A Novel Method for the Synthesis of Tin(II) Sulphide Using Tin(II) Sulphate Precursor via H2-Mediated Ultrasonic Spray Pyrolysis

This study presents a novel approach for the synthesis of tin(II) sulphide (SnS) by integrating ultrasonic spray pyrolysis (USP) with hydrogen reduction (HR), using tin(II) sulphate (SnSO₄) as a precursor. The method combines aerosol droplet generation using ultrasonic atomisation at 1.7 MHz with gas-phase reduction in a tube reactor under H₂-N₂ mixed gas flow. Thermochemical assessment indicated that SnS formation is thermodynamically favourable from 400 to 1000 °C, in reasonable agreement with experimental results. XRD analysis confirmed the formation of SnS as the main phase accompanied by SnO₂ as a secondary product without SnSO₄ when conducting USP-HR at 1000 °C. SEM images revealed flake-like, spherical, and agglomerated morphologies, with EDS confirming distinct Sn-S regions. This study demonstrates the feasibility of producing SnS powder using a simple precursor system and a clean reducing environment. The process offers a scalable and controllable synthesis route for SnS materials, providing an alternative to conventional substrate-based deposition techniques. Further optimisation of reaction temperature and residence time is expected to enhance phase purity and reduce agglomeration.