STUDY OF X-RAY DIFFRACTION

A dissertation submitted in partial fulfilment of the requirements for the degree of Bachelor/Master
in Science

IN PHYSICS

Submitted

by PUSHPENDRA KUMAR

Under the supervision of

DR. AMRITRAJ MAHTO

Assistant Professor

University Department of Physics

Shyama Prasad Mukherjee University, Ranchi

2023

UNIVERSITY DEPARTMENT OF PHYSICS

DR. SHYAMA PRASAD MUKHERJEE UNIVERSITY, RANCHI

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 Acknowledgement
I would like to express my special thanks and gratitude to my physics
teacher “DR. AMRITRAJ MAHTO” for his guidance and suggestion in
completing this project. The completion of this project was possible
under his guidance and support. Then, I would like to thank my
H.O.D sir ANUPAM KUMAR who gave me the golden opportunity to
do this wonderful project on the topic- “STUDY OF X-RAY
DIFFRACTION”. Secondly, I would also like to thank my friend and
family without them I would not have been able to complete this
project. Lastly, I like to thank all my supporters who have motivated
me to fulfil this project on time.

Thank You

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 CERTIFICATE
This is to certify that the research work reported in this thesis is entitled
“STUDY OF X-RAY DIFFRACTION” is an authentic record of the research
work independently carried out by Mr. PUSHPENDRA KUMAR,
Registration Number DSPMU2020000662, Roll Number 20B151893 at the
University Department of Physics, Dr. Shyama Prasad Mukherjee University,
Ranchi, Jharkhand, India under my guidance and supervision, in fulfilment of
the requirements for the award of a Master/Bachelor of Science degree at Dr.
Shyama Prasad Mukherjee University, Ranchi and further that no part thereof
has been presented elsewhere for award of any other degree or diploma as per
best of my knowledge. I further certify that he/ She inhabit good moral
character and is a fit and proper person for the award of Master/Bachelor of
Science degree of Dr. Shyama Prasad Mukherjee University, Ranchi.
DR. AMRITRAJ MAHTO
(Supervisor)
Department of Physics
Dr. Shyama Prasad Mukherjee University,
Ranchi, Jharkhand

Place....................
Date.....................

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 ,
Abstract

In this dissertation we found that X-ray diffraction (XRD) is a powerful tool

widely used in research and industry. While XRD is usually well known for
qualitative and quantitative analyses of crystalline phases in materials, far more
information can be obtained from a careful analysis of the diffraction patterns or
by using specific XRD settings: i.e., characterization of solid
solutions, crystallite size and shape, crystal orientation, internal elastic
strains/stresses at different levels, effect of temperature, close surface
characterization etc.

The objectives of this paper are first to summarize some basic principles of X-
ray diffraction, and next to provide some examples of applications of XRD in
the field of ceramics materials.

First time the X ray diffraction is observed in crystal by Max Von Loue in 1912
after that the British physicists William Henry Bragg and William Lawrence
Bragg in 1913 successfully performed X -ray diffraction experiment.

This study used X-ray diffraction to investigate the crystal structure of a new
material synthesized by a novel chemical method. The material was found to
have a complex crystal structure with multiple phases and significant disorder.

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Analysis of the diffraction pattern revealed a number of peaks corresponding to
different crystal planes, which were used to determine the lattice parameters and
symmetry of the crystal. The results suggest that the material has potential
applications in electronic and optical devices due to its unique structure and
properties.
Overall, this study demonstrates the utility of X-ray diffraction as a powerful
tool for investigating the structure of complex materials.

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 Introduction

X-ray:-

X-rays are a type of electromagnetic radiation with wavelengths shorter than

that of visible light. They have high energy and can penetrate through many
materials, including soft tissue and bones. X-rays are produced when high-
energy electrons collide with a target material, releasing energy in the form of
photons.

Soft X-rays and hard X-rays are two types of X-rays that differ in their energy
level and wavelength.

