XRD

MS&E 11
Raja Muhammad Usama
Muhammad Asim
Harris Hassan
Usman Ahmed Siddiqui
INTRODUCTION
By Raja Muhammad Usama
• Why do we study X ray diffraction?
• What is the advantage of having a data of X-ray
diffraction?
Solid matter consists out of two types of material:
amorphous and crystalline.
In an amorphous sample the atoms are arranged in a
random way, glasses are an example of amorphous
materials.
In a crystalline sample the atoms are arranged in a
regular or ordered pattern and there is a smallest
volume element that, by repetition in three
dimensions, can describe the crystal.
This smallest volume element is called a unit cell
About 95% of all solid materials can be described as crystalline

Crystals can be easily studied by X-ray diffraction. In fact, the

International Union of Crystallography defines crystals as substances
that produce sharp X-ray diffraction patterns. The study and
understanding of the unit cell of a crystal is largely done through the X-
ray diffraction experiment.
X-ray diffraction (XRD) is a powerful method for the study of
nanomaterials (materials with structural features of at least one
dimension in the range of 1-100 nm). The wavelength of X-rays is on the
atomic scale, so X-ray diffraction (XRD) is a primary tool for probing
structure of nano-materials. XRD offers unparalleled accuracy in the
measurement of atomic spacing and is the technique of choice for
determining strain states in thin films.
What is X-ray Diffraction
(XRD)

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, homogenized,
and average bulk composition is determined.
All diffraction methods are based on generation of X-rays in an X-ray
tube. These X-rays are directed at the sample, and the diffracted rays
are collected. A key component of all diffraction is the angle between
the incident and diffracted rays. Powder and single crystal diffraction
vary in instrumentation beyond this.
X-ray diffraction is based on constructive interference of
monochromatic X-rays and a crystalline sample. These X-rays are
generated by a cathode ray tube, filtered to produce monochromatic
radiation, collimated to concentrate, and directed toward the sample.
X RAY
DIFFRACTION
PROCESS

By Muhammad Asim
X Ray diffraction process is used to determine the crystal
structure of material.

X Rays are electromagnetic radiation of small wavelength.

The sample is placed in the instrument and illuminated with

the beam of X Rays.

The X Rays diffract through the atoms of material at some

called Diffraction angle.

The diffracted X Rays are received at a detector.

The diffraction phenomenon is due to constructive interference.

 The condition for Constructive Interference is that when the path
difference of ray 2 is an integral multiple of wavelength of ray 1
and a peak will be recorded at detector.
 William Henry Bragg was the first person to use this technique
for determining the crystal structure.
 He proposed the formula 2dsinØ=nλ
 The Graph of Intensity is
recorded against diffraction
angle.
 The crystal Structure is
determined by peaks obtained
of a certain material.
 XRD relationship to other scattering
techniques
Elastic scattering(XRD)
Kinetic Energy of incident particle is
conserved.
A collision between two hard things, like
billiard balls, is a good example
No change in wavelength.
The direction of propagation of the colliding
subjects might change however the initial
and final kinetic energy stays the same.
Muhammad Haris Hassan
180301012
Non Elastic scattering
Kinetic Energy of incident particle is not
conserved.
The Pre-collision kinetic energy can be used
to cause an internal state change in one of
the colliding objects. These changes can
include change in temperature and
deformation etc. A car accident is a good
example.
The direction of propagation may or may
not change depending on the collision
however, kinetic energy is lost.
 WHY ARE X-RAYS USED RATHER THAN ANY OTHER
ELECTROMAGNETIC RADIATIONS?
• X-rays range in wavelength from 10 to 0.01 nanometers; a typical wavelength used for
crystallography is 1 Angstrom (0.1 nm).
• Longer wavelength EM radiations don't possess the resolution to determine the atomic
positions.
• This brings us to the other extreme of the spectrum, however, gamma radiations can’t be
utilized too because they are hard to produce in large numbers, are difficult to focus, and
interact too strongly with matter, producing particle-antiparticle pairs(creation of a subatomic
particle and its antiparticle).

Muhammad Haris Hassan

180301012
 COMPARISON OF ELECTRON DIFFRACTION (ED) AND X-
RAY DIFFRACTION
ED and XRD, are caused by constructive interference of scattered waves, and the same
fundamental laws (e.g., Bragg law) can be applied for the interpretation of the resulting
diffraction patterns. In both cases, diffraction patterns of powders and of single crystals
appear.
However, ED and XRD show some distinct differences:
 The wavelength of electrons (e.g., 1.97 pm for 300 keV electrons) is much shorter than that
of X-rays (about 100 pm). Therefore, the radius of the Ewald sphere is much larger and
more reflections are observed by ED than by XRD.
 The diffraction angles are very small in ED.
 Electrons are scattered by the positive potential inside the electron cloud (Coulomb
interaction), while X-rays interact with the electron cloud. As the result, the interaction of
electrons with matter is much stronger (106-107×) than that of X-rays.
• The diffracted electron beams have a high intensity and exposure times are in the order of
a few seconds. ED patterns can be observed on the viewing screen of the electron
microscope.

