CN106966751A - High-performance and low-cost C/C SiC ceramic matrix composite material brake discs and preparation method and application - Google Patents
High-performance and low-cost C/C SiC ceramic matrix composite material brake discs and preparation method and application Download PDFInfo
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- CN106966751A CN106966751A CN201611049125.9A CN201611049125A CN106966751A CN 106966751 A CN106966751 A CN 106966751A CN 201611049125 A CN201611049125 A CN 201611049125A CN 106966751 A CN106966751 A CN 106966751A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000463 material Substances 0.000 title abstract description 22
- 239000011153 ceramic matrix composite Substances 0.000 title abstract description 6
- 239000002131 composite material Substances 0.000 claims abstract description 123
- 238000000034 method Methods 0.000 claims abstract description 69
- 230000008595 infiltration Effects 0.000 claims abstract description 38
- 238000001764 infiltration Methods 0.000 claims abstract description 38
- 239000002243 precursor Substances 0.000 claims abstract description 26
- 239000000126 substance Substances 0.000 claims abstract description 22
- 238000003763 carbonization Methods 0.000 claims abstract description 16
- 238000012545 processing Methods 0.000 claims abstract description 16
- 238000000197 pyrolysis Methods 0.000 claims abstract description 16
- 238000013461 design Methods 0.000 claims abstract description 6
- 238000000280 densification Methods 0.000 claims abstract description 4
- 239000007789 gas Substances 0.000 claims description 33
- 239000000835 fiber Substances 0.000 claims description 30
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 28
- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 19
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 229920003257 polycarbosilane Polymers 0.000 claims description 17
- 230000008569 process Effects 0.000 claims description 15
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910052786 argon Inorganic materials 0.000 claims description 14
- 238000007254 oxidation reaction Methods 0.000 claims description 14
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000011259 mixed solution Substances 0.000 claims description 11
- 239000003085 diluting agent Substances 0.000 claims description 10
- 238000009413 insulation Methods 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000012159 carrier gas Substances 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 239000001294 propane Substances 0.000 claims description 7
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 7
- 208000037656 Respiratory Sounds Diseases 0.000 claims description 6
- 238000003754 machining Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 6
- 239000000243 solution Substances 0.000 claims description 6
- 238000007598 dipping method Methods 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 5
- 238000005470 impregnation Methods 0.000 claims description 4
- 238000005336 cracking Methods 0.000 claims description 3
- 238000004132 cross linking Methods 0.000 claims description 3
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 claims description 3
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 claims description 3
- 238000007711 solidification Methods 0.000 claims description 3
- 230000008023 solidification Effects 0.000 claims description 3
- 239000003345 natural gas Substances 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 claims 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- IPBRIJAYQVOWRM-UHFFFAOYSA-N trichloromethylsilicon Chemical compound [Si]C(Cl)(Cl)Cl IPBRIJAYQVOWRM-UHFFFAOYSA-N 0.000 claims 1
- 238000005087 graphitization Methods 0.000 abstract description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 33
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 11
- 235000013312 flour Nutrition 0.000 description 11
- 239000011159 matrix material Substances 0.000 description 11
- 239000000377 silicon dioxide Substances 0.000 description 11
- 238000001467 acupuncture Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 8
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 238000006243 chemical reaction Methods 0.000 description 6
- 239000002296 pyrolytic carbon Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 229920000049 Carbon (fiber) Polymers 0.000 description 5
- 239000004917 carbon fiber Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 229910002804 graphite Inorganic materials 0.000 description 5
- 239000010439 graphite Substances 0.000 description 5
- 238000013016 damping Methods 0.000 description 4
- 238000011049 filling Methods 0.000 description 4
- 229920002239 polyacrylonitrile Polymers 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000004744 fabric Substances 0.000 description 3
- 238000000227 grinding Methods 0.000 description 3
- 239000010410 layer Substances 0.000 description 3
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 description 3
- 238000010923 batch production Methods 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005587 bubbling Effects 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 239000011229 interlayer Substances 0.000 description 2
- 239000012705 liquid precursor Substances 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000036632 reaction speed Effects 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000002153 silicon-carbon composite material Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 229910001018 Cast iron Inorganic materials 0.000 description 1
- 229910001208 Crucible steel Inorganic materials 0.000 description 1
- 241000482237 Senegalia mellifera Species 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- AZFVLHQDIIJLJG-UHFFFAOYSA-N chloromethylsilane Chemical compound [SiH3]CCl AZFVLHQDIIJLJG-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000006193 liquid solution Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 230000035800 maturation Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000012113 quantitative test Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- -1 trichloromethyl silicon Alkane Chemical class 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
