X-ray diffraction

Sudha R.

Aim

Introduction

X-ray production

XRD X-ray diffraction

XRD methods

Experiment

Sudha R.
Reg No: 1091316
M.Sc Physics(II-Yr)

PHYS 530 : Advanced Physics Lab M.Sc II CMP

20 October 2010
 Outline

X-ray diffraction

Sudha R.
1 Aim
Aim

Introduction
2 Introduction
X-ray production

XRD
3 X-ray production
XRD methods
Continuous X-rays
Experiment
Characteristic X-rays spectra

4 X-ray diffraction
Bragg’s law

5 XRD methods

6 Experiment
NaCl X-ray pattern
Experimental observation
Result
 Aim

X-ray diffraction

Sudha R.

Aim

Introduction

X-ray production

XRD

XRD methods To Measure the average spacings between layers or rows of atoms
Experiment To Determine the orientation of a single crystal or grain
To Find the crystal structure of an unknown Material
To Measure the size, shape and internal stress of small crystalline
regions
 Introduction : X-rays

X-ray diffraction

Sudha R.

Aim
What are X-rays?
Introduction
X-rays are electromagnetic waves of short wavelength in
X-ray production
the range 0.5Å to 10Å
XRD
How are X-rays produced?
XRD methods
Copper X-rays
glass
Experiment

Vacuum
Cooling water electrons
Tungsten filament To transformer

Target Metal focusing cap

Beryllum window X-rays

X-rays are produced when high velocity electrons strike a target material of
high atomic number.
 X-ray production : Continuous X-rays

X-ray diffraction High energy electrons are made to strike a target material. Most of the
Sudha R. energy of the electrons goes into heating the target material. A few fast
Aim
moving electrons penetrate deep into the interior of the atoms of target
Introduction
material and are attracted towards the nuclei by coulomb attraction. Due
X-ray production
to this, electrons are deflected from their original path. As a result of this,
Continuous the electrons are decelerated and hence energy of the electron decreases
X-rays
Characteristic continuously. This loss of energy during retardation is given off in the form
X-rays spectra
of X-rays of continuously varying energy with frequencies up to a max
XRD
frequency νmax or minimum wavelength λmin . This is called as continuous
XRD methods
x-rays.
Experiment
N
M
L ∆E = E − E0
e−
Photoelectron
K

Nucleus
e− E0

Incoming electron

Figure: An electron in the K shell is ejected from the atom by an external electron
 Characteristic X-rays spectra

X-ray diffraction

Sudha R. It consists of definite, well defined wavelength superimposed on Continuous

spectrum. These spectral lines generally occur in the form of small groups
Aim
and are characteristic of the target material.
Introduction

X-ray production
N
Continuous
X-rays M
Characteristic
X-rays spectra L ∆E = E − E0
e−
XRD K Photoelectron

XRD methods

Experiment Nucleus
e− E0

Incoming electron

An electron from the L or M shell Kβ and Kα2 will cause ex-

“jumps in” to fill the vacancy. In the tra peaks in XRD pattern, and
process, it emits a characteristic X-ray shape changes, but can be
unique to this element eliminated by adding filters
 X-ray diffraction

X-ray diffraction
What is X-ray diffraction?
Sudha R.
The atomic planes of a crystal cause an incident beam of X-rays to interfere
Aim with one another as they leave the crystal. The phenomenon is called X-ray
Introduction diffraction.
X-ray production X-ray diffraction (XRD) is a versatile, non-destructive technique that
XRD reveals detailed information about the chemical composition and
Bragg’s law
crystallographic structure of natural and manufactured materials.
XRD methods

Experiment
Diffraction pattern recorded

am
be
d r
acte
ffr
Di
2θ
Incident beam

Crystalline material
 Bragg’s law

X-ray diffraction

Sudha R.
Consider a set of parallel lattice planes having spacing d between each other
as shown below.
Aim
X-ray 2 X-ray 1
Introduction O
X-ray production

XRD
d
Bragg’s law
θ
XRD methods

Experiment
O
θ θ A B

A θ C
d
AB + BC = multiples of λ
B

Consider two rays incident on the lattice plane. After reflection, these rays
have a path difference of AB + BC. Constructive interference takes place if
this path difference is a multiple of wavelength. i.e.,

AB + BC = multiple of λ
 Bragg’s law. . .

X-ray diffraction

Sudha R.
O
Path difference = AB + BC
Aim
d
Introduction θ But AB = BC
X-ray production

XRD
∴ Path difference = 2AB
Bragg’s law A B
AB AB
XRD methods
From figure, sin θ = OB
= d
Experiment
∴ AB = d sin θ

∴ Path difference = 2d sin θ

Constructive interference takes place if path difference is an integral
multiple of wavelength.
∴ 2d sin θ = nλ
This relation is known as Bragg’s Law. The spacing of the atomic layers of
crystals can be found from the density and atomic weight. Both n and θ
can be measured and hence the wave length of X-rays can be measured by
using Bragg’s equation.
X-ray diffraction

Sudha R.
Constructive interference
Aim
In phase
Destructive interference
Introduction Out of phase

X-ray production D = Propagation direction

XRD AW D

Bragg’s law A = Amplitude

D = Propagation direction
C
XRD methods C = Vibration direction AW D

Experiment
A = Amplitude
AW 1 C D C
C = Vibration direction
Waves in phase: Path difference = 0

wavelength

AW 1 D

C
AR D
wavelength

C AR C D
Resultant AR = AW + AW 1 Resultant AR = AW − AW 1
 XRD methods

X-ray diffraction

Sudha R.

Aim

Introduction The Laue Method

X-ray production 1 Transmission laue technique
XRD
2 Back-reflection laue technique
XRD methods The Rotating crystal Method
Experiment The Powder Method
1 Debye-Scherrer Method
2 Focusing Technique
3 Pinhole Technique

Method λ θ
Laue method heterochromatic, variable fixed
Rotating crystal method monochromatic, fixed partly variable
Powder method monochromatic, fixed partly variable
 NaCl X-ray pattern

X-ray diffraction

Sudha R. NaCl
Aim

Introduction

X-ray production

XRD

XRD methods

Experiment
NaCl X-ray
pattern
Counts

Experimental
observation
Result

Position 2θ
 Experimental observation

X-ray diffraction
Measurement condition
Sudha R.
Starting position (2θ): 5.01
Aim

Introduction
End position (2θ): 59.99
X-ray production Anode material: Copper
XRD
Kα(Å): 1.54060
XRD methods

Experiment Peak values

NaCl X-ray
pattern
Position d spacing
Experimental
observation
(2θ) (Å)
Result 27.4652 3.24754
31.8217 2.81219
45.5522 1.99141
53.9710 1.69898
56.5932 1.62498

Formula to find lattice parameter:

dhkl
a0 = √
h2 + k 2 + l 2
 Result

X-ray diffraction

Sudha R.

Aim

Introduction

X-ray production

XRD

XRD methods

Experiment Lattice parameter for given sample (NaCl) :

NaCl X-ray
pattern Standard value : 5.635Å
Experimental
observation Calculated value : 4.867Å
Result