X-rays

X-rays were discovered accidentally by

Wilhem C. Roentgen in 1895, while working with
conduction of cathode rays.

Wilhem Conard Roentgen

Initially Nature unknown, name as X-rays.

First Nobel Prize for Physics in 1901.

First X-ray images

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Production of X-rays

X-rays are produced when rapidly moving electrons that have been
accelerated through a potential difference of order 1 kV to 1 MV strikes a
metal target.
Evacuated
glass tube

Target

Filament

Electrons from a hot element are accelerated onto a target anode.

When the electrons are suddenly decelerated on impact, some of the

kinetic energy is converted into EM energy, as X-rays.

Less than 1 % of the energy supplied is converted into X-radiation during

this process. The rest is converted into the internal energy of the target.

Bremsstrahlung:

Radiative energy loss (E) by electrons

slowing down on passage through a
material
is the deceleration of the incident
electron by the nuclear Coulomb
field
radiation energy (E) (photon) is
emitted.
With materials of high atomic number
the energy loss is higher
The energy loss by Bremsstrahlung
> 99% of kinetic E loss as heat
production
it increases with increasing electron
energy
X Rays are dominantly produced by
Bremsstrahlung

Characteristic x-rays:

Starts with ejection of emainly from k shell (also

possible for L, M,) by
ionization.
e- from L or M shell fall into
the vacancy created in the k
shell.
Energy difference is emitted
as photons.
A sequence of successive
electron transitions between
energy levels.
Energy of emitted photons
is characteristic of the atom

5
Complete X-rays spectrum form x-ray tube

Production of Characteristic X-rays

Properties of X-rays

X-rays travel in straight lines.

X-rays cannot be deflected by electric field or magnetic field.
X-rays have a high penetrating power.
Photographic film is blackened by X-rays.
Fluorescent materials glow when X-rays are directed at them.
Photoelectric emission can be produced by X-rays.
Ionization of a gas results when an X-ray beam is passed
through it.

X-ray Spectra

Using crystal as a wavelength selector, the intensity of different

wavelengths of X-rays can be measured.

The graph shows the following features.

A continuous background of X-radiation in which the intensity varies

smoothly with wavelength. The background intensity reaches a
maximum value as the wavelength increases, then the intensity falls at
greater wavelengths.

Minimum wavelength which depends on the tube voltage. The higher

the voltage the smaller the value of the minimum wavelength.

Sharp peaks of intensity occur at wavelengths unaffected by change of

tube voltage.
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Minimum wavelength in the X-ray

Spectra

When an electron hits the target its entire kinetic energy is converted into
a photon.
The work done on each electron when it is accelerated onto the anode is
eV.
Hence hf = eV and the maximum frequency

eV
f max
h

Therefore,

m in

hc 12400 X10 10

eV
V

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Characteristic X-ray Spectra

Different target materials give different wavelengths for the peaks in the
X-ray spectra.

The peaks are due to electrons knock out inner-shell electrons from target
atoms.

When these inner-shell vacancies are refilled by free electrons, X-ray

photons are emitted.

The peaks for any target element define its characteristic X-ray spectrum.

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Uses of X-rays

In medicine
To diagnose illness and for treatment, Detection
of fracture

In industry
To locate cracks in metals.

X-ray crystallography
To explore the structure of materials.

To identify unknown elements.

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Moseleys Law

Frequency of characteristic X-ray emitted

is proportional to square of the target atomic number.

Z2
a ( Z b)

Where a is constant of proportionality and b is the screening constant.

b=1 for K x-ray
b =7.4 for L x-ray
#This Law was also well supported by Bohrs theory.

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Importance of Moseleys Law

1.

It yields a unique method for identifying as well as for classifying

different elements in the periodic table.

2. It is helpful in determining Z of rare earth elements and position in

periodic table.
3. New elements were discovered and arranged in the periodic table using
this law.

