Novel group V and group VI transition metal precursors for thin film deposition
A precursor and selected technology, applied in the direction of metallocene, metal material coating technology, chemical instruments and methods, etc., can solve the problems of high temperature and complexity at the end of decomposition
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Embodiment 1
[0150] Trichloro(tert-amylimino)vanadium(V)
[0151] Dissolve 4.4g of tert-amylamine (50mmol) in 60mL of anhydrous hexane, and use activated Molecular sieves were dried overnight. The next day, the tert-amylamine solution was added dropwise to 13.1 g VOCl at -78 °C over the course of 1 hr 3 In solution (76 mmol) in 90 mL of anhydrous hexane. After this time, the reaction was slowly warmed to room temperature and stirred overnight. After 24h, the stirring was stopped, and the reaction suspension was allowed to settle for 1 hour, and then in N 2 Filter the solution. The filtrate was dried in vacuo to give 2.3 g of a dark orange liquid. This was further dried under vacuum to yield 1.9 g of solid (crude yield 10%).
[0152] The crude product was further purified by sublimation under vacuum (20 mtorr). First pump the sublimator under vacuum for several hours at room temperature to remove any residual VOCl 3 . Place a liquid nitrogen trap between the sublimator and the Sch...
Embodiment 2
[0157] tert-Amylimino-tris(dimethylamino)vanadium(V)
[0158] In a 100 mL Schlenk flask, trichloro(tert-amylimino)vanadium(V) (1.27 g, 5.287 mmol) was dissolved in 50 mL of anhydrous hexane. Add 812 mg LiNMe slowly over 10 minutes 2 (15.92 mmol, Sigma Aldrich), no significant exotherm was observed. The flask was removed from the glove box and connected to a Schlenk line. After stirring for 24 hours, a dark brown solution formed with a light brown precipitate. After filtering off the solids, the dark brown solution was pumped under vacuum to give 1.4 g of a dark brown oil.
[0159] The crude product was distilled at 80° C. under 0.1 Torr vacuum to obtain 1.0 g of orange liquid as the final product (71% overall yield). 1 H NMR (400MHz, D8 toluene) δ=3.41(s, 18H), 1.59(q, 2H), d=1.33(s, 6H), δ=1.12(t, 3H), shown in Figure 5 middle. 51V NMR (400MHz) δ=-251.76, shown in Figure 6 middle. Also through such as Figure 7 Thermogravimetric analysis (TGA) as shown and as Fig...
Embodiment 3
[0161] Trichloro(sec-butylimino)vanadium(V)
[0162] 7.3 g of sec-butylamine (0.1 mol) was dried in 100 mL of anhydrous hexane for 48 h using molecular sieves. In the glove box, add 26 g of VOCl to a 500 mL Schlenk flask 3 (0.15mol) and 200mL of anhydrous hexane. Transport the flask to a fume hood and connect to a Schlenk line. The flask was cooled to -78°C. The sec-butylamine hexane solution was added slowly over the course of 1 h. The solution darkened immediately. The solution was cooled under dry ice for an additional 1 hour, then the solution was allowed to warm slowly to room temperature. The mauve reaction mixture was stirred overnight at room temperature. After overnight, the mixture separated into two phases. Allow the mixture to settle for half an hour, and use a cannula under N 2 Next, transfer the supernatant to a separate 500 mL Schlenk flask. The precipitate was washed with an additional 50 mL of anhydrous hexane, then transferred.
[0163] will be imme...
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