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All Different Flavors of Synchrotron Single Crystal X-Ray Diffraction Experiments

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High-Pressure Crystallography

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.

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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.

    Article  Google Scholar 

  • Arndt, U.W. & Willis, B.T.M. (1966) Single Crystal Diffractometry. Cambridge: Cambridge University Press.

    Book  Google Scholar 

  • Baerlocher, C., McClusker L. B., et al. (2004) “Exploiting texture to estimate the relative intensities of overlapping reflections” Z. Kristallogr., 219, 803–812.

    Article  Google Scholar 

  • Burns, P.C. (1998): “CCD X-ray area detectors applied to the analysis of mineral structures” Canad. Mineral., 36, 847–853.

    Google Scholar 

  • Busing, W.R. & Levy, H.A. (1967) “Angle calculations for 3- and 4-circle X-ray and neutron diffractometers” Acta Cryst., 22, 457–464.

    Article  Google Scholar 

  • Dera, P. & Katrusiak, A. (1999) “Diffractometric crystal centering” J. Appl. Cryst., 32, 510–515.

    Article  Google Scholar 

  • 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.

    Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Hamilton, W. C. (1974). International Tables for X-ray Crystallography, Vol. IV, pp. 273–284. Birmingham: Kynoch Press. (Present distributor Kluwer, Dordrecht.)

    Google Scholar 

  • 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.

    Article  Google Scholar 

  • 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.

    Article  Google Scholar 

  • McMahon, M.I. (2005) “Structures from powders and poor-quality single crystals at high pressure” J. Synchrotron Rad. 12, 549–553.

    Article  Google Scholar 

  • 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.

    Google Scholar 

  • Poulsen, H.F. (2004) “Three dimensional X-ray diffraction microscopy” Springer Tracts in Modern Physics. Springer, Berlin.

    Book  Google Scholar 

  • 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.

    Article  Google Scholar 

  • Vaughan, G. B. M., Schmidt, S. et al. (2004) “Multicrystal approach to crystal structure solution and refinement” Z. Kristallogr. 219, 813–825.

    Article  Google Scholar 

  • Wessels, T., Baerlocher, C., et al. (1999) “Single-crystal-like diffraction from polycrystalline materials” Science, 284: 477–479.

    Article  ADS  Google Scholar 

  • Yamanaka, T. (2005) “Structural changes induced by lattice-electron interactions: SiO2 stishovite and FeTiO3 ilmenite” J. Synchrotron Rad., 12, 566–576.

    Article  Google Scholar 

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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.

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Correspondence to Przemyslaw Dera .

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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

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