In this paper, a commercial polymeric resin precursor (polystyrene sulphonate beads) was used as a source of carbon spheres. The resin was pyrolyzed at different temperatures (700, 800, and 900 °C) and the resulting carbons were analyzed by cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). From the result of EIS, carbon spheres obtained at 700 °C (CS−700) have the least ohmnic resistance and highest capacitance. In furtherance, the resin was chemically activated with iron (III) chloride FeCl3·6H2O at different concentration (0.1 M, 0.3 M, and 0.5 M) and pyrolyzed at 700 °C to obtain activated carbon sphere namely (ACS 700−0.1, ACS 700−0.3, and ACS 700−0.5) in which the last digit of the samples denotes the concentration of FeCl3. Scanning electron microscope (SEM) showed that the carbon is of spherical shape; X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), and X-ray photon electron spectroscopy (XPS) revealed successful introduction of Fe on the surface of the carbon. Out of all the activated carbon spheres, ACS 700−0.1 exhibited highest double layer capacitance of 9 µF cm−2 and lowest charge transfer resistance of 3.33 KΩ·cm2. This method shows that carbon spheres obtained from a polymeric source can be easily improved by simple resin modification and the carbon could be a potential candidate for an electrical double layer capacitor.

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