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.
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