期刊
JOURNAL OF PHYSICS-CONDENSED MATTER
卷 35, 期 5, 页码 -出版社
IOP Publishing Ltd
DOI: 10.1088/1361-648X/aca50b
关键词
DAC; high pressure; synchrotron radiation; crystalline materials; x-ray diffraction; phase transition
This article discusses the various experimental variables that affect the quality of high-pressure single-crystal X-ray diffraction data and presents an overview of recent advancements in X-ray diffraction techniques at extreme conditions, specifically within the European Synchrotron Radiation Facility (ESRF)- Extremely Bright Source (EBS). The ID15b and ID27 beamlines have benefitted from source upgrades, allowing for measurements of a few-micron crystals in the megabar range. Two case studies exploring the phase transitions and crystal structures of hypervalent CsI3 crystals and jadarite are presented, showcasing the recent developments within ESRF-EBS.
Highly brilliant synchrotron source is indispensable to track pressure-induced phenomena in confined crystalline samples in megabar range. In this article, a number of experimental variables affecting the quality high-pressure single-crystal x-ray diffraction data is discussed. An overview of the recent advancements in x-ray diffraction techniques at extreme conditions, in the frame of European Synchrotron Radiation Facility (ESRF)- Extremely Bright Source (EBS), is presented. Particularly, ID15b and ID27 beamlines have profited from the source upgrade, allowing for measurements of a few-micron crystals in megabar range. In case of ID27, a whole new beamline has been devised, including installation of double-multilayer mirrors and double crystal monochromator and construction of custom-made experimental stations. Two case studies from ID27 and ID15b are presented. Hypervalent CsI3 crystals, studied up to 24 GPa, have shown a series of phase transitions: Pnma -> P-3c1 -> Pm-3 n. First transition leads to formation of orthogonal linear iodine chains made of I-3 (-). Transformation to the cubic phase at around 21.7 GPa leads to equalization of interatomic I-I distances and formation of homoleptic I-n (m-) chains. The second study investigates elastic properties and structure of jadarite, which undergoes isosymmetric phase transition around 16.6 GPa. Despite a few-micron crystal size, twinning and dramatic loss of crystal quality, associated with pressure-induced phase transitions, crystal structures of both compounds have been determined in a straightforward matter, thanks to the recent developments within ESRF-EBS.
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