CdS nanostructured materials were prepared by a chemical synthesis via the reaction of Cd(NO 3 ) 2 ·4H 2 O and various sulfur sources. The products were characterized by X-ray powder diffraction (XRD) and transmission electron microscopy (TEM). The results indicated that the samples prepared with Na 2 S·9H 2 O were zinc blende crystal structure in sphere-like shape and the products prepared with thiourea and sulfur were both wurtzite crystal structures in rod-like shape. The room-temperature luminescence revealed that all the CdS nanostructured materials had a broad green emission band and a red emission band. In addition, the growth mechanisms of the CdS nanocrystals were preliminarily discussed.