| Summary: | In the present work we report the sol-gel synthesis of pure TiO<sub>2</sub> and (TiO<sub>2</sub>)<sub>1−x</sub>(Fe<sub>2</sub>O<sub>3</sub>)<sub>x</sub> nanocomposites with different Fe<sub>2</sub>O<sub>3</sub> contents (x = 0, 0.1, 0.5, and 1.0 for pure TiO<sub>2</sub>, Fe<sub>2</sub>O<sub>3</sub> incorporated 0.1, 0.5, and pure Fe<sub>2</sub>O<sub>3</sub> 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 Fe<sub>2</sub>O<sub>3</sub> contents on the crystallite sizes and dislocation values. The size of the crystallites was increased by the increase in Fe<sub>2</sub>O<sub>3</sub> contents. The bandgap values elucidated from DRS analysis were decreased from 3.15 eV to 1.91 eV with increasing Fe<sub>2</sub>O<sub>3</sub> contents. The N<sub>2</sub>-Physorption analysis has confirmed the mesoporous nature of the samples with a comparable specific surface area of 35 m<sup>2</sup>/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/cm<sup>2</sup>, while the photocurrent response was ca. 800, 450, 45, 35 µA/cm<sup>2</sup> for PT, 0.1F, 0.5F and PF samples, respectively. The EIS results showed that the (TiO<sub>2</sub>)<sub>1−x</sub>(Fe<sub>2</sub>O<sub>3</sub>)<sub>x</sub> nanocomposites exhibit lower charge transfer resistance than pure titania and hematite samples.
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