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US5376409A Expired / Lapsed US ⏱️ 0.0 years remaining

Process and apparatus for the use of solid precursor sources in liquid form for vapor deposition of materials

Assignee: Research Foundation of the State University of New York
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Filing: 1992-12-21
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Granted: 1994-12-27
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Expires: 2012-12-21
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Abstract

Abstract A process and apparatus for the use of liquid-source bubbler/delivery systems for the delivery of solid source precursors employed in the growth of advanced technical materials such as the deposition of copper films in microelectronic devices.

Inventors

  • 👤 Alain E. Kaloyeros
  • 👤 Eric T. Eisenbraun
  • 👤 Bo Zheng

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-31 01:51
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/06; C23C16/18; C23C16/44; C23C16/448; C23C16/4481; Y; Y10; Y10S; Y10S505/00; Y10S505/725; Y10S505/734

Claims Analysis

Total Claims: 28
Claim 1
Independent Claim 113 words
A process for the delivery of solid source precursors in liquid solution for the controlled growth of films on a selected substrate which comprises: providing a liquid mixture of a solid source precursor and compatible liquid solvent; liquid delivery system means for transporting the liquid mixture in a controlled flow to a first zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in said first zone; and delivering the vaporized liquid mixture onto a heated substrate in a reactor to decompose said liquid mixture and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature.
Claim 2
Dependent Claim 113 words
A process for the delivery of solid source precursors in liquid solution for the controlled growth of films on a selected substrate which comprises: providing a liquid mixture of a solid source precursor and compatible liquid solvent; liquid delivery system means for transporting the liquid mixture in a controlled flow to a first zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in said first zone; and delivering the vaporized liquid mixture onto a heated substrate in a reactor to decompose said liquid mixture and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature.
Claim 3
Dependent Claim 27 words
The process of claim 1 wherein said delivery system includes a zone which is heated to a temperature which is lower than that of the heated substrate.
Claim 4
Dependent Claim 22 words
The process of claim 2 wherein said liquid solvent is selected from the group consisting of ethanol, methanol, isopropanol, acetone, and hexane.
Claim 5
Dependent Claim 24 words
The process of claim 3 wherein the source precursor is selected from the group consisting of alkyls, hydrides, chlorides, halides, complexes and organometallic complexes.
Claim 6
Dependent Claim 21 words
The process of claim 3 wherein said solid source precursor is copper (II) β-diketonate, and said substrate is a microelectronic device.
Claim 7
Dependent Claim 18 words
The process of claim 5 wherein said solvent is selected from the group consisting of isopropanol and ethanol.
Claim 8
Dependent Claim 12 words
The process of claim 6 further including plasma assistance in said reactor.
Claim 9
Dependent Claim 13 words
The process of claim 7 wherein said plasma assistance is a hydrogen plasma.
Claim 10
Dependent Claim 19 words
The process of claim 7 wherein said substrate is heated to a temperature in the order of 160°-170° C.
Claim 11
Dependent Claim 20 words
The process of claim 9 wherein said reactor is maintained at a working pressure in the order of 1.0-1.7 torr.
Claim 12
Dependent Claim 27 words
The process of claim 10 wherein said plasma is a hydrogen plasma which is applied with a density in the order of 0.13-0.25 watts per square centimeter.
Claim 13
Dependent Claim 23 words
The process of claim 11 wherein said hydrogen plasma is formed by flowing 500-1200 cubic centimeters per minute of hydrogen into said reactor.
Claim 14
Dependent Claim 26 words
The process of claim 7 wherein said plasma is a hydrogen plasma which applied with a density in the order of 0.13-0.25 watts per square centimeter.
Claim 15
Dependent Claim 23 words
The process of claim 13 wherein said hydrogen plasma is formed by flowing 500-1200 cubic centimeters per minute of hydrogen into said reactor.
Claim 16
Dependent Claim 175 words
A process for the delivery of solid source precursors in liquid solution for the growth of films on a selected substrate which comprises: providing a liquid mixture of solid source precursors and a compatible liquid solvent; transporting the liquid mixture in a controlled flow to a zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in a reactor; and spraying the vaporized liquid mixture onto a heated substrate to decompose said precursors and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature; said zone is heated to a temperature which is lower than that of the heated substrate; said liquid solvent is selected from the group consisting of ethanol, methanol, isopropanol, acetone, and hexane; and wherein the process is utilized to grow a metal film in which a single solvent is utilized to dissolve multiple source precursors to form said liquid mixture, which is then provided to said heated substrate to grow a composite metallic film.
Claim 17
Dependent Claim 175 words
A process for the delivery of solid source precursors in liquid solution for the growth of films on a selected substrate which comprises: providing a liquid mixture of solid source precursors and a compatible liquid solvent; transporting the liquid mixture in a controlled flow to a zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in a reactor; and spraying the vaporized liquid mixture onto a heated substrate to decompose said precursors and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature; said zone is heated to a temperature which is lower than that of the heated substrate; said liquid solvent is selected from the group consisting of ethanol, methanol, isopropanol, acetone, and hexane; and wherein the process is utilized to grow a metal film in which a single solvent is utilized to dissolve multiple source precursors to form said liquid mixture, which is then provided to said heated substrate to grow a composite metallic film.
