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High Quality X-Ray Diffraction Data Using an Adjustable Divergence Slit and Thin Samples

Published online by Cambridge University Press:  28 October 2013

G. Kimmel
Affiliation:
Philips Laboratories, North American Philips Corporation, Briarcliff Manor, New York 10510, U.S.A.

Abstract

In the Bragg-Brentano X-ray powder diffractometer geometry the Automatic Divergence Slit (ADS) provides a fixed area of illumination on a flat specimen. For this case, the “constant volume” diffraction, appropriate for a Constant Divergence Slit (CDS) diffractometer, is not applicable and intensities must be corrected by a sinθ factor before comparison to CDS data.

It is shown that for thin layers the diffraction pattern may be treated as a “constant volume” diffraction case when the ADS is used. Moreover, the derivation of the unit cell dimensions using a common least-square procedure can result in excellent lattice parameters without using internal standards, because the transparency aberrations are minimized.

ADS data were obtained for a variety of reference materials including several NBS SRM powders. It was found that thin samples made of powder mixed with vaseline gave “constant volume” diffraction, less angular aberration, and yet had line intensities only somewhat less than bulk samples.

Three main benefits arise using a combination of thin layers and ADS: (a) The amount of material needed for routine chracterization is small, (b) The relative experimental intensities are approximately the same as those obtained from bulk specimens using a CDS. (c) The measured (Bragg) scattering angles are more accurate compared with those measured from bulk specimens.

Type
Research Article
Copyright
Copyright © Cambridge University Press 1987

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References

Bind, and McCarthy, , Penn. State Univ. (1973). PDF 251047 (1975).Google Scholar
Hubbard, C. R. (1983a). Certification of Si Powder Diffraction Standard Reference Material 640a. J. Appl. Crystallogr. 16 285288.CrossRefGoogle Scholar
Hubbard, C. R. (1983b). X-Ray Powder Diffraction Intensity Set, NBS Certificate, Standard Reference Material 674. Nat'l Bur. Stand. (U.S.) Office of Standard Reference Materials, Gaithersburg, MD 20899.Google Scholar
James, R. W. (1950). The Optical Principles of the Diffraction of X-Rays, p. 44. London: G. Bell and Sons, Ltd.Google Scholar
Jenkins, R. and Paolini, F. R. (1974). An Automatic Divergence Slit for the Powder Diffractometer. Norelco Reporter 21 No. 1, 914.Google Scholar
Morris, M. C., McMurdie, H. F., Evans, E. H., Paretzkin, B., Parker, H. S., Panagiotopoulos, N. C., and Hubbard, C. R. (1981). Nat'l Bur. Stand. (U.S.) Monogr. 25 18, 61.Google Scholar
Morris, M. C., McMurdie, H. F., Evans, E. H., Paretzkin, B., Parker, H. S., Pyrros, N. P., and Hubbard, C. R. (1984). Nat'l. Bur. Stand. (U.S.) Monogr. 25 20, 38.Google Scholar
Schreiner, W. N. and Surdukowski, C. (1982). Systematic and Random Powder Diffractometer Errors Relevant to Phase Identification. Norelco Reporter 29 No. 1, 4248.Google Scholar
Swanson, H. E., McMurdie, H. F., Morris, M. C. and Evans, E. H. (1969). Nat'l. But. Stand. (U.S.) Monogr. 25 7, 83.Google Scholar
Wilson, A. J. C. (1963). Mathematical Theory of X-Ray Powder Diffractometry. Philips Technical Library, Eindhoven.Google Scholar
Wolff de, P. M. (1957). Self-Centering Combined Aperture and Scatter-Slit for Powder Diffractometry with Constant Effective Specimen Area. Appl. Sci. Res. Sect. B 6, No. 5, 296300.CrossRefGoogle Scholar