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SEM-Chapter 2-1

Electron microscopy, developed in the 1930s, surpasses optical microscopy by utilizing electron beams for higher magnification and resolution. It provides detailed information on topography, morphology, composition, and structure of samples through various electron interactions. Key components of scanning electron microscopes include electron guns, electromagnetic lenses, and detectors, all operating in a high-vacuum environment to ensure optimal performance.

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0% found this document useful (0 votes)
4 views60 pages

SEM-Chapter 2-1

Electron microscopy, developed in the 1930s, surpasses optical microscopy by utilizing electron beams for higher magnification and resolution. It provides detailed information on topography, morphology, composition, and structure of samples through various electron interactions. Key components of scanning electron microscopes include electron guns, electromagnetic lenses, and detectors, all operating in a high-vacuum environment to ensure optimal performance.

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kumarmadhav990
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An Introduction to

Electron Microscopy
History
Electron microscopes were developed in the 1930s to overcome the limitations of optical microscopy and provide
increased magnification and resolution, far superior to optical systems. The first commercialized SEM was built by
Cambridge Instruments.
Electron microscope constructed by
Ernst Ruska in 1933
The Need for Electron Microscopy

 Electron microscopes were developed to overcome the limitations of traditional light microscopes, which use
visible light to magnify and observe samples. The fundamental constraint of light microscopes is the wavelength
of visible light, which limits their resolution to around 200 nanometers.
 Electron microscopes, on the other hand, use a focused beam of electrons instead of visible light. Electrons have
much shorter wavelengths than light, allowing electron microscopes to achieve much higher resolution.
 The resolving power of a microscope is directly related to its ability to distinguish between two closely spaced
objects. It is inversely proportional to the wavelength of the imaging radiation.
 The resolving power of an microscope can be improved either by reducing the wave length of light or by
increasing the NA value.
 SEM offers an exceptionally wide range of magnifications. SEM allows for easily adjustable magnifications.
Researchers can seamlessly transition between different magnification levels.
 SEM utilizes high-brightness electron sources. The combination of high-brightness sources and advanced electron
optics allows the formation of fine-focused electron beams.
 Depth of Focus in SEM: SEM provides superior depth of focus compared to traditional microscopes. SEM's
advanced imaging capabilities allow for a broader range of focus within a specimen.
 A SEM typically has orders of magnitude better depth of focus than a optical microscope making SEM suitable for
studying rough surfaces
What information can we obtain from electron microscopes?

 Topography: Surface features of an object. “How it looks.”

 Morphology: Size and shape of particles making up object.

 Composition: Relative amount of elements and compounds making up the object.

 Structure: Crystallography. How atoms are arranged in the object. Substructure. Defect type and content.
ELECTRON BEAM – SAMPLE INTERACTIONS
Interaction volume is larger for materials that have lower atomic numbers and for higher
incident beam energies!
There are two types of scattering interactions that are
possible when an electron beam impinges on atoms of the
sample:

1. Elastic Scattering: Interaction between the electron source


and atomic nuclei gives rise to elastic scattering, which
results in a large-angle deflection of the electron beam with
little or no energy loss. E.g. Backscattered Electrons
2. Inelastic Scattering: Electron–electron interactions between
(a) an elastically scattered
the source and electron clouds of individual atoms cause electron and (b) an
small-angle deflections with a significant loss of energy, inelastically scattered
electron.
known as inelastic scattering. E.g. Secondary Electrons
Electron bombardment can produce a wide variety of emissions from the specimen, including backscattered
electrons, secondary electrons, Auger electrons, X-rays, visible photons and so on.

