The invention discloses a preparation method of ultra-fine grain high-temperature-resistant high-frequency manganese zinc ferrite, which mainly comprises the following steps: taking Fe2O3, MnO2 and ZnO as main raw materials, taking SnO2 as an auxiliary raw material, proportioning, carrying out primary ball milling, pre-sintering, doping CaCO3, V2O5, TiO2 and Co2O3, carrying out secondary ball milling, adding PVA, granulating, pre-pressurizing and forming at room temperature, deforming at high temperature, pressurizing and forming at high temperature, sintering, and quenching and cooling to obtain the manganese zinc ferrite. According to the invention, SnO2 is used as an auxiliary raw material, and Sn can enter the crystal lattice of the manganese zinc ferrite, so that transition of electrons at high temperature and high frequency is hindered, and loss is reduced; CaCO3, V2O5, TiO2 and Co2O3 are adopted for doping, impurity elements are enriched in a grain boundary, the grain boundary resistivity is increased, and loss is reduced; high-temperature compression deformation is adopted, deformation storage energy is provided, crystal grain forming positions are increased, then crystal grains are refined, and loss is reduced; and by adopting quenching cooling, element diffusion in the cooling process is reduced, and the high-temperature characteristic of the ferrite is enhanced. The obtained manganese zinc ferrite has the advantages of ultra-fine grains, high saturation flux density, high temperature resistance and low high-frequency loss.