The TiO2/CdS semiconductor composites were prepared on indium tin oxide (ITO) substrates in di®erent mass proportions via wet-chemical techniques using bi-distilled water, acetyl-acetone, poly-propylene-glycol and Triton X-100 as additives. The composite layers were annealed in normal conditions at the temperature of 450±C, 120 min. with a rate of temperature increasing of 5±C/min. The structural and optical properties of all the TiO2/CdS ayers were characterized by X-ray di®raction, UV-VIS spectroscopy, spectrofluorimetry and FT/IR microscopy. The microstructural properties of the deposited TiO2/CdS layers can be modi¯ed by varying the mass proportions of TiO2:CdS. The good crystallinity level and the high optical adsorption of the TiO2/CdS layers make them attractive for photoelectrochemical cell applications.