This manuscript highlights the synthesis of semiconductor materials, specifically transition metal chalcogenide thin films and the characterization of the films to evaluate the suitability for application as a photoelectrochemical (PEC)/solar cell. With the utilization of electrodeposition technique, this paper aims to design and predict a safe, cost-efficient and relatively simple method for synthesis of the transition metal chalcogenide thin film for possible applications in PEC/solar cell manufacturing industry. Transition metal chalcogenide (MoX₂) thin films were successfully electrodeposited on indium-tin-oxide; (ITO)-coated glass substrates and metal substrates in which the deposition time for the thin films were set at 10 minutes to 30 minutes with an interval time of 5 minutes. The thin films were characterized for their structural, morphological and compositional characteristics by X-ray diffraction (XRD), scanning electron microscope (SEM) and energy dispersive X-ray (EDX) analysis, respectively. Their optical and semiconducting parameters were also analyzed in order to determine the suitability of the thin films for photoelectrochemical (PEC)-solar cell applications.