Abstract: Herein, CoWO4/g-C3N4, NiWO4/g-C3N4, and CoxNi1_xWO4/g-C3N4 (x = 0.66, 0.5, 0.33) nanostructures are synthesized via hydrothermal and calcination methods. The structural, electrochemical, and morphological characteristics of each nano-carrier are systematically analyzed. The fabricated heterostructures exhibit promising activities towards photocatalytic gas-phase CO2 reduction and photoelectrochemical (PEC) water splitting under visible light illumination, where the type II heterostructure interface plays a crucial role by enhancing the number of active sites and improving the charge-transfer efficiency, leading to a modified charge transfer pathway. Among the synthesized heterostructures, Co0.66Ni0.33WO4/g-C3N4 exhibits the lowest band gap compared to other catalysts, demonstrating superior photocatalytic performance for gas-phase CO2 conversion, achieving CO selectivity of 3.1% and H2 production rates of 651 µmol m-2 s-1 under visible light illumination. Optimal Co loading enhances H2 production and the solar-to-hydrogen conversion efficiency via PEC solar water splitting, while excessive Ni content may hinder process performance. These findings highlight the potential of the developed materials for solar fuel production via photo(electro)chemical processes.

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