Polyaniline/zirconium oxide (PANI/ZrO 2) nanocomposites have been synthesized by incorporating ZrO 2 nanoparticles into the PANI matrix via liquid-liquid interfacial polymerization method. The composite formation and structural changes in PANI/ZrO 2 nanocomposites were investigated by powder X-ray diffraction (PXRD), scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR). PXRD pattern of PANI/ZrO 2 nanocomposites exhibited sharp and well-defined peaks of monoclinic phase of ZrO 2 in PANI matrix. SEM images of the composites showed that ZrO 2 nanoparticles were dispersed in the PANI matrix. The FT-IR analysis revealed that there was strong interaction between PANI and ZrO 2. AC conductivity and dielectric properties of the nanocomposites were studied in the frequency range, 50-10 6 Hz. AC conductivity of the nanocomposites obeyed the power law indicating the universal behaviour of disordered media. The nanocomposites showed high dielectric constant in the order of 10 4 , which could be related to dielectric relaxation phenomenon. Further, the materials were checked for their supercapacitance performance by using cyclic voltammetry (CV), chronopotentiometry (CP) and electrochemical impedance spectroscopy (EIS). Among the synthesized nanocomposites, PANI/ZrO 2-25 wt.% showed a higher specific capacitance of 341 F g −1 at 2 m Vs −1 and good cyclic stability with capacitance retention of about 88% even after 500 charge-discharge cycles.