The traditional solid-state method was employed in this study to prepare Mn-Zn ferrite. By adjusting the sintering temperature and the MoO
3 doping ratio, the evolution of its structural and magnetic properties was systematically investigated. Fe
2O
3, MnO, and ZnO were used as the main raw materials, with MoO
3 serving as an additive. MoO
3 was doped at molar ratios ranging from 0 to 1000 ppm under experimental conditions involving a sintering temperature between 1125 °C and 1165 °C and an oxygen concentration of 1.5%. The addition of an appropriate amount of MoO
3 led to an increase in the Q value, which consequently resulted in a reduction in the loss. The formation of a single-phase spinel structure was confirmed by X-ray diffraction analysis. Observations of the surface morphology revealed that the grain size also increased with the increase in MoO
3 content, a trend consistent with the enhanced grain growth kinetics at higher MoO
3 levels. In this study, a Mn-Zn ferrite material with excellent comprehensive performance was successfully prepared under the optimal conditions of a sintering temperature of 1150 °C and a MoO
3 doping concentration of 500 ppm. A Q value of 22.3 was obtained for this material at 25 °C, while a Q value of 15.7 was obtained at 100 °C. At room temperature, a Q value of 192.4 was measured at a test frequency of 500 kHz, and a Q value of 137.2 was measured at 1 MHz. At a frequency of 500 kHz, a loss of 27.1 kW/m
3 was observed at 25 °C, and a loss of 53.6 kW/m
3 was observed at 100 °C. At a frequency of 1 MHz, a loss of 88.2 kW/m
3 was recorded at 25 °C, while a loss of 183.7 kW/m
3 was recorded at 100 °C. Additionally, the lattice constant was stabilized in the range of 8.52–8.53 Å, indicating favorable structural stability.
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