Publication date: 21st July 2025
Photoelectrochemical (PEC) CO2 conversion using a p-type semiconductor offers a sustainable pathway to transform greenhouse gases into value-added chemicals. Cu2WO4 has emerged as an interesting photocathode for PEC CO2 reduction reaction (CO2RR) due to its suitable electronic and optical properties (Eg 1.85 eV). The Cu2WO4 was synthesized by arc-melting method using a mixture of copper oxide and tungstate oxide as precursors. The XRD measurement of the particles synthetized revealed the triclinic-P1 Cu2WO4 pattern which was corroborated by Rietveld refinement, demonstrating that any additional phase would be below the detection limit of the diffractometer. A photoresponsive gas diffusion electrode (GDE) containing Cu2WO4 (GDE/Cu2WO4) was prepared by depositing an ink of Cu2WO4 particles onto commercial carbon paper followed by heating. Ethanol (1.9 μg h−1 cm−2) and formate (16.5 μg h−1 cm−2) were produced in unassisted photoelectrolyzer assembled with the GDE/Cu2WO4 and Ti|BiVO4/ FeOOH/NiOOH (9.0 cm2) photoanode. The morphological and structural properties of GDE/Cu2WO4 after CO2 photoelectrolysis were investigated by XRD measurements. These studies demonstrated diffraction peaks of Cu2WO4 that remained on the electrode surface, as well as Cu2O possibly resulting from Cu2WO4 photocorrosion. Additionally, we investigate the degradation process of arc-synthesized Cu₂WO₄ during PEC CO₂RR by systematically varying the applied bias and combining XRD, XPS, SEM, EDS, with in situ Raman spectroscopy employed to monitor light-induced structural changes in real time. The results reveal that light-driven degradation below 0.4 V vs. RHE primarily leads to Cu₂O formation as a product from Cu2WO4 instability, while purely electrochemical corrosion at 0.3 V vs. RHE favors the generation of metallic Cu. This study demonstrated the development of an innovative light-responsive gas diffusion electrode based on Cu2WO4 for CO2 conversion and provide mechanistic insights into Cu2WO4 photocorrosion pathways to enhance the its long-term stability for solar fuel production.
The authors gratefully acknowledge support from Unicamp, CINE, FAPESP (Process 2021/05853-8 and 2023/02684-6), CNPq and CAPES.
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