Joint electrochemical oxidation of copper and aluminum using alternating current (AC) was performed. The electrolysis products were dried on air (method carbonate) and at the residual pressure of 3-5 kPa (oxide method). Cu-Al layered double hydroxide (Cu-Al/LDH) is formed at air carbonization. Oxide method saves copper (I) oxide. Heat treatment causes the decomposition of LDH to CuO and Al2O3 as well as Cu2O oxidation to CuO. CuO/Al2O3 has a number of catalytic applications. Copper-aluminum spinel (CuAl2O4) is the product of solid-phase interaction of copper and aluminum oxides. IR-spectra revealed that oxide method provides the boehmite dehydration and metal oxides interaction at lower temperature despite the fact that the poorly crystallized copper (II) oxide is formed at LDH decomposition.