MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION -VTU

MODULE 5 -

Material Characterization Techniques and

Instrumentation
Introduction to materials: Nanomaterials and
nanocomposites. Principle,
construction and working of X-ray
Diffractometer, crystal size determination by
Scherrer equation, Principle, construction,
working and
applications of Atomic Force
Microscopy (AFM), X-ray Photoelectron Spectroscopy (XPS), Scanning Electron
Microscopy (SEM), Transmission Electron Microscopy (TEM).

INTRODUCTION TO MATERIALS: NANOMATERIALS AND

NANOCOMPOSITES.
DEFINITION:
Nano phase materials are the materials in which the atoms/grains size is in the
order of 1 to 100 nm and these items will not move away from each other.
Examples: zinc oxide, copper ferrous alloys, nickel, Pd, Pt.etc.

INTRODUCTION TO NANOMATERIALS:

Introduction Nanomaterials are cornerstones of nanoscience and

and
nanotechnology. Nanostructure science and technology is a broad and
interdisciplinary area of research and development activity that has been growing
explosively worldwide in the past few years. It has the potential for revolutionizing the
ways in which materials and products are created and the range and nature of
functionalities that can be accessed. It is already having a significant commercial
impact, which will assuredly increase in the future.

BASICS OF NANOMETRES:
We know materials are composed of atoms with different sizes, which has
movement with one another. Their exist a special clause of materials in which the
atoms do not move away from each other and its size will be in the order of 1 to
100 Nano meters. These new materials are called as Nano materials and the
developed technology is called nanotechnology.

Using this highly sophisticated latest technology, the Nano materials can be
formed from metals, ceramics, Polymers and even from liquids
 MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

EXPLANATION:
Nano material is one billionth of a metre. For comparison, single human hair is about
80000 nm or 80 micrometre, red blood cell is approximately 7ooo nm or 7 micrometre
wide and water molecule is almost point o.3nm across. Scientist and engineers on our days
interested in nanoscale materials, which is ranging from 1 to 10onm. At nanoscale, the

properties of materials are very difficult from those at larger scale. Therefore, the Nano world

is in between Quantum world and macro world. Nanoscience is concerned with the study of

phenomena and manipulation of materials at nm scales. Nanotechnology is the

design, production, characterization and application of structures, devices and Systems by
the nanometre scale.
controlling shape and size at

SPECIAL FEATURES OF NANO PHASE MATERIALS:

n addition to smaller grain size, nanomaterials contain less number (a few ten

thousands) of atoms. In contrast, the grain size of conventional materials vary

from a few microns to a few millimetres and contains several billions of atoms. These

basic differences make Nanomaterials unique and special. Nano materials contain a

very large number of grain boundaries, which may be 50% or more of the total volume
of the material. This unique microstructure makes this material to exhibit different
properties such as tremendous strength, formability toughness.
For example, crystalline copper is five times stronger than ordinary copper.
Further, the increased grain boundary increases magnetic and chemical properties.

INTRODUCTION TO NANOCOMPOSITES

materials that incorporate Nano-sized particles into a

Nanocomposites are

matrix of standard material. The result of the addition of nanoparlicles is a draslic

improvement in properties that can include mechanical strength, toughness and

electrical or thermal conductivity.

Composite structures whose characteristics dimensions are found at nanoscale.

Nanocomposite is a multiphase solid material where one of the phases has one, lwu or
three dimensions of less than 100 nanometres (nm) or structures having Nano-scale

material.
repeat distances between the different phases that make up the
The idea behind Nanocomposite is to use building blocks with dimensions in

nanometre range to design and create new materials with unprecedented flexibility
and improvement in their physical properties.
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

DIFFERENT FORMS OFNANOCOMPOSITES

Nanostructured material
The structures whose characteristics variations in design length is at the nanoscale.
Nano tubes or Carbon nanotubes
Carbon nanotube is a hollow tube made up of carbon of nanoscale diameter. In short,
It is represented as CNTs.
Carbon nanotubes are also called Bucky tubes. Nanotubes are formed by folding or
rolling two-dimensional graphite into a cylindrical shape structure. The particle size

is in the order of 109 m.

Nano Dots
Nanoparticles, which consists of homogeneous material, especially they are almost
spherical or cubical in shape.
Nano Rods
Nano structures which are shaped like sticks or rods with diameter in nanoscale and
their length very much longer.
Nanowires
Nanowires are Nano rods, which especially conduct electricity.
Fullerenes
A form of carbon having a large molecule sting of an Empty cage of 6o or more

carbon atoms.
Cluster
A collection of units atoms are reactive molecules up to about 50 units.

