TERM PAPER

OF
MECHANICS
(PHY 101)

TOPIC : XRD AND ITS APPLICATIONS

Submitted To: Submitted By:

Mrs. Jyoti Rajput Shivam S Verma
B.Tech-M.Tech (ME)
Section: D4003
Roll No. : B 72
ACKNOWLEDGEMENT

I Shivam S Verma, student of B.Tech. –

M.Tech. (ME) (Section – D4003 ) express
my deep gratitude to my teacher Mrs. Jyoti
Rajput . I m very thankful to her for support
that led me to the completion of this term
paper.
I m thankful to my parents who
encouraged me and provided me all the
necessary resources that had made possible
for me to be able to accomplish this task.
I also thank all my friends who
assisted me in completing this work.
Contents:
1. Introduction

2. X-Rays

3. History

4. How it works?

5. X-ray Diffraction and Bragg’s Law

6. How are Diffractions Patterns Made?

7. X-Ray diffraction techniques

8. Applications
 range 120 eV to 120 keV. They are shorter
Introduction: in wavelength than UV rays and longer than
gamma rays.

X-rays from about 0.12 to 12 keV (10 to

You have likely seen diffraction before. 0.10 nm wavelength) are classified as "soft"
For example if you look at a CD when X-rays, and from about 12 to 120 keV (0.10
exposed to white light you can see it to 0.01 nm wavelength) as "hard" X-rays,
diffracted into varies wavelengths of due to their penetrating abilities.
color. The pits (or grooves) in the CD
are the regularity of the material that
causes the diffraction.
Hard X-rays can penetrate solid objects, and
their most common use is to take images of
the inside of objects in diagnostic
radiography and crystallography.By
contrast, soft X-rays can hardly be said to
penetrate matter at all.

Diffraction can occur when any

electromagnetic radiation interacts with a
periodic structure. The repeat distance of the
periodic structure must be about the same
wavelength of the radiation. For example,
light can be diffracted by a grating having
scribed lines arranged on the order of the
wavelength of light.

X-Rays:
X-radiation (composed of X-rays) is a form
of electromagnetic radiation. X-rays have a
wavelength in the range of 0.01 to 10
nanometers, corresponding to frequencies in
the range 30 petahertz to 30 exahertz (3 ×
1016 Hz to 3 × 1019 Hz) and energies in the
 Diffraction occurs when waves pass over an
object that has approximately the same
repeat distance as the wave. Thist is seen
when light is passed through a grating with
repeat distances of approximately 1000
Angstroms. X-rays were thought to be much
smaller than light, having a size of
approximately 1 Angstrom – about the same
as the distance between atoms.
In 1910 scientists working with Max van
Laue conducted an experiment to see if x-
rays could be diffracted by a crystal of
sodium chloride. They were successful in
getting a diffraction pattern captured on
photographic film. The structure of the
crystal lattice of sodium chloride was no
longer a secret.

In 1912 W.L. Bragg, working with his

father, determined the mathematical
History: relationship between the angle of diffraction,
the wavelength, and the distance between
X-rays were discovered in 1895 by Wilhelm layers of atoms in a crystal. If the
Roentgen while he was experimenting with wavelength was known, and the angle of
a Crookes tube. A Crookes tube is a vacuum diffraction was known, the distance between
tube through which a high voltage is passed the atom in a crystal could be determined
causing the streaming of electrons between according to the following equation:
the cathode and anode. Fluorescent
materials paced in the tube glowed when the
current was present. Roentgen noticed that a
card painted with fluorescent material that nλ = 2dsinθ
was laying on the table near the tube,
glowed when the tube was turned on. The where
card would glow even if the Crookes tube n = an integer,
was covered in black paper . It also didn’t
matter if the fluorescent coated side of the λ = the wavelength of the x-ray
card was placed up or down. Roentgen soon
discovered that if a hand was placed d = the distance between atoms in
between the X(unknown)-rays and a angstroms, Ǻ
fluorescent screen, shadows of the bones of
the hand could be discerned. This discovery θ = the diffraction angle in degrees
was immediately applied to the medical field
for diagnostic purposes.
By knowing the distance and angles between monochromatized by passing through a
the atoms of a substance, the structure of the graphite crystal. The scintillation counter
crystal could be determined. which measures x-ray intensity is mounted
to an angle measuring device called a
goniometer. The goniometer is motorized
Today X-ray diffraction is used to identify and is controlled by a computer. Thus the
corrosion products on the surface of a metal angle and intensity of the diffracted x-ray
as well as the pigments used in wall beam are measured according to the
paintings. XRD is used by many museums parameters set in the computer. (The
to evaluate paintings to determine their age diffractometer records the x-ray intensity as
and artist by the pigments that were popular a function a 2-theta angle. Therefore to find
at a given time. the diffracted angle to use in Braggs
It is almost non-destructive in regards to the equation, you must divide the angle by 2.)
sample being analyzed.
In nanotechnology, XRD is a useful tool
since x-rays are in the nano-scale. At the Electronic signals from the goniometer and
University of Tulsa it is used to evaluate the scintillation counter are sent to a computer
deposition of one metal onto the surface of a where they are translated before being
substrate. displayed on an output device such as a
strip chart or computer monitor where a
diffraction pattern is recorded. A diffraction
pattern is the fingerprint of a mineral or
other sample. It records the x-ray intensity
at various 2 theta angles. By dividing the
angle from the strip readout by two and
How it Works? applying Braggs Law, we can now calculate
the

