CN106588060A - High-compactness silicon carbide ceramic-based composite material and preparation method thereof - Google Patents
High-compactness silicon carbide ceramic-based composite material and preparation method thereof Download PDFInfo
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- CN106588060A CN106588060A CN201610990055.0A CN201610990055A CN106588060A CN 106588060 A CN106588060 A CN 106588060A CN 201610990055 A CN201610990055 A CN 201610990055A CN 106588060 A CN106588060 A CN 106588060A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 56
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 239000000919 ceramic Substances 0.000 title claims abstract description 28
- 239000002131 composite material Substances 0.000 title abstract description 16
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 112
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 111
- 238000001764 infiltration Methods 0.000 claims abstract description 57
- 230000008595 infiltration Effects 0.000 claims abstract description 56
- 239000000835 fiber Substances 0.000 claims abstract description 52
- 229920005989 resin Polymers 0.000 claims abstract description 39
- 239000011347 resin Substances 0.000 claims abstract description 39
- 239000011159 matrix material Substances 0.000 claims abstract description 27
- 238000006243 chemical reaction Methods 0.000 claims abstract description 25
- 239000002243 precursor Substances 0.000 claims abstract description 17
- 238000005336 cracking Methods 0.000 claims abstract description 16
- 229920000620 organic polymer Polymers 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 229910001092 metal group alloy Inorganic materials 0.000 claims abstract description 3
- 239000011153 ceramic matrix composite Substances 0.000 claims description 27
- XPFVYQJUAUNWIW-UHFFFAOYSA-N furfuryl alcohol Chemical compound OCC1=CC=CO1 XPFVYQJUAUNWIW-UHFFFAOYSA-N 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims description 15
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- 238000007711 solidification Methods 0.000 claims description 12
- 230000008023 solidification Effects 0.000 claims description 12
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 10
- 229920001568 phenolic resin Polymers 0.000 claims description 10
- 239000005011 phenolic resin Substances 0.000 claims description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 9
- 239000002904 solvent Substances 0.000 claims description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 7
- 238000005452 bending Methods 0.000 claims description 7
- 238000007598 dipping method Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- 238000002844 melting Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 claims description 3
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 3
- 239000003822 epoxy resin Substances 0.000 claims description 3
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 3
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 3
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 229920000647 polyepoxide Polymers 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 24
- 229910052751 metal Inorganic materials 0.000 abstract description 15
- 239000002184 metal Substances 0.000 abstract description 15
- 229920000642 polymer Polymers 0.000 abstract description 14
- 229910052710 silicon Inorganic materials 0.000 abstract description 12
- 239000010703 silicon Substances 0.000 abstract description 10
- 229910000676 Si alloy Inorganic materials 0.000 abstract 1
- 239000000463 material Substances 0.000 description 27
- 238000009826 distribution Methods 0.000 description 14
- 239000007789 gas Substances 0.000 description 11
- 238000005498 polishing Methods 0.000 description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 9
- 239000003795 chemical substances by application Substances 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- 239000000243 solution Substances 0.000 description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 8
- 238000009954 braiding Methods 0.000 description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 8
- 230000001105 regulatory effect Effects 0.000 description 8
- 229910045601 alloy Inorganic materials 0.000 description 7
- 239000000956 alloy Substances 0.000 description 7
- 229920000049 Carbon (fiber) Polymers 0.000 description 6
- 239000004917 carbon fiber Substances 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000005470 impregnation Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 229910052786 argon Inorganic materials 0.000 description 4
- 238000000280 densification Methods 0.000 description 4
- 238000011065 in-situ storage Methods 0.000 description 4
- 238000002347 injection Methods 0.000 description 4
- 239000007924 injection Substances 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- -1 acyl Imide Chemical class 0.000 description 3
