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A heterostructural composite composed of g-C3N4 and Bi2O3 was achieved by the one-pot and thermal-induced polycondensation method using melamine and Bi(NO3)3 as precursor at 550 ℃ under air atmosphere. The crystalline phase, components and morphologies of the as-prepared composites were investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). Besides, the photocatalytic activity of composites was evaluated by degrading RhB aqueous solution at room temperature under visible light irradiation. Compared with bulk g-C3N4, the photocatalytic efficiency of the 0.5% Bi2O3/g-C3N4 (Bi–CN) was increased by up to four times. The introduction of Bi2O3 enhances not only the light absorption ability, but also the separation of photogenerated electron–hole pairs.
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