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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
- 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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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
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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
- C04B35/64—Burning or sintering processes
- C04B35/65—Reaction sintering of free metal- or free silicon-containing compositions
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- 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
- C04B41/46—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 organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
- C04B41/495—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon applied to the substrate as oligomers or polymers
- C04B41/4983—Polycarbosilanes, i.e. polymers with a -Si-C-Si-chain; Polysilazanes, i.e. polymers with a -Si-N-Si-chain; Polysilathianes, i.e. polymers with a -Si-S-Si-chain
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- 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
- C04B41/5093—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 with elements other than metals or carbon
- C04B41/5096—Silicon
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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
- C04B41/82—Coating or impregnation with organic materials
- C04B41/84—Compounds having one or more carbon-to-metal of carbon-to-silicon linkages
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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
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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
- F16D65/00—Parts or details
- F16D65/02—Braking members; Mounting thereof
- F16D65/12—Discs; Drums for disc brakes
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5212—Organic
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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
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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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
- F16D2200/00—Materials; Production methods therefor
- F16D2200/0034—Materials; Production methods therefor non-metallic
Abstract
The present invention relates to a kind of high-performance and low-cost C/C SiC ceramic matrix composite material brake discs and preparation method and application, preparation method includes：Brake disc precast body is carbonized, the brake disc precast body densification after carbonization is obtained by C/C composites using chemical vapor infiltration area method；Then it is heat-treated in an inert atmosphere, to improve the degree of graphitization of composite；It is machined again, obtains C/C composite bodies；Using siliconising method processing C/C composite bodies are melted, C/C SiC ceramic matrix composite material brake discs are obtained；Chemical vapor infiltration area method or precursor infiltration and pyrolysis method is recycled to handle C/C SiC ceramic matrix composite material brake discs；Obtained product is machined into final design size, composite brake disk finished product is produced.C/C SiC ceramic matrix composite material brake discs that the present invention is provided and preparation method thereof, can reduce preparation cost, improve mechanical property, heat conductivility and the friction and wear behavior of brake disc.
Description
Technical field
The present invention relates to technical field of composite preparation, and in particular to a kind of high-performance and low-cost C/C-SiC composite woods
Expect brake disc and preparation method and application.
Background technology
High-speed railway (hereinafter referred to as " high ferro ") is the trend of world's track traffic development, what current China's high ferro put into effect
Mileage has reached 10000 kilometers, more than 10000 kilometers of the high-speed railway built, it is contemplated that to Chinese high ferro in 2021 it is total in
Journey will rank first in the world more than 30000 kilometers.While high ferro is fast-developing, its security also gets most of the attention, wherein braking skill
Art is most important for safe train operation.At present, the mode of braking that high ferro is used mainly includes electric braking and air damping, this
There are the modes of braking such as eddy-current brake, magnetic rail braking and windage braking outside.Wherein air damping as a kind of brake hard means,
When bullet train meets with the emergencies such as earthquake, power failure or train fault, it is necessary to ensure that the train of high speed can be defined
Stopped within distance, it is ensured that the safety of train operation, therefore air damping is also known as " foundation brake ", be in high ferro brakes not
The important component that can or lack.
Air damping is mainly using reel braking and the discharge plate shape flowing mode of Multiple disc brake two, and its difference essentially consists in reel
Braking is that brake disc is installed on axletree, and Multiple disc brake is to install brake disc in wheel web side.Current brake disk material
Mainly based on cast iron, cast steel and forged steel, its advantage is mainly manufacturing technology maturation, and performance can meet the relatively low train of speed
Brake request.Constantly develop however as train to " high speed " and " heavy loading " direction, brake disc is proposed both have compared with
High braking energy has the requirement of lighter weight again, but existing disc material wears no resistance, and abrasion is very fast, and radiating effect is not
It is good, fire check is easily produced, heavier-weight, friction produces larger noise, thus is not well positioned to meet train speed needs
The growth requirement of continuous improvement.
The content of the invention
For defect of the prior art, present invention aims at provide a kind of high-performance and low-cost C/C-SiC composite woods
Expect brake disc and preparation method and application, to reduce preparation cost, improve mechanical property, heat conductivility and the friction of brake disc
Polishing machine.
