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Techniques

of Materials Characterization
FACULTY NAME: SHIBAYAN ROY
MATERIALS SCIENCE CENTER, IIT KHARAGPUR
Module 03: General concepts of electron microscopy
Lecture 01: Basic components of electron microscope
CONCEPTS COVERED

Ø History of electron microscopy


Ø Components of electron microscopes
Ø Electronic shell and band structure
Ø Electron wavelength and accelerating voltage relations
Ø Electron guns: Thermionic guns
Max Knoll and Ernst Ruska Manfred von Ardenne develops first SEM • Electron microscopes were
invented the electron microscope (1938) developed in the 1930s to
in 1931 enable us to look more
closely at objects than is
possible with a light
microscope.
Cambridge Scientific Instruments
releases the first commercial SEM
(1965)

Charles Oatley begins SEM development


at Cambridge University, UK (1948)
Introduction
• When thinking about light microscopy we tend to ignore most
of the interactions between the light and the specimen.
• It is sufficient that enough light is transmitted through or
reflected from the specimen that the image can easily be seen.
• The assumption is generally made that the specimen is
unchanged and for most specimens this is a reasonable
assumption.
• However, the interaction of electrons with the material through
which they pass may have more serious consequences.

• Real possibilities are that the specimen will be heated by the electron beam
and that chemical changes may take place.
• It is important (in order to appreciate the way in which an electron microscope
works and the meaning of the information which it provides) that we
understand nature of the possible interactions between
• Electron beam and the other parts of the microscope (e.g. lenses or
camera)
• Electrons and the specimen.
TEM fundamental design
A simplified ray diagram of a TEM consists of
• An electron source
• Condenser lens with aperture
• Specimen
• Objective lens with aperture
• Projector lens
• Fluorescent screen
Electronic shell structure
• The nucleus carries a positive charge and is surrounded by
a number of negative electrons which exactly neutralize
this charge.
• When atoms are close to one another in a solid most of
their electrons remain ‘localized’ that is they can be
considered to remain associated with a particular atom
• Some outer ones will be shared, to an extent which
depends on the type of bonding with neighboring atoms.
• The innermost (K shell) electrons are the most tightly
bound, and they would need to be given approximately 20
keV before they could leave the atom.
• It is common to define the zero of the energy scale as the potential energy of a free electron far from any atom.
• The energies of localized electrons are then negative.
• Alternatively, spectroscopists refer to a positive ‘binding energy“ or the energy of the atom with the specified
electron missing, which is the negative of the energy

Two alternative representations of the first three electron shells


around a molybdenum atom. The innermost (K shell) electrons are
the most tightly bound, and they would need to be given
approximately 20 keV before they could leave the atom
Electronic band structure
• For atoms which are bonded to others the energy
level diagram must be modified because the Pauli
exclusion principle forbids shared electrons to
occupy the same states.
• This leads to the development of energy bands,
the most common of which are referred to as the
valence and conduction bands.
• In a metal the conduction band holds the familiar
‘sea of electrons’ which are responsible for
conduction and much of the bonding.
Important for EM
• Inner shell electrons: Lowest energy, nearest to nucleus (usually in K or L shell), sharply defined energy,
localized
• Outer shell electrons: Highest energy (lowest binding energy), outermost occupied shell
• Conduction band: Shared electrons, range of possible energies, delocalized
• Outer electrons are fairly readily detached from their atoms since only a small amount of energy to be supplied.
• It is this easy availability" and low mass which makes ‘free’ electrons so useful.
Electron wavelength
• An electron. considered as a particle, carries a single negative charge of 𝒆 = 𝟏. 𝟔𝒙𝟏𝟎(𝟏𝟗 𝑪 and has a rest mass
𝒎~𝟗𝒙 𝟏𝟎(𝟑𝟏 kg.
• If a single electron is accelerated through a potential difference 𝑽 volts then its energy is 𝒆𝑽 electron volts (eV).
• If 𝑽 is large then its velocity, 𝒗, may well approach the velocity of light, 𝒄, and relativistic effects will become
important.
• Energy given to the electron, can be equated to the energy represented by the relativistic change of mass.
Wavelength-accelerating voltage correlation
• Wavelength of the electron depends on the potential difference, or accelerating voltage: At the accelerating
voltages which are most useful for electron microscopy, (2x104 V upwards) the electrons are accelerated to a
velocity which is a significant fraction of the velocity of light and relativistic effects are quite important.

