Crystal structures of two new high-pressure oxynitrides with composition SnGe 4 N 4 O 4 , from single-crystal electron diffraction.

Autor: Gollé-Leidreiter P; Glass and Mineral Materials, Fraunhofer ISC, Neunerplatz 2, Würzburg, 97082, Germany., Bhat S; Deutsches Elektronen-Synchrotron, DESY, Notkestr. 85, Hamburg, 22607, Germany., Wiehl L; FB Materialwissenschaft / FG Disperse Feststoffe, Technische Universität Darmstadt, Otto Berndt-Str. 3, Darmstadt, D-64287, Germany., Wen Q; State Key Laboratory of Powder Metallurgy, Central South University, Changsha, 410083, People's Republic of China., Kroll P; Department of Chemistry and Biochemistry, University of Texas at Arlington, Arlington, Texas 76019, USA., Ishikawa R; Institute of Engineering Innovation, University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo, 113-8656, Japan., Etter M; Deutsches Elektronen-Synchrotron, DESY, Notkestr. 85, Hamburg, 22607, Germany., Farla R; Deutsches Elektronen-Synchrotron, DESY, Notkestr. 85, Hamburg, 22607, Germany., Ikuhara Y; Institute of Engineering Innovation, University of Tokyo, 2-11-16 Yayoi, Bunkyo-ku, Tokyo, 113-8656, Japan., Riedel R; FB Materialwissenschaft / FG Disperse Feststoffe, Technische Universität Darmstadt, Otto Berndt-Str. 3, Darmstadt, D-64287, Germany., Kolb U; Institute for Applied Geosciences, Technische Universität Darmstadt, Schnittspahnstraße 9, Darmstadt, 64287, Germany.
Jazyk: angličtina
Zdroj: Acta crystallographica Section B, Structural science, crystal engineering and materials [Acta Crystallogr B Struct Sci Cryst Eng Mater] 2024 Jun 01; Vol. 80 (Pt 3), pp. 182-192. Date of Electronic Publication: 2024 May 08.
DOI: 10.1107/S2052520624002683
Abstrakt: SnGe 4 N 4 O 4 was synthesized at high pressure (16 and 20 GPa) and high temperature (1200 and 1500°C) in a large-volume press. Powder X-ray diffraction experiments using synchrotron radiation indicate that the derived samples are mixtures of known and unknown phases. However, the powder X-ray diffraction patterns are not sufficient for structural characterization. Transmission electron microscopy studies reveal crystals of several hundreds of nanometres in size with different chemical composition. Among them, crystals of a previously unknown phase with stoichiometry SnGe 4 N 4 O 4 were detected and investigated using automated diffraction tomography (ADT), a three-dimensional electron diffraction method. Via ADT, the crystal structure could be determined from single nanocrystals in space group P6 3 mc, exhibiting a nolanite-type structure. This was confirmed by density functional theory calculations and atomic resolution scanning transmission electron microscopy images. In one of the syntheses runs a rhombohedral 6R polytype of SnGe 4 N 4 O 4 could be found together with the nolanite-type SnGe 4 N 4 O 4 . The structure of this polymorph was solved as well using ADT.
(open access.)
Databáze: MEDLINE
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