A novel electrode material was prepared by electrochemical oxidation of [4,4′-phenylazo-2,2′-(ethylenediimino-κ²N-methyl)diphenolate-κ²O]nickel, a [Ni(ii)(salen)]-type complex, in chlorinated solvent. The chemical structure of the material was explored by FTIR, NMR and XPS techniques to determine the main components of the material and the nature of the linkage between them. The morphology of the material films was explored by SEM analysis. The electrochemical properties of the new material were studied by a set of voltammetric methods and an unusual stability of the material in aqueous medium was observed.