c = 2.998*108 ms-1
e = 1.602*10-19 C
h = 6.62*10-39 Js
me = 9.108*10-31 kg
Techniques of Materials Characterization
FACULTY NAME: SHIBAYAN ROY
MATERIALS SCIENCE CENTER, IIT KHARAGPUR
Module 03: General concepts of electron microscopy
Lecture 02: Basic components of electron microscope
(continued)
CONCEPTS COVERED

Ø Electron gun: Thermionic gun (continued)


Ø Electron gun: Field emission gun
Ø Comparing electron guns
Ø Electromagnetic lenses
Ø Scanning coils
Electron source (gun)
• Of the many ways of encourgaing electrons to leave a solid so that they may be accelerated towards the
specimen, two have proved particularly useful in the construction of electron guns.
• The most widespread system uses thermionic emission from a heated filament.
• At temperatures in excess of 2700K, a tungsten wire emits an abundance of both light and electrons.

• In a light bulb only the light is used but in an electron gun the electrons are
accelerated across a potential difference of tens or hundreds of kilovolts to generate
a beam of electrons of controlled energy (and hence of known wavelength
• A piece of tungsten, usually a wire bent into a hairpin,
acts as the cathode.
• This filament is heated by the passage of a current to
about 2800K while being held at a high negative
potential with respect to the anode (A) and the rest of
the microscope.
• Electrons thermionically emitted from the filament are
accelerated rapidly towards the anode and a beam of
high energy electrons is emitted through the circular
hole at its centre into the microscope column.
• The addition of a Wehnelt cap (W), which is held at a
voltage slightly more negative than the filament enables
the diameter of the area at the end of the filament
which emits electrons to be controlled.
• The Wehnelt cap acts rather like the grid in a triode
valve (or the base in a bipolar transistor) and hence
this gun is usually called a triode gun.
• The paths of the emitted electrons usually cross at one
point in space and the gun acts as a lens.
• The diameter of the beam at the crossover is
dependent on the area of the filament which is
emitting electrons and this can be controlled by the
difference in potential between the filament and the
grid.
• The crossover diameter is effectively the size of the
electron source.
• A small current flows when the potential is applied but
before the filament current is high enough to give rise to
thermionic emission.
• This is known as the dark current since it flows before the
filament is hot enough to emit light.
• As the emitted current increases so does the bias voltage
and this suppresses further electron emission.
• This is known as the autobias mechanism and accounts for
the characteristic shape of the emission curve.
• As the current through the filament is increased there is an
initial rise in the emitted electron beam current.
• This eventually saturates however and there is no point in
passing more than the critical current through the filament
since this merely increases the temperature of the filament
(thus reducing its lifetime) without giving rise to any
additional beam current.
Brightness of an electron gun
• In the context of electron microscopy brightness is defined as
the beam current density per unit solid angle
• Brightness is therefore a measure of how many electrons per
second can be directed at a given area of the specimen.
• 𝑩 increases rapidly as 𝑻 (temperature of the filament in Kelvin)
increases and as 𝝋 (thermionic work function of the filament
material in electron volts) decreases.
• It is best to use a filament material with as high a melting point
and as low a work function as possible.
• Tungsten has a high melting point (3653 K) and a work function
which is much the same as most metals (4-5 eV) and is the most
widely used filament material.
• Tungsten filaments give a brightness of about 109 Am-2 sr-1.
• The thermionic gun is satisfactory for many purposes but is
limited in the brightness of the beam it can produce.
Example of Tungsten thermionic guns

• Tungsten wire (Tm = 3653K, φ = 4.5 eV, Brightness ~109 Am-2sr-1)


LaB6 thermionic guns
• The brightness can be increased by a factor of 10 or more (from Tungsten)
if LaB6 with a work function of 3.0 eV, is used (𝑩~𝟏𝟎𝟏𝟎 Am-2sr-1).
• Electron guns which use LaB6 are quite common on microscopes which are
used for analytical or high resolution work since in both of these fields a
high brightness is desirable.

