SUBMITTED BY: BIJAYA KUMAR BHOI

Roll-25610
Regd.-0601105067
8th sem, B.Tech,
Department of Metallurgical and
Materials Engg.,
I.G.I.T. , Sarang.
UNDER THE GUIDANCE OF : Mr.P.K.MALLIK

Sr.
Lecturer, Department of Metallurgical and Materials
Engineering., I.G.I.T. , Sarang.
 INTRODUCTION
 BASIC PRINCIPLE
 TYPES OF X-RAY DIFFRACTION
 APPLICATIONS
 ADVANTAGES
 LIMITATIONS
 CONCLUSION
 REFERENCES
X-ray diffraction techniques are some of the most useful
in the characterization of crystalline materials, such as
metals, inter- metallic, ceramics, minerals, polymers,
plastics, or other inorganic or organic compounds. X-
ray diffraction techniques can be used to identify the
phases present in samples from raw starting materials
to finished product and to provide information on the
physical state of the sample, such as grain size, texture,
and crystal perfection. Most x-ray diffraction
techniques are rapid and non destructive; some
instruments are portable and can be transported to the
sample. The sample may be as small as an airborne
dust particle or as large as an airplane wing.
 Diffraction effects are observed when
electromagnetic radiation impinges on periodic
structures with geometrical variations on the length
scale of the wavelength of the radiation. The inter
atomic distances in crystals and molecules amount to
0.15–0.4 nm which correspond in the electromagnetic
spectrum with the wavelength
of x-rays having photon energies between 3 and 5 keV.
Accordingly, phenomena like constructive and
destructive interference should become observable
When crystalline and molecular structures are exposed
to x-rays.
 For electromagnetic radiation to be diffracted the spacing
in the grating should be of the same order as the wavelength.
 In crystals the typical interatomic spacing ~ 2-3 Å so the.
suitable radiation is X-rays
 Hence, X-rays can be used for the study of crystal structures.

Beam of electrons Target X-rays

An accelerating (/decelerating) charge radiates electromagnetic radiation

 Incident X-rays

SPECIMEN Heat

Fluorescent X-rays
Electrons
Scattered X-rays Compton recoil Photoelectrons

Coherent Incoherent (Compton modified)

From bound charges From loosely bound charges

Transmitted beam
 X-rays can also be refracted (refractive index slightly less than 1) and reflected (at very small angles)
 Refraction of X-rays is neglected for now.
 Incoherent Scattering (Compton modified) From loosely bound charges
 Here the particle picture of the electron & photon comes in handy

(1 , 1 ) E1  h 1 Electron knocked aside

2

E2  h 2 (2 , 2 )
  2  1  0.0243(1  Cos 2 )

No fixed phase relation between the incident and scattered waves

Incoherent  does not contribute to diffraction
(Darkens the background of the diffraction patterns)
Fluorescent X-rays
Knocked out electron
Vacuum from inner shell

Energy E L3 L3
levels
E L2 L2

E L1 L1
Characteristic x-rays
EK K (Fluorescent X-rays)
(10−16s later  seems like scattering!)
Nucleus
 BRAGG’s EQUATION

Deviation = 2
Ray 1

Ray 2  

 d

dS
in

 The path difference between ray 1 and ray 2 = 2d Sin

 For constructive interference: n = 2d Sin
Extra path traveled by incoming waves  AY These can be in phase if and only if
Extra path traveled by scattered waves  XB  incident = scattered

But this is still reinforced scattering

and NOT reflection
 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
Reflection versus Scattering

Reflection Diffraction
Occurs from surface Occurs throughout the bulk
Takes place at any angle Takes place only at Bragg angles
~100 % of the intensity may be reflected Small fraction of intensity is diffracted

X-rays can be reflected at very small angles of incidence

  n = 2d Sin
 n is an integer and is the order of the reflection
 For Cu K radiation ( = 1.54 Å) and d110= 2.22 Å

n Sin 

1 0.34 20.7º First order reflection from (110)

