ZnS:Cu/Poly(vinyl alcohol) (PVA) composite nanofibers have been successfully prepared by electrospinning technique. The formation of ZnS: Cu/PVA nanofibers were carried out by reacting H2S with Zn(AC)(2):Cu/PVA nanofibers, which were electrospun from the mixture aqueous solution of Zn(Ac)(2), Cu(Ac)(2) and PVA. Scanning electron microscopy (SEM), transmission electron microscopy (TEM) and X-ray-diffraction (XRD) analyses revealed that the morphology of the ZnS:Cu/PVA nanofibers consists of the dispersion of ZnS:Cu nanopaticles with cubic structure in PVA nanofibers. The coordinations between -OH and Zn2+:Cu were characterized by infrared spectroscopy. The photoluminescence spectroscopy studies showed the significant difference between the ZnS/PVA fibers and the ZnS:Cu/PVA fibers. The luminescence decay time measure further invested that the Cu was doped in the ZnS crystal. (c) 2006 Elsevier B.V. All rights reserved.