Electron Microscopy

• Electron microscope is a type of microscope that uses electrons to

illuminate a specimen and create an enlarged image.
• electron microscope uses electrostatic and electromagnetic lenses
in forming the image by controlling the electron beam to focus it at
a specific plane relative to the specimen in a manner similar to how
a light microscope uses glass lenses to focus light on or through a
specimen to form an image.
• Types of Electron Microscopes:
– TEM (Transmission EM)
– SEM (Scanning EM)
– REM (Reflection EM)
– STEM (Scanning Transmission EM)
– STM (Scanning Tunneling M)
 What is SEM
• Scanning electron microscope (SEM) is an EM that designed for
direct studying of the surfaces of solid objects.
 Advantages of Using SEM over OM
Magnification Depth of Field Resolution
OM 4x – 1000x 15.5mm – 0.19mm ~ 0.2mm
SEM 10x – 3000000x 4mm – 0.4mm 1-10nm

• The SEM has a large DOF (depth of field)

• The SEM also produces images of high resolution, which
means that closely features can be examined at a high
magnification
• The combination of higher magnification, larger depth of field,
greater resolution and compositional and crystallographic
information makes the SEM one of the most heavily used
instruments in research areas and industries.
Advantages of Using SEM over OM
 Main Applications
• Topography
The surface features of an object and its texture (hardness, reflectivity… etc.)

• Morphology
The shape and size of the particles making up the object (strength, defects in
IC and chips...etc.)

• Composition
The elements and compounds that the object is composed of and the relative
amounts of them (melting point, reactivity, hardness...etc.)

• Crystallographic Information
How the grains are arranged in the object (conductivity, electrical properties,
strength...etc.)
 Characteristics of a SEM
MAGNIFICATION:
– For most SEM: 10-200,000x (or more).
– Useful Magnification: ~20,000x
RESOLUTION:
– Theoretical Limit of Resolution: 50 Å (5 nm)
– Practical Resolution: 200 Å (20 nm)

The resolving power of the SEM depends primarily on the

effective beam diameter of the probe (spot size). For
two points having a inter-point distance, d, to be
resolved, spot size must be smaller than d.
Inside SEM
Inside SEM
• The electron beam produced by
an electron gun is focused to a
point on the sample surface by
two condenser lenses.
• The second condenser lens
(sometimes also called as
objective lens) focuses the beam
to an extraordinarily small
diameter of only 10-20 nm.
• Electrons, either SE or BSE,
from the sample surface are
detected by a detector and
amplified to form images on the
screen of a CRT.
Comparison of OM,TEM and SEM
 Electron Gun
• The electron beam comes from a filament,
made of various types of materials.
• The most common is the Tungsten hairpin
gun. This filament is a loop of tungsten
which functions as the cathode.
• A voltage is applied to the loop, causing it to
heat up.
• The anode, which is positive with respect to
the filament, forms powerful attractive
forces for electrons. This causes electrons
to accelerate toward the anode.
• Some accelerate right by the anode and on
down the column, to the sample.
• Other examples of filaments are
Lanthanum Hexaboride filaments and field
emission guns.
Hairpin Electron
• The hairpinGun
shape tungsten filament
functions as a cathode
• a small voltage differential applied across
the terminals of the filament causes
heating of the wire
• The flow of current through the wire is
called filament current
• Electrons thermionically emitted from the
filament are accelerated rapidly towards
the anode

Material : Tungsten
Operation temp : 2700 K to 3000 K
Service life : 25 – 100 hours
Vacuum system : 10-5 Torr
Lanthanum Hexaboride - gun
• A thermionic electron LaB 6
consists
essentially of a heated wire or
compound from which electrons are
given enough thermal energy to
overcome the work function of the
source, combined with an electric
potential to give the newly free
electrons a direction and velocity.

Material: Lanthanum Hexaboride (LaB6)

Operation temperature : 1700 - 1850 K
Service life : 500 hours
Vacuum system : 10-6 Torr
Field• Electron
Emission Gun
source is not heated to remove electrons and for this
reason are often referred to as being "cold" sources.
• Electrons are then pulled from a very small area of the pointed
tip and proceed down the column. Often this is aided by a
second anode that lies beneath the first.
• Acting like an electrostatic lens the two anodes serve to further
coalesce and demagnify the beam.
• The lost electrons are replenished by an electron source
attached to the tungsten tip.
• A primary electron beam generated by a field emission source
offers significant advantages over those produced by by
thermionic emitters.

