Lithium-based oxides (LiMOx, where M = Ni, Co, Mn) are attractive for electrode materials, because they are capable of reversibly intercalating lithium ions for rechargeable battery without altering the main unit. We developed a novel solution-based route for the synthesis of these lithium intercalation oxides, using acetates or oxides as precursors for lithium, manganese, nickel, and cobalt, respectively with proper organic solvents. The evolution of crystal structure of these materials was analyzed by X-ray diffraction. Further analysis of LiMn2O4 samples were carried out using impedance spectroscopy and Raman spectroscopy. These studies indicate that this synthetic route, without using expensive alkoxides of sol-gel process. produces high-quality lithium-based oxides useful for cathode in lithium-ion rechargeable battery. (C) 2000 International Association for Hydrogen Energy. Published by Elsevier Science Ltd. hll rights reserved.