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Diamond film deposition with a microwave plasma

Assignee: Saint Gobain Abrasives Inc
•
Filing: 1993-07-20
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Granted: 1994-12-06
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Expires: 2013-07-20
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Abstract

Abstract A method for depositing diamond film on a substrate utilizing a tuneable microwave cavity with an adjustable height and antenna and an electrically insulated chamber comprises the steps of decreasing the pressure within the chamber, creating a plasma including hydrogen gas within the chamber, tuning the cavity by varying its height and the depth of insertion of the antenna to minimize reflected power and properly position the plasma on the substrate, injecting a hydrocarbon gas into the chamber, and maintaining the plasma for a sufficient time for diamond film of the desired thickness to be deposited.

Inventors

  • 👤 Louis K. Bigelow
  • 👤 James T. Hoggins
  • 👤 Deborah Gunderson
  • 👤 Cristan Ellison

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-08 09:03
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/22; C23C16/26; C23C16/27; C23C16/274; C23C16/44; C23C16/50; C23C16/511

Claims Analysis

Total Claims: 39
Claim 1
Independent Claim 145 words
A process for depositing diamond film on the surface of a substrate comprising the steps of: providing a microwave plasma generating apparatus including a microwave cavity tuneable by means of adjusting the height thereof and the depth of insertion of an antenna, an electrically chamber comprising insulating material within said cavity, including a gas supply for injecting gases into said chamber and a platform for supporting a substrate within said chamber; decreasing the pressure within said chamber; creating a plasma including hydrogen gas within said chamber; tuning said cavity to position the plasma such that it encompasses the surface of said substrate on which diamond is to be deposited; heating said substrate to a temperature range in which deposition of diamond can occur; injecting a hydrocarbon gas into said plasma; and maintaining said plasma for sufficient time for depositing diamond film of a desired thickness.
Claim 2
Dependent Claim 145 words
A process for depositing diamond film on the surface of a substrate comprising the steps of: providing a microwave plasma generating apparatus including a microwave cavity tuneable by means of adjusting the height thereof and the depth of insertion of an antenna, an electrically chamber comprising insulating material within said cavity, including a gas supply for injecting gases into said chamber and a platform for supporting a substrate within said chamber; decreasing the pressure within said chamber; creating a plasma including hydrogen gas within said chamber; tuning said cavity to position the plasma such that it encompasses the surface of said substrate on which diamond is to be deposited; heating said substrate to a temperature range in which deposition of diamond can occur; injecting a hydrocarbon gas into said plasma; and maintaining said plasma for sufficient time for depositing diamond film of a desired thickness.
Claim 3
Dependent Claim 24 words
The process of claim 1 wherein said cavity has a continuously adjustable height and said tuning step comprises adjusting the height of said cavity.
Claim 4
Dependent Claim 33 words
The process of claims 1 or 2 wherein the depth of insertion of said antenna is continuously adjustable and said tuning step further comprises continuously adjusting the depth of insertion of said antenna.
Claim 5
Dependent Claim 15 words
The process of claim 1, wherein said plasma has a height less than its diameter.
Claim 6
Dependent Claim 22 words
The process of claim 1 further comprising maintaining said pressure in said cavity at at least 30 torr after creating said plasma.
Claim 7
Dependent Claim 18 words
The process of claims 1 or 5 wherein said substrate is heated to between about 950° C.-1,100° C.
Claim 8
Dependent Claim 17 words
The process of claims 1 or 5 further comprising polishing said substrate before depositing said diamond film.
Claim 9
Dependent Claim 25 words
The process of claims 1 or 5 wherein the concentration of said hydrocarbon gas is between about 0.2-2.5% of the concentration of said hydrogen gas.
Claim 10
Dependent Claim 27 words
The process of claims 1 or 5 wherein said substrate is chosen from the group consisting of silicon, silicon nitride, silicon carbide, sialon, aluminum oxide or germanium.
Claim 11
Dependent Claim 19 words
The process of claims 1 or 5 wherein said substrate comprises tungsten carbide coated with tungsten or titanium nitride.
Claim 12
Dependent Claim 23 words
The process of claims 1 or 5 wherein said substrate is supported by a graphite susceptor, pyrophyllite, boron nitride and a steel plate.
Claim 13
Dependent Claim 39 words
The process of claim 1 wherein said heating step comprises first heating said substrate to between about 800° C.-900° C. for between about 1-2 hours, and then increasing said temperature of said substrate to between about 950° C.-1,100° C.