Soft X-ray:-

Soft X-rays have lower energy levels and longer wavelengths than hard X-rays.
They are typically used for imaging soft tissues, such as organs, and for
studying electronic and molecular structures. Soft X-rays are absorbed by air
and cannot penetrate dense materials like bones or teeth.

Hard X-ray:-

hard X-rays have higher energy levels and shorter wavelengths than soft X-rays.
They can penetrate through dense materials like bones and teeth, making them
useful for imaging internal structures of the body. Hard X-rays are also used in

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radiation therapy to treat cancer. However, they can be harmful to living tissues
and require careful handling and shielding to prevent radiation exposure.

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Representation of soft X-ray and hard X-ray in a
graph :-

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Difference between soft X-ray and hard X-ray:-

Soft X-ray Hard X-ray

1.Those of larger wavelengths are called 1.Those of shorter wavelengths are called
soft X-ray. Hard X-ray.

2.Have law penetrating power. 2.Have high penetrating power.

3. Have less energy . 3. Have more energy .

4. Application: Mammography 4. Application: It is used to image

Inside of objects such as medical
Radiography.
5. Photon Energy: Lower 5. Photon Energy: Higher above to 10 KeV.

6. Wavelength: 100 to 1Pm. 6. Wavelength 10 to 0.1mm.

7. Frequency: 30 to 3000 PHZ 7. Frequency: 3 to 300 EHZ.

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 Production of X-ray

X-rays are produced when high-energy electrons collide with a target material,
typically a metal such as tungsten or molybdenum. This collision causes the
electrons in the target material to be excited and emit X-rays.

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There are two main methods for producing X-rays:

1. X-ray Tubes:

X-ray tubes are the most common method used to produce X-rays. They
consist of a vacuum-sealed glass tube that contains a cathode (a negatively
charged electrode) and an anode (a positively charged electrode).
When a high voltage is applied to the electrodes, a stream of electrons is
emitted from the cathode and accelerated towards the anode. The electrons
collide with the target material on the anode, producing X-rays.

2. Particle Accelerators:

Particle accelerators are used in some specialized applications, such as in

research and medical imaging.
In this method, high-energy electrons are produced using an accelerator and
directed towards a target material, producing X-rays when they collide with
the target.

Regardless of the method used, the production of X-rays involves high levels of
energy and can be potentially hazardous. Proper safety precautions must be
taken when handling X-ray equipment and materials.

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Definition of X -ray diffraction:-

X-ray diffraction is a technique used to study the atomic and molecular structure
of materials. It involves shining a beam of X-rays at a sample and measuring
how the X-rays scatter and diffract off the atoms in the sample. The scattered X-
rays create a unique diffraction pattern that can be analyzed to determine the
arrangement of atoms in the sample.

X-ray diffraction is widely used in materials science, chemistry, and physics to

study the crystal structure of materials such as minerals, metals, ceramics, and
biological molecules.

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It is also used in industry for quality control of materials, in geology for
identifying mineral samples, and in medicine for imaging bones and tissues.

X-ray diffraction can provide detailed information about the composition,

purity, and crystallinity of a material, making it a valuable tool in many X-ray
diffraction (XRD) is done to determine the atomic and molecular structure of a
crystalline material.

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 History of X -ray diffraction

 X-ray diffraction is a powerful technique used to study the structure of

materials at the atomic and molecular level.

(Wilhelm Conrad
Roentgen)

The history of X-ray diffraction can be traced back to the discovery of X-

rays by Wilhelm Conrad Roentgen in 1895.

Soon after Roentgen's discovery, physicists and chemists began to

explore the properties of X-rays and their interaction with matter.

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  In 1912, the German physicist Max von Laue proposed that X-rays could
be diffracted by crystals, and he performed experiments that confirmed
his hypothesis.

(Max von Loue)

Von Laue's work laid the foundation for the development of X-ray
crystallography, a technique that uses X-rays to determine the three-
dimensional structure of crystals.

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  The first successful X-ray diffraction experiment was performed by the
British physicists William Henry Bragg and William Lawrence Bragg in
1913.

