The effect of calcination temperature on the structural properties and phase formation of synthesized CaO-Al₂O₃ nanopowder was investigated and discussed. The calcination products were identified by differential thermal analysis (DTA) and the crystalline phase formation was analyzed by X-ray diffraction (XRD). The obtained results showed that the crystallization started at 460 °C. Finally, the microstructures of the nanoparticles were observed by scanning (SEM) and transmission electron (TEM) microscopes. The investigation showed that an increase in the calcination temperature led to the appreciable increase in the crystallite size and the crystallinity of the final product. The obtained data confirmed that the prepared materials were mayenite with different surface area in the range of 71.18 m²/g to 10.34 m²/g after annealing in the temperature range of 470 °C to 960 °C.

Yttrium iron garnet was obtained using four methods of synthesis. A modified citrate method and a modified citrate method with YIG (yttrium iron garnet, Y₃Fe₅O₁₂) nucleation were used. In two subsequent methods, YIP (yttrium iron perovskite, YFeO₃) and α-Fe₂O₃ obtained in the first case by the citrate method and in the second by precipitation of precursors with an ammonia solution were used as the input precursors for reaction sintering. Differential scanning calorimetry (DSC) measurements of the output powders obtained by all methods allowed to identify the effects observed during the temperature increase. Dilatometric measurements allowed to determine the changes in linear dimensions at individual stages of reaction sintering. In the case of materials obtained by the citrate method, two effects occur with the increasing temperature, the first of which corresponds to the reaction of the formation of yttrium iron perovskite (YIP), and the second is responsible for the reaction of the garnet (YIG) formation. However, in the case of heat treatment of the mixture of YIP and α-Fe₂O₃, we observe only the effect responsible for the solid state reaction leading to the formation of yttrium iron garnet. The obtained materials were reaction sintered at temperatures of 1300 and 1400 °C. Only in the case of material obtained from a mixture of perovskite and iron(III) oxide obtained by ammonia precipitation at temperature of 1400 °C were densities achieved higher than 98% of the theoretical density. The use of Hot Isostatic Pressing (HIP) in the case of this material allowed to eliminate the remaining porosity and to obtain full density.