In the present work we report the sol-gel synthesis of pure TiO₂ and (TiO₂)_1−x(Fe₂O₃)_x nanocomposites with different Fe₂O₃ contents (x = 0, 0.1, 0.5, and 1.0 for pure TiO₂, Fe₂O₃ incorporated 0.1, 0.5, and pure Fe₂O₃ which are denoted as PT, 0.1F, 0.5F, and PF, respectively). The structural, morphological, optical, and surface texture of the prepared nanocomposites were characterized using various techniques. The structural studies confirm the strong influence of Fe₂O₃ contents on the crystallite sizes and dislocation values. The size of the crystallites was increased by the increase in Fe₂O₃ contents. The bandgap values elucidated from DRS analysis were decreased from 3.15 eV to 1.91 eV with increasing Fe₂O₃ contents. The N₂-Physorption analysis has confirmed the mesoporous nature of the samples with a comparable specific surface area of 35 m²/g. The photoelectrochemical measurements (CV, CA and EIS) were performed to assess the photoelectric properties of the prepared materials. It was found that the PT samples have the highest catalytic activity and photocurrent response compared to other composites. The reduction in current density was as follows: 2.8, 1.65, 1.5 and 0.9 mA/cm², while the photocurrent response was ca. 800, 450, 45, 35 µA/cm² for PT, 0.1F, 0.5F and PF samples, respectively. The EIS results showed that the (TiO₂)_1−x(Fe₂O₃)_x nanocomposites exhibit lower charge transfer resistance than pure titania and hematite samples.