Electron Microscope

Electron microscopes have emerged as a powerful tool for the characterization of a wide range of
materials. Their versatility and extremely high spatial resolution render them a very valuable tool
for many applications. The two main types of electron microscopes are the Transmission
Electron Microscope (TEM) and the Scanning Electron Microscope (SEM).

Principle of electron microscope

The interaction between the primary beam of high energy electrons and the sample leads to
number of detectable signals as summarized in following scheme.

Schematic of electron beam interaction.

In SEM, mainly secondary and back scattered electrons are used for imaging. These electrons
have a very low energy (around 50 eV) compared to the energy of primary electrons (up to
30keV). Due to the low energy, these electrons can escape only from the surface area of the
specimen and provide the information about the surface topography.

In TEM analysis transmitted electrons like elastically scattered electrons are used for imaging.
These transmitted electrons provide a two-dimensional image of the object. As a result, TEM
offers invaluable information on the inner structure of the sample, such as crystal structure,
morphology and stress state information
 Scanning Electron Microscopy
The scanning electron microscope (SEM) produces images by scanning the sample with a high-
energy beam of electrons. 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.

Principle:

Accelerated electrons in an SEM has significant amounts of kinetic energy, and this
energy is dissipated as a variety of signals produced by electron-sample interactions when the
incident electrons are decelerated in the solid sample. As the electrons interact with the sample,
they produce secondary electrons, backscattered electrons, and characteristic X-rays. These
signals are collected by one or more detectors to form images which are then displayed on the
computer screen.

Secondary electrons and backscattered electrons are commonly used for imaging samples:
secondary electrons are most valuable for showing morphology and topography on samples and
backscattered electrons are most valuable for illustrating contrasts in composition in multiphase
samples (i.e. for rapid phase discrimination).

Instrumentation

The main SEM components include:

▪ Source of electrons (Electron gun)

▪ Electromagnetic lenses
▪ Electron detector
▪ Sample chamber
▪ Computer and display to view the images
1. Electron gun
Electrons are emitted from a metal by two methods:
1. Thermionic emission: In this method the electrons are emitted from the metals by heating
them.
2. Field emission: In this method the electrons are emitted from metals, under strong electric
fields.
Thermionic electron gun
The filament is made from a high melting point material or low work function, in order to emit
many electrons. Tungsten filament or lanthanide hexaborate are commonly used in thermionic
electron gun. Tungsten wire used as thermionic cathodes are of 0.1-0.2mm in diameter bent like
a hairpin and soldered on contacts. The wire is heated by a current of a few amperes.
Field emission electron gun
In field emission electron gun, a very strong electric field is used to extract electrons from a
metal filament. Temperatures are lower than that needed for thermionic emission. This gives
much higher source brightness than thermionic guns, but requires a very good vacuum.

Blog diagram of SEM

2. Magnetic lens system

The magnetic lens system consists of a:
1. Condenser lens
2. Objective lens/aperture
3. Scanning coils
Condenser lens

The condenser lenses are made up of magnets capable of bending the path of electrons. These
lens controls the intensity of the electron beam reaching the specimen.

Objective lens

The objective lens brings the electron beam into focus (de-magnifies) on the specimen.

Objective lens (OL) aperture

This aperture is used to reduce or exclude extraneous (scattered) electrons. An optimal aperture
diameter should be selected for obtaining high resolution secondary electron images.

Scanning Coils

The scanning coils deflect the electron beam horizontally andvertically over the specimen
surface. This is also called rastering.

The scanning coils consist of two solenoids oriented in such a way as to create two magnetic
fields perpendicular to each other. Varying the current in one solenoids causes the electrons to
move left to right and that of in other solenoid forces these electron to move right to left and
downwards.

3. Detectors:
Secondary electron detector (SED) – Everhart-Thornley Detector

Due to the low energies of secondary electrons (SE)

(~2 to 50 eV) they are ejected only from near-surface layers.
Therefore, secondary electron imaging (SEI) is ideal for
recording topographical information. To attract (collect)
theselow-energy electrons, a small bias (often +/- ve
selectable but usually around +200 to 300V) is applied to the
cage at thefront end of the detector to attract the negative
electrons towards the detector. [If the cage is negatively
biased it functionsas a BS detector]. A higher kV (e.g. 7 to
12kV) is applied inside the cage i.e. to the scintillator, to
accelerate the electronsinto the scintillator screen.

