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The Li-rich layered cathode material, Li [Ni 0.2 Li 0.2 Mn 0.6 ]O 2 , was synthesized via a ''mixed oxalate'' method, and its structural and electrochemical properties were compared with the same material synthesized by the sol-gel method. X-ray diffraction (XRD) shows that the synthesized powders have a layered O 3 -LiCoO 2 -type structure with the R-3m symmetry. X-ray photoelectron spectroscopy (XPS) indicates that in the above material, Ni and Mn exist in the oxidation states of ?2 and ?4, respectively. The layered material exhibits an excellent electrochemical performance. Its discharge capacity increases gradually from the initial value of 228 mA hg -1 to a stable capacity of over 260 mA hg -1 after the 10th cycle. It delivers a larger capacity of 258 mA hg -1 at the 30th cycle. The dQ/dV curves suggest that the increasing capacity results from the redox-reaction of Mn 4? /Mn 3? .