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000000197 pyrolysis Methods 0.000 description 3
- 238000002604 ultrasonography Methods 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 150000002739 metals Chemical class 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 229910001374 Invar Inorganic materials 0.000 description 1
- 229910003978 SiClx Inorganic materials 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- AYBYHHFARPYTPM-UHFFFAOYSA-N azane trichloroborane Chemical compound N.ClB(Cl)Cl AYBYHHFARPYTPM-UHFFFAOYSA-N 0.000 description 1
- 230000033228 biological regulation Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- AZFVLHQDIIJLJG-UHFFFAOYSA-N chloromethylsilane Chemical compound [SiH3]CCl AZFVLHQDIIJLJG-UHFFFAOYSA-N 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000005226 mechanical processes and functions Effects 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 229920000151 polyglycol Polymers 0.000 description 1
- 239000010695 polyglycol Substances 0.000 description 1
- 229920013657 polymer matrix composite Polymers 0.000 description 1
- 239000011160 polymer matrix composite Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 239000011226 reinforced ceramic Substances 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910000601 superalloy Inorganic materials 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
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- C04B35/806—
-
- 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
- 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
- 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
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/428—Silicon
-
- 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
- C04B2235/50—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
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- 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
- C04B2235/616—Liquid infiltration of green bodies or pre-forms
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- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Abstract
The invention relates to a high-compactness silicon carbide ceramic-based composite material and a preparation method thereof. The method comprises the following steps: impregnating a fiber perform in a precursor liquid containing high carbon yield resin and a low residual carbon rate organic polymer, and cracking the fiber perform to obtain a fiber/C infiltration perform; and infiltrating molten Si or molten Si and metal alloy in the fiber/C infiltration perform to carry out an infiltration reaction in order to obtain the silicon carbide ceramic-based composite material. Addition of the low residual carbon rate polymer changes the structure of carbon formed through cracking the resin in the infiltration perform and promotes the contact and the reaction of silicon and carbon in the reaction infiltration process, and infiltrated metal is dispersed in a matrix in a dispersive manner and effectively avoids generation of block residual carbon and block residual metal, so the mechanical performances and the heat conductivity of the composite material are substantially improved.
Description
Technical field
The present invention relates to a kind of high fine and close carbon/silicon carbide ceramic matrix composite and preparation method thereof, and in particular to one kind tool
There are the carbon/silicon carbide ceramic matrix composite and a kind of reaction infiltration preparation method of high-compactness and high heat conductance feature.
Background technology
With the development of the high-tech sectors such as Aeronautics and Astronautics, the energy, increasing part is in extreme Service Environment
In, therefore active demand is proposed to high performance material.Such as aero-engine, gas turbine are needed badly suitable for Li-heat-oxygen
Change the material of coupling environment, High Resolution Remote Sensing Satellites need lightweight, long-life badly and adapt to the material of space Service Environment.At present
The temperature extremes of the nickel base superalloy used in aero-engine is about 1100 DEG C, and the density of nickel-base alloy is relatively
Greatly, this greatly limits the further lifting of engine performance；Invar alloys used in remote sensing satellite supporting construction and
Polymer matrix composites can not meet the requirement of large-aperture long-focus camera.Silicon carbide fiber reinforced ceramic matric composite is close
Spend low, high temperature resistant, excellent in mechanical performance, designability strong, it is considered to be can replace or part replaces traditional material to be applied to
The structural material of new generation of high-tech sector.
