CdO, ZnS, and CdO/ZnS hybrid photocatalyst were prepared using a simple co-precipitation method, and its photocatalytical activity was studied. The materials were characterized using powder XRD, TEM, HRTEM, BET, Raman, optical absorption, FT-IR, Thermal analysis and PL. The XRD patterns confirmed the crystal structure of the prepared samples. The surface analysis shows that the CdO/ZnS hybrid photocatalyst have larger surface area than the CdO and ZnS. Optical analysis of the nanocomposites revealed that the bond energy decreased after adding ZnS nanoparticles due to interactions with CdO nanoparticles. Raman spectroscopy showed the phonon modes of the CdO and ZnS, and PL spectra showed the electronic interaction between them. The photo-induced electrons can be easily transferred from the CdO to the ZnS in the composite, which facilitates effective charge separation and enhances photocatalytic degradation. The highest photocatalytic activity was achieved using the CdO/ZnS hybrid photocatalyst, with which more than 92% degradation was achieved. The enhanced photocatalytic activity could be ascribed to the low recombination rate of the electron and hole pairs because of the interface action between the CdO and ZnS.