Nanocrystalline spinel NiFe2O4 was synthesized by a novel low temperature route. The crystal structure, composition and morphology of the as-prepared powder were characterized by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, X-ray photoelectron spectroscopy (XPS) and transmission electron microscopy (TEM). The average diameter of the particles prepared at 700 degrees C is about 30 nm. The electrochemical reaction mechanism and charge-discharge mechanism of the nanocrystalline NiFe2O4 were proposed based on thermogravimetric analysis (TGA) and cyclic voltammogram study. The charge-discharge tests indicated that the sample calcined at 700 degrees C shows the highest initial discharge capacity (1400 mAh g(-1)) attributed to the nanometer size and the better crystallinity of the powder. A discharge capacity stabilizes at about 600 mAh g(-1) after 10 cycles. The columbic efficiency is improved. The synthesis method is relatively low cost and convenient for large-scale production. Crown Copyright (C) 2013 Published by Elsevier Ltd. All rights reserved.