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Fujisima and Honda were the first to use n-TiO2 for photoelectrochemical decomposition of water upon irradiation with ultraviolet light [1]. An increase in the efficiency of photocatalytic and photoelectrocatalytic oxidation of various substrates on n-TiO2 is associated primarily with an increase in the visible light absorption by photocatalyst (λ = 400–780 nm) for a more complete use of solar radiation, as well as decrease in the rate of recombination of photogenerated electron–hole pairs. A method for the preparation of film coatings of titania, doped with bismuth (Bi3+) and lead (Pb2+) ions, separately and simultaneously, has been developed based on sol–gel synthesis. These films represent a single-phase system of titanium dioxide in anatase modification. The film coatings have been studied as catalysts of photoelectrooxidation of methanol, formic acid, and phenol under visible light illumination. It should be noted that non-doped titania films didn't exhibit activity in this region of spectrum [2]. It has been assumed that photoelectrochemical oxidation of the mentioned model systems with visible light is due to a decrease in the band gap of doped titania to 2.7 eV. References: 1. Fujishima A., Honda K. Nature. 1972, 238, 37. 2.. Grinberg V.A., Emets V.V., Maiorova N.A. et al. Protection of Metals and Physical Chemistry of Surfaces 2018, 54, 1, 51. This work was financially supported by the Program of Fundamental Studies of the Presidium of the Russian Academy of Sciences 1.8 P “Fundamental Aspects of the Chemistry of Carbon Energetics” and partially by the State Task for IPCE RAS, Theme 47.23.