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Co-pyrolysis process for forming carbonized composite bodies

Assignee: United States Department of the Air Force
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Filing: 1986-05-06
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Granted: 1988-02-02
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Expires: 2006-05-06
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Abstract

Abstract A co-pyrolysis process is disclosed for forming carbonized composite bodies in which co-pyrolysis of organic fibrous and matrix components is effected during initial pyrolysis. Improved interfacial bonding of composite bodies is achieved by combining fibrous precursors, or reinforcements with a controlled pre-shrink state, with an appropriate matrix to insure shrinkage matching during processing. Processing involves the heat treatment of an organic fibrous component, impregnation of the heat treated fibrous component with a resinous binder, forming a layup of the resin impregnated fibrous component, subjecting the layup to molding and curing cycles to form a laminate, pyrolysis of the laminate, and post-pyrolysis heat treatment of the pyrolized laminate.

Inventors

  • 👤 Robert E. Yeager
  • 👤 Earl L. Stone, III

Bibliographic Details

Application Number —
Jurisdiction US
Data Source google_patents
Last Synchronized 2026-11-09 07:20
CPC Classifications
C; C04; C04B; C04B35/00; C04B35/71; C04B35/78; C04B35/80; C04B35/83

Claims Analysis

Total Claims: 16
Claim 1
Independent Claim 181 words
A method for forming structural carbon-carbon composites, which comprises: pretreating an organic fibrous precursor by exposure for about three hours to an oxidizing atmosphere maintained at a temperature range of 260°-315° C.; impregnating the fibrous precursor with a matrix-forming resinous binder admixed with a solvent material; composing an assemblage of the resinous binder impregnated fibrous precursor cut to form a composite layup of predetermined configuration; subjecting the composite layup to a curing temperature and molding pressure cycle of about 165° C. over a rise time of about one hour and a holding time of about one hour at a pressure range of 15-80 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a heating cycle of 72-336 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of heat treated laminate to ambient temperature.
Claim 2
Independent Claim 181 words
A method for forming structural carbon-carbon composites, which comprises: pretreating an organic fibrous precursor by exposure for about three hours to an oxidizing atmosphere maintained at a temperature range of 260°-315° C.; impregnating the fibrous precursor with a matrix-forming resinous binder admixed with a solvent material; composing an assemblage of the resinous binder impregnated fibrous precursor cut to form a composite layup of predetermined configuration; subjecting the composite layup to a curing temperature and molding pressure cycle of about 165° C. over a rise time of about one hour and a holding time of about one hour at a pressure range of 15-80 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a heating cycle of 72-336 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of heat treated laminate to ambient temperature.
Claim 3
Dependent Claim 22 words
The method as recited in claim 1, wherein the organic fibrous precursor is selected from the group consisting of polyacrylonitrile, and phenolic.
Claim 4
Dependent Claim 25 words
The method as recited in claim 1, wherein the resinous binder is selected from the group consisting of polyphenylene resin, phenolic resin and furan resin.
Claim 5
Dependent Claim 24 words
The method as recited in claim 1, wherein the solvent material is selected from the group consisting of isopropyl alcohol and methyl ethyl ketone.
Claim 6
Independent Claim 189 words
A method for forming structural carbon-carbon composites, which comprises: pretreating woven cloth of organic fibrous material by exposure for about three hours to an oxidizing atmosphere maintained at a temperature range of 260°-315° C.; impregnating the fibrous material with a matrix-forming resinous binder admixed with a solvent material; composing one upon another a plurality of plies of the resinous binder impregnated fibrous material cut to form a composite layup of predetermined configuration; subjecting the composite layup to a curing temperature and molding pressure cycle of about 165° C. over a rise time of about one hour and a holding time of about one hour at a pressure range of 15-80 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a heating cycle of 72-336 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of the heat treated laminate to ambient temperature.
Claim 7
Independent Claim 189 words
A method for forming structural carbon-carbon composites, which comprises: pretreating woven cloth of organic fibrous material by exposure for about three hours to an oxidizing atmosphere maintained at a temperature range of 260°-315° C.; impregnating the fibrous material with a matrix-forming resinous binder admixed with a solvent material; composing one upon another a plurality of plies of the resinous binder impregnated fibrous material cut to form a composite layup of predetermined configuration; subjecting the composite layup to a curing temperature and molding pressure cycle of about 165° C. over a rise time of about one hour and a holding time of about one hour at a pressure range of 15-80 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a heating cycle of 72-336 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of the heat treated laminate to ambient temperature.
