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.