The preparation method of carbon/silicon carbide ceramic matrix composite mainly has chemical vapour deposition technique (CVI), organic precursor leaching
Stain-cracking process (PIP) and reaction infiltration method (RMI).CVI and PIP methods can at a lower temperature obtain carbon/silicon carbide ceramic matrix and answer
Condensation material, is beneficial to the damage for avoiding high temperature to fiber, but material long preparation period, and preparation-obtained composite gas
The defects such as hole, crackle are more, and material property has certain limitation.The RMI methods in several ceramic matric composite preparation technologies
It is the method that uniquely can at short notice obtain high dense material.First by Si or its alloy melting in preparation process, in hair
Metal bath is penetrated into inside porous fibre/C in the presence of tubule power, and includes carbonization with matrix C generation chemical reaction generations
Silicon is in interior ceramic matrix.But, due to being prepared using resin impregnating-pyrolytic process more than porous fibre/C-material, generate
C particle sizes it is big, crackle, pore size skewness.Further, since motlten metal and bulk carbon source connect during RMI
Touch and there is a large amount of unreacted residual carbons and metal in insufficient carbon/silicon carbide ceramic matrix composite for causing and finally obtaining.Document
“Jiping Wang,Min Lin,Zhuo Xu,et al.Microstructure and mechanical properties
of C/C–SiC composites fabricated by a rapid processing method[J].Journal of
The European Ceramic Society, (2009) 3091-3097. " makes the C of different aperture using RMI techniquesf/ C is prefabricated
Body is densified, and quickly obtains the C of densificationf/ C-SiC composites, but there is collection of the Si of residual in fiber interfascicular and beam
Middle distribution, so as to affect the mechanical property of composite.The carbon source that the method is used uses CVI process deposits, residual Si
It is layer structure that the reason for integrated distribution is CVI carbon, and Si can only be reacted with part carbon, so as to the concentration point for having residual silicon
Cloth.Document " Honglei Wang, Xingui Zhou, Jinshan Yu, et al.Fabrication of SiCf/SiC
composites by chemical vapor infiltration and vapor silicon infiltration[J]
.Materials 1691-1693. of Letters 64 (2010) " have prepared the SiC of densification by the method for gas phase siliconisingf/
SiC ceramic matrix composite material, but there is residual carbon and silicon large area integrated distribution in the composite.The carbon source that the method is used is to use
CVI process deposits, be the reason for residual Si integrated distribution CVI carbon be layer structure, Si can only be reacted with part carbon, from
And having the integrated distribution of residual silicon, the raising of this mechanical behavior under high temperature and thermal conductivity to composite is totally unfavorable.
The content of the invention
The present invention is for Si or Si in carbon/silicon carbide ceramic matrix composite tradition RMI preparation process and other metals
Alloy and C are not sufficiently reacted causes the presence of large scale remnants Si or alloy and large scale residual carbon in matrix, there is provided
A kind of improved fiber/C infiltrations precursor structure builds infiltration reaction method for preparing.
On the one hand, the invention provides a kind of preparation method of high fine and close carbon/silicon carbide ceramic matrix composite, including：
In using the dipping fiber preform of the precursor liquid containing high carbon output rate resin, low Residual carbon organic polymer, cracking is obtained
Obtain fiber/C infiltration precast bodies；And
The Si of melting or the Si of melting are penetrated in the fiber/C infiltration precast bodies with the alloy of metal carries out infiltration reaction, obtains
To the carbon/silicon carbide ceramic matrix composite.
The present invention starts with from source, and by the structure regulating to fiber-infiltration precast body, increase metal bath connects with C's
Contacting surface is accumulated, and promotes the carrying out of infiltration kinetics.Specially it is with high carbon output rate resin (producing resin of the carbon rate higher than 60%)
Carbon source, with the low Residual carbon organic polymer with resin with excellent compatibility, (or referred to as low Residual carbon polymer is referred specifically to residual
Organic polymer of the carbon rate less than 15%) it is carbon base body structure regulating agent, and by the intimate blending thing of the two in fiber preform
Impregnated inside and solidification.The present invention utilizes the solidification polymerisation of high carbon output rate resin itself, induction high carbon output rate resin/carbon-based
Body structure regulating agent split-phase, promotes the two (high carbon output rate resin and low Residual carbon polymer) to form network blackboard.Tie again
The low-carbon (LC) persistence characteristic of adjusting control agent in further high temperature pyrolysis carbonisation is closed, is had in fiber preform Internal architecture and is adapted to melt
Ooze the carbon base body structure of reaction, and significantly reduce the particle size of pyrolytic carbon in carbon base body, to break through the office of existing preparation method
Limit, realizes the abundant reaction of metal and C during reaction infiltration, it is to avoid bulk carbon and bulk metal are remained, and are further to carry
The combination property of high composite and lay a good foundation for practical application.
It is preferred that the high carbon output rate resin is in furfuryl alcohol resin, asphaltic resin, benzoxazine colophony, phenolic resin
The mixture of at least one, preferably furfuryl alcohol resin and phenolic resin.It is preferred that the low yield carbon rate organic polymer is poly- second
At least one in glycol, epoxy resin, microcrystalline cellulose, preferably polyethylene glycol.
It is preferred that in the precursor liquid, the mass ratio of high carbon output rate resin and low Residual carbon organic polymer is (0.05
～8)：1, preferably (2～4)：1.
Also, it is preferred that the low Residual carbon organic polymer is polyethylene glycol.
