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Relative merits of reflection and transmission techniques in laboratory powder diffraction

Published online by Cambridge University Press:  05 March 2012

Svend Erik Rasmussen
Svend Erik Rasmussen
Affiliation:
Department of Geology, Aarhus University, DK 8000 Aarhus C, Denmark
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Abstract

Data for the standard material NBS SRM 674, TiO2, were collected on two diffractometers: a) a Philips PW 1050/37 standard diffractometer of the Bragg-Brentano type equipped with a post diffraction curved Ge monochromator, b) a Stoe Stadi P diffractometer of transmission type equipped with a curved incident beam Ge monochromator. Both monochromators were set to select pure CuKα1 radiation. The reflection type instrument gives a much larger peak to background ratio than the transmission instrument, for which the background is much higher than with the reflection instrument. Rietveld refinements were carried out on both data sets with the programs DBWS-9807 and general structure analysis system (GSAS). The structural parameter of the oxygen atom of rutile depends neither on data set nor program, whereas, e.g., thermal displacement parameters seem to depend on both data set and program.

Type
Technical Articles
Information
Powder Diffraction , Volume 18 , Issue 4 , December 2003 , pp. 281 - 284
Copyright
Copyright © Cambridge University Press 2003

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References

Burdett, J. K., Hughbanks, T., Miller, G. J., Richardson, J. W., and Smith, J. V. (1987). “Structural-electronic relationships in inorganic solids: Powder neutron diffraction studies of the rutile and anatase polymorphs of titanium dioxide at 15 and 295 K,” J. Am. Chem. Soc. JACSAT 109, 3639–3646. acs, JACSAT CrossRefGoogle Scholar
Finger, L. W., Cox, D. E., and Jephcoat, A. P. (1994). “A Correction for Powder Diffraction Peak Asymmetry due to Axial Divergence,” J. Appl. Crystallogr. JACGAR 27, 892–900. acr, JACGAR CrossRefGoogle Scholar
Guinier, A. (1963). X-Ray Diffraction In Crystals, Imperfect Crystals, and Amorphous Bodies (W. H. Freeman, San Francisco), p. 104.Google Scholar
Inorganic Crystal Structure Database. (1999). Gmelin-Institut für Anorganische Chemie and Fachinformationszentrum FIZ Karlsruhe.Google Scholar
Larson, A. C., and Von Dreele, R. B. (2001). General Structure Analysis System (GSAS), Los Alamos National Laboratory Report LAUR 86-748.Google Scholar
Madsen, J. C., Skov, H. J., and Rasmussen, S. E. (1988). “An Inexpensive Automation of a Powder Diffractometer,” Powder Diffr. PODIE2 3, 91–92. pdj, PODIE2 CrossRefGoogle Scholar
Rasmussen, S. E. (1991). “Accessories for a Transmission Powder Diffractometer,” Powder Diffr. PODIE2 6, 172–173. pdj, PODIE2 CrossRefGoogle Scholar
Rasmussen, S. E. (1992). “The Use of a Post Diffraction Germanium Monochromator with a Bragg-Brentano Type Powder Diffractometer,” Powder Diffr. PODIE2 7, 164–165. pdj, PODIE2 CrossRefGoogle Scholar
Shintani, H., Sato, S., and Saito, Y. (1975). “Electron-density distribution in rutile crystals,” Acta Crystallogr., Sect. B: Struct. Crystallogr. Cryst. Chem. ACBCAR 31, 1981–1982. acb, ACBCAR CrossRefGoogle Scholar
Wölfel, E. R. (1983). “A novel curved position sensitive proportional counter for X-ray diffractometry,” J. Appl. Crystallogr. JACGAR 16, 341–348. acr, JACGAR CrossRefGoogle Scholar
Young, R. A., Sakthivel, A., Moss, T. S., and Paaiva-Santos, C. O. (1995). “DBWS-9411- an upgrade of the DBWS*.* programs for Rietveld refinement with PC and mainframe computers,” J. Appl. Crystallogr. JACGAR 28, 366–367. acr, JACGAR CrossRefGoogle Scholar