Nonequilibrium structure of Zn2SnO4 spinel nanoparticles

Vladimir Šepelák; Sebastian M. Becker; Ingo Bergmann; Sylvio Indris; Marco Scheuermann; Armin Feldhoff; Christian Kübel; Michael Bruns; Ninette Stürzl; Anne S. Ulrich; Mohammad Ghafari; Horst Hahn; Clare P. Grey; Klaus D. Becker; Paul Heitjans

doi:10.1039/C2JM15427G

Nonequilibrium structure of Zn₂SnO₄ spinel nanoparticles

Vladimir Šepelák,†*^ab Sebastian M. Becker,^ac Ingo Bergmann,^d Sylvio Indris,^a Marco Scheuermann,^a Armin Feldhoff,^be Christian Kübel,^a Michael Bruns,^f Ninette Stürzl,^a Anne S. Ulrich,^cgh Mohammad Ghafari,^a Horst Hahn,^ac Clare P. Grey,^ij Klaus D. Becker^bk and Paul Heitjans^be

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^a Institute of Nanotechnology, Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, Eggenstein-Leopoldshafen, Germany
E-mail: vladimir.sepelak@kit.edu
Fax: +49-721-60826368
Tel: +49-721-60828929

^b Center for Solid State Chemistry and New Materials, Leibniz University Hannover, Callinstr. 3-3A, Hannover, Germany

^c DFG Center for Functional Nanostructures, Karlsruhe Institute of Technology, Wolfgang-Gaede-Str. 1A, Karlsruhe, Germany

^d Volkswagen AG, Wolfsburg, Germany

^e Institute of Physical Chemistry and Electrochemistry, Leibniz University Hannover, Callinstr. 3-3A, Hannover, Germany

^f Institute for Applied Materials (IAM-WPT), Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, Eggenstein-Leopoldshafen, Germany

^g Institute of Organic Chemistry, Karlsruhe Institute of Technology, Fritz-Haber-Weg 6, Karlsruhe, Germany

^h Institute of Biological Interfaces (IBG-2), Karlsruhe Institute of Technology, Hermann-von-Helmholtz-Platz 1, Eggenstein-Leopoldshafen, Germany

ⁱ Chemistry Department, State University of New York, Stony Brook, New York, USA

^j Chemistry Department, University of Cambridge, Lensfield Rd, Cambridge, UK

^k Institute of Physical and Theoretical Chemistry, Braunschweig University of Technology, Hans-Sommer-Str. 10, Braunschweig, Germany

Abstract

Zinc stannate (Zn₂SnO₄) nanoparticles with an average size of about 26 nm are synthesized via single-step mechanochemical processing of binary oxide precursors (ZnO and SnO₂) at ambient temperature, without the need for the subsequent calcination, thus making the synthesis route very simple and cost-effective. The mechanically induced phase evolution of the 2ZnO + SnO₂ mixture is followed by XRD and by a variety of spectroscopic techniques including ¹¹⁹Sn MAS NMR, Raman spectroscopy, ¹¹⁹Sn Mössbauer spectroscopy, and XPS. High-resolution TEM studies reveal a non-uniform structure of mechanosynthesized Zn₂SnO₄ nanoparticles consisting of a crystalline core surrounded by a structurally disordered surface shell. Due to the ability of the applied solid-state spectroscopies to probe the local environment of Sn cations, valuable complementary insight into the nature of the local structural disorder of mechanosynthesized Zn₂SnO₄ is obtained. The findings hint at a highly nonequilibrium state of the as-prepared stannate characterized by its partly inverse spinel structure and the presence of deformed polyhedra in the surface shell of nanoparticles.

Journal of Materials Chemistry

Nonequilibrium structure of Zn₂SnO₄ spinel nanoparticles

Abstract

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Nonequilibrium structure of Zn₂SnO₄ spinel nanoparticles

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