CN116283355B - Carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics - Google Patents
Carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics Download PDFInfo
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- 239000000919 ceramic Substances 0.000 title claims abstract description 75
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 58
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 58
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 44
- 238000013329 compounding Methods 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 41
- 230000008569 process Effects 0.000 title claims abstract description 33
- 239000002131 composite material Substances 0.000 claims abstract description 66
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000000835 fiber Substances 0.000 claims abstract description 42
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 28
- MFRIHAYPQRLWNB-UHFFFAOYSA-N sodium tert-butoxide Chemical compound [Na+].CC(C)(C)[O-] MFRIHAYPQRLWNB-UHFFFAOYSA-N 0.000 claims abstract description 28
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 12
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 10
- 239000000956 alloy Substances 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims description 42
- 210000001170 unmyelinated nerve fiber Anatomy 0.000 claims description 32
- 238000002360 preparation method Methods 0.000 claims description 31
- 238000006243 chemical reaction Methods 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 22
- 238000000151 deposition Methods 0.000 claims description 20
- 230000008021 deposition Effects 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 16
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 16
- 239000004744 fabric Substances 0.000 claims description 16
- 210000001161 mammalian embryo Anatomy 0.000 claims description 16
- 239000002296 pyrolytic carbon Substances 0.000 claims description 16
- 239000007789 gas Substances 0.000 claims description 10
- GKOPSNQLSIJHDS-UHFFFAOYSA-N 4-sulfanylcyclohexa-1,5-diene-1,4-dicarboxylic acid Chemical compound C1C=C(C=CC1(C(=O)O)S)C(=O)O GKOPSNQLSIJHDS-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 239000003345 natural gas Substances 0.000 claims description 9
- CAYHVMBQBLYQMT-UHFFFAOYSA-N 2-decyltetradecan-1-ol Chemical compound CCCCCCCCCCCCC(CO)CCCCCCCCCC CAYHVMBQBLYQMT-UHFFFAOYSA-N 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 8
- 238000005516 engineering process Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 8
- 239000004745 nonwoven fabric Substances 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 8
- 239000001294 propane Substances 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- VGBAECKRTWHKHC-UHFFFAOYSA-N cyclopenta-1,3-diene;1-ethenylcyclopenta-1,3-diene;iron(2+) Chemical compound [Fe+2].C=1C=C[CH-]C=1.[CH2-]C=C1C=CC=C1 VGBAECKRTWHKHC-UHFFFAOYSA-N 0.000 claims description 7
- 230000035484 reaction time Effects 0.000 claims description 7
- 239000000463 material Substances 0.000 abstract description 14
- -1 vinyl ferrocene Chemical compound 0.000 abstract description 9
- XIOFCJYPVMLOKU-UHFFFAOYSA-N 2-decyltetradecane Natural products CCCCCCCCCCCCC(C)CCCCCCCCCC XIOFCJYPVMLOKU-UHFFFAOYSA-N 0.000 abstract description 6
- 238000005452 bending Methods 0.000 abstract description 6
- 229920002554 vinyl polymer Polymers 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 239000002243 precursor Substances 0.000 abstract description 3
- 230000008595 infiltration Effects 0.000 abstract description 2
- 238000001764 infiltration Methods 0.000 abstract description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007259 addition reaction Methods 0.000 description 3
- 238000011068 loading method Methods 0.000 description 3
- 125000003396 thiol group Chemical group [H]S* 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000005475 siliconizing Methods 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910001208 Crucible steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 238000005886 esterification reaction Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000013001 point bending Methods 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 230000001012 protector Effects 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
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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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/50—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with inorganic materials
- C04B41/51—Metallising, e.g. infiltration of sintered ceramic preforms with molten metal
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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
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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
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
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- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/80—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone of only ceramics
- C04B41/81—Coating or impregnation
- C04B41/85—Coating or impregnation with inorganic materials
- C04B41/88—Metals
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16D—COUPLINGS FOR TRANSMITTING ROTATION; CLUTCHES; BRAKES
- F16D69/00—Friction linings; Attachment thereof; Selection of coacting friction substances or surfaces
- F16D69/02—Composition of linings ; Methods of manufacturing
- F16D69/023—Composite materials containing carbon and carbon fibres or fibres made of carbonizable material
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- 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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- C04B2235/50—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
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Abstract
The invention relates to the field of brake materials, in particular to a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics; the invention adopts FeSi75 modified C/C-SiC composite material to prepare the carbon ceramic brake disc of ceramic uniform composite carbon fiber; 2-decyl tetradecane p-mercapto terephthalate reacts with vinyl ferrocene, propenyl silsesquioxane and sodium tert-butoxide to obtain a carbon fiber treating agent; the bundling property and smoothness of the fiber bundles of the carbon fiber precursor are improved, and the infiltration effect of the C/C porous composite material and FeSi75 alloy powder is improved, so that the bending strength and the fracture toughness of the carbon ceramic brake disc are improved.
