WO2005115945A1 - Method of producing carbon fiber reinforced ceramic matrix composites - Google Patents

Method of producing carbon fiber reinforced ceramic matrix composites Download PDF

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Publication number
WO2005115945A1
WO2005115945A1 PCT/KR2005/001581 KR2005001581W WO2005115945A1 WO 2005115945 A1 WO2005115945 A1 WO 2005115945A1 KR 2005001581 W KR2005001581 W KR 2005001581W WO 2005115945 A1 WO2005115945 A1 WO 2005115945A1
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Prior art keywords
fiber reinforced
carbon fiber
carbon
ceramic matrix
matrix composites
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PCT/KR2005/001581
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English (en)
French (fr)
Inventor
Dong Won Lim
Hong Sik Park
Dae Hyun Cho
Hyun Kyu Shin
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Dacc Co. Ltd.
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Priority to EP05746091A priority Critical patent/EP1758837A4/de
Priority to US11/579,445 priority patent/US20080143005A1/en
Priority to JP2007510630A priority patent/JP2007535461A/ja
Publication of WO2005115945A1 publication Critical patent/WO2005115945A1/en

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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
    • C04B38/0022—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors
    • C04B38/0032—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof obtained by a chemical conversion or reaction other than those relating to the setting or hardening of cement-like material or to the formation of a sol or a gel, e.g. by carbonising or pyrolysing preformed cellular materials based on polymers, organo-metallic or organo-silicon precursors one of the precursor materials being a monolithic element having approximately the same dimensions as the final article, e.g. a paper sheet which after carbonisation will react with silicon to form a porous silicon carbide porous body
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
    • C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
    • C—CHEMISTRY; METALLURGY
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/71—Ceramic products containing macroscopic reinforcing agents
    • C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
    • C04B35/80—Fibres, filaments, whiskers, platelets, or the like
    • C04B35/83—Carbon fibres in a carbon matrix
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
    • F16D69/02—Composition of linings ; Methods of manufacturing
    • F16D69/023—Composite materials containing carbon and carbon fibres or fibres made of carbonizable material
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
    • C04B2111/00362—Friction materials, e.g. used as brake linings, anti-skid materials
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/26—Corrosion of reinforcement resistance
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    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/20—Resistance against chemical, physical or biological attack
    • C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5208—Fibers
    • C04B2235/5216—Inorganic
    • C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248—Carbon, e.g. graphite
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
    • C04B2235/614—Gas infiltration of green bodies or pre-forms
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
    • F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
    • F16D2200/00—Materials; Production methods therefor
    • F16D2200/0034—Materials; Production methods therefor non-metallic
    • F16D2200/0039—Ceramics
    • F16D2200/0047—Ceramic composite, e.g. C/C composite infiltrated with Si or B, or ceramic matrix infiltrated with metal

Definitions

  • the present invention relates to a method of producing carbon fiber reinforced ceramic matrix composites, maintaining excellent mechanical strength at high temperature as well as having excellent properties in corrosion resistance, thermal resistance, friction and abrasion under a severe environment, such as heat, chemical erosion, etc.
  • Fiber reinforced ceramic matrix composites are lightweight materials having excellent mechanical and thermal properties at high temperature. With these properties, fiber reinforced ceramic matrix composites are applicable to friction and abrasion materials, such as brake disks, and pads for aircraft or ground transport means, and also to ultrahigh thermal resistant materials, such as ceramic engines, and rocket nozzle parts, which require mechanical strength, corrosion resistance, and thermal resistance. Fiber reinforced ceramic matrix composites have been studied to overcome the drawbacks to monolithic ceramics, such as brittle failure, or the like, and they can be produced by filling the pores of a preform made of carbon fibers or silicon carbide fibers with thermal resistant materials, such as pyrolytic carbon, silicon carbide, or boron nitride.