Claim 14
Dependent Claim 168 words
A process for depositing diamond film on the surface of a substrate in a tuneable microwave cavity having an adjustable height and an antenna having an adjustable depth of insertion, and including an electrically plasma chamber comprising insulating material, said process comprising the steps of; decreasing the pressure in said plasma chamber; injecting an inert gas into said plasma chamber; igniting said inert gas by microwave power; injecting hydrogen gas into said plasma chamber; ceasing the injection of said inert gas after said hydrogen gas ignites; maintaining the pressure in said chamber at a selected level; positioning said plasma and tuning said cavity by adjusting the height of said cavity and the depth of insertion of said antenna for minimizing reflected power and forming said plasma such that it encompasses said surface of said substrate; heating said substrate to a temperature at which diamond deposition can occur; injecting hydrocarbon gas into said plasma; maintaining said plasma for a sufficient time to deposit the desired thickness of diamond film.
Claim 15
Dependent Claim 168 words
A process for depositing diamond film on the surface of a substrate in a tuneable microwave cavity having an adjustable height and an antenna having an adjustable depth of insertion, and including an electrically plasma chamber comprising insulating material, said process comprising the steps of; decreasing the pressure in said plasma chamber; injecting an inert gas into said plasma chamber; igniting said inert gas by microwave power; injecting hydrogen gas into said plasma chamber; ceasing the injection of said inert gas after said hydrogen gas ignites; maintaining the pressure in said chamber at a selected level; positioning said plasma and tuning said cavity by adjusting the height of said cavity and the depth of insertion of said antenna for minimizing reflected power and forming said plasma such that it encompasses said surface of said substrate; heating said substrate to a temperature at which diamond deposition can occur; injecting hydrocarbon gas into said plasma; maintaining said plasma for a sufficient time to deposit the desired thickness of diamond film.
Claim 16
Dependent Claim 13 words
The process of claim 13 further comprising adjusting the height of said substrate.
Claim 17
Dependent Claim 15 words
The process of claim 13, further comprising roughening the surface of said substrate before coating.
Claim 18
Dependent Claim 32 words
The process of claim 15 wherein said polishing step comprises placing said substrate on a silk cloth, and rotating said silk cloth by a wheel with diamond paste between about 0.10-1 micron.
Claim 19
Dependent Claim 18 words
The process of claim 13 wherein the microwave power emitted by said antenna is between about 600-900 watts.
Claim 20
Dependent Claim 22 words
The process of claim 13, wherein said hydrocarbon is methane or acetylene, at a concentration between about 0.2-2.5% of the hydrogen concentration.
Claim 21
Dependent Claim 25 words
The process of claim 13 wherein said substrate is chosen from the group consisting of silicon, silicon nitride, silicon carbide, or sialon, alumina or germanium.
Claim 22
Dependent Claim 22 words
The process of claim 13 wherein said hydrocarbon gas is methane, at a concentration between 0.5-2.0% the concentration of the hydrogen gas.
Claim 23
Dependent Claim 54 words
The method of claim 13 further comprising heating said substrate to between about 800° C.-900° C. after positioning said plasma, injecting said hydrocarbon into said chamber, and maintaining said substrate at between about 600° C.-900° C. for about 1-2 hours, and then increasing said temperature of said substrate to between about 900° C.-1,100° C.
Claim 24
Dependent Claim 18 words
The process of claim 13 wherein said plasma overlaps at least 20% of the side of said substrate.
Claim 25
Dependent Claim 184 words
A process for coating identical substrates with diamond film in a tuneable microwave cavity having an adjustable height and an antenna having an adjustable depth of insertion, and including a plasma chamber comprising electrically insulating material, comprising the steps of placing a first substrate in said chamber of said apparatus; decreasing the pressure within said chamber; creating a plasma including hydrogen gas within said chamber; maintaining the pressure in said chamber at at least 30 torr; selecting the tuning of said cavity and the position of said substrate to position the plasma such that said surface of said substrate lies within said plasma; heating said substrate to a temperature sufficient for depositing the desired diamond film; injecting a hydrocarbon gas into said plasma; continuing said deposition for a sufficient time to deposit the desired thickness of diamond film on said substrate; replacing said substrate with an uncoated substrate of the same type; repeating said decreasing step, said creating step, said maintaining step, said heating step, said injecting step, said continuing step and said replacing step, until the desired number of substrates have been coated.