Backscattered electron detector (BSD) – solid state diode detector

 The BSD is mounted below the objective lens pole piece and centered around the optic
axis. As the specimen surface isscanned by the incident electron beam, backscattered electrons
(BSE) are generated, the yield of which is controlled by thetopographical, physical and chemical
characteristics of the sample. Both compositional or topographical backscatteredelectron images
(BEI) can be recorded depending on the window of electron energies selected for image
formation.

4. Sample chamber
The specimen chamber is maintained at high vacuum that minimizes
scattering of the electron beam before reaching thespecimen. This is
important as scattering or attenuation of the electron beam will
increase the probe size and reduce theresolution, especially in the SE
mode. A high vacuum condition also optimizes collection efficiency,
especially of thesecondary electrons.

Specimen stage

The specimen holder is fixed to the specimen stage by the dovetail locating slide. The stage can
be moved manually alongthe X, Y (in the specimen plane), and Z directions (at right angles to
the specimen plane). The Z adjustment is also knownas the specimen height. The specimen stage
can also rotate continuously.

Sample preparation

The samples for SEM analysis require a coating of electrically conducting layer (e.g., gold,
graphite, platinum, etc.) particularly if they are electrically non-conducting. However, metal
samples do not require such coatings. Biological samples require fixation to preserve their
structure by incubation in a fixation such as formalin or glutaraldehyde and also require
dehydration to remove water.

Working:
Electrons are produced at the top of the column, accelerated down and passed through a
combination of lenses and apertures to produce a focused beam of electrons which hits the
surface of the sample. The sample is mounted on a stage in the chamber area. The position of the
electron beam on the sample is controlled by scan coils situated above the objective lens. These
coils allow the beam to be scanned over the surface of the sample. This beam rastering or
scanning, as the name of the microscope suggests, enables information about a defined area on
the sample to be collected. As a result of the electron-sample interaction, a number of signals are
produced. These signals are then detected by appropriate detectors.
 Transmission Electron Microscopy
Instrumentation
The main components are
➢ An electron source;
➢ A series of electromagnetic and electrostatic lenses to control the shape and trajectory of
the electron beam;
➢ Electron apertures.

Block diagram of TEM

Working:

The beam of electrons from the electron gun is focused into a small, thin, coherent beam by the
use of the condenser lens. This beam is restricted by the condenser aperture, which excludes high
angle electrons. The beam then strikes the specimen and parts of it are transmitted depending
upon the thickness and electron transparency of the specimen. This transmitted portion is focused
by the objective lens into an image on phosphor screen or charge coupled device (CCD) camera.
Optional objective apertures can be used to enhance the contrast by blocking out high-angle
diffracted electrons. The image then passed down the column through the intermediate and
projector lenses, is enlarged all the way. The image strikes the phosphor screen and light is
generated, allowing the user to see the image. The darker areas of the image represent those areas
of the sample that fewer electrons are transmitted through while the lighter areas of the image
represent those areas of the sample that more electrons were transmitted through.

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 which are passing
through the sample) to create an image. As a result, TEM offers valuable information on the
inner structure of the sample, such as crystal structure, morphology and stress state information,
while SEM provides information on the sample’s surface (topographical information) and its
composition.

SEM TEM
Type of electrons Scattered, scanning electrons Transmitted electron
High tension ~1 – 30 kV ~60 – 300 kV
Specimen thickness Any typically, <150 nm
Type of info 3D image of surface 2D projection image
of inner structure
Max. magnification Up to ~1 – 2 million times More than 50 million
times
Max. Field of View Large Limited
Optimal spatial resolution ~0.5 nm < 50 pm
Image formation Electrons are captured and Direct imaging on
counted by detectors, image on fluorescent screen or PC
PC screen screen with CCD
Operation Little or no sample preparation, Laborious sample
easy to use preparation, trained users
required