In this research, the precursors of ZnO/ZnFe2O4 microcubes are synthesized by a facile mixed solution method using Prussian blue (PB) and Zn(AC)2. The precursors were heat-treated at the right temperature to obtain the desired compound. The structure and shape of desired specimens are characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and transmission electron microscopy (TEM) analysis techniques. The electrochemical properties of the samples are researched by battery testing system. The results show that ZnO/ZnFe2O4 samples obtained by solution method have good electrochemical properties. The ZnO/ZnFe2O4 shows a high discharge capacity of 863 mAh g−1 after 100 cycles under a current density of 100 mA g−1. This study shows that ZnO/ZnFe2O4 has the potential as a novel anode material for lithium ion batteries.