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.

Tracking structural phase transitions via single crystal x-ray diffraction at extreme conditions: advantages of extremely brilliant source / T. Poręba, D. Comboni, M. Mezouar, G. Garbarino, M. Hanfland. - In: JOURNAL OF PHYSICS. CONDENSED MATTER. - ISSN 0953-8984. - 35:5(2023 Feb 08), pp. 054001.1-054001.13. [10.1088/1361-648X/aca50b]

Tracking structural phase transitions via single crystal x-ray diffraction at extreme conditions: advantages of extremely brilliant source

D. Comboni
Secondo
;
2023

Abstract

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.
DAC; crystalline materials; high pressure; phase transition; synchrotron radiation; x-ray diffraction;
Settore GEO/09 - Georisorse Miner.Appl.Mineral.-Petrogr.per l'amb.e i Beni Cul
Settore GEO/06 - Mineralogia
8-feb-2023
14-dic-2022
Article (author)
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Utilizza questo identificativo per citare o creare un link a questo documento: https://hdl.handle.net/2434/970614
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