The photocatalytic H2 production technology exhibits promising potential in addressing the challenges of environmental pollution and energy crisis. In this work, CuS particles decorated MoS2 seaweed spheres (MoS2/CuS) were synthesized through a hydrothermal method, then they are loaded on the surface of g-C3N4 nanosheets using a solvent evaporation strategy to form MoS2/CuS/g-C3N4 double S-scheme heterojunction. The investigation reveals the H2 production rate of 25 wt% MoS2/CuS/g-C3N4 can reach up to 1438 μmol·g-1·h-1, which is 14.8-fold of g-C3N4 (97 μmol·g-1·h-1). Further studies indicate that the introduction of MoS2/CuS can broaden the light absorption range, increase electrochemical specific surface area, reduce the activation energy for H2 production and increase hydrophilicity of the composite. Especially, CuS can suppress carrier recombination effectively through its electron storage and release ability. Based on the experimental and theoretical analysis of band structures, the charge transfer in MoS2/CuS/g-C3N4 shares optimized double S-scheme charge transfer pathways with a dual reduction site, leading to an enhanced H2 evolution kinetics. This work offers valuable insights for the advancement of novel double S-scheme heterojunctions, showcasing their potential in energy storage and photothermal enhancement effects.
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