CN105835455A - 2D carbon/silicon-silicon carbide composite material pin preparation method and preparation method and structure of 2D carbon/silicon-silicon carbide composite material pin preform - Google Patents
2D carbon/silicon-silicon carbide composite material pin preparation method and preparation method and structure of 2D carbon/silicon-silicon carbide composite material pin preform Download PDFInfo
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- CN105835455A CN105835455A CN201510940375.0A CN201510940375A CN105835455A CN 105835455 A CN105835455 A CN 105835455A CN 201510940375 A CN201510940375 A CN 201510940375A CN 105835455 A CN105835455 A CN 105835455A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 101
- 239000002131 composite material Substances 0.000 title claims abstract description 68
- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 238000000151 deposition Methods 0.000 claims abstract description 39
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 38
- 239000010439 graphite Substances 0.000 claims abstract description 38
- 239000000835 fiber Substances 0.000 claims abstract description 32
- 239000002296 pyrolytic carbon Substances 0.000 claims abstract description 26
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000011241 protective layer Substances 0.000 claims abstract description 22
- 238000000626 liquid-phase infiltration Methods 0.000 claims abstract description 6
- 239000004744 fabric Substances 0.000 claims description 63
- 239000007789 gas Substances 0.000 claims description 60
- 238000000034 method Methods 0.000 claims description 50
- 229910003978 SiClx Inorganic materials 0.000 claims description 31
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 29
- 239000010410 layer Substances 0.000 claims description 24
- 230000001681 protective effect Effects 0.000 claims description 20
- 230000035515 penetration Effects 0.000 claims description 16
- 238000004062 sedimentation Methods 0.000 claims description 16
- 239000000758 substrate Substances 0.000 claims description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000012159 carrier gas Substances 0.000 claims description 10
- 238000009958 sewing Methods 0.000 claims description 9
- 230000008021 deposition Effects 0.000 claims description 6
- 239000011159 matrix material Substances 0.000 claims description 6
- 235000013312 flour Nutrition 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 5
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000002002 slurry Substances 0.000 claims description 5
- 238000009826 distribution Methods 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 238000003475 lamination Methods 0.000 claims description 2
- AZFVLHQDIIJLJG-UHFFFAOYSA-N chloromethylsilane Chemical compound [SiH3]CCl AZFVLHQDIIJLJG-UHFFFAOYSA-N 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 229920000049 Carbon (fiber) Polymers 0.000 abstract description 15
- 239000004917 carbon fiber Substances 0.000 abstract description 13
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000919 ceramic Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 238000001764 infiltration Methods 0.000 abstract description 5
- 230000008595 infiltration Effects 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 238000005520 cutting process Methods 0.000 abstract description 4
- 238000010923 batch production Methods 0.000 abstract 1
- 238000003801 milling Methods 0.000 abstract 1
- 238000004826 seaming Methods 0.000 abstract 1
- 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 10
- 238000004140 cleaning Methods 0.000 description 6
- 239000003575 carbonaceous material Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000008187 granular material Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 3
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 238000001467 acupuncture Methods 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001722 carbon compounds Chemical class 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 230000003204 osmotic effect Effects 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B28—WORKING CEMENT, CLAY, OR STONE
- B28D—WORKING STONE OR STONE-LIKE MATERIALS
- B28D1/00—Working stone or stone-like materials, e.g. brick, concrete or glass, not provided for elsewhere; Machines, devices, tools therefor
- B28D1/16—Working stone or stone-like materials, e.g. brick, concrete or glass, not provided for elsewhere; Machines, devices, tools therefor by turning
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/06—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by a fibrous or filamentary layer mechanically connected, e.g. by needling to another layer, e.g. of fibres, of paper
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
- B32B5/24—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer
- B32B5/26—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed one layer being a fibrous or filamentary layer another layer next to it also being fibrous or filamentary
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B9/047—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material made of fibres or filaments
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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
- C04B35/52—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 carbon, e.g. graphite
- C04B35/521—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 carbon, e.g. graphite obtained by impregnation of carbon products with a carbonisable material
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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
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
- B32B2262/10—Inorganic fibres
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- B32B2605/00—Vehicles
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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
- C04B2235/30—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
- C04B2235/483—Si-containing organic compounds, e.g. silicone resins, (poly)silanes, (poly)siloxanes or (poly)silazanes
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- 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
Abstract
The invention relates to a 2D carbon/silicon-silicon carbide composite material pin preparation method and a preparation method and structure of a 2D carbon/silicon-silicon carbide composite material pin preform. The pin preparation method comprises 1, preparing a preform through horizontal paving (0 degree)-inclined paving (45 degrees) alternative laying of a 2D carbon fabric, graphite mold-based setting and carbon fiber vertical seaming on the multilayer carbon fabric, 2, depositing a pyrolytic carbon protective layer in the preform, 3, carrying out chemical vapor infiltration (CVI) to obtain a silicon carbide base, 4, cutting a flat blank to obtain a strip-shaped pin blank with the square section, 5, carrying out CVI silicon carbide protection of exposed fibers, 6, carrying out reactive melt infiltration (RMI) treatment, 7, milling the pin blank to obtain a pin with a standard size and 8, carrying out examination to obtain a carbon/silicon-silicon carbide composite material pin finished product. Through combination of CVI and RMI, the preparation method has the advantages of low production cost, short production period, low product porosity, high density and batch production. The ceramic-based composite material prepared by the CVI and RMI has shear strength of 80-100MPa at the room temperature.
