Thermal decomposition of ammonium hexachloroosmate

T I Asanova; Innokenty Kantor; I. P. Asanov; S V Korenev; K. V. Yusenko

doi:10.1039/C6CP07133C

Thermal decomposition of ammonium hexachloroosmate

T I Asanova, Innokenty Kantor, I. P. Asanov, S V Korenev, K. V. Yusenko

Department of Physics

Research output: Contribution to journal › Journal article › Research › peer-review

Abstract

Structural changes of (NH₄)₂[OsCl₆] occurring during thermal decomposition in a reduction atmosphere have been studied in situ using combined energy-dispersive X-ray absorption spectroscopy (ED-XAFS) and powder X-ray diffraction (PXRD). According to PXRD, (NH₄)₂[OsCl₆] transforms directly to metallic Os without the formation of any crystalline intermediates but through a plateau where no reactions occur. XANES and EXAFS data by means of Multivariate Curve Resolution (MCR) analysis show that thermal decomposition occurs with the formation of an amorphous intermediate {OsCl₄}x with a possible polymeric structure. Being revealed for the first time the intermediate was subjected to determine the local atomic structure around osmium. The thermal decomposition of hexachloroosmate is much more complex and occurs within a minimum two-step process, which has never been observed before.

Original language	English
Journal	Physical Chemistry Chemical Physics
Volume	18
Pages (from-to)	33134-33141
Number of pages	8
ISSN	1463-9076
DOIs	https://doi.org/10.1039/C6CP07133C
Publication status	Published - 2016

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@article{02923e1351f841068cbf19e5cd85ec1d,

title = "Thermal decomposition of ammonium hexachloroosmate",

abstract = "Structural changes of (NH4)2[OsCl6] occurring during thermal decomposition in a reduction atmosphere have been studied in situ using combined energy-dispersive X-ray absorption spectroscopy (ED-XAFS) and powder X-ray diffraction (PXRD). According to PXRD, (NH4)2[OsCl6] transforms directly to metallic Os without the formation of any crystalline intermediates but through a plateau where no reactions occur. XANES and EXAFS data by means of Multivariate Curve Resolution (MCR) analysis show that thermal decomposition occurs with the formation of an amorphous intermediate {OsCl4}x with a possible polymeric structure. Being revealed for the first time the intermediate was subjected to determine the local atomic structure around osmium. The thermal decomposition of hexachloroosmate is much more complex and occurs within a minimum two-step process, which has never been observed before.",

author = "Asanova, {T I} and Innokenty Kantor and Asanov, {I. P.} and Korenev, {S V} and Yusenko, {K. V.}",

year = "2016",

doi = "10.1039/C6CP07133C",

language = "English",

volume = "18",

pages = "33134--33141",

journal = "Physical Chemistry Chemical Physics",

issn = "1463-9076",

publisher = "Royal Society of Chemistry",

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TY - JOUR

T1 - Thermal decomposition of ammonium hexachloroosmate

AU - Asanova, T I

AU - Kantor, Innokenty

AU - Asanov, I. P.

AU - Korenev, S V

AU - Yusenko, K. V.

PY - 2016

Y1 - 2016

N2 - Structural changes of (NH4)2[OsCl6] occurring during thermal decomposition in a reduction atmosphere have been studied in situ using combined energy-dispersive X-ray absorption spectroscopy (ED-XAFS) and powder X-ray diffraction (PXRD). According to PXRD, (NH4)2[OsCl6] transforms directly to metallic Os without the formation of any crystalline intermediates but through a plateau where no reactions occur. XANES and EXAFS data by means of Multivariate Curve Resolution (MCR) analysis show that thermal decomposition occurs with the formation of an amorphous intermediate {OsCl4}x with a possible polymeric structure. Being revealed for the first time the intermediate was subjected to determine the local atomic structure around osmium. The thermal decomposition of hexachloroosmate is much more complex and occurs within a minimum two-step process, which has never been observed before.

AB - Structural changes of (NH4)2[OsCl6] occurring during thermal decomposition in a reduction atmosphere have been studied in situ using combined energy-dispersive X-ray absorption spectroscopy (ED-XAFS) and powder X-ray diffraction (PXRD). According to PXRD, (NH4)2[OsCl6] transforms directly to metallic Os without the formation of any crystalline intermediates but through a plateau where no reactions occur. XANES and EXAFS data by means of Multivariate Curve Resolution (MCR) analysis show that thermal decomposition occurs with the formation of an amorphous intermediate {OsCl4}x with a possible polymeric structure. Being revealed for the first time the intermediate was subjected to determine the local atomic structure around osmium. The thermal decomposition of hexachloroosmate is much more complex and occurs within a minimum two-step process, which has never been observed before.

U2 - 10.1039/C6CP07133C

DO - 10.1039/C6CP07133C

M3 - Journal article

SN - 1463-9076

VL - 18

SP - 33134

EP - 33141

JO - Physical Chemistry Chemical Physics

JF - Physical Chemistry Chemical Physics

ER -

Thermal decomposition of ammonium hexachloroosmate

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