L3-PPT-Crystal-diffraction-by-X-ray

Crystal diffraction by X-
ray
What is X-ray
Diffraction?
Diffraction occurs when each object in a periodic
array scatters radiation coherently, producing
concerted constructive interference at specific angles.
 Crystalline substances (e.g. minerals) consist of
parallel rows of atoms separated by a ‘unique’
mo phone neiki asithiba
distance, d.
 Diffraction occurs when radiation enters a crystalline
substance and is scattered
 Direction and intensity of diffraction depends on
orientation of crystal lattice with radiation
Detector
X-Ray
Source
Powdered
sample
Bragg‘s Law
 Bragg considered crystals to be made up of parallel planes of
atoms. Incident waves are reflected specularly from parallel
planes of atoms in the crystal, with each plane reflecting only a
very small fraction of the radiation
EF  d sin
DE  d sin
DE  EF  2d
sin
n  2d sin
 Constructive interference of the radiation from successive planes

occurs when the path difference is an integral number of
wavelenghts. This is the Bragg Law.
Bragg Equation
Since Bragg's Law applies to all sets of crystal planes,
the lattice can be deduced from the diffraction pattern,
making use of general expressions for the spacing of the
planes in terms of their Miller indices. For cubic structures
a
d
 2
h 2 k 2

l
Note that the smaller the spacing the higher the angle
of diffraction, i.e. the spacing of peaks in the diffraction
pattern is inversely proportional to the spacing of the planes
in the lattice. The diffraction pattern will reflect the symmetry
properties of the lattice.
Sample XRD
Pattern
strong intensity = prominent crystal plane
weak intensity = subordinate crystal plane
background radiation
strong intensity = prominent crystal plane
nλ = 2dsinθ
(1)(1.54) = 2dsin(15.5 degrees)
1.54 = 2d(0.267)
d = 2.88 angstroms
background radiation
d-spacing Intensity
2.88 100
2.18 46
1.81 31
1.94 25
2.10 20
1.75 15
2.33 10
2.01 10
1.66 5
1.71 5
X-RAY DIFFRACTION
METHODS
X-Ray Diffraction
Method
Lau Rotating Powde

e Crystal r
Lattice Parameters
Orientation Lattice constant
Polycrystal
Single Crystal Single Crystal
Polychromatic (powdered)
Monochromatic Beam Monochromatic
Beam Variable Angle Beam
Fixed Angle
Variable Angle
Crystal structure
determination by
• Laue method
The symmetry of the spot pattern reflects the
symmetry of the crystal when viewed along the
direction of the incident beam.
• Laue method is often used to determine the
orientation of single crystals by means of
illuminating the crystal with a continuos spectrum
of X-rays
• Although the Laue method can also be used to
determine the crystal structure, several wavelengths
can reflect in different orders from the same set of
planes, with the different order reflections
superimposed on the same spot in the film. This
makes crystal structure determination by spot
ROTATING CRYSTAL
METHOD
 In the rotating crystal method, a
single crystal is mounted with an
axis normal to a monochromatic
x-ray beam. A cylindrical film is
placed around it and the crystal
is rotated about the chosen axis.
 As the crystal rotates, sets of lattice planes will at some

point make the correct Bragg angle for the
monochromatic incident beam, and at that point a
diffracted beam will be formed.
ROTATING CRYSTAL METHOD
 Lattice constant of the crystal can be determined
by means of this method; for a given wavelength if
the angle at which a redflhekcl tion occurs is known,
can be determined. a
d
 h2 k 2
 l 2
 The reflected beams are located on the surface of

imaginary cones. By recording the diffraction
patterns (both angles and intensities) for various
crystal orientations, one can determine the shape
and size of unit cell as well as arrangement of
atoms inside the cell.
THE POWDER
METHOD
 If a powdered specimen is used, instead of a
single crystal, then there is no need to rotate the
specimen, because there will always be some
crystals at an orientation for which diffraction is
permitted. Here a monochromatic X-ray beam is
incident on a powdered or polycrystalline sample.
 This method is useful for samples that
are difficult to obtain in single crystal
form.
 The powder method is used to determine the value of
the lattice parameters accurately. Lattice parameters are
the magnitudes of the unit vectors a, b and c which
define the unit cell for the crystal.
 For every set of crystal planes, by chance, one

or more crystals will be in the correct orientation to
give the correct Bragg angle to satisfy Bragg's
equation.
Every crystal plane is thus capable of diffraction. Each
diffraction line is made up of a large number of small
spots, each from a separate crystal. Each spot is so
small as to give the appearance of a continuous line.
DEBYE SCHERRER
METHOD
 A very small amount of powdered material is sealed into a
fine capillary tube made from glass that does not diffract x-
rays.
The specimen is placed in

the Debye Scherrer camera
and is accurately aligned to
be in the centre of the
camera. X-rays enter the
camera through a collimator.
17
Debye Scherrer
Camera
 The powder diffracts the x-

rays in accordance with
Braggs law to produce
cones of diffracted beams.
These cones intersect a
strip of photographic film
located in the
cylindrical to
characteristic
camera set produce
of arcs on
the film. a
Powder diffraction
film
 When the film is removed from the
camera, flattened and processed, it shows the
diffraction lines and the holes for the incident
and transmitted beams.
XRD Technique
 Takes a sample of the material and places a
powdered sample which is then illuminated
with x-rays of a fixed wave-length.
 The intensity of the reflected radiation is
recorded using a goniometer.
 The data is analyzed for the reflection angle to
calculate the inter-atomic spacing.
 The intensity is measured to discriminate the
various D spacing and the results are compared
to known data to identify possible matches.
Powdering
Samples
The samples are powdered to give a random
sampling of ALL atomic planes (crystal faces)
 Statistically accurate given samples are powdered
finely AND randomly oriented on sample holder
 Intensities are a reflection of d-spacing abundance
 Problems arise with minerals that may
preferentially orient on sample holder
 Micas and clays have special preparation
techniques
Applications of
XRD
XRD is a nondestructive technique. Some of the uses of
x-ray diffraction are;
1. Differentiation between crystalline and

amorphous materials;
2. Determination of the structure of crystalline materials;
3. Determination of electron distribution within the atoms, and
throughout the unit cell;
4. Determination of the orientation of single crystals;
5. Determination of the texture of polygrained materials;
6. Measurement of strain and small grain size…..etc

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L3-PPT-Crystal-diffraction-by-X-ray

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Crystal diffraction by X-

 Constructive interference of the radiation from successive planes

Lau Rotating Powde

 As the crystal rotates, sets of lattice planes will at some

 The reflected beams are located on the surface of

 For every set of crystal planes, by chance, one

The specimen is placed in

 The powder diffracts the x-

1. Differentiation between crystalline and

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