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Fe-doped cadmium sulfide was prepared by hydrothermal method in aqueous solution using cadmium nitrate, ferric nitrate and thiourea as raw materials. The samples were characterized by SEM, XRD, EDS and XPS. The photocatalytic degradation of methylene blue (MB) in aqueous solution was used as a target reaction to evaluate their photocatalytic activity. The experimental results show that the reaction temperature has a great effect on the morphology of cadmium sulfide, and spherical, flowerlike, clustered and rodlike cadmium sulfide are obtained in various reaction temperatures. Among them, the photocatalytic activity of flowerlike CdS is observed to be better than other CdS materials. The XRD indicates that Fe-doped cadmium sulfide is hexagonal crystal structure when the reaction temperature is 160℃. The experimental results also indicate that Fe-doped can obviously improve the photocatalytic activity of cadmium sulfide and when the doping ratio of Fe to Cd is 1:10, the photocatalytic effect is the best of all.