Fe 3O 4 nano-crystal with high purity and even particle size was prepared by combining microemulsion and hydrothermal method. This method can conquer the disadvantages of poor-purity in the W/O microemulsion method and uncontrollable-particle-size in the hydrothermal method. In a degree, the particle size of Fe 3O 4 nano-crystal could be controlled through tuning the ratio between H 2O and the surfactant in the microemulsion.