To achieve the above object, the technical scheme that provides of the present invention is：
In a first aspect, the invention provides a kind of preparation method of composite brake disk, comprising the following steps：
S1:Brake disc precast body is carbonized, then the brake disc precast body after carbonization is caused using chemical vapor infiltration area method
Densification, obtains C/C composites；Wherein, brake disc precast body is to use polyacrylonitrile-radical oxidization fiber fiber with D refraction statics
Into；S2:C/C composites are heat-treated in an inert atmosphere, C/C composite bodies are obtained；S3:Using melting siliconising
Method handles C/C composite bodies, obtains C/C-SiC composite brake disks；S4:By C/C-SiC composite brakes disk profit
Handled with chemical vapor infiltration area method or precursor infiltration and pyrolysis method；Wherein, the precursor of chemical vapor infiltration area method is trichlorine
Methyl-monosilane, the precursor solution of precursor infiltration and pyrolysis method is Polycarbosilane and the mixed solution of divinylbenzene；S5:Will step
The product that rapid S4 is obtained is machined into final design size, produces composite brake disk finished product.
It should be noted that three dimensional needle acupuncture manipulation is to circulate 0 ° of laminated cloth of individual layer, tire net, 90 ° of laminated cloths and tire net successively
Superposition, is then made using the method for relay-type acupuncture perpendicular to laying direction introducing polyacrylonitrile-radical oxidization fiber fiber
Moving plate precast body.During step S3 melting siliconising, silicon and matrix C reaction generation carborundum are melted, body after room temperature is cooled to
Product, which is shunk, causes the generation of micro-crack；Composite is during the high temperature of melting siliconising is gradually cooling to room temperature, due to multiple
Fiber in condensation material, pyrolytic carbon, the thermal coefficient of expansion of carborundum and remaining silicon have differences so that being produced in cooling procedure should
Power, produces micro-crack in the presence of stress.Step S4 be in order to fill out envelope C/C-SiC composite brake disks crackle, reduction
Si residual volume in composite, improves the creep-resistant property of composite.
In the further embodiment of the present invention, in step S1, chemical vapor infiltration area method is specially：With propane, naturally
One or more in gas and propylene are carbon-source gas, and nitrogen and/or hydrogen are diluent gas, and it is 900~1200 to ooze accumulated temperature degree
DEG C, overstocked power is oozed for 1000~5000Pa, oozes the long-pending time for 50~200h；Wherein, the volume ratio of carbon-source gas and diluent gas
For 1:(1~4).
In the further embodiment of the present invention, in step S2, the treatment temperature of heat treatment is 1800~2400 DEG C, place
1~5h of reason time, inert atmosphere is argon gas and/or nitrogen.Heat treatment is to improve the degree of graphitization of composite.
In the further embodiment of the present invention, in step S3, melting siliconising method is specially：Under vacuum, will
C/C composite bodies are placed in the silica flour that particle diameter is 100~300 mesh, then 1500~1700 DEG C of 1.5~3.5h of insulation, then
1750~2050 DEG C of 5~60min of insulation.
It should be noted that：, can be close according to the expections of C/C-SiC composite brake disks in order to meet reaction than needs
Degree and C/C composite body density difference calculate melting siliconising during need generation SiC content, so as to calculate
The theoretical Si amounts needed in Si, C reaction, 2.2~5 times of Si powder for weighing the theoretical amount for needing Si are placed in graphite crucible, Si powder
Purity be preferably greater than or equal to 99%, and C/C brake disc base substrates are buried in Si powder, are then placed in high temperature furnace and are melted
Melt siliconising, obtained C/C-SiC composite brakes disk, density is preferably 1.8~2.2g/cm3.In order to save production cost,
Multiple graphite crucibles equipped with Si powder and C/C composite bodies can also be stacked and placed on to progress melting in high temperature furnace simultaneously to ooze
Silicon.Melt during siliconising, molten silicon is oozed under the collective effect of capillary force and gravity by the hole of C/C composite bodies
Enter to material internal, while being reacted generation SiC matrix phase with the pyrolytic carbon that touches, obtain C/C-SiC composite systems
Moving plate, a small amount of unreacted melt of si is remained in C/C-SiC composite brake disks.
In the further embodiment of the present invention, in step S4, chemical vapor infiltration area method is specially：With trichloromethyl silicon
Alkane is precursor (CH3SiCl3, MTS), hydrogen is carrier gas, and argon gas is carrier gas, oozes accumulated temperature degree for 900~1400 DEG C, oozes overstocked
Power is 300~1200Pa, oozes the long-pending time for 15~25h；Wherein, the volume ratio of trichloromethyl silane, hydrogen and argon gas is 1:(7
~10):(3~5).It should be noted that MTS is liquid precursor raw material, hydrogen is carrier gas, by bubbling mode by gaseous state
MTS brings reative cell into, uses inert gas argon gas as diluent gas to adjust MTS pyrolytic reaction speed.
