Oxalate was generally used as a precipitant for synthesis of MnZn ferrites during the co-precipitation process. However, the MnZn ferrite couldn’t be directly obtained and a calcination process was needed. In this research, we reported a direct preparation of the MnZn ferrite nanoparticles by using co-precipitation method, together with refluxing process. XRD measurements proved that crystallite size of the obtained samples increased with an increase in pH value of the co-precipitation solution, and that the crystallite size of about 25 nm was obtained for the sample at a pH of 13. This sample showed the maximum Ms of 58.6 emu/g, which was about one times larger than that of 12 (pH value). Calcination to the obtained samples result in an enlargement in their crystal size and an improvement in their magnetic properties with an increase in temperatures. The samples calcinated in CO2 + H2 atmosphere presented good stability, and the maximum Ms value of 188.2 emu/g was obtained for the 1100。C-heated sample. Unfortunately, precipitation of some Fe2O3 at 800。C suggested poor stability of the nanocrystalline MnZn ferrite in N2 atmosphere.