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X-RAY DIFFRACTION

CONTENTS

Bragg`s Law
X-ray Powder Diffraction
X-ray Powder Diffractometer

X-ray diffraction
When a beam of X-ray radiation is incident upon a
substance, the electrons constituting the atoms of
the substance become as small oscillators.

These on oscillating at the same


frequency as that of incident X-ray
radiation emit EM radiations in all
directions at the same frequency.
Diffraction occurs as waves interact with a
regular structure whose repeat distance is
about the same as the wavelength .

When
certain
geometric
requirements
are
met,
X-rays
scattered from a crystalline solid can
constructively interfere, producing a
diffracted beam.

Bragg Equation History


English physicists Sir W.H.
Bragg and his son Sir W.L.
Bragg developed a relationship
in 1913 to explain why the
cleavage faces of crystals
appear to reflect X-ray beams
at certain angles of incidence
(theta, ).This observation is
an example of X-ray wave
interference.
Sir William Henry Bragg (1862-1942),
William Lawrence Bragg (1890-1971)

o In 1915, the father and son were


awarded the Nobel prize for physics "for
their services in the analysis of crystal
structure by means of X-rays".

Braggs law

The conditions for diffraction are


governed by Braggs law.
When the path length in the
crystal(2dsin) is a multiple of the
wavelength,
constructive
interference occurs and diffracted
intensity is obtained.

Above figure shows a monochromatic beam of Xrays incident on the surface of a crystal at an
angle .

P,Q & R represent the edges of a


family of planes distance d apart.
Plane P reflects AX in XD.
Plane Q reflects BY in YE at the same
angle .
Although the beam penetrates many
more planes we need to consider only
the top two.

Since Q is lower than P, the beam path


BYE is longer than AXD by the amount
GY+YH. This is called the path difference.
angle GXA=900
From GXY, sin=GY/d
Hence GY=d sin
From YXH, sin=YH/d
Hence YH=d sin
Therefore GY+YH=2d sin.

Now the two reflected rays, XD & YE


will constructively interfere when the
path difference is equal to the
wavelength or a multiple of it.
Thus condition for X-ray diffraction is
n=2d sin
where n is an integer(1.2.3 etc)
called the order of reflection.

X-RAY DIFFRACTION METHODS


X-Ray Diffraction Method

Laue

Rotating Crystal

Powder

Orientation
Single Crystal
Polychromatic Beam
Fixed Angle

Lattice constant
Single Crystal
Monochromatic Beam
Variable Angle

Lattice Parameters
Polycrystal (powdered)
Monochromatic Beam
Variable Angle

The Powder Method

The Powder Method


Experimental equipment consist of:
A X-ray source
Collimator
Powdered Crystals
A cylindrical film or camera to record the
diffraction pattern

If a monochromatic x-ray beam is directed at a


single crystal, then only one or two diffracted
beams may result.
A sample of some hundreds of crystals (i.e. a
powdered sample) show that the diffracted beams
form continuous cones. A circle of film is used to
record the diffraction pattern as shown. Each cone
intersects the film giving diffraction lines. The
lines are seen as arcs on the film.
If the sample consists of some tens of randomly
orientated single crystals, the diffracted beams
are seen to lie on the surface of several cones.
The cones may emerge in all directions, forwards
and backwards

A particular family of planes in a crystal will


only reflect an X-ray beam when the Bragg eqn
is fulfilled.
If a single crystal was placed in a X-ray beam,
then it would be a mere chance that a
particular family of plane was in the correct
position to satisfy the Bragg eqn.
Suppose we take the crystal and powder it. This
does not destroy the crystal structure, it simply
produces millions of very small crystals
pointing in all possible directions.

Thus if the powdered crystal is


placed in a monochromatic X-ray
beam, then for any particular family
of planes, there will be at least a few
having those planes satisfying the
Bragg eqn.

Above figure shows a powdered


crystal (A) irradiated with a
monochromatic X-ray beam.

CD represents a particular family of planes in a


crystal satisfying the Bragg eqn, so part of the
beam is reflected along AX.
In the same way a crystal having the same family
of planes orient along EF it reflects part of the
incident beam along AY.
Now the 2 crystals have the planes oriented at
to the beam and at right angles to the plane of
the paper.
The sample will also contain crystals having the
same family of planes oriented at to the beam
but not at right angles to the plane of the paper

This will give rise to reflections coming out of


and going into the plane of the paper.
Thus if we have all possible orientations of this
family of planes w.r.t to the plane of the paper
then a cone of reflected rays is produced of
semi vertical angle 2.
The sample will contain crystals having several
families of planes satisfying the Bragg eqn.
Since different families have different d
values the diffraction cones will have different
values of the semi vertical angle 2.

Thus the net result is the formation of a


series of concentric cones.

POWDER
DIFFRACTOMETER

Here a flat specimen is mounted on a turntable around which


moves a detector.
As the sample rotates , so the angle between the incident beam
and the sample changes.
Whenever the Bragg condition is fulfilled X-Rays are reflected to
the detector.
The detector is connected to the specimen table and geared in
such a way that when the table rotates through , the detector
rotates through 2 degrees.

This results in the detector always being in the correct


position to receive X-Rays from the sample.

Scintag PAD V diffractometer (-2)

Application of XRD
XRD is a nondestructive technique. Some of
the uses of x-ray diffraction are;

4.
5.

Differentiation between crystalline and amorphous


materials;
Determination of the structure of crystalline materials
Determination of electron distribution within the atoms,
and throughout the unit cell;
Determination of the orientation of single crystals;
Determination of the texture of polygrained materials;

6.

Measurement of strain and small grain size

1.
2.
3.

Advantages and disadvantages of Xrays


Advantages;
X-ray is the cheapest, the most
convenient and widely used method.
X-rays are not absorbed very much by air,
so the specimen need not be in an
evacuated chamber.
Disadvantage;
They do not interact very strongly with
lighter elements.

REFERENCES
Instrumental Methods of Chemical
Analysis by Gurdeep R. Chatwal and
Sham K. Anand.
X-Ray METHODS BY Clive Whiston.
Internet source.

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