Objectives. Catalytically active materials are required in different chemical engineering processes. This makes the development of new materials with high efficiency and original ways in which to obtain them of significant interest. The present work investigates the synthesis of catalytically active material including electrode materials, as well as their improved efficiency due to the nanodecoration of their surface.Methods. An aluminum folio was nanoperforated (nanoscalloped) by high-voltage anodization in an acidic medium. The effective electrode material was obtained as a metallic nickel replica rather than an oxide layer of the product. To study the surface state of aluminum obtained in this manner, a scanning electron microscope (Hitachi-SU8200) was used. The elementary composition of the aluminum was determined by back-scattered X-ray irradiation.Results. The nickel replica obtained in the above-described process exceeded the catalytic activity estimated by methanol oxidation of the unprocessed nickel 70–150 times.Conclusions. The present paper demonstrates the potential of creating effective catalytically active nanopillar materials using the metallic rather than metal-oxide part of a layer of anodized aluminum as a matrix template.