Abstract Cu 2 O nanoparticles and MoS 2 nanoflowers decorated with ZnO nanospheres were successfully co-deposited on Cu mesh via a mild electrodeposition method to build a dual direct Z-scheme heterostructure. The prepared materials can effectively synthesize ammonia with N 2 and H 2 O in the liquid membrane reactor under simulated visible light. The results indicate that 3D nanomaterials exhibit better performance compared to a pure semiconductor due to the synergistic effect of enhanced visible light absorption, longer photogenerated carrier lifetime and the specific charge transfer path of dual direct Z-scheme structure. Meanwhile, the hydrophilicity of Cu 2 O/MoS 2 /ZnO rapidly makes the surface of the catalyst wet when it participates in the photo reaction, which promotes the contact between the reactant and exciton. This work proposes the electron transfer and possible reaction mechanism corresponding to the designed catalyst, which can provide a reference for other photocatalytic applications using a semiconductor heterojunction as a catalyst.