Electrochemical studies were carried out on Ni 0.4 Co 2.6 O 4 powders prepared by sol-gel via propionic acid method using cyclic and steady state voltammetries. The oxide surface was characterized by scanning electron microscopy (SEM), X-ray diffraction, UV-vis-NIR and FTIR spectroscopies. The results showed that the formation of homogeneous oxide with a single spinel phase occurred at 350°C. The surface redox couple NiOOH/Ni(OH) 2 is confined on the surface material l.