Electrochemical properties of nano-size Ni-V, Ni-Fe and Mg-Fe multiple metal oxides, prepared from layered double hydroxides as precursors, for the anode electrode of lithium battery has been investigated using cyclic voltammetry, AC-impedance and ex-situ by SEM observation. In the CV curves of N-V multiple metal oxide, it became clear that the reaction voltage of vanadium-nickel oxide system shifted to lower voltage than non-dope NiO. AC-impedance and the morphology observation results that the electrochemical reaction of multiple metal oxides with lithium ion proceeds via the two-step reaction: the surface film formation above 1.0 V and the subsequent conversion reaction below 1.0 V. (C) 2014 Elsevier B.V. All rights reserved.