Chemical vapor reaction is a simple and efficient experimental means of preparing metal sulphide films. Through systematically studying the effect of vulcanisation temperature on the growth of copper sulfide (CuS) thin film. The copper antimony sulfide (Cu3SbS4) thin film was obtained by further vulcanized Sb/Cu mental film. The structure and optical properties of the as-prepared films were characterized by X-ray diffraction, Raman and photoluminescence spectra. The hexagonal structure of CuS film was confirmed and Cu3SbS4 grew preferentially along the (112) crystal plane. The surface grains of CuS and Cu3SbS4 films were finally condensed into spheres. The content of S and the resistance of the films increase with the increase in temperature, but the bandgap of the films will be decreased. The bandgap of Cu2-xS films prepared at 195℃-350℃ is in the range of 2.2-2.5 eV and that of Cu3SbS4 thin films prepared at 350℃ is 1.77 eV, and has good absorption in the visible light range. In addition, The Hall effect measurement indicated CuS and Cu3SbS4 films have p-type semiconducting behavior. The carrier concentration and mobility are 2.45×1021 cm-3 and 1.28 cm2/Vs for CuS, and 4.30×1017 cm-3 and 185.93 cm2/Vs for Cu3SbS4, respectively. The I-T tests show that the CuS and Cu3SbS4 thin films have photoconductive properties.