Nickel-doped zinc sulfide nanoparticles were successfully synthesized in air atmosphere through chemical precipitation method using surfactants in aqueous medium. The product was characterized by different techniques such as X-ray diffraction (XRD), transmission electron microscopy (TEM), fourier transform infrared spectrometer (FT-IR), UV-visible absorption and photoluminescence (PL). Crystal structure, size and morphology of the ZnS:Ni 2? nanoparticles were investigated by XRD and TEM. In the PL emission, a couple of new peaks were observed instead of a single peak by changing the precursor solution. In addition, an enhanced PL emission was observed using surfactants. Phase changes were also observed at different temperatures.