α-Fe 2 O 3 , as a promising photocatalyst in environmental aspects, was doped by a nonmetal to enhance the optical and electronic properties. Sulfur-doped hematite was synthesized by microwave irradiation. The samples were investigated by X-ray diffraction and energy dispersive X-ray-scanning electron microscopy. Nanostructure particles have a hexagonal structure that did not change after sulfur incorporation. The optical studies via UV-Visible spectroscopy proved the high absorbance of S/α-Fe 2 O 3 under the visible region. Moreover, the band gap of S/α-Fe 2 O 3 was shifted to higher wavelengths. However, nonmetals may exhibit a negative effect and act as recombination centers as the photoactivity of undoped hematite was still higher in the photodegradation of methyl orange as a pollutant. H 2 O 2 as an oxidant was fourfold better than O 2 , leading to the formation of the active oxygen species. The preparation method plays a crucial role in the shaping of nanostructure particles and its photoactivity.
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