Patent US3160308A successfully refreshed from Google Patents.
Patent US4336117A successfully refreshed from Google Patents.
US4336117A
Expired / Lapsed
US
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Refractory coatings and method of producing the same
Assignee: National Aeronautics and Space Administration
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Filing: 1979-12-07
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Granted: 1982-06-22
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Expires: 1999-12-07
Abstract
Abstract This invention is concerned with improving adhesion, friction and wear properties of sputtered refractory coatings on substrates of materials that form stable nitrides. Each substrate (10) is placed directly below a titanium carbide target (16) of a commercial radiofrequency diode apparatus (14) in a vacuum chamber (26). Nitrogen is bled into the system through a nozzle (30) resulting in a small partial pressure of about 0.5% to 2.5% during the first two minutes of deposition. The flow of nitrogen is then stopped, and the sputtering ambient is reduced to pure argon through a nozzle (28) without interrupting the sputtering process. When nitrogen is deliberately introduced during the crucial interface formation, some of the titanium at the interface reacts to form titanium nitride while the metal of the substrate also forms the nitride. These two nitrides atomically mixed together in the interfacial region (38) act to more strongly bond the growing titanium carbide coating (12) as it forms on the substrate (10).
Inventors
- 👤 William A. Brainard
- 👤 Donald R. Wheeler
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-01 20:47
CPC Classifications
C; C23; C23C; C23C14/00; C23C14/06; C23C14/0635; C23C14/02; C23C14/024; C23C14/0641
Claims Analysis
Total Claims: 7
Claim 1
Independent Claim
73 words
In a method of producing a hard coated article of manufacture wherein a titanium carbide coating is deposited on a steel substrate from a radiofrequency sputtering plasma, the improvement comprising introducing nitrogen into the sputtering environment during the formation of the interfacial region of the coating at the substrate thereby forming a mixture of titanium nitrides and iron nitrides in said interfacial region which improves the bond between the coating and the substrate.
Claim 2
Dependent Claim
73 words
In a method of producing a hard coated article of manufacture wherein a titanium carbide coating is deposited on a steel substrate from a radiofrequency sputtering plasma, the improvement comprising introducing nitrogen into the sputtering environment during the formation of the interfacial region of the coating at the substrate thereby forming a mixture of titanium nitrides and iron nitrides in said interfacial region which improves the bond between the coating and the substrate.
Claim 3
Dependent Claim
23 words
The method of claim 1 wherein nitrogen is introduced at a partial pressure sufficient to comprise about 0.5% to 2.5% of the plasma.
Claim 4
Dependent Claim
14 words
The method of claim 2 wherein the nitrogen is introduced for about two minutes.
Claim 5
Independent Claim
158 words
A method of producing a hard coated article of manufacture having improved adhesion between a titanium carbide refractory coating and a steel substrate comprising the steps of placing the substrate in a vacuum chamber containing radiofrequency diode apparatus, reducing the pressure in said chamber to a base pressure of about 10 -6 torr, supplying nitrogen to said vacuum chamber at a pressure in the range of about 1.3×10 -2 to about 6.6×10 -2 Newtons per square meter, admitting argon into said vacuum chamber to raise the total pressure to about 20 μm, sputtering to deposit from a plasma an interfacial region which contains a mixture of titanium nitride and iron nitride, interrupting the supply of nitrogen to said vacuum chamber, and sputtering to deposit the remainder of the titanium carbide refractory coating in an environment substantially free of nitrogen so that said remainder of the titanium carbide refractory coating is substantially free of titanium nitride and iron nitride.
Claim 6
Independent Claim
158 words
A method of producing a hard coated article of manufacture having improved adhesion between a titanium carbide refractory coating and a steel substrate comprising the steps of placing the substrate in a vacuum chamber containing radiofrequency diode apparatus, reducing the pressure in said chamber to a base pressure of about 10 -6 torr, supplying nitrogen to said vacuum chamber at a pressure in the range of about 1.3×10 -2 to about 6.6×10 -2 Newtons per square meter, admitting argon into said vacuum chamber to raise the total pressure to about 20 μm, sputtering to deposit from a plasma an interfacial region which contains a mixture of titanium nitride and iron nitride, interrupting the supply of nitrogen to said vacuum chamber, and sputtering to deposit the remainder of the titanium carbide refractory coating in an environment substantially free of nitrogen so that said remainder of the titanium carbide refractory coating is substantially free of titanium nitride and iron nitride.
Claim 7
Dependent Claim
35 words
A method of producing a hard coated article of manufacture as claimed in claim 4 wherein the supply of nitrogen to the vacuum chamber is interrupted about two minutes after the radiofrequency sputtering is started.
References Cited (Backward Citations)
GB1117009A
Cited
US3503787A
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US3912461A
Cited
US3793175A
Cited
US3798145A
Cited
US4098956A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-06-21 | 1985-12-21 | 1986-06-22 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-06-21 | 1989-12-21 | 1990-06-22 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-06-21 | 1993-12-21 | 1994-06-22 | $7700.00 | Window Closed / Lapsed |