Controlled electrochemical synthesis of high-purity stannous sulphate (SnSO4) microparticles via Nafion 115-assisted membrane separation

• High-purity stannous sulfate (SnSO₄) microparticles were synthesized electrochemically using a Nafion 115-assisted two-compartment cell system. • Process optimization via the Taguchi method enabled a maximum SnSO₄ yield of 98.83% under controlled electrolysis conditions. • The optimized SnSO₄ product demonstrated an orthorhombic crystal structure, well-defined prismatic morphology, and a narrow particle size distribution (D₅₀ ≈ 0.99 μm) • H₂SO₄ concentration, applied voltage, and electrolysis duration significantly influenced crystallinity, yield, current efficiency, particle size and morphology. Using a two-compartment electrolysis system separated by a Nafion 115 membrane, the present study synthesizes high-purity stannous sulfate (SnSO₄) through an electrochemical method. In this process, tin metal and graphite serve as the anode and cathode, respectively, while sulfuric acid acts as the electrolyte. The effects of H₂SO₄ concentration, applied voltage, and electrolysis duration on SnSO₄ yield, particle morphology, and crystal structure are systematically investigated. Application of the Taguchi method enables optimization of these parameters by evaluating the signal-to-noise (S/N) ratio, with the optimum yield of 98.83% obtained under 0.5 mol·L -1 H₂SO₄, 3.0 V, and 8 hours of electrolysis. Under these conditions, the synthesized SnSO₄ exhibits an orthorhombic phase with high crystallinity and a prismatic morphology, as confirmed by FTIR, XRD, SEM, and particle size distribution analysis. The average particle diameter is approximately 1.06 ± 0.003 µm, indicating a narrow size distribution and uniform shape. Increasing acid concentration and electrolysis time enhances both current efficiency and crystalline quality, while excessive voltage leads to side reactions and the formation of morphological imperfections. These findings suggest that precise control of electrochemical parameters is essential for tailoring the structural and morphological properties of SnSO₄, making the electrochemical route promising for scalable and efficient production of high-quality tin-based materials.