The alloy semiconductor material Mo_1-XW_XS₂ (X is concentration) is prepared by hydrothermal synthesis method. The morphology and crystal structure of Mo_1-XW_XS₂ are characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and Raman spectroscopy (Raman). The experimental results show that the surface of Mo_1-XW_XS₂ alloy becomes rough with the increase of doping concentration by SEM morphology test. The XRD crystal structure shows that the lattice constant of Mo_1-XW_XS₂ increases with the increase of doping concentration. In the Raman shift of the alloy material, with the increase of doping concentration, the A_1g vibration mode in Mo_1-XW_XS₂ has a blue shift, while the E2g1 vibration mode has a red shift. Through the detection and analysis of lattice structure and Raman frequency shift, it is proved that the hydrothermal synthesis method can prepare Mo_1-XW_XS₂ alloy semiconductor materials with different concentrations. This method can be further extended to the batch preparation method of disulfide alloy semiconductor materials, which provides a basis for the fabrication and design of alloy semiconductor devices.