Module 5 Applied Physics for ME streams 2022 scheme

Module 5: Material Characterization and Instrumentation Techniques:

Introduction to nano materials: Nanomaterial and nanocomposites. Principle, construction and
working of X-ray Diffractometer, Crystallite size determination by Scherrer equation, Atomic
Force Microscopy (AFM) : Principle, construction, working and applications, X-ray
photoelectron spectroscopy(XPS), Scanning electron microscopy (SEM), Transmission electron
microscopy (TEM), Numerical Problems.

Pre requisites: Quantum Mechanics

Self-learning: Crystallites

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 Introduction to Nanomaterials:
Nanomaterials can be defined as materials possessing, at minimum, one external
dimension measuring 1-100nm. The definition given by the European Commission states
that the particle size of at least half of the particles in the number size distribution must
measure 100nm or below. Nanomaterials can occur naturally, be created as the by-
products of combustion reactions, or be produced purposefully through engineering to
perform a specialized function. These materials can have different physical and chemical
properties to their bulk-form counterparts.

 Classification of Nanomaterials:
Based on the number of nano dimensions nano materials are classified in to the
following types.
i) Zero-dimensional(0D) nanomaterials: In case of OD nanomaterials all three
dimensions (x, y, z) are at nanoscale, i.e., no dimensions are greater than 100 nm.
It includes nano spheres and nanoclusters.
ii) One-dimensional (1D) nanomaterials: Here, two dimensions (x, y) are at
nanoscale and the other is outside the nanoscale. This leads to needle shaped
nanomaterials. It includes nanofibres, nanotubes, nanorods, and nanowires.
iii) Two-dimensional (2D) nanomaterials: Here, one dimension (x) is at nanoscale
and the other two are outside the nanoscale. The 2D nanomaterials exhibit
platelike shapes. It includes nanofilms, nanolayers and nanocoatings with
nanometre thickness.
iv) Three-dimensional(3D) nanomaterials: These are the nanomaterials that are not
confined to the nanoscale in any dimension. These materials have three arbitrary
dimensions above 100 nm. The bulk (3D) nanomaterials are composed of a
multiple arrangement of nanosize crystals in different orientations. It includes
dispersions of nanoparticles, bundles of nanowires and nanotubes as well as
multinanolayers (polycrystals) in which the 0D, 1D and 2D structural elements
are in close contact with each other and form interfaces.

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The steel plate is bent into a circular path of radius 10 metres. If the plate section
be 120 mm wide and 20 mm thick, then calculate the Bending Moment and
maximum bending stress. Given Young’s modulus = 200 GPa

 Introduction to Nanocomposites:
Nanocomposites are materials that incorporate nanosized particles into a matrix of
standard material. The result of the addition of nanoparticles is to improve the properties
of the materials that can include mechanical strength, toughness and electrical or thermal
conductivity.
 Properties of Nanocomposites:
i) Mechanical properties including strength, modulus and dimensional stability
ii) Electrical conductivity
iii) Thermal stability
iv) Chemical resistance
v) Optical clarity
vi) Surface to volume ratio (SA:V)

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 Classification of Nanocomposites based on the Matrix

i) Polymer Matrix Nanocomposites:
 Polymer - Polymer Nanocomposite
 Polymer - Metall Nanocomposite
 Polymer - Ceramic Nanocomposite
 Polymer - Clay Nanocomposite
ii) Non-Polymer Matrix Nanocomposites:
 Metal Matrix and Metal Filler Nanocomposite
 Metal Matrix and Ceramic Filler Nanocomposite
 Ceramic Matrix and Ceramic Filler Nanocomposite

 Types of Nanocomposites:
The nanocomposites are of several types out of which the following are some of the types
i) Thermoplastic Nanocomposites: These re the composites in which nanofillers are
incorporated into a thermo-plasitic resins.
ii) Thermoset Nanocomposites: The incorporation of nanofillers in to the thermosets
are called Thermoset Nanocomposites which find application in mechanical and
tribological applications.
iii) These nanomaterials are mixed with elastomers. They main aim is to enhance the
mechanical, the electrical, as well as the wear performance. They include
inorganic or organic fillers of metallic, ceramic, or polymeric structure.
iv) Carbon nanotube nanocomposites: The carbon nanotube nanocompostes are
fabricated by dispersigcarbonnano tubes in metal matrix or polymer matrix.
v) Graphene and Graphene sheet based nano composites: Graphene-based
nanocomposites, derived from the decoration of graphene sheets with metal/metal
oxide nanoparticles, are emerging as a new class of exciting materials that hold
promise for many applications.
vi) POSS (Poly OligomericSilsequioxane) nanocomposite: Polyhedral
oligomericsilsesquioxanes (POSS) are a class of nanostructured silica-based
compounds that can be considered as an organic and inorganic hybrid material.

