Electrochemical performance of Ni-V, Ni-Fe and Mg-Fe oxide nano-sized particles obtained from layered double hydroxide (LDH) precursors were investigated as anode of lithium secondary batteries. These binary metal oxides showed very high reversible charge discharge capacity for conversion reaction with lithium ion and good capacity retention. From the results of ex situ XRD and XANES measurements, it cleared the conversion reaction of the binary metal cation is occurring at the lower voltage range under 1.0 V. Especially for the Ni-V system, the lower hysteresis of voltage and the high capacity of 821 mAh/g in the lower voltage region were obtained owing to four step reduction of vanadium ion under 1.0 V. (C) 2013 Elsevier B.V. All rights reserved.