US4343836A
Expired / Lapsed
US
⏱️ 0.0 years remaining
One-directional uniformly coated fibers, method of preparation, and uses therefor
Assignee: United States Department of Energy
•
Filing: 1979-07-26
•
Granted: 1982-08-10
•
Expires: 1999-07-26
Abstract
Abstract A problem addressed by this invention was how to obtain very long lengths of refractory metal-coated multifilamentary yarns having a uniform coating on the filaments which make up each yarn, the coating being uniform throughout the length of the yarn such that the coated yarns are suitable for being woven and are suitable for a variety of other uses. The solution is a continuous process which employs a chemical vapor deposition reaction at relatively low temperature and pressure and a separation of the gaseous reaction products from the coated yarn prior to allowing the coated yarn to cool.
Inventors
- 👤 Lawrence R. Newkirk
- 👤 Flavio Valencia
- 👤 Robert E. Riley
- 👤 Terry C. Wallace, Sr.
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-10-23 09:55
CPC Classifications
C; C23; C23C; C23C16/00; C23C16/44; C23C16/54; C23C16/545; C23C16/06; C23C16/08; C23C16/14
Claims Analysis
Total Claims: 13
Claim 1
Independent Claim
297 words
A method of coating long lengths of at least one multifilamentary yarn with a first metal selected from the group consisting of tantalum, niobium, tungsten, molybdenum, and rhenium, said multifilamentary yarn being made up of a bundle of individual filaments and being made of a material selected from the group consisting of graphite, carbon, ceramics, and metals, so as to produce yarn which is substantially uniformly coated on all filaments throughout each yarn bundle, said method comprising: (a) passing said at least one multifilamentary yarn continuously through a coating chamber into which a mixture of a gaseous halide of said first metal and H 2 gas is being continuously introduced and then passed along a line which is substantially parallel to said yarn, said coating chamber being heated to a chosen temperature which is sufficiently high to enable said halide of said first metal and said hydrogen to react to form said first metal, said chosen temperature being lower than about 1100° C. and said coating chamber being operated at a total pressure within the range from about 1 to about 300 torr, (b) allowing said gaseous halide of said first metal and said H 2 gas to react at said chosen temperature to form said first metal at the surfaces of said yarn filaments, thus producing at least first metal-coated fibers and an acid halide gas, (c) separating said first metal-coated fibers from said acid halide gas and from all reactants and other gaseous reaction products in said coating chamber by passing an inert gas purge over said first metal-coated fibers so as to minimize contact by back-diffusion of said first metal-coated fibers with said reactants, said acid halide gas and said other gaseous reaction products, and then (d) allowing said first metal-coated fibers to cool.
Claim 2
Independent Claim
297 words
A method of coating long lengths of at least one multifilamentary yarn with a first metal selected from the group consisting of tantalum, niobium, tungsten, molybdenum, and rhenium, said multifilamentary yarn being made up of a bundle of individual filaments and being made of a material selected from the group consisting of graphite, carbon, ceramics, and metals, so as to produce yarn which is substantially uniformly coated on all filaments throughout each yarn bundle, said method comprising: (a) passing said at least one multifilamentary yarn continuously through a coating chamber into which a mixture of a gaseous halide of said first metal and H 2 gas is being continuously introduced and then passed along a line which is substantially parallel to said yarn, said coating chamber being heated to a chosen temperature which is sufficiently high to enable said halide of said first metal and said hydrogen to react to form said first metal, said chosen temperature being lower than about 1100° C. and said coating chamber being operated at a total pressure within the range from about 1 to about 300 torr, (b) allowing said gaseous halide of said first metal and said H 2 gas to react at said chosen temperature to form said first metal at the surfaces of said yarn filaments, thus producing at least first metal-coated fibers and an acid halide gas, (c) separating said first metal-coated fibers from said acid halide gas and from all reactants and other gaseous reaction products in said coating chamber by passing an inert gas purge over said first metal-coated fibers so as to minimize contact by back-diffusion of said first metal-coated fibers with said reactants, said acid halide gas and said other gaseous reaction products, and then (d) allowing said first metal-coated fibers to cool.
