In this paper, we successfully synthesized NiFe2O4 nanofibers via simple electrospinning process followed by calcination process. Only peaks of NiFe2O4 could be observed from X-ray diffractometry patterns, indicating the formation of pure compound. Scanning electron microscope and transmission electron microscopy images showed the as-spun NiFe2O4 nanofibers calcined at 800 A degrees C ranged from 130 to 220 nm in diameter. The electrochemical properties of the nanofibers anode material for lithium-ion batteries were tested. It was found that the obtained NiFe2O4 nanofibers calcined at 800 A degrees C possessed higher reversible capacity and cycling stability than that of the samples calcined at 600 A degrees C. The as-prepared NiFe2O4 nanofibers calcined at 800 A degrees C exhibited a high initial discharge capacity of 1,304 mAh g(-1) in the potential range of 3.0-0.01 V, and the stabilized capacity was as high as 514 mAh g(-1) after 60 cycles. Moreover, the as-prepared NiFe2O4 nanofibers calcined at 800 A degrees C also exhibited high capacity at higher charge/discharge rate.