In the further embodiment of the present invention, in step S4, precursor infiltration and pyrolysis method is specially：By C/C-SiC
Composite brake disk is impregnated in 30~60min of mixed solution of Polycarbosilane and divinylbenzene, and dipping temperature is 60~100
DEG C, impregnation pressure is 1~2MPa, then 110~200 DEG C of solidification 2~3.5h of crosslinking, then 1100~1300 DEG C of 0.5~2h of cracking；
The step of repeating precursor infiltration and pyrolysis method is until crackle is filled out envelope completely；Wherein, the mixing of Polycarbosilane and divinylbenzene
The mass fraction of Polycarbosilane is 40%~60% in solution.
In the further embodiment of the present invention, in step S1, the temperature of carbonization is 1000~1400 DEG C, and the time is 45
~75h, carbonization is carried out under vacuum.
The present invention further embodiment in, after step S2 heat treatment, obtain C/C composite bodies it
Before, in addition to the step of machining, specifically include：C/C composite material surfaces after heat treatment are processed into bolt hole and fixed
Position hole；And/or the size of C/C composite surroundings is processed, and reserved in thickness direction more than 1~2mm following process
Amount.It should be noted that：C/C composites after heat treatment are machined, can be the aperture chi according to brake disc
Very little to require, C/C composite material surfaces after heat treatment process bolt hole and positioning hole；Will by the negative common difference of brake disc size
Ask, the size to C/C composite surroundings is processed, and 1~2mm following process surplus is reserved in thickness direction.Step
S5 machining can carry out disposable thoroughly processing or herein step machining according to the size of brake disc
On the basis of, obtained C/C-SiC composite brakes disk is subjected to surface using skive on grinding machine to rubbing surface
Processing, the 1~2mm reserved before removal following process surplus.
Second aspect, the invention provides the composite brake disk prepared according to the method for any of the above-described.
The third aspect, the invention provides above-mentioned composite brake disk answering in manufacture train especially manufactures high ferro
With.
Composite brake disk that the present invention is provided and preparation method thereof, there is following good effect：(1) present invention is carried first
Going out can there is provided one kind as the reinforcement of the biradical composite brake disk of high ferro carbon pottery with polyacrylonitrile-radical oxidization fiber fiber
The manufacturing technology of batch production.Oxidization fiber fiber is very cheap with respect to carbon fiber price, and system is greatly reduced when preparing precast body
Standby cost；Oxidization fiber fibrous fracture elongation percentage is high, and pliability is good, is adapted to acupuncture, and carbon fiber is fragile material, and surface is ditch
Slot structure, the resistance that fiber is subject to during acupuncture is big, and easily coming off or be broken from hook thorn skids off, therefore oxidization fiber precast body is fine compared with carbon
Dimension precast body surface is smooth, and the introducing quantity and length of Z-direction fiber are high, and preparation-obtained carbon Tao Shuan based composites Z-directions are led
Hot coefficient is high, and inter-layer bonding force is strong, and friction and wear behavior is excellent, is particularly suitable for doing train especially high ferro disc material.(2)
The present invention is combined using chemical vapor infiltration area method (CVI) or precursor infiltration and pyrolysis method (PIP) to the C/C-SiC after melting siliconising
Material brake disc carries out filling out envelope Crack handling, and the C/C-Si composite brake disks after processing are practically free of crackle, improve it
Mechanical property；And PIP methods handle produced unnecessary C and can also carried out instead with Si remaining in material after melting siliconising processing
SiC should be generated, the residual volume of Si in composite is reduced, the creep-resistant property of composite is improved.(3) present invention selection
Melting siliconising is carried out under two different hot environments, this reactive mode can be such that Si is reacted more with the C in matrix
Fully, the closed pore quantity in C/C-SiC composites and the content of remaining silicon are reduced, composite creep-resistant property, is improved
Even property and mechanical property, reduce frictional wear amount.(4) mechanical property can be caused to reduce when pyrolytic carbon too high levels in matrix,
Ceramic matrix too high levels can then be caused when too low, brake disc fragility is high, while coefficient of friction is too high.The present invention is by adjusting base
The content of pyrolytic carbon in body, realizes the control to matrix carbon and carborundum content in composite, so that composite
Mechanical property and friction and wear behavior reach effect in a balanced way.
The additional aspect and advantage of the present invention will be set forth in part in the description, and will partly become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Brief description of the drawings
Fig. 1 is the melting siliconising schematic diagram in the embodiment of the present invention.
