NixZn1−xFe2O4 (x=0, 0.25, 0.5, 0.75, 1) compounds were prepared by a hydrothermal method and subsequent heat treatment. The physical characteristics of the samples were investigated by field-emission SEM, XRD, X-ray photoelectron spectroscopy, and TEM. The electrochemical properties of NixZn1−xFe2O4 (x=0, 0.25, 0.5, 0.75, 1) as anode materials were tested for lithium-ion batteries. The lithium-storage properties of the electrodes were assessed by cyclic voltammetry and galvanostatic cycling. Among the five samples, Ni0.25Zn0.75Fe2O4 shows good electrochemical performance with a discharge capacity of 1488 mAh g−1 in the initial cycle and 856 mAh g−1 after 100 cycles.