  • ceramic matrix composites are produced by injecting precursors in a gas state into a porous fiber preform having low density, and then pyrolizing it for the deposition of ceramic matrix-phase. Such a process is called chemical vapor infiltration, and the matrix-phase is infiltrated under a low temperature and pressure condition during this manufacturing process to solve the problem causing damage to fibers, which has been created when producing conventional ceramic matrix composites.
  • the carbon fiber reinforced ceramic matrix composite is produced by iterative impregnation of liquid organic binders or by changing the composition of the mixture, but it is impossible to prevent the reduction in mechanical properties caused by carbon fiber erosion and to improve friction and abrasion characteristics at high temperature.
  • the present invention is devised to solve the aforementioned problems, and it is an object of the invention to provide a method of producing carbon fiber reinforced ceramic matrix composites for improving thermal and mechanical properties of the carbon fiber reinforced ceramic matrix composites and for providing a solution to the problems due to its high manufacturing cost and processes as described above, by improving the method of producing starting material and a carbon fiber reinforced carbon composite, which are required for producing the carbon fiber reinforced ceramic matrix composites.
  • a method of producing carbon fiber reinforced ceramic matrix composites is provided by the inventors to simplify the manufacturing process by employing a carbon felt preform having a sandwich structure or a carbon fiber mixture as starting material, and to produce carbon fiber reinforced carbon composites having a uniform fiber protective layer with a rapid and low cost process by applying a rapid thermal gradient chemical vapor infiltration process as well as employing a liquid-phase silicon infiltration process.
  • a method of producing carbon fiber reinforced ceramic matrix (C/C-SiC) composites comprises the steps of: producing a carbon fiber reinforced resin composite that is molded with a mixture in which carbon fibers and polymer precursors containing carbon are mixed; producing a carbon fiber reinforced carbon composite by depositing pyrolytic carbon during a rapid thermal gradient chemical vapor infiltration process while increasing the deposition speed in a direction from the inside to the outside by performing a thermal treatment on said carbon fiber reinforced resin composite at high temperature; and infiltrating liquid-phase silicon into the pores of said carbon fiber reinforced carbon composite.
  • the mixture includes 10-60 wt % of the carbon fibers, and 30-60 wt % of the polymer precursors containing carbon.
  • the mixture includes less than 30 wt % silicon carbide powder, and less than 30 wt % carbon powder.
  • the carbon fiber reinforced resin composite is stacked with the mixture and carbon fabrics alternately.
  • the green body is formed with a first surface layer for preventing carbon fibers from reacting with silicon by means of the mixture that has been mixed during the mixing process, and the first surface layer is formed with a ceramic matrix layer including silicon carbide and silicon by chemically reacting with the liquid-phase silicon in the step of infiltrating the liquid-phase silicon.
  • the green body undergoes a thermal treatment in a range of 900-2,200 °C under inert gas atmosphere, and then a pyrolytic carbon matrix layer as a second surface layer is deposited on the first surface layer in a deposition step through the rapid thermal gradient chemical vapor infiltration process.
  • the deposition step by the rapid thermal gradient chemical vapor infiltration process is performed in a range of pyrolytic reaction temperatures 700-1,200 °C and reaction pressures 188-1,130 torr using hydro-carbon gas.
  • a deposition region is divided into a plurality of regions from the inside to the outside, and individual regions are deposited at different speeds one another in a deposition step through the rapid thermal gradient chemical vapor infiltration process.
  • the deposition region is deposited from the inside to the outside at a deposition speed in a range of 0.5-3.0 mm/hr.
  • the carbon fiber reinforced carbon composite has 1.0 - 1.7 g/cm apparent density, and 5-30 % of open pores that are used for infiltrating paths of the liquid-phase silicon.
  • the step of infiltrating liquid-phase silicon is performed by stacking the carbon fiber reinforced carbon composite on silicon powder, maintaining a pressure less than 100 torr within a reactor, and then heating it at the silicon melting point more than 1,410 °C, thereby infiltrating liquid-phase silicon into a preform while chemically reacting with a plurality of carbon layers.