It is preferred that the solvent is at least one in ethanol, acetone, formaldehyde.
It is preferred that the low Residual carbon organic polymer is (0.1～2) with the mass ratio of solvent：1, preferably (0.25～
0.5)：1.
It is preferred that fiber preform form includes what carbon fiber, silicon carbide fibre or carbon fiber mixed with silicon carbide fibre
Two dimension suture braiding structure, D refraction statics braiding structure, three-dimensional four-way braiding structure, three-dimensional five to braiding structure, one-dimentional structure,
Two-dimension laminate structure, but it is not limited to above-mentioned fiber architecture structure.
It is preferred that before the dipping, SiC ceramic matrix, cracking carbon interface, BN circle are prepared in the fiber preform
At least one in face.SiC ceramic matrix is prepared in fiber preform, SiC ceramic matrix is uniformly distributed in fiber preform
Interior fibrous inside and/or surface, primarily to loss when reducing Si infiltrations to fiber, so as to reach the work of protection fiber
With.In addition, cracking carbon interface, BN interfaces are prepared in precast body transmits load in addition to having and fiber is protected, also
Effect, so as to be conducive to the raising of material mechanical performance.
It is preferred that the technological parameter of the dipping includes：Vacuum -0.08MPa～-0.10MPa；The reaction temperature of solidification
For 100～150 DEG C；The reaction time of solidification is 1～3 hour.
It is preferred that described being cracked into is incubated 20～40 minutes in inert atmosphere at 850～1000 DEG C.
It is preferred that the inert atmosphere is argon gas atmosphere.
Also, it is preferred that the 3～8min/L of flow of control inert atmosphere.
It is preferred that the infiltration reaction is to be incubated 0.5～2 hour at 1250～1600 DEG C, vacuum ＜ 10Pa.
On the other hand, the invention provides a kind of carbon/silicon carbide ceramic matrix composite, the carbon/silicon carbide ceramic matrix composite wood
The porosity of material is 1～5%, and thermal conductivity is 25～40W/mK, and bending strength is 300～500MPa.
Beneficial effects of the present invention：
Change the structure that resin in infiltration precast body cracks the carbon to be formed by adding low Residual carbon polymer, promote reaction infiltration
When contact and reaction of the silicon with carbon, after infiltration metal be distributed in disperse shape in the base and effectively prevent block residual carbon and
The generation of block residual metal, so as to significantly improve the mechanical property and thermal conductivity of composite.
Description of the drawings
Fig. 1 is the process chart that the present invention prepares high-density silicon carbide ceramics based composites；
Fig. 2 is the C prepared by embodiment 1fThe SEM photograph of/C infiltration precast body polishing sections；
Fig. 3 is the C prepared by embodiment 1fThe graph of pore diameter distribution of/C infiltration precast bodies；
Fig. 4 is the C prepared by embodiment 1fThe SEM photograph of/SiC ceramic matrix composite material polishing section；
Fig. 5 is the C prepared by embodiment 1fThe X ray diffracting spectrum of/SiC ceramic matrix composite material polishing section；
Fig. 6 is the C prepared by comparative example 1fThe SEM photograph of/C infiltration precast body polishing sections；
Fig. 7 is the C prepared by comparative example 1fThe graph of pore diameter distribution of/C infiltration precast bodies；
Fig. 8 is the C prepared by comparative example 1fThe SEM photograph of/SiC ceramic matrix composite material polishing section.
Specific embodiment
The present invention is further illustrated below by way of following embodiments, it should be appreciated that following embodiments are merely to illustrate this
Invention, and the unrestricted present invention.
The present invention is with high carbon output rate resin as carbon source, low Residual carbon polymer is carbon base body structure regulating agent, by presoma
It is incorporated in fiber preform by vacuum impregnation, carries out being thermally treated resulting in fiber/C infiltration precast bodies under certain condition, then
By reacting infiltration method in-situ preparation including the ceramic matrix including SiC matrix, the carbon/silicon carbide ceramic matrix for obtaining high densification is combined
Material.Specially with high carbon output rate resin as carbon source, low Residual carbon polymer be carbon base body structure regulating agent, using dipping-heat
Solution technique introduces resin C in fibre preforms body, then obtains the carbon of high densification by RMI methods introducing Si or its alloy in-situ reaction
SiClx ceramic matric composite.
