Anodic aluminium oxide and the hexagonal phase of lyotropic liquid crystals containing zinc and nickel ions were used to prepare Zn-Ni alloy nanorods. Highly ordered alloy nanoparticles were obtained by direct electrochemical reduction of zinc and nickel ions from an aqueous solution into the pores of the alumina membrane. The combination of the hexagonal phase of a liquid crystal and the alumina membrane (double template deposition) leads to the reduction of size of the nanorods. Particles that grow from the bottom of the pore of alumina membrane have many subdivisions due to the columns of the liquid crystals. Potentiodynamic stripping of the film confirmed the presence of the alloy phases. Electrochemical impedance spectroscopy analysis reveals the existence of two-separated time constants and the diffusion of lithium ions in the pores of the nanostructured film. (c) 2007 Elsevier B.V. All rights reserved.