Nickel/epoxy composites have been fabricated by dispersing nickel powder in a polymeric matrix of epoxy resin. Nickel hydroxide, Ni(OH) 2 , was deposited on such nickel/epoxy surfaces by means of successive voltammetric cycles and galvanostatic reduction. Likewise, the same hydroxide was grown on polycrystalline nickel surfaces. The responses of such electrochemical systems was studied in KOH (aq) at several concentrations as well as in saturated Ca(OH) 2(aq) . Ni(OH) 2 grown on nickel/epoxy surfaces exhibited different potentiodynamic i-E profile and cathodic charges, which are largely affected by nickel/epoxy ratio, potential sweep rate and solution pH. The oxygen evolution on these types of electrodes is consistent with α-Ni(OH) 2 structure obtained by means of the voltammetric method.