We succeeded in preparing a layered Li-Ni-Ti oxide that contained divalent nickel and tetravalent titanium with a Ni2+/Ti4+ ratio of close to 1. This layered compound was synthesized by the ion exchange of Na-type precursor. The X-ray diffraction pattern of this compound was indexed in space group R (3) over barm. As a positive electrode material, the obtained sample had first charge and discharge capacities of 120 and 66 mAh g(-1), respectively, in voltages of 2.0-4.3 V. (C) 2004 The Electrochemical Society.