Hybrid nanofilms from zinc-peroxide/poly(acrylamide) (ZnO2/PAAm) and zinc-peroxide/poly(N-isopropyl-acrylamide) (ZnO2/PNIPAAm) were prepared using the photopolymerization procedure. The thin layers were prepared by the combination of the Layer-by-Layer (LbL) self-assembly method and photopolymerization using UV light in every step of the procedure. The hybrid multilayer films consisting of layers of zinc peroxide nanoparticles and hydrogel alternating in a sandwich-like fashion with thicknesses of 65-246 nm. The chemical structures of the hybrid films were investigated by FTIR spectroscopy, their morphology was studied by atomic force microscopy (AFM). The build up of the films was studied by measuring the optical reflection spectrum, and we have calculated the refractive index and layer thickness of the hybrid layers using simulating software. The adsorption properties of the ZnO2/hydrogel nanohybrid composite networks were investigated by measuring water and ethanol vapour adsorption by a quartz crystal microbalance (QCM). It was established that on partially hydrophobic ZnO2/PNIPAAm hybrids the adsorbed amounts were lower, against the hydrophilic ZnO2/PAAm film the vapour amount was higher. These results correspond to those of the bulk gel swelling results. (C) 2009 Elsevier B.V. All rights reserved.