Single crystal of LaB6 (φ = 3 eV,


Brightness ~1010 Am-2 sr-1)
Field emission guns (FEG)
• If still higher brightness is required then the field emission gun is used.
• If a metal surface is subjected to an extremely high electric field (> 109 V/m) there is a high probability that
an electron can leave the surface without needing to be given the amount of energy represented by the work
function.
• This is because of the effect predicted by quantum mechanics and known as tunnelling.
• The result is that many more electrons can be drawn from a piece of tungsten than is possible using
thermionic emission and the brightness can be increased in excess of 1013 Am-2 sr-1.
• The field emission current depends very strongly on the applied field.
• For a field in excess of about 5 x 109 Vm-1 the current emitted by field emission at
room temperature exceeds that which can be thermionically emitted: Cold FEG
• In order to apply such a high field the emitter, usually tungsten, has to be prepared in
the form of a sharp point.
• The diameter at the point must be about 0.1 μm, which is orders of magnitude finer
than a pin, so the emitter is a rather delicate structure.
• For this fine point to be preserved in use it must be operated in an environment with
very few ions and this dictates the use of ultra-high-vacuum (UHV) techniques.
• The vacuum in the gun must be lower than 10-7 Pa, which is rather better (and more
expensive to achieve) than the value of 10-2 or 10-3 Pa which is common in thermionic
guns.

• Electrons are extracted from the


fine tip by a first anode and then
accelerated down the column by
a second anode at a much higher
potential.
Advantage of FEG
• An important feature of field emission sources is that the
emitted electrons have very well defined energies.
• Whereas the electrons from a thermionic source inevitably
have an energy spread of 1-2 eV, the electrons from a cold
FEG have a much smaller energy spread, usually less than
0.5 eV.
• Thus for both analytical and high resolution electron
microscopy, field emission sources are important not just
because they provide a high brightness beam but because
they provide a ‘clean’ monochromatic supply of electrons.
• Electron beam energy distribution of cold FEG on HD-2700
(Hitachi High-Technologies Corp.) measured with Gatan
electron energy-loss spectroscopy detector (Gatan Inc.;
Acceleration voltage: 200 kV, acquisition time: 1 s,
dispersion: 0.05 eV/pixel).
Comparing electron guns
Techniques of Materials Characterization
FACULTY NAME: SHIBAYAN ROY
MATERIALS SCIENCE CENTER, IIT KHARAGPUR
Module 03: General concepts of electron microscopy
Lecture 03: Basic components of electron microscope
(continued)
CONCEPTS COVERED

