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Bragg's Law, Laue method, Powdermethod

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INTRODUCTION:”So far we have seen ideal crystal which is obtained by combining a basis with an infinite space lattice. In real crystal, the periodicity is not continuous within a crystal. So many properties of crystalline materials are structure sensitive. To explain this sensitivity the only possible way is X-Ray Diffraction.” Lattice Planes: A crystal is made up of a large number of parallel equidistant planes passing through lattice points called Lattice Planes. Interplanar Distance: The perpendicular distance between any two adjacent crystal planes is called Interplanar distance (d). Orientation of Planes:”In crystal analysis it is necessary to indicate the orientation of planes. The orientation of the planes can be described in terms of their intercepts on three axes(X, Y, and Z). This is shown in the figure.” In the figure the intercepts along X, Y and Z are pa, qb and rc respectively. Miller Indices: “The reciprocals of the intercepts made by a plane on the co-ordinate axis or crystallographic axis are called Miller Indices.” Procedure for finding Miller Indices: 1) Find the intercepts of the desired plane on the three co-ordinate axis. i.e., (pa, qb and rc) 2) Divide with primitives (a, b, c) then the intercepts are (p, q, r) 3) Take the reciprocals of the intercepts. i.e., (1/p, 1/q, 1/r). 4) Find the LCM of Denominators. 5) Reduce the reciprocals into integers by multiplying each of them with LCM. 6) Enclose these integers in brackets, which represent the Miller indices (h, k, l) of a given plane. Important Features of Miller Indices: 1) Miller indices represent the Orientation of Crystal Planes in a crystal. 2) A Plane parallel to any one of the co-ordinate axis will have infinite intercept, and the corresponding Miller index is Zero. 3) All equally parallel planes have the same Miller Indices (h, k, l). 4) When an intercept of plane is negative, the index is represented by bar over it. 5) If (h, k, l) are Miller Indices of a crystal plane, then the intercepts made by the plane with co-ordinate axis are a/h, b/k and c/l where a, b, c are lattice parameters. 6) A Plane passing through the origin is defined in terms of parallel planes having non zero intercepts.

PEC

Name of the Faculty: P.V.V.Satyanarayana

OY. k. and OZ and assume that a plane (hkl) parallel to the plane passing through the origin makes intercepts a/h. B and C respectively as shown in figure.V. In the case of Simple cubic system a = b = c. l] Planes (or) Relation between interplanar spacing and Miller indices: Let us consider three mutually perpendicular coordinate axis.Satyanarayana .V.Equation for Interplanar Distance (d) or Separation Between Successive [h. b/k and c/l on the three axes at A. then equation 2 becomes dhkl = 1 h + k +l 2 2 2 ∴ dhkl = a a 2 h +k +l 2 2 2 PEC Name of the Faculty: P. OX.

. this is called “Bragg’s Law”.. This angle also called Braggs Angle.” i.3... second order. at which the diffraction occurs.V. third order maxima ……………… etc respectively. O1Y1 respectively. For first maxima sin θ1 = λ/2d For second maxima sin θ2 = 2λ/2d For third maxima sin θ3 = 3λ/2d Therefore Sin θ1 : sin θ2 : sin θ3 = 1:2:3 PEC Name of the Faculty: P. 2d sin θ = nλ Where n = 1. Let us consider a set of parallel lattice planes of a crystal in which spacing between any two successive planes is ‘d’...e.V. So “Bragg’s law states that the X-Ray reflection from different parallel planes of a crystal... Let OP and OQ are perpendiculars drawn from ‘O’ on the rays X1O1 and O1Y1 respectively. Then the path difference between the incident and reflected ray is ∆ = PO1+O1Q------.Bragg’s Law: Bragg’s Law studied the diffraction of X-Rays from various parallel planes of a crystal and obtained condition called Bragg’s Condition.etc for first order...Satyanarayana . Consider the rays XO and X1O1 are incident on two consecutive planes AA1 and BB1. interfere constructively when the path difference is integral multiple of wave length of X-Rays. They are reflects along OY.(1) For the reflected light intensity to be maximum when the path difference ∆ = nλ Therefore 2d sin θ = nλ.2.. A narrow beam of XRay of wave length ‘λ’ be incident on the planes with glancing angle ‘θ’..

