Compounds LiNi1/3Co1/3Mn1/3O2 are prepared by adopting different carbonate, i.e., NaHCO3, NH4HCO3 and Na2CO3 under the same conditions, which results in the impressive differences in the morphology properties and electrochemical behaviors of LiNi1/3Co1/3Mn1/3O2. The microscopic structural features of LiNi1/3Co1/3Mn1/3O2 are investigated using X-ray diffraction (XRD) and Scanning Electron Microscopy (SEM). The electrochemical properties of LiNi1/3Co1/3Mn1/3O2 are carried out by charge-discharge cycling tests and the electrochemical reactions during charge-discharge process are also investigated by the cyclic voltammetry (CV). Experimental results show that the microscopic structural features, the morphology properties and electrochemical performances are deeply related to the precipitators. In addition, the cyclic voltammetry indicates that the oxidation of nickel occurs by two steps Ni2+ -> Ni3+ -> Ni4+. (C) 2009 Published by Elsevier B.V.