A high voltage is applied across electrodes

causing electrons to be propelled towards a
metal target – the anode. Electrons
bombarding the metal cause the expulsion of
x-rays with a wavelength characteristic of
the metal. Copper is very commonly used
metal. X-rays with a wavelength of 1.54Ǻ
are emitted from copper. The x-rays are
passed through a slit that collimates the x-
rays before they reach the sample chamber.
Upon hitting the sample the x-rays are
diffracted in all directions. Both distance between the atoms in the crystal.
constructive and destructive interference The smaller the angle of diffraction the
occur. Constructive interference occurs larger the distance between atoms. The
where the waves are in phase with one peaks are prioritized according to their
another. The waves can be detected by a height from tallest to shortest. By
scintillation counter after they are consulting a handbook of mineral diffraction
patterns, the sample can be identified.
 The relationship describing the angle at
which a beam of X-rays of a particular
wavelength diffracts from a crystalline
surface was discovered by Sir William H.
Bragg and Sir W. Lawrence Bragg and is
known as Bragg’s Law

Figure 1 2dsinθ= nλ

λ = wavelength of the x-ray

Quartz Diffractogram - TU θ = scattering angle

n = integer representing the order of the

system diffraction peak.

d = inter-plane distance of (i.e atoms, ions,

molecules)

Figure 2: How are Diffractions

Patterns Made?

When X-rays are scattered from a

crystalline solid they can constructively

X-ray Diffraction and

Bragg’s Law :

X-rays have wavelengths on the order of

a few angstroms (1 Angstrom = 0.1 nm).
This is the typical inter-atomic distance
in crystalline solids, making X-rays the
correct order of magnitude for diffraction
of atoms of crystalline materials.
interfere, producing a diffracted beam.
 structural information on unknown
materials. Powder diffraction is also
a common method for determining
strains in crystalline materials. An
effect of the finite crystallite sizes is
seen as a broadening of the peaks in
an X-ray diffraction as is explained
by the Scherrer Equation.
X-ray diffraction
techniques:
X-ray diffraction yields the atomic structure • Thin film diffraction and grazing
of materials and is based on the elastic incidence X-ray diffraction may be
scattering of X-rays from the electron clouds used to characterize the
of the individual atoms in the system. The crystallographic structure and
most comprehensive description of preferred orientation of substrate-
scattering from crystals is given by the anchored thin films.
dynamical theory of diffraction.

• Single-crystal X-ray diffraction is a

technique used to solve the complete • High-resolution X-ray diffraction is
structure of crystalline materials, used to characterize thickness,
ranging from simple inorganic solids crystallographic structure, and strain
to complex macromolecules, such as in thin epitaxial films. It employs
proteins. parallel-beam optics.

• Powder diffraction is a technique • X-ray pole figure analysis enables

used to characterise the one to analyze and determine the
crystallographic structure, crystallite distribution of crystalline
size (grain size), and preferred orientations within a crystalline thin-
orientation in polycrystalline or film sample.
powdered solid samples. Powder
diffraction is commonly used to
identify unknown substances, by
comparing diffraction data against a • X-ray rocking curve analysis is used
database maintained by the to quantify grain size and mosaic
International Centre for Diffraction spread in crystalline materials.
Data. It may also be used to
characterize heterogeneous solid
mixtures to determine relative
abundance of crystalline compounds
and, when coupled with lattice
refinement techniques, such as
Rietveld refinement, can provide
 X-Ray Diffraction (XRD) uses the
"fingerprint" of a crystalline material to allow
identification and quantification of unknown
phases in a mixture. It is commonly used in the
engineering, geological and materials sciences
Applications: for applications such as corrosion studies,
material fabrication, analysis of combustion
products, mineral identification and
X-ray diffraction is a very important method to
determination of lattice parameters.
characterize the structure of crystalline
material. The technique can typically be used
Rapid identification of unknowns is possible
for the lattice parameters analysis of single
using search/match software available at the
crystals, or the phase, texture or even stress
unit and quantification of the various phases is
analysis of polycrystalline materials (like
also possible. Information about crystal
powders). The technique is widely used in
structure, crystallite size and residual strain
research and development applications and its
may also be obtained.
use for production or quality control issues is
also growing, benefiting from developments in
Samples may be in solid or powder form, and
hardware and software for high throughput
the technique is non-destructive . A thirty five
capability.
position sample changer is available to allow
overnight, unattended operation of the XRD
Most of the applications of X-ray
diffractometry require a beam with well
defined spatial and spectral characteristics. X-
ray optics is a critical component for obtaining
the required beam specifications at the sample.
Multilayer X-ray optics are now widely used in
X-ray diffraction due to their balanced
performance in terms of divergence, spectral
purity, and flux.
References:
Jones, E.R. and Childers, R.L. Contemporary College Physics 2nd Edition, Addison Wesley
Publishing Co., 1993.

USGS Open-File Report 10-041; A Laboratory Manual for X-ray Diffraction

http://pubs.usgs.gov/of/of01-041/index.htm

History
www.rigakumsc.com/xrd/about.html

basic information and current applications

www.thebritishmuseum.ac.uk/science/techniques/sr-tech-xrd.html

Concise, well written explanation of how the XRD works

www.geosci.ipfw.edu/XRD/techniqueinformation.html

Cornell, Winton. Power Point Presentation on XRD

www.ens.utulsa.edu/nanomaterialsworkshop/

A tutorial on XRD
http://www.matter.org.uk/diffraction/x-ray/default.htm