High Resolution Powder Diffraction and Structure Determination

It is clear that high-resolution synchrotrons X-ray powder diffraction is a very powerful and convenient tool for material characterization and structure determination. Most investigations to date have been carried out under ambient conditions and have focused on structure solution and refinement. The application of high-resolution techniques to increasingly complex structures will certainly represent an important part of future studies, and it has been seen how ab initio solution of structures with perhaps 100 atoms in the asymmetric unit is within the realms of possibility. However, the ease with which temperature-dependence measurements can be made combined with improvements in the technology of position-sensitive detectors will undoubtedly stimulate precise in situ structural studies of phase transitions and related phenomena. One challenge in this area will be to develop high-resolution techniques for ultra-high pressure investigations in diamond anvil cells. This will require highly focused beams and very precise collimation in front of the cell down to dimensions of 50 {micro}m or less. Anomalous scattering offers many interesting possibilities as well. As a means of enhancing scattering contrast it has applications not only to the determination of cation distribution in mixed systems such as the superconducting oxides discussed in Section 9.5.3, but also to the location of specific cations in partially occupied sites, such as the extra-framework positions in zeolites, for example. Another possible application is to provide phasing information for ab initio structure solution. Finally, the precise determination of f as a function of energy through an absorption edge can provide useful information about cation oxidation states, particularly in conjunction with XANES data. In contrast to many experiments at a synchrotron facility, powder diffraction is a relatively simple and user-friendly technique, and most of the procedures and software for data analysis are familiar to laboratory diffractionists. This is reflected in the fact that there are already dedicated instruments for powder diffraction at a number of synchrotrons sources, including the NSLS, the Synchrotrons Radiation Source, Daresbury, the Photon Factory, Tsukuba and HASYLAB. In addition, most general purpose beamlines can be adapted for powder diffraction experiments fairly easily. Dedicated beamlines are also planned or under consideration at the next generation of synchrotrons sources, the European Synchrotron Radiation Facility, Grenoble, the Advanced Photon Source, Argonne, and the SPring-8 machine at Harima. These will be high brilliance sources with a much harder radiation spectrum that will offer many new possibilities for powder diffraction experiments, especially at energies above 10 keV