Second order reflection from (110)
2 0.69 43.92º
Also written as (220)

a a
d hkl  d 220  d 220 1
8 
h2  k 2  l 2 d110 2
a
d110 
2
  Powder diffraction
1. a polycrystalline material
2. all possible orientations of the crystals
3. similar planes in different crystals will scatter in different
directions.
Scattering in X-ray powder diffraction

single crystal X-ray diffraction

1.only one orientation
2. for a given wavelength and sample setting relatively few reflections
The X-ray beam comes from the tube, though slits, is diffracted from the sample, goes
though another set of slits, diffracted from the secondary beam monochromator and
measured by the detector
THE POWDER METHOD

Cone of diffracted rays

 POWDER METHOD (HULL /DEBYE-SCHERRER METHOD)
Diffraction cones and the Debye-Scherrer geometry
Different cones for different reflections

Film may be replaced with detector

http://www.matter.org.uk/diffraction/x-ray/powder_method.htm
 THE POWDER METHOD
  2dSin d Cubic  a
Cubic crystal
h2  k 2  l 2

4 a 2
sin 2
 4a 2
  2
2
(h  k  l ) 
2 2 2
sin 2 
h  k2  l2 2

2
a 
2
(h 2  k 2  l 2 ) ( h 2  k 2  l 2 )  sin 2 
4 sin 2
 Laue method is generally divided into two types
such as transmission laue method and back
reflection Laue methods.
 In case of transmission Laue method electron
beam transmits through the specimen and the
transmitted beam which obeys the Braggs angle
forms an elliptical or hyperbola transmission
pattern.
 When the film is placed between the crystal and
x-ray source,the incident beam passes through
hole in film and forms back reflection pattern.
Applications of XRD

Bravais lattice determination

Lattice parameter determination

Determination of solvus line in phase diagrams

Long range order

Crystallite size and Strain

More
Intensity Crystal
Schematic of difference between
the diffraction patterns of various phases

0 90 180
Diffraction angle (2) →
Monoatomic gas

Intensity →
Diffraction angle (2) → Diffraction angle (2) →
Intensity →

Liquid / Amorphous solid

0 90 180
 X-ray diffraction techniques can be used to identify
the phases present in samples from raw starting
materials to finished product and to provide
information on the physical state of the sample,
such as grain size, texture, and crystal perfection.
 Most x-ray diffraction techniques are rapid and
nondestructive; some instruments are portable and
can be transported to the sample.
 Energy tenability and energy resolution.
Resonant scattering studies of charge and orbital
order, resonant magnetic scattering.
 X-ray scattering techniques are a family of non-destructive
analytical techniques which reveal information about the
crystallographic structure, chemical composition, and
physical properties of materials and thin films. These
techniques are based on observing the scattered intensity of
an X-ray beam hitting a sample as a function of incident and
scattered angle, polarization, and wavelength or energy.
 By using x-rays we can dectet atomic and molecular
structure of atoms ,electronic structure and bonding of
electrons,magnetic structure and properties of the spin .
1.International Tables for X-Ray Crystallography, Vol II, Kynoch Press, 1959

2.H.P. Klug and L.E. Alexander, X-ray Diffraction Procedures for Polycrystalline
and Amorphous Materials, 2nd ed., John Wiley & Sons, 1974

3.D.K. Smith, C.S. Barrett, D.E. Leyden, and P.K. Predecki, Ed., Advances in X-
Ray Analysis, Vol 24, Plenum Press, 1981

4. B.D. Cullity, X-Ray Diffraction, 2nd ed., Addison Wesley, 1978, p 175-177

5. H.E. Goebel, Adv. X-Ray Anal., Vol 25, 1982, p 315-324

6.C.R. Hubbard and D.K. Smith, Adv. X-Ray Anal., Vol 20, 1977, p 27