X-Ray Diffraction

&
Bragg’s Law
Presented by:
Yash Mire-1132220303
Aakanksha Gonnade- 1132220395
Pranjal Thombre- 1132220017
Chaitanya Channe- 1132220483
 Index
• What is X-Ray Diffraction?
• History of XRD

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• Working
• Instrumentation
• Bragg’s Law
• Advantages
• Disadvantages
• Applications
• References
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 What is X-Ray Diffraction?
Introduction
• The atomic planes of a crystal cause an
incident beam of X-rays to interfere with one
another as they leave the crystal, is known as
XRD or X-ray diffraction.

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• A technique for analyzing the atomic or
molecular structure of materials.
• Powerful and non-destructive technique for
characterizing crystalline materials.
• Also known as X-ray powder diffraction
 Because the material to be analysed typically
is finely ground down to uniform state.
• Works on Diffraction- When light bends
slightly as it passes around the edge of an
object or encounters an obstacle or aperture.
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History of XRD
• 1895: X-ray discovered by Roentgen
• 1912: Von Laue demonstrates that X-ray can be diffracted by crystals.
• 1914: 1st diffraction pattern of crystal made by Kalpping and Von

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• 1915: theory to determine crystal structure from diffraction pattern
developed by Bragg.
• 1935: Le Galley constructs 1st X-ray powder diffractometer.
• 1947: Phillips introduces 1st commercial powder diffractometer
• 1950: Powder diffraction used primarily to study structural
imperfections largely by metallurgist and mineralogist
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 XRD Working

• Based on constructive interference of

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2. Bombardment of X-ray monochromatic
beam on the sample.
3. Diffraction of electron surrounding the
molecule as the X-ray hit them.
4. Then diffracted rays reaches to film
which is connected to detector.
5. Formation of a pattern occurs which is
known as X-ray diffraction pattern.
6. Each spot formed on film are called
Reflection. 5
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XRD graph
 Instrumentation of XRD
The parts of XRD are as follows:
 Radiation sources
 Collimator
 Monochromator
• Filters

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• Crystal monochromators
 Detectors
• Photographic method
• Counter method
1. Geiger-Muller Tube Counter
2. Proportional counter
3. Scintillation detectors
4. Solid state semiconductor detector
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5. Semiconductor detector
 Radiation source
1. X-ray tube
2. Radioisotopes
3. Secondary fluorescent

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• X-Ray tube: Composed of evacuated tube possessing cathode (tungsten filament) at one end
and anode (metal target) at another end.
• Passage of current through tube causes tungsten filament to glow and emit electrons.
• Among the 2 electrodes, large voltage difference is applied causing electrons to move at high
velocity from filament and strike to anode.
• Due to high velocity impact of electrons onto the target, inertial electrons of metal gates
dislodge which causes the outer shell electrons to jump to a lower energy shell to replace the
dislodge electrons.
• Electronic transition results in the generation of X rays produced. X rays are allowed to
move through a window of X ray tube. 9
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X-Ray Tube
 Collimator Monochromators
• X-Ray are generated by the target material • Filters: The filter is a window of materials
when allowed to pass through collimator. that absorbs undesirable radiation, but

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• It consists of 2 sets of closely packed metal allows the radiation of the required
plates separated by a small gap. wavelength to pass.
• Collimator absorbs all the X-rays, but the • Crystal monochromators: These are made
narrow beam that passes between the gaps up of a suitable crystalline material
is not absorbed. positioned in the X ray beam so that the
angle of reflecting plane satisfied the
Bragg’s equation for the required
wavelength, and the beam is split up into
component wavelength.

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 Detectors
Photographic method Counter methods
• Plane or cylindrical films is used which is • There are 3 main types of detectors used in
developed after exposure of X rays. X ray diffraction.

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• Blackening of the developed film is always • Proportional
expressed in terms of density units D. • Scintillation
D=log I0 / I • Semiconductor
Where, • For instrument dedicated for Powder works,
I0= incident intensities a proportional detector is probably used.
I =transmitted intensities • Scintillation, although still available, is not
D=total energy that causes the blackening widely used in new types of diffractometer.
• Semiconductor detector offers many
advantages example very efficient.
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 Bragg’s Law
• Introduced by Sir W.H. Bragg and his Son W.L. Bragg.
• Statement: When the X-ray is incident onto a crystal surface, its angle of incidence will
reflect back with a same angle of scattering. And when the path difference, d, is equal to
whole number, n, of wavelength, a constructive interference will occur.

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• Conditions for Bragg’s Law:
 the angle of incidence is equal to the angle of scattering
 The path length difference is equal to an integer number of wavelengths
• If these conditions are fulfilled, it will allow maximum intensity which enables a calculation
about the details of the crystal structure observed.

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 Bragg’s Equation

where:
• is wavelength of the X ray.

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• d is the spacing of the crystal layers (path difference)
• is the incident angle (the angle between incident ray and the scattered plane)
• n is an integer.

The principal of Bragg’s law is applied in construction of instruments such as Bragg’s

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Derivation of Bragg’s Law

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 Advantages
• Rapid and powerful technique for identifying unknown minerals and material.
• Minimal sample requirement
• Straightforward interpretation of the resulting data

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• Instruments are widely available
• Clear and unambiguous results are obtained
• Measure the internal stress, the size and shape of small crystalline areas, and measure the
average spacings between the layers of rows of atoms in samples
• Can readily differentiate polymorphs
• Is a non-destructive technique
• Relatively easy to design experiments and in situ cells

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 Disadvantages
• The sample should be homogeneous if one wants to find the unknown powder sample best
• Standard reference data is required for XRD analysis
• Samples are mostly required to be grinded for analysis

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• If the crystal sample is non-isometric, then the indexing of patterns can be complex when
determining unit cells
• X-Rays do not interact strongly with lighter elements
• X-Ray hazard
• Very expensive
• Sensitive to sample preparation technique
• Requires radiation license and fees to operate
• Data collection generally requires between 24 and 72 hours.
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 Applications

Geology Engineering Biology Material science

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Environmental Thin flame
Battery research Electronics
science coatings

Pharmaceuticals
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 Applications
X-Ray Diffraction can do the following:
• Measure the average spacing between layers of rows of atoms in a substance.
• Determine the orientation of an individual grain or crystal.

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• Measure the size, shape and internal stress of small crystalline areas.
• Identify the crystal structure of an unknown substance.
• Find structure to determine the function of proteins.
• Study crystal deformation and stress properties.
• Study of rapid chemical and biological processes.
• Differentiate between crystalline and amorphous materials.

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 References
• https://www.slideshare.net/BiNduXtrEiy/xray-diffraction-instrumentation
• https://pubmed.ncbi.nlm.nih.gov/25831472/
• https://www.scimed.co.uk/education/what-is-x-ray-diffraction-xrd/

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• https://chem.libretexts.org/Bookshelves/Analytical_Chemistry/Supplemental_Modules_(Ana
lytical_Chemistry)/Instrumentation_and_Analysis/Diffraction_Scattering_Techniques/Bragg'
s_Law
• https://byjus.com/physics/braggs-law/
• https://onlinelibrary.wiley.com/doi/10.1002/3527600906.mcb.200400058
• Video- https://youtu.be/QHMzFUo0NL8

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Thank
You