Colloids
Stable liquid phase containing particles of size 1 100onm range. A number of metals, alloys
intermetallic, ceramics, polymers as well as composites are synthesized in Nano form.

WHAT ARE NANOMATERIALS?

Nanoscale materials are defined as a set of substances where at least one

dimension is less than approximately 100 nanometres. A nanometre is one millionth

of a millimetre approximately 100,o00 times smaller than the diameter of a human

-

hair. Nanomaterials are of interest because at this scale unique optical, magnetic,
have the potential
electrical, and other properties emerge. These emergent properties
for great impacts in electronics, medicine, and other fields.
MODULE 5 MATERLAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

Mcro
mirn)

Solid-state Eneg
****
A SynhNeSIS

Adi aturization :

ASSEroeiy

1950 19 2010a 2030 2050

ear
Fig. 1. Evolution o fscience and technology and the future

CLASSIFICATION OF NANOMATERIALS

Nanomaterials have extremely small size which having at least one dimension
100 nm or less. Nanomaterials can be nanoscale in one dimension (eg. surface films),
two dimensions (eg. strands or fibres), or three dimensions (eg. particles). They can
exist in single, fused, aggregated or agglomerated forms with spherical, tubular, and
irregular shapes. Common types of nanomaterials include nanotubes, dendrimers
quantum dots and fullerenes. Nanomaterials have applications in the field of nano
technology, and displays different physical chemical characteristics from normal
chemicals (i.e., silver nano, carbon nanotube, fullerene, photo catalyst, carbon Nano,
and silica). According to Siegel, Nanostructured materials are classified as Zero
dimensional, one dimensional, two dimensional, three-dimensional nanostructures.

(a) (b (c) (d)

Fig. 3. Classification of Nanonmaterials (a) OD spheres and clusters, (b) 1D nanof+bers,

wires, and rocds, (c) 2D films, plates, and networks, (d) 3D nanomaterials.
 MODULE5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

Examples of Nanomaterials Nanomaterials (gold, carbon, metals, meta oxides

and alloys) with variety of morphologies (shapes) are depicted in Fig.

Au nanoparticle Buckminsterfullerene FePtnanosphere

64.0nm

Titanium nanotlower Silver nanocubes Sn02 nanoflower

Fig
PRINCIPLE, CONSTRUCTION AND WORKING OF X-RAY
DIFFRACTOMETER:

PRINCIPLE:

X-ray diffraction is based on constructive interference of monochromatic X-

rays and a crystalline sample. This law relates the wavelength of electromagnetic
radiation to the diffraction angle and the lattice spacing ina crystalline sample. These
diffracted X-rays are then detected, processed and counted.

CONSTRUCTION:

Consider a set of parallel atomic planes of the Crystal with Miller Indices
[hkl, such that the distance between the two successive planes is d. Let a
parallel beam of monochromatic X-rays of wavelength A be incident on the
Plane at a glancing angle 6 such that the incident rays lie in the plane of the
paper.
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION VTU

A'

B B

Crystal planes

Let AP and BQ be two parallel incident rays that are reflected from points
P and Q on the Crystal planes and travel along with PA' and QB' respectively. If
the path difference between APA' and BQB' is an integral multiple of ), there
will be constructive interference and a maximum will be observed.
Therefore, Braggs law is given as n^= 2d sine

WORKING:

The technique of single crystal x-ray erystallography has three basic steps.
The Crystal is placed in an intense beam ofX-rays usually of a single wavelength
of monochromatic X rays producing the regular pattern of deflections. The Crystal is
gradually rotate at previous reflections disappear and new ones appear the intensity
of every spot is recorded at every orientation of the Crystal.

Multiple data sets may have to be collected set of covering slightly more than
half a full rotation of the Crystal and type weekly containing of tens of thousands of
reflections.

Third step this data source or combined computationally with complimentary

chemical information to produce and refine your model of the arrangement of atom
within the Crystal the final refined model of the atomic
arrangement now called as
crystal structure.
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION-VTU

The first tees to after in an adequate crystal of the material under study which
is often most difficult. The Crystal should be sufficiently large typically larger than o.1
mm in all dimensions. The material should be pure in composition in structure, no
significant internal in perfections such as tracks for Twinning.