Description
Technical field
The present invention relates to ceramic matric composite preparation and processing technique field, the preparation technology of a kind of Two-dimensional Carbon/silico-carbo SiClx composite pin, be mainly used in high intensity, high temperature resistant, corrosion-resistant, antioxidative composite connection area.
Background technology
Ceramic matric composite is favored by all kinds of Aeronautics and Astronautics fields with thermophysical property and the mechanical property of the excellences such as its high intensity, high rigidity, high temperature resistant, wear-resistant, anticorrosive, low-density, particularly use the part that environment is harsh on aircraft, ceramic matric composite can substitute tradition special metal material, improves parts combination property in the present context.
Restriction due to composite woven technique, it is achieved large-scale, accurate, complex component is the most difficult.Therefore, composite application is had great importance by research and development high-performance, connector safe and reliable, low cost.Connector used by Aeronautics and Astronautics class, according to different service temperatures and mechanical property, selects different materials.Carbon/carbon compound material connector has low-density, the wear-resisting height that undermines compares the series of advantages such as strong, and its high-temperature oxidation resistance is the most poor also limits its long-life, high performance performance；Carbon/composite material of silicon carbide connector in addition to possessing low-density, high temperature resistant, Gao Biqiang, high-temperature oxidation resistance, be also equipped with anti-yaw damper, insensitive to crackle, there is not the excellent properties such as calamitous damage.But its manufacturing cost is higher, the cycle is longer limits its application in civilian goods direction；And carbon/silico-carbo SiClx composite connector is not only less with the performance difference of carbon/composite material of silicon carbide, also than the low cost of manufacture of carbon/composite material of silicon carbide connector.Therefore carbon/silico-carbo SiClx composite class connector not only can meet the space field using environment harsh, it is also possible to applies the civil area in some low cost.
A kind of ceramic matric composite pin needling preform structure and preparation method is disclosed in the patent of invention of Publication No. CN103601523 A.This needling preform structure is the needling structure that long fibre laminated cloth and web of staple fibers tire replace laying；Its medium-length fibre direction and the axial angle of pin be the laminated cloth number of plies of-5 °～5 ° be 3～9 times of the long fibre direction laminated cloth number of plies with the axial angle of pin 85 °～95 °.The method includes, initially with chemical vapor infiltration technique, needling preform structure is carried out pyrocarbon, then uses chemical vapor infiltration technique to carry out the deposition of carborundum, finally uses mach mode that the precast body after densification is processed into pin.It is more difficult that the needling structure of the multilamellar alternately laying that the method uses makes, it is difficult to realizes precast body stable performance uniform.The room temperature shear strength of pin needling preform pin prepared by employing the method is about 81～105MPa.Meanwhile, manufacturing cycle length when chemical vapor infiltration prepares C/SiC composite, relatively costly is had been used up.
Summary of the invention
In order to overcome the technology of preparing production cycle length of acupuncture C/SiC composite (CVI technique) pin of labyrinth, cost high, the shortcomings such as properties of product instability differs greatly, the present invention provides the preparation method of a kind of Two-dimensional Carbon/silico-carbo SiClx composite pin, additionally provides preparation method and the structure of pin precast body simultaneously.