Claim 18
Dependent Claim 18 words
The process of claim 15 wherein a single spray means is provided for spraying the vaporized liquid mixture.
Claim 19
Dependent Claim 173 words
A process for the delivery of solid source precursors in liquid solution for the growth of composite films controlled thickness on a selected substrate which comprises: providing a liquid mixture of a solid source precursor and compatible liquid solvent; transporting the liquid mixture in a controlled flow to a zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in a reactor; and spraying the vaporized liquid mixture onto a heated substrate to decompose said precursor and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature; said zone is heated to a temperature which is lower than that of the heated substrate; said liquid solvent is selected from the group consisting of ethanol, methanol, isopropanol, acetone, and hexane; and wherein there is a plurality of solids dissolved in a plurality of liquid solvents to form a plurality of mixtures, and controlled flow of each of said mixtures enables selective proportioning of the composite film formed.
Claim 20
Dependent Claim 173 words
A process for the delivery of solid source precursors in liquid solution for the growth of composite films controlled thickness on a selected substrate which comprises: providing a liquid mixture of a solid source precursor and compatible liquid solvent; transporting the liquid mixture in a controlled flow to a zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in a reactor; and spraying the vaporized liquid mixture onto a heated substrate to decompose said precursor and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature; said zone is heated to a temperature which is lower than that of the heated substrate; said liquid solvent is selected from the group consisting of ethanol, methanol, isopropanol, acetone, and hexane; and wherein there is a plurality of solids dissolved in a plurality of liquid solvents to form a plurality of mixtures, and controlled flow of each of said mixtures enables selective proportioning of the composite film formed.
Claim 21
Dependent Claim 28 words
The process of claim 17 wherein each of said mixtures are connected to a single spray means for spraying a combined vaporized liquid mixture onto said heated substrate.
Claim 22
Dependent Claim 19 words
The process of claim 18 wherein at least two solid source precursors are dissolved in a single liquid solvent.
Claim 23
Dependent Claim 49 words
The process of claim 17 wherein said film is an aluminum-copper alloy and an aluminum precursor is mixed with a first solvent to form one of said plurality of mixtures, and a copper precursor is separately mixed with a second solvent to form another of said plurality of mixtures.
Claim 24
Dependent Claim 14 words
The process of claim 19 wherein said solid source precursors include copper and gold.
Claim 25
Dependent Claim 31 words
The process of claim 19 wherein said solid source precursors include precursors for metallic alloys of yttrium, barium and copper, all three of which are dissolved into a single solvent solution.
Claim 26
Dependent Claim 25 words
The process of claim 19 in which copper and yttrium precursors are dissolved in ethanol, and in addition a barium precursor is dissolved in hexane.
Claim 27
Dependent Claim 143 words
A process for the delivery of solid source precursors in liquid solution for the growth of films of controlled thickness on a selected substrate which comprises: providing a liquid mixture of a solid source precursor and compatible liquid solvent; transporting the liquid mixture in a controlled flow to a zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in a reactor; and spraying the vaporized liquid mixture onto a heated substrate to decompose said precursor and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature; said zone is heated to a temperature which is lower than that of the heated substrate; said liquid solvent is selected from the group consisting of ethanol, methanol, isopropanol, acetone, and hexane; and wherein said liquid mixture includes copper.
Claim 28
Dependent Claim 143 words
A process for the delivery of solid source precursors in liquid solution for the growth of films of controlled thickness on a selected substrate which comprises: providing a liquid mixture of a solid source precursor and compatible liquid solvent; transporting the liquid mixture in a controlled flow to a zone heated to a first temperature sufficient to vaporize the mixture without precursor decomposition; vaporizing said liquid mixture in a reactor; and spraying the vaporized liquid mixture onto a heated substrate to decompose said precursor and form a film on said heated substrate; the temperature of said heated substrate being higher than said first temperature; said zone is heated to a temperature which is lower than that of the heated substrate; said liquid solvent is selected from the group consisting of ethanol, methanol, isopropanol, acetone, and hexane; and wherein said liquid mixture includes copper.

References Cited (Backward Citations)

JPS5420967A Cited
US4707383A Cited
US4917717A Cited
US5110622A Cited
US4880670A Cited
US4992305A Cited
US5021399A Cited
US5120703A Cited
EP0470274A1 Cited
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USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1997-12-26 1998-06-27 1998-12-27 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2001-12-26 2002-06-27 2002-12-27 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2005-12-26 2006-06-27 2006-12-27 $7700.00 Window Closed / Lapsed

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