Abstract: TiO₂/CuS composites with different molar ratios (1∶1, 1.5∶1, 2∶1, 2.5∶1, 3∶1, 3.5∶1, 4∶1) were prepared using homogeneous precipitation hydrothermal method. The representative sample (3:1) TiO₂/CuS contained Cu-S characteristic bonds and Ti-O-Ti bonds by FTIR. XRD characterization showed that the (101) and (204) characteristic crystal planes containing CuS(102) and TiO₂ were successfully combined. UV vis DRS characterization showed that after recombination, the absorption band edge shifted red and the light response range was enhanced. PEC and PL characterization showed that TiO₂/CuS composite formed a heterojunction to delay photo-generated electron (e^-)-hole (h⁺) recombination. After using a 350W xenon lamp to simulate the degradation of phenol and tetracycline (TC) under sunlight, the photocatalytic activity of the sample was tested. It was found that the optimal photocatalytic degradation activity was achieved when the TiO₂/CuS molar ratio (3:1) was used, with degradation rates of 99.38% and 97.99% for phenol and TC, respectively. The rate constants were 0.052 48 min^-1 and 0.036 43 min^-1, respectively, which were 3.503 3 and 2.207 8 times higher than pure TiO₂. Free radical capture experiments conducted on (3:1) TiO₂/CuS samples found that the inhibitory effect of superoxide radical (O^2-) was the most significant, indicating that O^2- was the main active substance involved in the reaction. The heterojunction formed by the combination of TiO₂ and CuS is beneficial for the separation of e^--h⁺, promoting the increase of active free radical content and improving photocatalytic activity, which has application prospects.