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US4874642A
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Method for depositing a hard, fine-grained, non-columnar alloy of tungsten and carbon on a substrate
Assignee: Air Products and Chemicals Inc
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Filing: 1987-09-03
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Granted: 1989-10-17
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Expires: 2007-09-03
Abstract
Abstract Extremely hard, fine grained tungsten/carbon alloys are described which are produced by thermochemical deposition. The alloys consist primarily of a mixture of a substantially pure tungsten phase and at least one carbide phase wherein the carbide phase consists of W2C or W3C or a mixture of W2C and W3C. The disclosed tungsten/carbon alloys are free of columnar grains and consist essentially of extremely fine, equiaxial crystals. Also disclosed is a method of producing the disclosed material.
Inventors
- 👤 Diwaker Garg
- 👤 Beth A. Klucher
- 👤 Paul N. Dyer
- 👤 Richard W. Kidd
- 👤 Christopher Ceccarelli
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-07 19:57
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/06; C23C16/08; C23C16/22; C23C16/30; C23C16/32
Claims Analysis
Total Claims: 32
Claim 1
Independent Claim
208 words
A method for depositing a hard, fine-grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is selected from the group consisting of (1) W 2 C, (2) W 3 C, and (3) a mixture of W 2 C+W 3 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound, and (3) hydrogen; controlling the ratio of said tungsten hexafluoride to said oxygen- and hydrogen-containing organic compound within said reactor so that the W/C atomic ratio is within the range of about 1 to about 6; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the total pressure within the range of about 1 Torr. to about 1,000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 2 C, W and W 3 C, or W and W 2 C and W 3 C.
Claim 2
Independent Claim
208 words
A method for depositing a hard, fine-grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is selected from the group consisting of (1) W 2 C, (2) W 3 C, and (3) a mixture of W 2 C+W 3 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound, and (3) hydrogen; controlling the ratio of said tungsten hexafluoride to said oxygen- and hydrogen-containing organic compound within said reactor so that the W/C atomic ratio is within the range of about 1 to about 6; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the total pressure within the range of about 1 Torr. to about 1,000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 2 C, W and W 3 C, or W and W 2 C and W 3 C.
Claim 3
Dependent Claim
41 words
A method according to claim 1 wherein said oxygen- and hydrogen-containing organic compound is selected from the group consisting of C 1 -C 4 alcohols and aldehydes, C 2 -C 4 ethers, epoxides and ketenes and C 3 -C 4 ketones.
Claim 4
Dependent Claim
16 words
A method according to claim 1 wherein said oxygen- and hydrogen-containing organic compound is dimethyl ether.
Claim 5
Dependent Claim
24 words
A method to claim 1 wherein the ratio of H 2 to WF 6 is within the range of about 5 to about 10.
Claim 6
Dependent Claim
26 words
A method according to claim 1 wherein said reaction temperature is controlled so it is within the range of about 400° C. to about 485° C.
Claim 7
Dependent Claim
25 words
A method according to claim 1 wherein said reaction pressure is controlled so it is within the range of about 20 to about 100 Torr.
Claim 8
Dependent Claim
27 words
A method according to claim 1 wherein said mixture of process gases further includes an inert gas selected from the group consisting of argon, nitrogen and helium.
Claim 9
Independent Claim
180 words
A method for depositing a hard, fine-grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is W 2 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound containing from one to four carbon atoms, and (3) hydrogen; controlling the ratio of said tungsten halide to said oxygen- and hydrogen-containing organic compound within said reactor so that the W/C atomic ratio is within the range of about 1 to about 3.5; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the reaction pressure so it is within the range of about 1 to 1000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 2 C.
Claim 10
Independent Claim
180 words
A method for depositing a hard, fine-grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is W 2 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound containing from one to four carbon atoms, and (3) hydrogen; controlling the ratio of said tungsten halide to said oxygen- and hydrogen-containing organic compound within said reactor so that the W/C atomic ratio is within the range of about 1 to about 3.5; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the reaction pressure so it is within the range of about 1 to 1000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 2 C.
Claim 11
Dependent Claim
41 words
A method according to claim 8 wherein said oxygen- and hydrogen-containing organic compound is selected from the group consisting of C 1 -C 4 alcohols and aldehydes, C 2 -C 4 ethers, epoxides and ketenes and C 3 -C 4 ketones.
Claim 12
Dependent Claim
16 words
A method according to claim 8 wherein said oxygen- and hydrogen-containing organic compound is dimethyl ether.
Claim 13
Dependent Claim
24 words
A method to claim 8 wherein the ratio of H 2 to WF 6 is within the range of about 5 to about 10.
Claim 14
Dependent Claim
26 words
A method according to claim 8 wherein said reaction temperature is controlled so it is within the range of about 400° C. to about 485° C.
Claim 15
Dependent Claim
25 words
A method according to claim 8 wherein said reaction pressure is controlled so it is within the range of about 20 to about 100 Torr.