Muhammad Haris Hassan

180301012
 COMPARISON OF NEUTRON DIFFRACTION (ND) AND X-RAY
DIFFRACTION
• The neutron is uncharged it can easily approach the atomic nuclei found in a material
and nuclear scattering occurs at very short distances of ca. 10−14 to 10−15 m.
• It is this scattering from an ordered crystalline material that produces coherent Bragg
scattering and yields either the intensity of the various ’hkl’ reflections from
a single crystal.
• A distinct difference in the scattering lengths for X-ray and neutron scattering is,
because X-ray diffraction results from scattering by the electrons, atoms of
similar atomic number exhibit very similar scattering and it is hard to distinguish
between them by X-ray diffraction.
• In contrast, neutron scattering depends upon the nature of the scattering nuclide and,
as a consequence, atoms of similar atomic number often have quite different neutron
scattering lengths.
• Secondly, because the neutron has a magnetic moment, it also is scattered by
interaction with any magnetic moments found within a material.

Muhammad Haris Hassan

180301012
 WHY IS XRD USED WHEN NEUTRON AND ELECTRON
DIFFRACTION CAN BE ALSO USED?
• Any home laboratory can afford an X-ray source and a few diffractometers whereas
electron diffraction instruments are too expensive for home laboratories.
• ND and ED processes are much more complex and require more advanced capital
investment.
•  X-ray diffraction is more versatile because you can study relatively small amount of
sample, especially with synchrotron X-rays.
• Another reason is the degree of damage. Many material is sensitive to electron beam
and the original structure is easily modified. Compared to electron beam, damage by X-
ray is very small. 
• Sample preparation is relatively cheap and less time consuming, moreover, the
instruments are more widely available.

Muhammad Haris Hassan

180301012
APPLICATIONS OF XRD
BY: USMAN AHMED SIDDIQUI
 STRUCTURE OF CRYSTALS
• The analytical applications of X-ray
diffraction are numerous. The method
is non-destructive and gives
information on the molecular structure
of the sample. Perhaps its most
important use has been to measure
the size of crystal planes. The patterns
obtained are characteristic of the
particulars compounds from which the
crystal was formed
POLYMER CHARACTERIZATION

• Powder method can be used to determine the degree of

crystalline of the polymer. The non-crystalline portion simply
scatters the x-ray beam to give a continuous background,
while the crystalline portion causes diffraction lines that are
not continuous.
STATE OF ANNEAL IN METALS

• A property of metals that can be determined by x-ray

diffraction is the state of anneal.
• Well-annealed metals are in well-ordered crystal form and
give sharp diffraction lines.
• If the metal is subjected to drilling, hammering, or bending, it
becomes fatigued, “that is, its crystals become broken and
the x-ray pattern more diffuse.
GEOLOGICAL APPLICATIONS
• XRD is the key tool in mineral exploration. Mineralogists have been amongst the
foremost to develop and promote the new field of X-ray crystallography after its
discovery. Thus, the advent of XRD has literally revolutionized the geological
sciences to such a degree that they have become unthinkable without this tool.
Nowadays, any geological group actively involved in mineralogical studies would
be lost without XRD to unambiguously characterise the individual crystal
structures. Each mineral type is defined by a characteristic crystal structure,
which will give a unique x-ray diffraction pattern, allowing rapid identification of
minerals present within a rock or soil sample. The XRD data can be analysed to
determine the proportion of the different minerals present.
MICROELECTRONICS
INDUSTRY
• As the microelectronics industry uses
silicon and gallium arsenide single crystal
substrates in integrated circuit production,
there is a need to fully characterise these
materials using the XRD. XRD topography
can easily detect and image the presence
of defects within a crystal, making it a
powerful non-destructive evaluation tool
for characterising industrially important
single crystal specimens.
GLASS INDUSTRY

• While glasses are X-ray amorphous and do not themselves

give X-ray diffraction patterns, there are still manifold uses of
XRD in the glass industry. They include identification of
crystalline particles which cause tiny faults in bulk glass, and
measurements of crystalline coatings for texture, crystallite
size and crystallinity.
NANO AND MATERIAL SCIENCE

• The term particle size and crystallite size refer to two distinct
properties in a material. Particles comprise of several small
crystallite. Crystallite size is the fundamental property of
materials. Properties of nanomaterials depend on crystals
size and not particle size. PXRD can measure millions of
crystals and accurately determine the size distribution of
nanomaterials. It can be widely used for studying the nature
of polymers and composites in Material Science
FORENSIC SCIENCE

• XRD is used mainly in contact trace analysis. Examples of

contact traces are paint flakes, hair, glass fragments, stains
of any description and loose powdered materials.
Identification and comparison of trace quantities of material
can help in the conviction or exoneration of a person
suspected of involvement in a crime.
OTHER APPLICATIONS
• This has been used to locate trace elements such as barium and iodine
in the body.
• This has been used to detect below holes or the segregation of
impurities such as oxides in welds and other joints.
• It can also be used to measure the volume of liquids in closed vessels
or pipes without opening or breaking the vessels or pipes.
• XRD is the key technique for solid-state drug analysis, benefiting all
stages of drug development, testing and production.