NiFe2O4 of 30 nm average size was synthesized by microwave combustion and subsequent solid state reaction at 1273 K. The materials were characterized by X-ray diffraction, TEM, vibrating sample magnetometery and Mossbauer spectroscopy. The microwave combustion produced materials were comprised chemically of ferrites and a smaller amount of hematite. The NiFe2O4 particles have the cubic spinet structure with crystallites of sizes less than 10 nm, and were found to have low magnetization, and essentially no hysteresis loop; characteristics of superparamagnetism. Upon annealing at temperatures 973 K and below, crystallite growth was accompanied by increase in both coercive held and magnetization. The coercive held was a maximum for the sample annealed at 973 K. On the other hand, crystallite growth at higher annealing temperatures yielded mainly ferrites and improvement in soft magnetic properties. Mtissbauer and magnetization measurements indicate that the fine NiFe2O4 particles produced at the annealing temperature of 1273 K are in good chemical and magnetic order, excluding the spins arrangement at the surface of the particles which show spin glass-like behavior. (C) 2014 Elsevier B.V. All rights reserved