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4.2.1.1.3 Procedure Both hot and cold wall reactors are used to experiment with different precursor systems and pressure and temperature ranges. For a typical reaction in the cold wall reactor, a 25 mm by 19 mm silicon <100> wafer with 30 nm TaN layer on top, is mounted to the aluminum heated stage and secured with clips. A known amount of precursor is loaded into the vessel. Reaction conditions are listed in Table 4.1. The vessel is sealed and placed behind protective polycarbonate housing. Then, using a constant flow of nitrogen, the reaction vessel is purged continuously over a 30 minute period. The reactor wall and stage are then heated to the desired preheating temperature and allowed to equilibrate (t = 60 min.). Carbon dioxide is introduced into the reactor using a computer-controlled syringe pump (Teledyne Isco, Inc., Lincoln, NE), which enables precise volume measurement of the added CO2. The reactor sits at this condition for a set time (t = 60 min.) to allow for dissolution of the precursor into the CO2. Next, hydrogen is loaded into the system using a manifold of known volume (70 mL). The aluminum stage is then quickly heated (~ 15 s.) to the desired reaction temperature and maintained for a set time. The heated stage is then allowed to cool down (~ 15 s.) while fresh CO2 is used to flush multiple reactor volumes through the system to remove reaction byproducts and unreacted precursor. The effluent is passed through an activated carbon bed and silicon oil bubbler before being vented to the atmosphere. For a typical reaction in the hot wall reactor, a thin (0.001”) 3.25” by 3.25” polyamide (Kapton) film is used to line the inside of the reactor. A 25 mm by 19 mm silicon <100> wafer with 30 nm TaN layer on top, is then placed into the long tubular 82PDF Image | Supercritical Fluid Deposition Of Thin Metal Films
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