Photoelectrochemical (PEC) devices based on Fe-doped and Pt-loaded nanostructured- TiO2 films acting as working electrodes were fabricated for solar hydrogen production. Anatase nanocrystalline titania (nano-TiO2) thin films were deposited on glass slides and Ti metal sheet substrates by a sol-gel dip-coating method. The sol-gel of nano-TiO2 was prepared in nitrogen atmosphere using a home-made nitrogen dry box and titanium tetraisopropoxide Ti[OCH(CH3)2]4 was used as a precursor. The effects of annealing temperatures on the crystallite size and the phase transformation also were investigated. The diameters of the particles in the rage of 12 nm were obtained in different methods of making the sol-gels and different annealing temperatures. Photoelectrochemical (PEC) devices consist of the Fe-doped and Pt-loaded TiO2 films as working electrodes, Pt as counter electrodes, 1.0 M KOH as electrolyte, and Nafion Perfluorinated membrane as a proton exchange membrane. The maximum photocurrent density occurred of 0.80 mA/cm2 without an external applied bias potential under irradiation of 100 mW/cm2 corresponding with photoconversion efficiency of 0.98 %. Impurity and undesired phases may be the cause of electron-hole recombination that results in lowering photocatalytic activity.