They used a crystal of sodium chloride to diffract X-rays and observed a

diffraction pattern on a photographic plate.
They then used the diffraction pattern to determine the arrangement of
atoms in the crystal.

 In the following years, X-ray diffraction became an important tool for

studying the structure of materials.

In 1929, the American chemist Linus Pauling used X-ray diffraction to

determine the structure of the mineral molybdenite, the first time that the
technique had been used to determine the structure of a non-organic
material.

Pauling later went on to use X-ray diffraction to study the structures of

many other materials, including proteins.

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  During World War II, X-ray diffraction played a crucial role in the
development of radar and the atomic bomb. After the war, X-ray
diffraction became increasingly important in fields such as materials
science, chemistry, and biology.

 In 1962, the British chemist Dorothy Hodgkin used X-ray diffraction to

determine the structure of insulin, a milestone in the development of the
field of structural biology.

 Today, X-ray diffraction continues to be an important technique for

studying the structure of materials.

It is used in fields such as materials science, chemistry, physics, and

biology to study the structure of a wide variety of materials, from metals
and minerals to proteins and DNA.

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 Bragg’s Law

What is Bragg’s Law?

Bragg’s law is the special case of law diffraction which determines the angle of
coherent and incoherent scattering from a crystal lattice.
When a x-rays are incident on the particular atom, they make electronic cloud
move like an electromagnetic waves, the movement of the charge radiates wave
again with similar frequency, slightly bloused due to different effects, and this
phenomenon is known as Rayleigh scattering. Basically this law explain the
relationship between an x-ray shooting and its reflection from a crystal surface.

Bragg’s Law States The Following:-

When the x-ray incident on to a crystal surface, it angle of incidence θ with the
same angle of scattering θ . And when the path difference, d is equal to a whole
number n, of wave length λ, constructive interference will occur .

The extract process take place upon scattering neutron wave via nuclei or a
coherent spin interaction with an isolated electron. These wave field that are re-
emitted interfere with other destructively or constructively. Creating a
diffraction pattern on a film or detector. The diffraction analysis is the resulting
wave interference, and this analysis is known as Bragg diffraction.

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Bragg Equation:-

Acc. To Bragg Equation:-

nλ = 2d sinΘ

Therefor According to the equation of Bragg’s law:-

 The equation Explain why the faces of crystal reflect x-ray beam at
particles angle of incidence   (Θ, λ).

 The variable d indicates the distance between the atomic layer, and the
variables d indicates the distance between the atomic layers, and the
variable λ specifics the wavelength of the incident x-ray beam and n as an
integer.

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This observation illustrates the x-ray wave interface called x-ray diffraction
(XRD) and proof of the atomic structure of the crystals.

Bragg was also awarded to Nobel Prize in physics for identifying crystal
structure starting with Nacl, Zns and diamond.

In addition to understand the structure of every state of matter by any beam, e.g
– ions, protons, electrons, neutron, with a wavelength similar to length between
the molecular structure, diffraction was developed.

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Derivation Of Bragg’s Law :-

Consider the following figures of beams in which the phase of the beam
coincide when the incident beam is equal to the reflecting angle. The incident
beam are parallel to each other. Until they reach point Z.

When they are at point Z, they strike the surface and travel upwards. At point B,
the second beam scatters AB+BC is the distance travelled by the second beam.

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The extra distance is known as the integral multiple of the wavelength.

nλ = AB + BC
We also know that AB = BC
nλ = 2AB (equation 1)
d is the hypotenuse of the right triangle Abz. Ab is the opposite of the angle θ.
AB = d sinθ (equation 2)
Substituting equation 2 in equation 1
nλ = 2d sinθ

The above equation is Bragg’s law expression.

Application Of Bragg’s Law:-

There are numerous applications of Bragg’s law in the field of science. Some
common applications are given in the points below.
 In the case of XRF (X-ray fluorescence spectroscopy) or WDS
(Wavelength Dispersive Spectrometry), crystals of known d-spacings are
used for analyzing crystals in the spectrometer.

