Abstract. The synthesis of LiNiO2, an attractive 4 V lithium ion battery cathode material, was investigated in view of identifying optimum preparation conditions by adopting various methods and comparing the structural, physical and electrochemical properties of the products. The conventional high temperature method (solid state annealing at 800 ~ and a novel low temperature method (self propagating high temperature method at 300 ~ allowed to synthesise crystalline LiNiO~ with a composition close to the ideal stoichiometry. Optimisation of the preparation conditions which are responsible for forming high performance LiNiO_~ favoured LiNO3 and Ni(NO3)2 as starting material along with an internal fuel (glycine) and a temperature of 300 ~ for about three hours as most suitable heat treating condition. The electrochemical performance of LiNiOz synthesized via the various methods is reported.