NiFe 2 O 4 nanorods have been successfully synthesized via thermal treatment of the rod-like precursor fabricated by Ni-doped -FeOOH, which was enwrapped by the complex of citric acid and Ni 2+ . The morphology evolution during the calcination of the precursor nanorods was investigated with transmission electron microscopy (TEM), and the phase and the magnetic properties of samples were analyzed through X-ray diffraction (XRD) and vibrating sample magnetometer (VSM). The results indicated that the diameter of the NiFe 2 O 4 nanorods obtained ranged between 30 and 50 nm, and the length ranged between 2 and 3 μm. As the calcination temperature was up to 600°C, the coercivity, saturation magnetization, and remanent magnetization of the samples were 36.1 kAm 1 , 27.2 Am 2 kg 1 , and 5.3 Am 2 kg 1 , respectively. The NiFe 2 O 4 nanorods prepared have higher shape anisotropy and superior magnetic properties than those with irregular shapes.