The precursors of ZnMn2O4 were synthesized by different methods (the rheological phase reaction method or the mixed solvothermal method). The precursors were heat-treated at a suitable temperature to obtain the expected product (ZnMn2O4). The synthesized samples were characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The electrochemical properties of the samples were also investigated. The results show that ZnMn2O4 was synthesized successfully. The particles of ZnMn2O4 were irregular quasi-spheres with sizes of about 50 nm. The ZnMn2O4 nanoparticles synthesized through the mixed solvothermal method were clustered together to form microspheres about 1 μm in diameter. The electrochemical testing results showed that the ZnMn2O4 synthesized through the mixed solvothermal method featured higher reversible capacity and better cycling performance than the sample synthesized by the rheological phase reaction method. The ZnMn2O4 synthesized through the mixed solvothermal method could be a promising anode material for lithium ion battery application.