Ni1/3Co1/3Mn1/3(OH)2, a precursor of LiNi1/3Co1/3Mn1/3O2 in new-generation Li-ion batteries, was prepared by a hydroxide coprecipitation method. Scanning electronic microscopy (SEM) micrographs reveal that the precursor particles thus obtained, show regular shape with uniform size under optimized conditions. X-ray diffraction (XRD) indicates that well-ordered layer-structured LiNi1/3Co1/3Mn1/3O2 was prepared after calcination at high temperature. The final product exhibited a spherical morphology with uniform size distribution (10 μm in diameter). At the terminal charging voltage of 4.3 and 4.5 V (vs. Li/Li+), the testing cells of LiNi1/3Co1/3Mn1/3O2 delivered a specific capacity of 161.2 and 184.1 mAh g-1, respectively. The high capacity retention of 98.0 and 96.1 % after charging to 4.3 and 4.5 V for 50 cycles, respectively, indicates that this material displays excellent cycling stability even at high cut-off voltage.