A pure NiFe2O4 spinel has been prepared from an Ni-Fe2C+Fe3C+LDHs precursor under mild conditions for use as the anode material in Liion batteries. XRD, elemental analysis and a combination of TG-DTG-DTA and evolved gas mass spectrometry (EGMS) were carried out to characterize the calcined products. The main factors, affecting the electrochemical performance of the materials, were investigated. The material calcined at 700℃ for 3 h performs best with an initial discharge capacity of 1239 mAh g-1 and a reversible capacity of 701 mAh g-1. The major advantage of the LDHs precursor method for the synthesis of NiFe2O4 is that it uses a readily available precursor and affords a spinel with a small particle size and uniform distribution of metal cations, hence, resulting in a good electrochemical performance.