Abstract: A series of MoS₂/Ti_xO_y catalysts were prepared by a one pot solvothermal synthesis method and the effects of solvent, sulfur source, molybdenum source and titanium subdioxide conductive agent on the electrocatalytic activity of MoS₂/Ti_xO_y in hydrogen evolution from water splitting were investigated. The results showed that the crystal structure of MoS₂/Ti_xO_y catalyst as well as its catalytic performance is greatly influenced by the solvent, sulfur source, molybdenum source and titanium subdioxide conductive agent. Water, sulfur and molybdenum sources which can produce ammonium ions via hydrolysis, and the conductive agents are beneficial to improving the hydrogen evolution activity of the MoS₂/Ti_xO_y catalyst in water splitting. In particular, with water as the solvent, thioacetamide and ammonium molybdate as the sulfur and molybdenum sources, respectively, the MoS₂/Ti_xO_y catalyst with the highest hydrogen evolution activity was obtained; it needs only 280 mV overpotential to reach 10 mA/cm² current density in the electrolysis of water.