A b s t r a c t P o l y a n i l i n e / N i C o 2 O 4 nan oco mpos ites (PANI/NiCo 2 O 4 ) with different amounts of NiCo 2 O 4 (5, 8, 10, 15, and 20 wt%) were prepared via in situ chemical oxidation polymerization in the presence of the NiCo 2 O 4 particles, while the NiCo 2 O 4 nanoparticles were synthesized by a modified sol-gel method. The structure and morphology of PANI/NiCo 2 O 4 nanocomposites were characterized by Fourier transform infrared (FT-IR), X-ray diffraction (XRD), and scanning electron microscopy (SEM) techniques, respectively. The electrochemical properties of PANI/NiCo 2 O 4 nanocomposites were investigated by cyclic voltammetry, galvanostatic charge-discharge test, and electrochemical impedance spectroscopy (EIS) in 0.5 mol L −1 H 2 SO 4 electrolyte in three-electrode system. The PANI/10 wt% NiCo 2 O 4 nanocomposites show larger specific capacitance of 439.4 F g −1 at a current density of 5 mA cm −2 and lower resistance compared with the pure PANI. The charge-discharge tests showed that the PANI/NiCo 2 O 4 nanocomposites possessed good cycling stability. It maintained about 66.11 % of the initial capacitance after 1000 cycles at a current density of 5 mA cm −2 . The results indicated that the PANI/NiCo 2 O 4 nanocomposites are a promising material for supercapacitors.