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4.2.3.1.3.1 Precursor Synthesis Reaction conditions are listed in Table 4.4. In an N2 glove box, a known mass Baip is added to a known volume of EtOH. Ttip is then added drop wise to the solution. Solution should be clear, if precipitate is seen, Baip may have degraded due to presence of oxygen. The beaker is sealed and stirred for 2 to 3 hours. 4.2.3.1.3.2 Film Deposition For a typical reaction, a 2” <100> silicon wafer is mounted to the stainless steel heated stage and secured with clips. 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 precursor solution that finished mixing is now collected into a large syringe. The precursor solution is injected into the reactor. A known volume of H2O is injected into the reactor and nitrogen is used to quickly purge the inlet and outlet of the reactor. The valves through which the precursor solution and H2O were injected are now sealed. The system is heated to 150 oC and maintained for 30 min (to induce film formation and to improve stoichiometry). The system is heated to 250 oC and maintained for 30 min (EtOH decomposes via dehydration). Ideally, the system would be heated to 380 oC and maintained for 30 minutes to allow crystallization. However, due to reactor limitations, the system is heated to 290 oC and maintained for 30 minutes. The system is cooled overnight and opened the next day. The deposited films are characterized with XPS (Ba99, 100, Sr100 and Ti22, 25, 101-104) in order to obtain their purity and composition. 107PDF Image | Supercritical Fluid Deposition Of Thin Metal Films
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