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US5391407A Expired / Lapsed US ⏱️ 0.0 years remaining

Process for forming protective diamond-like carbon coatings on metallic surfaces

Assignee: Southwest Research Institute
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Filing: 1994-03-18
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Granted: 1995-02-21
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Expires: 2014-03-18
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Abstract

Abstract Process for forming diamond-like carbon coatings on metal surfaces to produce increased resistance to penetration, abrasion, and corrosion. A Ni/P coating is formed on an uncoated metal workpiece by-electroless deposition. While the workpiece is heated to harden the Ni/P coating, a vaporized stream of silicon is directed onto the Ni/P coating and the stream of silicon over the Ni/P coating is bombarded with an ion beam such that a NiSi 2 layer is formed at the interface of the Ni/P coating and silicon and a silicon overlayer is formed over the NiSi 2 layer. A vaporized stream of carbon-containing precursor molecules is directed onto the silicon overlayer such that a film of the precursor molecules condenses on the silicon overlayer. The film of precursor molecules is bombarded with an ion beam sufficiently to form a layer of diamond-like carbon on the silicon overlayer. A Ni/B solution or Ni/SiC solution can be used instead of the Ni/P solution, and germanium can be used instead of silicon.

Inventors

  • 👤 Geoffrey Dearnaley

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-10-23 13:36
CPC Classifications
C; C23; C23C; C23C14/00; C23C14/22; C23C14/02; C23C14/024; C23C14/06; C23C14/0605