The technical solution adopted for the present invention to solve the technical problems:
Two-dimensional Carbon provided by the present invention/silico-carbo SiClx composite pin precast body, including multilayer two-dimension carbon cloth, it is characterized in that
In described multilayer two-dimension carbon cloth, the angle of the corresponding fiber of adjacent two layers two dimension carbon cloth is 45 °,
Described Two-dimensional Carbon/silico-carbo SiClx composite pin precast body also includes sewing structure, and described sewing structure includes that the multiple U-shaped fiber of squarely matrix distribution, multiple U-shaped fibers vertically penetrate multilayer two-dimension carbon cloth from the one side of multilayer two-dimension carbon cloth.Adjacent two ends arranging U-shaped fiber in above-mentioned square matrix are additionally provided with 1 U-shaped fiber.
The preparation method of Two-dimensional Carbon provided by the present invention/silico-carbo SiClx composite pin precast body, it is characterized in that and comprises the following steps:
1) the graphite planar horizontal positioned in hole will be equipped with；
2) tile on graphite planar multilayer two-dimension carbon cloth, until the laminated thickness of two dimension carbon cloth meets pin diameter and leaves allowance；The angle of the corresponding fiber of adjacent two layers two dimension carbon cloth is 45 °,
3) multilayer two-dimension carbon cloth is stepped up with graphite planar, graphite planar is holded up；
4) graphite planar is fixed with support；
5) use fiber vertically to sew carbon cloth by the hole arranged on graphite planar, make two-dimensional flat plate precast body.
Above-mentioned steps 2) to be used the cellosilk in two dimension carbon cloth be vertical intertexture, during lamination, adjacent two layers carbon cloth angle at 45 °.
The hole of above-mentioned graphite planar arranges according to the mode of 8～15 × 8～15mm.
The preparation method of Two-dimensional Carbon provided by the present invention/silico-carbo SiClx composite pin, comprises the following steps:
1) two-dimensional flat plate precast body is made；
2) by cvd furnace at two-dimensional flat plate precast body internal penetration pyrolytic carbon protective layer；
3) it is being impregnated with the two-dimensional flat plate internal penetration silicon carbide substrate of pyrolytic carbon protective layer；
4) tooling pin nailing strip shape blank；
5) pin blank clamping is pressed on lathe figure paper size car cylinder and length, obtain Two-dimensional Carbon/silico-carbo SiClx composite pin finished product；
It is characterized in that described step 1) particularly as follows:
1.1) the graphite planar horizontal positioned in hole will be equipped with；
1.2) tile on graphite planar multilayer two-dimension carbon cloth, until the laminated thickness of two dimension carbon cloth meets pin diameter and leaves allowance；The corresponding fiber angle of adjacent two layers two dimension carbon cloth is 45 °,
1.3) multilayer two-dimension carbon cloth is stepped up with graphite planar, graphite planar is holded up；
1.4) by graphite planar and between fixing；
1.5) use fiber vertically to sew carbon cloth by the hole arranged on graphite planar, make two-dimensional flat plate precast body.
Above-mentioned steps 4) and step 5) between also include:
A) pin blank is put into stove depositing silicon carbide layers；
B) will scribble the pin blank of bn slurry and drain in crucible, pin blank is embedded by the mass ratio mixing using silica flour and carborundum powder to press 1:1～2, puts into and carries out RMI process in melt infiltration furnace；
Above-mentioned steps 2) process conditions be: depositing temperature is 600～1000 DEG C, and cvd furnace is evacuated to 1～10kPa, and using propylene gas that flow is 2～8L/min as deposition gases, the Ar gas of 4～10L/min is as protective gas, and sedimentation time is 60～100h；Obtain depositing the two-dimensional flat plate precast body of pyrolytic carbon protective layer.
Above-mentioned steps 3) process conditions be: depositing temperature is 1000～1200 DEG C, and cvd furnace is evacuated to 1～10kPa, and using Ar gas that flow is 4～10L/min as protective gas, flow is the H of 4～10L/min2Gas, as carrier gas, reacts in trichloromethyl silane is brought into cvd furnace inside two-dimensional flat plate, generates silicon carbide substrate, and is deposited on the pyrolytic carbon protective layer within described two-dimensional flat plate, generates density (or porosity) and is about 1.3～1.5g/cm3Composite material flat plate；The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is 60～100h；
Above-mentioned steps 5) process conditions be: depositing temperature is 1000～1200 DEG C; cvd furnace is evacuated to 1～10kPa; using Ar gas that flow is 4～10L/min as protective gas; flow is that the H2 gas of 4～10L/min is as carrier gas; react in pin blank inside and surface in trichloromethyl silane is brought into cvd furnace, generate density (or porosity) and be about 1.5～1.7g/cm3 composite bar shaped blanks.The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, and H2 is 9～11 with the molal weight ratio of trichloromethyl silane, and sedimentation time is 30～50h.
