Mn2+, Co2+, or Ni2+ monodoped CdS (or ZnS) and Mn2+-Co2+-Ni2+ tridoped CdS (or ZnS) have been successfully synthesized by novel one-step thermolysis method using thiourea as a sulphur source. The synthesized nanomaterials were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). It is found that the average diameter and