The sluggish kinetics of Oxygen Evolution Reaction (OER) is a challenge for the development of efficient photoelectrochemical (PEC) systems for sustainable hydrogen production. In this work, α-Fe₂O₃/g-C₃N₄ photoanodes were prepared from g-C₃N₄ of different precursors (urea, melamine and/or dicyandiamide) to investigate the influence of hybrid precursor engineering on the photoelectrochemical properties of the heterostructures. The incorporation of hybrid precursor derived g-C₃N₄ modified the structural and optical properties of the composite photoanodes and resulted in enhanced PEC response compared to single precursor systems. The as prepared composite with g-C₃N₄ prepared from ternary hybrid precursors (urea, melamine and dicyandiamide) showed the best performance among the as prepared samples with lowest onset potential (0.01 V) and highest ΔE (0.88 V) under the present experimental conditions. Photoluminescence analysis indicated a lower emission intensity of the ternary hybrid precursor-derived sample, which was attributed to the inhibited charge carriers recombination. Furthermore, the addition of 5-hydroxymethylfurfural (HMF) as a model organic substrate increased the photocurrent density (~95%) with no change in the onset potential, demonstrating the effective hole scavenging ability of the HMF. Chronopotentiometry measurements confirmed stable operation during continuous illumination. These findings demonstrate that the hybrid precursor engineering of g-C₃N₄ can affect the PEC behavior of α-Fe₂O₃/g-C₃N₄ photoanodes under HMF-assisted conditions.
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