C.Suryanarayana 8: M.G. Norton, "X-Ray
`
`Diffraction - A Practical Approach",
`
`Plenum, (1998), p. 240
`
`RS 1031 - 000001
`
`

`
`X-Ray Diffraction
`A Practical Approach
`
`C. Suryanarayana
`Coforado Schooi of Mines
`Golden, Coforado
`
`and
`
`M. Grant Non‘on
`
`Washingxon State University
`Pullman, Washington
`
`Plenum Press 0 New York and London
`
`RS 1031 - 000002
`
`

`
`Library ofCongress Cataloging in Publication Data _
`On file
`
`ISBN O-306-45744-X
`
`© ‘I998 Plenum Press, New York
`A Division of Plenum Publishing Corporation
`233 Spring Street, New York, N.Y. 10013
`http:/I'www.p1enum.com
`I0 9 8 7 6 5 4 3 2 1
`
`All rights reserved
`No part of this book may be reproduced, stored in a retrieval system, or transmitted in any
`form or by any means, electronic, mechanical, photocopying, rnicrofiin-ling, recording, or
`otherwise, without written permission from the Publisher
`Printed in the United States of America
`
`RS 1031 - 000003
`
`

`
`ii
`
`0 Experimental Modules
`
`It is desirable that you record the x-ray diffraction pattern with Cu Kot
`radiation since all the standard patterns in the PDF are recorded with this
`radiation, and it would be better to have the unknown and standard
`patterns recorded under similar conditions.
`(However, with modern
`computer software you can easily convert the data from one radiation to
`another. But you should realize that the relative intensities of the reflec-
`tions can be different when different radiations are used. Further, you can
`have the card display either the 29 values or the d spacings; d spacings are
`preferred because the search manuals list only a‘ spacings.) Convert all 29
`values into interplanar spacings (d values) and list the relative integrated
`intensities of all the reflections (remember to subtract the background
`intensity), assuming that the most intense reflection has an intensity of
`100%. Compute the d spacings to the nearest 0.01 A for low-angle peaks
`and to 0.001 A for high-angle peaks.
`Identifying the unknown material involves the following steps:
`1. Identify the three most intense reflections in the recorded pattern.
`Designate the interplanar spacing corresponding to the most in-
`tense peak by d,, that for the next most intense by dz, and the next
`one by d,.
`. Locate the proper d, group in the Hanawalt Search Manual.
`. Once you have found a reasonable match for dl, look for the closest
`match to dz.
`. Repeat the procedure for d,.
`. After the closest match has been found for d1, d2, and d3, compare
`their relative integrated intensities with the tabulated values.
`. When the d values and the intensities for the three most intense
`reflections from the observed pattern match well with any of those
`listed in the manual, locate the proper card and compare the d and
`intensity values for all the reflections. When full agreement is
`obtained, identification is complete.
`
`In practice, the unknown material may contain one or more phases.
`The procedure for identification, however, is the same in both cases except
`that if the material contains only one phase the identification is easy and
`relatively straightforward. Let's now see how an unknown material can
`be identified by using the x-ray diffraction technique and the Hanawalt
`Search Manual.
`
`Single-Phase Material
`
`The experimental 26, d, and 111, (where I is the intensity of any peak
`and III, is the ratio of any given peak to that of the most intense peak,
`
`RS 1031 - 000004