APPLICATION OF XRD:

XRD is non-destructive technique.

T o identify crystalline phases and orientation.
To determine structural properties train grain size face composition
orientation disorder transformation and thermal expansion extra.
T o measure thickness ofthin films multilayers.
To determine atomie arrangement.
Structure of crystals.
Polymer characterization state of anneal of metals.
Particle size determination.

ADVANTAGES:

XRD is there least expensive the most convenient and the most widely used
method to determine crystal structures.
.XRD techniques gives information about the structures of solids inmates ofthe
atoms that compose the solid.

.XRD permits non-destructive structural analysis.

DISADVANTAGES:

.XRD has size limitations.

I t is much more accurate for measuring large crystalline structures rather than
small ones.

X rays do not interact very strongly with lighter elements.

It is relatively low in sensitivity.
 MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

CRYSTAL SIZE DETERMINATION BY SCHERRER EQUATION:

The Scherrer equation, in X-ray diffraction and crystallography, is a formula

that relates the size of sub-micrometre crystallites in a solid to the broadening of a
peak in a diffraction pattern. It is often referred to, incorrectly, as a formula for particle
size measurement or analysis. It is named after Paul Scherrer. It is used in the
determination of size of crystals in the form of powder. The Scherrer equation can be

written as: D= Ka
(B cos )
D is the mean size of the ordered (crystalline) domains, which may be smaller
or equal to the grain size, which may be smaller or equal to the particle size

K is a dimensionless shape factor, with a value close to unity. The shape

factor has a typical value of about o.9, but varies with the actual shape of the

crystallite.

Ais the X-ray wavelength;

B is the line broadening at half the maximum intensity (full width at half
maximum -FWHM value in radians), after subtracting the instrumental line

broadening, in radians.

is the peak position Bragg angle.

The Scherrer equation is limited to Nano-scale crystallites, or more-strictly, the

cohcrently scattcring domain size, which can be smaller than the crystallite size (due to factors
mentioned below). It is not applicable to grains larger than about o.1 to o.21um, which

precludes those observed in most metallographic and ceramographic microstructures.

It is important to realize that the Scherrer equation provides a lower bound on
the coherently scattering domain size, referred to here as the crystallite size for
width
readability. The reason for this is that a variety of factors can contribute to the
of a diffraction peak besides instrumental effects and crystallite size; the most
important of these are usually inhomogeneous strain and crystal lattice imperfection.

The Scherrer equation is a widely used tool to determine the crystallite size of

polycrystalline samples. However, it is not clear if one apply it to large crystallite

can

diffraction.
sizes because its derivation is based on the kinematical theory of X-ray
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATiON - VTU

For large and perfect crystals, it is more appropriate to use the dynamical theory
of X-ray diffraction. Because of the appearance of polycrystalline nmaterials with a high
degree of crystalline perfection and large sizes,

The full width at half-maximum is then extracted and the crystallite size
is computed using the Scherrer equation. It is shown that for crystals with linear

absorption coefficients below 2117.3 em -1 the Scherrer equation is valid for

crystallites with sizes up to 600 nm.

It is also shown that as the size increases only the peaks at higher 20 angles give
good results, and if one uses peaks with 20> 60° the limit for use of the Scherrer
equation would go up to 1 un.

PRINCIPLE, CONSTRUCTION, WORKING AND APPLICATIONS OF

ATOMIC FORCE MICROSCOPY (AFM):
INTRODUCTON:

The atomic force microscope (AFM) is a type of scanning probe

microscope whose primary roles include mcasuring properties such as
magnetism, height, friction. The resolution is measured in a nanometer, which
is much more accurate and effective than the optical diffraction limit. It uses a
probe for measuring and collection of data involves touching the surface that
has the probe.

PRINCIPLE:
Deteotorund
The Atomic Force Microscope Feedback
Electronics
works on the principle measuring Photodiode

intermolecular forces and sees atoms by Lser

using probed surfaces of the specimen in

nanoscale.

