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Phase identification and structure determination from multiphase crystalline powder samples by rotation electron diffraction
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
Stockholm University, Faculty of Science, Department of Materials and Environmental Chemistry (MMK).
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2014 (English)In: Journal of applied crystallography, ISSN 0021-8898, E-ISSN 1600-5767, Vol. 47, 2048-2054 p.Article in journal (Refereed) Published
Abstract [en]

Phase identification and structure characterization are important in synthetic and materials science. It is difficult to characterize the individual phases from multiphase crystalline powder samples, especially if some of the phases are unknown. This problem can be solved by combining rotation electron diffraction (RED) and powder X-ray diffraction (PXRD). Four phases were identified on the same transmission electron microscopy grid from a multiphase sample in the Ni-Se-O-Cl system, and their structures were solved from the RED data. Phase 1 (NiSeO3) was found in the Inorganic Crystal Structure Database using the information from RED. Phase 2 (Ni3Se4O10Cl2) is an unknown compound, but it is isostructural to Co3Se4O10Cl2, which was recently solved by single-crystal X-ray diffraction. Phase 3 (Ni5Se6O16Cl4H2) and Phase 4 (Ni5Se4O12Cl2) are new compounds. The fact that there are at least four different compounds in the as-synthesized material explains why the phase identification and structure determination could not be done by PXRD alone. The RED method makes phase identification from such multiphase powder samples much easier than would be the case using powder X-ray diffraction. The RED method also makes structure determination of submicrometre-sized crystals from multiphase samples possible.

Place, publisher, year, edition, pages
2014. Vol. 47, 2048-2054 p.
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Chemical Sciences
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URN: urn:nbn:se:su:diva-113111DOI: 10.1107/S1600576714023875ISI: 000345877900028OAI: oai:DiVA.org:su-113111DiVA: diva2:783130
Note

AuthorCount:8;

Available from: 2015-01-23 Created: 2015-01-23 Last updated: 2017-12-05Bibliographically approved

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Yun, YifengWan, WeiSu, JieXu, HongyiHovmöller, SvenJohnsson, MatsZou, Xiaodong
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