The preparation method of the high fine and close carbon/silicon carbide ceramic matrix composite that the explanation present invention in following exemplary ground is provided.
The pretreatment of fiber preform.A small amount of ceramic matrix is prepared in fiber preform, (pottery is protected to fiber
Porcelain basal body can be 0.5-4 times of fibre preforms weight).Ceramic matrix is only SiC ceramic matrix, but can be in precast body
Prepare and such as crack carbon interface, BN interfaces.The ceramic matrix can be SiC ceramic matrix, crack in carbon interface, BN interfaces extremely
Few one kind.Preparing the method for SiC ceramic matrix includes：SiC ceramic matrix is prepared by chemical vapor deposition osmosis, three are utilized
Used as source of the gas, hydrogen is carrier gas to chloromethyl silane, is placed in 1000 DEG C of tube furnace and deposits 100-200h..Cracking carbon interface
Forming method includes：It is source of the gas using methane, is placed in 1000 DEG C of tube furnaces and deposits 3-6h.The forming method at BN interfaces includes：
It is source of the gas using boron chloride ammonia, is placed in 1000 DEG C of tube furnaces and deposits 3-6h.
The preparation of precursor liquid.By high carbon output rate resin, low Residual carbon organic polymeric disperse in solvent (for example, second
Alcohol, acetone, formaldehyde etc.) after, water bath with thermostatic control ultrasound obtains precursor liquid.In one example, by low Residual carbon polymer (LCP)
Dissolving, obtains low Residual carbon polymer solution, adds a certain amount of high carbon output rate resin (HCR), and water bath with thermostatic control ultrasound is obtained
Precursor solution.It should be understood that the addition sequence not limited to this of low Residual carbon polymer (LCP) and high carbon output rate resin (HCR)
As long as (in theory can be dissolved in solvent just can be with for LCP and HCR, but in actual mechanical process, first plus after LCP plus HCR compares appearance
In being soluble in solvent).
Above-mentioned high carbon output rate resin includes but is not limited to furfuryl alcohol resin, asphaltic resin, benzoxazine colophony, span and carrys out acyl
Imide resin, phenolic resin or its hybrid resin, preferred furfuryl alcohol resin, phenolic resin and the hybrid resin of the two.Low Residual carbon
Polymer includes but is not limited to polyethylene glycol, epoxy resin, microcrystalline cellulose, preferred polyethylene glycol.The high carbon output rate tree
The mass ratio of fat and low Residual carbon polymer can be (0.05～8)：1, preferably (2～4)：1.Low Residual carbon organic polymer ratio
It is too low, the effect without adjustment apertures.The low Residual carbon polymer can be (0.1～2) with the mass ratio of solvent：, preferably
(0.25～0.5)：1.
The presoma is introduced into fiber preform or pretreated fiber preform using vacuum impregnation, solidification is obtained
Fiber/HCR-LCP formed bodys.Wherein, vacuum-impregnated vacuum is -0.08MPa～-0.10MPa.The reaction temperature of solidification can
For 100～150 DEG C.The reaction time of solidification can be 1～3 hour.Using the solidification polymerisation of resin, resin/regulation and control are induced
Agent split-phase, promotes the two (high carbon output rate resin and low Residual carbon polymer) to form network blackboard.
Above-mentioned fiber preform form includes the two dimension that carbon fiber, silicon carbide fibre or carbon fiber mix with silicon carbide fibre
Suture braiding structure, D refraction statics braiding structure, three-dimensional four-way braiding structure, three-dimensional five are to braiding structure, one-dimentional structure, two dimension
Laminated construction, but it is not limited to above-mentioned fiber architecture structure.
Fiber/HCR-LCP formed bodys are cracked under inert atmosphere (for example, argon gas etc.).The condition of wherein described cracking
To be incubated 20～40 minutes at 850～1000 DEG C.3～the 8min/L of flow of control inert gas argon gas.
Cleavage step 1-5 time, obtains fiber/C infiltration precast bodies under repeating vacuum dipping and inert atmosphere.Wherein, obtained
Fiber/C infiltration precast bodies pore-size distribution can be 0.1～10 μm, the porosity be 20～40%, median pore size be 0.5～5 μ
M, preferred 0.8-1.2 μm.
