We prepared nanocrystalline CoFe2O4 by changing its ignition temperatures, using moderate and intense low-oxygen dilution (MILD) combustion technique. The effect of ignition temperature on the particle size and its magnetic behavior was investigated by HR-TEM and VSM respectively. We observed a vast change in the structural behavior and the magnetic properties of the prepared samples. X-ray diffraction studies revealed that the resultant samples had single phase with different grain sizes from 23±5 nm to 16±5 nm, which was understood by observing the growth of the grains through heat released from the combustion reaction. FE-SEM analysis showed high porosity with heterogeneous distribution of the pore size based on the adiabatic temperature and EPMA analysis, which confirmed the elemental compositions of the prepared samples. The saturation magnetization values measured at room temperature, employing vibrating sample magnetometer (VSM) decreased gradually from 50 to 34 emu/g when the ignition temperature was increased from 243 °C to 400 °C. Some of Fe ions on the B sites moved periodically to the A sites because of quenching treatment. The presence of Fe2+ ions in the existing ferrite structure ruled the magnetic behavior of the sample, as confirmed by the Mössbauer analysis. © 2016 Elsevier B.V.