Synthesis and thermal decomposition of magnesium aluminum spinel powder precursor composed of ammonium aluminum carbonate hydroxide and Mg-Al-CO₃ layered double hydroxide (hydrotalcite) was studied. The precursor was prepared by co-precipitation technique using ammonium bicarbonate as the precipitant. The morphology of precursor and calcined nanometric spinel powders were observed by SEM and TEM. To enable accurate monitoring of the decomposition process, the thermal evolution of structure, nature and stability of the resulting phases several in-situ techniques (DTA and TG coupled with MS of evolved gases, FTIR and HT-XRD) were used. Based on the results obtained a model describing spinel formation in this system has been proposed.

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