The procedure for the electrodeposition of a mesoporous nickel/cobalt layer from a liquid crystalline plating bath based on the cheap, commercial surfactant, cetyltrimethylammonium bromide and an aqueous solution containing 0.84 M NiCl2 and 0.20 M CoCl2, has been investigated. The phase diagram for these mixtures is reported and it is shown that the H, liquid crystalline phase has a high conductivity. The conditions for deposition have been established using cyclic voltammetry and potential step and deposits are characterised using scanning electron microscopy (SEM), electron diffraction analysis (EDX) and helium ion microscopy (HIM). Uniform thickness deposits with a Ni/Co ratio similar to 4/1 can be prepared and they have a high surface area; in 1 M NaOH Ni/Co alloy layers with a thickness of similar to 2 gm can store similar to 1 C cm(-2) in the Ni(OH)(2)/NiOOH couple. This charge may be cycled >20 times. (C) 2012 Elsevier B.V. All rights reserved.