The poly(methyl methacrylate-co-vinylbenzyl chloride) (P(MMA-co-VBC))@PbS hybrid nanofibers prepared by a surface-initiated atom transfer radical polymerization (ATRP) of lead dimethacrylate (LDMA) and acidolysis by H2S were reported. The P(MMA-co-VBC) nanofibers were synthesized by the solution copolymerization of methyl methacrylate (MMA) and vinylbenzyl chloride (VBC) monomers, followed by the use of electrospinning technique. After the ATRP of LDMA and acidolysis by H2S, the resulting P(MMA-co-VBC)@PbS hybrid nanofibers were obtained. The results indicated that the hybrid nanofibers were successfully prepared and exhibited absorption and emission behaviors due to the existence of PbS nanoparticles. (C) 2009 Elsevier B.V. All rights reserved.