A new class of LiNi1-xCaxO2 (x = 0.0, 0.1, 0.2, 0.3 and 0.5) layered oxide materials has been synthesized by a simple low temperature solid-state route with mixed nitrates/urea with glycerol as the starting materials. First we have taken TG/DTA for observing the phase transformations of LiNi0.9Ca0.1O2. The structure of the synthesized oxides was analyzed using X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) to identify the crystal structure and cation environment, respectively. The synthesized ceramic oxide battery materials were examined by using transmission electron microscope (TEM), scanning electron microscope (SEM) analysis to determine the particle size, nature and morphological structure. SEM with energy dispersive X-ray spectroscopic analysis (EDAX) analysis was carried out to explore the composition of the prepared materials. The electrochemical performance of LiNi1-xCaxO2 electrodes was analyzed using cyclic voltammetry (CV) and galvanostatic charge-discharge cycling studies in the voltage range 3.0-4.5 V. Electrode made with cathode active material, acetylene black and poly(vinylidene difluoride) yield a discharge capacity of 178.1 mAh g(-1) (x = 0.2) with good specific capacity over several charge-discharge cycles. These results have been also supported by cyclic voltammograms. (c) 2006 Elsevier Ltd. All rights reserved.