Abstract
This lecture reviews the main concepts, applications and capabilities of different non-conventional approaches to single-crystal x-ray diffraction (SXD) experiment utilizing synchrotron radiation for applications in high-pressure research. You will learn how such experiment can be designed and performed to best answer the scientific goals of your study and, at the same time overcome the main technical limitations imposed by the high-pressure device and type of measurement. The emphasis will be placed on experiments that cannot be performed using laboratory instruments, e.g. involving ultrahigh (>50 GPa) pressures, poor quality samples, laser heating in diamond anvil cell (DAC), etc. The main goal of the presentation is to convince you that even if you are not an expert crystallographer, with good understanding of the general basic principles of synchrotron SXD experiments in a DAC you can successfully use these techniques as valuable and easy tools in your own high-pressure research.
Access this chapter
Tax calculation will be finalised at checkout
Purchases are for personal use only
References
Angel, R.J., Bujak, M., Zhao, J., Gatta, G.D., & Jacobsen, S.D. (2007) “Effective hydrostatic limits of pressure media for high-pressure crystallographic studies” J. Appl. Cryst., 40, 26–32.
Arndt, U.W. & Willis, B.T.M. (1966) Single Crystal Diffractometry. Cambridge: Cambridge University Press.
Baerlocher, C., McClusker L. B., et al. (2004) “Exploiting texture to estimate the relative intensities of overlapping reflections” Z. Kristallogr., 219, 803–812.
Burns, P.C. (1998): “CCD X-ray area detectors applied to the analysis of mineral structures” Canad. Mineral., 36, 847–853.
Busing, W.R. & Levy, H.A. (1967) “Angle calculations for 3- and 4-circle X-ray and neutron diffractometers” Acta Cryst., 22, 457–464.
Dera, P. & Katrusiak, A. (1999) “Diffractometric crystal centering” J. Appl. Cryst., 32, 510–515.
Finger, L.W. & King, H. (1978) “A revised method of operation of the single-crystal diamond cell and refinement of the structure of NaCl at 32 kbar” Am. Mineral., 63, 337–342.
Friedrich, A., Haussühl, E., Boehler, R., Morgenroth, W., Juarez-Arellano, E.A., & Winkler, B. (2007) “Single-crystal structure refinement of diaspore at 50 GPa” Amer. Mineral., 97, 1640–1644.
Ice, G.E., Dera P., Liu, W., & Mao, H.K. (2005) “Adapting polychromatic X-ray microdiffraction techniques to high-pressure research: energy scan approach” J. Synchrotr. Rad., 12, 608–617.
Hamilton, W. C. (1974). International Tables for X-ray Crystallography, Vol. IV, pp. 273–284. Birmingham: Kynoch Press. (Present distributor Kluwer, Dordrecht.)
King, H.E. Jr & Finger, L.W. (1979) “Diffracted beam crystal centering and its application to high-pressure crystallography” J. Appl. Cryst., 12, 374–378.
Loveday, J.S., McMahon, M.I., & Nelmes R.J. (1990) “The effect of diffraction by the diamonds of a diamond-anvil cell on single-crystal sample intensities” J. Appl. Cryst., 23, 392–396.
McMahon, M.I. (2005) “Structures from powders and poor-quality single crystals at high pressure” J. Synchrotron Rad. 12, 549–553.
Miletich, R., Allan, D.R., & Kuhs, W.F. (2001) “High-pressure single-crystal techniques” chapter 14 in Hazen, R.M., Downs, R.T (eds.), Comparative Crystal Chemistry, Reviews in Mineralogy Vol. XLI, pp. 445–519. Washington, DC: Mineralogical Society of America and Geochemical Society.
Poulsen, H.F. (2004) “Three dimensional X-ray diffraction microscopy” Springer Tracts in Modern Physics. Springer, Berlin.
Sowa, H. & Ahsbahs, H. (2006) “High-pressure X-ray investigation of zincite ZnO single crystals using diamond anvils with an improved shape.” J. Appl. Cryst. 39, 169–175.
Vaughan, G. B. M., Schmidt, S. et al. (2004) “Multicrystal approach to crystal structure solution and refinement” Z. Kristallogr. 219, 813–825.
Wessels, T., Baerlocher, C., et al. (1999) “Single-crystal-like diffraction from polycrystalline materials” Science, 284: 477–479.
Yamanaka, T. (2005) “Structural changes induced by lattice-electron interactions: SiO2 stishovite and FeTiO3 ilmenite” J. Synchrotron Rad., 12, 566–576.
Acknowledgments
Development of novel high-pressure synchrotron SXD methodology and instrumentation at GSECARS, Sector 13, APS was supported by a grant from the MRI Program, Division of Materials Research, National Science Foundation (NSF-DMR-0521179). X-ray data were collected at GSECARS and HPCAT sectors, APS, Argonne National Laboratory. GSECARS is supported by the National Science Foundation, the U.S. Department of Energy, the W.M Keck Foundation, the U.S. Department of Agriculture and the State of Illinois. Use of the APS was supported by DOE-BES, under Contract No. DE-AC02-06CH11357. Help from and collaboration with Robert T. Downs, Charles T. Prewitt, Barbara Lavina, Lauren A. Borkowski, Oliver Tschauner, Hans-Peter Liermann, Wenge Yang, Vitali B. Prakapenka, Mark Rivers and Steven Sutton is gratefully acknowledged.
Author information
Authors and Affiliations
Corresponding author
Editor information
Editors and Affiliations
Rights and permissions
Copyright information
© 2010 Springer Science+Business Media B.V.
About this paper
Cite this paper
Dera, P. (2010). All Different Flavors of Synchrotron Single Crystal X-Ray Diffraction Experiments. In: Boldyreva, E., Dera, P. (eds) High-Pressure Crystallography. NATO Science for Peace and Security Series B: Physics and Biophysics. Springer, Dordrecht. https://doi.org/10.1007/978-90-481-9258-8_2
Download citation
DOI: https://doi.org/10.1007/978-90-481-9258-8_2
Published:
Publisher Name: Springer, Dordrecht
Print ISBN: 978-90-481-9257-1
Online ISBN: 978-90-481-9258-8
eBook Packages: Physics and AstronomyPhysics and Astronomy (R0)