Process for the generation of metal-containing films

Abstract

A process including bringing a solid substrate in contact with a compound of general formula (I), (II), (III), or (IV) in the gaseous state ##STR00001##
where A is NR.sub.2 or OR with R being an alkyl group, an alkenyl group, an aryl group, or a silyl group,
E is NR or O,
n is 0, 1 or 2, m is 0, 1 or 2, and
R′ is hydrogen, an alkyl group, an alkenyl group, an aryl group, or a silyl group.

Claims

1. A process for preparing inorganic metal-containing films comprising bringing a solid substrate in contact with a compound of general formula (I), (II), (III), or (IV) in the gaseous state ##STR00053## wherein A is NR.sub.2 or OR with R being an alkyl group, an alkenyl group, an aryl group, or a silyl group, E is NR or O, n is 0, 1 or 2, m is 0, 1 or 2, and R′ is hydrogen, an alkyl group, an alkenyl group, an aryl group, or a silyl group.

2. The process according to claim 1, wherein R is methyl, ethyl, tert-butyl, trimethylsilyl or two R form together a five membered ring and R′ is hydrogen.

3. The process according to claim 1, wherein if E is NR or A is OR, R in NR or OR bears no hydrogen atom in the 1-position.

4. The process according to claim 1, wherein a metal-containing compound is deposited from the gaseous state onto the solid substrate before bringing it in contact with a compound of general formula (I), (II), (III), or (IV).

5. The process according to claim 4, wherein the metal-containing compound contains Ti, Ta, Mn, Mo, W, Al, Co, Ga, Ge, Sb, or Te.

6. The process according to claim 4, wherein the metal-containing compound is a metal halide.

7. The process according to claim 1, wherein the compound of general formula (I), (II), (III), or (IV) adsorbs to a surface of the solid substrate and the adsorbed compound of general formula (I), (II), (III), or (IV) is decomposed.

8. The process according to claim 4, wherein the sequence containing bringing a solid substrate in contact with a compound of general formula (I), (II), (III), or (IV) and depositing a metal-containing compound is performed at least twice.

9. The process according to claim 1, wherein the compound of general formula (I) has a molecular weight of not more than 600 g/mol.

10. The process according to claim 1, wherein the compound of general formula (I) has a vapor pressure at least 1 mbar at a temperature of 200° C.

11. A compound of general formula (I), (II), (III), or (IV) ##STR00054## wherein A is NR.sub.2 or OR with R being an alkyl group, an alkenyl group, an aryl group, or a silyl group, E is NR or O, n is 0, 1 or 2, m is 0, 1 or 2, and R′ is hydrogen, an alkyl group, an alkenyl group, an aryl group, or a silyl group wherein at least one E or A contains oxygen or n is 2 or m is 2.

12. The compound according to claim 11, wherein the compound is a compound of general formula (Ib), (Ic), (Ih), or (Ij) ##STR00055##

13. The compound according to claim 10, wherein R′ is hydrogen and R is methyl, ethyl, tert-butyl or trimethylsilyl, or two R form together a five-membered ring.

Description

EXAMPLES

Example 1a: Synthesis of [2-(dimethylamino)ethyl](2-methoxyethyl)amine

(1) A mixture of 2-chloroethyl methyl ether (6.092 g, 0.063 mol), N,N-dimethylethylenediamine (19.382 g, 0.213 mol), and water (5 mL) was refluxed for 18 h in a 250 mL round bottomed flask. Hexane (15 mL) and water (10 mL) were added to the resultant solution at ambient temperature. The flask contents were transferred to a separatory funnel. The aqueous fraction was washed with hexane (14×15 mL) and the combined organic fractions were dried over anhydrous MgSO.sub.4. The solvent was evaporated under reduced pressure to yield an intense yellow oil (5.513 g, 59.8% yield).

(2) .sup.1H NMR (400 MHz, C.sub.6D.sub.6, δ in ppm): 2.04 (s, 6H), 2.29 (t, 2H), 2.60 (t, 2H), 2.71 (t, 2H), 3.09 (s, 3H), 3.32 (t, 2H). .sup.1H NMR (400 MHz, C.sub.6D.sub.6, δ in ppm):

(3) .sup.13C NMR (100 MHz, C.sub.6D.sub.6, δ in ppm): 45.91, 48.34, 50.35, 58.81, 60.08, 73.15.

Example 1 b: Synthesis of AlH.SUB.2.[CH.SUB.3.OCH.SUB.2.CH.SUB.2.NCH.SUB.2.CH.SUB.2.NMe.SUB.2.] (Ib-1)

(4) ##STR00051##

(5) A solution of AlCl.sub.3 (0.788 g, 5.9 mmol) in 30 mL of diethyl ether was cannulated into a stirred solution of LiAlH.sub.4 (0.708 g, 17.7 mmol) in 30 mL of diethyl ether at 0° C. in an ice bath. The resultant cloudy solution was warmed to room temperature, stirred for 40 min and re-cooled to −30° C. Then, a solution of [2-(dimethylamino)ethyl](2-methoxyethyl)amine (3.458 g, 23.6 mmol) in 45 mL of diethyl ether was added dropwise. The resultant mixture was stirred at ambient temperature for 18 h and was then filtered through a 2-cm plug of Celite on a coarse glass frit. The diethyl ether was evaporated from the filtrate under reduced pressure to collect the intense yellow colored, oily product (2.745 g, 66.7% yield). The crude product was purified by distillation at 74° C. under reduced pressure affording a colorless oil (1.645 g, 40% yield).

(6) .sup.1H NMR (400 MHz, C.sub.6D.sub.6, δ in ppm): 2.12 (s, 6H), 2.33 (t, 2H), 2.90 (t, 2H), 3.03 (t, 3H), 3.20 (s, 3H), 3.37 (t, 2H).

(7) .sup.13C NMR (100 MHz, C.sub.6D.sub.6, δ in ppm): 45.51, 47.85, 49.29, 57.91, 60.73, 74.19. IR: v.sub.AlH/cm.sup.−1 1764.

Example 2: Synthesis of H.SUB.2.Al[N(CH.SUB.2.CH.SUB.2.CH.SUB.2.NMe.SUB.2.).SUB.2.] (Ih-1)

(8) ##STR00052##

(9) A solution of AlCl.sub.3 (0.690 g, 5.2 mmol) in 40 mL of diethyl ether was cannulated into a stirred solution of LiAlH.sub.4 (0.621 g, 15.5 mmol) in 40 mL of diethyl ether at 0° C. in an ice bath. The resulting cloudy solution was warmed to room temperature, stirred for 40 min, and then cooled to −30° C. At this point, a solution of 3,3′-iminobis(N,N-dimethyl-propylamine) (4.003 g, 20.7 mmol) in 55 mL of diethyl ether was added dropwise. The resultant mixture stirred at ambient temperature for 18 h and was then filtered through a 2-cm pad of Celite on a coarse glass frit. The diethyl ether was evaporated from the filtrate under reduced pressure to obtain a colorless, oily product (4.003 g, 91% yield). A portion of resultant product (2.043 g) was distilled at 65° C. under reduced pressure to afford a colorless oil (1.604 g, 79% yield).

(10) .sup.1H NMR (400 MHz, C.sub.6D.sub.6, δ in ppm): 1.51 (p, 4H), 2.17 (s, 12H), 2.36 (t, 4H), 3.25 (t, 4H).

(11) .sup.13C NMR (100 MHz, C.sub.6D.sub.6, δ in ppm): 28.61, 46.76, 57.77, 60.69. IR: v.sub.AlH/cm.sup.−1 1691.