Chemically and structurally uniform Mn‐Zn ferrites have been produced using powders synthesized by the spray decomposition of mixed, aqueous Mn, Fe, and Zn nitrate solutions. The particle size of the as‐formed powder depended strongly on the metal ion concentration in solution; higher concentrations produced larger sizes. The as‐formed particles are spherical, internally hollow, and consisted mostly of Fe2O3. A 900 °C, 6‐h argon treatment removed the internal void space and converted the particles mostly to the ferrite spinel phase. Sintering of compacts from heat‐treated powders produced microstructures superior to those from as‐formed powders. Uniform, fine‐grained materials, with a densification level comparable to that of commercial sintered ferrite, have been produced at the very low sintering temperature of 1100 °C. Preliminary work indicates that a higher initial permeability is obtained when a higher sintering temperature was used and the level of its disaccommodation depended on the oxygen partial pressure present during sintering. Both ‘‘accommodation’’ and disaccommodation were observed in the permeability; their magnitudes depended on the peak value of the applied excitation field.