This study investigates a simple and rapid process for directly preparing M-type barium ferrite using high-temperature ball milling. By adjusting the rotation speed of the high-temperature ball milling, the morphology and size of the powder can be altered to regulate its electromagnetic properties, aiming for an overall good absorbing effect. The powder’s morphology, agglomeration properties, elemental valence states, and electromagnetic parameters were characterized using SEM, BET, XPS, EDS, and VNA. The results show that as the milling speed increases, the particle size of the M-type barium ferrite decreases, transitioning from the typical hexagonal flake particles to spherical block particles, forming a porous loose structure with richer dielectric loss mechanisms and enhanced electromagnetic wave loss capacity. Electromagnetic loss performance analysis indicates that at a milling speed of 50 rpm, the powder achieves the best electromagnetic loss of −61.16 dB at a matching thickness of 8.77 mm and a microwave absorption bandwidth of 4.1 GHz.
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