Above-mentioned RMI treatment temperature is 1300～1500 DEG C, is evacuated to 1～10kPa in stove, using Ar gas that flow is 2～8L/min as protective gas, time of penetration 60～100h, makes density (or porosity) and is about 1.9～2.1g/cm3Bar shaped blank after siliconising.
The invention has the beneficial effects as follows:
1, the present invention uses two dimension carbon cloth tiling, the two-dimensional flat plate precast body prepared by the method for carbon fiber vertical puncturing again, in precast body, the angle of the corresponding fiber of adjacent two layers two dimension carbon cloth is 45 °, this structure not only ensure that uniform force between the fiber in every layer of carbon cloth plane, and the carbon fiber of vertical puncturing also is able to strengthen the stress in third dimension space；Make pin be not easy to produce weak load-bearing point, improve the mechanical property of pin.
2, the preparation method of precast body of the present invention is simple, and efficiency is high.
3, use the blank of CVI carborundum protection (rather than pyrolytic carbon protection) pin, it is possible to make carborundum penetrate into internal carbon fibers surface, liquid-phase silicone solution can be exempted from sustainable protection carbon fiber and corrode.
4, using RMI technique (rather than CVI technique) to prepare pin process of semi-finished, not only osmotic efficiency is high, product air holes rate is low, and only needs a stove just can complete, and greatly reduces the manufacturing cost of product.
5, the shear strength under the ceramic matric composite room temperature of embodiment 2 preparation is used to be about 80～100Mpa.
6, two-dimentional carbon cloth precast body pin prepared by the present invention has the shear strength level of pin of the prior art, can be used for preparing the ceramic matric composite complex component of high bonding strength.
Accompanying drawing explanation
Fig. 1 is the flow chart of Two-dimensional Carbon/silico-carbo SiClx composite pin preparation method；
Fig. 2 is that composite material flat plate precast body sews schematic diagram；
Fig. 3 is the section view of composite material flat plate precast body；
Fig. 4 is the enlarged drawing at the A of Fig. 3；
Fig. 5 is the enlarged drawing at the B of Fig. 2.
Wherein 1-carbon fiber, 2-lockstitch a border carbon fiber, 3-graphite planar, 4-multilamellar carbon cloth, 5-threading via hole.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in detail.
As Figure 2-3, the Two-dimensional Carbon of the present invention/silico-carbo SiClx composite pin precast body, including multilayer two-dimension carbon cloth, in multilayer two-dimension carbon cloth, the angle of the corresponding fiber of adjacent two layers two dimension carbon cloth is 45 °, Two-dimensional Carbon/silico-carbo SiClx composite pin precast body also includes sewing structure, sewing structure includes the multiple U-shaped fiber of squarely matrix distribution, and multiple U-shaped fibers vertically penetrate multilayer two-dimension carbon cloth from the one side of multilayer two-dimension carbon cloth.Four limit carbon fibers of multilayer two-dimension carbon cloth are lockstitched a border, and sometimes, adjacent two ends arranging U-shaped fiber in square matrix are additionally provided with 1 U-shaped fiber.The preparation method of this Two-dimensional Carbon/silico-carbo SiClx composite pin precast body, comprises the following steps:
1) the graphite planar horizontal positioned in hole will be equipped with；
2) tile on graphite planar multilayer two-dimension carbon cloth, until the laminated thickness of two dimension carbon cloth meets pin diameter and leaves allowance；The angle of the corresponding fiber of adjacent two layers two dimension carbon cloth is 45 °；
3) multilayer two-dimension carbon cloth is stepped up with graphite planar, graphite planar is holded up；
4) graphite planar is fixed with support；
5) use fiber vertically to sew carbon cloth by the hole arranged on graphite planar, make two-dimensional flat plate precast body.Two-dimensional flat plate precast body, after depositing silicon carbide layers, removes graphite planar, forms pin precast body.
Hereinafter for three embodiments, the pin preparation method of the present invention is described in detail.
