METAL DETECTION BY XRD

Deb kumar Rath

419PH2122
 CONTENTS
 INTRODUCTION
 GENERATION OF X-RAYS
 PRINCIPLE
 INSTRUMENTATION
 METHODS
 APPLICATIONS
 CONCLUSIONS
 REFERENCES
 INTRODUCTION
 X-rays were first discovered by Wilhelm Roentgen who called
them x-rays because the nature at first was unknown so, x-rays
are also called the Roentgen rays.

 X-ray diffraction was first discovered by Max von laue.

 The wavelength range is 10-7 to about 10-15 m.

 X-RAYS
 X-rays are short wave length electromagnetic radiations
produced by the deceleration of high energy electrons in the
inner orbital of the atoms.
 X-ray region is 0.1 to 100 Aο.
 PRINCIPLE
 x-ray diffraction is based on constructive interference of
monochromatic x-rays and a crystalline sample. These x-rays are
generated by a cathode ray tube, filtered to produce
monochromatic radiation, collimated to concentrate and directed
towards the sample. The interaction of incident rays with the
sample produces constructive interference when
conditions satisfy Bragg’s law.
 BRAGG’S EQUATION
The path difference between ray1 and ray2 is equals to
Δ=2dsinƟ
For constructive interference the path difference should be the integral multiple of wavelength of the x-rays.
So 2dsinƟ = nλ
This is called Bragg’s law.
 INSTRUMENTATION
 Production of x-rays
 Collimator
 Monochromator
a.Filter
b.Crystal monochromator
 Detectors
a.Photographic methods
b.Counter methods
INSTRUMENTATION OF XRD
3D VIEW
 PRODUCTION OF X-RAYS
 X-rays are produced when high velocity electrons impinge on
metal target.
 Approximately 1%of the total energy of electron beam is
converted into x-ray radiations.
 Remaining are dissipated as heat.
 Many types of x-rays tube are available which are used for
producing x-rays.
 On striking the target electron transfer their energy to its
metallic surface which gives off x-ray.
X-ray tube
 COLLIMATOR
•In order to get a narrow beam of x-rays ,the x-rays generated by the target materials are allowed to pass
through a collimator which consists of two sets of metallic plate separated by a small gap.
•The collimator absorbs all the x-rays except the narrow beam to pass through the gap.
 TYPES OF MONOCHROMATORS
 Two methods of monochromatization are used.
 One is 1) filter and another is 2) crystal monochromator.
 Again the later is also two types
a)flat crystal monochromator
b)curved crystal monochromator
 The material used for monochromator are NaCl,quartz etc.
 FILTER: X-ray beam may be partly monochromatized by
insertion of a suitable filter. Filter allows the radiation of
required wavelength to pass.
 CRYSTAL MONOCHROMATOR: It is made up of suitable
crystalline material poistioned in the x-ray beam so that the
angle of reflecting planes satisfied the Bragg’s equation for
the required wavelength.the beam is split up into components
of wavelengths.Nacl,lithium fluoride, quart are used.
 DETECTORS
 The x-ray intensities can be measured and recorded either by
1)Photographic method
2)Counter methods
 Again counter methods is also five types
a)Geiger-Muller tube counter
b)Proportional counter
c)Scintillation detector
d)Solid state semiconductor detector
e)Semiconductor detectors
 Both these types of methods depends upon ability of x-rays to ionize matter and differ
only in the subsequent fate of electrons produced by the ionizing process.
 X-RAY DIFFRACTION METHODS
 These are generally used for investigating the internal structures
and crystal structures of various solid compounds.
 They are
1)Laue’s photographic method
a)Transmission method
b)Back reflection method
2)Bragg’s X-ray spectrometer method
3)Rotating crystal method
4)Powder method
 a)TRANSMISSION LAUE METHOD
 In the transmission Laue method, the film is placed behind the crystal to record beams which are
transmitted through the crystal.
 One side of the cone of Laue reflections is defined by the transmitted beam. The film intersect the
cone, with the diffraction spots generally lying on an ellipse.
 Can be used to orient crystals for solid state experiments.
 Most suitable for the investigation of preferred orientation sheet particularly confined to lower
diffraction angles.
 Also used in determination of symmetry of single crystals.
 b)BACK-REFLECTION METHOD
 In the back-reflection method, the film is placed between the x-ray source
and the crystal. The beam which are diffracted in a backward direction are
recorded.
 One side of the cone of Laue reflections is defined by the transmitted beam.
The film intersects the cone , with the diffraction spots generally lying on an
hyparabola.
 This method is similar to Transmission method however, back-reflection is
the only method for the study of large and thick specimens.
 Crystal orientation is determined from the position of the
spots.Each spot can be indexed , i.e. attributed to a particular
plane, using special charts.
 The Greninger chart is used for back-reflection patterns and the
Leonhardt chart for transmission patterns.
 The Laue technique is also used to assess crystal perfection from
the size and shape
 The Bragg’s X-RAY SPECTROMETER METHOD