Ø Electromagnetic lenses
Ø Scanning coils
Ø Aberrations in EM
Ø Electron waves
Electromagnetic lenses
• A beam of electrons could be focused by either an
electrostatic or a magnetic field.
• Both types of field have been used in electron lenses but the
electromagnetic lens is by now virtually universal in
commercial electron microscopes.
• The key to an understanding of what is essentially a very
simple lens is the direction of the force which acts on a
moving electron in a magnetic field.
• If an electron moving with velocity 𝒗 experiences a magnetic
field of strength 𝑩, then it suffers a force 𝑭 = 𝒆(𝐁 ∧ 𝒗) in a
direction perpendicular to both the direction of motion and
the magnetic field.
Forces on electrons in EM lenses
• A typical electromagnetic lens is designed to provide a magnetic field almost parallel to the direction of travel
of the electrons.
• An electron entering the lens experiences a magnetic field 𝑩 which can be resolved into components 𝑩𝒂𝒙
along the axis of the microscope and 𝑩𝒓𝒂𝒅 in a radial direction.
• Initially the electron is unaffected by 𝑩𝒂𝒙 , which is parallel to its direction of travel, but experiences a small
force of magnitude 𝑭𝒓𝒂𝒅 = 𝑩𝒓𝒂𝒅𝒆𝒗 from the small radial component.
Forces on electrons in EM lenses
• Initially the electron is unaffected by 𝑩𝒂𝒙 , which is parallel to its direction of travel, but
experiences a small force of magnitude 𝑭𝒓𝒂𝒅 = 𝑩𝒓𝒂𝒅𝒆𝒗 from the small radial
component.
• This force causes the electron to travel in a helix along the lens.
• As soon as it starts to spiral it has a component of velocity 𝒗𝒄𝒊𝒓𝒄𝒖𝒎 perpendicular to the
plane of the paper and therefore experiences a force of magnitude 𝑭𝒂𝒙 = 𝑩𝒂𝒙𝒆𝒗𝒄𝒊𝒓𝒄𝒖𝒎
in a radial direction.
• The helical path follows a tighter and tighter radius
• The effect is that a parallel beam of electrons entering the lens is caused to converge to
a point exactly as light is focused by a glass lens.
How the EM lenses works?
• If the magnetic field only extends over a short distance along the axis, then the
lens behaves as a ‘thin lens’.
• A coil consisting of a large number of turns of wire is wound on a soft iron core
(pole piece) which has only a very small accurately machined air gap across which
the field is produced.
• By varying the current passing through the coil (typically in the range 0-1 A) the
magnetic field strength and hence the focal length of the lens can be varied.
How the EM lenses works?
• An important feature for which there is no analogy in the light
microscope is the spiraling of the electrons as they travel through an
electromagnetic lens.
• Since it is very rare for the electron to travel an integral number of
turns of the spiral as it passes through the lens in general there is a
rotation of the image caused by the lens.
• This is not a distortion since the image is otherwise unaffected.
• Cunning design of electron-optical systems in modern microscopes
sometimes involves using lenses in combinations which cancel out the
image rotation.
Scanning coils
• Electromagnetic fields are also
used to deflect the entire beam of
electrons to scan the beam back
and forth in an electron
microscope.
• For these applications, the field
needs to be perpendicular to the
electron beam, but much smaller
fields sufiice for these smaller
deflections so the coils are quite
small.
• Most microscopes will contain a
dozen or more such coils,
designed to enable the
microscopist to optimize the
position of the beam in the
column of the microscope.
Aberrations in EM
