Multilayer structures of alternate organic and inorganic semiconductors were fabricated by the wet processes that control thickness of each layer with nanometre level. Organic layers were deposited as electron-donor including poly (p-phenylene vinylene) by the layer-by-layer adsorption method. Inorganic layers composed of titanium oxide were fabricated as electron-acceptor by the surface sol-gel process. Clearly, periodic and uniform nanostructures were confirmed by glow discharge optical emission spectroscopy and transmission electron microscopy analyses. The multilayer exhibited a photovoltaic effect under illumination. The fabrication of those structures by wet process under room temperature and normal pressure will be one of the important methods in energy-saving nano-technology. (C) 2003 Elsevier B.V. All rights reserved.