Fine nickel ferrite precursors NiFe2（C204）3·6H2O were obtained via co-precipitation method with low grade nickel matte as the raw material. Thermodynamic analysis of NiClz-FeC12-（NH4）2C204-H20 system for precipitation identified that the theoretical optimum co-precipitation pH value is 2, and C2O2 has strong complexation with Ni2＋ and Fe2＋ ions. Based on these theoretical considerations, the effects of parameters on the precipitation rates and precursors size were investigated systematically. The results show that the optimum co-precipitation conditions are pH=2, temperature 45 ℃, 1.2 times theoretical amount of （NH4）2C204 dosage and 3% PEG400 addition. Under these conditions, the precipitation rates of Ni2＋ and Fe2＋ are both over 99.8%, with the precursors size of 1-2 urn. Furthermore, X-ray diffraction （XRD） and thermogravimetry-differential thermal analysis （TG-DTA） demonstrate that the precursors are single-phase solid solution, wherein the nickel/iron atoms are replaced by the iron/nickel atoms reciprocally.
