Panoramic Synthesis as an Effective Materials Discovery Tool: The System Cs/Sn/P/Se as a Test Case.
The common approach to the synthesis of a new material involves reactions held at high temperatures under certain conditions such as heating in a robust vessel in the dark for a period until it is judged to have concluded. Analysis of the vessel contents afterward provides knowledge of the final pro...
| Publicado en: | Journal of the American Chemical Society Vol. 139; no. 31; pp. 10814 - 10822 |
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| Autores principales: | , , , , |
| Formato: | Artículo |
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American Chemical Society
8/9/2017
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| Materias: | |
| Acceso en línea: | Ver este registro en EBSCOhost |
| fields | @attributes: recordID: 1 pdfLink: plink: https://search.ebscohost.com/login.aspx?direct=true&db=hlh&AN=124566605&site=ehost-live header: @attributes: shortDbName: hlh uiTerm: 124566605 longDbName: Humanities International Complete uiTag: AN controlInfo: bkinfo: jinfo: jid: 00027863 ACS jtl: Journal of the American Chemical Society issn: 00027863 maglogo: N pubinfo: dt: 8/9/2017 vid: 139 iid: 31 pid: 997 pub: American Chemical Society artinfo: ui: 124566605 10.1021/jacs.7b05423 ppf: 10814 ppct: 8 formats: tig: atl: Panoramic Synthesis as an Effective Materials Discovery Tool: The System Cs/Sn/P/Se as a Test Case. aug: au: Haynes, Alyssa S. Stoumpos, Constantinos C. Haijie Chen Chica, Daniel Kanatzidis, Mercouri G. affil: Department of Chemistry, Northwestern University, Evanston, Illinois 60208, United States Materials Science Division, Argonne National Laboratory, Lemont, Illinois 60439, United States su: Heating X-ray diffraction Ships Synchrotrons Crystallization sug: subj: Heating X-ray diffraction Ships Synchrotrons Crystallization ab: The common approach to the synthesis of a new material involves reactions held at high temperatures under certain conditions such as heating in a robust vessel in the dark for a period until it is judged to have concluded. Analysis of the vessel contents afterward provides knowledge of the final products only. Intermediates that may form during the reaction process remain unknown. This lack of awareness of transient intermediates represents lost opportunities for discovering materials or understanding how the final products form. Here we present new results using an emerging in situ monitoring approach that shows high potential in discovering new compounds. In situ synchrotron X-ray diffraction studies were conducted in the Cs/Sn/P/Se system. Powder mixtures of CsSe, Sn, and PSe were heated to 650 °C and then cooled to room temperature while acquiring consecutive in situ synchrotron diffraction patterns from the beginning to the end of the reaction process. The diffraction data was translated into the relationship of phases present versus temperature. Seven known crystalline phases were observed to form on warming in the experiment: Sn, CsSe, CsSe, CsSe, CsSnSe, CsPSe, and CsPSe. Six unknown phases were also detected; using the in situ synchrotron data as a guide three of them were isolated and characterized ex situ. These are CsSn(PSe), α-CsSnPSe, and Cs(SnSe)[Sn(PSe )]. Cs(SnSe)[Sn(PSe )] is a two-dimensional compound that behaves as an n-type doped semiconductor below 50 K and acts more like a semimetal at higher temperatures. Because all crystalline phases are revealed during the reaction, we call this approach "panoramic synthesis". pubtype: Academic Journal doctype: Article src: R language: English refInfo: copyright: @attributes: flag: Y dt: @attributes: year: 2017 holdings: @attributes: islocal: N |
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