We report the synthesis and characterization of nanostructured semiconductors such as CdS, CuInSe 2 (CIS) and TiO 2 for photovoltaic cells and photoelectrochemical cells for hydrogen production. The CdS was prepared by chemical deposition, CuInSe 2 by electrodeposition and chemical method and TiO 2 by sol-gel method. All the three semiconductors were prepared in the thin film and powder form. The CdS was synthesized as wide band gap n-type material in the nanostructured form. The p-CdS was prepared also in the nanostructured form with Cu doping. P-type CuInSe 2 films and powders were synthesized in the nanostructured form. TiO 2 was always formed in the nanostructured and n-type form. The films and powders were characterized by x-ray diffraction, atomic force microscopy, and opto-electronic methods. All the semiconductors were formed in the nanostructured form with different band gaps depending on the particle size and post-deposition treatments.