Micro-nanostructured nickel has been prepared as anode materials for Li ion batteries. via a theological phase reaction method. Ni2C2O4 center dot xH(2)O (x = 2 or 2.5) as precursors are obtained from the solid-liquid theological mixture of (NH4)(2)C2O4 center dot H2O and Ni(NO3)(2). The nickel powders are prepared by thermal decomposition of the precursors. The structural, morphological and electrochemical performance are investigated by means of thermogravimetry (TG), differential scanning calorimetry (DSC), powder Xray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscope ITEM) and typical electrochemical tests. The micro-nanostructured nickel displays an initial discharge capacity of 457 mAh g(-1). It also has a remarkable cycling stability with an average capacity fade of 0.17% per cycle from 13th to 50th cycle in 0.01-3.00V versus Li at a constant current density of 100 mA g(-1). (C) 2009 Elsevier Ltd. All rights reserved.