Description
Technical Field
The invention relates to the technical field of brake materials, in particular to a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics.
Background
The C/C-SiC composite material is used as a thermal structural material in the 80 th century at the earliest, such as an engine of a spacecraft and a thermal protector of a spacecraft, and is a novel structural and functional material capable of well meeting the condition of 1650 ℃. By the beginning of the 90 s of the 20 th century, the talents of the German aerospace institute (DLR) WalterKrenkel et al began to study the C/C-SiC composite material prepared by the RMI method, and intensive researches on the process and performance of the preparation of the C/SiC brake disc by the RMI method and the structural design of the C/SiC brake disc were carried out. Full-size C/C-SiC brake disc models of high-speed trains and buses are produced in 1994-1997. By 2001, the C/C-SiC brake disc has been successfully applied to a Porsche 911GT2 brake device for the first time. In 2008, C/C-SiC has begun to be mass produced, and has begun to gradually replace cast iron and cast steel brake discs used on heavy-duty automobiles. In addition, C/C-SiC composites have also begun to be used on elevators and cranes.
The Chinese patent with the application number of CN201510991783.9 discloses a preparation method of a carbon ceramic brake material, which comprises the following steps: 1) Preparing a first carbon fiber preform; 2) Preparing a phenolic resin solution; 3) Preparing mixed slurry of phenolic resin and ceramic powder; 4) Preparing a second carbon fiber preform; 5) Drying the second carbon fiber preform; 6) Hot pressing and solidifying the dried preform; 7) Cracking the carbon/phenolic-ceramic composite material; 8) The first porous carbon/carbon-ceramic powder composite material is subjected to high temperature treatment. The invention also provides a preparation method of the carbon ceramic brake disc, which comprises the following steps of: 9) Preprocessing; 10 Siliconizing the first brake disc; 11 Finish machining. The invention greatly reduces the manufacturing cycle and cost of the carbon ceramic brake material, has simple process and good repeatability, and is suitable for industrialized mass production.
The Chinese patent with the application number of CN201810988553.0 discloses a preparation method of a carbon ceramic brake disc. The preparation method of the carbon ceramic brake disc combines a vapor deposition method, a precursor dipping method and a melt siliconizing method, and adjusts parameters in the reaction by limiting the types and the amounts of solvents and gases in each step, thereby realizing the good and bad complementation of each method, and providing the carbon ceramic brake disc with excellent mechanical property, high fracture toughness, good thermal conductivity, small thermal expansion coefficient and excellent thermal shock resistance.
The Chinese patent with the application number of CN202010190744.X discloses a preparation method of a carbon ceramic brake disc, which comprises the following steps: 1) Preparing a carbon fiber preform; 2) CVI densification: loading the prepared carbon fiber preform into a CVI furnace, performing CVI densification by taking natural gas as carbon source gas, and obtaining a C/C brake disc after pre-deposition, accelerated deposition and gap adjustment deposition; 3) Graphitizing: and (5) placing the C/C brake disc into a high-temperature heat treatment furnace to obtain the required carbon ceramic brake disc. The invention can accurately and effectively control the density and the open porosity of the carbon Tao Yuzhi body, and the density of the carbon Tao Yuzhi body prepared by the invention can be accurately controlled at (1.45+/-0.05) g/cm 3 The open porosity was (25.+ -.5)%.
The existence of the ceramic phase SiC and Si in the carbon ceramic brake disc prepared by the patent and the prior art can obviously improve the friction coefficient of the carbon ceramic brake material, but in the braking process, the existence of the Si phase in the material can cause high-frequency vibration, so that the brake material has high wear rate and unstable braking; in addition, the preparation process of the carbon ceramic brake disc is complex, particularly in the slurry impregnation stage, multiple impregnations are needed, the production period is long, and therefore the production cost is high.
