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Nanoscale Li-rich Li1.2Mn0.54Ni0.13Co0.13O2 material is synthesized by a co-precipitation combined freeze drying (CP-FD) method, and compared with a conventional co-precipitation method combined vacuum drying (CP-VD). With the combination of X-ray diffraction (XRD) and scanning electron microscopy (SEM), it is found that the sample from CP-FD method consists of a pure phase with good crystallinity and small, homogenous particles (100-300 nm) with uniform particle size distribution. Inductively coupled plasma spectroscopy (ICP) shows that the sample has a stoichiometric ratio of n(Li): n(Mn): n(Ni): n(Co)=9:4:1:1; and its Brunauer-Emmett-Teller (BET) specific surface area is 5.749 m2 g−1. This sample achieves excellent electrochemical properties: its initial discharge capacities are 298.9 mAh g−1 at 0.1 C (20 mA g−1), 246.1 mAh g−1 at 0.5 C, 215.8 mAh g−1 at 1 C, and 154.2 mAh g−1 at 5 C (5 C charge and 5 C discharge), as well as good cycling performance. In addition, the Li+ chemical diffusion coefficient of Li1.2Mn0.54Ni0.13Co0.13O2 material prepared by the CP-FD method is 4.59×10−11 cm2 s−1, which is higher than that of the Li1.2Mn0.54Ni0.13Co0.13O2 material prepared by CP-VD. This phenomenon illustrates the potential for Li1.2Mn0.54Ni0.13Co0.13O2 with good rate performance synthesized by CP-FD method. [ABSTRACT FROM AUTHOR]