The Si or the Si of melting and the alloy infiltrated fiber/C infiltrations of other metals (for example, Y, Yb, Al etc.) of melting is pre-
Infiltration is carried out in body processed and reacts in-situ preparation including the ceramic matrix including SiC, obtain the carbon/silicon carbide ceramic matrix composite.
Wherein the condition of infiltration reaction can be to be incubated 0.5～2 hour at 1250～1600 DEG C, and vacuum is better than 10Pa.
It is specifically described by taking furfuryl alcohol resin, phenolic resin, polyethylene glycol, Si systems as an example below, technological process such as Fig. 1
It is shown：(1) precast body is processed：A certain amount of SiC ceramic matrix is prepared in carbon fiber precast body, fiber is protected.(2)
It is prepared by precursor liquid：During polyethylene glycol (PEG) is dissolved in into ethanol, polyglycol solution is obtained, add a certain amount of furfuryl alcohol resin
(FFR), phenolic resin (PFR), water bath sonicator obtains precursor liquid.Wherein furfuryl alcohol resin and phenolic resin mass ratio for (0.1～
9)：1, preferably (1～3)：1；The mass ratio of furfuryl alcohol resin and polyethylene glycol is (0.1～4)：1, preferably (1.5～2.5)：1；It is poly-
The mass ratio of ethylene glycol and ethanol is (0.1～2)：1, preferably (0.25～0.5)：1.(3) vacuum impregnation solidification：Before in (2)
Drive liquid to be introduced in (1) in fiber preform in the way of vacuum impregnation (- 0.08MPa～-0.10MPa vacuums), 100～
Insulation at 150 DEG C completes solidification for 6～10 hours, obtains Cf/FFR-PFR-PEG.(4) crack：By the C in (3)f/ FFR-PFR is put
Enter cracking in pyrolysis furnace (cracking condition is 850～1000 DEG C and is incubated 20～40 minutes), period keeps argon gas atmosphere (for example, Ar
Throughput is 3～8min/L), C is obtained after crackingf/ C infiltration precast bodies, resulting CfThe pore-size distribution of/C infiltration precast bodies is
0.1～10 μm, the porosity is 20～40%, and median pore size is 0.5～5 μm.(5) (3) (4) step 1-5 time is repeated, is obtained
The C of different porositiesf/ C infiltration precast bodies.(6) infiltration is reacted：Under vacuum, under the conditions of uniform temperature by melt of si penetrate into
CfSiC matrix is generated with C reaction in-situs in/C, the preparation of material is completed.Wherein, Si infiltrations condition is 1380～1600 DEG C of insulations
0.5～2 hour.
In above-mentioned example, the key reaction being related to is：
Cracking reaction：FFR+PFR→C；
Infiltration reacts：Si+C→SiC.
Metal and carbon is fully contacted and reacts, the carbon/silicon carbide ceramic matrix after infiltration when the present invention can promote to react infiltration
Without block residual metal in matrices of composite material, the ceramic matrix particle rich in metal is tiny in the distribution of disperse shape, without bulk carbon
Integrated distribution, significantly improve material mechanical performance and thermal conductivity.The hole of wherein described carbon/silicon carbide ceramic matrix composite
Rate can be 1～5%, and thermal conductivity can be 25～40W/mK, and bending strength can be 300～500MPa.
Enumerate embodiment further below to describe the present invention in detail.It will similarly be understood that following examples are served only for this
Invention is further described, it is impossible to be interpreted as limiting the scope of the invention, those skilled in the art is according to this
Some nonessential modifications and adaptations that bright the above is made belong to protection scope of the present invention.Following examples are specific
Technological parameter etc. is also only that an example in OK range, i.e. those skilled in the art can be done properly by the explanation of this paper
In the range of select, and do not really want to be defined in the concrete numerical value of hereafter example.
