Nanocrystals of ZnS have been synthesized through simple chemical precipitation method using thiourea as sulphur source. The synthesized products were annealed at different temperatures in the range of 200–800∘C. The as-synthesized and annealed samples were characterized by X-ray diffraction (XRD), UV-Visible absorption (UV-Vis), and room temperature photoluminescence (PL) measurements. The morphological features of ZnS annealed at 200 and 500∘C were studied by atomic force microscope (AFM) and transmission electron microscope (TEM) techniques. The phase transformation of ZnS and formation of ZnO were confirmed by thermogravimetric (TG) and differential thermal analysis (DTA) curves.