Direct methanol fuel cell (DMFC) will be an encouraging energy source in the near future. The current study discusses an ultrasonication method of preparation of poly 2,5 - dimethoxy aniline (PDMA) and nickel nanoparticles by simple and facile method. The as prepared electrocatalyst viz., FTO / PDMA - Ni modified electrocatalyst were investigated for its methanol oxidation reaction (MOR) on to the surface of fluorine doped tin oxide (FTO) electrode. The modified electrocatalyst were characterized for its physicochemical characterization by field emission scanning electron microscope equipped with energy-dispersive X-ray spectroscopy techniques, X-ray diffraction, Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy. The Bode and phase diagrams are also provided The electrochemical characterizations were done in 0.5 M KOH and 1 M methanol. The FTO / PDMA - Ni modified electrocatalyst shows an excellent response towards methanol owing to DMFC application. The potential for MOR for electrocatalyst FTO / Ni and FTO / PDMA - Ni modified electrocatalysts were 0.66 V with a current density of 2.03 mA / cm2. The ECSA value for FTO /Ni and FTO / PDMA - Ni modified electrocatalyst was found to be 1.4124 cm2/g and 5.0050 cm2/g respectively. The electrocatalytic activity of PDMA - Ni modified electrocatalyst is due to the synergistic interaction of Ni over the PDMA matrix which favors MOR. Based on the above findings, the FTO / PDMA - Ni modified electrocatalyst can be conveniently used as an anode catalyst for DMFC application.