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EFFECT OF POWDER SAMPLE GRANULARITY ON FLUORESCENT INTENSITY AND ON THERMAL PARAMETERS IN X-RAY DIFFRACTION RIETVELD ANALYSIS C. J. Sparks, R. Kumar,* R D. Specht, P. Zschack,* G. E. Ice, T. Shiraishi,+ and K. Hisatsune* Oak Ridge National Laboratory P.O. Box 2008 Oak Ridge, Tennessee 37831-6118 INTRODUCTION The effect of sample granularity on diffracted x-ray intensity was evaluated by measuring the 28 dependence of x-ray fluorescence from various samples. Measurements were made in the symmetric geometry on samples ranging from single crystals to highly absorbing coarse powders. A characteristic shape for the absorption correction was observed. A demonstration of the sensitivity of Rietveld refined site occupation parameters is made on CuAu and CU5QAU44N15 alloys refined with and without granularity corrections. These alloys provide a good example of the effect of granularity due to their large linear x-ray absorption coefficients. Sample granularity and refined thermal parameters obtained from the Rietveld analysis were found to be correlated. Without a granularity correction, the refined thermal parameters are too low and can actually become negative in an attempt to compensate for granularity. A general shape for granularity correction can be included in refinement procedures. If no granularity correction is included, data should be restricted to above 30° 26, and thermal parameters should be ignored unless extreme precautions are taken to produce
