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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.