MATERIAL CHARACTERIZATION LAB 2

BY SCHOLAR NO. GUIDED BY:

161119016 Dr. JAYA SHREE
161119017 Dr. Ramesh k. Nayak
161119018
161119019
161119020
OBJECTIVE
To study the crystal structure, internal stress analysis and indexing
using X-ray Diffraction.

MATERIALS REQUIRED
1. XRD(x-Ray diffraction)

2. sample

THEORY
The atomic planes of a crystal cause an incident beam of X-rays to
interfere with one another as they leave the crystal. The phenomenon
is called X-ray diffraction.

Diffraction occurs only when Bragg’s Law is satisfied Condition for

constructive interference from planes with spacing d

Bragg’s law => 2dsinθ = nλ

This law relates the wavelength of electromagnetic radiation to the
diffraction angle and the lattice spacing in a crystalline sample.

The characterstics X-ray Diffraction pattern generated in a typical XRD

analysis provides a unique fingerprint of the crystals present in sample.

Characterstic peak is done with the help of a software like Xpert high
score plus and JCPDS. International centre for diffraction data
maintains a database of powder diffraction patterns, d-spacing and
relative intensities of observable diffraction peaks.

JCPDS stands for joint committee on powder diffraction standards. One

examines a material using XRD and compare the spectre against JCPDS
reference pattern for the material and determines the crystal structure,
indices etc.

INDEXING
When you index a diffraction pattern, you assign the correct Miller
indices to each peak (reflection) in the diffraction pattern. An XRD
pattern is properly indexed when ALL of the peaks in the
diffraction pattern are labeled and no peaks expected for the
particular structure are missing.

This is an example of a properly indexed diffraction pattern. All

peaks are accounted for. One now needs only to assign the
correct Bravais lattice and to calculate lattice parameters.

PROCEDURE FOR INDEXING

Since h, k, and l are always integers, we can obtain h2 +k2 +l2 values by
dividing the 2 sin θ values for the different XRD peaks with the
minimum one in the pattern and multiplying that ratio by the proper
integer. This should yield a list of integers that represent the various
values. You can identify the correct Bravais lattice by recognizing the
sequence of allowed reflections for cubic lattices (i.e., the sequence of
allowed peaks written in terms of the quadratic form of the Miller
indices). h2 +k2 + l2

Primitive h2 +k2 + l2 = 1,2,3,4,5,6,8,9,10,11,12,13,14,16…

Body-centered h2 +k2 +l2 = 2,4,6,8,10,12,14,16…

Face-centered h2 +k2 +l2 = 3,4,8,11,12,16,19,20,24,27,32…

Diamond cubic h2 +k2 +l2 = 3,8,11,16,19,24,27,32…

Steps:
(1) Identify the peaks.
(2) Determine 2 sin θ .
(3) Calculate the ratio sin2 θ / sin2 θmin and multiply by the
appropriate integers.
(4) Select the result that yields h2 +k2 +l2

as an integer.
(5) Compare results with the sequences of h2 +k2 +l2 values to
identify the Bravais lattice.
(6) Calculate lattice parameters.

Crystal structure
After the XRD graph is obtained, zoom on the area for which you
want to calculate crystal size and note down theangle and peak
full width at maximum(FWHM)
Scherrer formula
Dp = 0.94* ƛ/ β* cos(θ)
Where, Dp = average crystalline size
Β = line broading in radians
Θ = bragg’s angle
ƛ = X-Ray wavelength

Residual Stresses
Any factor that changes lattice parameter of crystalline specimen
can also distant their x-ray diffraction spectra. Residual stress
generate strain in crystalline material by stretching or
compressing bonds between atoms.
The tensile stress of increasing the spacing shifts a peak to lower
2 θ while compression stress of decreasing the spacing shifts the
peak to higher 2 θ in the specimen.

CONCLUSION
We can find the crystal structure, internal stress and indexing by
using X-Ray Diffraction.

Precautions :
1. Sample should be prepare carefully in powder form(random
orientation)
2. Lab user must understand radiation safety issues and pass
can exam to use lab.