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Layered Manganese and aluminum double hydroxides (Mn-Al LDH) were electrochemically synthesized on a Ni, or a Pt substrate by galvanostatic electrochemical reduction of Mn(NO 3 ) 2 and Al(NO 3 ) 3 aqueous solutions mixtures. The obtained XRD data indicated that the interlayer spacing of the Mn-Al LDH was 0.87 nm and was in good agreement with that reported for NO 3 /Mn-Al LDH. The contents of trivalent cation, Al 3+ , in the products were almost identical to those in the corresponding electrolyte solutions. During electrochemical oxidation and reduction of NO 3 /Mn-Al LDH precipitated from a Mn(NO 3 ) 2 and Al(NO 3 ) 3 aqueous solutions 3:1 mixture in a 2 mol dm −3 KOH solution, Al contents in the NO 3 /Mn-Al LDH deviated products decreased by ca. 0.2. Although the dissolution of Al 3+ in the LDHs occurred at the first electrochemical oxidation in a 2 mol dm −3 KOH solution, reversible redox peaks were observed at around −0.2 V vs. Hg/HgO after 2nd cycle of CVs.