Crystal structure refinement of mantle minerals under high pressure and temperature using Rietveld method

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In-situ X-ray diffraction measurements under pressure were performed on several minerals and obtained powder diffraction patterns were analyzed by means of Rietveld structure refinement method. High pressure is generated by a diamond anvil cell (DAC) and X-ray diffraction experiments were mainly performed in synchrotron radiation facilities, such as PF and SPring8.Shortening of hydrogen bonded oxygen-oxygen distances controls compression of some hydrous minerals, such as KHCO_3 and NaHCO_3. A phase transition occurs on KHCO_3 at about 2.8 Gpa. It is interesting thai hydrogen bonded O-O distance in NaHCO_3 reaches to 2.4 A^^○ at 9 Gpa and this suggests a possibility of hydrogen bond symmetrization. Shortening of hydrogen bonded O-O distance also controls compression behavior of goethite and its shortening behavior is quite similar to that of ice VII.Laser annealing is quile useful for relaxing strain in materials caused by nonhydrostatic pressure Laser annealing was applied to compression experiments of NiTiO_3-ilmenite in PF. Obtained diffraction patterns after annealing treatment were greatly improved and Rietveld analysis could be done successfully up to 20 Gpa.Laser heating is a powerful method for creating lower mantle conditions on the earth. We performed insitu X-ray diffraction experiments under high pressure and temperature conditions at SPnng8 to clarify a possibility of a reaction between maguesite and iron. No evidence of the reaction was observed at 2000℃ and 1000℃ at 40 Gpa Diffraction patterns of CaSiO_3 perovskite could be observed at 20 Gpa and 1500-1600 K. Technical improvements are still needed but quite good quality diffraction patterns were recorded.EOS of CaO was determined by X-ray diffraction measurements using a hydraulically operated DAC and discusses a possibility of dissociation reaction of CaSiO_3 perovskile at the lowest part of the lower mantle.