Limitations: 1.” The experimental arrangement consists of X-Ray Source. Crystal holder and Photographic Plate as shown in the figure. These X-Rays are allowed to pass through two collimating slits S1 and S2 to form a fine and sharp beam. This fine sharp beam allowed to fall on a single crystal specimen which is held at fixed angle. The X-Rays diffracted through the crystal is made to fall on photographic film placed in its front as shown in the figure. and Monochromatic Source) The Laue Method: “Laue method is used to study the crystal orientation and to verify the symmetry. PEC Name of the Faculty: P. The Symmetrical pattern of spots is called Laue Pattern. From Laue method it is possible to find the lattice constant and Interplanar spacing. Collimating slits (S1 and S2). Determination of Unit cell Dimensions is not possible. symmetry and also to study the crystal imperfections. Laue method is used to determine the structure of single crystal only.V.Satyanarayana . Poly chromatic Source) The Powder Method (Poly crystal in form of Powder. The Source produce the continues X-Rays of NaCl wave length (0. X-ray diffraction pattern of rock salt (common salt). The diffraction pattern consists of central spot surrounded by concentric circular spots.X-Ray diffraction Methods The Laue Method (Single fixed Crystal. Apparatus used by Max von Laue In Laue’s method diffraction pattern caused. and the wave lengths which satisfy the Bragg’s equation (2d sin θ = nλ). 2. Each spot in the Laue pattern corresponds to an interference maximum for a set of planes satisfying the Bragg’s condition. This method is useful for determine the crystal orientation.2 to 2Ao). by scattering of X-Rays at different atomic diffraction centers.V. The atomic arrangement can be understood from the position and intensities of the Laue’s Spots as shown in the figure. and Monochromatic Source) The Rotating Crystal Method (Single crystal at different angles.

Basic Principle The basic principle in this powder technique is that. The diffraction takes place for these values of θ and d which satisfy Bragg’s condition.. For the value of θ. The glancing angles (θ) corresponding to the rings on the films can be calculated by measuring the diameter of the rings (s) and knowing the camera radius R. which satisfy the Bragg’s condition. the crystal structures can be determined. the specimen contains a large number of micro crystals with random orientations. From the figure Diameter of the ring S = 4θ x R ∴ 4θ (radians) = S R Using the above expression. i. compounds and alloys also. the beam appears at the corresponding 2θ deviation. the specimen contains a large number of micro crystals (~1012 in 1mm3 of powder sample) with random orientations. This method is used to study the structure of crystals which cannot be obtained in the form of perfect crystals in shapes and sizes. 2d sinθ = nλ . i.1 Figure-1 Figure-2 Theory: The basic principle in this powder technique is that. The curvature of arcs reverses when the angle of diffraction exceeds900.. This monochromatic (or homogenous) x-rays can be converted into fine pencil beam by passing through the collimator.e.Powder Method (Debye.Satyanarayana . only parts of circular rings are register on it. λ PEC Name of the Faculty: P. 2 sin θ By knowing all parameters.V. Reflection takes place at the lattice planes. θ can be calculated. The pencil beam of X-rays is allowed to fall on the powder specimen (sample) as shown in the figure.. The finely powdered sample is filled in a thin capillary tube and mounted at the center of the drum shaped camera with photographic film at the inner circumference which Collect the monochromatic Xrays from the X-ray tube. i. d = . Then the interplanar spacing for various sets of parallel planes can be evaluated from the Bragg’s law as follows.V. Due to the narrow width of the film. When the film is laid flat the pattern recorded on the photographic film is shown in the figure-2. so almost all the possible θ and d values are available.e. It is shown in the figure. This method can be used for pure metals. almost all the possible θ and d values are available. The diffraction takes place for these values of θ and d which satisfy Bragg’s condition.Seherrer Method): The powder method was developed by Debye and Sherrer in Germany and by Hill in America simultaneously.e. 2d sinθ = nλ Experimental arrangement:The experimental arrangement is shown in figure.

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