Reference：
1- high-temperature heaters；2- sensing heating bodies；3- silica flours；4- graphite crucibles；5-C/C composite bodies.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation is described, it is clear that described embodiment is only a part of embodiment of the invention, rather than whole embodiments.It is based on
Embodiment in the present invention, it is every other that those of ordinary skill in the art are obtained under the premise of creative work is not made
Embodiment, belongs to the scope of protection of the invention.
Experimental method in following embodiments, is conventional method unless otherwise specified.
Test material used, is to be commercially available from conventional reagent shop unless otherwise specified in following embodiments.
Quantitative test in following examples, is respectively provided with three repetition experiments, and data are the average value of three repetition experiments
Or mean+SD.
The present invention provides a kind of preparation method of composite brake disk, it is characterised in that comprise the following steps：
S1:Brake disc precast body is carbonized, then the brake disc precast body after carbonization is caused using chemical vapor infiltration area method
Densification, obtains C/C composites；Wherein, brake disc precast body is to use polyacrylonitrile-radical oxidization fiber fiber with D refraction statics
Into；The temperature of carbonization is 1000~1400 DEG C, and the time is 45~75h, and carbonization is carried out under vacuum；Chemical vapor infiltration area method
Specially：With the one or more in propane, natural gas and propylene for carbon-source gas, nitrogen and/or hydrogen are diluent gas, are oozed
Accumulated temperature degree is 900~1200 DEG C, oozes overstocked power for 1000~5000Pa, oozes the long-pending time for 50~200h；Wherein, carbon-source gas and
The volume ratio of diluent gas is 1:(1~4).
S2:C/C composites are heat-treated in an inert atmosphere, the degree of graphitization of composite is improved；Heat treatment
Treatment temperature be 1800~2400 DEG C, 1~5h of processing time, inert atmosphere be argon gas and/or nitrogen.By the C/ after heat treatment
C composite be machined obtaining C/C composite bodies, specifically includes：By the C/C composite material surfaces after heat treatment
Process bolt hole and positioning hole；And/or the size of C/C composite surroundings is processed, and 1 is reserved in thickness direction~
2mm following process surplus.
S3:Using siliconising method processing C/C composite bodies are melted, C/C-SiC composite brake disks are obtained；Melting is oozed
Silicon process is specially：Under vacuum, C/C composite bodies are placed in the silica flour that particle diameter is 100~300 mesh, then
1500~1700 DEG C of 1.5~3.5h of insulation, then 1750~2050 DEG C of 5~60min of insulation.
S4:C/C-SiC composite brake disks are filled out using chemical vapor infiltration area method or precursor infiltration and pyrolysis method
Seal micro-crack processing；Wherein, the precursor of chemical vapor infiltration area method is trichloromethyl silane, the pioneer of precursor infiltration and pyrolysis method
Liquid solution is the mixed solution of Polycarbosilane and divinylbenzene；Chemical vapor infiltration area method is specially：With trichloromethyl silane
(CH3SiCl3, MTS) and it is precursor, hydrogen is carrier gas, and argon gas is carrier gas, oozes accumulated temperature degree for 900~1400 DEG C, oozes overstocked power
For 300~1200Pa, the long-pending time is oozed for 15~25h；Wherein, the volume ratio of trichloromethyl silane, hydrogen and argon gas is 1:(7~
10):(3~5)；Precursor infiltration and pyrolysis method is specially：Under vacuum, C/C-SiC composite brake disks are impregnated in
30~60min of mixed solution of Polycarbosilane and divinylbenzene, dipping temperature be 60~100 DEG C, impregnation pressure be 1~
2MPa, then 110~200 DEG C of solidification 2~3.5h of crosslinking, then 1100~1300 DEG C of 0.5~2h of cracking；Precursor dipping is repeated to split
Solution is until crackle is filled out envelope completely；Wherein, the quality of Polycarbosilane is divided in the mixed solution of Polycarbosilane and divinylbenzene
Number is 40%~60%.
S5:The obtained products of step S4 are machined into final design size, composite brake disk finished product is produced.
Composite brake disk and its preparation side that the present invention provided with reference to specific embodiment the present invention is provided
Method is described further.
Embodiment one
0 ° of laminated cloth of individual layer, tire net, 90 ° of laminated cloths, tire nets are circulated into superposition successively, then using the side of relay-type acupuncture
Method is introducing polyacrylonitrile (PAN) base oxidization fiber fiber perpendicular to laying direction, and brake disc precast body is made；In vacuum condition
Under, brake disc precast body is subjected to carbonization treatment, carbonization time 60 hours at a temperature of 1200 DEG C；Recycle chemical vapor infiltration product
Brake disc precast body after carbonization is densified by method, and using propane as carbon-source gas, nitrogen is the body of diluent gas, propane and nitrogen
Product is than being 1:2, accumulated temperature degree is oozed for 1150 DEG C, overstocked power is oozed for 3000Pa, the long-pending time is oozed for 120h, obtains density for 1.3g/cm3
C/C composites.
