MM-141 Materials Lab I

X-RAY DIFFRACTION

Muhammad Mudasser Khan

Salman Khalid
Abeera Fatima
Azhar Tanveer

Lab Instructor: Syed

Ali Afraz
Problem Statement
Some Industrial Problems.

How will you determine the crystallographic structure of unknown

material?

How will you determine the structure of a novel (newly discovered)

material?

Suppose a gear fails in action because of high residual stresses.

(How can we know the presence, amount and nature of residual
stresses)?

Phase identification in the manufacturing of semiconductor-related

ceramics is very important. How can we identify different phases
for a material with same composition?
 Problem Statement
Continued..

Residual stresses in case of deposited thin films can lead to

cracking (in electronic circuits, silicon wafers, transistors). How to
avoid such cracking?

How can we determine what happens in a material at high

temperatures? Like Phase Transformation in SMA, stress-induced
transformation, grain growth etc.

Steel can become drastically weak if certain phases are developed.

How can we determine which phase is responsible for this?

Electromigration (Major failure mechanism for Integrated circuits IC)

depends on the grain misorientation (Texture). How can we find
preferred orientation in a material?
Solution?

X-RAY DIFFRACTION
Terminology used in XRD

X-Rays
Short-wavelength beams of electromagnetic radiation produced by rapid
deceleration of electrons or through collision of high speed electrons
with a metal target

Diffraction
Scattering of X-Rays by atoms of a crystal
Constructive Versus Destructive Interference

Lattice Parameter
Refers to the physical dimension of unit cells in a crystal lattice (a, b, and c)

Interplanar Spacing (d)

Distance between two planes (of the same type/family)
Terminology used in XRD
Continued..

Phase
A homogeneous, physically distinct portion of matter (with a unique
lattice parameter)

Preferred Orientation of Planes/Grains ?

Residual Stresses
Stresses present in an object in the absence of any external force
Introduction
Overview

A scattering of X-rays by the atoms of a crystal that

produces an interference effect so that the diffraction
pattern gives information on the structure of the crystal
or the identity of a crystalline substance
Instrumentation
Interplanar 2
Spacing (d)
1
In
Be cid
am en
tX
RA
Y

D
Be ifr
am ac
te
d
XR
AY
 1 Path Difference b/w
2 In Beam 1 & 2 ?
Be cid

AY
XR
am en
tX

d
te
RA

am ac
Y

Be ifr
D
S

9 R
P 0 d

Path Difference between

Beam 1 and 2
This Path Difference is equal to 2dsin
 1 What is Braggs
2 In Diffraction?
Be cid

AY
XR
am en
t

d
XR

te
AY

am ac
Be ifr
D
The diffracted Beams can either interfere constructively or
destructively
The diffracted Beams will be in phase if the path
difference is equal to multiple of wavelength, i.e. (n)

Thus, Constructive Interference takes place if

n=2dsin is satisfied. This is called Braggs
Bragg-Brentano Arrangement
To enable scanning over a range of

The X-ray incident beam is fixed, but a sample stage

rotates at while detector rotates at 2
 This Peak represents the no. of
diffracted beams from (111) planes
of Si at an angle of 29
Relative Intensity
(Counts)
This Peak represents the no. of
diffracted beams from (220)
planes of Si at an angle of 47

Diffraction Angle
Relationship between diffraction data and crystal
parameters
For a cubic crystal system

Everything else except d is known so d-

spacing is found using the above equation
What about lattice parameter?

There are two unknown values in the second

equation. Can we find lattice parameter from
this Data?
Cohens Least-Square Method or Extrapolation
Method is used for determining Lattice
How XRD Identify Phases??????
By Comparison Method

It identify the crystal structure by analyzing and then

comparing the spectrum with a database of known
crystalline substances.

What is a database?
A library that contains over one million diffraction
spectra of known crystalline substances.

What is the best analogy to the above description?

The Overall Picture
Very Important

Hit a sample by X-Rays

The X-Rays that undergo Braggs Diffraction are

detected

The Detected signals carry important Information

about the material (Plane index and angle of
Diffraction)

The data are compared with previous information

in the database using a software Xpert Highscore
 Thin film X-ray Diffractometry
Detecting crystal structure of coatings
Signals are coming from
substrate, but we want coating
to be analyzed? What to Do?
Let us check what
happens by decreasing
incident angle of x-rays

Coati
ng of
WC

Substr
ate
(Steel)
Glancing Angle X-ray Diffractometry
Detecting crystal structure of coatings

The incident beam is directed to the specimen at a small glancing

angle (usually < 1)
Residual Stresses

Residual stress generates strain in crystalline materials by stretching

or compressing bonds between atoms.

Bond stretching or compressing changes the interplanar spacing (d)

n = 2dsin

If stresses are compressive, d decreases

If d decreases, what happens to the above equation?

The left hand side of the above equation is constant

So, the likely result is if d decreases, should increase

accordingly which shifts the peak position to the right
Steel specimen with no
residual stresses 2

2
Steel specimen with tensile
residual stresses
Applications

Phase Identification

Quantitative Measurement: Relative amounts of

compounds or phases in a sample can be determined

Residual stresses

Preferred Orientation (Texture)

Studying High Temperature Phenomena taking place in

a material like Phase transformation, grain growth
Model Question For Quizzes etc.
Any idea????

1. Can we perform XRD analysis of a single graphene sheet?

Yes or No? Justify in either case.

2. What will happen to the peak if a specimen contain both

compressive and tensile stresses in the same area
simultaneously?

3. Why the incoming X-Ray beams do not undergo

interference before hitting the sample?