Achimovičová, Marcela

Fabián, Martin

Myndyk, Maxym

Rečnik, Aleksander

Šepelák, Vladimír

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A one-step mechanochemical synthesis and characterization of SnSe and SnSe 2

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diffusion-fundamentals   The Open-Access Journal for the Basic Principles of Diffusion Theory, Experiment and Application www.diffusion-fundamentals.org, ISSN 1862-4138; © 2005-2010   Diffusion Fundamentals 12 (2010) 75  © M. Achimovičová A One-Step Mechanochemical Synthesis  and Characterization of SnSe and SnSe2 Marcela Achimovičová,*,1 Aleksander Rečnik,2 Maxym Myndyk,3 Martin Fabián,1  Vladimír Šepelák1,4 1 Slovak Academy of Sciences, Institute of Geotechnics,  Watsonova 45, 043 53 Košice, Slovakia 2 Jožef Stefan Institute, Department for Nanostructured Materials,  Jamova 39, SI-1000, Ljubljana, Slovenia 3 Braunschweig University of Technology, Institute of Physical and Theoretical Chemistry,  Hans-Sommer-Str. 10, 38106 Braunschweig, Germany 4 Karlsruhe Institute of Technology, Institute of Nanotechnology,  Hermann-von-Helmholtz-Platz 1, 76344 Eggenstein-Leopoldshafen, Germany  E-Mail: achimovic@saske.sk  Presented at the Bunsen Colloquium: Spectroscopic Methods in Solid State Diffusion and Reactions September 24th − 25th, 2009, Leibniz University Hannover, Germany   Tin selenides belong to the AIVBVI group of semiconductors and have brilliant application prospects due to their excellent optical and electrical properties, which can be applied in film electrodes, infrared optoelectronic devices, thermoelectric refrigerators and solar cells [1]. Various methods have been developed to prepare metal selenides such as solid-state reactions [2], solvothermal method [3], self-propagating high-temperature synthesis [4] and mechanical alloying of metal and elemental selenium at room temperature [5]. In the present work, a simple mechanochemical synthesis of binary tin selenides was performed by high-energy milling in a planetary ball mill Pulverisette 6 (Fritsch, Germany). SnSe and SnSe2 were prepared from powdered elements (Sn 99.85 %, Se 99.5 %) at ambient temperature and in a relatively short reaction time. The products were characterized by XRD, transmission electron microscopy and 119Sn Mössbauer spectroscopy. The XRD pattern (Fig. 1A) confirmed that the mechanochemical syn-thesis of orthorhombic SnSe (JCPDS 32-1382) takes place, and the degree of conversion of the reac-tion reaches 83% after 10 min of milling. Similarly, the degree of conversion of the mechanochemical synthesis of SnSe2 (JCPDS 23-0602) reaches 72 % after 20 min of milling (Fig. 1B). It was revealed that in addition to the hexagonal SnSe2, the milled Sn/2Se mixture contains also the orthorhombic SnSe phase. TEM analysis of the mechanochemically synthesized SnSe demonstrated the formation of crystals with the orthorhombic shape and the size between 2 and 8 nm. Note that several hexagonal crystallites were also found in the mechanosynthesized selenides. The room-temperature 119Sn Möss-bauer spectra of the mechanosynthesized selenides are shown in Fig. 2. A striking feature observed is the broad shape of the spectral lines of the mechanosynthesized products, implying the presence of a broad distribution of local environments around the Sn nuclei due to the mechanically induced defor-Achimovičová et al., Mechanochemical synthesis of SnSe and SnSe2  diffusion-fundamentals    www.diffusion-online.org  Diffusion Fundamentals 12 (2010) 76  © M. Achimovičová  mation of Sn-Se polyhedra. The detailed analysis of Mössbauer spectra of the mechanosynthesized SnSe and SnSe2 nanomaterials is in progress.   Fig. 1 XRD patterns of mechanochemically synthesized SnSe (A) and SnSe2 (B).    Fig. 2 119Sn Mössbauer spectra of mechanochemically synthesized SnSe (A) and SnSe2 (B).    Acknowledgement. The present work was supported by the Slovak Grant Agency VEGA (project 2/0035/08), the Slovak Research and Developing Agency APVV (0347-06), Center of Excellence of the Slovak Academy of Sciences (NANOS-MART), and Center of Excellence of Advanced Materials with Nano- and Submicron-Structure (NANOCEXMAT) that is supported by the Operational Program “Research and Development” financed through European Regional Development Achimovičová et al., Mechanochemical synthesis of SnSe and SnSe2  diffusion-fundamentals    www.diffusion-online.org  Diffusion Fundamentals 12 (2010) 77  © M. Achimovičová  Fund. One of the authors (V.Š.) thanks the Deutsche Forschungsgemeinschaft for supporting his work in the framework of the Priority Program “Crystalline Nonequilibrium Phases” (SPP 1415). References [1] K. Liu, H. Liu, J. Wang, L. Feng, Mater. Lett. 63 (2009) 512. [2] R. Coustal, J. Chim. Phys. 38 (1958) 277. [3] Y. Xie, H. Su, B. Li, Y. Qian, Mater. Res. Bull. 35 (2000) 459.  [4] I. P. Parkin, Chem. Soc. Rev. 25 (1996) 199. [5] T. Ohtani, M. Motoki, Mater. Res. Bull. 30 (1995) 1495. 

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A one-step mechanochemical synthesis and characterization of SnSe and SnSe 2

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