Environmental pollution is becoming ever more serious, and photodegradation using sustainable energy-solar energy is of great importance. Studies have revealed that semiconductor compound photocatalysts have a wide range of promising applications in the treatment of environmental pollution. Based on the current view, we synthesized flower-like 3NiS/Zn 0.5 Cd 0.5 S composite catalyst for photodegradation reaction by a two-step method. We analyzed the growth mechanism of the catalysts in terms of reaction time and reaction temperature, and characterized the composites utilizing FSEM, XRD, UV–vis, and XPS. The results showed that the 3NiS/Zn 0.5 Cd 0.5 S composites synthesized under the optimal conditions we obtained experimentally had higher photocatalytic performance with 99.1% final conversion rate in 1h compared to the 97.7% final conversion efficiency of pure Zn 0.5 Cd 0.5 S in 1.5 h, which showed higher conversion efficiency and conversion rate, meanwhile, after 8 cycles of stability experiments, the stability of the composite remained good. Of course, the stability of the photocatalyst is also essential. Fig. 6(d) shows the cycle stability test of 3NiS/ZCS photodegradation. After eight cycles, the final conversion efficiency remains high at 95.4%, which shows good cycling stability. • Flower-like 3NiS/Zn 0.5 Cd 0.5 S were obtained by Simple and low-cost hydrothermal and solution impregnation methods. • Flower-like 3NiS/Zn 0.5 Cd 0.5 S has a higher visible light utilization efficiency than pure Zn 0.5 Cd 0.5 S. • The synthesis of our flower-like 3NiS/Zn 0.5 Cd 0.5 S with high photocatalytic properties and good cycling stability is promising for industrial applications. [ABSTRACT FROM AUTHOR]