Claims Analysis

Total Claims: 27
Claim 1
Independent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/P electroless deposition solution heated to a sufficient temperature that a Ni/P coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/P coating; (c) simultaneously with the heating step (b), directing a vaporized stream of silicon onto the Ni/P coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of silicon over the Ni/P coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiSi 2 forms at the interface of the Ni/P coating and the silicon and that a silicon overlayer forms above the NiSi 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the silicon overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the silicon overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the silicon overlayer.
Claim 2
Dependent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/P electroless deposition solution heated to a sufficient temperature that a Ni/P coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/P coating; (c) simultaneously with the heating step (b), directing a vaporized stream of silicon onto the Ni/P coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of silicon over the Ni/P coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiSi 2 forms at the interface of the Ni/P coating and the silicon and that a silicon overlayer forms above the NiSi 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the silicon overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the silicon overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the silicon overlayer.
Claim 3
Dependent Claim 15 words
The process of claim 1, wherein the Ni/P solution is 3-12% phosphorus by atomic percent.
Claim 4
Dependent Claim 21 words
The process of claim 1, wherein the Ni/P solution comprises nickel sulfate, sodium hypophosphite, amino-acetic acid, acetic acid, and filtered water.
Claim 5
Dependent Claim 18 words
The process of claim 1, wherein the vaporized stream of silicon originates in an electron beam heated hearth.
Claim 6
Dependent Claim 36 words
The process of claim 1, wherein the ion beam used to bombard the stream of silicon over the Ni/P coating is aligned at approximately a 30° angle to the direction of the vaporized stream of silicon.
Claim 7
Dependent Claim 25 words
The process of claim 5, wherein the vaporized stream of silicon is directed at a substantially right angle to a surface of the Ni/P coating.
Claim 8
Dependent Claim 16 words
The process of claim 1, wherein the ion beam used to bombard the silicon comprises nitrogen.
Claim 9
Dependent Claim 16 words
The process of claim 1, wherein the ion beam used to bombard the silicon comprises argon.
Claim 10
Dependent Claim 20 words
The process of claim 1, wherein the heating of the workpiece to approximately 315° C. is for approximately three hours.
Claim 11
Dependent Claim 11 words
The process of claim 1, wherein the precursor is polydimethyl siloxane.
Claim 12
Dependent Claim 22 words
The process of claim 1, wherein the vaporized stream of precursor molecules originates from a vessel electrically heated to approximately 140° C.
Claim 13
Dependent Claim 11 words
The process of claim 1, wherein the precursor is polyphenyl ether.
Claim 14
Dependent Claim 25 words
The process of claim 1, wherein the step of directing a vaporized stream of carbon-containing precursor molecules takes place at a temperature below 100° C.
Claim 15
Dependent Claim 27 words
The process of claim 1, wherein the ion beam used to bombard the film of precursor molecules comprises nitrogen ions at energy levels of approximately 10 KeV.
Claim 16
Dependent Claim 21 words
The process of claim 1, further comprising the step of bombarding the diamond-like carbon coating with an ion beam comprising fluorine.
Claim 17
Dependent Claim 21 words
The process of claim 1, further comprising the step of bombarding the diamond-like carbon coating with an ion beam comprising sulfur.
Claim 18
Dependent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/B electroless deposition solution heated to a sufficient temperature that a Ni/B coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/B coating; (c) simultaneously with the heating step (b), directing a vaporized stream of silicon onto the Ni/B coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of silicon over the Ni/B coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiSi 2 forms at the interface of the Ni/B coating and the silicon and that a silicon overlayer forms above the NiSi 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the silicon overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the silicon overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the silicon overlayer.
Claim 19
Dependent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/B electroless deposition solution heated to a sufficient temperature that a Ni/B coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/B coating; (c) simultaneously with the heating step (b), directing a vaporized stream of silicon onto the Ni/B coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of silicon over the Ni/B coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiSi 2 forms at the interface of the Ni/B coating and the silicon and that a silicon overlayer forms above the NiSi 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the silicon overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the silicon overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the silicon overlayer.
Claim 20
Dependent Claim 15 words
The process of claim 17, wherein the Ni/B solution is 5% boron by atomic weight.
Claim 21
Dependent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/SiC electroless deposition solution heated to a sufficient temperature that a Ni/SiC coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/SiC coating; (c) simultaneously with the heating step (b), directing a vaporized stream of silicon onto the Ni/SiC coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of silicon over the Ni/SiC coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiSi 2 forms at the interface of the Ni/SiC coating and the silicon and that a silicon overlayer forms above the NiSi 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the silicon overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the silicon overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the silicon overlayer.
Claim 22
Dependent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/SiC electroless deposition solution heated to a sufficient temperature that a Ni/SiC coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/SiC coating; (c) simultaneously with the heating step (b), directing a vaporized stream of silicon onto the Ni/SiC coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of silicon over the Ni/SiC coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiSi 2 forms at the interface of the Ni/SiC coating and the silicon and that a silicon overlayer forms above the NiSi 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the silicon overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the silicon overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the silicon overlayer.
Claim 23
Dependent Claim 14 words
The process of claim 1, wherein the Ni/SiC solution is 25% SiC by volume.
Claim 24
Dependent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/P electroless deposition solution heated to a sufficient temperature that a Ni/P coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/P coating; (c) simultaneously with the heating step (b), directing a vaporized stream of germanium onto the Ni/P coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of germanium over the Ni/P coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiGe 2 forms at the interface of the Ni/P coating and the germanium and that a germanium overlayer forms above the NiGe 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the germanium overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the germanium overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the germanium overlayer.
Claim 25
Dependent Claim 246 words
A process for coating a metal surface, comprising the steps of: (a) immersing a metal workpiece comprising an uncoated metal surface in a Ni/P electroless deposition solution heated to a sufficient temperature that a Ni/P coating forms on the metal surface; (b) placing the workpiece in a vacuum chamber and heating the workpiece to approximately 315° C. for a sufficient amount of time to harden the Ni/P coating; (c) simultaneously with the heating step (b), directing a vaporized stream of germanium onto the Ni/P coating; (d) simultaneously with the heating and directing of steps (b) and (c), bombarding the stream of germanium over the Ni/P coating with an ion beam and at an energy level of 200 eV-100 KeV for a sufficient amount of time that a layer of NiGe 2 forms at the interface of the Ni/P coating and the germanium and that a germanium overlayer forms above the NiGe 2 interface layer; (e) directing a vaporized stream of carbon-containing precursor molecules having carbon-to-carbon and carbon-to-hydrogen bonds onto the surface of the germanium overlayer for a sufficient amount of time that a film of the precursor molecules condenses on the germanium overlayer; and (f) bombarding the film of precursor molecules with an ion beam of a sufficient energy level and for a sufficient amount of time that a sufficient number of the carbon-to-carbon and carbon-to-hydrogen bonds in the precursor molecules break to result in the formation of a diamond-like carbon coating on the germanium overlayer.
Claim 26
Dependent Claim 18 words
The process of claim 21, wherein the vaporized stream of germanium originates in an electron beam heated hearth.
Claim 27
Dependent Claim 36 words
The process of claim 21, wherein the ion beam used to bombard the stream of germanium over the Ni/P coating is aligned at approximately a 30° angle to the direction of the vaporized stream of germanium.

References Cited (Backward Citations)

US4554208A Cited
US4634600A Cited
US5009923A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1998-02-20 1998-08-22 1999-02-21 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 2002-02-20 2002-08-22 2003-02-21 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 2006-02-20 2006-08-22 2007-02-21 $7700.00 Window Closed / Lapsed

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