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# X-RAY DIFFRACTION X-rays are electromagnetic waves with wavelengths thousand of times smaller than that of visible light.

For diffraction of X-rays, a grating of corresponding dimensions is required and hence a simple grating cannot be used. More over it is rather impossible to prepare artificially a grating of such fine dimensions. Atoms in crystals are arranged in a regular manner, the spacing between them is comparable to the wavelength of X-rays, and hence a crystal could act as a suitable natural grating for diffracting X-rays. Braggs law of X-ray diffraction:

Let us consider a crystal made up of equidistant parallel planes of atoms with the inter planner spacing d (Shown in Fig). Let a wave front of monochromatic X-ray beam of wavelength fall at a glancing angle on these atomic planes . Each atom acts as scattering center and scatters the X-rays in all directions. In a certain direction these scattered rays are in phase i.e., they interfere constructively while in other directions the rays are out of phase i.e., they interfere destructively. Let us consider the rays PE and QC inclined at an angle with the surface of the planes. They are scattered along ER and CS. Let us draw perpendiculars EB and ED to QC and CS. The length of the path QCS is greater than the length of the path PER. The path difference is BC+CD. From the figure BC = CD = d sin Therefore the path difference = 2d sin. According to the condition for constructive interference the path difference must be equal to integral multiples of wavelength. i.e., 2 d sin = n. Where n = 1,2,3,4 etc., is the order of the reflection. This condition is known as Braggs law. The Braggs law is a consequence of the periodicity of the space lattice. The law does not refer to the arrangement of basis of atoms associated with each lattice point. The composition of the basis determines the relative intensity of various orders for a given set of planes.
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Laue method:

Laue method of X-ray diffraction The experimental arrangement of Laue X-ray diffraction is shown in the figure above. It consists a source producing a beam of X-rays over a wide range of wavelengths. A single crystal is held stationary in the beam of X-rays. The rays after passing through the crystal are diffracted and recorded on a photographic plate at a certain distance from the crystal. Before passing through the crystal the X-rays are limited to a fine pencil of beam by slits. If a beam of X-rays of a certain wavelength passes in a given direction through the crystal diffractions cannot be expected. This is because very few sets of planes would be in a favorable position to meet the requirements for Bragg condition and reflection, of course be rare. But the source of X-rays is producing a whole range of wavelength in the continuous spectrum. Therefore for any value of d (inter planer spacing) and (glancing angle) there will be found in the X-ray beam some value of such that diffraction occurs. It is known that atoms of a crystal have an orderly arrangement in space. Hence the diffraction of X-rays will occur from many families of atomic planes. These diffracted rays are recorded on a photographic plate and form bright spots. The diffraction pattern on the photographic plate consists of a central spot and a set of spots arranged in a definite pattern about the central spot. This method is never used for crystal structure determination. In this case, several wavelengths may be reflected in different orders from a single plane, so that different orders of reflection may super impose on a single spot. Due to this fact, determination of basis is not possible. Laue method is used to study of the symmetry of the crystal and in the determination of orientation of crystals. The crystal used should be thin. The crystal otherwise would absorb Xrays.
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## Powder (Debye-Scherrer) Method:

In this method, a monochromatic X-ray beam is used and the specimen is in the form of fine powder (poly-crystalline). In this powder, every atomic plane is present in every possible orientation. The geometry of powder method is shown in figure. It consists a powder camera, in which the filmstrip is enclosed on the inner wall. The powder specimen is placed at center, either pasted on a thin fiber of glass or filled in a capillary glass tube. The monochromatic X-ray beam
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enters through a small hole in the camera and falls on the powder specimen. The powder diffracts some part of the beam while the remaining passes out through the exit. Since a large number of the crystals are randomly oriented in the powder, set of planes, which make an angle with the incident beam can have a number of possible orientations. Some of them will be in a position to reflect the radiation from an important set of planes. Hence, the reflected radiation lies on the surface of a cone whose apex is at the point of contact of the incident radiation with the specimen. If all the crystal planes of inter planar spacing d reflect at the same Bragg angle all reflections from a family lie on the same cone, whose vertex angle is 4. In this way a number of combinations of d and would satisfy Braggs law. Hence, the powder specimen emits many cones of diffracted rays. A part of each diffracted X-ray beam is recorded on the filmstrip. The recorded lines from any cone are a pair of arcs as shown in figure. It is observed that when rays are diffracted through small angles, they make arcs around the central spot on the film. When rays are diffracted through 900, the cones become flat and the corresponding trace is a straight line. When diffracted angle increases above 900, the traces are nearly circular. The cone angle 4 is determined by measuring distance between two corresponding arcs on the filmstrip. (Shown in figure). 4 2S/R (radians) where S is radius of an arc that belongs to a cone. Bragg angle S/2R Where R is the radius of the camera. Substitution of and in Braggs equation gives a list of inter planer spacing d. From these inter planer spacing; the type of the lattice can be identified.

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