Abstract: In this paper, Ni/Ni(OH)₂/PANI electrode materials were synthesized on Cu foil substrates by the electrodeposition method. The Ni/Ni(OH)₂ nanolayer was firstly prepared on the Cu foil surface by the electrodeposition method, then the PANI layer was deposited on the Ni/Ni(OH)₂ surface via the electrochemical polymerization method. The morphology, structure and electrochemical properties of Ni/Ni(OH)₂/PANI were investigated by SEM, TEM, FT-IR, XPS, CV, GCD and EIS. The results showed that the Ni/Ni(OH)₂/PANI electrode materials had a high specific capacitance and excellent cycle performance. The Ni/Ni(OH)₂/PANI electrode materials had an outstanding specific capacitance of 1 400 F/g at 1 A/g, excellent rate capability with a capacitance retention rate of 62.7% from 1 to 10 A/g and good cycling stability with a capacitance retention rate of 76% after 2 000 cycles. PANI layer deposited on Ni/Ni(OH)₂ surface could reduce the charge transfer impedance of the electrode surface and protect the electrode, thus improving the electrochemical cycle performance of the electrode.