B.
Tech 4th Semester MMC403
Materials Characterization By Dr. Bijay Kumar Show
Lecture-10
Date: 16-02-2022
Department of Metallurgical & Materials Engineering
National Institute of Technology Durgapur
LECTURE-10
Determination of crystallite size
Required Textbook
1. “Elements of X-Ray Diffraction”, by B.D. Cullity, Addision Wesley Publishing Co., Massachusetts, 1968.
2. “X-ray diffraction-a practical approach”, by C. Suryanarayana and M. Grant Norton, Springer, 1998.
3. “X-ray Diffraction: Its Theory and Applications”, by S. K. Chatterjee, Prentice-Hall of India Pvt. Limited, 2004.
Determination of crystallite size
XRD Line Broadening
Instrumental Unresolved 1 , 2 peaks
Non-monochromaticity of the source (finite width of peak)
Bi
Crystallite size
Bc
Strain ‘Residual Strain’ arising from dislocations, coherent
Bs precipitates etc. leading to broadening
Stacking fault
Other defects
In principle every defect contributes to some broadening
B ( FWHM ) Bi Bc Bs BSF ...
B ( FWHM ) Bi Bc Bs BSF ... 5
B ( FWHM ) Bi Bc Bs BSF ...
For a peak with a B Bi Bc Bs Br
Lorentzian profile
Longer tail
For a peak with a Gaussian
profile Br2 B 2 Bi2
A geometric mean can
also used
Br2 ( B Bi ) B 2 Bi2
Separating crystallite size broadening and strain broadening
k
Br Bc Bs Bc Bs tan( )
L Cos ( )
Williamson-Hull plot
k
Br tan( )
L Cos ( ) Plot of [Br Cos] vs [Sin]
k
Br Cos ( ) Sin( )
L
8
Strain= slope = 3.5 X 10-3
Crystallite Size= 90 nm
Bragg’s equation is a negative law
If Bragg’s eq. is NOT satisfied NO reflection can occur
If Bragg’s eq. is satisfied reflection MAY occur
Diffraction = Reinforced Coherent Scattering
Intensity of the Scattered beam
Scattering by a crystal
A
Electron Polarization factor
Atom Atomic scattering factor (f)
C
Unit cell (uc) Structure factor (F)
Scattering by an electron
X-ray beam is an electromagnetic wave characterized by an electric field whose strength
varies sinusoidally with time at any one point in the beam.
Since an electric field exerts a force on a charged particle such as an electron, the oscillating
electric field of the x-ray beam will set any electron it encounters into oscillatory motion
about its mean position.
Now an oscillating electron emits an electromagnetic wave.
In this sense, an electron is said to scatter x-rays, the scattered beam being simply the
beam radiated by the electron under the action of the incident beam.
The scattered beam has the same wavelength and frequency as the incident beam and is
said to be coherent with it, since there is a definite relationship between the phase of the
scattered beam and that of the incident beam which produced it.
Scattering by an electron
Although x-rays are scattered in all directions by an electron, the intensity of the scattered
beam depends on the angle of scattering, in a way which was first worked out by J. J.
Thomson.
He found that the intensity I of the beam scattered by a single electron of charge e and mass
m, at a distance r from the electron, is given by
Scattering by an electron
Suppose the incident beam is traveling in the direction
ox (Fig. 4-3) and encounters an electron at 0.
We wish to know the scattered intensity at P in the xz
plane where OP is inclined at a scattering angle of 2θ to
the incident beam.
An unpolarized incident beam, such as that issuing
from an x-ray tube, has its electric vector E in a
random direction in the yz plane.
This beam may be resolved into two plane polarized
components, having electric vectors Ey and Ez where
Scattering by an electron
