The ability to produce high performance electronic devices by metalorganic chemical vapor deposition (MOCVD) is critically dependent on reagent purity and deposition chemistry. MOCVD based metallization processes are also strongly affected by reagent cost. The ideal aluminum MOCVD reagent would meet the demands of high purity and chemical compatibility required for electronic film growth yet be economically attractive for metallization applications. Alane:trimethylamine (AlH3:N(CH3)3) is a promising aluminum reagent both for MOCVD of aluminum gallium arsenide films and metallization. Widespread adoption of this reagent has been hindered by concerns about purity and cost. Alane:trimethylamine is currently purified by sublimation, a time-consuming process difficult to scale up. In Phase I, alane:trimethylamine will be purified using supercritical fluid (SCF) extraction/recrystallization. A high pressure synthesis of alane:trimethylamine in the same SCF medium used for extraction will also be performed to demonstrate feasibility of combining high pressure synthesis with SCF extraction. In Phase II, production scale methodology will be developed and this novel combination of techniques will be profilerated to a broad range of semiconductor grade reagents. Supercritical fluid technology may provide a means of coupling the synthesis and purification of alane:trimethylamine in one process. This process could supply higher purity, lower cost, alane:trimethylamine for the electronics industry.