In this study, Z-scheme NiO/BiO 2Àx heterojunction was successfully constructed by hydrothermal method, which can maintain strong redox potential and excellent visible light response and effectively improve the separation efficiency of photogenerated carrier. Under visible irradiation, the impact of different contents of NiO in NiO/BiO 2Àx on photocatalytic activity was explored, and the results shown that 3-NiO/BiO 2Àx had the highest photocatalytic activity. The degradation rate of 3-NiO/BiO 2Àx for methyl orange (MO) was 7.69 times and 19.7 times higher than pure BiO 2Àx and NiO, respectively. Moreover, the degradation rate of 3-NiO/BiO 2Àx for ciprofloxacin (CIP) was 7.54 times and 60.8 times higher than that of the pure BiO 2Àx and NiO, respectively. NiO/BiO 2Àx heterojunction can be used in the field of wastewater treatment due to their excellent degradation activity for organic pollutants.