Organotin sulfides as precursors for nanometric γ‐Sn₂S₃ powders: a study by ¹¹⁹Sn Mössbauer spectroscopy and X‐ray powder diffraction

Abstract

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.

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

“…Most of the synthetic approaches for the preparation of SnS use toxic H 2 S atmospheres as co‐reagent or render mixtures of tin sulfides, SnS, SnS 2 , Sn 2 S 3 or Sn 3 S 4 in different stoichiometry or combinations. Complexes 1 – 4 not only preserve the mild conditions required for good organometallic precursors, but also avoid the presence of undesired and secondary products, as detected previously 21. Herein we have described the preparation of phase‐pure SnS in N 2 by experiments of thermal decomposition at low temperature, 350 °C, employing [Sn{S 2 CN(C 2 H 5 ) 2 } 2 Ph 2 ] ( 1 ), [Sn{S 2 CN(C 2 H 5 ) 2 }Ph 3 ] ( 2 ), [Sn{S 2 CN(C 2 H 5 ) 2 } 3 Ph] ( 3 ) and [Sn{S 2 CN(C 4 H 8 )} 2 Bu 2 ] ( 4 ), as single source precursor.…”

“…Complexes 1-4 not only preserve the mild conditions required for good organometallic precursors, but also avoid the presence of undesired and secondary products, as detected previously. [21] Herein we have described the preparation of phase-pure SnS in N 2 by experiments of thermal decomposition at low temperature, 350 4), as single source precursor. The TG experiments show similar decomposition profiles for all precursors.…”

“…Nanometric tin(II) sulfide particles have been produced by thermal decomposition, at 350 °C in air, of R 4 Sn 4 S 6 [R = Me, Bu and Ph] 20. Further heating to 500 °C in a N 2 atmosphere led to pure phase orthorhombic Sn 2 S 3 21. The thermal decomposition of diphenyl and triphenyl‐tin pyrrolidinedithiocarbamate complexes22 or of the asymmetric dithiocarbamate organotin complexes [SnMe 3 {S 2 CN(Bu)(Me)}] and [SnPh{S 2 CN(Bu)(Me)} 3 ]23 yielded mixtures of SnS and Sn 2 S 3 .…”

Structural and optical studies of chemically deposited Sn2S3 thin films

“…Among these, Sn x S y is very promising as a material for the researchers, due to its different phases and properties [5]. Most of the studies working on Sn x S y thin films have fabricated SnS, SnS 2 thin films by using different deposition methods [6][7][8][9][10][11][12].…”

The effect of different annealing temperatures on tin and cadmium telluride phases obtained by a modified chemical route

“…The annealed materials were characterized by X-ray powder diffraction (XRD), X-ray photoelectron (XPS) and 119 Sn Mö ssbauer spectroscopies. This last technique, which has been extensively used by our group [15][16][17] showed to be an efficient tool for identifying mixtures of tin oxides and selenides with different oxidation states in a detection limit quite lower than X-ray powder diffraction. Rietveld method [18] was used to determine the structural parameters of each phase obtained in the annealed samples.…”