This study builds on our earlier efforts by incorporating two different semiconductors (WO3 and TiO2) in a Ni film matrix by occlusion electrosynthesis. Three such composite films along with Ni/WO3 and Ni/TiO2 end-members were characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, electron probe microanalysis, stylus profilometry, and UV-vis reflectance spectroscopy. The photoelectrochemical (PEC) activity of these films was monitored in 0.1 M KNO3 supporting electrolyte with and without organic additives. Morphological trends as well as those in the PEC activity of the film when the relative amounts of WO3 and TiO2 are varied in the deposition bath are discussed along with factors related to particle uptake in the occlusion film deposition process. (C) 2003 Elsevier Science B.V. All rights reserved.