Nickel oxide species, palladium metal and complex Ni–Pd particles were deposited on the glassy carbon electrode by pulsed electrochemical conditions from 0.5MNaOH solution containing 5mM gluconate ion, 0.5mMNi(NO3)2 and/or 2mMPd(NO3)2. The electrodeposition process was performed using the following potentials and pulse durations: E 1 =−1.0V and E 2 =+0.8V vs. SCE, t 1 =50ms and t 2 =50ms for the relevant times of 600s. The nickel oxide particles were deposited during the anodic pulse of potentials, while the palladium particles were deposited during the cathodic sequence of the potential pulses. The Ni–Pd system shows an acceptable character of electrochemical reversibility and a high affinity for oxygen adsorption. The XPS and SEM techniques were used in order to define the surface chemical composition and the actual morphology of the deposited material. An average surface chemical composition of Pd0.5Ni was established and the composite appears formed of well dispersed single globular particles having an average size comprised between 50nm and 150nm of diameter.