The monograph presents a brief overview of literature data on the application of advanced oxidation processes to water/wastewater treatment. A special attention was paid to heterogeneous photocatalysis using TiO2 catalyst under the action of UV light. The structures, physicochemical and photochemical properties of titania as well as the mechanism of photocatalysis on titanium dioxide surface were reviewed. Various methods of immobilisation of TiO2 onto various supporting materials were described. The electrochemical deposition of composites containing TiO2 dispersed particles is a very promising approach in searching perspective supports for TiO2 photocatalysts. Our original experimental findings on electrodeposition of composite Fe/TiO2 coatings from methanesulfonate electrolyte were presented in detail. The electrochemical kinetics and mechanisms of Fe and Fe/TiO2 electrodeposition from methanesulfonate baths were investigated. The synthesized Fe/TiO2 composite coatings manifest a high photocatalytic activity towards the destruction of organic dye as a model pollutant under exposure to UV radiation. A possible mechanism of photocatalytic degradation was proposed.