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A new approach to the study of processes of thermal decomposition and formation of nanoalloys: double complex salt [Pd(NH3)4][PtCl6]

Abstract

A new approach based on a combination of synchrotron radiation techniques such as X-ray Absorption Fine Structure (XAFS), X-ray photoelectron spectroscopy (XPS), HArd X-ray PhotoElectron Spectroscopy (HAXPES) and Powder X-Ray Diffraction (PXRD) has applied for in situ studying processes of thermal decomposition of inorganic compound and formation of bimetallic nanoalloy. As an example, a double complex salt [Pd(NH3)4][PtCl6] was selected because of i) enough complicated structure and previously studied by thermal analysis and ex situ PXRD, XPS, and ii) as a perspective single-source precursor for preparing bimetallic nanoparticles or nanoalloy (PdPt). The difference between mechanisms based on ex situ and in situ data are discussed for the first time. It was found that the first step of thermal decomposition relates with a formation of crystalline [Pd(NH3)2Cl2][Pt(NH3)2Cl4]. Further decomposition results in a formation of {PdCl2}, {PtCl2} and (NH4)2[PtCl6] at the second step. At a final step, the intermediates are completely reduced forming bimetallic nanoalloy. Different means of Pd and Pt reduction on the surface and bulk results in the formation of disordered nanoalloy with possible monometallic inclusions. Further heating orders nanoalloy that is accompanied by a decrease in positive charge on Pt.

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Publication details

The article was received on 27 Nov 2017, accepted on 12 Feb 2018 and first published on 13 Feb 2018


Article type: Paper
DOI: 10.1039/C7NJ04626J
Citation: New J. Chem., 2018, Accepted Manuscript
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    A new approach to the study of processes of thermal decomposition and formation of nanoalloys: double complex salt [Pd(NH3)4][PtCl6]

    T. Asanova, I. P. Asanov, M. G. Kim, M. Gorgoi, J. Sottmann, S. Korenev and K. V. Yusenko, New J. Chem., 2018, Accepted Manuscript , DOI: 10.1039/C7NJ04626J

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