[특허]Methods of producing continuous boron carbide fibers

ADVANCED CERAMIC FIBERS, LLC

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Methods of producing continuous boron carbide fibers

특허상세정보
국가/구분	United States(US) Patent 등록
국제특허분류(IPC7판)	C04B-035/00 B01J-027/22 B32B-009/04 C01B-031/36 D01F-009/08 C04B-035/10 C04B-035/563 C04B-035/565 C04B-035/58 C04B-035/583 C04B-035/622 C04B-035/628 C04B-035/80 C22C-049/14 C09K-005/14
출원번호	US-0215967 (2011-08-23)
등록번호	US-9199227 (2015-12-01)
발명자 / 주소	Garnier, John E. Griffith, George W.
출원인 / 주소	ADVANCED CERAMIC FIBERS, LLC
대리인 / 주소	Workman Nydegger
인용정보	피인용 횟수 : 2 인용 특허 : 57

초록

Methods of producing continuous boron carbide fibers. The method comprises reacting a continuous carbon fiber material and a boron oxide gas within a temperature range of from approximately 1400° C. to approximately 2200° C. Continuous boron carbide fibers, continuous fibers comprising boron carbide, and articles including at least a boron carbide coating are also disclosed.

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1. A continuous method of producing continuous boron carbide fibers from a continuous carbon fiber material, comprising: heating a solid boron source to form a boron oxide gas in a reaction zone of a continuous throughput tube furnace having a single reaction zone in which both (i) the boron oxide gas is formed and (ii) the boron oxide gas is reacted with the continuous carbon fiber material;continuously drawing the continuous carbon fiber material through the continuous throughput tube furnace so that only a portion of the continuous carbon fiber material being converted to boron carbide is disposed within the reaction zone of the continuous throughput tube furnace at any given time, that portion of the continuous carbon fiber material disposed within the reaction zone reacting with the boron oxide gas in the reaction zone of the tube furnace to convert at least a portion of the carbon of the continuous carbon fiber material to boron carbide fiber as the carbon reacts with the boron oxide gas; andthe reaction zone being maintained at a temperature within a range of from approximately 1400° C. to approximately 2200° C. 2. The method of claim 1, wherein the formed boron oxide gas is selected from the group consisting of diboron trioxide, diboron dioxide, boron monoxide, and combinations thereof. 3. The method of claim 1, wherein heating a solid boron source to form a boron oxide gas and reacting the boron oxide gas with a continuous carbon fiber material comprises heating a solid diboron trioxide to produce gaseous boron species and reacting the gaseous boron species with the continuous carbon fiber material. 4. The method of claim 1, wherein the continuous carbon fiber material comprises a material selected from the group consisting of a continuous pitch-based resin carbon fiber, a continuous polyacrylonitrile-based carbon fiber, a carbon nanotube, and combinations thereof. 5. The method of claim 1, wherein the reaction zone is maintained at a temperature within a range of from approximately 1600° C. to approximately 1800° C. 6. The method of claim 1, wherein the formed continuous boron carbide fibers have a stoichiometry of from B4C to B10.4C. 7. The method of claim 6, wherein the formed continuous boron carbide fibers have a diameter of from approximately 2 μm to approximately 20 μm. 8. The method of claim 1, wherein the boron oxide gas is formed at a ratio greater than approximately 3 moles of carbon fiber material per mole of boron oxide gas. 9. The method of claim 1, wherein heating a solid boron source to form a boron oxide gas comprises heating solid boron trioxide. 10. The method of claim 1, wherein heating a solid boron source to form a boron oxide gas comprises heating a composition consisting of the solid boron source, the composition consisting of boron and oxygen. 11. The method of claim 1, wherein only a portion of the carbon of the continuous carbon fiber feedstock material is converted to boron carbide so as to form a conversion layer of boron carbide in fiber form on a continuous carbon fiber core. 12. The method of claim 1, wherein substantially all of the carbon of the continuous carbon fiber material is converted to boron carbide so as to form a homogeneous, continuous boron carbide fiber material. 13. The method of claim 12, wherein the continuous boron carbide fiber material consists essentially of boron carbide, so as to be substantially free of unreacted carbon. 14. The method of claim 1, further comprising maintaining a tensile pull force on the carbon fiber material as it is drawn through the continuous throughput tube furnace. 15. The method of claim 1, wherein the pressure within the continuous throughput tube furnace is maintained at a pressure of about 1 atm. 16. The method of claim 1, wherein the continuous carbon fiber material is in the form of an elongate, continuous, generally straight carbon fiber. 17. A continuous method of producing continuous boron carbide fibers from a continuous carbon fiber feedstock material that is continuously fed through a continuous throughput tube furnace, the method comprising: heating solid boron oxide in a reaction zone of the continuous throughput tube furnace having a single reaction zone to a first temperature greater than approximately 600° C. to form a boron oxide gas;increasing the temperature of the single reaction zone to a second temperature different from the first temperature, the second temperature being between approximately 1600° C. and approximately 2200° C.; andcontinuously drawing the continuous carbon fiber feedstock material through the single reaction zone in which the boron oxide gas was formed, only a portion of the continuous carbon fiber feedstock material being disposed within the single reaction zone at a given time, the boron oxide gas reacting with that portion of the continuous carbon fiber feedstock material disposed within the single reaction zone to convert at least a portion of the carbon of the continuous carbon fiber feedstock material to boron carbidefurnace to convert at least a portion of the carbon of the continuous carbon fiber material to boron carbide fiber as the carbon reacts with the boron oxide gas. 18. The method of claim 17, wherein heating to a first temperature of greater than approximately 600° C. comprises forming at least one of diboron trioxide, diboron dioxide, or boron monoxide. 