Claim 3
Dependent Claim
25 words
A method according to claim 1 wherein said chosen temperature is a temperature higher than the temperature at which hydriding of said first metal occurs.
Claim 4
Dependent Claim
61 words
A method according to claim 2 wherein said first metal is selected from the group consisting of niobium and tantalum, wherein said acid halide gas is HCl, wherein said yarn fibers are made of a material selected from the group consisting of graphite and carbon, and wherein said coating temperature is within the range from about 900° to about 1100° C.
Claim 5
Dependent Claim
41 words
A method according to claim 3 wherein said gaseous halide of said first metal and said H 2 gas are passed into said coating chamber in a direction which is substantially opposite to the direction of motion of said yarn fibers.
Claim 6
Dependent Claim
122 words
A method according to claim 4 wherein the total pressure in said reaction chamber is within the range from about 1 torr to about 100 torr, wherein a first inert gas is passed continuously over said fibers before they are coated so as to minimize degradation of said fibers before they are coated, and wherein said first metal-coated fibers are separated from said HCl, from said H 2 , and from said gaseous halide of said first metal by passing a continuous flow of a second inert gas over said first metal-coated fibers so as to prevent hydride of said first metal from forming on said coated fibers and so as to minimize degradation of said first-metal coated fibers by said HCl.
Claim 7
Dependent Claim
82 words
A method according to claim 5 wherein said first metal is Ta, wherein said gaseous halide of said first metal is TaCl 5 , wherein said TaCl 5 is produced by passing a flow of Cl 2 gas over Ta chips at a temperature of about 425° C. and wherein said Cl 2 and said H 2 are used in relative amounts such that said flow ratio of H 2 :Cl 2 is within the range from about 15:1 to about 0.5:1.
Claim 8
Dependent Claim
29 words
A method according to claim 5 wherein Ta metal is deposited onto said yarn fibers in an amount less than about 370 weight percent Ta, thus producing Ta-coated fibers.
Claim 9
Dependent Claim
41 words
A method according to claim 5 wherein Ta is present on said Ta-coated yarn fibers in an amount less than the amount of Ta which would be required to convert essentially all of said yarn fibers to tantalum carbide upon heating.
Claim 10
Dependent Claim
69 words
A method of forming unidirectional billets comprising the method according to claim 8 and including also the step of hot pressing a multiplicity of Ta-coated unidirectional fibers at a temperature within the range from about 1900° to about 2400° C. and at a pressure within the range from about 20 to 40 Megapascals for a period of time sufficient to convert essentially all of said tantalum to tantalum carbide.
Claim 11
Dependent Claim
105 words
A method of producing a strengthened, heat-resistant, unidirectional fiber reinforced ceramic matrix composite, said method comprising the method according to claim 9 and including also the step of hot pressing said fiber at a temperature within the range from about 1900° to about 2400° C. and at a pressure within the range from about 20 to about 40 Megapascals for a period of time sufficient to convert essentially all of said Ta to tantalum carbide, thus producing a fiber-reinforced composite comprising an inner core of a material selected from the group consisting of carbon and graphite and a coating on said core of tantalum carbide.
Claim 12
Dependent Claim
23 words
A method according to claim 8 and including also the step of weaving said Ta-coated yarn fibers, thus forming a woven metal-coated fabric.
Claim 13
Dependent Claim
23 words
A method according to claim 11 and including also the step of hot pressing at least one layer of said woven metal-coated fabric.
References Cited (Backward Citations)
US2885310A
Cited
US3189563A
Cited
US3269802A
Cited
US3294880A
Cited
US3369920A
Cited
US3617359A
Cited
US3625755A
Cited
US3991248A
Cited
US4138512A
Cited
US4180428A
Cited
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1985-08-09 | 1986-02-08 | 1986-08-10 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1989-08-09 | 1990-02-08 | 1990-08-10 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 1993-08-09 | 1994-02-08 | 1994-08-10 | $7700.00 | Window Closed / Lapsed |