CS2-modified titanate nanotubes (CS2/TiO2–NTs) are fabricated by reaction of CS2 and Ti–O2Na+ species on titanate nanotubes. Pb2+ ions are coated on the modified nanotubes by ion exchange (Pb/CS2/TiO2–NTs). The products are characterized by means of nitrogen adsorption-desorption isotherms at 77 K (BET method), transmission electron microscopy (TEM), X-ray photoelectron spectrometry (XPS), X-ray diffraction (XRD), atomic absorption spectrometry (AAS), and diffuse reflectance spectroscopy (DRS). The photocatalytic performances of the products are evaluated by monitoring their catalytic activities for degradation of methyl orange under UV light irradiation. The effects of calcination temperature and atmosphere on the photocatalytic performance are investigated. The results reveal that the photocatalytic activities of CS2/TiO2–NTs and Pb/CS2/TiO2–NTs are far higher than that of primary nanotubes, and the optimum calcination temperature is 500 °C under N2 atmosphere. It is also discovered that physically adsorbed Pb2+ ions affect the photocatalytic activity of Pb/CS2/TiO2–NTs obviously. The photocatalytic activity of washed Pb/CS2/TiO2–NTs is higher than that of the unwashed one under the same thermal treatment and reaction conditions.
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