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Rapid Recording of Powder Diffraction Patterns With Si(Li) X-Ray Energy Analysis System: W and Cu Targets and Error Analysis*

Published online by Cambridge University Press:  06 March 2019

Cullie J. Sparks Jr
Cullie J. Sparks Jr*
Affiliation:
Oak Ridge National Laboratory Dale A. Gedcke, ORTEC, Inc. Oak Ridge, Tennessee 37S30
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Abstract

X-ray diffraction patterns using continuous radiation from copper and tungsten target x-ray tubes and detected with a Si(Li) energy analysis system are presented. Errors caused by a misaligned diffractometer and x-ray penetration into the sample are shown to be more difficult to correct and larger in magnitude than errors arising from energy calibration. All these errors can be minimized by mixing a standard with the unknown sample.

The energy resolution of the detector influences the breadth of the diffraction peaks more strongly than the standard slit systems available with commercial diffractometers. Thus, to reduce the recording time and maintain the same standard deviation for the data, one should increase the sizes of the front and receiving slits including the Soller slits. X-ray energy diffraction patterns can be recorded with standard deviations less than +0.001 Å in the d spacing with only 200 sec measurement time using the standard diffractometer slit system. Copper targets are probably as useful as tungsten even though the continuous intensity is about three times.less. Copper has fewer interfering characteristic lines, and its use permits convenient conversion to normal θ scanning diffractometer operation.

Type
Research Article
Information
Advances in X-Ray Analysis , Volume 15: Twentieth Annual Conference on Applications of X-ray Analysis, August 11-13, 1971 , 1971 , pp. 240 - 253
Copyright
Copyright © International Centre for Diffraction Data 1971

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Footnotes

*

Research sponsored by the U.S. Atomic Energy Commission under contract with the Union Carbide Corporation.

References

1. Giessen, B. C. and Gordon, G. E., “X-Kay Diffraction: New High Speed Technique Based on X-ray Spectrography,” Science 159, 973–975 (1968).Google Scholar
2. Energy Dispersion X-Ray Analysis: X-Ray and Electron Probe Analysis, Amer. Soc. Test. Mater. Spec. Tech. Publ. 4-85, American Society for Testing and Materials, Philadelphia (1971).Google Scholar
3. Edmunds, I. G., Lipson, H., and Steeple, H., “The Determination of Accurate Lattice Parameters,” Chap. 15 in X-Ray Diffraction by Polycrystalline Materials, ed. by Peiser, H. S., Roaksby, H. P., and Wilson, A.J.C., The Institute of Physics, London (1955).Google Scholar
4. Bearden, J. A., X-Ray Wavelengths, NY0-105S6, U.S. Atomic Energy Commission, Division of Technical Information (1964).Google Scholar
5. Wilson, A.J.C., “Geiger-Counter X-Ray Spectrometer — Influence of Size and Absorption Coefficient of Specimen on Position and Shape of Powder Diffraction Maxima,” J. Sci. Instr. 27, 321–325 (1950).Google Scholar
6. Cole, H., “Bragg's Law and Energy Sensitive Detectors,” J. Appl. Cryst. 3, 405 (1970).Google Scholar
7. Gilfrich, J. V. and Birks, L. S., “Spectral Distribution of X-Ray Tubes for Quantitative X-Ray Fluorescence Analysis,” Anal.Chem. 40, 1077–1080 (1968).Google Scholar