Partnership for eXtreme Xtallography (PX<sup>2</sup>)—A state-of-the-art experimental facility for extreme-conditions crystallography: A case study of pressure-induced phase transition in natural ilvaite

Xu Jingui; Zhang Dongzhou; Tkachev Sergey N.; Dera Przemyslaw K.

doi:10.1063/5.0075795

Volume 7 Issue 2

Mar. 2022

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Xu Jingui, Zhang Dongzhou, Tkachev Sergey N., Dera Przemyslaw K.. Partnership for eXtreme Xtallography (PX2)—A state-of-the-art experimental facility for extreme-conditions crystallography: A case study of pressure-induced phase transition in natural ilvaite[J]. Matter and Radiation at Extremes, 2022, 7(2): 028401. doi: 10.1063/5.0075795

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Xu Jingui, Zhang Dongzhou, Tkachev Sergey N., Dera Przemyslaw K.. Partnership for eXtreme Xtallography (PX²)—A state-of-the-art experimental facility for extreme-conditions crystallography: A case study of pressure-induced phase transition in natural ilvaite[J]. Matter and Radiation at Extremes, 2022, 7(2): 028401. doi: 10.1063/5.0075795

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Partnership for eXtreme Xtallography (PX²)—A state-of-the-art experimental facility for extreme-conditions crystallography: A case study of pressure-induced phase transition in natural ilvaite

doi: 10.1063/5.0075795

1.
School of Ocean and Earth Science and Technology, Hawai’i Institute of Geophysics and Planetology, University of Hawai’i at Manoa, Honolulu, Hawaii 96822, USA
2.
Center for Advanced Radiation Sources, University of Chicago, Chicago, Illinois 60437, USA

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Corresponding author: a)Author to whom correspondence should be addressed: dzhang@hawaii.edu
Received Date: 2021-10-18
Accepted Date: 2022-01-21

Available Online: 2022-03-01

Publish Date: 2022-03-01

Abstract

Abstract

Single-crystal x-ray diffraction (SCXRD) is an important tool to study the crystal structure and phase transitions of crystalline materials at elevated pressures. The Partnership for eXtreme Xtallography (PX²) program at the GSECARS 13-BM-C beamline of the Advanced Photon Source aims to provide state-of-the-art experimental capabilities to determine the crystal structures of materials under extreme conditions using SCXRD. PX² provides a focused x-ray beam (12 × 18 µm²) at a monochromatic energy of 28.6 keV. High-pressure SCXRD experiments are performed with a six-circle diffractometer and a Pilatus3 photon-counting detector, facilitated by a membrane system for remote pressure control and an online ruby fluorescence system for pressure determination. The efficient, high-quality crystal structure determination at PX² is exemplified by a study of pressure-induced phase transitions in natural ilvaite [CaFe²⁺₂Fe³⁺Si₂O₇O(OH), P2₁/a space group]. Two phase transitions are observed at high pressure. The SCXRD data confirm the already-known ilvaite-I (P2₁/a) → ilvaite-II (Pnam) transformation at 0.4(1) GPa, and, a further phase transition is found to occur at 22.8(2) GPa where ilvaite-II transforms into ilvaite-III (P2₁/a). The crystal structure of the ilvaite-III is solved and refined in the P2₁/a space group. In addition to the ilvaite-I → ilvaite-II → ilvaite-III phase transitions, two minor structural modifications are observed as discontinuities in the evolution of the FeO₆ polyhedral geometries with pressure, which are likely associated with magnetic transitions.

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References(34)

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