Using sonochemistry to provide the thermal energy and mixing, we demonstrate the ability to synthesize air-stable aluminum nanoparticles of two different size distributions from the titanium-catalyzed thermal decomposition of alane. Characterization data indicate the presence of spherical face-centered-cubic aluminum nanoparticles with average sizes of either 5 or 30 nm that are capped with an organic shell. The average size of the nanoparticles correlates with the concentration of the passivation agent oleic acid, where a higher concentration results in smaller particles. Thermal analysis data demonstrates that at elevated temperatures (>550 °C), these particles react via a typical aluminum oxidation mechanism, whereas at low temperatures (<550 °C), the behavior of these particles is unique and directly related to the presence of the organic shell.