A simple combustion method has been tried for the preparation of nanoparticle-sized LiBiO2 powder with urea as the igniter and glycerol as the binding material. Nitrates of Li+ and Bi3+ were mixed together to form a uniform mixture. Required quantities of urea and glycerol were added to this mixture to form a paste. This paste was carefully heated to 100° C initially and finally heated to 460° C for 5 h. The product obtained was subjected to TG/DTA and XRD analysis. The particle size of the cathode material was roughly calculated from the X-ray data using Scherer equation. However, SEM and EDAX analysis were carried out in detail to confirm the particle size and the composition of LiBiO2 respectively. A 2016 coin type button cell was assembled with LiBiO2 as cathode and graphite as anode containing polypropylene separator and a solution of 1 M LiClO4 dissolved in 1:1 (EC+DEC) mixture as the electrolyte. Charge/discharge studies were conducted to establish viability of the reversible cell