Electrochemical sensors need high efficient electro-catalyst to facilitate the redox reactions and to effectively convert their information to the strong measurable electrical signal. Nickel (Ni) is a non-precious metal with outstanding electro-catalytic activity. The aim of this project was the establishment of the most efficient procedure for the electro-deposition of Ni film on the glassy carbon electrode (GCE). Galvanostatic, potentiostatic and cyclic voltammetric techniques were employed for Ni electro-deposition. The cyclic voltammetry was known as the most effective technique for which the effective variables on the electro-deposition of Ni were optimized. The electrochemical properties of the Ni/GCEs were evaluated by cyclic voltammetry and electrochemical impedance spectroscopy methods. In addition, electro-catalytic ability of the constructed Ni/GCEs toward electro-oxidation of ethanol were studied. Obtained results revealed that activation step of the Ni/GCE in KOH solution effectively improved its electro-catalytic and stability properties. Furthermore, the optimized conditions led to high stability and sensitivity of the prepared modified GCE toward electro-oxidation of ethanol. The results of this study indicated that the engineering of the nickel oxide thin film deposited on the electrode surface could be a cost effective approach to attainment of low prices meanwhile high efficient electro-catalyst usable for ethanol electro-oxidation process.