This paper presents a new synthetic route to hybridize ZnS semiconductor nanoparticles and poly(vinyl alcohol) (PVA) based electrospinning nanofibers. At first, zinc ions are introduced onto the surface of carboxylic PVA nanofibers. Then sulfide ions are added to react with zinc ions to form ZnS nanoparticles. The average diameter of the nanofibers is about 300 run, and the diameter of the ZnS nanoparticles is about 5 nm. The photoluminescence spectrum of ZnS/carboxylic PVA nanocomposites has a 60 nm blue shift compared with that of the corresponding bulk ZnS sample. The carboxylic PVA enhances the quantum effects of the ZnS nanoparticles. (C) 2007 Elsevier B.V. All rights reserved.