1) Secondary Electrons: If an incident electron collides with an electron in a sample atom, it


will knock the electron out of its orbital shell and the atom will become ionised. Because the
incident electron loses little energy during each collision, multiple collisions are possible,
continuing until the incident electron no longer has the energy to dislodge secondary electrons.
Each freed secondary electron has a very small kinetic energy (<50 eV), which is independent of
the incident electron energy. If generated close enough to the sample surface (<10 nm), these
secondary electrons can escape to be collected by the detector. As a direct result, secondary
electron imaging is closely related to sample topography.
2) Backscattered Electrons: If an incident electron collides with the nucleus of surface atom, the
electron will bounce or scatter ‘backward’ out of the sample as a backscattered electron (BSE).
These electrons have high energies, typically between 50 eV and that of the original incident
electron. The production of backscattered electrons varies directly with atomic number, and thus
backscattered electron images can be used to discern differences in sample atomic number.
3) Characteristic X-rays: X-rays are also produced by interactions of the incident electron beam
with a sample surface. As a result of secondary electron generation, a vacancy is left in an ionised
atom’s electron shell. To fill this vacancy, an electron from a higher energy outer shell (from the
same atom) can drop down to fill the vacancy. Similar to the Auger electron generating process,
the excess energy produced by reshuffling electrons to fill shell vacancies can also be emitted in
the form of an X-ray rather than an Auger electron. X-rays have a characteristic energy unique to
the element from which they originate and so provide compositional information about a sample.
4) Auger Electrons: As a result of secondary electron generation, a vacancy is left in an
ionised atom’s electron shell. To fill this vacancy, an electron from a higher energy outer shell
(from the same atom) can drop down to fill the vacancy. This creates an energy surplus in the
atom that can be corrected by emitting an outer electron, an Auger electron. Auger electrons have
a characteristic energy unique to the element from which they are emitted and can be used to give
compositional information about the target sample. Auger electrons have a relatively low kinetic
energy and are only emitted from shallow sample depths (<3 nm).
Configuration of Scanning Electron Microscopes
 In this section, we will present a detailed discussion of the major components in an SEM.
 The electron gun, which is on the top of the column, produces the electrons and accelerates them to an energy
level of 0.1–30 keV. It consists of an electron gun to produce high energy electron beam.
 The diameter of electron beam produced by hairpin tungsten gun is too large to form a high-resolution image. So,
electromagnetic lenses and apertures are used to focus and define the electron beam and to form a small focused
electron spot on the specimen. A magnetic condensing lens is used to condense the electron beam. This process
demagnifies the size of the electron source (~50 µm for a tungsten filament) down to the final required spot size
(1–100 nm).
 A scanning coil is arranged in-between magnetic condensing lens and the sample.
 A high-vacuum environment, which allows electron travel without scattering by the air, is needed.
 The electron detector (Scintillator) is used to collect the secondary electrons and can be converted into electrical
signal.
 The specimen stage, electron beam scanning coils, signal detection, and processing system provide real-time
observation and image recording of the specimen surface.
The basic components used in electron optical system are:
 A source of electrons, called electron gun
 Lenses
 Scanning Coils
 Detectors to collect signals
 Sample Stage Infrastructure Requirement
 Display/Data output devices  Power supply
 Vacuum system
 Cooling system
 Vibration free floor
 Room free of ambient electric and magnetic fields
Electron Sources:
Electron Gun: It is used to produce fine electron beam (and is also called as electron probe). Several different
types of electron guns used are:
a) TE (Thermionic- Emission) gun
b) FE (Field- Emission) gun
c) SE (Schottky- Emission) gun
Anatomy of an electron source
(i.e., electron gun)
The filament is resistively heated to 2000
– 2700K by applying a high voltage and a
small amount of current to a point that
valence electrons are released from its tip
in what is called a space charge cloud.
The amount of energy needed to cause
electrons to leave the filament is called the
work function.
Thinnest point of beam known as cross-
over (15-20μm Diameter), regarded as
actual electron source.
LaB6 crystal is used as a cathode. It used
to reduce the spot size. It requires high
vacuum due to its higher activity.
Tungsten: LaB6:
stable beam current stable beam current
short life 10 times longer life
large tip smaller tip
large emitting area (probe diameter) smaller emitting area (probe diameter)
low brightness higher brightness (10 times higher current)
high work function lower work function
high evaporation rate medium evaporation rate
lower vacuum (10-6 Torr) higher vacuum (10-7 Torr)
low resolution higher resolution (due to thinner beam)
2700 K 1700 K
This is based on the fact that electrons can be drawn off from a material by applying a high voltage in ultra high vacuum
conditions.  very high brightness (1000 times compared to hot guns)
 stable beam current if heated, unstable if cold
 concentrated electric field can tunnel through energy barrier
 very long life
 low evaporation rate
 more monochromatic
 very high vacuum (10-10 Torr)
 small tip
 very high resolution (electrons are emitted from a very fine
 very small emitting area (small probe diameter)
tip) and three types – cold, thermal, Schottky
Electromagnetic Lenses
Consists of a soft magnetic core (case) that encloses a
solenoid. Poles located at annular opening in case.
Concentrates magnetic field between poles.
Focus the electron beam to as small a spot as is possible.
They are equivalent to convex lenses in optical lens
systems.

