Two sets of samples of LiCo1-xNixO2(0 less than or equal to x less than or equal to 1) in unquenched and quenched states have been synthesized by microwave dielectric heating. Lattice constants determined from powder XRD are found to vary with the composition. SEM/TEM micrographs of the samples have shown defined facets. The BET surface areas of quenched samples are higher than the unquenched samples. Electrochemical charge-discharge cycling has been done on the samples in order to study their activity as cathode materials for Li-ion secondary battery. The samples show appreciable discharge capacity for several charge-discharge cycles. The discharge capacity of the quenched samples is found to be higher than unquenched samples. (C) 2004 Elsevier Ltd. All rights reserved.