A facile layer-by-layer method was used to prepare ZnO nanoparticles embedded in multilayers polymer films. The polymer matrix was formed by layer-by-layer self-assembly technique. By repetitive adsorption of zinc nitrate and subsequent precipitation with ammonium hydroxide, polyelectrolyte multilayer films containing ZnO nanoparticles were fabricated. UV-vis spectra indicate the regular growth of ZnO nanoparticles. Transmission electron microscopy study shows that morphology of the nanoparticles is controlled by the precipitation cycles number. The formation process of the nanoparticles in the multilayers was also discussed. (c) 2007 Elsevier B.V. All rights reserved.