CdIn2S4 microspheres were synthesized by a facile hydrothermal method with the temperature ranging from 120 to 200 ℃. X-ray diffraction, UV-vis diffuse reflectance spectroscopy, nitrogen sorption analysis, X-ray photoelectron spectroscopy, scanning electron microscopy and transmission electron microscopy were used to characterize the products. It was found that the crystallographic structure and optical property of the products synthesized at different temperature were almost the same. The SBEX of CdIn2S4 products decreased when the synthesized temperature increased, and the largest SBET was 33.16 m2 g-1 （120 ℃ sample）. The degradation of methyl orange （MO） under the visible-light irradiation had been used as a probe reaction to investigate the photocatalytic activity of the as-prepared CdIn2S4, which showed that the CdIn2S4 sample synthesized at 120 ℃ presented the best photocatalytic activity for MO degradation.