CONSTRUCTION: Cantuliever
Sample Surface & Tip

Its functioning is enabled by three

of its major working principles that PZT

include Surface sensing, Detection, and

Imaging
MODULE S MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

1. The Atomic Force Microscope (AFM) performs surface sensing by using a

cantilever (an element that is made of a rigid block like a beam or plate,
that attaches to the end ofsupport, from which it protrudes makinga
perpendicularly flat connection that is vertical like a wall). The cantilever
has a sharp tip that scans over the sample surface, by forming an attractive
force between the surface and the tip when it draws closer to the sample
surface. When it draws very close making contact with the surface of the
sample, a repulsive force gradually takes control making the cantilever
avert from the surface.
2. During the deflection of the cantilever away from the sample surface, there

is a change in direction of reflection of the beam, and a laser beam detects

the aversion, by reflecting off a beam from the flat surface of the cantilever.
Using a positive-sensitive photo-diode (PSPD- a component that is based
on silicon PIN diode technology and is used to measure the position of the
integral focus of an incoming light signal), it tracks these changes of
deflection and change in direction of the reflected beam and records them.
3. The Atomic Force Microscope (AFM) takes the image of the surface
topography of the sample by force by scanning the cantilever over a section
of interest. Depending on how raised or how low the surface of the sample
is, it determines the deflection of the beam, which is monitored by the
Positive-sensitive photo-diode (PSDP). The microscope has a feedback
loop that controls the length of the cantilever tip just above the sample
surface, therefore, it will maintain the laser position thus generating an
accurate imaging map of the surface of the image.
WORKING:

Atomic Force Microseopes have several techniques for measuring force

interactions such as van der Waals, thermal, electrical and magnetic force
interactions for these interactions done by the AFM, it has the following parts
that assist in controlling its functions.
.Modified tips which are used to detect the sample surface and undergo
deflections
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

Software adjustments used to image the samples.

Feedback loop control - they control the force interactions and the tip

positions using a laser deflector. The laser reflects from the back of the
cantilever and the tip and while the tip interacts with the surface of the
sample, the laser's position on the photodetector is used in the feedback
loop for tracking the surface of the sample and measurement.
Deflection - The Atomic Force Microscope is constructed with a laser

beam deflection system. The laser is reflected from the back of the AFM
lever to the sensitive detector. They are made from silicon compounds with
a tip radius of about 1onm.
Force measurement - the AFM works and depends highly on the force

interactions, they contribute to the image produced. The forces are

measured by calculation of the deflection lever when the stiffness of the
cantilever is known. This calculation is defined by Hooke's law, defined as

follows:
F -kz, where F is the force, k is the stiffness of the lever, and z is the
distance the lever is bent.
APPLICATIONS:
This type of microseopy has been used in various disciplines in natural

science such as solid-state physics, semiconductor studies, molecular

engineering, polymer chemistry, surface chemistry, molecular biology, cell

biology, medicine, and physics.
Some of these applications include:

Identifying atoms from samples

.Evaluating force interactions between atoms
Studying the physical changing properties of atoms
Studying the structural and mechanical properties of protein complexes
and assembly, such as microtubules.
Used to differentiate cancercells and normal cells
and
Evaluating and differentiating neighbouring cells and their shape
cell wall rigidity.
MODULE S MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

Advantages:
1. Easy to prepare samples for observation
2. It can be used in vacuums, air, and liquids.

3. Measurement of sample sizes is accurate

4. It has a 3D imaging
5. It can be used to study living and non-living elements
6. It can be used to quantify the roughness of surfaces
7. It is used in dynamic environments.

Disadvantages:
1. It can only scan a single Nano sized image at a time of about 150x150nm.
2. They have a low scanning time, which might cause thermal drift on the

sample.
3. The tip and the sample can be damaged during detection.
4. It has a limited magnification and vertical range.

X-RAY PHOTOELECTRON SPECTROSCOPY (XPS):

INTRODUCTION:

The technique of X-Ray photoelectron Spectroscopy is also known as Electron

Spectroscopy for chemical analysis. X-ray photoelectron Spectroscopy is a type of
electron Spectroscopy it is an analytical technique to study the electronic
it is dynamic in atoms and molecules.

XPS was invented by Kai SIEGBAHN 1954 and received Nohel Prize in 1981. In
x-ray photoelectron spectroscopy, primary beam x-ray Photon, which are irradiated
on sample surface, the secondary beam (electron) obtained is then analysed. The
Secondary beam is made up of electrons. The spectrum of X-Ray photoelectron
spectroscopy consists plot of number of electrons or power of electron as a function of
energy i.e., kinetic energy or binding energy.
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

PRINCIPLE:

Due to the bombardment of X-Ray Photon on the sample surface K and L

electron are ejected which are further analysed by the analyser. Let us consider Eb,Eb
and Eb" are binding energy of lower energy levels inner core orbitals. Where Ev,
Ev'and Ev" are the energies of the valence shell electron.

