X-RAY DEFFRACTROMETRY FOR QUALITATIVE ANALYSIS OF MATERIALS

INSTRUCTED BY: Dr. JAYARATHNA M. PARTNERS NAME: MADURAPPERUMA C 1. KUMARA R.S.C.K 2. LIYANARACHCHI K.N 3. MADURANGA L.B.W.R 4. PRASATH T 5. PULLE V.A.S.A 6. PERERA R.A.D COURSE: MT GROUP: C DATE OF PRE: 28/10/2010 DATE OF SUB: 30/11/2010

TITLE: X-RAY DEFFRACTROMETRY FOR QUALITATIVE ANALYSIS OF MATERIALS INTRODUCTION: Analysis of a crystalline material using X ray diffraction patterns has become an extremely useful method of material analysis. The main X ray diffraction methods used to identify materials are, (1) Laue method (Transmission method, Back reflection method) (2) Rotating crystal method (3) Powder method (Debye-Schrrer camera method, Diffractometer method) During this practical, an attempt was made to identify a ceramic material using the Diffractometer method. THEORY: X rays that are being deflected off two parallel planes can either be superimposed constructively or destructively as shown below.

For first order constructive diffraction, = 2dsin MATERIALS AND APPARATUS: Apparatus: X-ray diffractometer Glass plate Materials: Ceramic powder sample

PROCEDURE: The ceramic sample was prepared to powder specimen of a size less than 10microns. The specimen was then prepared by placing the powder in the recess of the glass plate compacting it with enough pressure to cause cohesion between the powder and the glass plate. Then the surface was smoothened off. The slide was then fixed on the sample holder of the X ray diffractometer and the scanning unit was moved continuously over a circular scale and the variation of intensity was obtained against the changing angle on a strip chart. CALCULATIONS: = 1.5418 Imax= I4 = 150 = 150 Intensity for I2 th peak = 31100% = 100 d value for I2 th peak = 1.5418__ 2sin(20.9/2) Peak no.(Ii) I1 I2 I3 I4 I5 I6 I7 I8 I9 I10 I11 I12 I13 RESULTS: From the Hanwalt manual and the JCPPS card, the minerals that closely matched the given sample is closed to Genkinite mineral. 20.67% = 4.25036 d= 2 26.6 20.9 36.6 50.2 60 39.4 68 46.8 42.5 40.25 54.9 64.2 55.4 Intensity (%) 100 20.67 12.67 11.34 8 7 6.67 4.67 4.34 4 4 2.67 1.34 __ () 2sin 3.351101 4.25036 2.45521 1.81735 1.87184 2.28694 1.37862 1.94114 2.12703 2.24059 1.67237 1.45073 1.65845

DISCUSSION: We can get the maximum 3 peaks as I4, I7 & I9 . They have d values of 3.018, 2.276 & 1.907. In the genkinite, it has maximum intensity d values of 3.02, 2.27 & 1.93. In the chalcocite-high, it has maximum intensity d values of 3.05, 2.40 & 1.98. In the stetefeldtite, it has maximum intensity d values of 3.02, 2.61 & 1.85. Therefore firstly we can approximate the genkinite {(Pt,Pb)4Sb3}as prepared sample. Our 2 Vs intensity graph has 14 peaks. But chart has only 8d values. Except above 3 values, it has 5d values (1.91, 0.9, 2.15, 2.12, 1.27). Above observation table gives other values for practical intensities.

It can also be seen that in most of the d values for both quartz and Berlinite, the expected values for intensity are half of that of the obtained values. This may occur due to several reasons such as using a powder which contains a considerable no of particles whose size is greater than 10 microns, mixing of other impurity materials that have d values as those in which the intensity has shown a considerable increase. Another reason for the difference between the data collected from the Intensity~2 graph and the data obtained from the cards maybe due to the error that may have occurred in calculating the maximum intensity. As this intensity was calculated by projecting it beyond the boundaries of the paper an error may have occurred in calculating this value and this value may have been in turn been transferred to the other intensities as the other intensities are calculated relative to the maximum intensity. Another error that may have occurred is in selecting the average curve from which the height of a peak is calculated. Applying a high pressure without using a binder to cause cohesion while inserting the powder into the recess in the glass plate can also result in the particle taking certain orientations. This can also lead to high intensities for certain d values (this error can be avoided by using a binder to cause cohesion between the powder and the glass face.