Embodiment 1
(1) precast body is processed：800gSiC ceramic matrixs are prepared in 800g carbon fiber precast bodies.Concrete grammar can be to utilize trichlorine
Used as source of the gas, hydrogen is carrier gas to methyl-monosilane, fiber preform is placed in 1000 DEG C of tube furnace and deposits 100h.；
(2) prepared by presoma：100g polyethylene glycol (PEG) is dissolved in 400g ethanol；By 200g furfuryl alcohol resins (FFR) and 200g
Phenolic resin (PFR) is added in above-mentioned solution, and precursor liquid is obtained within 6 hours in 50 DEG C of water bath sonicators；
(3) vacuum impregnation：Under -0.08MPa～-0.10MPa vacuum conditions, precursor liquid in (2) is introduced to into C in (1)fIn advance
In body processed, solidify within 2 hours in 120 DEG C of insulations, obtain Cf/FFR-PFR-PEG；
(4) crack：By the C in (3)f/ FFR-PFR-PEG is put in pyrolysis furnace and cracks, and is incubated 0.5 hour at 1000 DEG C, period
The Ar atmosphere of 5L/min is kept, C is obtained after crackingf/ C infiltration precast bodies；
(5) infiltration is reacted：Melt of si is penetrated into C under the conditions of vacuum, 1500 DEG C of insulations infiltration of 1 hourfIt is in/C and former with C
Position reaction generates SiC matrix, completes the preparation of material.
Prepared C in the present embodimentfThe SEM photograph of/C infiltration precast body polishing sections as shown in fig. 2, it can be seen that
Resin carbon is presented cellular and is distributed in fiber interfascicular.C prepared by the present embodimentfPore-size distribution such as Fig. 3 of/C infiltration precast bodies
Shown, aperture is distributed more between 0.3～5 μm.C prepared by the present embodimentfThe SEM of/SiC ceramic matrix composite material polishing section shines
Piece is as shown in figure 4, the Silicon-rich ceramic matrix Dispersed precipitate of point-like, and the presence without residual carbon.Prepared Cf/ SiC is multiple
The X ray diffracting spectrum of condensation material polishing section as shown in figure 5, be with silicon and carborundum two-phase in explanation matrices of composite material
It is main.
C prepared by the present embodimentf/ C infiltrations precast body is by the Mercury-injection tests of Autopore IV 9500V 1.09, middle position
Aperture is 1.78 μm；The C for preparingf/ SiC ceramic matrix composite material is tested by Archimedes's drainage, and porosity is 4.2%, is led to
It is 30W/mK to cross NETZSCHLFA427 laser heat conducting instruments and measure thermal conductivity, through CIMACH DDL20 electronic universal testers
Test, bending strength is 344MPa.
Embodiment 2
It is similar with the step in embodiment 1, except that, (3) (4) step is repeated 1 times；
C prepared by the present embodimentf/ C infiltrations precast body is by the Mercury-injection tests of Autopore IV 9500V 1.09, median pore size
For 1.16 μm；The C for preparingf/ SiC ceramic matrix composite material is tested by Archimedes's drainage, and porosity is 3.3%, is passed through
It is 33W/mK that NETZSCHLFA427 laser heat conducting instruments measure thermal conductivity, is surveyed through CIMACH DDL20 electronic universal testers
Examination, bending strength is 398MPa.
Embodiment 3
It is similar with the step in embodiment 1, except that, (3) (4) step is repeated 2 times；
C prepared by the present embodimentf/ C infiltrations precast body is by the Mercury-injection tests of Autopore IV 9500V 1.09, median pore size
For 0.92 μm；The C for preparingf/ SiC ceramic matrix composite material is tested by Archimedes's drainage, and porosity is 2.0%, is passed through
It is 38W/mK that NETZSCHLFA427 laser heat conducting instruments measure thermal conductivity, is surveyed through CIMACH DDL20 electronic universal testers
Examination, bending strength is 460MPa.
(mass ratio of the high carbon output rate resin and low Residual carbon organic polymer is 2 to embodiment 4:1)
It is similar with the step in embodiment 1, except that：100g polyethylene glycol is added in 400g ethanol；By 200g furfuryl alcohols
Resin (FFR) adds above-mentioned solution to add above-mentioned solution, and water bath sonicator obtains precursor solution in 6 hours at 50 DEG C；
C prepared by the present embodimentf/ C infiltrations precast body is by the Mercury-injection tests of Autopore IV 9500V 1.09, median pore size
For 2.58 μm；The C for preparingf/ SiC ceramic matrix composite material is tested by Archimedes's drainage, and porosity is 3.7%, is passed through
It is 35W/mK that NETZSCHLFA427 laser heat conducting instruments measure thermal conductivity, is surveyed through CIMACH DDL20 electronic universal testers
Examination, bending strength is 380MPa.
