CNFs had been well addressed due to numerous promising applications in science and technology. Besides the same physicochemical properties of ordinary carbon materials such as active carbons and carbon black, they exhibit specific, e.g., tubular or fibrous structures, a large surface area, high electrical conductivity stability, as well as extremely high mechanical strengh and modulus, which make them a superior material for electrochemical capacitors. In this study, CNFs were pretreated by mechanical milling with different time in mortar and pestle. The milled CNFs were used as active material of electrode whose electrochemical property was tested to find physicochemical characterization variation. CNF electrode milled for 5 min has the highest electric capacitance. XPS spectrum were employed to explore changes in functional group induced from mechanical milling. Crystal size was calculated to analyze change of peak from different milling time by XRD. The CNF milled for 5 min has the largest crystal size and the highest electric capacitance.