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Electromagnetic waves show rapid development in electronics, telecommunications, and the military. One of the efforts to overcome the effects of electromagnetic interference is by developing microwave-absorbing materials. Barium hexaferrite is the best candidate for development as an absorber material. Microwave absorption in barium hexaferrite can be increased through Mg-Al doping and reducing the particle size. This study aimed to analyze sonication parameters to reduce the particle size by combining destruction methods using mechanical alloying followed by high-power ultrasonic irradiation. Barium hexaferrite was synthesized through mechanical alloying by mixing stoichiometric BaCO3, Fe2O3, Al2O3, and MgO (Sigma-Aldrich p.a 99%) (Mg-Al 0.4%wt). The samples continued the sintering process at 1200 °C for 2 h to grow crystal embryos. The optimal parameters for ultrasonic destruction were using a transducer:reactor diameter ratio of 1:10, a particle density of 5 g/250 mL, and adding a non-ionic surfactant of 0.01% at an amplitude of 55% and a sonication time of 8 h. These methods resulted in the saturation magnetization of 18.50 emu/g and a coercivity of 0.08 Tesla. The reduction in the particle size of BHF doped with Mg-Al was successfully up to 21 nm, resulting in a reflection loss of up to −40.8697 dB at 11.896 GHz (x-band, 8–12 GHz). The BHF nanoparticles doped with Mg-Al effectively absorbed up to 99.99% electromagnetic waves.