  • a method of producing carbon fiber reinforced ceramic matrix composites is characterized in that the method comprises the steps of: producing a carbon felt preform; producing a carbon fiber reinforced carbon composite by depositing the carbon felt preform through a rapid thermal gradient chemical vapor infiltration process while increasing the deposition speed from the inside to the outside; and infiltrating liquid- phase silicon into the pores of the carbon fiber reinforced carbon composite.
  • the carbon felt preform is any one of carbon-based fibers, such as oxyphene, phene, rayon, pitch-based, etc.
  • the carbon felt preform has mat laminates with quasi- isotropic orientations, such as 0/+60/-60 0 , and it is reinforced with carbon fibers less than 10 mm in the Z-direction.
  • the carbon felt preform is deposited with a pyrolytic layer having 5-100 D in thickness by means of a deposition step through the rapid thermal gradient chemical vapor infiltration process.
  • carbon fibers are reinforced in the three X, Y and Z axes by impregnating liquid-phase silicon into the carbon fiber reinforced carbon composite in the step of infiltrating liquid-phase silicon.
  • the deposition step by the rapid thermal gradient chemical vapor infiltration process is performed in a range of pyrolytic reaction temperatures 700-1,200 °C and reaction pressures 188-1,130 torr using hydro-carbon gas.
  • a deposition region is divided into a plurality of regions from the inside to the outside, and individual regions are deposited at different speeds one another in a deposition step through the rapid thermal gradient chemical vapor infiltration process.
  • the deposition region is deposited from the inside to the outside at a deposition speed in a range of 0.5-3.0 mm/hr.
  • the carbon fiber reinforced carbon composite has 1.0 - 1.7 g/cm apparent density, and 5-30 % of open pores that are used for infiltrating paths of the liquid-phase silicon.
  • the step of infiltrating liquid-phase silicon is performed by stacking the carbon fiber reinforced carbon composite on silicon powder, maintaining a pressure less than 100 torr within a reactor, and then heating it at the silicon melting point more than 1,410 °C, thereby infiltrating liquid-phase silicon into the carbon felt preform while chemically reacting with a plurality of carbon layers.
  • the method of producing carbon fiber reinforced ceramic matrix composites according to the present invention as shown above has the effect of improving the properties of carbon fiber reinforced ceramic matrix composites, and it is possible to deposit a pyrolytic carbon layer at a deposition speed 5-10 times faster than other conventional chemical vapor infiltration processes, thereby providing a remarkably improved effect in terms of manufacturing process, time, and cost.
  • FIG. 1 is a block diagram illustrating a method of producing carbon fiber reinforced ceramic matrix composites using carbon fabrics and a carbon fiber mixture according to the present invention.
  • FIG. 2 is a block diagram illustrating a method of producing carbon fiber reinforced ceramic matrix composites using a carbon felt preform according to the present invention.
  • FIG. 3 is a microscopic structural view of a carbon fiber reinforced ceramic matrix composite according to the present invention.
  • FIG. 4 is a conceptual view illustrating a rapid thermal gradient chemical vapor infiltration process according to the present invention.
  • a carbon felt preform reinforced with carbon fibers in the direction of three X, Y, and Z axes may be employed, or a sandwich structure that is produced by stacking a mixture comprising carbon fibers 0.3-150 mm in length, polymer precursors containing carbon, silicon carbide powder, and graphite powder with carbon fabrics alternately may be applied, or a carbon fiber reinforced resin composite (CFRP) comprising only the aforementioned mixture may be employed.
  • CFRP carbon fiber reinforced resin composite
  • pyrolytic carbon is deposited on the produced starting material by means of a rapid thermal gradient chemical vapor infiltration process to produce a porous carbon fiber reinforced carbon composite, and then liquid-phase silicon is infiltrated into the pores of the carbon fiber reinforced carbon composite to produce a carbon fiber reinforced ceramic matrix composite.
