Langmuir-Blodgett (LB) technique has been applied to fabrications of various nanoparticulate assemblies such as monolayer and multilayer of US particles, in-plane mixed monolayer and alternate multilayer of CdS/TiO2 particles on the solid substrate. We examined the most favorable conditions for yielding uniform and dense packing of the particles in a 2-dimensional arrangement, followed by structural characterization of the as-deposited particulate layers. As a result, it was found for the Us particulate films that charge density of cationic Langmuir monolayer markedly influences the amount of particles embedded on the substrate and that multilayer LB deposition enables stepwise control of thickness for the particulate assemblies. For the composite CdS/TiO2 particulate films, desired in-plane mixing ratio and alternating layer structure of two kinds of particles were achieved, on which basis the possibilities of fabricating a variety of heteroparticulate layers are pointed out. In addition, photocatalytic activities of TiO2 and CdS/TiO2 particulate films fabricated by the LB technique were evaluated in terms of decomposition of both oleic acid cast film and stearic acid (SA) LB film by irradiating with UV light. The results exhibited that when the bilayer of TiO2 particulate film is employed in place of the monolayer film, the photodecomposition rate of SA is sufficiently accelerated and that the alternate CdS/TiO2 particulate layer is less active for the oxidative decomposition. (c) 2005 Elsevier B.V. All rights reserved.