Organotinsulfides Sn 4 S 4 R 6 (R = methyl, n-butyl and phenyl) were employed as single-source precursors for nanometric tin sulfides. The residues obtained after pyrolysis in hydrogen, nitrogen and oxygen were characterized by X-ray diffraction, 119 Sn Mössbauer spectroscopy, scanning electron microscopy and X-ray electron probe microanalysis. The results clearly showed the formation of tetragonal SnO 2 (rutile-type structure) in oxygen and pure phase orthorhombic γ -Sn 2 S 3 in nitrogen when Sn 4 Bu 4 S 6 (2) was employed as precursor. The 119 Sn Mössbauer spectroscopic results were very important in the elucidation of the decomposition process. Compound 2 is the best starting material for the process.
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