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In this work, the synergism between the nano nickel particles and its carbon xerogel support, CX, together with their graphite substrate, G, leads to an efficient Nickel/CX/G electrode for electrocatalysis of ethanol oxidation reaction, EOR. The preparation conditions are optimized. The optimum electrode is made of 6 % weight of Ni doped in CX matrix and drop‐casted on a graphite surface, Ni‐6/CX/G. The catalyst structure and morphology are investigated using XRD, SEM, TEM and FTIR techniques. The electrochemical activity towards EOR is tested in 1 M NaOH+1 M Ethanol solutions by cyclic voltammetry combined with a rotating ring disk electrode. The optimum electrode shows an oxidation peak current density value of 5925  normalA.gnormalNnormali-1 ${{\rm A}.{{\rm g}}_{{\rm N}{\rm i}}^{-1}}$ and considerable stability. This electrode may serve as a good candidate for the anode in the Direct Alkaline Ethanol Fuel Cell, DAEFC.

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