Abstract: Direct methanol fuel cell (DMFC) research is highly focused due to its high energy density, portability and inexpensive. In the present study conventional platinum catalyst used for methanol oxidation is being replaced with nickel catalyst supported over nickel mesh. The electrode is synthesized by single step electro deposition technique. Synthesized electrode was characterized by SEM, EDAX and AFM techniques to know the surface morphology, composition and thickness of the catalyst respectively. The electro catalytic behavior of the nickel for methanol oxidation was evaluated using cyclic voltammetry technique. As the DMFC is compatible with both the acidic and alkaline electrolytes the working of the nickel mesh electrode is analyzed in both media. The results showed maximum current density of 0.025 and 0.030 A/cm² in alkaline and acidic medium respectively with less potential around 0.4 and 0.2 V. The other parameters such as varying the concentration of methanol, electrolyte medium, scan rate and thickness of the catalytic layer were analyzed and optimized.