US4895765A
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US
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Titanium nitride and zirconium nitride coating compositions, coated articles and methods of manufacture
Assignee: Praxair ST Technology Inc
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Filing: 1986-09-10
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Granted: 1990-01-23
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Expires: 2006-09-10
Abstract
Abstract The present invention is directed to polycrystalline titanium nitride and zirconium nitride coating compositions and coated articles with a I(111)/I(200) x-ray diffraction intensity ratio of at least about 75 for the titanium nitride composition and at least about 15 for the zirconium nitride composition and to a method of forming a highly oriented polycrystalline titanium nitride or zirconium nitride coating composition with a high I(111)/I(200) x-ray diffraction intensity ratio. This invention also concerns polycrystalline titanium nitride and zirconium nitride coating compositions and coated articles of the type described with an interplanar spacing, d 111 , of 2.460 Angstroms or less for TiN and an interplanar spacing, d 111 , of 2.660 Angstroms or less for ZrN and to methods for producing same. The composition is deposited upon a substrate in an evacuated chamber from a titanium or zirconium cathode source surrounded by an elongated member which overhangs the cathode to form a cathode chamber. Nitrogen gas is passed through the cathode chamber into the vacuum chamber.
Inventors
- 👤 Jiinjen A. Sue
- 👤 Harden H. Troue
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-24 08:54
CPC Classifications
C; C23; C23C; C23C14/00; C23C14/06; C23C14/0641; C23C14/0021; Y; Y10; Y10T; Y10T428/00; Y10T428/12; Y10T428/12493; Y10T428/12535; Y10T428/12576
Claims Analysis
Total Claims: 34
Claim 1
Independent Claim
25 words
A polycrystalline zirconium nitride coating composition having a highly oriented crystallographic structure consisting of an I(111)/I(200) x-ray diffraction intensity ratio of at least about 15.
Claim 2
Dependent Claim
25 words
A polycrystalline zirconium nitride coating composition having a highly oriented crystallographic structure consisting of an I(111)/I(200) x-ray diffraction intensity ratio of at least about 15.
Claim 3
Dependent Claim
21 words
A zirconium nitride polycrystalline coating composition as defined in claim 1 having an I(111)/I(200) x-ray diffraction intensity ratio greater than 50.
Claim 4
Dependent Claim
24 words
A ZrN polycrystalline coating composition as defined in claim 1 having an x-ray diffraction interplanar spacing, d 111 , of 2.660 Angstroms or less.
Claim 5
Dependent Claim
25 words
A polycrystalline titanium nitride coating composition having a highly oriented crystallographic structure consisting of an I(111)/I(200) x-ray diffraction intensity ratio of at least about 75.
Claim 6
Dependent Claim
25 words
A polycrystalline titanium nitride coating composition having a highly oriented crystallographic structure consisting of an I(111)/I(200) x-ray diffraction intensity ratio of at least about 75.
Claim 7
Dependent Claim
21 words
A titanium nitride polycrystalline coating composition as defined in claim 4 having an I(111)/I(200) x-ray diffraction intensity ratio greater than 100.
Claim 8
Dependent Claim
24 words
A TiN polycrystalline coating composition as defined in claim 4 having an x-ray diffraction interplanar spacing, d 111 , of 2.460 Angstroms or less.
Claim 9
Dependent Claim
41 words
A zirconium nitride coated article having highly erosion resistant characteristics comprising a substrate and a coating of a polycrystalline zirconium nitride coating composition having a highly oriented crystallographic structure with an I(111)/I(200) x-ray diffraction intensity ratio of at least about 15.
Claim 10
Dependent Claim
41 words
A zirconium nitride coated article having highly erosion resistant characteristics comprising a substrate and a coating of a polycrystalline zirconium nitride coating composition having a highly oriented crystallographic structure with an I(111)/I(200) x-ray diffraction intensity ratio of at least about 15.
Claim 11
Dependent Claim
27 words
A ZrN coated article as defined in claim 7 wherein said ZrN coating has an x-ray diffraction interplanar spacing, d 111 , of 2.660 Angstroms or less.
Claim 12
Dependent Claim
40 words
A TiN coated article having highly erosion resistant characteristics comprising a substrate and a coating of a polycrystalline titanium nitride coating composition having a highly oriented crystallographic structure with an I(111)/I(200) x-ray diffraction intensity ratio of at least about 75.
Claim 13
Dependent Claim
40 words
A TiN coated article having highly erosion resistant characteristics comprising a substrate and a coating of a polycrystalline titanium nitride coating composition having a highly oriented crystallographic structure with an I(111)/I(200) x-ray diffraction intensity ratio of at least about 75.
Claim 14
Dependent Claim
31 words
A TiN or ZrN coated article as defined in claim 7 wherein said substrate is composed of either a refractory metal, refractory alloy, aluminum alloy, superalloy, stainless steel, or ceramic composites.
Claim 15
Dependent Claim
30 words
A TiN or ZrN coated article as defined in claim 10 wherein said refractory metal is selected from the class consisting of Ti, Zr, V, Ta, Cr, Mo and W.
Claim 16
Dependent Claim
28 words
A TiN or ZrN coated article as defined in claim 10 wherein said superalloy is selected from the class consisting of Inconel 718, Inconel 738, A-286 and Waspaloy.
Claim 17
Dependent Claim
36 words
A TiN or ZrN coated article as defined in claim 10 wherein said stainless steel is selected from the class consisting of 17-4PH, AISI 304, AISI 316, AISI 403, AISI 422, AISI 410 and AM 355.
