| Summary: | Hematite (α-Fe<sub>2</sub>O<sub>3</sub>) and pseudobrookite (Fe<sub>2</sub>TiO<sub>5</sub>) suffer from poor charge transport and a high recombination effect under visible light irradiation. This study investigates the design and production of a 2D graphene-like r-GO/GO coupled α-Fe<sub>2</sub>O<sub>3</sub>/Fe<sub>2</sub>TiO<sub>5</sub> heterojunction composite with better charge separation. It uses a simple sonochemical and hydrothermal approach followed by L-ascorbic acid chemical reduction pathway. The advantageous band offset of the α-Fe<sub>2</sub>O<sub>3</sub>/Fe<sub>2</sub>TiO<sub>5</sub> (TF) nanocomposite between α-Fe<sub>2</sub>O<sub>3</sub> and Fe<sub>2</sub>TiO<sub>5</sub> forms a Type-II heterojunction at the Fe<sub>2</sub>O<sub>3</sub>/Fe<sub>2</sub>TiO<sub>5</sub> interface, which efficiently promotes electron-hole separation. Importantly, very corrosive acid leachate resulting from the hydrochloric acid leaching of ilmenite sand, was successfully exploited to fabricate α-Fe<sub>2</sub>O<sub>3</sub>/Fe<sub>2</sub>TiO<sub>5</sub> heterojunction. In this paper, a straightforward synthesis strategy was employed to create 2D graphene-like reduced graphene oxide (r-GO) from Ceylon graphite. The two-step process comprises oxidation of graphite to graphene oxide (GO) using the improved Hummer’s method, followed by controlled reduction of GO to r-GO using L-ascorbic acid. Before the reduction of GO to the r-GO, the surface of TF heterojunction was coupled with GO and was allowed for the controlled L-ascorbic acid reduction to yield r-GO/GO/α-Fe<sub>2</sub>O<sub>3</sub>/Fe<sub>2</sub>TiO<sub>5</sub> nanocomposite. Under visible light illumination, the photocatalytic performance of the 30% GO/TF loaded composite material greatly improved (1240 Wcm<sup>−2</sup>). Field emission scanning electron microscopy (FE-SEM) and high-resolution transmission electron microscopy (HR-TEM) examined the morphological characteristics of fabricated composites. X-ray photoelectron spectroscopy (XPS), Raman, X-ray diffraction (XRD), X-ray fluorescence (XRF), and diffuse reflectance spectroscopy (DRS) served to analyze the structural features of the produced composites.
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