This investigation is focused on the synthesis of magnetite (Fe3O4) and metallic copper mixed films. This magnetic/metal system is considered a model for fouling layers that are formed by corrosion products on steam generators of nuclear reactors. Additionally, such films are relevant to electronic and catalytic applications. The method described in this study was based on the electrodeposition of mixed magnetite-copper films on Inconel substrates by the reduction of soluble ferric/cupric complexes with triethanolamine. The possibility of electrodeposition of a copper film from an alkaline Cu(II)-triethanolamine solution was also studied. The effect of the solution composition and surface roughness of the Inconel samples was investigated. The electrodeposited mixed copper-magnetite films were determined to be non-congruent with an enrichment of metallic copper.