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Research results: The change of technological parameters (concentration of electrolyte solution, current density, electrolysis temperature) of the process of joint electrochemical oxidation of two metals using alternating current makes it possible to obtain dispersed materials including nanoscale phases, the ratio of which can vary over a wide range. Phase transformations of AC electrolysis products occur at lower temperatures than the temperatures during heat treatment of materials obtained by traditional stationary methods. It is grows from non-equilibrium conditions at AC electrolysis that results in the formation of nanodispersed materials with a significant internal energy reserve. Porous structure of the electrolysis products is deteriorated at calcination due to recrystallization and sintering. At the same time, the specific surface area of electrolysis products after high-temperature treatment is 6–10 times higher than the specific surface area of precipitation products. High thermal stability results from the formation of mesoporous structure in the process of electrode polarity change during electrochemical oxidation using alternating current, as well as the release of gaseous products of electrolysis.
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