This article is concerned with the synthesis of high-quality (Mg, Zn)2Z hexaferrites. A series of the ferrites Ba3(ZnxMg1−x)2Fe24O41 (x = 0.5, 0.7, and 1.0) were prepared by high-energy ball milling and sintering at 1250 • C for 2 h. The structural and magnetic properties of the samples were investigated using X-ray diffraction, scanning electron microscopy, and vibrating sample magnetometer. X-ray diffraction and thermomagnetic studies indicated that the Z-type phase was dominant at x = 0.5, and decreased with the increase of x, whereas the fraction of the Y-type hexaferrite increased. The saturation magnetization and initial permeability, however, increased slightly with the increase of x. The coercivity, on the other hand, was in the range 40-54 Oe for all samples, and the magnetocrystalline anisotropy field did not change significantly with increasing x. The FMR frequency estimated from the static magnetic parameters was ≈ 19 GHz for all samples.