Photoelectrochemical and electrophysical properties of semiconductor heterostructures based on TiO 2 films with Pd particles distributed thoughout the bulk of the oxide have been investigated. These heterostructures were prepared by pyrolysis of titanium resinate and PdCl 2 mixture followed by reduction thermal treatment. The reduction process in the TiO 2-Pd films takes place not only in the surface layer but in the entire volume as well and TiO 2 films possess a high donor concentration (N d ~ 10 20 − 10 21cm −3). Here, the TiO 2 energy gap determined from quantum yield spectra increases due to the Burstein shift from 3.11 eV for TiO 2 films to 3.21 eV for heterostructures.