Using CdSO4 and Na2S as the precursor, nanocrystalline CdS with a crystallite size of 4.6 nm was prepared in oleic acid system, while the same thing with a crystallite size of 10nm was prepared in hydrothermal system. The characteristics of obtained CdS were studied by XRD and TEM. The photocatalytic activities of the prepared samples were evaluated by decoloration reaction of methylorange. The results of experimentation showed that nanocrystalline CdS had good photocatalytic activities.