To produce finest beam of electron with desired crossover


diameter, two- level lens system, i.e., condenser and
objective lens, made of metal cylinders with cylindrical
hole, operating in vacuum is used. These lenses are located
beneath the electron gun. Magnetic field is generated in the
inner part of the lenses to focus or de-focus the beam.
We use combinations of electromagnetic
lenses to increase magnification.
Role of condenser lens:
Condenser lens affects the probe size. If it is strengthened then probe size is narrowed with a smaller ratio of b/a, whereas if it
is weakened then probe size is broadened. C1 and C2 lenses control the beam current by varying size and intensity of beam
spot. Aperture is formed by making a small hole in the metal placed between the two condenser lenses and the objective lensto
allow the beam to pass through it and reach the objective. Resolution is dependent upon aperture as it controls the spot size.

Role of objective lens:


It is used for focusing and determines the final diameter of probe.
Detectors

Traditional Detectors:
 Secondary electron detector: (Everhart-
Thornley)
 Backscattered electron detector: (Solid-State
Detector)
 X-rays: Energy dispersive spectrometer (EDS)
Secondary Electron Detectors:
The majority of the work done on a SEM is for topographical information. Topographical
information is mainly provided by secondary electrons that are produced by the interaction of the
beam with the specimen. A secondary electron detector magnetically attracts emitted secondary
electrons by a +200 volt potential applied to a ring around the detector (Faraday Cup). Upon
entering the ring, the secondary electron is attracted and accelerated by the +10 kilovolt potential
on the scintillator. The secondary electrons hit the scintillator causing photons to be emitted.
Photons emitted from the scintillator travel down the light pipe hitting the photomultiplier (PM).
The function of the photomultiplier is to increase or amplify original signal. Thus, for every
photon generated several electrons will be produced, this will result in a significant amplification
of the original signal. The amount of amplification of the photomultiplier tube is controlled by the
PM voltage control (Contrast Control).
The BSE detector :solid state semiconductor diode
 The backscattered electron detector is usually a solid state semiconductor diode operating on the principle of
electron-hole production induced by energetic electrons. It has the form of a flat, thin plate with an annular
opening in the middle.
 Solid state BSE detectors are positioned between the sample and the objective lens. The electron beam passes
through a hole in the centre of the detector and backscattered electrons are collected as they are returned from the
sample.
 The resulting image has greyscales based on the contrast produced by the sample.
 The contrast of the image depends on various factors like the atomic number (Z) of the sample material, the
acceleration voltage of the primary beam, and the specimen angle (tilt) with relation to the primary beam.
 Backscattered electrons therefore give us useful information about the composition and surface topography of the
sample. Material with a high atomic number (Z), like gold (Au) will generate more BSEs than material with a
lower atomic number, like silicon (Si). Because of these differences in backscatter electron yield the detector can
be used to identify different phases or inclusions.
The BSE detector
Why do we need vacuum?
• Chemical (corrosion!!) and thermal stability is necessary for a well functioning filament (gun
pressure)
– A field emission gun requires ~ 10-10 Torr
– LaB6: ~ 10-6 Torr
• The signal electrons must travel from the sample to the detector (chamber pressure)
– Vacuum requirements is dependant of the type of detector
Douglas BM. Fundamentals of Light Microscopy and Electronic
Imaging. A John Wiley & Sons, Inc., Publication. 7Edn.

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