ABSTRACTAl2O3 has been synthesized from aluminum propionate [A1(CO2CH2CH3)3] bySol-Gel techniques. Methods of characterization include: x-ray powder diffraction, scanning electron microscopy (SEM) and nuclear magnetic resonance(NMR). Solution and solid state 13C and 27Al NMR data is coupled with bothx-ray diffraction powder data and SEM in order to understand the transitionfrom sol + gel + amorphous powder + crystalline powder In the sonicated andunsonicated aluminum propionate precursor, and A12O3 powders. Resultsindicate that the sonicated dried powder is crystalline, having the γA12O3structure while the unsonicated dried powder is amorphous and crystallizesat 800°C with the a A12O3 structure. These differences in crystallinity arefurther substantiated by solid state 27AL NMR chemical shifts and linewidths at half height.