Embodiment 1:
The present embodiment is the preparation method of a kind of Two-dimensional Carbon/silico-carbo SiClx composite pin, and its detailed process is:
Step 1, makes two-dimensional flat plate precast body.(thickness ensures more than pin diameter and leaves allowance) is the most successively tiled with tiling (0 °) and oblique paving (45 °) direction with two dimension carbon cloth, the graphite planar using surface to be equipped with hole (8～15 × 8～15mm arrangement mode) flattens carbon cloth, segmental support is fixed on support, using carbon fiber through each hole, two-dimensional flat plate precast body made by vertical sewing carbon cloth.
Step 2, deposits pyrolytic carbon boundary layer.By cvd furnace at two-dimensional flat plate precast body internal penetration pyrolytic carbon protective layer; its process conditions are: depositing temperature is 700 DEG C, and cvd furnace is evacuated to 5kPa, and the propylene gas using flow as 3L/min is as deposition gases; the Ar gas of 6L/min is as protective gas, and sedimentation time is about 70h；Obtain depositing the two-dimensional flat plate precast body of pyrolytic carbon protective layer.
Step 3, demoulding depositing silicon silicon substrate.Being impregnated with the two-dimensional flat plate internal penetration silicon carbide substrate of pyrolytic carbon protective layer, process conditions are: depositing temperature is 1000 DEG C, and cvd furnace is evacuated to 5kPa, and the Ar gas using flow as 6L/min is as protective gas, and flow is the H of 6L/min2Gas, as carrier gas, reacts in trichloromethyl silane is loaded into cvd furnace inside two-dimensional flat plate, generates silicon carbide substrate, and is deposited on the pyrolytic carbon protective layer within described two-dimensional flat plate, generates density (or porosity) and is about 1.3～1.5g/cm3Composite material flat plate；The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is about 70h.
Step 4, processes bar shaped pin blank；First with grinding machine, the upper and lower surface of two-dimensional flat plate is polished, it is ensured that thickness is more than pin diameter (leaving allowance).Cleaning up planar surface, to be as the criterion without granule, then flat plate cutting is slit into cross section is foursquare strip blank.
Step 5, depositing silicon carbide layers；Bar shaped blank is put into stove depositing silicon carbide layers, and depositing temperature is 1000 DEG C, and cvd furnace is evacuated to 5kPa, and the Ar gas using flow as 6L/min is as protective gas, and flow is the H of 6L/min2Gas, as carrier gas, reacts in pin blank inside and surface in trichloromethyl silane is loaded into cvd furnace, generates density (or porosity) and be about 1.5～1.7g/cm3Composite blank.The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is about 70h.
Step 6, RMI process；The bar shaped pin blank of bn slurry will be scribbled and drain in crucible; silica flour and carborundum powder (mixing by 1:1～2 mass ratioes) is used to be embedded by bar shaped pin blank; put into high-temperature process in melt infiltration furnace; treatment temperature is 1300 DEG C; 3kPa it is evacuated in stove; Ar gas using flow as 2L/min is as protective gas, about time of penetration 70h, generates density (or porosity) and is about 1.9～2.1g/cm3Bar shaped blank after siliconising.
Step 7, processes pin standard component；The bar shaped pin blank clamping infiltrated by melt, on lathe, cuts into pin standard component.Then pin standard component is carried out ultrasonic waves for cleaning, drying, obtain Two-dimensional Carbon/silico-carbo SiClx composite pin finished product.
Embodiment 2:
Step 1, makes two-dimensional flat plate precast body.(thickness ensures more than pin diameter and leaves allowance) is the most successively tiled with tiling (0 °) and oblique paving (45 °) direction with two dimension carbon cloth, the graphite planar using surface to be equipped with hole (8～15 × 8～15mm arrangement mode) flattens carbon cloth, segmental support is fixed on support, using carbon fiber through each hole, two-dimensional flat plate precast body made by vertical sewing carbon cloth.
Step 2, deposits pyrolytic carbon boundary layer.By cvd furnace at two-dimensional flat plate precast body internal penetration pyrolytic carbon protective layer; its process conditions are: depositing temperature is 800 DEG C, and cvd furnace is evacuated to 3kPa, and the propylene gas using flow as 4L/min is as deposition gases; the Ar gas of 8L/min is as protective gas, and sedimentation time is about 70h；Obtain depositing the two-dimensional flat plate precast body of pyrolytic carbon protective layer.
