By using a powder method, a new method for producing semiconductor/polymer nanocomposites, lead sulfide (PbS) nanoparticles were prepared and dispersed in either poly(methylmethacrylate-co-methacrylic acid) or poly(styrene-co-styrenesulfonic acid). The size of the nanoclusters was less than 2 nm, and the size distribution was rather sharp, determined by UV-vis absorption spectroscopy. The absorption spectra of the PbS-containing sheets showed a blue shift and the absorption edges were steep, reflecting the formation of nano-sized PbS clusters. The spectra also exhibited an absorption maximum, which is an indication of a narrow particle size distribution. The glass transition temperature (T-g) of the PbS-containing nanocomposites was higher than that of the corresponding ionomer. The effect of heat treatment on the aggregation of PbS is also discussed. The dissolution of powder samples, followed by neutralization of acidic groups, led to reduction of particle sizes, suggesting the usefulness of ionic groups for stabilizing PbS nanoclusters. (c) 2005 Elsevier Ltd. All rights reserved.