19. The method of claim 18, wherein drawing a continuous carbon fiber feedstock material through the reaction zone comprises reacting the continuous carbon fiber feedstock material with the at least one of diboron trioxide, diboron dioxide, or boron monoxide. 20. The method of claim 19, wherein drawing a continuous carbon fiber feedstock material through the reaction zone comprises reacting at least a portion of the continuous carbon fiber feedstock material with the at least one of diboron trioxide, diboron dioxide, or boron monoxide to convert a portion of the carbon of the continuous carbon fiber material so as to form a boron carbide fiber conversion layer on a carbon fiber core. 21. The method of claim 19, wherein drawing a continuous carbon fiber material through the reaction zone comprises reacting substantially all of the continuous carbon fiber feedstock material with the at least one of diboron trioxide, diboron dioxide, or boron monoxide to convert the carbon fiber feedstock material to the continuous boron carbide fiber material. 22. A continuous method of producing continuous boron carbide fiber from a continuous carbon fiber feedstock material, the method comprising: heating a composition comprising a solid boron source to form a boron oxide gas, the composition consisting of boron and oxygen; andreacting the boron oxide gas with the continuous carbon fiber feedstock material within a temperature range of from approximately 1400° C. to approximately 2200° C. to convert at least an outer portion of carbon of the continuous carbon fiber feedstock material to boron carbide fiber as the carbon of the fiber reacts with the boron oxide gas;the reacting the boron oxide gas with the continuous carbon fiber feedstock material being achieved by continuously drawing the carbon fiber through a reaction zone of a continuous throughput tube furnace so that only a portion of the continuous carbon fiber feedstock material is within the reaction zone of the continuous throughput tube furnace at any given time, that portion of the continuous carbon fiber feedstock material that is within the reaction zone at a given time reacting with the boron oxide gas, converting the carbon fiber feedstock material to the boron carbide fiber. 23. The method of claim 22, wherein heating a composition comprising a solid boron source to form a boron oxide gas comprises heating the composition to a temperature greater than approximately 600° C. and less than approximately 1650° C. to form a boron oxide gas comprising a greater gaseous molar concentration of diboron trioxide relative to a gaseous molar concentration of diboron dioxide, and a greater gaseous molar concentration of diboron dioxide relative to a gaseous molar concentration of boron monoxide. 24. The method of claim 22, wherein heating a composition comprising a solid boron source to form a boron oxide gas comprises heating the composition to a temperature between approximately 1650° C. and approximately 1750° C. to form a boron oxide gas comprising a greater gaseous molar concentration of diboron dioxide relative to a gaseous molar concentration of boron monoxide, and a greater gaseous molar concentration of boron monoxide relative to a gaseous molar concentration of diboron trioxide. 25. The method of claim 22, wherein heating a composition comprising a solid boron source to form a boron oxide gas comprises heating the composition to a temperature between approximately 1750° C. and approximately 2200° C. to form a boron oxide gas comprising a greater gaseous molar concentration of boron dioxide relative to a gaseous molar concentration of diboron dioxide, and a greater gaseous molar concentration of diboron dioxide relative to a gaseous molar concentration of diboron trioxide. 26. A continuous method of converting a continuous, elongate carbon fiber material into a continuous boron carbide fiber material, the method comprising: providing a boron oxide gas within a reaction zone of a continuous throughput tube furnace;continuously drawing the continuous carbon fiber material through the continuous throughput tube furnace so that only a portion of the continuous, elongate carbon fiber material is disposed within the reaction zone of the continuous throughput tube furnace at any given time, that portion of the continuous carbon fiber disposed within the reaction zone at a given time reacting with the boron oxide gas in the reaction zone of the tube furnace to convert at least an outside portion of the carbon of the continuous carbon fiber material to boron carbide fiber as the carbon reacts with the boron oxide gas;the reaction zone being maintained at a temperature within a range of from approximately 1400° C. to approximately 2200° C.;the reaction zone being maintained at a pressure of about 1 atm;wherein the method converts at least about 99.8% of the carbon of the continuous carbon fiber material into the elongate, continuous boron carbide fiber within a reaction time of less than about 10 minutes. 27. The method of claim 26, wherein the elongate, continuous boron carbide fiber produced by the method comprises at least 99% B4C. 28. The method of claim 26, wherein the continuous carbon fiber material resides within the reaction zone for a period of time of less than 10 minutes such that only an outer portion of the carbon fiber is converted to boron carbide fiber, producing a fiber having a boron carbide conversion layer disposed about a carbon fiber core.

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