Claim 26
Dependent Claim 184 words
A process for coating identical substrates with diamond film in a tuneable microwave cavity having an adjustable height and an antenna having an adjustable depth of insertion, and including a plasma chamber comprising electrically insulating material, comprising the steps of placing a first substrate in said chamber of said apparatus; decreasing the pressure within said chamber; creating a plasma including hydrogen gas within said chamber; maintaining the pressure in said chamber at at least 30 torr; selecting the tuning of said cavity and the position of said substrate to position the plasma such that said surface of said substrate lies within said plasma; heating said substrate to a temperature sufficient for depositing the desired diamond film; injecting a hydrocarbon gas into said plasma; continuing said deposition for a sufficient time to deposit the desired thickness of diamond film on said substrate; replacing said substrate with an uncoated substrate of the same type; repeating said decreasing step, said creating step, said maintaining step, said heating step, said injecting step, said continuing step and said replacing step, until the desired number of substrates have been coated.
Claim 27
Dependent Claim 20 words
The process of claim 23 wherein said hydrocarbon gas comprises methane, at a concentration between 0.2-2.5% of the hydrogen concentration.
Claim 28
Dependent Claim 16 words
The process of claim 23 further comprising heating said substrate to between about 800° C.-1,200° C.
Claim 29
Dependent Claim 16 words
The process of claims 23 further comprising heating said substrate to between about 950° C.-1,100° C.
Claim 30
Dependent Claim 33 words
The process of claim 26 further comprising varying the tuning of said plasma to properly position said plasma by varying the height of the cavity and the depth of insertion of said antenna.
Claim 31
Dependent Claim 119 words
A process for depositing diamond film on the surface of a substrate in a tuneable microwave cavity having a continuously adjustable height and an antenna having a continuously adjustable depth of insertion, and including an plasma chamber comprising electrically insulating material, comprising the steps of: setting said height and said depth of insertion of said tuneable microwave cavity, said setting based on said substrate and said deposition conditions; decreasing the pressure within said chamber; creating a plasma including hydrogen gas within said chamber at a pressure of at least about 30 torr; heating said substrate to between 800° C.-1,200° C.; injecting a hydrocarbon gas into said plasma; and monitoring said plasma to ensure it is in its proper position.
Claim 32
Dependent Claim 119 words
A process for depositing diamond film on the surface of a substrate in a tuneable microwave cavity having a continuously adjustable height and an antenna having a continuously adjustable depth of insertion, and including an plasma chamber comprising electrically insulating material, comprising the steps of: setting said height and said depth of insertion of said tuneable microwave cavity, said setting based on said substrate and said deposition conditions; decreasing the pressure within said chamber; creating a plasma including hydrogen gas within said chamber at a pressure of at least about 30 torr; heating said substrate to between 800° C.-1,200° C.; injecting a hydrocarbon gas into said plasma; and monitoring said plasma to ensure it is in its proper position.
Claim 33
Dependent Claim 19 words
The process of claim 28 wherein said heating step comprises heating said substrate to between about 950° C.-1,100° C.
Claim 34
Dependent Claim 23 words
The process of claim 28 wherein said hydrocarbon gas is set on a concentration between about 0.2-2.5% of the concentration of said hydrogen.
Claim 35
Dependent Claim 11 words
The process of claim 1, wherein said substrate is a tool.
Claim 36
Dependent Claim 20 words
The process of claim 1, wherein said surface of said substrate is uneven, said uneven surface lying within said plasma.
Claim 37
Dependent Claim 36 words
The process of claim 1, wherein said chamber comprising electrically insulating material comprises a quartz bell jar resting on a base plate, said base plate including cooling means for carrying fluid for cooling said base plate.
Claim 38
Dependent Claim 21 words
The process of claims 1, wherein said method further comprises pumping nitrogen gas into said cavity for cooling said bell jar.
Claim 39
Dependent Claim 20 words
The process of claim 1, wherein said substrate is placed on a graphite susceptor for supporting and heating said substrate.

References Cited (Backward Citations)

US4434188A Cited
US4507588A Cited
US4585668A Cited
US4591662A Cited
US4630566A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1997-12-05 1998-06-06 1998-12-06 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2001-12-05 2002-06-06 2002-12-06 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2005-12-05 2006-06-06 2006-12-06 $7700.00 Window Closed / Lapsed

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