US3656995A
Expired / Lapsed
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Chemical vapor deposition coatings on titanium
Assignee: Texas Instruments Inc
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Filing: 1969-05-02
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Granted: 1972-04-18
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Expires: 1989-05-02
Abstract
Abstract A process for coating titanium-containing substrates with a dense, adherent, chemically vapor deposited coating by initially effecting a protective, adhesion-promoting, intermediate layer on the titanium surface and subsequently depositing from the vapor phase a metal nitride, carbide, or carbonitride coating on the intermediate film. For example, a titanium article may be initially nitrided to provide a titanium carbonitride protective layer and titanium nitride, titanium carbide, or titanium carbonitride may subsequently be deposited from the vapor phase onto this film to provide a dense, adherent, protective coating on the titanium article. The barrier layer serves to promote adhesion between the titanium substrate and the final overlay and to prevent reaction between the substrate and such a reaction ingredient as titanium tetrachloride, which is preferred constituent for supplying titanium in the titanium carbide, nitride, or carbonitride final coating.
Inventors
- 👤 Carl D Reedy Jr
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 18:04
CPC Classifications
C; C23; C23C; C23C26/00; C23C16/00; C23C16/02; C23C16/0209; C23C16/0218; C23C16/0272; C23C16/22; C23C16/30; C23C16/36
Claims Analysis
Total Claims: 36
Claim 1
Independent Claim
33 words
The process of claim 1, wheRein said barrier layer is formed by exposing said substrate to a nitrogen atmosphere at elevated temperatures to form a diffused layer of titanium nitride on said substrate.
Claim 2
Dependent Claim
13 words
The process of claim 2, wherein hydrogen is introduced into said nitrogen atmosphere.
Claim 3
Dependent Claim
32 words
The process of claim 2, wherein said exposing is effected at a temperature within the range of from about 750* C to about 1, 100* C for about 1/2 to 2 hours.
Claim 4
Dependent Claim
37 words
The process of claim 1, wherein: a. said carbon is introduced into said gaseous stream in the form of at least one hydrocarbon, and b. said metal is introduced into said gaseous stream as a metal halide.
Claim 5
Dependent Claim
72 words
The process of claim 1, wherein: a. said barrier layer is formed by exposing said substrate to a nitrogen atmosphere at a temperature within the range of from about 800* C to about 1,000* C for about 1/2 to 1 1/2 hours; and b. said gaseous stream contains hydrogen, said nitrogen, and said carbon in the form of at least one hydrocarbon and said metal in the form of a metal halide.
Claim 6
Dependent Claim
21 words
The process of claim 6, wherein said at least one hydrocarbon is natural gas and said metal halide is titanium tetrachloride.
Claim 7
Dependent Claim
121 words
A process for coating a titanium-containing substrate with a solid solution layer of titanium carbonitride which comprises: a. cleaning said substrate; b. exposing said substrate to a nitrogen and hydrogen atmosphere at a temperature within the range of from about 850* C to about 950* C for about 1/2 to 1 hour to form a titanium nitride diffused layer on the substrate; c. introducing titanium tetrachloride into the nitrogen and hydrogen atmosphere to form an additional layer of titanium nitride on the substrate; and then d. introducing natural gas with said atmosphere at a temperature within the range of from about 750* C to about 1,200* C for a time sufficient to form said titanium carbonitride layer on said titanium nitride.
Claim 8
Dependent Claim
13 words
The process of claim 8, wherein said titanium-containing substrate is essentially pure titanium.
Claim 9
Dependent Claim
13 words
The process of claim 8, wherein said titanium-containing substrate is a titanium alloy.
Claim 10
Dependent Claim
41 words
The process of claim 1, wherein: a. said nitrogen and said carbon are introduced into said gaseous stream in the form of at least one nitrogen-containing hydrocarbon, and b. said metal is introduced into said gaseous stream as a metal halide.
Claim 11
Dependent Claim
22 words
The process of claim 11, wherein said at least one nitrogen-containing hydrocarbon is ethylene diamine and said metal halide is titanium tetrachloride.
Claim 12
Dependent Claim
21 words
The process of claim 11, wherein said at least one nitrogen-containing hydrocarbon is trimethylamine and said metal halide is titanium tetrachloride.
Claim 13
Dependent Claim
21 words
The process of claim 11, wherein said at least one nitrogen-containing hydrocarbon is pyridine and said metal halide is titanium tetrachloride.
Claim 14
Dependent Claim
73 words
The process of claim 1, wherein: a. said barrier layer is formed by exposing said substrate to a nitrogen atmosphere at a temperature within the range of from about 800* C to about 1,000* C for about 1/2 to 1 1/2 hours; and b. said gaseous stream contains hydrogen, said nitrogen, and said carbon in the form of at least one nitrogen-containing hydrocarbon and said metal in the form of a metal halide.
Claim 15
Dependent Claim
113 words
A process for coating a titanium-containing substrate with a solid solution layer of titanium carbonitride which comprises: a. exposing said substrate to a nitrogen atmosphere at a temperature within the range of from about 850* C to about 950* C for about 1/2 to 1 hour to form a titanium nitride diffused layer on the substrate; and b. contacting said substrate with a gaseous stream containing hydrogen, titanium tetrachloride, and at least one nitrogen-containing hydrocarbon selected form the group ethylene diamine, trimethylAmine, and pyridine, at a temperature within the range of from about 500* C to about 1,200* C for a time sufficient to form said titanium carbonitride layer on said nitride film.