• In the electron microscope (TEM in particular), resolution limited by
ONLY diffraction cannot be obtained because of the lens aberrations.
• Whereas in a light microscope it is possible to correct both chromatic
and achromatic aberrations by using subtle combinations of lenses,
this is very difficult using electron lenses and has only been seriously
attempted in the 1990s.
Corrections of aberrations
• Chromatic aberrations can be virtually eliminated by using electrons of a very
small range of wavelengths (by using FEG electron sources).
• It is not possible to eliminate the monochromatic aberrations, principally
spherical aberration.
• The spherical aberration is caused by the lens field acting inhomogeneously on
the off-axis rays.
• The rays which are "parallel" to the optic axis but at different distances from the
optic axis fail to converge at the same point.
• The further off-axis the electron is, the more strongly it is bent back toward the
axis.
• A point object is imaged as a disk of finite size, which limits the ability to
magnify detail, because features are degraded by the imaging process.
• A point 𝑷 is imaged as a disk with a minimum radius in the plane of "least
confusion" and as 𝑷4 with an intense central bright region with a surrounding
halo in the image plane.
Effect of spherical aberration
• A point source imaged by a system with
negative (top), zero (center), and positive
(bottom) spherical aberration.
• Images left of the center column are
defocused toward the inside; images
right of the center column are defocused
toward the outside.
• Only the central point is a dot; the image
above and below it appears as a disc.
• The amount of blur i.e. degradation of resolution caused
by spherical aberration on the object plane,
𝒓𝟐 = 𝑪𝒔 𝜷𝟑
• 𝑪𝒔 is spherical aberration coefficient and 𝜷 is the angle
between electron beam and the optical axis i.e. the
maximum semi-angle of collection of the objective lens
aperture.
• 𝑪𝒔 has the dimensions of length.
• For a rotationally symmetric lens with respect to the
optical axis, the value of 𝑪𝒔 is always positive.
• The practical way of minimizing this is to restrict the
electrons to paths very near the optical axis, i.e. near the
centre of the lens, by using asmall objective aperture (by
reducing 𝜷).
• The use of a small aperture reduces spherical aberration but makes the
difraction-limited resolution (𝒓𝟏) worse.
• There is an optimum size of aperture (i.e. value of 𝜷) for which the net
resolution is smallest.
• Net resolution 𝒓 = 𝒓𝟏 + 𝒓𝟐
𝟏 𝟏 𝟑 𝟏
E
• Minimizing 𝒓 with respect to 𝜷, 𝜷𝒐𝒑𝒕 = 𝟎. 𝟔𝟕𝝀 𝑪𝒔 ; 𝒓𝒐𝒑𝒕 = 𝟏. 𝟐𝟏𝝀 𝑪
𝟒 𝟒 𝟒 𝒔𝟒
• The resolution can be improved by reducing the factor 1.21 to as low as
0.7 in favourable circumstances.
• Using the optimum aperture it is now possible with a good TEM to
resolve two points about 0.2 nm apart (approximately the separation of
atoms in a solid).
• Since it is necessary to keep 𝜷 small in order to reduce the effect of
spherical aberrations, electron microscopes always gain the advantage of
a large depth of field.
𝟎.𝟔𝟏𝝀
• For EM, 𝒉 = 𝜷𝟐 , as 𝜷 is reduced the depth of field increases very
rapidly.
• One way to minimize spherical aberration is to use a short focal length
lens (i.e. small 𝑪𝒔).
• Spherical aberration coefficient (𝑪𝒔) is decreasing as the relative 𝜽 =
𝜷 𝒙 𝑳 increasing (𝑳 = Effective length of lens)
Techniques of Materials Characterization
FACULTY NAME: SHIBAYAN ROY
MATERIALS SCIENCE CENTER, IIT KHARAGPUR
Module 03: General concepts of electron microscopy
Lecture 04: Electron-material interaction
CONCEPTS COVERED