Claim 18
Dependent Claim
19 words
A TiN or ZrN coated article as defined in claim 10 wherein the substrates are Ti-6Al-4V, Ti-8Al-1Mo-1Va and Ti-6Al-2Sn-4Zr-2Mo.
Claim 19
Dependent Claim
27 words
A TiN coated article as defined in claim 9 wherein said TiN coating has an x-ray diffraction interplanar spacing, d 111 , of 2.460 Angstroms or less.
Claim 20
Independent Claim
212 words
A method of forming a highly oriented polycrystalline titanium nitride or zirconium nitride coating upon a substrate with the TiN or ZrN coating having a high I(111)/I(200) x-ray diffraction intensity ratio comprising the steps of: (a) providing within a vacuum chamber cathode comprising a source material of titanium or zirconium upon an evaporable end surface, and an anode spaced apart from the cathode; (b) generating an electric arc between the evaporable end surface of the cathode and the anode to form a plasma of material from the source material; (c) surrounding the cathode with an elongated member positioned between and spaced from the cathode and the anode, wherein the elongated member is electrically insulated from the cathode and the anode and has an open end extending a distance x beyond the evaporable end surface of the cathode to form a cathode chamber containing the plasma; (d) directing a flow of nitrogen gas through the plasma in the cathode chamber and into the vacuum chamber such that the gas envelops the electric arc over at least the distance x before entering the vacuum chamber; (e) withdrawing gas from the vacuum chamber to maintain a predetermined pressure within the vacuum chamber; and (f) depositing a coating of material from the plasma upon the object.
Claim 21
Independent Claim
212 words
A method of forming a highly oriented polycrystalline titanium nitride or zirconium nitride coating upon a substrate with the TiN or ZrN coating having a high I(111)/I(200) x-ray diffraction intensity ratio comprising the steps of: (a) providing within a vacuum chamber cathode comprising a source material of titanium or zirconium upon an evaporable end surface, and an anode spaced apart from the cathode; (b) generating an electric arc between the evaporable end surface of the cathode and the anode to form a plasma of material from the source material; (c) surrounding the cathode with an elongated member positioned between and spaced from the cathode and the anode, wherein the elongated member is electrically insulated from the cathode and the anode and has an open end extending a distance x beyond the evaporable end surface of the cathode to form a cathode chamber containing the plasma; (d) directing a flow of nitrogen gas through the plasma in the cathode chamber and into the vacuum chamber such that the gas envelops the electric arc over at least the distance x before entering the vacuum chamber; (e) withdrawing gas from the vacuum chamber to maintain a predetermined pressure within the vacuum chamber; and (f) depositing a coating of material from the plasma upon the object.
Claim 22
Dependent Claim
19 words
A method as defined in claim 16 wherein the I(111)/I(200) x-ray diffraction intensity ratio is at least about 75.
Claim 23
Dependent Claim
38 words
A method as defined in claim 16 wherein step (c) the cathode is surrounded with the elongated member to form a space between the cathode and the elongated member and the nitrogen gas is introduced into the space.
Claim 24
Dependent Claim
32 words
A method as defined in claim 16 wherein the elongated member has a circular cross-section and surrounds the cathode which has a circular cross-section, to form the space having an annular cross-section.
Claim 25
Dependent Claim
57 words
A method as defined in claim 16 wherein d is the major dimension of the cathode evaporable end surface, and the cathode is surrounded by the elongated member in step (b) such that the open end of the elongated member extends beyond the evaporable end surface of the cathode such that x/d is from 0.07 to 2.
Claim 26
Dependent Claim
14 words
A method as defined in claim 20 wherein x/d is between 0.3 and 1.0.
Claim 27
Dependent Claim
24 words
A method as defined in claim 16 wherein the vacuum chamber is evacuated to a pressure of between 10 -1 and 5×10 -4 torr.
Claim 28
Dependent Claim
20 words
A method as defined in claim 16 wherein the electrical potential of the substrate is more negative than the anode.
Claim 29
Dependent Claim
23 words
A method as defined in claim 16 wherein the electrical potential of the substrate is more negative than the anode and the cathode.
Claim 30
Dependent Claim
36 words
A method as defined in claim 16 wherein material from the source material is deposited on said elongated member to form a converging nozzle having a nozzle aperture greater than zero and less than 0.4 cm.
Claim 31
Dependent Claim
33 words
A method as defined in claim 16 wherein the object is composed of a material selected from the class consisting of refractory metals, refractory alloys, superalloys, aluminum alloys, stainless steels, and ceramic composites.
Claim 32
Dependent Claim
29 words
A method as defined in claim 16 wherein said coating is a highly oriented polycrystalline titanium nitride having an interplanar spacing, d 111 , of 2.460 Angstroms or less.
Claim 33
Dependent Claim
28 words
A method as defined in claim 16 wherein said coating is a highly oriented zirconium nitride having an interplanar spacing d 111 , or 2.660 Angstroms or less.
Claim 34
Dependent Claim
27 words
A method as defined in claim 16 wherein said coating is a highly oriented zirconium nitride having an I(111)/I(200) x-ray diffraction intensity ratio of at least 15.
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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) | 1993-01-22 | 1993-07-24 | 1994-01-23 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1997-01-22 | 1997-07-24 | 1998-01-23 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2001-01-22 | 2001-07-24 | 2002-01-23 | $7700.00 | Window Closed / Lapsed |