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Diffraction methods
In practice, many different experimental methods have been
designed since diffraction was discovered.
Each method has its own specialties and can be selected
according to the nature of the sample and the nature of the
problem to be solved.
Various types of radiation can also be selected, X-rays,
neutron or electron.
In this case and for the sake of simplicity, we shall limit our
choice to X-ray radiation although the techniques presented
here are also valid for neutron diffraction and partially for
electron diffraction.
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Braggs law

The diagram shows only two scattering planes, but implicit here is the presence of
many parallel, identical planes, each of which is separated from its adjacent
neighbor by a spacing d.
Constructive interference occurs when (A+B)/= n, coinciding with Braggs law, n
= 2dsin . The integer n refers to the order of diffraction. For n = 1, (A+B) = and
for n = 2, (A+B) = 2 etc.
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X-Rays to Determine Crystal Structure

The X-ray are used for crystal structure determination because the
wavelength of x-rays is comparable to interplanar spacing of crystals.

reflections must
be in phase for
a detectable signal

extra
distance
traveled
by wave 2

Braggs law: 2d sin = n

Measurement of critical angle, , allows
computation of planar spacing, d.

X-ray intensity

spacing
between
planes

n
2 sin

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Single crystal diffraction

Laues method - variable, fixed.
Rotating crystal method - fixed, variable to some extent.
Why not single crystal methods?
It may be difficult to obtain a single crystal.
The usual form of a material may be polycrystalline.
Powder diffraction
In this method the crystal is reduced to a fine powder and is
placed in a beam of monochromatic X-rays. Each particle is a
tiny crystal or an assemblage of smaller crystals randomly
oriented with respect to the incident beam.
Powder methods - fixed, variable.

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Laue method:
The method is based on;

a fixed crystal and

a variable spectrum of wavelength

work in transmission mode, i.e. the diffracting crystal

lies between the source of the incident beam and the
recording screen
whereas in the reflection mode, the screen is located
between the source and the crystal.
their directions are determined solely by the orientations
of the set of planes with Miller indices hkl.
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The Laue method:Schematic of Bragg spectrometer.

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Q. The Bragg angle for the first order reflection from (1,1,1) plane in a
crystal is 600. Calculate the inter-atomic spacing if X-ray of
wavelength 1.8 10-10 m is used.

Given

600

1.8 1010 m,
n 1
h k l 1
Let Inter atomic spacing a
and int er planer spacing d
a
a
Since d hkl

3
h2 k 2 l 2
from Bragg' s law 2d sin n
a 1.8 1010 m
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Rotating crystal
Method:

One of the most popular method to measure diffraction

patterns from single crystal.
used mainly for the resolution of unknown structures.
used a monochromatic beam (fixed wavelength) and the
crystal is rotated relative to the incident beam (variation in
).
The crystal is turned at constant angular speed through the
Bragg law position, and the total diffracted energy received
by the ionization chamber during this process is measured.

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Schematic of rotation camera:

The
monochromatic
primary beam s0 falls on
a small single crystal at
O. The crystal is mounted
with one of its axes (say,
a3) vertical, and it rotates
with constant velocity
about the vertical axis
during the exposure. The
various diffracted beams
are registered on a
cylindrical
film
concentric with the axis
of rotation.
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Numerical problem related to XRD:

Q. X-rays of wavelength 1.4 Ao is found to be Bragg reflected

from the (111) plane of an FCC structure. If the lattice
parameter of the crystal is 5 Ao, find the angle at which x-rays
are incident on the (111) plane of the crystal.
Ans.
a
a 5 1010 m
d111

h k
2

......m

n
140
111 sin
2d111
1

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Numerical problem related to XRD:

Q. Electrons accelerated from the state of rest by 120 V are reflected from
an fcc crystal. The reflection maximum is observed at 220. Calculate the
lattice parameter if the Bragg reflection occurs from the (111) plane.
Hint:

h
h
h

.
p
2mT
2meV
once is knownthen
d111 ..........as is known.

a
and as for fcc d111
a 2.589 Ao
3

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NON DESTRUCTIVE TECHNIQUES

Nondestructive techniques are a wide group of analysis techniques used in
science and industry to evaluate the properties of a material, without causing
any damage to it.
These techniques are highly-valuable because these can save both money and
time in troubleshooting, and research.

Some common Non-destructive Techniques:

1. X-ray Diffraction: Laue method, Braggs method
2. X-ray Fluorescence Spectrometry
3. Particle Induced X-ray emission technique
4. Neutron Activation analysis.

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Some Uses of Non destructive techniques:

Determination of impurity atoms in solids

Flaw Detection and Evaluation

Leak Detection

Location Determination

Dimensional Measurements

Structure and Microstructure Characterization

Estimation of Mechanical and Physical Properties

Stress (Strain) and Dynamic Response Measurements

Material Sorting and Chemical Composition Determination