Step 3, demoulding depositing silicon silicon substrate.Being impregnated with the two-dimensional flat plate internal penetration silicon carbide substrate of pyrolytic carbon protective layer, process conditions are: depositing temperature is 1050 DEG C, and cvd furnace is evacuated to 3kPa, and the Ar gas using flow as 8L/min is as protective gas, and flow is the H of 8L/min2Gas, as carrier gas, reacts in trichloromethyl silane is loaded into cvd furnace inside two-dimensional flat plate, generates silicon carbide substrate, and is deposited on the pyrolytic carbon protective layer within described two-dimensional flat plate, generates density (or porosity) and is about 1.3～1.5g/cm3Composite material flat plate；The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is about 70h.
Step 4, processes bar shaped pin blank；First with grinding machine, the upper and lower surface of two-dimensional flat plate is polished, it is ensured that thickness is more than pin diameter (leaving allowance).Cleaning up planar surface, to be as the criterion without granule, then flat plate cutting is slit into cross section is foursquare strip blank.
Step 5, depositing silicon carbide layers；Bar shaped blank is put into stove depositing silicon carbide layers, and depositing temperature is 1050 DEG C, and cvd furnace is evacuated to 3kPa, and the Ar gas using flow as 8L/min is as protective gas, and flow is the H of 8L/min2Gas, as carrier gas, reacts in pin blank inside and surface in trichloromethyl silane is loaded into cvd furnace, generates density (or porosity) and be about 1.5～1.7g/cm3Composite blank.The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is about 70h.
Step 6, RMI process；The bar shaped pin blank of bn slurry will be scribbled and drain in crucible; silica flour and carborundum powder (mixing by 1:1～2 mass ratioes) is used to be embedded by bar shaped pin blank; put into high-temperature process in melt infiltration furnace; treatment temperature is 1350 DEG C; 2kPa it is evacuated in stove; Ar gas using flow as 3L/min is as protective gas, about time of penetration 70h, generates density (or porosity) and is about 1.9～2.1g/cm3Bar shaped blank after siliconising.
Step 7, processes pin standard component；The bar shaped pin blank clamping infiltrated by melt, on lathe, cuts into pin standard component.Then pin standard component is carried out ultrasonic waves for cleaning, drying, obtain Two-dimensional Carbon/silico-carbo SiClx composite pin finished product.
Embodiment 3:
Step 1, makes two-dimensional flat plate precast body.(thickness ensures more than pin diameter and leaves allowance) is the most successively tiled with tiling (0 °) and oblique paving (45 °) direction with two dimension carbon cloth, the graphite planar using surface to be equipped with hole (8～15 × 8～15mm arrangement mode) flattens carbon cloth, segmental support is fixed on support, using carbon fiber through each hole, two-dimensional flat plate precast body made by vertical sewing carbon cloth.
Step 2, deposits pyrolytic carbon boundary layer.By cvd furnace at two-dimensional flat plate precast body internal penetration pyrolytic carbon protective layer; its process conditions are: depositing temperature is 900 DEG C, and cvd furnace is evacuated to 1kPa, and the propylene gas using flow as 5L/min is as deposition gases; the Ar gas of 10L/min is as protective gas, and sedimentation time is about 70h；Obtain depositing the two-dimensional flat plate precast body of pyrolytic carbon protective layer.
Step 3, demoulding depositing silicon silicon substrate.Being impregnated with the two-dimensional flat plate internal penetration silicon carbide substrate of pyrolytic carbon protective layer, process conditions are: depositing temperature is 1100 DEG C, and cvd furnace is evacuated to 1kPa, and the Ar gas using flow as 10L/min is as protective gas, and flow is the H of 10L/min2Gas, as carrier gas, reacts in trichloromethyl silane is loaded into cvd furnace inside two-dimensional flat plate, generates silicon carbide substrate, and is deposited on the pyrolytic carbon protective layer within described two-dimensional flat plate, generates density (or porosity) and is about 1.3～1.5g/cm3Composite material flat plate；The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is about 70h.
Step 4, processes bar shaped pin blank；First with grinding machine, the upper and lower surface of two-dimensional flat plate is polished, it is ensured that thickness is more than pin diameter (leaving allowance).Cleaning up planar surface, to be as the criterion without granule, then flat plate cutting is slit into cross section is foursquare strip blank.
