This study focuses on synthesis of polyaniline composites and application as electrode material in the fabrication of hybrid supercapacitors. Hybrid supercapacitors were fabricated using aluminum foil as current collector, and conductive Polyaniline (PANI) composites as electrode materials. Cobalt oxide (Co 2 O 3 ), ammonium peroxydisulfate (APS) were used along with PANI in the preparation of electrodes of the supercapacitor. Polyaniline and its various composites were used in the cathode and activated carbon in the anode (positive electrodes) of the asymmetric hybrid supercapacitor. Electrochemical performance of the supercapacitors has been evaluated on the basis of capacitive properties (i.e. capacitance, energy density and power density). Area of the supercapacitor, applied voltage for charging and composition of cathode materials have been optimized in this study. The optimum area of the supercapacitor was found 30 cm 2 at optimum voltage 5 V. The result showed that supercapacitor fabricated using polyaniline (PANI) as cathode material with Al foil as current collector provided highest capacitance of 249 F/g, Energy density of 31 Wh/kg and Power density of 18 W/kg. Among various PANI composites (Ni-PANI, Cu-PANI, CNF-PANI) synthesized in this study, Ni-PANI composite showed highest capacitance of 336 F/g, energy density of 42 Wh/kg, and power density of 31 W/kg. The result indicates that Ni-PANI composite has high potential as cathode materials for the hybrid supercapacitor.