Sonochemical preparation of SnS and SnS2 nano- and micropowders and their characterization

Sonochemical production of tin(II) and tin(IV) sulfides is investigated. Different conditions of syntheses are examined: used solvent (ethanol or ethylenediamine), source of tin (SnCl2 or SnCl4), the molar ratio of thioacetamide to the tin source, and time of sonication. The obtained powders are characterized by the X-ray diffraction method (PXRD), scanning electron microscopy (SEM), scanning transmission electron microscopy (STEM), energy-dispersive X-ray spectroscopy (EDX), and the Tauc method. Raman and FT-IR measurements were performed for the obtained samples, which additionally confirmed the crystallinity and phase composition of the samples. The influence of experimental conditions on composition (is it SnS or SnS2), morphology, and on the bandgap of obtained products is elucidated. It was found that longer sonication times favor more crystalline product. Each of bandgaps is direct and most of them show typical values - c.a. 1.3 eV for SnS and 2.4 eV for SnS2. However, there are some exceptions. Synthesized powders show a variety of forms such as needles, flowerlike, rods, random agglomerates (SnS2) and balls (SnS). Using ethanol as a solvent led to powders of SnS2 independently of which tin chloride is used. Sonochemistry in ethylenediamine is more diverse: this solvent protects Sn2+ cations from oxidation so mostly SnS is obtained, while SnCl4 does not produce powder of SnS2 but Sn(SO4)2 instead or, at a higher ratio of thioacetamide to SnCl4, green clear mixture.

Automated summary

The sonochemical production of tin(II) and tin(IV) sulfides was investigated under different synthesis conditions, leading to insights on the influence of experimental parameters on the composition, morphology, and bandgap of the obtained products. Longer sonication times were found to favor more crystalline products, with most bandgaps showing typical values but some exceptions existing. Various forms of synthesized powders were observed, with ethanol and ethylenediamine as solvents exhibiting different outcomes in terms of product composition.