The study of environmentally friendly semiconductor photocatalysts has important practical significance for efficient photocatalytic hydrogen evolution. In this experiment, type II heterojunction NiCo-LDH/CeO₂ was prepared by in situ loading, and the NiCo-LDH/CeO₂ catalyst showed good activity under simulated sunlight irradiation. Under simulated visible light irradiation, its hydrogen production rate reached 2.7 mmol h⁻¹ g⁻¹, which was higher than that of NiCo-LDH (0.86 mmol h⁻¹ g⁻¹). Through a series of characterization data, it can be concluded that the heterojunction successfully constructed by the close contact between NiCo-LDH and CeO₂ accelerates the separation of photogenerated electrons and holes and can effectively inhibit the recombination of the two so that more electrons are involved in the hydrogen evolution reaction. The material has good interfacial charge transfer performance, which improves the photocatalytic performance. This work can provide an effective method for the research and development of NiCo-LDH.