Abstract: This experiment converts the research topic “Preparation of Fe₂O₃/Ni_1-xFe_xS photoanodes and investigation of their photoelectrochemical oxygen evolution performance” into a project-based inquiry comprehensive chemistry experiment for senior undergraduates. Composite photoanodes were synthesized on F-SnO₂ (FTO) conductive glass by a hydrothermal-sulfidation method. The phase composition and morphology of the materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM), while the oxygen evolution performance was evaluated by linear sweep voltammetry (LSV) and photoelectrochemical impedance spectroscopy (PEIS) under simulated solar irradiation. The results show that the composite photoanode achieves a photocurrent density of 3.10 mA·cm^-2 at 1.23 V vs. RHE, which is 2.3 times that of pristine Fe₂O₃. The teaching practice follows a five-stage project-based process: problem guidance, scheme design, experimental implementation, data analysis, and achievement reporting. Most students reported that this experiment deepened their understanding of photoelectrocatalysis principles. The experimental content integrates multidisciplinary knowledge, including material synthesis, photoelectrochemistry, interfacial catalysis, and instrumental analysis, aiming to consolidate students’ fundamental theories while cultivating their scientific research thinking and comprehensive analytical abilities. This design provides a reference case for integrating photoelectrocatalysis into comprehensive chemistry laboratory teaching.

Key words: Project-based inquiry, Comprehensive chemistry experiment, Photoelectrocatalysis, Oxygen evolution reaction, Fe₂O₃ photoanode, Ni_1-xFe_xS co-catalyst