Synthesis of phase-pure SnS particles employing dithiocarbamate organotin(IV) complexes as single source precursors in thermal decomposition experiments

• Published in: Applied organometallic chemistry Vol. 24; no. 9; pp. 650 - 655
• Main Authors: Menezes, D. C., de Lima, G. M., Carvalho, F. A., Coelho, M. G., Porto, A. O., Augusti, R., Ardisson, J. D.
• Format: Journal Article
• Language: English
• Published: Chichester, UK John Wiley & Sons, Ltd 01-09-2010; Wiley Subscription Services, Inc
• Subjects: composites; Decomposition; Electron probe microanalysis; Electron probes; Electronics; inorganic compounds; Mossbauer spectroscopy; Precursors; Pyrolysis; Semiconductor materials; semiconductors; Spectrometry; Spectroscopy; Spectrum analysis; Sulfides; Thermal decomposition; Thermogravimetric analysis; X-rays
• ISSN: 0268-2605; 1099-0739; 1099-0739
• DOI: 10.1002/aoc.1663

Preparation of tin(II) sulfide, semiconductor material, has been accomplished by thermal decomposition of easily prepared organotin dithiocarbamate complexes: [Sn{S2CNEt2}2Ph2] (1), [Sn{S2CNEt2}Ph3] (2), [Sn{S2CNEt2}3Ph] (3) and [Sn{S2CN(C4H8)}2Bu2] (4). Phase‐pure tin(II) sulfide has been obtained by pyrolysis of these precursors at 350 °C in N2. Thermogravimetric analysis, X‐ray powder diffraction, scanning electron microscopy, X‐ray electron probe microanalysis and 119Sn Mössbauer spectroscopy revealed that the complexes decompose in a single and sharp step (1 and 2), or in pseudo‐single stage (3 and 4), to produce SnS. We have also measured the bandgap energies of the residues using electronic spectroscopy in the solid state and the result relates well to that in the literature for SnS, 1.3 eV. A decomposition mechanism was also proposed for each complex based on electrospray ionization tandem mass spectrometric results. The synthetic method used in this work might be useful for the preparation of pure SnS on a large scale. Copyright © 2010 John Wiley & Sons, Ltd.
Tin(II) sulfide was obtained and characterized by X‐ray powder diffraction, scanning electron microscopy, X‐ray electron probe microanalysis, electronic and 119Sn Mössbauer spectroscopy.