Monolithic Al2O3 and Al2O3/SiC nanocomposite powders were prepared by sol-gel processing. The process involved the precipitation of Al(NO3)(3)(.)9H(2)O with NH4OH in excess water to form boehmite (AIOOH). XRD indicates that the subsequent thermal reaction proceeds by the phase transformation sequence AIOOH, gamma-, delta-, theta, to alpha-Al2O3. The Al-27 NMR spectra indicate a gradual increase in the proportion of Al in the tetrahedral sites of the gamma-, delta- and theta-Al2O3 formed at increasing calcination temperatures. Complete transformation to octahedral Al (alpha-Al2O3) is marked by the abrupt disappearance of tetrahedral Al. Al-2-O-3/ SiC nanocomposite powders were prepared by adding alpha-SiC powder to the boehmite precursor at the precipitation stage. Upon heating, the Si-29 NMR spectra of the Al2O3/SiC Powders reveal alpha-SiC, Al2O3.xSiO(2) and SiO2 phases. Stable alpha-Al2O3 and alpha-Al2O3/ SiC nanocomposite powders are formed at 1200 and 1300 degrees C, respectively. It appears likely that the presence of SiC modifies the thermal behaviour of the Al2O3 in the nanocomposites by stabilising the Al2O3 phases with concomitant oxidation of SiO2. (c) 2005 Elsevier Ltd. All rights reserved.