A simple polymer pyrolysis method for the synthesis of hierarchically nanostructured NiFe2O4/C composites is reported in this study. The characteristics of the material are examined by thermogravimetry, X-ray diffraction and scanning electron microscopy. The electrochemical performances of the nano-material composites are investigated in detail. The results show that the obtained composite retains a high specific capacity of 780 mAh g(-1) even after 40 cycles at a current density of 1/8C, and the coulombic efficiency approaches 99%. The reversible specific capacity can still be as high as 200 mAh g(-1), at high rate of 4C. The nanostructured NiFe2O4/C composite is a potential competitive anode for lithium-ion batteries. (C) 2013 Elsevier B.V. All rights reserved.