Ø Electron-atom interaction
Ø Elastic and inelastic interaction
Ø Elastic scattering of electrons
Ø Interaction cross section
Electron waves
• Waves in electron beams can be either coherent or incoherent.
• Waves that have the same wavelength and are in phase (wave
maxima appear at the same site) with each other are designated
as coherent.
• The analogue in light optics is a Laser beam.
Coherent wave
• On contrast, beams comprising waves that have different
wavelengths (like sun rays) and/or are not in phase are called
incoherent.

Incoherent wave
Interference of waves
• Waves do interact with each other. By linear
superposition, the amplitudes of the two waves
are added up to form a new one.
• The interference of two waves with the same
wavelength can result in two extreme cases.
• Constructive interference: If the waves are
completely in phase with each other, meaning
that the maxima (and minima) are at the same
position plus have the same amplitude, then the
amplitude of the resulting wave is twice that of
the original ones.

• Destructive interference: If two waves with the same


amplitude are exactly out of phase, meaning that the
maximum of one wave is at the position of the minimum
of the other, they are extinguished.
Non rel. Rel. λ / V /108
V / kV m x m0
λ / pm pm m/s
• Electrons accelerated to a selected energy have the
same wavelength. 100 3.86 3.70 1.20 1.64
• Depending on the electron gun, the energy spread and 200 2.73 2.51 1.39 2.09
as a result the wave length as well varies. 300 2.23 1.97 1.59 2.33
• The electron waves are only nearly in phase with each 400 1.93 1.64 1.78 2.48
other in a thermoionic electron gun while the 1000 1.22 0.87 2.96 2.82
coherency is much higher if a field emitter is the
electron source. Table : Properties of electrons depending on the
accelerating voltage
• The generation of a highly monochromatic and
coherent electron beam is an important challenge in
the design of modern electron microscopes.
• Electron beam from an electron source is a bundle of
coherent electron waves, before hitting a specimen
• After interacting with specimen, electron waves can
form either coherent or incoherent beams
Importance of electron-material interaction
• Electron microscopy today, is not just a single technique but a diversity of different ones that offer unique
possibilities to gain insights into structure, topology, morphology, and composition of a material.
• Various imaging and spectroscopic methods represent indispensable tools for the characterization of all kinds of
specimens on an increasingly smaller size scale with the ultimate limit of a single atom.
• The observable specimens include inorganic and organic materials, micro and nano structures, minerals as well
as biological objects
• The wealth of very different information that is obtainable by various methods is caused by the multitude of
signals that arise when an electron interacts with a specimen.
• Gaining a basic understanding of these interactions is an essential prerequisite: The different types of electron
scattering are the basis of most electron microscopy methods
Electron-material interaction
• The positive charge of the atom in strongly concentrated at the nucleus,
whereas negatively charge electron atoms are much more dispersed
• Electron entering a material interacts with electric fields of nucleus and
specimen electrons.
• Elastic interactions: No energy is transferred from electron to atoms;
electron leaving the sample still has the original energy.
• No energy is transferred if the electron passes the sample without any
interaction at all.
• Such electrons contribute to the direct beam which contains the
electrons that passes the sample in direction of the incident beam.
• Elastic scattering happens if the electron is deflected from its path by
Coulomb interaction with the positive potential inside the electron
cloud.
• By this, the primary electron loses no energy or, to be accurate, only a
negligible amount of energy.
Elastic interaction
• Elastic interaction or scattering is defined as
a process which, although it might change
the direction of the primary electron, does
not change its energy detectably.
• Electrons are scattered from electron cloud
and nucleus of a single atom at the angle 𝜽.

• This type of scattering results from Coulombic interactions (i.e. involving


electrostatic charges) between the primary electron and both the nucleus
and all the electrons around it.
• This is known as Rutherford scattering and it gives rise to a strongly ‘forward
peaked‘ distribution of scattered electrons.
• Elastic scattering is important in electron microscopy because it is a major
mechanism by which electrons are deflected and also because elastically
scattered electrons are the main contributors to diffraction patterns.
Inelastic interaction
• Inelastic interactions: The energy of the incident
electron is transferred to the sample atoms.
• After interaction electron energy is reduced.
• The energy transferred to the specimen can cause
different signals such as X-rays, Auger or secondary
electrons, plasmons, phonons, UV quanta or
cathodoluminescence.
• Signals caused by inelastic electron-matter
interactions are predominantly utilized in the methods
of analytical electron microscopy plus in scanning
electron microscopy.

• Most of the energy of an electron beam will eventually end up heating


the sample (phonon excitation of the atomic lattice)
• Before the electrons come to rest, they undergo two types of scattering:
Coherent and incoherent.
Elastic interaction: Scattering
• An electron penetrating into the electron cloud of an atom is attracted
by the positive potential of the nucleus (electrostatic or Coulombic
interaction), and its path is deflected towards the core.
• The Coulombic force 𝑭 is defined as:
𝑸𝟏 𝑸𝟐
𝑭 =
𝟒𝝅𝜺𝒐 𝒓𝟐
𝒓 = distance between the charges 𝑸𝟏 and 𝑸𝟐; 𝜺𝒐 = dielectric constant.
• The closer the electron comes to the nucleus, i.e. the smaller 𝒓, the
larger is 𝑭 and consequently the scattering angle, 𝜽.
Elastic interaction: Scattering
• Elastic interactions deflects the electron beam along new trajectory, causing
them to spread laterally.
• A strong elastic scatter very near to the nucleus may result in a beam of
electrons leaving the specimen via back scattering, called Backscattered
electrons (BSE).
• These electrons provide an important class of information for SEM imaging.
• The strength of scattering by an atom depends on its atomic number and is
usually described in terms of its atomic scattering factor.
• This is defined as the amplitude of scattering from the atom divided by the
amplitude of scattering from a single electron.
Elastic interaction: Scattering
• If the energy of the primary electron is 𝑬𝒐, the probability 𝒑 𝜽 of it
being scattered through an angle 𝜽 is given by
𝟏
𝒑 𝜽 ∝ 𝟐
𝑬𝒐 𝒔𝒊𝒏𝟒𝜽
• The probability of a small angle of scatter is very much greater than that
of a large angle.
• The probability of scattering through any angle decreases as the energy
of the electron increases.
Elastic interaction: Scattering
• Because of its dependence on the charge, the force 𝑭 with which an atom
attracts an electron is stronger for atoms containing more positives
charges, i.e. more protons.
• Thus, the Coulomb force increases with increasing atomic number 𝒁 of
the respective element.
• Probability of elastic scattering,
• Increases strongly with atomic number (as 𝒁𝟐), as heavier atoms
have much stronger positive charge at nucleus
𝟏
• Decreases as electron energy increases (as ) Probability of elastic
𝑬𝟐
scattering

