Uniform hexagonal-shaped cobalt oxide (Co3O4) nanodisks were prepared in large scale via facile aqueous solution based hydrothermal process at 110°C. The detailed structural characterizations confirmed that the synthesized products are hexagonal cobalt oxide nanodisks, possessing very well-crystalline cubic spinel structure. A coin cell of type −2032 was assembled using the synthesized Co3O4 nanodisks and its charge–discharge profile was analyzed between the voltages 0.01 and to 2.5V vs. Li/Li+ reference electrode. The electrochemical cell composed of Li/Co3O4 delivered an initial lithium insertion capacity of 2039mAh/g. Although the cell exhibited high irreversible capacity during the first four cycles, the columbic efficiency has been improved upon cycling.