In situ electropolymerization as a facile synthetic procedure has been used to obtain highly sensitive composites of multi-walled carbon nanotubes(MWCNT) and poly tyramine (PT). Nickel was accumulated by complex formation between Ni (II) in solution and amines sites in the polymer backbone to obtain Ni-MWCNT-PT/G (graphite) electrode. Surface morphology of composite was characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS). The reflectance and transmittance amplitudes were obtained, using the continuity of the tangential components of electrical and magnetic fields at interfaces and solving the algebraic matrix equation. Furthermore, the experimental absorbance spectra of nanocomposite were compared with the results from the Maxwell-Garnett theory (MGT) and the value of energy, E-g = 3.75 eV, of composite obtained. The electrochemical performance of Ni-MWCNT-PT/G composite electrodes were investigated by common electrochemical techniques. Compared with Ni-PT/G, a Ni-MWCNT-PT/G electrode shows a higher catalytic performance in the electrocatalytic oxidation of methanol. (C) 2015 Elsevier Ltd. All rights reserved.