𝑸𝟏 𝑸𝟐
𝑭 =
𝟒𝝅𝜺𝒐 𝒓𝟐
Probability of electron scattering

• If an electron passes through a specimen, it may be scattered


not at all, once (single scattering), several times (plural
scattering), or many times (multiple scattering).
• Although electron scattering occurs most likely in forward
direction, there is even a small chance for backscattering
• The chance that an electron is scattered can be described by
• Probability of a scattering event, as determined by the
interaction cross-section, 𝝈
• Average distance an electron travels between two
interactions, the mean free path, 𝝀𝒎𝒑𝒇
Techniques of Materials Characterization
FACULTY NAME: SHIBAYAN ROY
MATERIALS SCIENCE CENTER, IIT KHARAGPUR
Module 03: General concepts of electron microscopy
Lecture 05: Electron-material interaction (continued)
CONCEPTS COVERED

Ø Interaction cross section


Ø Mean free path
Ø Interaction volume
Ø Size of interaction volume
Ø Monte-Carlo simulation and K-O range
Interaction cross-section
• The concept of the interaction cross-section is based on
the simple model of an effective area.
• If an electron passes within this area, an interaction will
certainly occur.
• The cross-section is expressed as the area which the
scattering particle appears to present to the electron.
• If the cross section of an atom is divided by the actual
area, then a probability for an interaction event is
obtained.
• If there are 𝑵 particles per unit volume of the specimen
and the cross-section for a particular scattering event is
𝝈, the probability of a single electron being scattered in
its passage through a thickness 𝒅𝒙 of the specimen
𝒑 𝜽 = 𝑵𝝈𝒅𝒙
• The likelihood for a definite interaction increases with
increasing cross-section.
Interaction cross-section
• Each scattering event might occur as elastic or as inelastic
interaction.
• The total interaction cross section is the sum of all elastic and
inelastic terms, 𝝈 = 𝝈𝒆𝒍𝒂𝒔𝒕𝒊𝒄 + 𝝈𝒊𝒏𝒆𝒍𝒂𝒔𝒕𝒊𝒄
• Each type of possible interaction of electrons with a material
has a certain cross section that depends on the electron
beam energy.
• For every interaction, the cross section can be defined
depending on the effective radius, 𝝈 = 𝝅𝒓𝟐
• The cross-section and thus the likelihood of scattering events
increases for larger radii.
• For the case of elastic scattering,
𝒁𝒆
𝒓𝒆𝒍𝒂𝒔𝒕. =
𝑬𝜽
𝒁 = atomic number; 𝒆 = elementary charge; 𝑬 = electron
potential; 𝜽 = scattering angle.
• Scattering is stronger for heavier atoms (with high 𝒁) than for
light elements.
Interaction cross-section
𝒁𝒆
𝒓𝒆𝒍𝒂𝒔𝒕. =
𝑬𝜽
• Electrons scatter less at high voltage 𝑬 and that scattering
into high angles 𝜽 is rather unlikely.
• Considering that a sample contains 𝑵 number of atoms in a
unit volume, total scattering interaction cross section
𝑵𝒐 𝝈𝑻 𝝆
𝑸𝑻 = 𝑵𝝈 =
𝑨
𝑵𝒐: Avogadro number; 𝑨: atomic mass of the atom of density 𝝆.
• Introducing the sample thickness (𝒕),
𝑵𝒐𝝈𝑻 𝝆𝒕
𝑸𝑻 𝒕 =
𝑨
• This gives the likelihood of a scattering event.
• The term 𝝆𝒕 is designated as mass-thickness. Doubling 𝝆 leads
to the same 𝑸 as doubling 𝒕.
Mean free path (𝝀 𝒎𝒇𝒑 )
• For a scattering process, 𝝀 𝒎𝒇𝒑 is the average distance travelled by an
electron between two scattering events.
• This means, that an electron in average interacts two times within the
distance of 𝟐𝝀 𝒎𝒇𝒑.
• Mean free path is related to the scattering cross section,
𝟏
𝝀 𝒎𝒇𝒑 = 𝑸
𝑻
• For scattering events in the TEM, typical mean free paths are in the
range of some tens of nmsimilar to the thickness of a TEM specimen.
• This means that electrons will tend to be scattered either once or not at all
while passing through a thin specimen.
• If an electron is incident on a thick specimen (e.g. SEM), it will be scattered