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vii) Zeolites and Composites: Zeolites are microporous, three-dimensional crystalline solids
of aluminium silicate. Zeolites have small openings of fixed size in them which allow
small molecules to pass through them easily but larger molecules cannot pass through
them. Geopolymer-zeolite composites may merge interesting properties of both
aluminosilicate materials.

 Applications of Nanocomposites:
Applications of Nanocomposites are;
 Thin-film capacitors for computer chips.
 Solid polymer electrolytes for batteries.
 Automotive engine parts and fuel tanks.
 Impellers and blades.
 Oxygen and gas barriers.
 Food packaging.

 X-ray Diffraction and Bragg’s Law

X-ray Diffraction:
The wavelength of X-Ray is comparable with the dimension of atoms. Thus crystals diffract X-
rays and the diffraction patter depends on the crystal structure.
Bragg Diffraction/Reflection:
Definition The condition for the constructive interference for the diffraction of X-rays from the
crystal surface is given Bragg’s Law. The diffraction satisfies the laws of reflection and hence
called Bragg Reflection.
Mathematical Form:
Consider an X-ray beam incident on a crystal at glancing angle "𝜃" with a lattice spacing "d". The
condition for constructive interference is given by Braggs’ Law
2𝑑 𝑠𝑖𝑛𝜃 = 𝑛𝜆
Here ’n’ is the order of diffraction.

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X-ray Diffractometer-XRD:
Introduction: XRD technique is used to examine the crystal structure of powder samples,
so it is also called as X-ray powder diffractometry
Principle:
X-ray diffractometer is based on the principle of Braggs’ Law The constructive
interference of monochromatic Xrays reflected by a crystalline sample is studied.
Construction:
 The main arrangements consist of X-Ray source, Specimen and Detector.
 The X-ray radiation generated by an X-ray tube is collimated by passing through
soller slits.
 Soller Slits are the arrangement of closely spaced thin metal plates in parallel to
prevent beam divergence.
 A divergent X-ray beam from the soller slits strikes the specimen.
 X-rays are diffracted by the specimen on the mount(turntable) and form a
convergent beam at the receiving soller slits before they enter a detector.
 The diffracted X-ray beam is passed through the monochromator before being
received by the detector.
 The monochromatic filter is used suppress wavelengths other than 𝐾𝛼 radiation.
 The detector and the turn-table are so coupled, if the crystal is rotated through an
angle 𝜃 then the detector turns through an angle 2𝜃.

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Working:

 The basic function of a diffractometer is to detect X-ray diffraction from materials

and to record the diffraction intensity in a range of the diffraction angle (2𝜃).
 Diverging X-ray beam is collimated and incident at a fixed angle on the sample
mounted on the turntable.
 The detector scans for the diffracted X-rays.
 The reflected X-rays are collimated and manochromatic X-rays from the
monochromator are collected by the detector.
 The intensity of the reflected X-ray beam as a function of 2𝜃 is recorded in a
computer.
 A plot of Intensity as a function of 2𝜃. thin-film XRD requires a parallel incident
beam, not a divergent beam as in regular diffractometry.
 The small glancing angle of the incident beam ensures that sufficient diffraction
signals come from a thin film or a coating layer instead of the substrate

Applications

 XRD is a non-destructive technique

 To identify crystalline phases and orientation.
 To determine structural properties: Lattice parameters (10 −4), strain, grain size,
expitaxy, phase composition, preferred orientation (Laue) order-disorder
transformation, thermal expansion.
 To measure thickness of thin films and multi-layers.
 To determine atomic arrangement.

