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each deposition. For a typical reaction, a 35 mm by 45 mm silicon <100> wafer with 30 nm TaN deposited by CVD is mounted to the aluminum stage and secured with two clips. An amount of solid Cu(tmod)2 precursor is loaded into the reactor so that zero order kinetics are attained and conformal deposition is achieved. Typically, precursor loading is approximately between 0.2 – 0.9 wt. %. The vessel is then sealed and placed behind protective polycarbonate housing. Then, using a constant flow of nitrogen, the reaction vessel is purged continuously over a 15 minute period. Simultaneously, the reactor wall is heated to the desired temperature (T = 60 oC) and reaches equilibrium within 10 min. Supercritical carbon dioxide (P = 103 bar, T = 60 oC) is then introduced into the reactor using the computer controlled syringe pump, which enables precise volume measurement of the added CO2. A suitable amount of time is allowed for the complete dissolution of precursor in the convection dominated flow of the supercritical CO2 in the reactor (1 hr.). Next, using a pressure drop, hydrogen is loaded into the reactor via a manifold of known volume (70 mL) and higher pressure. The moles of hydrogen injected are then calculated by pressure drop using the ideal gas law. Typically, hydrogen concentration is approximately 0.5 wt. % which is at least 100 times in excess of what is needed for complete conversion of the precursor. The aluminum stage is quickly heated (~1 min.) to the desired reaction temperature (270 – 285 oC) and maintained at this temperature for a known amount of time. The heated stage is allowed to cool down (~5 min.) while fresh CO2 is used to flush multiple reactor volumes though the system to remove reaction byproducts and unreacted precursor. The effluent is passed through an activated carbon bed and silicone oil bubbler before being vented to the atmosphere. During select reactions, small gas phase samples of known volume are collected using HPLC sample 62PDF Image | Supercritical Fluid Deposition Of Thin Metal Films
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