  • the carbon fiber reinforced ceramic matrix composites has physical properties of more than 2.2 g/cm apparent density, less than 1% apparent porosity, more than 100 MPa bending strength, and more than 35 W/mk thermal conductivity.
  • the method of producing carbon fiber reinforced ceramic matrix composites can be divided into two types of processes based upon its starting material as shown in FIG. 1 and FIG. 2.
  • FIG. 1 illustrates a process for producing a carbon fiber reinforced resin composite using a mixture comprising carbon fibers cut in the size of 0.3-150 mm, polymer precursors containing carbon, silicon carbide powder, and graphite powder with carbon fabrics.
  • carbon fibers cut in the size of 0.3-150 mm is added to distilled water together with polymer precursors containing carbon, silicon carbide powder, graphite powder, and carbon fabrics to produce a uniform mixture through dispersion and mixing processes.
  • this mixture will be formed with a first surface layer comprising polymer precursors containing carbon, silicon carbide powder, and graphite powder on a carbon fiber surface, whose mixture ratio is 10-60 wt % carbon fibers, 30-60 wt % polymer precursors containing carbon.
  • silicon carbide powder and carbon powder will be included selectively. In other words, it may be composed of 0-30 wt % silicon carbide powder, and 0-30 wt % carbon powder (S101 and S102).
  • the mixture produced in this way is alternately stacked with carbon fabrics to form a green body having a sandwich structure (SI 10).
  • the carbon fabrics may be formed with plain, satin, and twill weaves.
  • the green body may be produced by stacking only the mixture, without stacking carbon fabrics alternately.
  • the produced green body is placed in a mold, and then heated and pressurized simultaneously in a range of 80-250 °C and l-20MPa to produce a carbon fiber reinforced resin composite.
  • the produced carbon fiber reinforced resin composite has physical properties of apparent density 1.2-1.6 g/cm , and apparent porosity 1-20% (SI 10, S120 and S130).
  • the produced carbon fiber reinforced resin composite is subjected to thermal treatment in a range of 700-2,200°C under inert gas atmosphere, and then a rapid thermal gradient chemical vapor infiltration process is performed to produce a carbon fiber reinforced carbon composite.
  • the rapid thermal gradient chemical vapor infiltration process is provided to produce a carbon fiber reinforced carbon composite having high density greater than 1.3 g/cm , and this rapid thermal gradient chemical vapor infiltration process performs a rapid deposition by dividing a region to be deposited into three or more portions to control its deposition speed for each portion.
  • deposition speed is controllable by moving a thermocouple that has been installed in a chemical vapor deposition apparatus to increase the speed gradually in the green body from the inside to the outside.
  • a carbon fiber reinforced resin composite 500 is installed in a reactor, and a heating element 400 is installed in the center. Furthermore, it may be implemented by supplying hydrocarbon gas as a process gas. In addition, deposition speed is controllable by using a thermocouple (not shown) as described above, and the deposition process may be performed from the inside to the outside.
  • deposition speed will be within a range of 0.5-3.0 mm/hr, and it will be deposited from the inside to the outside.
  • a region can be divided into three portions, such as the inside, the middle, and the outside, and then they may be deposited at 1.0 mm/hr, 1.5 mm/hr, and 2.0 mm/hr respectively to perform a deposition process more rapidly.
  • deposition speed is set to be low in the inside portion, because the deposition in the inside will be relatively slower than the outside.
  • This rapid thermal gradient chemical vapor infiltration process may be performed at a deposition speed 10 times faster and more densely than the thermal gradient chemical vapor infiltration process disclosed in Korean Patent No. 0198154 owned by this applicant to form a pyrolytic carbon layer approximately 5-100D in thickness.
  • the pyrolytic carbon layer that has been formed at this time will act as a reaction layer to form silicon carbide matrix-phase by reacting with liquid-phase silicon during the liquid-phase silicon impregnation process.