Material : Tungten (W)

Operation temperature : 300 K
Service life : over 1000 h
Vacuum system : 10-9 Torr
Comparison of 3 common electron sources
 Why Need a Vacuum
When a SEM is used, the electron-optical column and
sample chamber must always be at a vacuum:
1. If the column is in a gas filled environment, electrons will be
scattered by gas molecules which would lead to reduction
of the beam intensity and stability.
2. Other gas molecules, which could come from the sample or
the microscope itself, could form compounds and condense
on the sample. This would lower the contrast and obscure
detail in the image.
3. 1 all electron =source
atmosphere 760mmneed
Hg = a760
vacuum environment
torr = 1.013bar = 101.3tokPa
operate
 Vacuum Pump
There are four types of vacuum pumps that are at
least somewhat commonly employed in SEMs:
1. Roughing pump/mechanical pump
2. Diffusion pump
3. Turbo Molecular pump
4. Ion pump
SEM Detector
Electron – Sample Interaction
The interactions may be elastic or
inelastic
• The elastic interactions:
– incident electrons and nucleus
– a large-angle deflection of incident
electrons.
– little energy loss
• The inelastic interactions:
– incident electrons and orbital shell
electrons
– a small-angle deflection of incident
electrons.
– heavy energy loss
Elastic Vs Inelastic
 Elastic Vs Inelastic
• Elastic
– Back-scattered electrons
• Inelastic
– Secondary electrons
– Bremsstrahlung X-rays
– Characteristic X-rays
– Auger electrons
• Other
– Cathodoluminescence
– Specimen current
• SEMElectron – Sample
Electron - Photon Interaction

Secondary Back scattered Auger Cathodoluminescence

Secondary Electron
• Produced by inelastic interactions of high
energy electrons with valence (or
conduction) electrons of atoms in the
specimen, causing the ejection of the
electrons from the atoms. These ejected
electrons with energy less than 50eV are
termed "secondary electrons".
• Each incident electron can produce
several secondary electrons.
• Production of SE is very topography
related. Due to their low energy, only SE
that are very near the surface (<10nm)
can exit the sample and be examined
(small escape depth).
 Secondary Electron Detector

• A conventional secondary electron detector is positioned off to the side of

the specimen. A faraday cage (kept at a positive bias) draws in the low
energy secondary electrons. The electrons are then accelerated towards a
scintillator which is kept at a very high bias in order to accelerate them into
the phosphor.
 Secondary Electron Detector

A typical scintillator/PMT secondary-electron detector, often named an

Everhart-Thornley (ET) detector after its two inventors

• A PMT works by converting the incoming photons into electrons which are
then drawn to dynodes kept at a positive bias. The dynodes are made of
material with a low work function and thus give up excess electrons for
every electron that strikes them. The result “multiplies” the signal
contained in each photon produced by the scintillator.
 Backscattered electrons (BSE)
Formation
– Caused when incident electrons collide with an atom in a
specimen that is nearly normal to the path of the incident
beam.
– Incident electron is scattered backward (“reflected”).
Use
– Imaging and diffraction analysis in the SEM.
– Production varies with atomic number (Z).
– Higher Z elements appear brighter than lower Z elements.
– Differentiate parts of specimen having different atomic
Backscattered
number electrons are not as numerous as others. However, they
generally carry higher energies than other types of electrons
EBSD (Electron Back Scattered Detector)
• The most common detector used is
called a surface barrier detector. It sits
above the sample, below the objective
lens. BSE which strike it are detected.
1. When a BSE electron strikes the
detector, electrons in the material move
from valence to conduction band.
2. The electrons are now free to move in
the conduction band or drop back into
the valence band.
3. If a potential is applied, the e- and e+
can be separated, collected, and the
current measured. The strength of the
current is proportional to the number of
BSE that hit the detector.
QBSD (Quadrant Back Scattered Detector)

The most common design is a four quadrant solid state

detector that is positioned directly above the specimen
 Magnification
• An image is obtained by taking the signal from the
sample and transferring it to a CRT screen. By
decreasing the size of the scanned area (from
which we get the signal), magnification is produced.

Magnification is determined by taking the ratio of the lengths of

the scans:
Mag. = L / I
Magnification
 Resolution
• Resolution is the ability to resolve two closely spaced points. While
you may have to be at a high magnification to see small features,
resolution is NOT the same as magnification.
• One way to improve resolution is by reducing the size of the
dmin = 1.29Cs1/43/4[7.92 (iT/Jc)x109 + 1]3/8
• electron beam that strikes the sample:
at low current: dmin = 1.29Cs1/43/4

Jc = current density of the source,

 = electron wavelength
Cs = spherical aberration,
i = current,
T = temperature.
Resolution
1.
Improving Resolution
reducing spot size by using different types of filament.
2. using optimum accelerating voltages.
3. changing the angle of tilt (i.e. emissive area hence number of SEs).
4. using high beam current
5. short working distance
6. using secondary electron (SE) image, as the optimum resolutions
are:
7. 5 nm for SE; 25 nm for BSE and 2 μm for X-ray mapping.
8. long exposure times, leading to more electrons being detected.
9. reducing lens aberrations to minimum
 Effect of Spot Size

A) using smallest spot,

B) using a slightly larger size of spot
C) using a large size of spot
Effects of Accelerating• Voltage
Higher voltage
generates shorter
wavelength of
electrons → better
resolution.
• Higher voltage
causes an increase
of the volume of
electrons/specimen
interactions →
worse resolution
Effects of Accelerating Voltage

