2:15 PM - 2:45 PM
★ [SIT06-10] The Revolutionary Multigrain Crystallography Method for High-Pressure X-ray Diffraction
Keywords:High pressure X-ray diffraction, Crystallography
Single-crystal XRD contains orientation and geometrical relationship in addition to d-spacings and thus provides a definitive characterization of the unit cell and symmetry. Unless the crystal is orientated exactly relative to the incident monochromatic x-ray beam to satisfy the Bragg relation, the crystal gives no signal, and the detector remains empty. Rotating the crystal around the w-axis (perpendicular to the incident x-ray beam) can bring the crystal to Bragg condition and occasionally obtain single diffraction spots at a given angle and scanning step. In spite of the advantages, single crystal cannot be sustained through phase transitions and often breaks down into multiple crystals and generate spotty XRD patterns.
Spottiness, that is generally regarded as a flaw in powder XRD, can be turned into great advantages if we can separate individual crystallites and handle them as individual single crystals. The high-brilliance x-ray beam available at synchrotron facilities has made it possible to collect diffraction spots in a powder sample comprised of up to hundreds of submicron crystallites. The newly developed Multigrain Crystallography (MGC) package, which is a suite of programs used for processing and indexing diffraction spots, has been developed to separate and identify the crystallographic orientation of each individual crystallite in the aggregate of hundreds of crystallites. Once separated, the data set for each crystallite can be handled with the standard single-crystal refinement program identical to a stand-alone single crystal, resulting in excellent statistics in refinement and full coverage of the reciprocal space. The MGC method is very powerful in unequivocal determination of symmetry and unit cells, testing different indexing models, picking out minor phases, and resolving strain of individual crystallites, and will very likely replace the powder and single-crystal x-ray diffraction methods as the dominant crystallographic tool for future high pressure-temperature studies in DAC.