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通过单晶电子衍射确定的两种新型高压氧氮化物SnGeNO的晶体结构。

Crystal structures of two new high-pressure oxynitrides with composition SnGeNO, from single-crystal electron diffraction.

作者信息

Gollé-Leidreiter Philipp, Bhat Shrikant, Wiehl Leonore, Wen Qingbo, Kroll Peter, Ishikawa Ryo, Etter Martin, Farla Robert, Ikuhara Yuichi, Riedel Ralf, Kolb Ute

机构信息

Glass and Mineral Materials, Fraunhofer ISC, Neunerplatz 2, Würzburg, 97082, Germany.

Deutsches Elektronen-Synchrotron, DESY, Notkestr. 85, Hamburg, 22607, Germany.

出版信息

Acta Crystallogr B Struct Sci Cryst Eng Mater. 2024 Jun 1;80(Pt 3):182-192. doi: 10.1107/S2052520624002683. Epub 2024 May 8.

DOI:10.1107/S2052520624002683
PMID:38728046
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11157342/
Abstract

SnGeNO 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 SnGeNO 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 P6mc, 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 SnGeNO could be found together with the nolanite-type SnGeNO. The structure of this polymorph was solved as well using ADT.

摘要

SnGeNO是在大体积压机中于高压（16和20吉帕）和高温（1200和1500°C）下合成的。使用同步辐射的粉末X射线衍射实验表明，所得样品是已知相和未知相的混合物。然而，粉末X射线衍射图谱不足以进行结构表征。透射电子显微镜研究揭示了尺寸为几百纳米、具有不同化学成分的晶体。其中，使用自动衍射断层扫描（ADT，一种三维电子衍射方法）检测并研究了一种化学计量比为SnGeNO的先前未知相的晶体。通过ADT，晶体结构可从空间群P6mc中的单个纳米晶体确定，呈现出诺兰石型结构。这通过密度泛函理论计算和原子分辨率扫描透射电子显微镜图像得到了证实。在一次合成过程中，发现了一种菱形6R多型的SnGeNO与诺兰石型SnGeNO共存。该多晶型的结构也使用ADT解析出来了。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/7c361b90cfdc/b-80-00182-fig11.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/48a0cb059ecb/b-80-00182-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/3975a47cd422/b-80-00182-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/6a877b72cf94/b-80-00182-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/de9c50267ee9/b-80-00182-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/6e7b48b5affd/b-80-00182-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/9cf95c51bd6b/b-80-00182-fig6.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/7e9b0fe8c123/b-80-00182-fig7.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/f3ac85a524a6/b-80-00182-fig8.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/2700d012af77/b-80-00182-fig10.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/651a94f81d35/b-80-00182-fig9.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/7c361b90cfdc/b-80-00182-fig11.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/48a0cb059ecb/b-80-00182-fig1.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/3975a47cd422/b-80-00182-fig2.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/6a877b72cf94/b-80-00182-fig3.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/de9c50267ee9/b-80-00182-fig4.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/6e7b48b5affd/b-80-00182-fig5.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/9cf95c51bd6b/b-80-00182-fig6.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/7e9b0fe8c123/b-80-00182-fig7.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/f3ac85a524a6/b-80-00182-fig8.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/2700d012af77/b-80-00182-fig10.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/651a94f81d35/b-80-00182-fig9.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5e00/11157342/7c361b90cfdc/b-80-00182-fig11.jpg

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