Electric double layer capacitors (EDLC) using carbon materials electrodes is one of anticipated energy storage device because of its superior characteristics have been employed for the micro electronics, such as memory backup system. However, it is necessary to improve the various properties of EDLC for the future applications such as the energy storage for the small scale distributed energy system and the electric vehicle. The capacitance of electrode materials such as activated carbons in powder or fiber form is depending mainly on the surface area of its carbons, although it was often observed that the higher surface area carbons obtained from the same precursor did not show the larger capacitance per unit weight or surface area. In this study, the exfoliated carbon fibers (ExCFs) synthesized through the rapid heating of the intercalation compounds of carbon fibers were examined as capacitor electrodes. The measurements of EDLC behavior of its ExCFs were performed using standard three-electrode cell with 1mol/dm
3 and 18mol/dm
3 sulfuric acid electrolyte. The capacitance reached 160 and 555F/g in 1mol/dm
3 and 18mol/dm
3 H
2SO
4 electrolyte, respectively, even though ExCFs had relativity small surface area of about 300m
2/g. Its capacitance slightly depends on specific surface area of ExCFs in 1mol/dm
3 H
2SO
4 electrolyte. On the other hands, the capacitance of ExCFs obtained in 18mol/dm
3 H
2SO
4 electrolyte was significantly large. The most provable chemical reaction in 18mol/dm
3 H
2SO
4 to give large capacitance is intercalation of H
2SO
4 molecules into the ExCFs having developed carbon layers stacking. The intercalation reaction of acid molecules is known to possible only with well crystallized carbon materials. All ExCFs were found to be split into a number of thin filaments along the original fiber axis. From its TEM observation, these filaments were recognized to consist of thin sheets. In these sheets, hexagonal carbon layers were found to be oriented along the original fiber axis. This structural feature having well-oriented graphite layers after exfoliation might be important for giving a large capacitance for EDLC. The intercalation of H
2SO
4 molecules into ExCFs in concentrated electrolyte might be responsible for resultant large capacitance of EDLC.
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