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Nanostructured materials are currently attracting considerable attention due to the possibility of their use in various fields of science and technology, especially in the development of new catalysts, storage devices, photonic crystals and biosensors. Within the framework provided by the work electrochemical synthesis of functional nanomaterials based on transition metal oxides was carried out. As used synthesis method produces nanoparticles in the form of nanospheres, nanorods, nanotubes. Potentiostat Autolab PGSTAT 302N and electron microscope Zeiss LEO EVO-50 XVP were used in the work. The electrochemical oxidation of the metal surface was synthesized at room temperature. The particle size was controlled by parameters such as voltage, current density, and electrolyte properties. Ionic liquid BmimNTf2 (1-butyl-3-methylimidazolium bis (trifluoromethylsulfonyl) imide) was used as electrolyte. The samples used as electrodes were prepared from pure Co (99.99 wt. %), Re (99.95 wt. %) and Ta (99.95 wt. %) by arc-melting with non-consumable tungsten electrode on a water-cooled copper hearth in an argon atmosphere. The obtained samples were annealed in a resistance furnace during 240 h at 13755 K in evacuated silica capsules. In the first case, working and auxiliary electrodes were prepared from cobalt and in the second case these electrodes were prepared from alloy containing 64.8 at. % Co, 9.8 at. % Re and 25.4 at. % Ta representing a Laves phase. The reference electrode used in both cases is the silver electrode. Nanostructure metal oxides of a spherical shape and their clusters, randomly positioned, have been synthesized on the surface of the working electrode at currents 0.1 and 0.05 mA (for the cobalt electrode) and 0.1 mA (for the Laves phase electrode) during 100 s in each cases. These results have been confirmed by cyclic voltammetry and SEM.