 Determination of Crystallite Size - 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. The Scherrer equation is given by
𝑘𝜆
𝐵(2𝜃) =
𝐿 𝑐𝑜𝑠𝜃

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Here
 Peak width (B) or Full Width at Half Maximum (FWHM) is inversely
proportional to crystallite size (L).
 𝜆 is the wavelength of X-ray used.
 𝜃 is the glancing angle
 K Schrerrer Constant: The constant of proportionality, it depends on the how the
width is determined, the shape of thecrystal, and the size distribution.
 The most common values for K are: 0.94 for FWHM (fullwidth at half maximum)
of spherical crystals with cubic symmetry.

 Atomic Force Microscoph (AFM):

Introduction:
 The atomic force microscopy (AFM) is a subcategory of scanning probe
microscopy (SPM).
 It uses raster-scanning tip to measure surface properties such as the local height,
friction, electronic or magnetic properties, and construct a map of this data to
form an image.

Principle:

 The AFM measures the forces acting between a fine tip and a sample.

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 The tip is attached to the free end of a spring cantilever and is brought very close
to a surface.
 The inter-atomic potential developed between the tip and the sample at inter-
atomic separation results in attractive or repulsive forces.
 As the tip scans the surface of the sample, the force between the tip and the sample
varies which is sensed by the tip.
 The amount of force between the probe and the sample is dependent on the spring
constant of the cantilever and the distance between the probe and the sample
surface. This force can be characterized with Hooke’s Law, F= k x
here F = Force, k = spring constant, x = cantilever deflection.
 If the spring constant of cantilever (typically, 0.1 - 1 N/m) is less than surface,
cantilever bends and the deflection is monitored.

Working:

 As the tip travels across the sample surface the interaction with the asperities
(Surface Profile) causes up and down motion.
 These fluctuations are sourced by the interactions (electrostatic, magnetic,
capillary, Van der Waals forces) between the tip and the sample.
 The displacement of the Laser beam reflected from the backside of the tip traces
the surface profile.
 The laser and the photo-detector arrangement detects the position of the
cantilever.
 The vertical deflection measures the interaction forces while the horizontal
deflection measures the lateral forces.

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 Thus a three-dimensional image of the surface topography of the sample under a

constant applied force (as low as nano-Newton range) is obtained.

Uses:

 An AFM is used to achieve 3D topographical image of the surface on a nanoscale.

 It is a versatile and powerful tool for imaging and measuring small-scale objects
such as nanoparticles, single molecules, semiconductor devices and etc., at atomic
resolutions of 10−10𝑚 or one tenth of nanometre.

 X-ray Photoelectron Spectroscopy (XPS):

Introduction
 In the X-ray photo-electron spectroscopy (XPS) the sample under investigation is
bombarded with photons or charges for exciting the emission of photons and
charges.
 Highest available vacuum conditions are required for XPS experiments.
 Contamination is an important concern in XPS.
 it is a surface sensitive technique with a sampling depth of a few nano-meter.

Principle:

 Surface analysis by XPS involved irradiation of the sample by low-energy (and

mono-energetic) X-rays and the subsequent analysis of the energy of emitted
electrons. Typically used x-rays are K lines of Mg (1.2536 keV) and Al (1.4866
keV).
 The penetration depth of these photons in solids is limited to a few microns. Thus,
interactions take place between the incident photons are the surface atoms leading
to the photoelectric emission of electrons.
 The kinetic energy (K.E.) of the emitted electrons is expressed as 𝐾𝐸 = ℎ𝜈 − (𝐵.𝐸.
+ 𝜙𝑠). Here ℎ𝜈 is the energy of the photon, B.E. is the binding energy of the
atomic orbital from the electron is released, 𝜙𝑠 is the work-function of the
spectrometer.

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Construction and Working:

 A typical X-ray photoelectron spectrometer consists of an X-ray source, an

electron energy analyser, and a photo-electron detector.
 X-ray source emits monochromatized x-ray with a narrow line width of energy
ℎ𝜈 falls on the sample and photo electrons are emitted from the sample.
 The ejected photo-electrons are transferred to an electron energy analyzer (An
electrostatic hemispherical analyzer (HSA)) through the electron lens and
separated according to their kinetic energy.
 The separated electrons are subjected to channel electron multiplier which is
connected to Microcomputer.
 The transfer lens system retards the photo-electrons there by enhancing the
energy resolution of the analyzer (≤ 0.1 eV)

Uses of XPS:

 Elemental composition of the surface (top 1–10 nm usually).