By C/C composites under the protection of argon gas, high-temperature heat treatment is carried out in 2200 DEG C, processing time is 2h；Then
It is machined, is required according to the aperture size of brake disc, the C/C composite material surfaces after the heat treatment processes spiral shell
Keyhole and positioning hole；By the negative common difference requirement of brake disc size, the size to the C/C composite surroundings after the heat treatment is entered
Row processing, and 1mm following process surplus is reserved in thickness direction, obtain C/C composite bodies.
C/C composite bodies are placed in the graphite crucible equipped with silica flour, progress melting siliconising in high temperature furnace are put into, such as
Shown in Fig. 1, it is specially：Under vacuum, C/C composite bodies are buried in the silica flour that particle diameter is 300 mesh, then
1650 DEG C of insulation 2.5h, then 1850 DEG C of insulation 10min, obtain density for 1.95g/cm3C/C-SiC composite brake disks；
Wherein silica flour purity is 99.5%, and the amount of silica flour is 4 times of reaction theory requirements.
Obtained C/C-SiC composite brakes disk is carried out filling out envelope Crack handling using chemical vapor infiltration area method, with three
Chloromethyl silane (CH3SiCl3, MTS) and it is liquid precursor raw material, hydrogen is carrier gas, is brought into gaseous state MTS by bubbling mode
Reative cell, uses inert gas argon gas as diluent gas to adjust MTS pyrolytic reaction speed, oozes accumulated temperature degree for 1150 DEG C,
Overstocked power is oozed for 500Pa, the long-pending time is oozed for 20h, and the volume ratio of trichloromethyl silane, hydrogen and argon gas is 1：9：3, obtain density
For 1.97g/cm3C/C-SiC composite brake disks；Then obtained product is carried out being machined into final design chi
It is very little, Surface Machining is carried out to rubbing surface using skive on grinding machine, more than the 1mm reserved before removal following process
Amount, obtains composite brake disk finished product.
Embodiment two
0 ° of laminated cloth of individual layer, tire net, 90 ° of laminated cloths, tire nets are circulated into superposition successively, then using the side of relay-type acupuncture
Method is introducing polyacrylonitrile (PAN) base oxidization fiber fiber perpendicular to laying direction, and brake disc precast body is made；In vacuum condition
Under, brake disc precast body is subjected to carbonization treatment, carbonization time 60 hours at a temperature of 1200 DEG C；Recycle chemical vapor infiltration product
Brake disc precast body after carbonization is densified by method, and using propane as carbon-source gas, nitrogen is the body of diluent gas, propane and nitrogen
Product is than being 1:2, accumulated temperature degree is oozed for 1150 DEG C, overstocked power is oozed for 3000Pa, the long-pending time is oozed for 120h, obtains density for 1.3g/cm3
C/C composites.
By C/C composites under the protection of argon gas, high-temperature heat treatment is carried out in 2200 DEG C, processing time is 2h；Then
It is machined, is required according to the aperture size of brake disc, the C/C composite material surfaces after the heat treatment processes spiral shell
Keyhole and positioning hole；By the negative common difference requirement of brake disc size, the size to the C/C composite surroundings after the heat treatment is entered
Row processing, and 1mm following process surplus is reserved in thickness direction, obtain C/C composite bodies.
C/C composite bodies are placed in the graphite crucible equipped with silica flour, progress melting siliconising in high temperature furnace are put into, such as
Shown in Fig. 1, it is specially：Under vacuum, C/C composite bodies are buried in the silica flour that particle diameter is 300 mesh, then
1650 DEG C of insulation 2.5h, then 1850 DEG C of insulation 10min, obtain density for 1.95g/cm3C/C-SiC composite brake disks；
Wherein silica flour purity is 99.5%, and the amount of silica flour is 4 times of reaction theory requirement.
Obtained C/C-SiC composite brakes disk is carried out filling out envelope Crack handling using precursor infiltration and pyrolysis method, with
The mixed solution of Polycarbosilane (PCS) and divinylbenzene is as precursor solution, wherein Polycarbosilane and divinylbenzene
The mass fraction of Polycarbosilane is 45% in mixed solution, and C/C-SiC composite brake disks are impregnated in into Polycarbosilane and two
30min in the mixed solution of vinyl benzene, dipping temperature is 70 DEG C, and impregnation pressure is 1.5MPa, then solidifies at 150 DEG C and hands over
Join 3h, then 1h is cracked under 1200 DEG C of high temperature；The above-mentioned precursor infiltration and pyrolysis method of repetition 5 times, obtains density for 1.96g/cm3's
C/C-SiC composite brake disks.Then obtained product is carried out being machined into final design size, adopted on grinding machine
Surface Machining is carried out to rubbing surface with skive, the 1mm reserved before removal following process surplus obtains composite
Brake disc finished product.