The monochromatic x-ray Photon incident on the sample surface cell electron
abstract the energy from this x-ray Photon and get ejected in terms of electron. Kinetic
energy of the ejected electron is recorded by spectrometer and is given by

Ek= hv- Eb-

Where, Ek is kinetic energy of the ejected electron

hu - energy associated with incident Photon

Eb - binding energy ejected electron

-Work function ofthe instrument

CONSTRUCTION:

Hemispherical
Energy Analyzer
.
***~*~
*********
..
Elecuostatic field
**.

Collector
Slit
Electron Multipiler Lens System

crystal disperser
Photoelectrons Source Slit

Sample
Recorder
Sigmal processor
and detector
 INSTRUMENTATION VTU
TECHNIQUES AND
-

MODULE 5 MATERIAL CHARACTERISATION

The electron spectrometer made up of following components.

Source
Sample Holder

Analyserr
Detector
Processor And The Read-Out

SOURCE:

M is x ray tube
The simple x-ray Photon source for x-ray photoelectron spectra
equipped with magnesium or aluminium metal target. Monochromator crystal can

surface to
provide having bandwidth of o.3 electron volt. Much smaller spots
on a
also
be examined.

SAMPLE HOLDER:

slit of
Sample holder is located in between the source and the
entrance

from the
spectrometer. Crystal disperser selects the photon of known energy
source

and incident on the sample. The area inside the sample holder should be evacuated

within 105 Torr. Pressure to avoid contamination of the surface sample.

The gaseous sample for introduced into a sample compartment through a slit,
to provide a Pressure of 1012torr. If the pressure is higher than attenuation of electron

beam may take place, weaker signal may be obtained.

ANALYSER:

It is hemispherical in shape with very high electrostatic field is applied on

analyser. Pressure maintained inside the analyser is 105 torr. When the electron
enters, inlo lhe hemispherical analyser, it lravels in curved path and radius of
curvature depends upon magnitude of field and kinetic energy of the electron.
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

DETECTOR:
Pulses of electron
The electron channel multiplayer tube or
transducer are required of X-Ray photoelectron
Spectroscopy. When single electron pass through Glass tube coated with V/Pb
the electron multiplier tube it is converted into
number of electrons are pulses of electrons.

SIGNAL PROCESSOR AND READ OUT: Single electron

The function of signal processor is to amplify the signal and read out device
converts signal into spectrum.

APPLICATION OF XPS.

Identification of active sites

Determination of surface contamination on semiconductors
Study of oxide layers on metals
Analysis of dust on the sample
Determination of Oxidation State all the elements of periodic table can be
determined or identified except hydrogen and Helium, as they don't emit inner
core electron.

ADVANTAGES:

It is surface sensitive technique

Wide range of solid surface sample can be identified
Relative non-destructive

DISADVANTAGES:

It is very expensive
Slow and poorresolution power

Required high vacuum.

MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

SCANNING ELECTRON MICROSCOPE

Scanning electron microscope is an improved model of an electron microscope.
SEM is used to study the three dimensional image of the specimen.
PRINCIPLE:
When the accelerated primary electrons strikes the sample, it produces

secondary electron. These secondary electrons are collected by A positively charged

electron detector which in turn gives a three dimensional image of the sample.

CONSTRUCTION
It consists of an electron gun to produced high-energy electron beam. Magnetic
condensing lens is used to condense the electron beam and scanning coil is arrange in

between the magnetic condensing lens and the sample.

The electron detector scintillator is used to collect the secondary electrons and
converted into electrical signal. These signals can be fed into CRO through video
amplifier as shown in figure.

