In this study, the ZnS composite powders for host material in phosphor was synthesized in situ by mechanical alloying. As the mechanical alloying time increases, particle size of ZnS decreases. ZnS powders of in a mean size was fabricated by mechanical alloying for 10h. The crystal structures of ZnS powders were investigated by X-ray diffraction and the photo-luminescence properties was evaluated with the optical spectra analyzer. The steady state condition of mechanically alloyed ZnS was obtained as a mean particle size of in 5h milling. The sphalerite and wurtize structures coexist in the ZnS mechanically alloyed for 5h. The ZnS powder mechanically alloyed for 10h grows to the sphalerite structure. And the strong emission peaks of ZnS are observed at 480 nm wave length at the powders of mechanically alloyed for 10h, but the sphalerite and wurtize structures in ZnS coexist and emission peaks are not appeared at the powders of mechanically alloyed for 10h.