Disclosure of Invention
The invention aims to provide a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics, so as to solve the problems in the background art.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics comprises the following operation steps:
s1: weighing 20-30 parts by weight of a C/C porous composite material, 100-200 parts by weight of a carbon fiber treating agent, stirring for 5-10 hours at 50-70 ℃, filtering, and drying to obtain a uniformly dispersed C/C porous composite material;
s2: adding 3-7 parts of FeSi75 alloy powder, heating, and after the reaction is finished, preparing a FeSi75 modified C/C-SiC composite material;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: and finally, processing and forming the composite material to obtain the carbon ceramic brake disc.
Preferably, the reaction temperature of S2 is 1350-1500 ℃ and the time is 0.5-2h.
Preferably, the heat treatment temperature of the S3 is 1600-1700 ℃.
Preferably, the preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, 45-70 parts of mixed gas of natural gas and propane is introduced, the ratio is 1:1, and pyrolytic carbon is deposited in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
Preferably, the deposition pyrolytic carbon temperature is 900-1200 ℃, and the deposition time is 800-1000h.
Preferably, the high temperature heat treatment temperature is 1800-2500 ℃.
Preferably, the preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
Preferably, the preparation method of the carbon fiber treating agent comprises the following steps:
s1: according to parts by weight, 350-450 parts of 2-decyl tetradecanol, 220-305 parts of p-mercapto terephthalic acid and 3-8 parts of sulfuric acid are heated and stirred for reaction;
s2: continuously adding 0.3-3.8 parts of vinylferrocene, 0.03-0.8 part of propenyl silsesquioxane, 0.03-0.8 part of sodium tert-butoxide and 1000-2000 parts of white oil, heating, stirring, reacting, and distilling to remove the white oil to obtain the carbon fiber treating agent.
Preferably, the S1 is stirred at 60-80 ℃ for 1-4h.
Preferably, the S2 is stirred at 60-70 ℃ for reaction for 100-200min.
Reaction mechanism:
in the invention, 2-decyl tetradecyl is subjected to esterification reaction with p-mercapto terephthalic acid to obtain 2-decyl tetradecyl p-mercapto terephthalic acid ester; and (3) carrying out sulfhydryl addition reaction on the 2-decyl tetradecane p-sulfhydryl terephthalate, vinyl ferrocene, propenyl silsesquioxane and sodium tert-butoxide to obtain the carbon fiber treating agent.
The beneficial effects are that: compared with the prior art, the carbon ceramic brake disc compounding process for uniformly compounding the carbon fibers with the ceramics has the following remarkable effects:
1. the carbon ceramic brake disc prepared by the invention can generate the maximum braking force immediately in the initial stage of braking, so that the friction and wear performance can be greatly improved, and the linear wear rate is greatly reduced.
2. The C/C-SiC composite material of the carbon ceramic brake disc has the advantages of low density, high temperature resistance, high strength, stable friction performance, small abrasion loss, long service life and the like, and because the SiC ceramic hard material is introduced into the C/C-SiC composite material as a matrix, the bending strength and the fracture toughness are effectively improved.
3. 2-decyl tetradecane sulfhydryl terephthalate, vinyl ferrocene, propenyl silsesquioxane and sodium tert-butoxide undergo sulfhydryl addition reaction to obtain a long carbon chain carbon fiber treating agent; the bundling property and smoothness of the fiber bundles of the carbon fiber precursor can be improved, and the infiltration effect of the C/C porous composite material and FeSi75 alloy powder is improved, so that the bending strength and fracture toughness of the carbon ceramic brake disc are improved.
Detailed Description
The following describes the invention in more detail. The description of these embodiments is provided to assist understanding of the present invention, but is not intended to limit the present invention. In addition, the technical features of the embodiments of the present invention described below may be combined with each other as long as they do not collide with each other.
According to the specific service environment of the brake disc, 6 groups of samples are tested for bending strength and fracture toughness, and all test tests are completed by a CMT4304 type universal tester (Shenzhen SANS material detection Co., ltd.).
(1) Flexural Strength
The bending strength of the material was tested using a three-point bending method. For the samples prepared from the three-dimensional needled preforms, the dimensions were 60mm by 9mm by 3mm, the span was 50mm and the loading speed was 0.5mm/min. Samples were taken in a direction parallel to the friction surface. According to astm c1341-00 standard.
