Abstract
In this Chapter we give an overview of the use of modern powder diffraction techniques that are applied to real data collected with in angular-dispersive geometry at a state-ofthe-art synchrotron beamline, using large-volume apparatus to generate high-pressure and temperature conditions. The general theme is to obtain as much information as possible from the data, and we touch, without going into excessive detail, all steps that could be involved in any study undertaken at a beamline similar to ID30 at the ESRF. The techniques described here provide the basic grounding for all in situ investigations that couple this diffracting geometry with large-volume samples. The various stages of data collection and analysis are shown with examples, using, as far as possible, those programs that are freely available.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
Preview
Unable to display preview. Download preview PDF.
References
Hammersley, A. P., Svensson, S. O., Hanfland, M., Fitch, A. N., Haüsermann, D. (1996) Two-dimensional detector systems: From real detector to idealised image of two-theta scan. High Pressure Research, 14, 235–248
Crichton, W. A., Parise, J. B., Breger, J., Müller, H., Hanson, T. (2003) Hydrothermal synthesis, powder structure determination and equation of state of MgOHF (in preparation)
The POWDER DIFFRACTION FILE (PDF-2, PDF-4) databases are property of the International Center for Diffraction Data, http://www.icdd.com
Cheary, R. W., Coelho, A. A. (1996). XFIT deposited, with tutorials at http://www.ccp14.ac.uk/tutorial/xfit95/xfit.htm
Dragoe, N (1999) POWDER V2.00 written by N. Dragoe, version E: 1999–03-03, http://www.ccpl4.ac.uk
Crichton, W. A., Vaughan, G. M. B., Mezouar, M. (2001) In situ structure solution of helical sulphur at 3 GPa and 400°C. Zeischrift für Kristallographie, 216, 417- 419
Finger, L. W., Cox, D. E., Jephcoat, A. P. (1994) A correction for powder diffraction peak asymmetry due to axial divergence. Journal ofApplied Crystallography, 27, 892–900
Shirley, R. (2000) “The CRYSFIRE system for automatic powder indexing: user’s manual” The Lattice Press, 41 Guilford Park Avenue, Guilford, Surrey, England.
Visser, J. W. (1969) A fully automatic program for finding the unit cell from powder data. Journal of Applied Crystallography, 2, 89–95
Taupin, D. (1973) A powder-diagram automatic-indexing program. Journal of Applied Crystallography, 6, 380–385
Boultif, A. and D. Loüer (1991) Indexing of powder diffraction patterns for low symmetry lattices by the successive dichotomy method. Journal ofApplied Crystallography, 24, 987–993
CHECKCELL and CELREF part of the suite of programs written at the Laboratoire des Materiaux et du Genie Physique de l’Ecole Supérieure de Physique de Grenoble by Jean Laugier and Bernard Bochu. Full tutorials available at http://www.ccpl4.ac.uk
Wolff, P. M. de (1972) The definition of the indexing figure of merit M(20). Journal of Applied Crystallography, 5, 243 - 245
POWDERCELL, written by W. Kraus and G. Nolze of the Federal Institute for Materials Research and Testing (BAM), Berlin, version 2.3 1999
ERACEL, written by A. Le Bail. Archived at http://www.cristal.org/ftp/eracel.zip
Holland, T. J. B., Redfern, S. A. T. (1997) Unit cell refinement from powder diffraction data: the use of regression diagnostics. Mineralogical Magazine, 61, 65–77
Hahn, T. (1996) Editor, “The international tables for crystallography” Volume 3. 4th Edn Kluwer Academic, Dordrecht.
