In this paper, we successfully synthesized NiFe 2 O 4 nanofibers via simple electrospinning process followed by calcination process. Only peaks of NiFe 2 O 4 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 NiFe 2 O 4 nanofibers calcined at 800 °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 NiFe 2 O 4 nanofibers calcined at 800 °C possessed higher reversible capacity and cycling stability than that of the samples calcined at 600 °C. The as-prepared NiFe 2 O 4 nanofibers calcined at 800 °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 NiFe 2 O 4 nanofibers calcined at 800 °C also exhibited high capacity at higher charge/discharge rate.