A novel soft chemistry route (rheological phase reaction method) was developed to synthesize nanocrystalline NiFe 2 O 4 . The as-prepared samples were characterized by powder X-ray diffractometer (XRD), transmission electron microscope (TEM) and vibrating sample magnetometer (VSM). The effects of the calcination temperature on the particle sizes and magnetic properties of the samples were investigated. The results indicated that the samples obtained by this method had the single-phase spinel. Particle sizes estimated from Scherrer's formula increased with the calcination temperature, which were consistent with the results of TEM. The magnetic properties of the samples were strongly affected by the calcination temperature. The coercivity initially increased and then decreased with increasing calcination temperature whereas the saturation magnetization continuously increased.