We studied electrochemical characteristics of Langmuir-Blodgett(LB) films by using cyclic voltammetry with a three-electrode system. An Ag/AgCl as a reference electrode, a platinum wire as a counter electrode and LB film-coated indium tin oxide(ITO) as a working electrode were used to study electrochemical characteristics at a various concentration of NaClO4 solution. LB films were reduced from initial potential to -1350 mV, continuously oxidized to l650mV and returned to the initial point. The scan rate was l00mV/s. The monolayer surface morphology of the LB film have been measured by Atomic Force Microscope(AFM). As a result, We comfirmed that the microscopic properties of LB film by AFM showed the good orientation of momolayer molecules and the thickness of monolayer was 3.5-4.lnm. The cyclic voltammograms(CV) of the ITO-coated glass showed the peak potentials for the reduction-oxidation reation. LB films of 4-octyl-4'-(5-carboxypentamethyleneoxy) azobenzene(8A5H) / L-α-phosphayidyl choline, dilauroyl(DLPC) seemed to be irreversible process caused by only the oxidation current from the cyclic voltammogram. The current of oxidatation increased at cyclic voltammogram by increasing 8A5H density in LB films. The diffusivity(D) of LB films increased with increasing of a 8A5H amount and was inversely proportional to the concentration of NaClO4 solution.