A densely packed TiO2 thin film onto an indium doped-tin oxide (ITO) substrate was synthesized at room temperature by chemical deposition and a US thin film was deposited onto the pre-deposited TiO2 film by a doctor blade route (powder of US was obtained from chemical deposition). TiO2/CdS film was annealed at 300 degrees C for 1 h in air for crystallinity improvement. The first grown TiO2 film was nanocrystalline, whereas the US film was polycrystalline as evidenced by X-ray diffraction (XRD) and selected area electron diffraction (SAED). Scanning electron microscopy (SEM) images show formation of mono-dispersed US spherical grains onto compact, densely packed spherical nanocrystalline grains of TiO2. The TiO2/CdS bilayer film was used in a photo-electrochemical cell as a working electrode, and a platinum electrode as a counter electrode (0.1 M lithium iodide electrolyte) under 80 mW/cm(2) light illumination intensity. (c) 2006 Elsevier Ltd. All rights reserved.