Research into corrosion resistance of multilayer materials obtained by the method of potentiostatic pulse electrolysis was conducted. The purpose of the work was to select materials for the creation of multilayer steel coatings with high corrosion resistance, as well as to develop technology for their formation. The formation of galvanic coatings was carried out in stationary and potentiostatic pulse electrolysis modes. The study of corrosion resistance was carried out by accelerated methods in solutions simulating the marine environment. Corrosion resistance of samples made of St3 steel coated with nickel and zinc-nickel alloys of different compositions when using various electrolysis modes was studied. It has been experimentally proved that the potentiostatic mode of pulse electrolysis allows the formation of galvanic coatings with a zinc-nickel alloy of various compositions from one electrolyte. Based on the study of electrode potentials of coatings in various media, the composition of the outer and inner layers of a multilayer heterogeneous structure was substantiated. It was experimentally proved that the formation of multilayer coatings on the surface of steel could significantly increase the protective properties of these coatings. It was theoretically justified that the materials of the layers should have different values of electrode potentials, and the inner layer should have a more negative value of the potential than the outer one has.