Electron gun

- Grid

Magnetic Condensing Lenses

Scanning OUUOOOT0
Coil Primary Electrons
Secondary CRO
elcctronns

Video
(Scintillator)
Collector Amplifier |i
Sample
Scan
Generator
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

WORKING:
Stream of electrons are produced by the electron gun and the primary electrons
are accelerated by the grid and anode. These accelerated primary electrons are made
to didn't on the sample through condensing lenses and scanning coil
This high-speed primary electron on falling over the sample produces low-
energy secondary electrons. The collection of secondary electrons are very difficult
because of their low-energy. Therefore, to collect the secondary electrons a very high
voltage is applied to the collector.
This is collected electrons produce skin t relations on photomultiplier tube or
detector and are converted into electrical signals. These signals are amplified by the
video amplifier and is fed to the CRO.
civil procedure the electron beam scan the sample from the left to right and
again from the left to right Etc.
Similar to read a book and the whole picture of the sample is obtained in the
CRO.
ADVANTAGES:
It can be used to examine specimens of large thickness
It has the large depth of focus
It can be used to get a three dimensional image of the object
Since the image can be directly viewed in the screen call details can be resolved
in a precise manner.
The magnification may be up to 300000 times greater than that of the size of
the object.
DISADVANTAGE:
The resolution of image is limited to about 10 - 20nm, hence it is very poor.

APPLICATIONS:
It is used to examine the structure of very large specimens in a three-
dimensional view.
Similar to the application of electron microscope this scanning electron
microscope also as application over various fields such as Biology Industries
engineering physics chemistry etc.
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION VTU

TRANSMISSION ELECTRON MICROSCOPE:

INTRODUCTION:
We know in scanning electron microscope the resolution of the image is limited only
upto 10 to 20 nm. This will not be useful to view the internal features of an atom or the

morphology of a sample of size saw o.2nm.

To examine the sample of size of 2 to NM the transmission electron microscope
can be used. In this microscope, the image is obtained by transmitting the electron
through the specimen.
PRINCIPLE:
Electrons are made to pass through the specimen and the image is formed in
the fluorescent screen there by using transmitted Beam (bright field image) on by
using the diffracted beam (dark field image).

cONSTRUCTION:
It consists of an electron gun to
produce electron. Magnetic condensing lens Electron
Gun
is used to condense the electron and is used
Magnetic
to adjust the size of the electron that fall onto condensin9
lens
the specimen. The specimen is placed in
between the condensing lens and objective
lens as shown in figure.
Specimen
The magnetic objective lens is used to
Magnetic
block the high angle difracted bcam the ,,
E E objective
lens
aperture is used to eliminate the diffracted
beam and in turn, it increases the contrast of V Aperture
the image.
,
.
Magnetic
The magnetic projector lens is placed projector
lens
above the fluorescent screen in order to
achieve high magnification. Can be recorded lmage Fluorescent
by using a fluorescent screen CCD charge Screen
coupled devices also.
MODULE 5 MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION -VTU

WORKING:
Stream of electrons are produced by the electron and is made to fall over the
specimen using magnetic condensing lens.
Based on the angle of incidence the Beam is partly transmitted and partly
diffracted as shown in figure. Both the transmitted Beam andthe diffracted beams are
recombined at the E-WALLED SPHERE of reflection, which encloses all possible
reflections from the Crystal are specimen satisfying the bragg's law image as shown in
figure. The combined image is called the phase contrast image.
In order to increase the intensity and the contrast of the image and amplitude
contrast image has to be obtained for stop this can be achieved only by using the
transmitting beam and does the diffracted beam has to be eliminated.
Now in order to eliminate the diffracted beam that beam is passed through the
magnetic objective lens and the aperture is shown in figure adjusted in such a way that
the diffracted image is illuminated. Thus, the final image being alone is passed
through the projector lens for further magnification. Find image is recorded in the
fluorescent screen or CCD this high contrast image is called Bright Field image. In
addition, it has to be noted that the bright field image obtained is purely due to the
elastic scattering non no energy change that is due to the transmitted beam alone
ADVANTAGES:
I t is used to examine the specimen of size of o.2 to 2 nm
The magnification is 10 lakh times greater than the size ofthe object
It has high resolution
.The resolution poweris 1Å to 2Å
We can get high contrast image due to both transmitted be bright field and the
diffracted be dark Beam.
DISADVANTAGES:
The specimen should be very thing.
Answers for
thestructural change during sample preparation
Three-dimensional image cannotbe obtained
I n case of biological samples, the electrons may interact with the samples,
which may even damage the sample.
MODULE S MATERIAL CHARACTERISATION TECHNIQUES AND INSTRUMENTATION - VTU

APPLICATIONS:
The main application oftransmission electron microscope is in nanoscience
nanotubes micro machines used to find the internal structures of
Nanomaterials.
It is used to find the two-dimensional image of very small biological cells
virus bacteria etc
It is used in thin film Technology metallurgy biochemistry microbiology etc
It is used to study the composition of paints papers fibres composite materials
alloys etc.