Step 5, depositing silicon carbide layers；Bar shaped blank is put into stove depositing silicon carbide layers, and depositing temperature is 1100 DEG C, and cvd furnace is evacuated to 1kPa, and the Ar gas using flow as 10L/min is as protective gas, and flow is the H of 10L/min2Gas, as carrier gas, reacts in pin blank inside and surface in trichloromethyl silane is loaded into cvd furnace, generates density (or porosity) and be about 1.5～1.7g/cm3Composite blank.The temperature of described trichloromethyl silane is 30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is about 70h.
Step 6, RMI process；The bar shaped pin blank of bn slurry will be scribbled and drain in crucible; silica flour and carborundum powder (mixing by 1:1～2 mass ratioes) is used to be embedded by bar shaped pin blank; put into high-temperature process in melt infiltration furnace; treatment temperature is 1400 DEG C; 1kPa it is evacuated in stove; Ar gas using flow as 5L/min is as protective gas, about time of penetration 70h, generates density (or porosity) and is about 1.9～2.1g/cm3Bar shaped blank after siliconising.
Step 7, processes pin standard component；The bar shaped pin blank clamping infiltrated by melt, on lathe, cuts into pin standard component.Then pin standard component is carried out ultrasonic waves for cleaning, drying, obtain Two-dimensional Carbon/silico-carbo SiClx composite pin finished product.
Shear strength under ceramic matric composite room temperature prepared by employing CVI+RMI technique (embodiment 2) is about 80～100Mpa；Obtain shear strength under ceramic matric composite room temperature prepared by employing CVI and be about 81～105MPa.Both strength differences are little, but owing to CVI sedimentation rate is relatively slow, ceramic matric composite total heat needs 11～12 stove prepared by CVI technique, and ceramic matric composite total heat needs 7～8 stove prepared by CVI+RMI technique.From figure 3, it can be seen that pin surface carbon fiber prepared by CVI technique is more obvious, also there is partial operation to damage, under high-temperature condition, be susceptible to oxidation；The coated parcel in pin surface prepared by CVI+RMI technique, more can antioxidation under high-temperature condition.
The present invention uses two dimension carbon cloth tiling and oblique paving to prepare two-dimensional flat plate precast body by the method for carbon fiber vertical puncturing again; first at precast body internal penetration pyrolytic carbon protective layer; then CVI (chemical vapor infiltration)+RMI (reaction melt method of impregnation) technique is used to prepare Two-dimensional Carbon/silico-carbo SiClx composite pin; the pin not only intensity of preparation is high and preparation cost is relatively low, and carbon/silico-carbo SiClx composite property difference is less, stability is high.
Claims (10)
1. Two-dimensional Carbon/silico-carbo SiClx composite pin precast body, including multilayer two-dimension carbon cloth, its
It is characterised by:
In described multilayer two-dimension carbon cloth, the angle of the corresponding fiber of adjacent two layers two dimension carbon cloth is 45 °,
Described Two-dimensional Carbon/silico-carbo SiClx composite pin precast body also includes sewing structure, described sewing
Structure includes the multiple U-shaped fiber of squarely matrix distribution, and multiple U-shaped fibers are from multilayer two-dimension carbon cloth
One side vertically penetrates multilayer two-dimension carbon cloth.
Two-dimensional Carbon the most according to claim 1/silico-carbo SiClx composite pin precast body, it is special
Levy and be: adjacent two ends arranging U-shaped fiber in described square matrix are additionally provided with 1 U-shaped fibre
Dimension.
3. a preparation method for Two-dimensional Carbon/silico-carbo SiClx composite pin precast body, its feature exists
In: comprise the following steps:
1) the graphite planar horizontal positioned in hole will be equipped with；
2) tile on graphite planar multilayer two-dimension carbon cloth, until the laminated thickness of two dimension carbon cloth meets pin
Follow closely diameter and leave allowance；The angle of the corresponding fiber of adjacent two layers two dimension carbon cloth is 45 °,
3) multilayer two-dimension carbon cloth is stepped up with graphite planar, graphite planar is holded up；
4) graphite planar is fixed with support；
5) use fiber vertically to sew carbon cloth by the hole arranged on graphite planar, make two-dimensional flat plate pre-
Body processed.
The preparation of Two-dimensional Carbon the most according to claim 3/silico-carbo SiClx composite pin precast body
Method, it is characterised in that:
Step 2) to be used the cellosilk in two dimension carbon cloth be vertical intertexture, during lamination, adjacent two layers
Carbon cloth angle at 45 °.
