In this study, we have successfully created nanopebble structure of FeVO4 (FVO) on FTO substrate by an in-situ solid-state transformation of hydrothermally grown FeOOH nanostructured thin film. A novel heterojunction has been created through the dropcoating of Fe2TiO5 (FTiO) nanoparticles (NPs) over the FVO nanopebble structure. Structural, morphological, and optical analyses proved that the FVO/FTiO composite had formed. XPS showed oxygen vacancies within the heterojunction. Photoelectrochemical (PEC) and photoluminescence measurements verified enhanced charge separation and carrier transport. Notably, an optimum coating of FTiO NPs exhibited an impressive photocurrent measure of 0.7 mA cm-2 at 1.6 V vs VRHE in 0.1 M KPi electrolyte, which is 2.35 fold stronger compared to the performance of bare FVO nanopebble thin film. Along with this the better stability of FVO/FTiO photoelectrode indicates the enhanced performance of the FVO/FTiO heterojunction. A comprehensive analysis using various techniques was conducted to delve deeper into the improved PEC performance for the above heterojunction. These included photoelectrochemical impedance spectroscopy (PEIS), Mott-Schottky curves, and band structure diagrams. These methods provide a more thorough understanding of the underlying mechanisms behind developing superior n-n heterojunction photoanodes for enhanced PEC performance.
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