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The BiFe1−xNixO3 (x  =  0, 0.05, 0.1, 0.2, and 0.3) nanoparticles were prepared by a simple solution method. Their nanostructures were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), x-ray absorption spectroscopy (XAS) and gas absorption techniques. The magnetic properties of the nanoparticles were studied by using a vibrating sample magnetometer (VSM). The increasing of Ni content with decreasing of crystallize size can improve magnetization. Moreover, the samples were fabricated as electrodes to study the electrochemical properties by cyclic voltammetry (CV), galvanostatic charge-discharge (GCD) and electrochemical impedance spectroscopy (EIS). The high specific capacitances of the electrodes are in the range of 193–514 F g−1. Although the increasing of the Ni content leads to decreasing of the specific capacitances, the 5% Ni-doped BiFeO3 can improve the capacity retention (82%) after 500 cycles at 10 A g−1.

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