Comparative example 1 (precursor solution does not contain low Residual carbon polymer)
It is similar with the step in embodiment 1, except that prepared by (2) presoma：By 200g furfuryl alcohol resins and 200g phenolic aldehyde trees
Fat mixing is made into furfuryl alcohol phenolic aldehyde hybrid resin；400g ethanol, ultrasound is added to obtain presoma in 2 hours.
C prepared by this comparative examplefThe SEM photograph of/C infiltration precast body polishing sections is as shown in fig. 6, can from figure
Go out, when carbon base body structure regulating agent is not added, the resin carbon of cracking is distributed in fiber interfascicular in big bulk.Fig. 7 is that this is right
C prepared by ratiofThe graph of pore diameter distribution of/C infiltration precast bodies, as can be seen from Fig., does not add carbon base body structure regulating agent
When CfThe aperture of/C infiltration precast bodies is between 10～30 μm.C prepared by this comparative examplef/ SiC ceramic matrix composite material polishing section
As shown in figure 8, it can be seen that when being not added with carbon base body structure regulating agent, there is unreacted in matrix complete in SEM photograph
Bulk carbon, and silicon integrated distribution.
Claims (11)
1. a kind of preparation method of high fine and close carbon/silicon carbide ceramic matrix composite, it is characterised in that include：
In using the dipping fiber preform of the precursor liquid containing high carbon output rate resin, low Residual carbon organic polymer, after cracking
Obtain fiber/C infiltration precast bodies；And
The Si of melting or the Si of melting are penetrated in the fiber/C infiltration precast bodies with the alloy of metal carries out infiltration reaction, obtains
To the carbon/silicon carbide ceramic matrix composite.
2. preparation method according to claim 1, it is characterised in that the high carbon output rate resin is furfuryl alcohol resin, pitch
The mixture of at least one in resin, benzoxazine colophony, phenolic resin, preferably furfuryl alcohol resin and phenolic resin.
3. preparation method according to claim 1 and 2, it is characterised in that the low yield carbon rate organic polymer is poly- second
At least one in glycol, epoxy resin, microcrystalline cellulose, preferably polyethylene glycol.
4. the preparation method according to any one of claim 1-3, it is characterised in that in the precursor liquid, high yield carbon
The mass ratio of rate resin and low Residual carbon organic polymer is（0.05～8）：1, preferably（2～4）：1.
5. the preparation method according to any one of claim 1-4, it is characterised in that the precursor liquid solvent for use is
At least one in ethanol, acetone, formaldehyde.
6. the preparation method according to any one of claim 1-5, it is characterised in that the low Residual carbon organic polymer
It is with the mass ratio of solvent（0.1～2）：1, preferably（0.25～0.5）：1.
7. the preparation method according to any one of claim 1-6, it is characterised in that the technological parameter bag of the dipping
Include：Vacuum -0.08MPa～-0.10MPa；The reaction temperature of solidification is 100～150 DEG C；The reaction time of solidification is 1～3 little
When.
8. the preparation method according to any one of claim 1-7, it is characterised in that before the dipping, in the fibre
At least one in SiC ceramic matrix, cracking carbon interface, BN interfaces is prepared in dimension precast body.
9. the preparation method according to any one of claim 1-8, it is characterised in that described being cracked into exists in inert atmosphere
20～40 minutes are incubated at 850～1000 DEG C.
10. the preparation method according to any one of claim 1-9, it is characterised in that the infiltration reaction is 1250
0.5～2 hour is incubated at～1600 DEG C, vacuum ＜ 10Pa.
Carbon/silicon carbide ceramic matrix composite prepared by a kind of 11. preparation methods according to any one of claim 1-10, its
It is characterised by, the porosity of the carbon/silicon carbide ceramic matrix composite is 1～5%, and thermal conductivity is 25～40W/mK, and bending is strong
Spend for 300～500MPa.
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