Assignment-2

Name: Md Amanullah Saifee

Subject: characterization Technique
Paper code: PHDNT1-02

Submitted to: Dr. Manika Khanuja Ma’am

 Transmission electron microscopy (TEM)

1) Why are thin sections of specimens necessary in TEM?

a) Electrons are negatively charged

b) Electrons have a wave nature
c) Electrons have no mass
d) Electrons have a poor penetrating power.

2) Why TEM images have much higher resolution than images from light microscope?

a) TEM is much greater in size than light microscope

b) Electrons travelling as waves have wavelength much shorter than visible light
c) TEM can achieve greater magnification
d) The fluorescent screen of TEM can generate high resolution images

3) Which of the following is the correct pathway of electrons in the TEM?

a) Anode → electromagnetic lens system → sample → fluorescent screen

b) Anode → electromagnetic lens system → sample → electromagnetic lens system →
fluorescent screen
c) Cathode → electromagnetic lens system → sample → electromagnetic lens system →
fluorescent screen
d) Cathode → electromagnetic lens system → sample → fluorescent screen

4) What should be done right after the TEM column is shown to be evacuated?

a) Insert the sample holder

b) Further insert the sample holder
c) Remove the dummy holder
d) Shift the beam

5) Before loading the sample, the following softwares have to be turned on, except…

a) Electron gun tilt/shift

b) TEM imaging and analysis
c) Microscope user interface
d) Digital Micrograph
True/False:

1) Ultra-violet light is applied to the sample to warm up the sample. False

2) The main purpose of cutting extremely thin slices of samples is for better observation of
intracellular components instead of extracellular components. True

3) TEM cannot be used to examine live specimen. True

4) We should turn off the light before examination of sample using the fluorescent screen.
True

5) We need to do the alignment of the electron gun, beam and rotation centre every time we
use the TEM. False

Fill in the Blanks:

1) The gun requires the vacuum of the order of 10-9 Pa.

2) The specimen requires the vacuum of the order of 10-6 Pa.

3) Projection chamber and camera requires the vacuum of the order of 10-5 Pa.

Long type questions:

1) Explain the working principle of TEM

The transmission electron microscope is a very powerful tool for material science. A high
energy beam of electrons is shone through a very thin sample, and the interactions between
the electrons and the atoms can be used to observe features such as the crystal structure and
features in the structure like dislocations and grain boundaries. Chemical analysis can also be
performed. TEM can be used to study the growth of layers, their composition and defects in
semiconductors. High resolution can be used to analyze the quality, shape, size and density
of quantum wells, wires and dots.
An extremely thin sample is required for scanning in TEM from which electron beam is passed
through rendering its interaction with the sample as a result of which image is produced. This
image can be magnified and focused on the device used for imaging, like a fluorescent screen,
on a photographic film layer, or to be identified by a sensor like a CCD camera.
The TEM operates on the same basic principles as the light microscope but uses electrons
instead of light. Because the wavelength of electrons is much smaller than that of light, the
optimal resolution attainable for TEM images is many orders of magnitude better than that
from a light microscope. Thus, TEMs can reveal the finest details of internal structure - in
some cases as small as individual atoms.

Figure 1 - General layout of a TEM describing the path of electron beam in a TEM (Taken from
JEOL 2000FX Handbook)
Figure 2 - A ray diagram for the diffraction mechanism in TEM
Figure 3: Instrumentation of TEM.
Imaging
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.

Diffraction
Figure 2 shows a simple sketch of the path of a beam of electrons in a TEM from just above
the specimen and down the column to the phosphor screen. As the electrons pass through
the sample, they are scattered by the electrostatic potential set up by the constituent
elements in the specimen. After passing through the specimen, they pass through the
electromagnetic objective lens which focuses all the electrons scattered from one point of
the specimen into one point in the image plane. Also, shown in fig 2 is a dotted line where the
electrons scattered in the same direction by the sample are collected into a single point. This
is the back focal plane of the objective lens and is where the diffraction pattern is formed.

2) Describe various types of pumps used to achieve vacuum?

The main vacuum system on a typical electron microscope has a roughing pump, a diffusion
pump and an ion pump.

The roughing pump is a large mechanical contraption which is easy to hear. It is used to pump
the chamber from 'air' (atmospheric pressure) when necessary, to pump the specimen
transfer chamber (also from atmospheric pressure), and to back the diffusion pump. Because
it is used to do so many things, it is usually attached to a 'roughing manifold' - a pipe with
lots of other pipes coming off it. By opening and closing various valves off the roughing
manifold, the roughing pump can be switched from one role to another.

The diffusion pump is usually positioned at the bottom of the column, near the back, and its
front end is used to pump the viewing chamber and the photographic film casement. There
is usually a large empty volume between the back end of the diffusion pump and the roughing
manifold, so that when the microscope is being used, the roughing pump can be switched off
(it creates a lot of vibration).
Vacuum system is employed in electron microscopes for 4 reasons:
As electrons are readily scattered, electrons have a mean free path of ~1cm at atmospheric
pressure; however, at 10-6 Pa they can have mean free path as high as 6.5m.
The purpose of the vacuum system is to provide insulation between the filament of both
anode and cathode as well as in the region around the field emitters, thus hampering
undesirable discharge of the electron gun.
In order to inhibit the oxidation and ‘burning out’ of the filament, oxygen is eliminated
around the filament.
Samples contamination is decreased by reducing the interaction amongst electron beam and
molecules of the gas.

Various microscope parts are differently vacuumed as per their requirements. The gun
requires 10-9 Pa vacuum, while the specimen requires 10-6 Pa and the projection chamber plus
camera requires 10-5 Pa.
Vacuums can be categorized as: rough (100 - 0.1 Pa), low (10-1 - 10-4 Pa), high (10-4 - 10-7 Pa),
or ultrahigh (< 10-7 Pa).

Figure 4: typical vacuum system for a TEM. RP-rotary pump, TMP-turbo molecular pump, IGP-
ion getter pump, ODF-oil diffusion pump.