The composite brake disk that the embodiment of the present invention one and embodiment two are prepared carries out performance measurement, specific to survey
Method for testing and test result are as follows.
Method of testing：1 is carried out respectively to the composite brake disk that embodiment one and embodiment two are prepared:1 power
Bench test, confirms its friction and wear behavior.Experimental condition is that 40 less urgent brakings are repeated under 400km/h speed
(each under dry state and hygrometric state condition to carry out 20 times), and the friction and wear behavior of brake disc friction surface is tested.
Test result：Concrete outcome is as shown in table 1 below.
The composite brake disk the performance test results of table 1
The composite brake disk that embodiment one and embodiment two are prepared all is shown in hygrometric state wheels-locked testing
The dry and wet state coefficient of friction rate of change for the composite brake disk that excellent performance, wherein embodiment one are prepared is only
2.6%, the dry and wet state coefficient of friction rate of change for the composite brake disk that embodiment two is prepared is only 2.7%, therefore all
It there's almost no the problem of hygrometric state frictional behaviour decays.
It should be noted that situation about enumerating except above-described embodiment one and embodiment two, from other preparation methods
Parameter is also feasible.
C/C-SiC composite brake disks that the present invention is provided and preparation method thereof, can reduce preparation cost, improve system
Mechanical property, heat conductivility and the friction and wear behavior of Moving plate.
Composite brake disk that the present invention is provided and preparation method thereof, there is following good effect：(1) present invention is carried first
Going out can there is provided one kind as the reinforcement of the biradical composite brake disk of high ferro carbon pottery with polyacrylonitrile-radical oxidization fiber fiber
The manufacturing technology of batch production.Oxidization fiber fiber is very cheap with respect to carbon fiber price, and system is greatly reduced when preparing precast body
Standby cost；Oxidization fiber fibrous fracture elongation percentage is high, and pliability is good, is adapted to acupuncture, and carbon fiber is fragile material, and surface is ditch
Slot structure, fiber is subject to during acupuncture resistance is big, easily skids off from hooking to come off or be broken in thorn, thus oxidization fiber fiber preform compared with
Carbon fiber precast body surfacing, the introducing quantity and length of Z-direction fiber is high, preparation-obtained carbon Tao Shuan based composites Z
High to thermal conductivity factor, inter-layer bonding force is strong, and friction and wear behavior is excellent, is particularly suitable for doing train especially high ferro brake disc material
Material.(2) present invention uses chemical vapor infiltration area method (CVI) or precursor infiltration and pyrolysis method (PIP) to the C/C- after melting siliconising
SiC ceramic matrix composite material brake disc carries out filling out envelope Crack handling, and the C/C-Si composite brake disks after processing are practically free of crackle, carry
Its high mechanical property；And the unnecessary C produced by the processing of PIP methods can also be with Si remaining in material after melting siliconising processing
Reaction generation SiC is carried out, the residual volume of Si in composite is reduced, improves the creep-resistant property of composite.(3) this hair
Bright selection carries out melting siliconising under two different hot environments, and this reactive mode can be such that Si is reacted with the C in matrix
More fully, reduce the closed pore quantity in C/C-SiC composites and the content of remaining silicon, improve composite creep resistance
Energy, uniformity and mechanical property, reduce frictional wear amount.(4) mechanical property can be caused when pyrolytic carbon too high levels in matrix
Reduction, can then cause ceramic matrix too high levels when too low, brake disc fragility is high, while coefficient of friction is too high.The present invention passes through
The content of the pyrolytic carbon in matrix is adjusted, the control to matrix carbon and carborundum content in composite is realized, so that compound
The mechanical property and friction and wear behavior of material reach effect in a balanced way.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means to combine specific features, structure, material or the feature that the embodiment or example are described
It is contained at least one embodiment of the present invention or example.In this manual, need not to the schematic representation of above-mentioned term
Identical embodiment or example must be directed to.Moreover, specific features, structure, material or the feature of description can be any
Combined in an appropriate manner in individual or multiple embodiments or example.In addition, in the case of not conflicting, the technology of this area
Not be the same as Example or the feature of example and non-be the same as Example or example described in this specification can be combined by personnel
And combination.
