For the first time, the preparation and characterization of a novel anode material Li2NiFe2O4 are reported in this work. The preparation of Li2NiFe2O4 is conducted under the air conditions by using a subsection calcination method. The influence of annealing periods on the properties of the resultant materials is thoroughly explored. The characteristics of the materials are mainly examined by X-ray diffraction (XRD), scanning electron microscopy (SEM), cyclic voltammetry (CV), galvanostatic charge-discharge tests and electrochemical impedance spectroscopy (EIS). The results of the XRD patterns effectively demonstrate the formation of crystalline Li2NiFe2O4, and the SEM images indicate that particles with octahedron crystal morphology are prepared and the 9 h-annealed sample has the smallest particle size among all the prepared samples. The results of electrochemical measurements reveal that 9 h-calcined sample delivers a high specific capacity of 203 mAh g(-1), after 20 cycles at a current density of 100 mA g(-1). The successful preparation of Li2NiFe2O4 is believed to be able to trigger the research work concerning the novel group of Li2MFe2O4 materials. (C) 2016 Elsevier B.V. All rights reserved.