Claim 16
Dependent Claim
13 words
The process of claim 16, wherein said titanium-containing substrate is essentially pure titanium.
Claim 17
Dependent Claim
13 words
The process of claim 16, wherein said titanium-containing substrate is a titanium alloy.
Claim 18
Dependent Claim
39 words
The process of claim 1, wherein said carbon, nitrogen, and metal are constituents of a vaporous, hydrogen-containing organic compound capable of being decomposed to yield said carbon, nitrogen, and metal in the reactive state to form said metal-carbon-nitrogen compound.
Claim 19
Dependent Claim
32 words
The process of claim 19, wherein said barrier layer is formed by exposing said substrate to a nitrogen atmosphere at elevated temperatures to form a film of titanium nitride on said substrate.
Claim 20
Dependent Claim
22 words
The process of claim 20, wherein said organic compound is dispersed within a carrier gas selected from nitrogen, hydrogen, and mixtures thereof.
Claim 21
Dependent Claim
77 words
The process of claim 20, wherein said organic compound has the generic formula ((R)2N)n Me wherein: Me is a metal of the group boron, silicon, and the transition metals of Groups IVB, VB, and VIB of the Periodic Chart; n is a valence of Me; and R is selected from hydrogen and hydrocarbon radicals each having from one to about 18 carbon atoms, provided at least one R group is at least one of said hydrocarbon radicals.
Claim 22
Dependent Claim
145 words
The process of claim 1, wherein: a. said barrier layer is formed by exposing said substrate to a nitrogen atmosphere at a temperature within the range of from about 800* C to about 1,000* C for about 1/2 to 1 1/2 hours; and b. said carbon, nitrogen, and metal are constituents of a vaporous, hydrogen-containing organic compound having the generic formula ((R)2N)n Me wherein: Me is a metal of the group boron, silicon, and the transition metals of Groups IVB, VB, and VIB of the Periodic Chart; n is a valence of Me; and R is selected from hydrogen and hydrocarbon radicals each having from one to about 18 carbon atoms, provided at least one R group is at least one of said hydrocarbon radicals, said compound being capable of decomposition at temperatures within the range of from about 400* C to about 1,200* C.
Claim 23
Dependent Claim
23 words
The process of claim 23, wherein said compound is dispersed within a carrier gas selected from the group nitrogen, hydrogen, and mixtures thereof.
Claim 24
Dependent Claim
13 words
The process of claim 24, wherein said titanium-containing substrate is essentially pure titanium.
Claim 25
Dependent Claim
13 words
The process of claim 24, wherein said titanium-containing substrate is a titanium alloy.
Claim 26
Dependent Claim
13 words
The process of claim 24, wherein said organic compound is tetrakis (dimethylamino) titanium.
Claim 27
Dependent Claim
13 words
The process of claim 24, wherein said organic compound is tetrakis (diethylamino) titanium.
Claim 28
Dependent Claim
13 words
The process of claim 24, wherein said organic compound is tetrakis (diphenylamino) titanium.
Claim 29
Dependent Claim
78 words
The process of claim 1, wherein: a. said metal is in the form of a metal halide having the general formula Me(x)n and wherein x is a halogen, n is a valence of Me, and Me is a metal of the group boron, silicon, and the transition metals of Groups IVB, VB, and VIB of the Periodic Chart; and b. said carbon and said nitrogen are in the form of at least one of the following reactant compositions:
Claim 30
Dependent Claim
33 words
The process of claim 30, wherein said barrier layer is formed by exposing said substrate to a nitrogen atmosphere at elevated temperatures to form a diffused layer of titanium nitride on said substrate.
Claim 31
Dependent Claim
15 words
The process of claim 31, wherein said compound is dispersed within a nitrogen carrier gas.
Claim 32
Dependent Claim
108 words
The process of claim 1, wherein: a. said barrier layer is formed by exposing said substrate to a nitrogen atmosphere at a temperature within the range of from about 800* C to about 1,000* C for about 1/2 to 1 1/2 hours; b. said metal is in the form of a metal halide having the general formula Me(x)n and wherein x is a halogen, n is a valence of Me, and Me is a metal of the group boron, silicon, and the transition metals of Groups IVB, VB, and VIB of the Periodic Chart; and c. said carbon and said nitrogen are constituents of reactant compounds selected from:
Claim 33
Dependent Claim
13 words
The process of claim 33, wherein said titanium-containing substrate is essentially pure titanium.
Claim 34
Dependent Claim
13 words
The process of claim 33, wherein said titanium-containing substrate is a titanium alloy.
Claim 35
Dependent Claim
31 words
The process of claim 33, wherein: a. said metal halide is titanium tetrachloride, said carbon-containing compound is 1,1-dimethylhydrazine; and b. nitrogen is added to said gaseous stream as a carrier gas.
Claim 36
Dependent Claim
30 words
The process of claim 33, wherein: a. said metal halide is titanium tetrachloride, said reactant compounds are hydrazine and natural gas; and b. nitrogen is added to said gaseous stream.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1975-04-18 | 1975-10-18 | 1976-04-18 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1979-04-18 | 1979-10-18 | 1980-04-18 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1983-04-18 | 1983-10-18 | 1984-04-18 | $7700.00 | Window Closed / Lapsed |