Using Ni(NO3)2·6H2O and FeCl3·6H2O mixed hydrothermal method, we synthesized nanometer NiFe2O4 powders, and characterized the samples by X-ray diffraction (XRD) and transmission electron microscopy (TEM). Meanwhile, in order to evaluate the stability of product, we tested the samples for charge and discharge cycle. The experimental results show that the nanometer NiFe2O4 power is spherical quasi\|crystal structure, high degree of crystallinity, crystalline intact and uniform particle size distribution; the 1st,30th,50th,70th specific capacity of the charge and discharge are (997,1 019),(726,750.2),(560.9,578.4),(514.8,528.2)(mA·h)/g, which show that NiFe2O4 has good electrochemical stability.