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A novel visible-light photocatalyst, Sb2S3, was synthesized with a simple method. The specimen was characterized by X-ray diffraction, transmission electron microscopy, Brunauer−Emmett−Teller (BET) surface area analysis, and UV−vis diffuse reflectance spectroscopy. The results revealed that the as-synthesized sample was orthorhombic phase and consisted of rodlike particles. It possessed a surface area of 15.1 m2·g−1, and the band gap was about 1.66 eV. The photocatalytic activity of Sb2S3 nanorods was evaluated by the decomposition of methyl orange in aqueous solution under visible-light irradiation. The results demonstrated that the photodegradation ratio of methyl orange was up to 97% after 30 min of irradiation, which was much better than that of CdS and TiO2−x N x under the same condition. Meanwhile, the possible mechanism of the photocatalytic reaction had also been studied by liquid chromatography−mass spectrometry, and the •OH had been detected also by terephthalic acid photoluminescence probing technique.

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A cost- and time-saving coupling method was developed to prepare a novel Sb2S3/TiO2 heterostructure photocatalyst. The obtained sample was characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and UV–vis diffuse reflectance spectroscopy (DRS). UV–vis diffuse reflectance spectra showed a great shift to longer wavelengths and an extension of the absorption in the visible region for all of the samples compared to pure TiO2. The photocatalytic activity of the sample was investigated for the liquid-phase photocatalytic degradation of azo dyes under visible light irradiation. The influences of different mass ratios of Sb2S3 and sintered temperatures on the photocatalytic activity have also been investigated, and the highest efficiency is observed when calcined at 673 K with 60 wt % Sb2S3 content. Moreover, •OH has also been detected in the suspension of Sb2S3/TiO2 heterojunction under visible light irradiation, which leads to the decomposition of azo dyes.