Using NiCl[Formula: see text]O and Y(NO)3 solution as raw material and urea as the precipitating agent, Yttrium-doped NiO hollow spheres (Y-NiOHS) were prepared through homogeneous precipitation method with melamine–formaldehyde polymer microspheres (MF) as templates. The electrochemical performances of Y-NiOHS with difference Y-doped mole ratios (Y:[Formula: see text]%, 0.5%, 1%Y-NiOHS) were characterized by cyclic voltammetry (CV), constant current charge–discharge test (GCD) and AC impedance test (EIS). The results of CV show that 0.5%Y-NiOHS in 5[Formula: see text]mV/s scan rate can achieve the maximum capacity of 320.92[Formula: see text]F/g. The results of GCD show that the capacity of 0.5%Y-NiOHS is 226.2[Formula: see text]F/g at 0.5[Formula: see text]A/g discharge current density and the 1000 charge–discharge cycles after the capacitance retention rate is 85%. The electrochemical performance of 0.5%Y-NiOHS are better than NiOHS and NiO powder.