Nanometer aluminum powders have been prepared from the catalytic thermal decomposition of aluminum hydride adducts in organic solvents. This process provides excellent control of particle size and uniformity with batch particle sizes ranging from 50 to 600 nm. Variables affecting particle size were explored, including reaction temperature, catalyst concentration, and adducting amine concentration. Passivation techniques of the reactive aluminum powders were established for safe handling in air. Samples were mainly characterized by scanning electron microscopy and thermogravimetric analysis.