  • the carbon fiber reinforced resin composite that has been produced by the rapid thermal gradient chemical vapor infiltration process according to the present invention has physical properties of apparent density 1.0-1.7 g/cm , and apparent porosity 5-30 %.
  • the carbon fiber reinforced carbon composite produced by the rapid thermal gradient chemical vapor infiltration process is placed on silicon powder having particles in a range of 1 D- 10 mm in size during a liquid-phase silicon infiltration process.
  • the finally produced carbon fiber reinforced ceramic matrix composite is composed of 30-60 wt % carbon, 35-60 wt % silicon carbide, and less than 5 wt % non-reaction silicon.
  • the carbon fiber reinforced ceramic matrix composite can be produced using a green body made of a carbon felt preform as starting material as illustrated in FIG. 2.
  • a carbon felt preform reinforced in the three X, Y and Z axes is produced (S200); more specifically, carbon-based fibers, such as oxyphene, phene, rayon, pitch- based, or the like are wound around a mandrel to produce unidirectional carbon mats, and the carbon mats produced by this method are stacked together. For its stacking method, they are alternately stacked with quasi-isotropic orientation at 0/+60/-60 °.
  • At least two layers may be stacked, and then punched using a needle to reinforce all layers in the z-direction, and the above process will be reiterated to produce a felt preform greater than 30 mm in thickness.
  • This felt preform is made by a fiber volume ratio approximately 10-55%, where the thickness of one layer is approximately less than 0.1 mm, the length of fabrics in length is less than 10 mm, and the fabric ratio is approximately 10%. Furthermore, a needle having density of 15penetration/cm may be used for the Z-direction.
  • a carbon fiber reinforced carbon composite is produced by means of a rapid thermal gradient chemical vapor infiltration process (S210).
  • S210 a rapid thermal gradient chemical vapor infiltration process
  • the same rapid thermal gradient chemical vapor infiltration process as in the embodiment of the aforementioned first process will be applied to this.
  • a carbon fiber reinforced ceramic matrix composite is produced by means of a liquid-phase silicon infiltration process (S220).
  • S220 liquid-phase silicon infiltration process
  • the same liquid-phase silicon infiltration process as in the embodiment of the aforementioned first process will be applied to this.
  • a mixture comprising 30 wt % carbon fibers that have been cut out in the size of 30 mm, 40 wt % phenol resin, 5 wt % carbon powder, and 5 wt % silicon carbide powder is prepared and stacked alternately with carbon fabrics in the form of 20 wt % satin weave to produce a green body.
  • the produced green body is placed in a mold, and then cured while being pressurized at a pressure 2 MPa for 10 minutes to produce a carbon fiber reinforced resin composite.
  • the carbon fiber reinforced resin composite is subjected to thermal treatment in inert gas atmosphere. Furthermore, pyrolytic carbon is deposited in a condition of rapid thermal gradient chemical vapor infiltration process to produce a carbon fiber reinforced carbon composite.
  • the produced carbon fiber reinforced carbon composite is stacked on silicon powder, and heated at 1,550 °C in vacuum atmosphere, and infiltrated with liquid- phase silicon to produce a carbon fiber reinforced ceramic matrix composite.
  • physical properties of the produced carbon fiber reinforced ceramic matrix composite are shown in Table 1.
  • a mixture comprising 55 wt % carbon fibers that have been cut out in the size of 30 mm, 35 wt % phenol resin, 5 wt % carbon powder, and 5 wt % silicon carbide powder is prepared to produce a green body. Stacking alternately with carbon fabrics is not implemented in the second embodiment. The produced green body is placed in the mold, and then cured while being pressurized at a pressure 2 MPa for 10 minutes to produce a carbon fiber reinforced resin composite.
