The influence of deposition parameters of LB films on structural, optical, and electrophysical properties of graphene oxide films was studied. It was shown that the film, obtained at low surface pressure, is more uniform in structure, but its optical density is 30% smaller than that for the film obtained at high pressure. When analyzing the area occupied by the LB film on the surface, it was found that all monolayers on a solid substrate occupy about 80% of the total area under study, which agrees well with data of the film transfer coefficient. On the basis of the data obtained from impedanceometry, it is established that for electrodes based on SLGO LB films, the resistance to charge transfer associated with the recombination of an electron into an electrolyte is in many times greater than the value obtained for a platinum electrode, which may be due to the lack of good contact between individual particles of graphene oxide on the FTO surface.