many times until it comes to rest.
• The mean free path for elastic scattering depends quite strongly on the atomic
number of the scattering atom.
• To give an example for 100 kV electrons, it is about 5 nm for gold (atomic
number Z = 79) but about 150 nm for carbon (Z = 6).
Plural and multiple scattering
• In single or plural scattering situations, the probability of an
incident electron suffering an scattering events while
travelling any distance is given by the Poisson equation.
𝟏 𝒙 𝒏 𝒙
𝒑 𝒏 = 𝒆𝒙𝒑 −
𝒏! 𝝀 𝝀
• 𝒑 𝟎 is the probability of the electron not being scattered
and that 𝟏 − 𝒑 𝟎 is the probability of it being scattered
once or more.
• The Poisson equation approach is not much use for multiple
scattering, where all primary electrons can be assumed to
be scattered very many times, possibly by several different
mechanisms.
• In these cases other averaging approaches are more fruitful;
one example is the Monte Carlo method.
Annular distribution of electron scattering: Differential cross
section
• Electrons are scattered by an angle 𝜽 and collected within a solid angle 𝜴.
• The scattering semi-angle 𝜽 (and incremental changes 𝒅𝜽) and the solid angle 𝛀
of their collection (and incremental changes 𝒅𝛀) are used to describe the
scattering process quantitatively.
• The angular distribution of electrons scattered by an atom is described by the
𝒅𝝈
differential cross section 𝒅𝜴.
• Scattering into high angles is rather unlikely.
• If the scattering angle increases, the cross-section decreases.
• The differential cross-section is important since it is often the measured quantity.
Interaction volume
• Region generated because of electron-specimen
interaction is interaction volume.
• Elastic and Inelastic scattering together distribute
a single incident electron beam over a 3-
Dimensional region inside the material.
• Size and shape of the interaction volume
depends on the relative amount of elastic
and inelastic scattering on electron beams.
• Direct measurement of interaction volume for materials with intermediate and high atomic number materials is
not possible.
• Etching plastic can directly reveal the interaction volume for the low atomic number materials, but it can not do
the same for intermediate or high atomic number materials, such as metals.
Signal production after interaction
• The size and shape of the interaction volume is limited by
two factors:
• Energy loss through inelastic interactions
• Electron loss or backscattering through elastic
interactions.
• A beam of electrons lose energy as they traverse the sample
due to interactions with it.
• If too much energy is required to produce an effect, it will
not be possible to produce it from deeper portions of the
volume.
Size of interaction volume
• The depth of electron penetration of an electron beam
and the volume of sample with which it interacts are a
function of
• Angle of incidence,
• Magnitude of current,
• Accelerating voltage, and
• Average atomic number (𝒁)
• The degree to which an effect, once produced,
can be observed is controlled by how strongly it
is diminished by absorption and scattering in the
sample.
• For example, although secondary and Auger
electrons are produced throughout the
interaction volume, they have very low energies
and can only escape from a thin layer near the
sample's surface.
Size of interaction volume
• Two important parameters describing interaction volume:
• Depth of electron penetration (𝒙)
• Width of the excited volume (𝒚)
• Electron penetration generally ranges from 1-5 µm with the
beam incident perpendicular to the sample.
• Better results are obtained using Monte Carlo approximations.

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