Submitted To: Dr.

Siraj ul Haq

Submitted by: Malik muhammad
Arfan

Bibi Ruman

Ayesha Islam

Kiran bibi

Uswa yusaf

Session: 2024-2026

Program: M.Phil.

Semester: 1st




X-RAY DIFFRACTION
 OUTLINE
 Introduction
 What is X-ray & X-ray Diffraction
 History
 Instrumentation and Working Principles
 X-ray diffraction methods
 Applications
 Safety
 Summary & Conclusions
 References
 Introduction
X-ray diffraction is used to obtain structural information about
crystalline solids.
• X-ray are the short wavelength electromagnetic radiation reduced
by the deceleration of high energy electron or by electronic
transition of electron in inner orbit of atom.
• The penetration power of X-ray depend on the energy and on the
basis of this, there are two types of X-ray:
1. Hard X-ray
2. Soft X-ray
 History of X-Ray Diffraction
• 1895 X-rays discovered by Roentgen
• 1914 First diffraction pattern of a crystal
made by Knipping and von Laue
• 1915 Theory to determine crystal structure
from diffraction pattern developed by Bragg.
• 1953 DNA structure solved by Watson and
Crick
• Now Diffraction improved by computer
technology; methods used to determine
atomic structures and in medical
applications
 What is X-ray Diffraction
• Crystalline substance (e.g. minerals) consist of a parallel rows of atoms separated by
unique distance. When X-ray is incident on a crystal layer, diffraction occur called scattering
or X-ray diffraction.

Why X-ray Diffraction is done?

• X-ray diffraction is done for the for the analyzing the atomic or molecular structure of
materials (used for phase identification of a crystalline material and can provide
information on unit cell dimensions).
• Measure the average spacing’s between layers of rows of atoms in a substance
• Determine the orientation of an individual grain or crystal.
• Measure the size, shape and internal stress of small crystalline areas.
• Identify the crystal structure of an unknown substance.
 X-ray Production
• When high energy electrons
strike an anode in a sealed
vacuum, x-rays are generated.
Anodes are often made of
copper, iron or molybdenum.
• X-rays are electromagnetic
radiation.
• They have enough energy to
cause ionization.
 Bragg’s Law
• The beam reflected from the lower
surface travels farther than the one
reflected from the upper surface
• If the path difference equals some
integral multiple of the wavelength,
constructive interference occurs
• Bragg’s Law gives the conditions for
constructive interference
λ= 2d sinθ
 INSTRUMENTATION & WORKING
• The instrument consist of three main
elements:
1. X-ray cathode
2. Collimators
3. Detectors
• X-ray tube or cathode tube:
• The cathode tube are the vacuum
tube generates X ray. Here a tungsten
filament is heated by giving high
voltage 30-4-Kev.
 Collimators

• Collimator is a device that narrow a beam

of particles or wave of X-ray.
• In order to get a narrow beam of X-ray the
X-ray generated by a targeted molecule
are allowed to pass through collimator
which consist of two set of closely
packed metal plate separated by a small
gap.
• The collimator absorb all the X-ray except
the narrow beam that passes between
gap.
 DETECTORS

• In detector the X-ray intensity can be measured or recorded by two

methods:
1. Photographic method
2. Counter method
 X-ray diffraction methods
• There are several XRD methods that are generally used for
investigating the internal structures and crystal structures of
various solid compounds.
 The Laue method
• Laue in his very first experiments used white
radiation of all possible wavelengths and allowed
this radiation to fall on a stationary crystal.
• The crystal diffracted the X-ray beam and
produced a very beautiful pattern of spots which
conformed exactly with the internal symmetry of
the crystal.
• Let us analyze the experiment with the aid of the
Bragg equation. The crystal was fixed in position
relative to the X-ray beam, For each set of planes
hkl, the spacing d(hkl) and the Bragg angle 0(hkl)
are fixed
 Rotating Crystal Method
• Single crystal mounted with one axis
normal to a monochromatic X-ray beam.
• Cylindrical film placed around the sample
as the sample rotates, some sets of planes
momentarily satisfy Bragg condition.
• When the film is laid flat, a series of
horizontal lines appears.
• Because crystal rotates about a single axis,
possible Bragg angles are limited - not
every plane can produce a diffracted spot.
• Sometimes used to determine unknown
crystal structures
 Powder crystal method
• X-ray powder diffraction (XRD) is a rapid
analytical technique primarily used for phase
identification of a crystalline material and can
provide information on unit cell dimensions. The
analyzed material is finely ground, and
homogenized, and average bulk composition is
determined. If the angle of incidence is θ then
the angle of reflection will be 2θ. If the radius is r
the circumference 2πr corresponds to a
scattering angle of 360°. θ =360*1/πr From the
above equation the value of θ can be calculated
and substituted in Bragg’s equation to get the
value of d.
 KEY STEPS IN XRD SAMPLE PREPARATION:


Sample Collection


Grinding and milling


Mixing and homogenization


Sample mounting
To prepare a sample for X-ray diffraction analysis, you typically
need to grind the material into a fine powder, ensuring a
consistent particle size, then carefully mount it on a sample
holder to create a thin, even layer for the optimal X-ray interaction
 Applications of X-Ray Diffraction
• Determination of Crystal structure
• Phase identification / transition
• Grain size / micro-strain
• Texture/stress( i.e. Polymer , fiber )
• Determination of thin film composition
• Industry Identification of archeological materials
 Safety in XRD
• Exposure types
 Short-term high-dose
 Long-term low-dose
• Invisible, odorless, colorless (most exposures undetectable)
• Lab users must understand radiation safety issues and pass an
exam to use lab
• Safeguards present in lab do not substitute for knowledge and
following safe procedures
 Summary & Conclusion
• X-ray diffraction is a technique for analyzing structures of biological
molecules
• X-ray beam hits a crystal, scattering the beam in a manner
characterized by the atomic structure
• Even complex structures can be analyzed by x-ray diffraction, such
as DNA and proteins.
• This will provide useful in the future for combining knowledge from
physics, chemistry, and biology
 References
• Lee, M. X-ray Diffraction for Materials Research from Fundamentals
to Applications; CRC Press: Boca Raton, FL, USA, 2021.
• Macías-Quiroga, I.F.; Giraldo-Gómez, G.I.; Sanabria-González, N.R.
Characterization of Colombian Clay and Its Potential Use as
Adsorbent. Sci. World J. 2018, 2018, 5969178. Authier, A.
Dynamical Theory of X-ray Diffraction; Oxford University Press:
Oxford, UK, 2001.
• Sivia, D.S. Elementary Scattering Theory for X-ray and Neutron
Users; Oxford University Press: New York, NY, USA, 2011.
• Ameh, E.S. A review of basic crystallography and X-ray diffraction
applications. Int. J. Adv. Manuf. Technol. 2019, 105, 3289–3302.
THANK
YOU