X-RAY DIFFRACTION (XRD):
BASIC CONCEPTS &
DEMONSTRATION
ME 205: MATERIAL SCIENCE LAB
OBJECTIVES
The purpose of this experiment is to introduce
students to the use of X-ray diffraction techniques
for investigating various types of crystal structure
encountered in metallic materials.
Understand the fundamental concepts of X-Ray
Diffraction (XRD) technique and Bragg’s Law
Understand diffraction pattern (DP) and how to calculate
the interplanar spacing, lattice parameter and diffraction
angle using the Bragg’s equation
Know when to use XRD techniques
INTRODUCTION
X-rays were discovered in 1895 by the German physicist
Wilhelm Conrad Röntgen.
X-rays are high-energy electromagnetic radiation with
energies ranging from about 200 eV to 1 MeV.
X-ray wavelengths vary from about 10 nm to 1 pm. (The
shorter wavelength corresponds to the higher energy of
the radiation).
Visible light wavelength is 0.56 µm (560 nm)
The useful range of wavelengths for X-ray diffraction
study is, however, between 0.05 and 0.25 nm.
Spacing between atoms in metals range from 2-3 A (0.2-0.3
nm)
X-RAY DIFFRACTION
The electromagnetic spectrum is the term used by scientists to describe the
entire range of light that exists
APPLICATIONS OF X-RAYS IN MATERIAL SCIENCE
X-ray diffraction (XRD) is a powerful technique to
determine many structural and microstructural
parameters of crystalline materials including:
Crystal structure of materials – metals, alloys,
compounds, intermetallics, quasicrystals,
semiconductors, and ceramic materials.
Solid-state phase boundaries in phase diagrams.
crystallite size and lattice strain in heavily cold-
worked materials.
Long-range order parameter in ordered alloys.
Phase proportions in multi-phase alloys and powder
mixtures.
Textures.
Magnitude of residual stresses.
PRODUCTION OF X-RAY
X-rays are produced when fast-moving free electrons are suddenly
stopped by a metal target.
This is achieved in an X-ray tube consisting of two metal electrodes enclosed in a vacuum
chamber.
• Current is passed through the tungsten filament and heats it up.
• Electrons are released from the filament through thermionic emission.
• The electrons are attracted towards the positively charged anode and hit
the tungsten target with a maximum energy determined by the tube
potential (voltage).
• As the electrons bombard the target they interact and result in conversion
of energy into heat (99%) and x-ray photons (1%). The x-ray photons are
released in a beam with a range of energies (x-ray spectrum) out of the
window and form the basis for x-ray image formation.
PRODUCTION OF X-RAY
CAUTION !!!
It is important to note that the X-ray beams are:
• Non visible.
• Travel in all directions.
• Penetrate ‘encountering’ matter easily.
X-rays are damaging because they penetrate the human body and
break up molecules of DNA in our cells. If these molecules do not
repair themselves, they die. On the other hand, if the molecules
are broken and they rejoin in a wrong way, then a mutant cell is
produced and this can lead to cancer.
Precaution must be taken to avoid exposure to X-ray.
X-RAY –ELECTRON INTERACTION
An x-ray photon can interact with the electrons in the target by one of 4
ways:
No interaction (the x-ray photons
experience no change in energy)
Completely absorbed (photon energy is
transferred to the target electrons. X-
ray radiography)
Complete Absorption and another x-ray
photon of lower energy is produced (x-
ray fluorescence) 1 2 1 < 2
The x-ray photon produces an
oscillating electric field in the electrons
of the target object.
The target object generate photons of the same
wavelength at many different angles w.r.t. the incident
photons.
X-RAY INTERACTION WITH MATTER
Rayleigh Interaction
Compton Effect
Photoelectric Effect
INTERFERENCE OF WAVES
Destructive interference: scattered beams are out of phase and cancel
each other. (d = n*/2)
Constructive interference: mutual reinforcement of the scattered
x-rays : Diffraction
A diffracted beam is defined as a beam consisting of a large number of scattered beams
reinforcing one another. The diffraction directions are governed by: (i) wavelength (λ) of the
incident radiation, and (ii) nature of the crystalline sample.
BRAGG’S LAW
BRAGG EQUATION represents conditions for diffraction to occur from crystals
by relating the wavelength of the X-rays to the spacing of the atomic planes,
d, in a crystal.
n = 2dsin
BRAGG’S LAW
Bragg’s law is necessary (but not sufficient)
n = 2dsin
n is the diffraction order =1,2,3,.
: wavelength
: Bragg’s angle
d: Spacing between planes
For cubic crystals,
EXAMPLE 1 ON BRAGG’S LAW
For a BCC crystal, compute the diffraction
angles of the {110} planes assuming d(110) = 0.1181
nm and a monochromatic x-ray of = 0.1541 nm.
n = 2dsin
n =1
2 = 81.4
n =2
= sin-1 (1.305)
Hence, 2nd order diffraction is not possible
EXAMPLE 2 ON BRAGG’S LAW
Determine the diffraction angles when {111} planes of
Cu (a = 3.6151 Aº) are in diffraction condition? =
1.660 Aº
n =1
2 = 46.9o
n =2
2 = 105.4o
n =3
Hence, 3rd order diffraction is not possible
DIFFRACTION TECHNIQUES
The diffractometer is an apparatus used to determine the
angles (2theta) at which diffraction occurs for different
specimens
The primary uses of x-ray diffractometry includes:
Identify crystalline phases.
Determine unit cell size and radius.
Structure determination by indexing.
Residual stress analysis
DIFFRACTION PATTERN (DP)
Each peak in the diffraction pattern correspond to
a set of crystallographic planes {hkl}
WHY XRD?
Measure the average spacing between layers or
rows of atoms
Determine the orientation of a single crystal or
grain
Find the crystal structure of an unknown material
Measure the size, shape and internal stress of
small crystalline regions
LINKS
[Link]
[Link]
DIFFRACTION PATTERN (DP)
Diffraction rules:
SC all planes
BCC h+k+l=even
FCC h,k,l unmixed
THANK YOU
REFLECTION PLANES IN CUBIC LATTICE