 In XRD (X-ray diffraction) the inter-planar spacing or d-spacing of a

crystal is used for characterization and identification purposes.

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Bragg’s Diffraction:-

Bragg’s diffraction was first proposed by William Henry Bragg and William
Lawrence Bragg, in 1913. Bragg’s diffraction occurs when a subatomic particle
or electromagnetic radiation waves have wavelengths that are comparable to
atomic spacing in a crystal lattice.

Bragg’s law Conclusion:-

The concluding ideas from Bragg’s law are:

 The diffraction has three parameters i.e, the wavelength of X rays,λ

 The crystal orientation defined by the angle θ
 The spacing of the crystal planes, d.
The diffraction can be considered to occur for a given wavelength and set of
planes. For instance, changing the orientation continuously, i.e., changing θ
until Bragg’s Law is satisfied.

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 X -ray diffraction by crystal

The equipment used in X-ray diffraction includes:-

 X-ray Source:

A high-energy X-ray source, such as a copper or molybdenum anode

tube, is used to generate a beam of X-rays.

 Collimator:

The collimator is used to limit the width of the X-ray beam and ensure
that the beam is parallel.

 Monochromator:

The monochromator is used to select a specific wavelength of X-rays to

use in the experiment. This ensures that only X-rays of the desired
wavelength are used, which is necessary for accurate analysis.

 Sample Holder:

The sample holder is used to hold the sample in place and ensure that it
remains stationary during the experiment.

 Detector:

The detector is used to measure the intensity of the diffracted X-rays. The
most common type of detector used in XRD is the scintillation detector,
which detects X-rays by producing flashes of light.

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  Data Acquisition System:

The data acquisition system is used to collect and process the data
obtained from the detector. The data is typically displayed as a
diffractogram, which shows the intensity of the diffracted X-rays as a
function of the diffraction angle.

 Computer:

The computer is used to control the X-ray source, collimator,

monochromator, and detector, as well as to collect and analyze the data
obtained during the experiment.

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 Procedure for X ray diffraction by crystal

Here is a general procedure for performing X-ray

diffraction:

 Sample preparation:

The first step is to prepare the sample for analysis. This involves grinding the
sample into a fine powder and spreading it uniformly on a sample holder.
The sample holder is usually a flat glass slide or a thin film made of a
suitable material.

 Instrument setup:

Once the sample is prepared, the X-ray diffractometer needs to be set up.
This involves adjusting the X-ray source, detector, and other parameters. The
X-ray source emits a beam of X-rays which is directed towards the sample.
The detector measures the intensity of the X-rays that are
diffrected by the sample.

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  Calibration:

Before starting the analysis, the X-ray diffractometer needs to be

calibrated. This involves measuring the diffraction pattern of a standard
material, such as silicon or alumina, and comparing it to the known
diffraction pattern.

This ensures that the instrument is operating correctly.

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  Data collection:

The X-ray beam is directed towards the sample, and the detector
measures the intensity of the diffracted X-rays at different angles. The
sample is rotated in small increments, and the diffraction pattern is
recorded at each angle.
This produces a series of data points that can be plotted as a diffraction
pattern.

 Data analysis:

The diffraction pattern is then analyzed to determine the crystal structure

of the sample. This involves comparing the pattern to a database of
known diffraction patterns to identify the crystal structure.
The peak positions and intensities can also be used to determine the
lattice parameters, which describe the size and shape of the crystal unit
cell.

 Interpretation and reporting:

Finally, the results are interpreted and reported. This includes identifying
the crystal structure and any impurities or defects in the sample.
The results are often presented as a diffraction pattern or as a crystal
structure diagram.

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 Overall, X-ray diffraction is a powerful technique that provides detailed
information about the internal structure of crystalline materials. It is
widely used in materials science, chemistry, and other fields to study the
properties and behavior of materials.

