Solid material comprising a thin metal film on its surface and methods for producing the same

• US 6,958,174 B1
• Filed: 03/10/2000
• Issued: 10/25/2005
• Est. Priority Date: 03/15/1999
• Status: Expired due to Term

• Current Assignee: University Technology Corporation
• Original Assignee: The Board of Regents of the University of Colorado (University of Colorado System)
• Inventors: George, Steven M., Klaus, Jason W.
• Primary Examiner(s): Meeks, Timothy
• Assistant Examiner(s): Fuller, Eric B
• Application Number:
  US09/523,491
• Time in Patent Office: 2,055 Days
• Field of Search: 427/250, 427/251, 427/252, 427/253, 427/255.26, 427/255.27
• US Class Current: 427/250
• CPC Class Codes: C23C 16/08 from metal halides
• CPC Class Codes: C23C 16/45525 Atomic layer deposition [ALD]

Abstract

The present invention provides a solid material comprising a solid substrate having a thin metal film and methods for producing the same. The method generally involves using a plurality self-limiting reactions to control the thickness of the metal film.

Claims

1. A method for producing a solid material comprising a thin film of metal on a solid substrate surface, said method comprising:

(a) contacting said solid substrate surface with a metal halide gas, wherein the metal is selected from the group consisting of tungsten, rhenium, molybdenum, antimony, selenium, thallium, chromium, platinum, ruthenium, iridium, and germanium, under conditions including a temperature from 425 to 600 K sufficient to deposit a layer of said metal halide on said solid substrate surface;

(b) thereafter contacting said surface with a reducing agent consisting of a gaseous silylating agent under conditions including a temperature from 425 to 600 K, such that the silylating agent reacts with metal halide species on said solid substrate surface to form silane moieties at the surface of the substrate;

(c) then contacting said surface with additional metal halide gas under conditions including a temperature from 425 to 600 K such that the additional metal halide gas reacts with the silane moieties formed at the surface of the substrate in step (b) to form a metal film layer having metal halide surface species;

and thereafter sequentially repeating steps (b) and (c) one or more additional times, whereby in each cycle of steps (b) and (c), the metal halide and silylating agent react to produce a metal film layer having a thickness substantially corresponding to the atomic spacing of said metal.

2. The method of claim 1, wherein said solid substrate surface comprises a group selected from oxides, nitrates, metals, semiconductors, polymers with a functional group, and mixtures thereof.

3. The method of claim 1, wherein said metal halide is tungsten fluoride.

4. The method of claim 1, wherein the silylating agent comprises silane, disilane, trisilane and mixtures thereof.

5. The method of claim 1, wherein said thin metal film surface comprises metal—

metal halide surface.

6. The method of claim 1 further comprising repeating said steps (b) and (c) to obtain a desired thickness of said metal film.

7. The method of claim 1 further comprising contacting said solid surface with the silylating agent prior to said step (a).

8. The method of claim 7, wherein said solid substrate surface comprises a hydroxide.

9. A method for producing a solid material comprising a thin film of metal on a solid substrate surface, said method comprising:

(a) contacting said solid substrate surface with a metal fluoride gas, wherein the metal is selected from the group consisting of tungsten, rhenium, molybdenum, antimony, selenium, thallium, chromium, platinum, ruthenium, iridium, and germanium, under conditions including a temperature from 425 to 600 K sufficient to deposit a layer of said metal fluoride on said solid substrate surface;

(b) thereafter contacting said surface with a reducing agent consisting of a gaseous silylating agent under conditions including a temperature from 425 to 600 K, such that the silylating agent reacts with metal fluoride species on said solid substrate surface to form silane moieties at the surface of the solid substrate;

(c) then contacting said surface with additional metal fluoride gas under conditions including a temperature from 425 to 600 K such that the additional metal fluoride gas reacts with the silane moieties formed at the surface of the substrate in step (b) to form a metal layer having metal fluoride surface species;

and thereafter sequentially repeating steps (b) and (c) one or more additional times, whereby in each cycle of steps (b) and (c), the metal fluoride and silylating agent react to produce a metal film layer having a thickness substantially corresponding to the atomic spacing of said metal.

10. The method of claim 9, wherein said thin metal film surface comprises metal—

metal halide surface.

11. The method of claim 9 further comprising repeating said steps (b) and (c) to obtain a desired thickness of said metal film.

12. The method of claim 9, wherein said solid substrate surface comprises a group selected from oxides, nitrates, metals, semiconductors, polymers with a functional group, and mixtures thereof.

13. The method of claim 9 further comprising contacting said solid substrate surface with the silylating agent prior to said step (a).

14. The method of claim 13, wherein said solid substrate surface comprises a hydroxide.