Le Bail, A. Duroy, H. Duroy, Fourquet, J. L. (1988) Ab-initio structure determination of LiSbW06 by x-ray powder diffraction. Materials Research Bulletin, 23, 447–452
Larson, B., Von Dreele, A. C. (1994) “General Structure Analysis System (GSAS)” Los Alamos National Laboratory Report LAUR 86–748
RIETICA, written by B. A. Hunter, current version 1.7.7; references to IUCR Powder Diffraction, 22, 21 (1997) and Le Bail ibid. available from http://www.ansto.gov.au/ansto/neut/s_hun.html
Toby, B. H. (2001) ExPGUI, a graphical user interface for GSAS. Journal ofApplied Crystallography, 34, 210–213
Altomare, A., Burla, M. C., Carnalli, M., Carrozzini, B., Cascarano, G., Giacovazzo, C., Guagliardi, A., Moliterni, A. G. G., Polodori, G., Rizzi, R. (2003) EXPO and SIR97 release 1.01, available from http://www.irmec.ba.cnr.it
Putz, H., Schön, J. C., Jansen, M. (1999) Combined method for ab initio structure solution from powder diffraction data. Journal ofApplied Crystallography, 32, 864- 870
Le Bail, A. (2001) EsPOIR: A program for solving crystal structures by Monte Carlo analysis of powder diffraction data. Materials Science Forum, 378, 47–52
Favre-Nicolin, N., Cerny, R. (2002) Fox, ‘free objects for crystallography’: a modular approach to ab initio structure determination from powder diffraction. Journal ofApplied Crystallography, 35, 734–743
Hannemann, A., Hundt, R., Schön, J. C., Jansen, M. (1998) A new algorithm for space-group determination. Journal ofApplied Crystallography, 31, 922–928
Hundt, R., Schön, J. C., Hannemann, A., Jansen, M. (1999) Determination of symmetries and idealized cell parameters for simulated structures. Journal ofApplied Crystallography, 32, 413–416
OVFRLAP, written by A. Le Bail. Available at http:/www.cristal.org
Crichton, W. A., Mezouar, M., Monaco G., Falconi, S. (2003) Phosphorus: New in situ powder data from large-volume apparatus. Powder Diffraction, 18, 155–158
Grzechnik, A., Crichton, W. A., Syassen, K., Adler, P., Mezouar, M. (2001) A new polymorph of ZrW2O8 synthesized at high pressures and temperatures. Chemistry of Materials, 14, 4255–4259
ICSD database, property of FIZ-Karlsruhe, http://www.fiz-karlsruhe.de
Ackermann, R. J., Chang, A. T., Sorrell, C. A. (1977) Thermal expansion and phase transition of the U3O8-Z phase in air. Journal of Inorganic and Nuclear Chemistry, 39, 75–85
Young, R. A. (1993) Editor “The Rietveld method”, Oxford University Press.
McClusker R., Von Dreele, R. B., Cox, D. E., Loüer, D., Scardi, P. (1999) Rietveld Refinement Guidelines. Journal ofApplied Crystallography, 32, 36–50
ATOMS, version 5.0.4, written by E. Dowty (1999). Commercial software, betas are available for download at http://www.shapesoftware.com
Burnett, M. N., Johnson C. K.(1996) “ORTEP-III: Oak Ridge Thermal Ellipsoid Plot program for crystal structure illustrations”. Oak Ridge National Laboratory Report ORNL-6895
Hall, S. R, Allen, F. H., Brown, I. D. (1991) The Crystallographic Information File (CIF): A new standard archive file for crystallography. Acta Crystallographica, A47, 655–685.
Spek, A. L. (2003) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands.
Author information
Authors and Affiliations
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2004 Springer Science+Business Media New York
About this paper
Cite this paper
Crichton, W.A., Mezouar, M. (2004). From Phase Identification to Structure Solution: X-Ray Crystallography at High Pressures. In: Katrusiak, A., McMillan, P. (eds) High-Pressure Crystallography. NATO Science Series, vol 140. Springer, Dordrecht. https://doi.org/10.1007/978-1-4020-2102-2_8
Download citation
DOI: https://doi.org/10.1007/978-1-4020-2102-2_8
Publisher Name: Springer, Dordrecht
Print ISBN: 978-1-4020-1954-8
Online ISBN: 978-1-4020-2102-2
eBook Packages: Springer Book Archive