CdSe nanoparticles of improved stability against aggregation were synthesized by using amphiphilic block copolymer polyacrylonitrile-block-poly(ethylene glycol)-block-polyacrylonitrile (PAN-b-PEG-b-PAN, PEA). The products were characterized by X-ray diffraction (XRD), high-resolution transmission electron microscopic (HRTEM). The optical properties were characterized by UV-vis spectrophotometer and the room temperature photoluminescence (PL). The results revealed that the CdSe nanoparticles have been uniformly distributed throughout the copolymer with diameters of 6-7 nm and the produced novel hybrid nanocomposites displayed obviously quantum size effects and interesting fluorescence features. FTIR results provided the information on the interaction between the copolymer and the nanoparticles. The TGA revealed that the thermal property of the copolymer enhanced due to the interaction of the nanoparticles and the groups of the copolymer. (c) 2006 Published by Elsevier Inc.