to operate equipment
▪ Quick results
▪ Micro-chemical analysis capability
▪ Samples can be dry or wet
Limitation
▪ Sample size is limited
▪ Samples are solid
▪ EDS detectors cannot detect H, N, Li, etc
▪ Poor detectability limit of elements (with EDS) compared to wet chemical
methods