Abstract: Mo-doped Zn_0.5Cd_0.5S was prepared and compounded with Ti₃C₂ nanosheets by hydrothermal method. The crystal structure, surface composition, microscopic morphology, and photoelectric properties of the photocatalysts were analyzed by XRD, SEM, TEM, XPS, UV-vis DRS, fluorescence spectroscopy, transient photocurrent methods. The results showed that the doping of Mo caused changes in the lattice structure of Zn_0.5Cd_0.5S, while the loading of Ti₃C₂ increased the photocatalytic active site and accelerated the electron transfer rate. The photocatalytic activity was investigated by degrading the tetracycline solution under visible light irradiation with simultaneous H₂ production. The results showed that with the synergistic effect of Mo doping and loaded Ti₃C₂, the degradation rate of tetracycline (TC) reached more than 70% within 60 min, while the H₂ yield reached 883 μmol/(g·h). The radical capture experiments proved that the main active substance for degradation was holes and for H₂ production was electrons.