So fine cobalt oxide xerogel powders were prepared by using a unique solution chemistry associated with the sol-gel process. The effect of thermal treatment on the crystalinity, particle structure, and corresponding electrochemical properties of the resulting xerogel remained amorphous as $Co(OH)_2$ up to $160^{circ}C$ With an increase in the temperature above $200^{circ}C$, both the surface area and pore volume decreased sharply, because the amorphous $Co(OH)_2$ decomposed to form CoO that was subsequently oxidized to form crystalline Co304. In addition, the changes in the crystallinity, and particle structure all had significant but coupled effects on the electrochemical properties of the xerogels. A maximum capacitance of 192F1g was obtained for an electrode prepared with the $CoO_x$ Xerogel calcined at$150^{circ}C$, which was consistent with the maxima exhibited in both the surface area and pore volume. This capacitance was attributed solely to a surface redox mechanism.