5. prefabricated according to a kind of Two-dimensional Carbon described in claim 3 or 4/silico-carbo SiClx composite pin
The preparation method of body, it is characterised in that:
The hole of graphite planar arranges according to the mode of 8～15 × 8～15mm.
6. a preparation method for Two-dimensional Carbon/silico-carbo SiClx composite pin, comprises the following steps:
1) two-dimensional flat plate precast body is made；
2) by cvd furnace at two-dimensional flat plate precast body internal penetration pyrolytic carbon protective layer；
3) it is being impregnated with the two-dimensional flat plate internal penetration silicon carbide substrate of pyrolytic carbon protective layer；
4) tooling pin nailing strip shape blank；
5) pin blank clamping is pressed on lathe figure paper size car cylinder and length, obtain Two-dimensional Carbon/silicon-
Composite material of silicon carbide pin finished product；
It is characterized in that: described step 1) particularly as follows:
1.1) the graphite planar horizontal positioned in hole will be equipped with；
1.2) tile on graphite planar multilayer two-dimension carbon cloth, until the laminated thickness of two dimension carbon cloth meets pin
Follow closely diameter and leave allowance；The corresponding fiber angle of adjacent two layers two dimension carbon cloth is 45 °,
1.3) multilayer two-dimension carbon cloth is stepped up with graphite planar, graphite planar is holded up；
1.4) by graphite planar and between fixing；
1.5) use fiber vertically to sew carbon cloth by the hole arranged on graphite planar, make two-dimensional flat plate pre-
Body processed.
The preparation method of Two-dimensional Carbon the most according to claim 6/silico-carbo SiClx composite pin,
It is characterized in that:
Step 4) and step 5) between also include:
A) pin blank is put into stove depositing silicon carbide layers；
B) the pin blank of bn slurry will be scribbled and drain in crucible, use silica flour and carborundum
Powder is pressed the mass ratio mixing of 1:1～2 and is embedded by pin blank, puts in melt infiltration furnace and carries out at RMI
Reason.
8. according to the preparation side of the Two-dimensional Carbon described in claim 6 or 7/silico-carbo SiClx composite pin
Method, it is characterised in that:
Step 2) process conditions be: depositing temperature is 600～1000 DEG C, and cvd furnace is evacuated to
1～10kPa, make using the propylene gas that flow is 2～8L/min as deposition gases, the Ar gas of 4～10L/min
For protective gas, sedimentation time is 60～100h；The two-dimensional flat plate obtaining depositing pyrolytic carbon protective layer is pre-
Body processed.
9. according to the preparation side of the Two-dimensional Carbon described in claim 6 or 7/silico-carbo SiClx composite pin
Method, it is characterised in that:
Step 3) process conditions be: depositing temperature is 1000～1200 DEG C, and cvd furnace is evacuated to
1～10kPa, using Ar gas that flow is 4～10L/min as protective gas, flow is 4～10L/min
H2Gas, as carrier gas, reacts in trichloromethyl silane is brought into cvd furnace inside two-dimensional flat plate, raw
Become silicon carbide substrate, and be deposited on the pyrolytic carbon protective layer within described two-dimensional flat plate, generate density
(or porosity) is about 1.3～1.5g/cm3Composite material flat plate；The temperature of described trichloromethyl silane is
30 DEG C～35 DEG C, H2Being 9～11 with the molal weight ratio of trichloromethyl silane, sedimentation time is
60～100h；
Step 5) process conditions be: depositing temperature is 1000～1200 DEG C, and cvd furnace is evacuated to
1～10kPa, using Ar gas that flow is 4～10L/min as protective gas, flow is 4～10L/min
H2 gas, as carrier gas, occurs in pin blank inside and surface in trichloromethyl silane is brought into cvd furnace
Reaction, generates density (or porosity) and is about 1.5～1.7g/cm3 composite bar shaped blanks.Described three
The temperature of chloromethyl silane is 30 DEG C～35 DEG C, the molal weight ratio of H2 and trichloromethyl silane be 9～
11, sedimentation time is 30～50h.
10. according to the preparation of the Two-dimensional Carbon described in claim 6 or 7/silico-carbo SiClx composite pin
Method, it is characterised in that:
RMI treatment temperature is 1300～1500 DEG C, is evacuated to 1～10kPa in stove, with flow is
The Ar gas of 2～8L/min, as protective gas, time of penetration 60～100h, makes density (or pore
Rate) it is about 1.9～2.1g/cm3Bar shaped blank after siliconising.
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