A simple, non-toxic, low-priced, and reproducible manipulation, which meets the standards of green chemistry, is introduced for the synthesis of ZnSxSe1-x nanofibers. ZnSxSe1-x nanofibers have been prepared in the entire composition range from ZnSe to ZnS by using a low-cost wet-chemical method. The effects of polymer (PVB) concentrations, reactant.S/Se) concentrations and reaction conditions (applied voltage, viscosity, and work distance) have been investigated. We have demonstrated that wurtzite ZnSxSe1-x showing a fiber-like morphology can be kinetically stabilized in the presence of an electrospinning system.