PROCESS FOR THE GENERATION OF METAL- OR SEMIMETAL-CONTAINING FILMS

Abstract

The present invention is in the field of processes for preparing inorganic metal- or semimetal-containing films. The process for preparing inorganic metal- or semimetal-containing films comprising (a) depositing a metal- or semimetal-containing compound from the gaseous state onto a solid substrate and (b) bringing the solid substrate with the deposited metal- or semimetal-containing compound in contact with a compound of general formula (I) or (II) wherein Z is NR.sub.2, PR.sub.2, OR, SR, CR.sub.2, SiR.sub.2, X is H, R′ or NR′.sub.2, wherein at least one X is H, n is 1 or 2, and R and R′ is an alkyl group, an alkenyl group, an aryl group, or a silyl group.

##STR00001##

Claims

1.-10. (canceled)

11. A process for preparing inorganic metal- or semimetal-containing films comprising (a) depositing a metal- or semimetal-containing compound from the gaseous state onto a solid substrate and (b) bringing the solid substrate with the deposited metal- or semimetal-containing compound in contact with a compound of general formula (I) or (II) ##STR00005## wherein Z is NR.sub.2, PR.sub.2, OR, SR, CR.sub.2, SiR.sub.2, X is H, R′ or NR′.sub.2, wherein at least one X is H, n is 1 or 2, and R and R′ is an alkyl group, an alkenyl group, an aryl group, or a silyl group.

12. The process according to claim 11, wherein R is methyl, ethyl, iso-propyl, sec-butyl, tert-butyl, trimethylsilyl.

13. The process according to claim 11, wherein at least one X for each Al atom is H.

14. The process according to a claim 11, wherein Z is NR.sub.2, PR.sub.2, OR, or SR.

15. The process according to a claim 11, wherein the metal- or semimetal-containing compound contains Ti, Ta, Mn, Mo, W, Ge, Ga, As, In, Sb, Te, Al or Si.

16. The process according to claim 11, wherein the metal- or semimetal-containing compound is a metal or semimetal halide.

17. The process according to claim 11, wherein the sequence containing (a) and (b) is performed at least twice.

18. The process according to claim 11, wherein the compound of general formula (I) or (II) has a molecular weight of not more than 600 g/mol.

19. The process according to claim 11, wherein the compound of general formula (I) or (II) has a vapor pressure at least 1 mbar at a temperature of 200° C.

20. Use of a compound of general formula (I) or (II) as reducing agent in a vapor deposition process.

Description

EXAMPLES

Example 1

[0056] An atomic layer deposition process was carried out using GeBr.sub.4 as a semimetal-containing compound and compound IIa-1. Each of these compounds was contained in a stainless-steel cylinder and connected to a crossflow ALD reactor with a 1 inch diameter deposition area and an Ar (5N) carrier gas flow of 5 sccm. The base pressure was approximately 50 Pa. The GeBr.sub.4 was heated to 55° C. and compound IIa-1 was heated to 75° C. 100 ALD cycles, each comprising a sequence of a 100 ms GeBr.sub.4 exposure, first 7.9 s purge, 100 ms compound IIa-1 exposure and second 7.9 s purge, were run and monitored by an in situ quartz crystal microbalance (QCM). At reactor temperatures of 160° C. to 200° C., the average QCM frequency change was observed to be −1 Hz/cycle, indicating a steady mass increase and the existence of an ALD window of temperature-independent growth rate. The GeBr.sub.4 exposure resulted in a mass increase, whereas the mass was decreased by the subsequent exposure with compound IIa-1, indicating a specific reactivity of compound IIa-1 with the surface generated by GeBr.sub.4 exposure, but no deposition of compound IIa-1.

Example 2

[0057] The same apparatus, compounds and ALD cycle as in example 1 were used. Blanket Si wafer substrates with either the native oxide or a 100 nm thermal oxide surface were placed in the reactor and were held at a temperature of 160° C. 1000 ALD cycles as described in example 1 were performed and the substrates were analyzed after removal from the reactor. A layer of approximately 14 nm thickness, as determined by ellipsometry, was deposited on the native oxide wafer substrate. The rms roughness of a similar ALD layer deposited on a thermal oxide substrate was found to be 2 nm according to AFM analysis.

Example 3

[0058] The same apparatus as in example 1 was used. GeCl.sub.4 as a semimetal-containing compound and compound IIa-1 were used. GeCl.sub.4 was contained in a stainless-steel cylinder and kept at 0° C. during the ALD process. 100 ALD cycles, each comprising a sequence of a 20 ms GeCl.sub.4 exposure, a 7.98 s purge, a 100 ms compound IIa-1 exposure and a 7.9 s purge, were run and monitored by an in situ quartz crystal microbalance (QCM). At a reactor temperature of 140° C. the average QCM frequency change was −0.4 Hz/cycle, indicating a steady mass increase. The GeCl.sub.4 exposure resulted in a mass increase, whereas the mass was decreased by the subsequent exposure with compound IIa-1, indicating a specific reactivity of compound IIa-1 with the surface generated by GeCl.sub.4 exposure, but no deposition of compound IIa-1.