NiFe2O4 is an important high frequency soft magnetic material due to its ultra high resistivity; however, its initial permeability is rather low. Conventional magnetic ferrites are manufactured through ceramic processing. In an effort to explore innovative approaches for fabricating ferrite materials with improved performance, a study of fabricating nanostructured NiFe2O4 using wet chemical approaches has been carried out. The synthetic NiFe2O4 precursor was synthesized by a citrate reaction method followed by calcinating at various temperatures. Systematic studies concerning the crystallographic structure, the nanostructure and morphology of the particle, the phase homogeneity, the conditions for chemical reaction completion, and the magnetic properties have been carried out using x-ray diffraction, transmission electron microscopy, and magnetic measurements. The results show that by using a citrate reaction approach, pure phase and stoichiometric NiFe2O4 can be fabricated easily, and the particle size can be controlled on a nanometer scale, even at high calcination temperatures. In addition, a comparative study of the NiFe2O4 fabricated by conventional ceramic processing and this new citrate processing will be presented.