In this investigation, hollow sphere-like ZnS/ZnAl2S4 nanocomposites have been successfully synthesized by solvothermal process in propylene glycol as solvent. To study the effect of sulfur source on the morphology of ZnS/ZnAl2S4 nanocomposites, thioacetamid and thiourea were applied. In the all experiments, Al(NO3)3·9H2O and Zn(OAc)2 were used as aluminium and zinc precursors, respectively. The as-synthesized products were characterized by XRD, SEM, FT-IR, TEM, PL, and EDS. According to SEM images, it was found that the type of sulfur source, capping agent and reaction time had a great influence on the morphology of ZnS/ZnAl2S4 nanocomposites. The novelty of this investigation is related to the synthesis hollow and hierarchical microspheres of ZnS/ZnAl2S4 by using thiourea as sulfur source in the absence and presence of sodium dodecyl sulfate as capping agent, respectively.