<p>Transition metal dichalcogenides (TMDCs) derived from molybdenum (Mo), such as MoS₂ and MoSe₂, have gained tremendous interest due to its highlighting electronic and optoelectronic properties. This work mainly focused on synthesis of MoX₂–MoO₃ at extremely low temperature by non-vacuum process. The temperature-dependent mechanochemical technique is employed to synthesize MoX₂–MoO₃ composite powder, which is subsequently deposited on a p-Si substrate using the thermal evaporation method. The elemental composition and morphology of all synthesized powders have been analyzed using EDX and FESEM techniques. The presence of the oxide phase in the composite powder has been confirmed through XRD and Raman spectroscopy analysis. The hexagonal crystal structure of MoX₂–MoO₃ thin film is analyzed using XRD technique. Photoluminescence (PL) spectroscopy was employed to examine the bandgap and impurity levels in both films. XPS analysis confirmed the presence of the oxide phase associated with the higher oxidation state of Mo, specifically Mo⁽⁶⁺⁾. The current–voltage (<i>I</i>–<i>V</i>) measurement is employed to analyze the electrical properties of all films. The properties indicate that the presence of the oxide phase is crucial for achieving optimal optical and electrical characteristics in MoX₂–MoO₃ composite films, which can be advantageous for various optoelectronic applications and photovoltaic devices.</p>