  • the carbon fiber reinforced resin composite is subjected to thermal treatment in inert gas atmosphere. Furthermore, pyrolytic carbon is deposited in a condition of rapid thermal gradient chemical vapor infiltration process to produce a carbon fiber reinforced carbon composite.
  • the produced carbon fiber reinforced carbon composite is stacked on silicon powder, and heated at 1,550 °C in vacuum atmosphere, and infiltrated with liquid- phase silicon to produce a carbon fiber reinforced ceramic matrix composite.
  • physical properties of the produced carbon fiber reinforced ceramic matrix composite are shown in Table 1.
  • At least two layers are stacked together, and then punched using a needle to reinforce every layer in the z-direction, and the process is reiterated to produce a felt preform having 30 mm in thickness.
  • This felt preform is produced at approximately 45% of oxyphene fiber volume ratio, where the thickness of a layer is approximately 0.9 mm, and the fiber ratio in the z-direction is approximately 10%.
  • the produced preform is subjected to thermal treatment at 1,700 °C in vacuum atmosphere to remove the impurities of the preform.
  • Pyrolytic carbon is deposited on the produced carbon felt preform in a condition of rapid thermal gradient chemical vapor infiltration process to produce a carbon fiber reinforced carbon composite.
  • the produced carbon fiber reinforced carbon composite is stacked on silicon powder and heated at 1,550 °C in vacuum atmosphere, and infiltrated with liquid-phase silicon to produce a carbon fiber reinforced ceramic matrix composite.
  • the physical properties of the produced carbon fiber reinforced ceramic matrix composite are shown in Table 1.
  • Comparative Example 1 A mixture is prepared by mixing 54 wt % of carbon fibers that have been cut out in the size of 130 mm, 36 wt % of phenol resin, and 10 wt % of carbon powder, and is placed in a mold, and then cured while being pressurized at 3 MPa of pressure to produce a carbon fiber reinforced resin composite.
  • the carbon fiber reinforced resin composite is subjected to thermal treatment at 900 °C in inert gas atmosphere to produce a carbon fiber reinforced carbon composite.
  • the produced carbon fiber reinforced carbon composite is stacked on silicon powder and heated at 1,600 °C in vacuum atmosphere, and infiltrated with liquid-phase silicon to produce a carbon fiber reinforced ceramic matrix composite.
  • the physical properties of the produced carbon fiber reinforced ceramic matrix composite are shown in Table 1.
  • carbon fibers in the carbon fiber reinforced carbon composites which have been produced by the rapid thermal gradient chemical vapor infiltration process, have a uniformly deposited pyrolytic carbon layer, and such a pyrolytic carbon layer is reacted with silicon to form silicon carbide during the liquid-phase silicon impregnation process.
  • the pyrolytic carbon layer has excellent properties for a fiber protection layer to prevent carbon fiber erosion, which is a most difficult problem during the liquid-phase silicon permeation process, as well as for a reaction layer to form silicon carbide; moreover, it improves physical properties of carbon fiber reinforced ceramic matrix composites by forming a new interface between carbon fibers and silicon carbide matrix-phase.
  • pyrolytic carbon layer can be deposited at a deposition speed 10 times faster or more than conventional chemical vapor infiltration processes, or 5 times faster or more than conventional thermal gradient chemical permeation processes, thereby remarkably reducing the cost of producing carbon fiber reinforced carbon composites.
  • carbon fiber reinforced resin composites can be simply produced by onetime process without performing iterative densification processes that are typically employed in the process of producing carbon fiber reinforced resin composites using liquid-phase precursors containing carbon.
  • the present invention is applicable to the transportation industry, such as aerospace, or ground vehicles.

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  • Manufacturing & Machinery (AREA)
  • Chemical Kinetics & Catalysis (AREA)
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  • General Engineering & Computer Science (AREA)
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  • Dispersion Chemistry (AREA)
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PCT/KR2005/001581 2004-05-28 2005-05-27 Method of producing carbon fiber reinforced ceramic matrix composites WO2005115945A1 (en)

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