Aerosol chemical vapor deposition of metal oxide films

• US 5,278,138 A
• Filed: 10/11/1991
• Issued: 01/11/1994
• Est. Priority Date: 04/16/1990
• Status: Expired due to Fees

• Current Assignee: The United States of America As Represented By The Secretary of Agriculture
• Original Assignee: The United States of America As Represented By The Secretary of Agriculture
• Inventors: Kodas, Toivo T., Ott, Kevin C.
• Primary Examiner(s): KING, ROY V
• Application Number:
  US07/774,748
• Time in Patent Office: 823 Days
• Field of Search: 505/1, 505/734, 505/737, 505/742, 427/62, 427/63, 427/314, 427/126.3, 427/255.3, 427/255.2, 427/255.1
• US Class Current: 505/446
• CPC Class Codes: C23C 16/408 of copper or solid solutions thereof
• CPC Class Codes: C23C 16/4486 by producing an aerosol and subsequent evaporation of the droplets or particles
• CPC Class Codes: H10N 60/0436 by chemical vapour deposition [CVD]
• CPC Class Codes: Y10S 427/101 Liquid Source Chemical Depostion, i.e. LSCVD or Aerosol Chemical Vapor Deposition, i.e. ACVD
• CPC Class Codes: Y10S 505/734 From organometallic precursors, e.g. acetylacetonates
• CPC Class Codes: Y10S 505/737 From inorganic salt precursors, e.g. nitrates
• CPC Class Codes: Y10S 505/742 Annealing

Abstract

A process of preparing a film of a multicomponent metal oxide including: forming an aerosol from a solution comprised of a suitable solvent and at least two precursor compounds capable of volatilizing at temperatures lower than the decomposition temperature of said precursor compounds; passing said aerosol in combination with a suitable oxygen-containing carrier gas into a heated zone, said heated zone having a temperature sufficient to evaporate the solvent and volatilize said precursor compounds; and passing said volatilized precursor compounds against the surface of a substrate, said substrate having a sufficient temperature to decompose said volatilized precursor compounds whereby metal atoms contained within said volatilized precursor compounds are deposited as a metal oxide film upon the substrate is disclosed. In addition, a coated article comprising a multicomponent metal oxide film conforming to the surface of a substrate selected from the group consisting of silicon, magnesium oxide, yttrium-stabilized zirconium oxide, sapphire, or lanthanum gallate, said multicomponent metal oxide film characterized as having a substantially uniform thickness upon said

FIELD OF THE INVENTION

The present invention relates to the field of film coating deposition techniques, and more particularly to the deposition of multicomponent metal oxide films by aerosol chemical vapor deposition. This invention is the result of a contract with the Department of Energy (Contract No. W-7405-ENG-36).

Claims

1. A process of preparing a conformal film of a multicomponent metal oxide comprising the steps of:

(a) forming an aerosol from a solution comprised of an organic solvent and at least two precursor compounds capable of volatilizing temperatures of said precursor compounds;

(b) passing said aerosol in combination with an oxygen-containing carrier gas into a heated zone, said heated zone having a temperature sufficient to evaporate the organic solvent and volatilize said precursor compounds, said temperature is insufficient to decompose said precursor compounds; and

(c) passing said volatilized precursor compounds in contact with a surface of a heated substrate, said substrate heated at temperatures greater than the temperature of the heated zone whereat said precursor compounds are volatilized and sufficient to decompose said volatilized precursor compounds whereby metal atoms contained within said volatilized precursor compounds are deposited as said multicomponent metal oxide film upon said surface of said substrate.

2. The process of claim 1 wherein the substrate is selected from the group consisting of silicon, magnesium oxide, yttrium-stabilized zirconium oxide, sapphire, lanthanum aluminate and lanthanum gallate.

3. The process of claim 1 wherein said solvent is selected from the group consisting of alcohols, ketones and aromatics, and said precursor compounds are a mixture of barium, yttrium and copper compounds having volatilities at temperatures lower than their respective decomposition temperatures.

4. The process of claim 3 wherein the molar ratios of the barium:

copper;

yttrium compounds in the solution are in the range of about 1.15-12.0 ;

1.5-4.5 ;

0.5-1.5.

5. A process of preparing a conformal film of a high temperature superconductive metal oxide comprising the steps of:

(a) forming an aerosol from a solution comprised of an organic solvent and precursor compounds selected from the group consisting of the respective metal acetates, the respective metal halides, and the respective metal diketonates, said precursor compounds capable of volatilizing at temperatures lower than the decomposition temperatures of said precursor compounds;

(b) passing said aerosol in combination with an oxygen-containing carrier gas into a heated zone, said heated zone having a temperature sufficient to evaporate the organic solvent and volatilize said precursor compounds, said temperature is insufficient to decompose said precursor compounds;

(c) passing said volatilized precursor compounds in contact with a surface of a heated substrate, said substrate heated at temperatures greater than the temperature of the heated zone whereat said precursor compounds are volatilized and sufficient to decompose said volatilized precursor compounds whereby metal atoms contained within said volatilized precursor compounds are deposited as a metal oxide film upon the substrate; and

,

(d) heating said deposited metal oxide film in an oxygen-containing atmosphere at temperatures sufficient to form said high temperature superconductive metal oxide film.

6. The process of claim 5 wherein said deposited metal oxide film is heated in an oxygen-containing atmosphere at temperatures from about 750°

C. to about 950°

C. for sufficient time to form said high temperature superconductive metal oxide film.

7. The process of claim 5 wherein said precursor compounds are a mixture of a barium compound, a copper compound, and a yttrium compound.

8. The process of claim 5 wherein the substrate is selected from the group consisting of silicon, magnesium oxide, yttrium-stabilized zirconium oxide, sapphire, lanthanum aluminate and lanthanum gallage.

9. The process of claim 5 wherein said solvent is selected from the group consisting of alcohols, ketones and aromatics, and said precursor a mixture of barium, yttrium and copper compounds having volatilities at temperatures lower than their respective decomposition temperatures.

10. The process of claim 9 wherein the molar ratios of the barium:

copper;

yttrium compounds in the solution are in the range of about 1.5-12.0 ;

1.5-4.5 ;

0.5-1.5.