Bibliographic Citation
| Document |  836 K |
|---|---|
| Title | X-Ray Powder Diffraction Study of Synthetic Palmierite, K{sub 2}Pb(SO{sub 4}){sub 2} |
| Creator/Author | TISSOT JR.,RALPH G. ; RODRIGUEZ,MARK A. ; SIPOLA,DIANA L. ; VOIGT,JAMES A. |
| Publication Date | 2000 Dec 19 |
| OSTI Identifier | OSTI ID: 772052 |
| Report Number(s) | SAND2000-3189J |
| DOE Contract Number | AC04-94AL85000 |
| Other Number(s) | TRN: AH200115%%405 |
| Resource Type | Journal Article |
| Resource Relation | Journal Name: Powder Diffraction; Other Information: Submitted to Powder Diffraction; PBD: 19 Dec 2000 |
| Research Org | Sandia National Labs., Albuquerque, NM (US); Sandia National Labs., Livermore, CA (US) |
| Sponsoring Org | US Department of Energy (US) |
| Subject | 36 MATERIALS SCIENCE; ANNEALING; X-RAY DIFFRACTION; ELECTRON MICROPROBE ANALYSIS; GRAIN ORIENTATION; POTASSIUM SULFATES; LEAD SULFATES; CHEMICAL PREPARATION; CRYSTAL STRUCTURE |
| Related Subject | PALMIERITE; X-RAY POWDER DIFFRACTION; RIETVELD REFINEMENT; PREFERRED ORIENTATION; SYNTHESIS |
| Description/Abstract | Palmierite (K{sub 2}Pb(SO{sub 4}){sub 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 (00{ell}) 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 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 K{sub 2}Pb(SO{sub 4}){sub 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){angstrom}, c = 20.864(2) {angstrom}, space group R-3m (166), and Z = 3. |
| Country of Publication | United States |
| Language | English |
| Format | Medium: P; Size: 16 pages |
| Availability | OSTI as DE00772052 |
| System Entry Date | 2009 Dec 16 |
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