3.0 KeV 20.0 KeV

More signal (brighter)

Effects of Accelerating Voltage

3.0 KeV 20.0 KeV

But (sometimes) reduced resolution

 Depth of Field
• Depth field of the SEM is the greatest among microscopes:
– 20 mm at 10X
– 5 μm at 10,000X
• Large depth of field is a great advantage for keeping in focus all parts
of a rough topography, but a compromise must be made between
field depth and resolution
• Means to improve depth of field:
1. using large spot size.
2. using long working distance.
3. using small final aperture size.
• It is noted here that the machine variables for larger depth of field
would cause a reduce in the resolution power of the SEM.
 Depth of Field
Working distance and aperture size affect depth of field and resolution
• Working distance is the distance between the surface of the specimen and the front
surface of the objective lens, which is around 5-25 mm for most SEMs.
• Aperture size controls the semi-angle, α.
• The working distance between objective lens and specimen can also control the semi-
angle. Thus, smaller aperture and longer working distance → larger depth of field

ds is the spot size.

α can be expressed as aperture size A and working distance, WD
• However,
– The smaller aperture reduces the current of beam → worse resolution.
– The longer working distance increases lens spherical aberration → worse resolution.
 Depth of Field
The depth of field is greater at
long working distance than
that at short working
Depth of Field
 Contrast
• Contrast is the ratio of the change in signal between any two points on the
specimenand the average signal.

• Topographic Contrast: -- mainly given by secondary electron signal, which

is sensitive to the surface structure of specimens. Secondary electrons can
escape from the surface of most materials at depths about 5 nm (50 Å).

• Compositional Contrast: -- given by the backscattered electron signal,

which change with the differences in atomic number, i.e., nuclear charge of
the atoms composing the specimen. The higher the atomic number, the
greater the backscattering. In smooth plane surfaces we are dealing entirely
with compositional contrast
 Contrast
• Major Influences on Contrast
– the incidence angle of impinging electrons onto the
specimen.
– the collecting angle from the specimen to the positively
charged collector.

• Machine Variables for Contrast Improvement

– Reducing working distance
– Using smaller aperture
– Using larger electron beam size
Topography Contras
Composition Contrast
Because of this dependence of on atomic number,
images produced using BSE show characteristic
atomic number contrast.

That is, features of high average Z appear brighter

than those of low average Z
Contrast Comparison

The topography of the

specimen will also affect the
amount of backscatter signal
and so backscatter imaging is
often carried out on flat
polished samples
 More information about SEM Image
• Go to :
– http://www.emal.engin.umich.edu/courses/semlectures/if
orm1.html
– http://micro.magnet.fsu.edu/primer/java/electronmicrosc
opy/magnify1/index.html
– http://education.denniskunkel.com
Specimen Preparation

Stub
 Specimen Preparation
• Sampling: Cutting or Replica formation
– Caution: surface contamination with dust must be avoid during cutting.

• Specimen mounting: using of a conductive cement, gluing the

specimen onto a aluminum stub.
– Caution: contamination of sample surface or the SEM by out gassing of solvent in the
adhesive.

• Specimen surface treatment:

a. No surface treatment is needed if the surface is conductive or if the insulating
layer of the specimen is thin enough for some electrons to penetrate an
underlying conductor. For example: fracture surface of a metal or thin plastic
coating on a metal surface.
 Specimen Preparation
b. A thin layer (~100 Å) of conductive coating (gold or gold
plus palladium or carbon) is needed, if the interesting
surface is an insulator. For example: fracture surfaces of
polymer and ceramics.
c. Surfaces of wet specimens are preserved by freeze-
drying or use of a cold stage. For example, fibers of wet
paper or liquid sample.
d. Morphology of biological and polymeric materials may be
observed with specially prepared samples. For example:
Generating a fast fracture surfaces, using chemical or
plasma etching, etc.
 Preparation for biological samples
• Fixation: to stabilize samples in life like condition and to protect the sample
from disruption, dimensional change and loss of materials during
subsequent processing.
– Chemical fixation: primary fixing in aldehyde or mixture of aldehydes, the
secondary fixing in osmium tetroxide (OsO4).
– Cryogenic fixation: ultra rapid freezing
• Dehydration:
– Solvent drying: in a graded series of solutions containing acetone and ethanol.
– Critical-point drying: the sample is infiltrated with liquid CO2 in a chamber.
As the temperature increases, the pressure increases, finally driving all the liquid into
the gas phase, at which the point sample is dry and gas can be exhausted from
chamber.
• Freeze-substitution method: for ultra-rapid freezing samples.
– Air drying
– Freeze-drying
 Sputtering Equipment

• Sputtering a thin gold or carbon layer (~ 10 nm) on a

specimen surface can improve the conductivity of
specimens. Also you need ensure the conductive layer
connected to the base of specimen holder.