Molybdenum doped layered Li[Ni1/3+x Co1/3Mn1/3−2x Mo x ]O2 materials were synthesized by an ultrasonic spray pyrolysis method. A single phase of Li[Ni1/3+x Co1/3Mn1/3−2x Mo x ]O2 could be prepared in 0≤ x ≤0.05 region. Structural and electrochemical properties of the Li[Ni1/3+x Co1/3Mn1/3−2x Mo x ]O2 were characterized by X-ray diffraction, Rietveld refinements and galvanostatic charge/discharge tests. The discharge capacity increased with the molybdenum doped, x in 0.01 sample is exhibited a higher discharge capacity of 175mAhg−1 with a good capacity retention.