The oxidation treatment of several carbon materials with a sodium chlorate and 70 wt.% of nitric acid, combined with heat treatment, were attempted to achieve an electrochemical active material with a larger capacitance. Among pitch, needle coke, calcinated needle coke and natural graphite, the structure of needle coke and calacinated needle coke were changed to the graphite oxide structure with the expansion of the inter-layer. On the other hand, the calcinated needle coke after oxidation and heating at $200^{circ}C$ has exhibited largest capacitance per weight and volume of 29.5 F/g and 24.5 F/ml at the two-electrode system in the potential range of 0 to 2.5 V. The electrochemical performance of the calcinated needle coke was discussed with the phenomenon of the electric field activation and the formation of new pores between the expanded inter-layer at first charge.