The precursore Zn(en)2S (en=ethylenediamine) were prepared via a solvothermal process from elemental sulfur and zinc using ethylenediamine as a solvent. Detailed characterizations of the infrared (IR) absorption spectrum, powder X-ray diffraction (XRD) and thermogravimetric analysis (TG) confirmed two en coordinated with Zn2+to form a complex cation. The morphological property was also characterized by transmission electron microscopy (TEM ) and electron diffraction analysis (ED). Phase-pure hexagonal wurtzite ZnS products were obtained by annealing the precursor in nitrogen stream at about 900℃. Zn(en)2S showed a nanosize of about 30 nm, and ZnS of about 60 nm. The fluorescence spectra were also studied. PL results showed that Zn(en)2S excited a fluorescence at 452 nm.