(2) Fracture toughness
The fracture toughness of the material was tested using a single-side notched beam method. The test piece was 40mm by 7mm by 3.5mm in size, 30mm in span and 0.05mm/min in loading speed, according to the ASTME399-74 standard. Samples were taken in a direction parallel to the friction surface.
(3) Frictional wear Property
The friction and wear performance of the material is tested by adopting an MM-1000 friction and wear testing machine produced by the West Anshun machine electric research institute.
Example 1: a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics comprises the following operation steps:
s1: weighing 20g of C/C porous composite material, 100g of carbon fiber treating agent, stirring for 5 hours at 50 ℃, filtering, and drying to obtain uniformly dispersed C/C porous composite material;
s2: adding 3g of FeSi75 alloy powder, heating, and after the reaction is finished, preparing a FeSi75 modified C/C-SiC composite material;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: and finally, processing and forming the composite material to obtain the carbon ceramic brake disc.
The reaction temperature of S2 is 1350 ℃ and the reaction time is 0.5h.
The heat treatment temperature of the S3 is 1600 ℃.
The preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, 45g of mixed gas of natural gas and propane is introduced, the ratio is 1:1, and pyrolytic carbon is deposited in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
The deposition pyrolytic carbon temperature is 900 ℃, and the deposition time is 800 hours.
The high-temperature heat treatment temperature is 1800 ℃.
The preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
The preparation method of the carbon fiber treating agent comprises the following steps:
s1: 350g of 2-decyl tetradecanol, 220g of p-mercapto terephthalic acid, 3g of sulfuric acid and stirring and reacting at 60 ℃ for 1h;
s2: continuously adding 0.3g of vinylferrocene, 0.03g of propenyl silsesquioxane, 0.03g of sodium tert-butoxide, 1000g of white oil, stirring at 60 ℃ for reaction for 100min, and distilling to remove the white oil to obtain the carbon fiber treating agent.
Example 2: a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics comprises the following operation steps:
s1: weighing 24g of C/C porous composite material, 140g of carbon fiber treating agent, stirring at 55 ℃ for 6 hours, filtering, and drying to obtain uniformly dispersed C/C porous composite material;
s2: adding 4g of FeSi75 alloy powder, heating, and after the reaction is finished, preparing a FeSi75 modified C/C-SiC composite material;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: and finally, processing and forming the composite material to obtain the carbon ceramic brake disc.
The reaction temperature of S2 is 1400 ℃ and the reaction time is 1h.
The heat treatment temperature of the S3 is 1640 ℃.
The preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, 50g of mixed gas of natural gas and propane is introduced, the ratio is 1:1, and pyrolytic carbon is deposited in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
The deposition pyrolytic carbon temperature is 1000 ℃, and the deposition time is 850h.
The high-temperature heat treatment temperature is 2000 ℃.
The preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
The preparation method of the carbon fiber treating agent comprises the following steps:
s1: 380g of 2-decyl tetradecanol, 250g of p-mercapto terephthalic acid, 4g of sulfuric acid and stirring and reacting for 2 hours at 65 ℃;
s2: continuously adding 1g of vinylferrocene, 0.2g of propenyl silsesquioxane, 0.2g of sodium tert-butoxide, 1400g of white oil, stirring at 65 ℃ for reaction for 140min, and distilling to remove the white oil to obtain the carbon fiber treating agent.
Example 3: a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics comprises the following operation steps:
s1: weighing 28g of C/C porous composite material, 180g of carbon fiber treating agent, stirring at 65 ℃ for 8 hours, filtering, and drying to obtain uniformly dispersed C/C porous composite material;
s2: adding 6g of FeSi75 alloy powder, heating, and after the reaction is finished, preparing a FeSi75 modified C/C-SiC composite material;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: and finally, processing and forming the composite material to obtain the carbon ceramic brake disc.
The reaction temperature of the S2 is 1450 ℃ and the reaction time is 1h.
The heat treatment temperature of the S3 is 1680 ℃.
The preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, introducing 65g of mixed gas of natural gas and propane in a ratio of 1:1, and depositing pyrolytic carbon in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
The deposition pyrolytic carbon temperature is 1100 ℃, and the deposition time is 950h.
The high-temperature heat treatment temperature is 2300 ℃.
The preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
The preparation method of the carbon fiber treating agent comprises the following steps:
s1: 420g of 2-decyl tetradecanol, 280g of p-mercapto terephthalic acid, 7g of sulfuric acid and stirring for reaction at 75 ℃ for 3 hours;
s2: continuously adding 3g of vinylferrocene, 0.6g of propenyl silsesquioxane, 0.6g of sodium tert-butoxide and 1800g of white oil, stirring at 65 ℃ for reacting for 180min, and distilling to remove the white oil to obtain the carbon fiber treating agent.
Example 4: a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics comprises the following operation steps:
s1: weighing 30g of C/C porous composite material, 200g of carbon fiber treating agent, stirring at 70 ℃ for 10 hours, filtering, and drying to obtain uniformly dispersed C/C porous composite material;
s2: 7g of FeSi75 alloy powder is added, the temperature is raised, and after the reaction is finished, the FeSi75 modified C/C-SiC composite material is prepared;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: and finally, processing and forming the composite material to obtain the carbon ceramic brake disc.
The reaction temperature of S2 is 1500 ℃ and the reaction time is 2h.
The heat treatment temperature of the S3 is 1700 ℃.
The preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, 70g of mixed gas of natural gas and propane is introduced, the ratio is 1:1, and pyrolytic carbon is deposited in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
The deposition pyrolytic carbon temperature is 1200 ℃, and the deposition time is 1000 hours.
The high-temperature heat treatment temperature is 2500 ℃.
The preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
The preparation method of the carbon fiber treating agent comprises the following steps:
s1: 450g of 2-decyl tetradecanol, 305g of p-mercapto terephthalic acid, 8g of sulfuric acid and stirring and reacting for 4 hours at 80 ℃;
s2: continuously adding 3.8g of vinylferrocene, 0.8g of propenyl silsesquioxane, 0.8g of sodium tert-butoxide, 2000g of white oil, stirring at 70 ℃ for reaction for 200min, and distilling to remove the white oil to obtain the carbon fiber treating agent.
Comparative example 1: a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics comprises the following operation steps:
s1: weighing 20g of C/C porous composite material, 100g of carbon fiber treating agent, stirring for 5 hours at 50 ℃, filtering, and drying to obtain uniformly dispersed C/C porous composite material;
s2: adding 3g of FeSi75 alloy powder, heating, and after the reaction is finished, preparing a FeSi75 modified C/C-SiC composite material;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: and finally, processing and forming the composite material to obtain the carbon ceramic brake disc.
The reaction temperature of S2 is 1350 ℃ and the reaction time is 0.5h.
The heat treatment temperature of the S3 is 1600 ℃.
The preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, 45g of mixed gas of natural gas and propane is introduced, the ratio is 1:1, and pyrolytic carbon is deposited in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
The deposition pyrolytic carbon temperature is 900 ℃, and the deposition time is 800 hours.
The high-temperature heat treatment temperature is 1800 ℃.
The preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
The preparation method of the carbon fiber treating agent comprises the following steps:
s1: 350g of 2-decyl tetradecanol, 220g of p-mercapto terephthalic acid, 3g of sulfuric acid and stirring and reacting at 60 ℃ for 1h;
s2: continuously adding 0.03g of propenyl silsesquioxane, 0.03g of sodium tert-butoxide and 1000g of white oil, stirring at 60 ℃ for reaction for 100min, and distilling to remove the white oil to obtain the carbon fiber treating agent.
Comparative example 2: a carbon ceramic brake disc compounding process for uniformly compounding carbon fibers with ceramics comprises the following operation steps:
s1: weighing 20g of C/C porous composite material, 100g of carbon fiber treating agent, stirring for 5 hours at 50 ℃, filtering, and drying to obtain uniformly dispersed C/C porous composite material;
s2: adding 3g of FeSi75 alloy powder, heating, and after the reaction is finished, preparing a FeSi75 modified C/C-SiC composite material;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: and finally, processing and forming the composite material to obtain the carbon ceramic brake disc.
The reaction temperature of S2 is 1350 ℃ and the reaction time is 0.5h.
The heat treatment temperature of the S3 is 1600 ℃.
The preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, 45g of mixed gas of natural gas and propane is introduced, the ratio is 1:1, and pyrolytic carbon is deposited in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
The deposition pyrolytic carbon temperature is 900 ℃, and the deposition time is 800 hours.
The high-temperature heat treatment temperature is 1800 ℃.
The preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
The preparation method of the carbon fiber treating agent comprises the following steps:
s1: 350g of 2-decyl tetradecanol, 220g of p-mercapto terephthalic acid, 3g of sulfuric acid and stirring and reacting at 60 ℃ for 1h;
s2: continuously adding 0.3g of vinylferrocene, 0.03g of sodium tert-butoxide and 1000g of white oil, stirring at 60 ℃ for reaction for 100min, and distilling to remove the white oil to obtain the carbon fiber treating agent.
The test results of the carbon ceramic brake disc prepared by the specific embodiment are shown in the following table 1:
as can be seen from table 1: adding 2-decyl tetradecane to generate sulfhydryl addition reaction with vinyl ferrocene, propenyl silsesquioxane and sodium tert-butoxide to obtain the carbon fiber treating agent. The line wear rate can reach 0.29 mu m/time; the bending strength can reach 153 MPa, and the fracture toughness is 9.8MPa.m 1/2 The method comprises the steps of carrying out a first treatment on the surface of the The vinyl ferrocene, propenyl silsesquioxane and sodium tert-butoxide have synergistic effects, and the technical effects can be reduced without adding any one of the vinyl ferrocene, propenyl silsesquioxane and sodium tert-butoxide.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, and yet fall within the scope of the invention.
Claims (9)
1. A carbon ceramic brake disc compounding process for uniformly compounding ceramic with carbon fibers is characterized by comprising the following steps of: the operation steps are as follows:
s1: weighing 20-30 parts by weight of a C/C porous composite material, 100-200 parts by weight of a carbon fiber treating agent, stirring for 5-10 hours at 50-70 ℃, filtering, and drying to obtain a uniformly dispersed C/C porous composite material;
s2: adding 3-7 parts of FeSi75 alloy powder, heating, and after the reaction is finished, preparing a FeSi75 modified C/C-SiC composite material;
s3: then carrying out heat treatment on the FeSi75 modified C/C-SiC composite material under a vacuum condition;
s4: finally, processing and forming the composite material to obtain the carbon ceramic brake disc;
the preparation method of the carbon fiber treating agent comprises the following steps:
step 1: according to parts by weight, 350-450 parts of 2-decyl tetradecanol, 220-305 parts of p-mercapto terephthalic acid and 3-8 parts of sulfuric acid are heated and stirred for reaction;
step 2: continuously adding 0.3-3.8 parts of vinylferrocene, 0.03-0.8 part of propenyl silsesquioxane, 0.03-0.8 part of sodium tert-butoxide and 1000-2000 parts of white oil, heating, stirring, reacting, and distilling to remove the white oil to obtain the carbon fiber treating agent.
2. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 1, wherein the process comprises the following steps of: the reaction temperature of the S2 is 1350-1500 ℃ and the reaction time is 0.5-2h.
3. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 1, wherein the process comprises the following steps of: the heat treatment temperature of the S3 is 1600-1700 ℃.
4. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 1, wherein the process comprises the following steps of: the preparation method of the C/C porous composite material comprises the following steps:
s1: under the protection of argon, 45-70 parts of mixed gas of natural gas and propane is introduced, the ratio is 1:1, and pyrolytic carbon is deposited in the three-dimensional needled C fiber preform;
s2: and then carrying out high-temperature heat treatment to obtain the C/C porous composite material.
5. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 4, wherein the process comprises the following steps of: the deposition pyrolytic carbon temperature is 900-1200 ℃, and the deposition time is 800-1000h.
6. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 4, wherein the process comprises the following steps of: the high-temperature heat treatment temperature is 1800-2500 ℃.
7. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 4, wherein the process comprises the following steps of: the preparation method of the three-dimensional needled C fiber preform comprises the following steps:
s1: preparing the C fibers into a short fiber tire net and a non-woven fabric;
s2: overlapping the 0 degree non-woven cloth, the short fiber tire net and the 90 degree non-woven cloth in sequence;
s3: and then, the fibers at the short fiber embryo net are led to the vertical direction by utilizing the needling technology, so that the short fiber embryo net layer and the non-woven layer are integrated into a whole, and the required three-dimensional needled C fiber preform is prepared.
8. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 1, wherein the process comprises the following steps of: the step 1 is stirred and reacted for 1 to 4 hours at the temperature of 60 to 80 ℃.
9. The carbon-ceramic brake disc compounding process for uniformly compounding ceramic carbon fibers according to claim 1, wherein the process comprises the following steps of: and the step 2 is stirred and reacted for 100-200min at the temperature of 60-70 ℃.
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