The principle of double template deposition technique was developed to prepare NiCo and NiCu alloy nanomaterials. Ordered particles of about 800 nm high were obtained by reduction of ions from aqueous solution into the pores of anodic aluminum oxide (AAO) membrane with intact barrier layer. The size of the nanoparticles was significantly reduced by combination of AAO and the hexagonal phase of a lyotropic liquid crystal. The scanning tunneling microscopy (STM) micrograph of the material prepared in the presence of liquid crystal reveals the hexagonal array of cylindrical pores. The corrosion potential of the alloy nanofilm shifted to more negative values when the sizes of the particles decrease. The anodic linear sweep voltammetry shows, in each case, various current peaks characteristic of the dissolution of chemical elements in the film.