The photoelectrochemical efficiency of ZnCd(SSe)2 thin films shows a notable enhancement, increasing from 0.08 % to 0.28 %, when deposited at different temperatures (room temperature, 40 °C, 50 °C, and 60 °C). This study aims to develop ZnCd(SSe)2 thin films using a cost-effective single-step process called the Arrested Precipitation Technique (APT). This study demonstrates that varying the deposition temperatures significantly impacts the optical, structural, and morphological properties of the resulting thin films. Optical analysis shows a reduction in the optical energy band gap from 1.92 to 1.63 eV as the bath temperature increases. X-ray diffraction confirms the formation of nanocrystalline thin film samples with improved crystallinity, as indicated by the increased intensity of the (100) diffraction peak. Scanning electron microscopy reveals changes in surface morphology corresponding to different deposition temperatures. The thin films exhibit polycrystalline characteristics, as verified by transmission electron microscopy and selected area electron diffraction pattern analysis. Energy Dispersive Spectroscopy analysis identifies the presence of Cd, Zn, S, and Se elements with near-ideal stoichiometry, suggesting a favorable composition. Importantly, the photoelectrochemical performance increases significantly from 0.08 % to 0.28 % with rising deposition temperature, marking a substantial improvement with potential for further investigation and development in the field.