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Starting from the raw materials of Li2S and P2S5, Li7P3S11glass-ceramic electrolytes were prepared via mechanical milling and heat treatment.By controlling the temperature and the duration of the heat treatment, the influence of sulfur losson the formation of Li7P3S11metastable crystalline phase have been studied.Thestructure and compositionof theglass-ceramic electrolytes were characterizedby XRD,raman spectra and EDS.which indicate that a high-temperature long-duration heat treatment would result in the loss of sulfur, and consequently leads to the formation of P-P homopolar bonds and the decomposition of the highly ionic-conductive meta-stable phase.It is demonstrated that the glass-ceramic electrolyte has lowest sulfur loss and complete crystallization after a 260 ℃ heat treatment for 1 h.Thus the highest ionic conductivity can be achieved under this synthetic condition.