The NiMoO4 samples were synthesized by rheological phase-hydrothermal method. The efforts of different annealed temperatures on the morphologies and electrochemical properties of the final products were systematically investigated. The NiMoO4 samples exhibit the best electrochemical properties with a high reversible capability (640 mAh g−1 at current density of 50 mA g−1) and cycling stability, compared with the other samples. These results indicate that the NiMoO4 samples could be promising electrode materials for lithium ion batteries.