Apparatus for growing metal oxides using organometallic vapor phase epitaxy

The methods and apparatus disclosed enable controlled growth of multicomponent metal oxide thin films, including high temperature superconducting (HTS) thin films, which are uniform and reproducible. The method and apparatus enable a controlled flow and pressure of a gaseous phase of metal containing molecules to be introduced into a reaction chamber, or into an analysis chamber, or into both. The flow into the reaction chamber enables deposition of metal oxides on a substrate and, therefore, growth of multicomponent metal oxide thin films, including HTS thin films, on the substrate. The flow into the analysis chamber enables compositional analysis of the gas. The apparatus also allows adjustment of the gaseous phase flow and pressure into the reaction chamber based upon the results of the compositional analysis. In one aspect of this invention, a heating mantle provides substantially uniform heating throughout the apparatus.

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Claims

1. An apparatus for enabling composition controlled deposition of multicomponent metal oxide film on a substrate comprising:

more than one solid source each for holding a solid metal-containing compound and including a gas flow controller, a temperature controller, and a pressure controller, for providing controlled vaporization of the solid metal-containing compound into gaseous phase and for enabling flow of the gaseous phase to at least one of a reaction chamber and a composition analyzer,
the reaction chamber for holding a heated substrate and accepting gas flow of the gaseous phase, the heated substrate enabling decomposition of the gaseous phase and deposition of the metal in the gaseous phase onto the substrate,
a gaseous phase composition analyzer for accepting gas flow of the gaseous phase and analyzing the composition of the gaseous phase, and
a controller for receiving information regarding the composition of the gaseous phase from the composition analyzer and for controlling the composition of the gaseous phase through adjusting at least one of the gas flow controller, the temperature controller, and the pressure controller of the solid sources.

2. The apparatus claimed in claim 1 wherein the analyzer for accepting gas flow comprises a mass spectrometer.

3. The apparatus of claim 1 further comprising a heating enclosure which uniformly heats and controls the temperature of all process piping downstream from the solid sources to prevent precursor condensation prior to reaching the reaction chamber.

4. An apparatus of claim 1 further comprising closed-loop real time adjustment of gas composition in the reaction chamber to maintain metal oxide film composition.

5. The apparatus of claim 1 wherein the vaporization of the solid metal-containing compound occurs at a pressure of about 1-100 torr, at a temperature of about 100.degree.-200.degree. C., and at a gaseous flow rate of about 100-2000 sccm.

6. The apparatus of claim 5 wherein the gaseous phase composition analyzer is operatively connected to accept gas flow of gaseous phase prior to entry into the reaction chamber..Iadd.

7. An apparatus for enabling composition controlled deposition of multicomponent metal oxide film on a substrate comprising:

more than one solid source each for holding a solid metal-containing compound and including a gas flow controller, a temperature controller, and a pressure controller, for providing controlled vaporization of the solid metal-containing compound into a gaseous phase and for enabling flow of the gaseous phase to a reaction chamber,
the reaction chamber for holding a heated substrate and accepting gas flow of the gaseous phase, the heated substrate enabling decomposition of the gaseous phase and deposition of the metal in the gaseous phase onto the substrate,
a gaseous phase composition analyzer for analyzing the composition of the gaseous phase, and
a controller for receiving information regarding the composition of the gaseous phase from the composition analyzer and for controlling the composition of the gaseous phase through adjusting at least one of the gas flow controller, the temperature controller, and the pressure controller of the solid sources..Iaddend..Iadd.8. The apparatus of claim 7 further comprising closed-loop real time adjustment of gas composition of the gaseous phase to maintain metal oxide film composition..Iaddend..Iadd.9. The apparatus of claim 7 wherein the gaseous phase composition analyzer analyzes the composition of the gaseous phase composition prior to its

entry into the reaction chamber..Iaddend..Iadd.10. An apparatus for enabling composition controlled deposition of multicomponent metal oxide film on a substrate comprising:

more than one solid source each for holding a solid metal-containing compound and each including a gas flow controller, a temperature controller, a pressure controller, for providing controlled vaporization of the solid metal-containing compound into a gaseous phase and for enabling flow of the gaseous phase to a reaction chamber, and a gaseous phase composition analyzer for analyzing the composition of the gaseous phase from each source,
the reaction chamber for holding a heated substrate and accepting gas flow of the gaseous phase, the heated substrate enabling decomposition of the gaseous phase and deposition of the metal in the gaseous phase onto the substrate, and
a controller for receiving information regarding the composition of the gaseous phase from the composition analyzer and for controlling the composition of the gaseous phase through adjusting at least one of the gas flow controller, the temperature controller, and the pressure controller of the solid sources..Iaddend..Iadd.11. The apparatus of claim 10 further comprising closed-loop real time adjustment of gas composition of the gaseous phase to maintain metal oxide film composition..Iaddend.
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Patent History
Patent number: RE36295
Type: Grant
Filed: Oct 16, 1997
Date of Patent: Sep 14, 1999
Assignee: Superconductor Technologies, Inc. (Santa Barbara, CA)
Inventors: Eric J. Smith (Goleta, CA), Steven P. DenBaars (Goleta, CA), Boo J. L. Nilsson (Santa Barbara, CA)
Primary Examiner: Felisa Garrett
Law Firm: Lyon & Lyon LLP
Application Number: 8/951,397
Classifications
Current U.S. Class: Apparatus (117/200); Gas Or Vapor Deposition (118/715); By Means To Heat Or Cool (118/724)
International Classification: C30B 3500;