Layered LiNi0.9Co0.1O2 cathode material has been successfully synthesized with a calcination time of 0.5 h by a rheological phase reaction method. The obtained powder was characterized by X-ray diffraction (XRD), particle size and particle size distribution, scanning electronic microscope (SEM) and electrochemical measurements. The powder is confirmed to be alpha-NaFeO2 structure. Cyclic voltammetry (CV) studies imply that the phase transitions from hexagonal to monoclinic exist during charge-discharge cycling. The LiNi0.9CO0.1O2 cathode demonstrated a good electrochemical property with an initial discharge capacity of 193 mAh g(-1) and capacity retention of 88.6% after 15 cycles. (C) 2008 Elsevier B.V. All rights reserved.