Although embodiments of the invention have been shown and described above, it is to be understood that above-described embodiment is example
Property, it is impossible to limitation of the present invention is interpreted as, one of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, changed, replacing and modification, and the essence of appropriate technical solution is departed from various embodiments of the present invention skill
The scope of art scheme, it all should cover among the claim of the present invention and the scope of specification.
Claims (10)
1. a kind of preparation method of composite brake disk, it is characterised in that comprise the following steps：
S1:Brake disc precast body is carbonized, then the brake disc precast body after the carbonization is caused using chemical vapor infiltration area method
Densification, obtains C/C composites；Wherein, the brake disc precast body is to use polyacrylonitrile-radical oxidization fiber fiber with three dimensional needle
Thorn is formed；
S2:The C/C composites are heat-treated in an inert atmosphere, C/C composite bodies are obtained；
S3:The C/C composite bodies are handled using siliconising method is melted, C/C-SiC composite brake disks are obtained；
S4:By the C/C-SiC composite brakes disk using chemical vapor infiltration area method or precursor infiltration and pyrolysis method at
Reason；Wherein, the precursor of the chemical vapor infiltration area method is trichloromethyl silane, the precursor of the precursor infiltration and pyrolysis method
Solution is the mixed solution of Polycarbosilane and divinylbenzene；
S5:The obtained products of the step S4 are machined into final design size, composite brake disk finished product is produced.
2. the preparation method of composite brake disk according to claim 1, it is characterised in that：In the step S1, institute
Stating chemical vapor infiltration area method is specially：With in propane, natural gas and propylene one or more for carbon-source gas, nitrogen and/or
Hydrogen is diluent gas, oozes accumulated temperature degree for 900~1200 DEG C, oozes overstocked power for 1000~5000Pa, ooze the long-pending time for 50~
200h；Wherein, the volume ratio of the carbon-source gas and the diluent gas is 1:(1~4).
3. the preparation method of composite brake disk according to claim 1, it is characterised in that：In the step S2, institute
The treatment temperature for stating heat treatment is 1800~2400 DEG C, and processing time is 1~5h, and the inert atmosphere is argon gas and/or nitrogen.
4. the preparation method of composite brake disk according to claim 1, it is characterised in that：In the step S3, institute
Stating melting siliconising method is specially：Under vacuum, the C/C composite bodies are placed in the silicon that particle diameter is 100~300 mesh
In powder, then 1500~1700 DEG C of 1.5~3.5h of insulation, then 1750~2050 DEG C of 5~60min of insulation.
5. the preparation method of composite brake disk according to claim 1, it is characterised in that in the step S4, institute
Stating chemical vapor infiltration area method is specially：Using trichloromethyl silane as precursor, hydrogen is carrier gas, and argon gas is carrier gas, oozes accumulated temperature
Spend for 900~1400 DEG C, ooze overstocked power for 300~1200Pa, ooze the long-pending time for 15~25h；Wherein, the trichloromethyl silicon
The volume ratio of alkane, the hydrogen and the argon gas is 1:(7~10):(3~5).
6. the preparation method of composite brake disk according to claim 1, it is characterised in that：In the step S4, institute
Stating precursor infiltration and pyrolysis method is specially：The C/C-SiC composite brakes disk is impregnated in Polycarbosilane and divinyl
30~60min of mixed solution of benzene, the dipping temperature is 60~100 DEG C, and the impregnation pressure is 1~2MPa, then 110~
200 DEG C of solidification 2~3.5h of crosslinking, then 1100~1300 DEG C of 0.5~2h of cracking；The step of repeating the precursor infiltration and pyrolysis method
Until crackle is filled out envelope completely；Wherein, the quality of Polycarbosilane is divided in the mixed solution of the Polycarbosilane and divinylbenzene
Number is 40%~60%.
7. the preparation method of composite brake disk according to claim 1, it is characterised in that：In the step S1, institute
The temperature for stating carbonization is 1000~1400 DEG C, and the time is 45~75h, and the carbonization is carried out under vacuum.
8. the preparation method of composite brake disk according to claim 1, it is characterised in that：In the institute of the step S2
After stating heat treatment, before obtaining the C/C composite bodies, in addition to the step of machining, specifically include：Will be described
C/C composite material surfaces after heat treatment process bolt hole and positioning hole；And/or to the chi of the C/C composites surrounding
It is very little to be processed, and reserve 1~2mm following process surplus in thickness direction.
9. the composite brake disk that the method described in any one of claim 1~8 is prepared.
10. application of the composite brake disk in manufacture train especially manufactures high ferro described in claim 9.
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