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.
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