Claim 8
Dependent Claim 19 words
The method as recited in claim 5, wherein the organic fibrous material is preferably pitch fibers woven into cloth.
Claim 9
Independent Claim 170 words
A method for forming structural carbon-carbon composites, which comprises: pretreating organic fibrous material by exposure for about three hours to an oxidizing atmosphere maintained at a temperature of 260°-315° C.; composing a layered mat of the fibrous material shaped to form a composite layup of predetermined configuration; impregnating the composite layup with a matrix-forming resinous binder admixed with a solvent material; subjecting the composite layup to a curing temperature and molding pressure cycle of about 180° C. over a rise time range of 40-140 minutes at a pressure range of 200-1000 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a healing cycle of 72-382 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of the heat treated laminate to ambient temperature.
Claim 10
Independent Claim 170 words
A method for forming structural carbon-carbon composites, which comprises: pretreating organic fibrous material by exposure for about three hours to an oxidizing atmosphere maintained at a temperature of 260°-315° C.; composing a layered mat of the fibrous material shaped to form a composite layup of predetermined configuration; impregnating the composite layup with a matrix-forming resinous binder admixed with a solvent material; subjecting the composite layup to a curing temperature and molding pressure cycle of about 180° C. over a rise time range of 40-140 minutes at a pressure range of 200-1000 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a healing cycle of 72-382 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of the heat treated laminate to ambient temperature.
Claim 11
Dependent Claim 29 words
The method as recited in claim 7, wherein the layered mat consists of organic fibrous material chopped in one-half inch lengths and fluffed in a blender at high speed.
Claim 12
Independent Claim 192 words
A method for forming structural carbon-carbon composites, which comprises: pretreating elongated bodies of unidirectional organic fibrous material by exposure for about three hours to an oxidizing atmosphere maintained at a temperature range of 260°-315° C.; impregnating the fibrous material with a matrix-forming resinous binder admixed with a solvent material; composing one upon another a plurality of plies of the resinous binder impregnated, parallel oriented fibrous material cut to form a composite layup of predetermined configuration; subjecting the composite layup to a curing temperature and molding pressure cycle of about 165° C. over a rise time of about one hour and a holding time of about one hour at a pressure range of 15-80 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a heating cycle of 72 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of the heat treated laminate to ambient temperature.
Claim 13
Independent Claim 192 words
A method for forming structural carbon-carbon composites, which comprises: pretreating elongated bodies of unidirectional organic fibrous material by exposure for about three hours to an oxidizing atmosphere maintained at a temperature range of 260°-315° C.; impregnating the fibrous material with a matrix-forming resinous binder admixed with a solvent material; composing one upon another a plurality of plies of the resinous binder impregnated, parallel oriented fibrous material cut to form a composite layup of predetermined configuration; subjecting the composite layup to a curing temperature and molding pressure cycle of about 165° C. over a rise time of about one hour and a holding time of about one hour at a pressure range of 15-80 psi to form a cured laminate; pyrolyzing the cured laminate in a pyrolization furnace by gradually raising the furnace temperature to about 815° C. over a heating cycle of 72 hours to form a pyrolyzed laminate; and heat treating the pyrolyzed laminate over a heating cycle of about 14 hours to a temperature of about 2000° C. and maintaining such temperature for about two additional hours followed by a gradual cooling of the heat treated laminate to ambient temperature.
Claim 14
Dependent Claim 23 words
The method as recited in claim 9, wherein the elongated bodies of unidirectional organic fibrous material are wound under tension around a drum.
Claim 15
Dependent Claim 28 words
The method as recited in claim 9, wherein the elongated bodies of unidirectional organic fibrous material are wound under tension in successive layers onto a two bladed wheel.
Claim 16
Dependent Claim 27 words
The method as recited in claim 9, wherein the elongated bodies of unidirectional organic fibrous material are impregnated in a vacuum chamber with the matrix-forming resinous binder.

References Cited (Backward Citations)

US2875503A Cited
US3552533A Cited
US3814642A Cited
US3700535A Cited
US3728423A Cited
US4237109A Cited
US4225569A Cited

USPTO Annuity & Maintenance Windows

Annuity Stage Window Opens Payment Deadline Surcharge Period Until Estimated Fee Status
3.5 Years (Year 4) 1991-02-01 1991-08-03 1992-02-02 $2000.00 Window Closed / Lapsed
7.5 Years (Year 8) 1995-02-01 1995-08-03 1996-02-02 $3760.00 Window Closed / Lapsed
11.5 Years (Year 12) 1999-02-01 1999-08-03 2000-02-02 $7700.00 Window Closed / Lapsed

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