The adduct of Al(NO3)3·6CO(NH2)2 has been prepared and characterized by means of chemical analysis, IR spectroscopy, X-ray patterns and microscopy. A thermoanalytical study of Al(NO3)3·6CO(NH2)2 as well as urea, for comparison purposes, under conventional dynamic and quasi-isothermal—quasi-isobaric conditions in air has been carried out. It has been found that the adduct is thermally stable up to about 200°C, i.e. up to higher temperature than the decomposition temperature of the constituent compounds. The thermal decomposition mechanism of the adduct is complex, thus infrared spectroscopy and X-ray diffraction techniques have been used to determine the intermediate products. Aluminium oxide(III) is the final decomposition product.