 Empirical formula of pure materials.
 Elements that contaminate a surface.
 Chemical or electronic state of each element in the surface.
 Uniformity of elemental composition across the top surface (or line profiling or
mapping)
 Uniformity of elemental composition as a function of ion beam etching (or depth
profiling)

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 Scanning Electron Microscope (SEM):

Introduction:
Scanning Electron Microscope (SEM) is a type of electron microscope that scans
surfaces of microorganisms that uses a beam of electrons moving at low energy to
focus and scan specimens.

Principle:

 The Scanning electron microscope works on the principle of applying kinetic

energy to produce signals on the interaction of the electrons with the specimen.
 These electrons are secondary, backs-cattered, diffracted backs-cattered electrons
and auger electrons are used to view crystallized elements and photons.

Working:

 A SEM consists of a field emission electron gun and a series of electromagnetic

lenses and apertures. The electron beam emitted from an electron gun is
condensed to a fine probe for surface scanning.
 An electron gun—emits electrons that get accelerated by an applied voltage.
Magnetic lenses converge the stream of electrons into a focused beam, which then
hits the sample surface in a fine, precise spot.

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 The electron beam then scans the surface of the specimen in a rectangular raster.
 The user can increase the magnification by reducing the size of the scanned area
on the specimen.
 Detectors collect the backscattered and secondary electrons (SE). The
corresponding signals are measured and the values are mapped as variations in
brightness on the image display.
 The secondary electrons are more frequently used as read-out signal. They
highlight the topography of the sample surface: bright areas represent edges while
dark regions represent recesses.

Applications of SEM:

 For investigation of virus structure.

 3D tissue imaging.
 Insect, spore other microorganism or cellular component visualize.
 Geologist often use same to learn more about crystalline structure.
 Industries including Microelectronics, medical devices, food processing, all use
SEM as a way to examine the surface composition of component and products.

 Transmission Electron Microscope:

Introduction:

Transmission electron microscopes (TEM) are microscopes that use a particle beam of
electrons to visualize specimens and generate a highly-magnified image. TEMs can
magnify objects up to 2 million times.

Principle:

It is based on the principle of diffraction of electrons while transmitting through the thin
sample specimen.

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Construction and Working:

 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
fluorescent screen, photographic film, CCD Camera.
 A heated tungsten filament in the electron gun produces electrons that get focus
on the specimen by the condenser lenses.
 Magnetic lenses are used to focus the beam of electrons on the specimen. The
vacuum in the column tube allows electrons to produce a clear image without
collision with any air molecules which may deflect them.
 On reaching the specimen, the specimen scatters the electrons focusing them on
the magnetic lenses forming a large clear image, and if it passes through a
fluorescent screen it forms a polychromatic image.
 The denser the specimen, the more the electrons are scattered forming a darker
image because fewer electron reaches the screen for visualization while thinner,
more transparent specimens appear brighter.

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Applications of TEM:

 TEM is used in a wide variety of fields from Biology, Microbiology,

Nanotechnology, forensic studies.
 To visualize and study the cell structures of bacteria, viruses, and fungi and
also shapes and sizes of microbial cell organelles.
 To study and differentiate between plant and animal cells.
 It is also used in nanotechnology to study nanoparticles such as ZnO
nanoparticles.
 It is used to detect and identify fractures, damaged microparticles which
further enables repair mechanisms of the particles.

 Difference Between TEM and SEM The differences between the Transmission
Electron Microscope and Scanning Electron Microscope is as given below.

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Model Questions

1. Write a Note on Nanomaterials.

2. Explain the types of nanocomposites. Mention the applications of nanocomposites.
3. State and derive Braggs’law of X-ray Diffraction.
4. With a neat sketch explain the construction and working of X-ray Diffractometer.
5. Mention Scherrers Equation. Explain the calculation of crystallite size using
Scherrer’s equation.
6. Explain the construction and working of X-ray Photoelectron Spectrometer with the
help of a neat sketch.
7. Describe the construction and working of Scanning Electron Microscope using
necessary diagrams.
8. Explain the principle, Construction and working of Transmission Electron
Microscope with neat sketch.
9. Discuss the Scanning Tunneling Electron Microscope.
10. Distinguish between TEM and SEM.
11. Mention the applications of TEM and SEM.
12. State the applications of XRD and XPS.
13. Demonstrate STEM is based on the combined principles of TEM and SEM

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