Claim 16
Dependent Claim
27 words
A method according to claim 8 wherein said mixture of process gases further includes an inert gas selected from the group consisting of argon, nitrogen and helium.
Claim 17
Independent Claim
181 words
A method for depositing a hard, fine grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is W 3 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound containing from one to four carbon atoms, and (3) hydrogen; controlling the ratio of said tungsten halide to said oxygen- and hydrogen-containing organic compound within said reactor so that the W/C atomic ratio is within the range of about 2.5 to about 6; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the reaction pressure so it is within the range of about 1 to 1000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 3 C.
Claim 18
Independent Claim
181 words
A method for depositing a hard, fine grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is W 3 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound containing from one to four carbon atoms, and (3) hydrogen; controlling the ratio of said tungsten halide to said oxygen- and hydrogen-containing organic compound within said reactor so that the W/C atomic ratio is within the range of about 2.5 to about 6; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the reaction pressure so it is within the range of about 1 to 1000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 3 C.
Claim 19
Dependent Claim
41 words
A method according to claim 15 wherein said oxygen- and hydrogen-containing organic compound is selected from the group consisting of C 1 -C 4 alcohols and aldehydes, C 2 -C 4 ethers, epoxides and ketenes and C 3 -C 4 ketones.
Claim 20
Dependent Claim
16 words
A method according to claim 15 wherein said oxygen- and hydrogen-containing organic compound is dimethyl ether.
Claim 21
Dependent Claim
24 words
A method to claim 15 wherein the ratio of H 2 to WF 6 is within the range of about 5 to about 10.
Claim 22
Dependent Claim
26 words
A method according to claim 15 wherein said reaction temperature is controlled so it is within the range of about 400° C. to about 485° C.
Claim 23
Dependent Claim
25 words
A method according to claim 15 wherein said reaction pressure is controlled so it is within the range of about 20 to about 100 Torr.
Claim 24
Dependent Claim
27 words
A method according to claim 15 wherein said mixture of process gases further includes an inert gas selected from the group consisting of argon, nitrogen and helium.
Claim 25
Independent Claim
188 words
A method for depositing a hard, fine grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is a mixture of W 2 C+W 3 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound containing from one to four carbon atoms, and (3) hydrogen; controlling the ratio of said tungsten halide to said oxygen- and hydrogen-containing organic compound within said reactor so said the W/C atomic ratio is within the range of about 2.0 to about 4.5; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the reaction pressure so it is within the range of about 1 to 1000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 2 C+W 3 C.
Claim 26
Independent Claim
188 words
A method for depositing a hard, fine grained, non-columnar alloy of tungsten and carbon having a substantially lamellar or layered microstructure on a substrate, said alloy consisting essentially of a mixture of a tungsten phase and a carbide phase wherein said carbide phase is a mixture of W 2 C+W 3 C, said method comprising the steps of: providing, in a chemical vapor deposition reactor, a mixture of process gases comprised essentially of (1) tungsten hexafluoride, (2) a volatile oxygen- and hydrogen-containing organic compound containing from one to four carbon atoms, and (3) hydrogen; controlling the ratio of said tungsten halide to said oxygen- and hydrogen-containing organic compound within said reactor so said the W/C atomic ratio is within the range of about 2.0 to about 4.5; controlling the reaction temperature so it is within the range of about 350° to about 550° C.; controlling the reaction pressure so it is within the range of about 1 to 1000 Torr.; and controlling the ratio of H 2 to WF 6 within the range of about 4 to about 20 to produce W and W 2 C+W 3 C.
Claim 27
Dependent Claim
41 words
A method according to claim 22 wherein said oxygen- and hydrogen-containing organic compound is selected from the group consisting of C 1 -C 4 alcohols and aldehydes, C 2 -C 4 ethers, epoxides and ketenes and C 3 -C 4 ketones.
Claim 28
Dependent Claim
16 words
A method according to claim 22 wherein said oxygen- and hydrogen-containing organic compound is dimethyl ether.
Claim 29
Dependent Claim
24 words
A method to claim 22 wherein the ratio of H 2 to WF 6 is within the range of about 5 to about 10.
Claim 30
Dependent Claim
26 words
A method according to claim 22 wherein said reaction temperature is controlled so it is within the range of about 400° C. to about 485° C.
Claim 31
Dependent Claim
25 words
A method according to claim 22 wherein said reaction pressure is controlled so it is within the range of about 20 to about 100 Torr.
Claim 32
Dependent Claim
27 words
A method according to claim 22 wherein said mixture of process gases further includes an inert gas selected from the group consisting of argon, nitrogen and helium.
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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) | 1992-10-16 | 1993-04-17 | 1993-10-17 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1996-10-16 | 1997-04-17 | 1997-10-17 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2000-10-16 | 2001-04-17 | 2001-10-17 | $7700.00 | Window Closed / Lapsed |