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 Powder method of X -ray diffraction by crystal

Powder Diffraction:-

A powder may be composed of many small and finely ground crystals, known
as crystallites.These crystallites are (assumed to be) randomly oriented to one
another.
If the powder is placed in the path of a monochromatic X-ray beam,diffraction
will occur from the planes in those crystallites that are
oriented at the correct angle to fulfill the Bragg condition.The diffracted beams
make an angle of 2θ with the incident beam.

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In the Debye-Scherrer photographic method, a film was wrapped around the
inside of a X-ray camera.
The powder, sealed in a glass capillary tube, diffracts the X-rays (Bragg’s law)
to produce cones of diffracted beams. These cones intersect a strip of
photographic film located in the cylindrical camera to produce a characteristic
set of arcs on the film.

The film can be removed and examined. Using the radius of the camera and the
distance along the film from the center, the Bragg angle 2θ and therefore the d-
spacing for each reflection can be calculated.

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 Advantages of X -ray diffraction

Some of the main advantages of XRD are:-

1. Identification of crystalline materials:

XRD can identify the presence of crystalline materials in a sample and

provide information on the crystal structure and composition.

2. Non-destructive:

X-ray diffraction is a non-destructive technique, which means that

the sample does not need to be destroyed or altered in any way
during the analysis. This makes XRD a valuable tool for analyzing
valuable or irreplaceable samples.

3. Quantitative analysis:

X-ray diffraction can be used for quantitative analysis, such as

determining the amount of a specific mineral in a rock or the degree of
crystallinity in a polymer.

4. High resolution:

X-ray diffraction provides high resolution and detailed structural

information about a material at the atomic level. This allows
researchers to study the arrangement of atoms in crystals and the
bonding between them.

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 5. Wide applicability:

XRD can be used to study a wide range of materials, including

metals, ceramics, minerals, polymers, and biological materials.

6. Minimal sample preparation:

XRD requires minimal sample preparation, making it a quick and

efficient technique.

7. In situ analysis:

XRD can be used to study materials under various conditions, such as

high temperature, high pressure, or in a gas or liquid environment.

8. Structural determination:

XRD can be used to determine the structure of complex molecules,

such as proteins and DNA, which is important in drug discovery and
development.

Therefore XRD is a versatile and powerful technique that can provide valuable
information on the structure and properties of materials.

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 Disadvantages or limitations of X -ray diffraction

there are some disadvantages and limitations to its use:-

 Limited to crystalline materials:

X-ray diffraction requires a crystalline sample to work. This means that

it cannot be used to analyze amorphous materials, such as glasses or
liquids, which do not have a well-defined crystal structure.

 Sample preparation:

Preparing a sample for X-ray diffraction can be time-consuming and

technically challenging. The sample must be finely ground and
homogenous, and any impurities or defects in the crystal structure can
affect the results.

 Instrumentation:

X-ray diffraction requires specialized equipment, including an X-ray

source and a detector. These instruments can be expensive, and their
operation requires specialized training.

 Limitations on sample size:

The size of the sample is limited by the size of the X-ray beam used. This
can make it difficult to analyze small or irregularly shaped samples.

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  Information limited to the crystal structure:

X-ray diffraction provides information about the arrangement of atoms in

a crystal, but it does not provide information about other properties such
as the chemical composition, electronic structure, or mechanical
properties.

 Destructive nature:

X-ray diffraction is a destructive technique, which means that the sample

cannot be used for further analysis once it has been analyzed.

 Low sensitivity:

X-ray diffraction is not very sensitive to light elements like hydrogen,

helium, and lithium, which can limit its use in some applications

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 Conclusion

In conclusion, X -ray diffraction is a valuable technique for analyzing the

crystal structure of materials.
It has been widely used in many fields, including material science, chemistry,
physics and geology. Despite it’s limitations, X-ray diffraction has provided us
with a wealth of knowledge about the arrangement of atoms in solids and it
continues to be essential tool in the study of materials.
By understanding the advantages and disadvantages of X -ray diffraction,
researchers can use this technique effectively and interpret the results with
confidence.

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