PROCESS FOR THE GENERATION OF METALLIC FILMS

Abstract

The present invention is in the field of processes for the generation of thin inorganic films on substrates, in particular atomic layer deposition processes. It relates to a process for preparing metal films comprising (a) depositing a metal-containing compound from the gaseous state onto a solid substrate and (b) bringing the solid substrate with the deposited metal-containing compound in contact with a reducing agent in the gaseous state, wherein the reducing agent is or at least partially forms at the surface of the solid substrate a carbene, a silylene or a phosphor radical.

Claims

1. A process for preparing a metal film, comprising: (a) depositing a metal-containing compound from the gaseous state onto a solid substrate; and (b) bringing the solid substrate with the deposited metal-containing compound in contact with a reducing agent in the gaseous state or in solution, wherein the reducing agent is or at least partially forms at the surface of the solid substrate a carbene, a silylene or a phosphor radical, wherein the carbene is a compound of formula (I), (II), (IVa), (IVb), (Va) or (Vb): ##STR00014## wherein R is hydrogen, an alkyl, alkenyl, aryl, or silyl group X is C, Si, or P, Y is S, NR, or CR.sub.2, Z is nothing, H, alkyl, halogen, an amine, PR.sub.2 or a boron species, and n is 0, 1 or 2.

2. The process according to claim 1, wherein the reducing agent is a compound of formula (Ia), (Ib), (Ic), (Id), (Ie), or (If): ##STR00015##

3. The process according to claim 1, wherein the reducing agent is a compound of formula (III): ##STR00016##

4. The process according to claim 1, wherein the reducing agent is a compound of formula (IVa) or a compound of formula (IVb): ##STR00017##

5. The process according to claim 1, wherein the reducing agent is a compound of formula (Va) or a compound of formula (Vb): ##STR00018##

6. The process according to claim 1, wherein the reducing agent has a vapor pressure of at least 0.1 mbar at 200 C.

7. The process according to claim 1, wherein (a) and (b) are successively performed at least twice.

8. The process according to claim 1, wherein the metal-containing compound comprises Ti, Ta, Mn, Mo, W, or Al.

9. The process according to claim 1, wherein the temperature does not exceed 350 C.

10. (canceled)

Description

BRIEF DESCRIPTION OF THE FIGURES

[0055] FIGS. 1, 4, and 5 show thermal gravimetry analysis data of the compounds in the examples.

[0056] FIGS. 2, 3, and 6 show differential scanning calorimetry data of the compound in the examples.

EXAMPLES

Example 1

[0057] ##STR00012##

[0058] Sodium (4.1 g, 0.18 mol) was added to a solution of degassed, dry dibutylether (150 ml) under inert conditions. The reaction mixture was heated to 110 C. and chloro-di-isopropylphosphine added slowly (25 g, 0.16 mol). After addition, the mixture was stirred for another 2 h at 110 C. Subsequently, 80 mL degassed, distilled water was added carefully. Phases were separated and organic layer washed with degassed, distilled water. Organic phase was dried over Na.sub.2SO.sub.4, filtered off the drying agent and distilled to yield the pure compound III-1.

[0059] Boiling point: 74-75 C. at 0.75 mbar

[0060] The result of the thermal gravimetry (TG) analysis including the relative mass loss per minute (DTG) is shown in FIG. 1. The fact that less then 1% mass remain at 200 C. indicate that compound III-1 evaporates completely without decomposition. The differential scanning calorimetry (DSC) data depicted in FIG. 2 support this fact, as the first sign of a reaction occurs at 279 C.

Example 2

[0061] ##STR00013##

[0062] Sodium (3.5 g, 0.15 mol) was added to a solution of degassed, dry dibutylether (150 ml) under inert conditions. The reaction mixture was heated to 110 C. and chloro-di-isopropylphosphine added slowly (25 g, 0.14 mol). After addition, the mixture was stirred for another 2 h at 110 C. Subsequently, 80 mL degassed, distilled water was added carefully. Phases were separated and organic layer washed with degassed, distilled water. Organic phase was dried over Na.sub.2SO.sub.4, filtered off the drying agent and distilled to yield the pure compound III-2.

[0063] Boiling point: 117 C. at 0.5 mbar

[0064] In the DSC curve depicted in FIG. 3, a first sign of a reaction occurs at 195 C. indicating that compound III-2 can be evaporated without decomposition.

Example 3

[0065] A TG analysis was performed on compound IV-1. The result is depicted in FIG. 4. A mass loss of 98.5% between 35 C. and 250 C. indicates that compound IV-1 can be evaporated without decomposition.

Example 4

[0066] A TG analysis was performed on compound I-Si-1. The result is depicted in FIG. 5. A mass loss of 98.8% between 25 C. and 200 C. indicates that compound I-Si-1 can be evaporated without decomposition. The vapor pressure of compound I-Si-1 was measured to be 1 mbar at 80 C. FIG. 6 shows the DSC curve with an endothermic peak in the range of 60 C. to 100 C. and an exothermic peak above 260 C. which can be attributed to decomposition.