<![CDATA[Photoelectrocatalytic (PEC) water splitting utilizing titanium dioxide (TiO2) photoanodes presents a promising avenue for sustainable hydrogen production. Understanding the correlation linking the synthesis conditions to structural and phase evolution of semiconductor materials, which is essential for the development of photoanodes with improved PEC activity, remains challenging. This study aims to elucidate the structure- and phase-dependent PEC activity of TiO2 nanoparticles (NPs) obtained via the non-isothermal decomposition of titanium oxyacetylacetonate (TiO(acac)₂) precursor at varying final temperatures (Tfin). The microstructural parameters and phase composition of the TiO2 NPs were determined via Rietveld refinement of X-ray diffraction (XRD) data. The PEC activity of spin-coated TiO2/FTO photoanodes was evaluated via open-circuit potential (OCP) measurements, OCP decay, and linear sweep voltammetry (LSV) under chopped illumination. The results indicate that the anatase-rutile ratio and crystallite dimensions can be modulated by varying Tfin in the range of 500-700 °C. An optimized mixed-phase TiO2 comprising 71.7% anatase and 28.3% rutile, with the crystallite sizes Dav of 29.6 nm and 55.6 nm, respectively, is achieved at 650 °C enabling an efficient transition to free-electron transport and maximized photoactivity. These findings offer essential design principles for managing structural and phase transformations in TiO2-based photoanodes via the metal-organic decomposition route. Copyright © 2026 by Authors, Published by BCREC Publishing Group. This is an open access article under the CC BY-SA License (https://creativecommons.org/licenses/by-sa/4.0).]]>
Copyrights © 2026
