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X-ray powder diffraction study of synthetic Palmierite, K2Pb(SO4)2

Published online by Cambridge University Press:  05 March 2012

Ralph G. Tissot ,
Mark A. Rodriguez ,
Diana L. Sipola  and
James A. Voigt
Ralph G. Tissot*
Affiliation:
Materials Characterization Department 1822, Sandia National Laboratories, Albuquerque, New Mexico 87185
Mark A. Rodriguez
Affiliation:
Materials Characterization Department 1822, Sandia National Laboratories, Albuquerque, New Mexico 87185
Diana L. Sipola
Affiliation:
Ceramic Materials Department 1843, Sandia National Laboratories, Albuquerque, New Mexico 87185
James A. Voigt
Affiliation:
Ceramic Materials Department 1843, Sandia National Laboratories, Albuquerque, New Mexico 87185
*
a)Electronic mail: rgtisso@sandia.gov
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Abstract

Palmierite (K2Pb(SO4)2) has been prepared via a chemical synthesis method. Intensity differences were observed when X-ray powder data from the newly synthesized compound were compared to the published powder diffraction card (PDF) 29-1015 for Palmierite. Investigation of these differences indicated the possibility of preferred orientation and/or chemical inhomogeneity affecting intensities, particularly those of the basal (00l) reflections. Annealing of the Palmierite was found to reduce the effects of preferred orientation. Electron microprobe analysis confirmed K:Pb:S as 2:1:2 for the for the annealed Palmierite powder. Subsequent least-squares refinement and Rietveld analysis of the annealed powder showed peak intensities very close to that of a calculated Palmierite pattern (based on single crystal data), yet substantially higher than many of the PDF 29-1015 published intensities. Further investigation of peak intensity variation via calculated patterns suggested that the intensity discrepancies between the annealed sample and those found in PDF 29-1015 were potentially due to chemical variation in the K2Pb(SO4)2 composition. X-ray powder diffraction and crystal data for Palmierite are reported for the annealed sample. Palmierite is trigonal/hexagonal with unit cell parameters a=5.497(1) Å, c=20.864(2) Å, space group R-3m(166), and Z=3.

Keywords

PalmieriteX-ray powder diffractionRietveld refinementpreferred orientationsynthesis

Information

Type
New Diffraction Data
Information
Powder Diffraction , Volume 16 , Issue 2 , June 2001 , pp. 92 - 97
Copyright
Copyright © Cambridge University Press 2001

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