 A-anti cathode
 B-B’-Adjustable slits
 C-crystal
 E-ionization chamber
 One end of ionization chamber is connected to the
positive terminal of a H.T. battery , while negetive terminal is
connected to quadrant electrometer(measures the strength of
ionization current.)
 The Bragg’s X-RAY SPECTROMETER METHOD

Working;
 Crystal is mounted such that Ө=00 and ionization chamber is adjusted to
receive x-rays.
 Crystal and ionization chamber are allowed to move in small steps
 The angle through which the chamber is moved is twice the angle through
which the crystal rotated
 X-ray spectrum is obtained by plotting a graph between ionization current
and the glancing angle
 Peaks are obtained.Peaks corresponds to Bragg’s reflection
 Different order glancing angle are obtained with known values of d and
nand from the observed value of θ , λ can be measured.
 DETERMINATION OF CRYSTAL STRUCTURE BY
BRAGG’S LAW
 X-ray falls on the crystal surface
 The crystal is rotated and x-rays are made to reflect from
various lattice planes
 The intense reflections are measured by bragg’s spectromter and
the glancing angles for each reflection is recorded.
 Then on applying Bragg’s equation ,ratio of lattice spacing for
various groups of planes can be obtained.
 Ratio will be different for different crystals.
 Experimentally observed ratio are compared with the calculated
ratios , particular structure may be identified.
 ROTATING CRYSTAL METHOD

 Photograph can be taken by

 1-Complete rotation method;in this method series of complete revolutions occur
 Each set of a plane in a crystal diffracts four times during rotation
 Four diffracted beams are distributed into a rectangular pattern in the central point of
photograph
 2-Oscillation method;the crystal is oscillated at an angle of 150 or 20
 The photographic plate is also moved forth and back with the crystal
 The position of the spot on the [plate indicates the orientation of the crystal at which the
spot was formed.
 POWDER CRYSTAL METHOD
 X-ray powder diffraction is a rapid analytical
technique primarily used for phase identification
of a crystalline material and can provide information
on unit cell dimensions.The analyzed material is finely
ground, homogenized, and avarage bulk composition is determined.
 Fine powder is struck on a hair with a gum , it is suspended vertically in the axix of a
vertical camera.
 When monochromatic beam is allowed to pass different possibilities may happen
1. There will be some particles out of random orientation of small crystals in the fine powder.
2. Another fraction of grains will have another set of planes in the correct positions for the
reflections to occur.
3. Reflection are possible in different orders for each set
 If the angle of incidence is θ then the angle of reflection will be 2θ.
 If the radius is r , the circumference 2πr corresponds to a scattering angle of 3600 .

Θ=360/ πr
 From the above equation the value of θ can be calculated and substituted in Bragg’s equation
to get the value of d .
 APPLICATIONS;
 Useful for determining the complex structure of metals and alloys.
 Characterization of crystalline materials
 Identification of fine-grained minerals such as clays and mixed layer clays that are difficult to
determine optically
optically.
 Determination of unit cell dimensions
 Measurement of sample purity
 APPLICATIONS OF XRD
1. Structure of crystals
2. Polymer characterization
3. State of anneal in metals
4. Particle size determination
5. Applications of diffraction methods to complexex.
a)Determination of cis trans isomerism
b)Determination of linkage isomerism
 CONCLUSIONS
 For materials including metals, minerals, plastics,
pharmaceuticals and semiconductors XRD apparatus provide
highly accurate tools for nondestructive analysis.
 The diffraction systems are also supported by an extensive range
of application software
REFERENCES
A. Elements of X-ray diffraction by B. D. Cullity
B. Google
C. youtube
THANK YOU