MgAl2O4 is a stable catalyst support with potential for replacing gamma-alumina in several applications. However, synthesis of magnesium spinel requires elevated temperatures to avoid phase separation (in MgO and Al2O3) at low temperatures, leading to coarsening and reduction of active surface area. In this work, nano CaO-doped and undoped magnesium aluminate were successfully prepared by Ultrasonic Spray Pyrolysis (USP), using a simple adapted experimental set-up operating at 1100 °C. During the process, the particles stay at high temperatures for a short period of time, allowing phase stability and limited coarsening. The influence of calcium oxide on the particles morphology and structure was investigated via X-ray diffraction, N2 adsorption, X-ray fluorescence, scanning electron microscopy and transmission electron microscopy. The spinel nanopowders were obtained as spherical porous agglomerates of ~1 µm. The resulting powder showed low crystallite sizes in the 5–10 nm range and high specific surface area from 110.0 to 76.6 m2 g−1.
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