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Herein, the crystal structure, surface morphology, and magnetic and thermal properties of the BaFe11.9In0.1O19‐substituted M‐type hexaferrite are investigated. This solid solution is fabricated using “two‐step” topotactic reactions. It is determined through the X‐ray diffraction method that the crystal structure of this solid solution under normal conditions has hexagonal symmetry with P63/mmc space group (No. 194) with the unit cell parameters a = 5.8992(1) Å and c = 23.2275(7) Å. It is determined by the scanning electron microscope (SEM) researches that the average size of the grains is true d ¯  = 6 μm. It is determined by the vibration magnetometry that the ferrimagnet–paramagnet phase transition happens at around T C = 420 °C. Using differential scanning calorimetry (DSC), it is found that air and water molecules leave the sample surface up to 420 °C and the resulting oxygen anions appearing as a result of a solvothermal reaction fill the oxygen vacancies in the crystal structure at high temperatures up to 800 °C. The thermal transitions repeated in the high temperatures are established. The oxidation behavior of this compound is determined from thermogravimetric analysis (TGA) in a wide temperature range.

The compound BaFe[Formula: see text]In[Formula: see text]O[Formula: see text] was synthesized in the solid phase and its chemical composition and structural properties were studied. SEM analysis showed that the size of crystallites in the resulting polycrystal is [Formula: see text][Formula: see text][Formula: see text]m. When analyzing the microcomposition of the surface, 55.8% of Fe, 19.7% of O, 14.3% of Ba, and 10.0% of In atoms were determined. XRD analysis showed that the crystal structure of this compound corresponds to hexagonal (P63mmc) symmetry. The crystallographic parameters of the compound were determined by the Rietveld method.