Usually, glassy carbon electrode (GC) is used as it is as a substrate for electrochemically deposited nickel or nickel oxide (NiO x ) nanoparticles. In the present study, GC carbon is anodically oxidized in different media prior to electrode position of NiO x and the impacts of this pretreatment on the structural and electrochemical characteristics of NiO x are studied. Upon anodic pretreatment of GC electrode in acid (0.1 M H 2 SO 4 , GC OX-AC ) and in alkali (0.1 M NaOH, GC OX-AL ), the structural and electrochemical characterizations of nickel oxide (NiO x ) nanoparticles are highly modified. Cyclic voltammetry (CV), scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDX) are used for characterization of the electrodes. While NiOx nanoparticles deposited on GC OX-AC reveal a bird-like shape, it shows semi-spherical shape when it is deposited on either GC or GC OX-AL , with smaller size on the GC OX-AL . The reversibility of the Ni(OH) 2