CN109485444A - A kind of preparation method of silicon carbide fiber reinforced composite material - Google Patents
A kind of preparation method of silicon carbide fiber reinforced composite material Download PDFInfo
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- CN109485444A CN109485444A CN201811588718.1A CN201811588718A CN109485444A CN 109485444 A CN109485444 A CN 109485444A CN 201811588718 A CN201811588718 A CN 201811588718A CN 109485444 A CN109485444 A CN 109485444A
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- 229910010271 silicon carbide Inorganic materials 0.000 title claims abstract description 170
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 title claims abstract description 169
- 239000000463 material Substances 0.000 title claims abstract description 48
- 239000003733 fiber-reinforced composite Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000000835 fiber Substances 0.000 claims abstract description 106
- 238000000034 method Methods 0.000 claims abstract description 25
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 20
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 230000008569 process Effects 0.000 claims abstract description 12
- 239000010703 silicon Substances 0.000 claims abstract description 11
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 11
- 239000011248 coating agent Substances 0.000 claims description 55
- 238000000576 coating method Methods 0.000 claims description 55
- 239000002002 slurry Substances 0.000 claims description 54
- 239000002131 composite material Substances 0.000 claims description 46
- 239000007789 gas Substances 0.000 claims description 36
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 36
- 238000009941 weaving Methods 0.000 claims description 36
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 26
- 239000004917 carbon fiber Substances 0.000 claims description 26
- 230000002787 reinforcement Effects 0.000 claims description 26
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 24
- 239000003054 catalyst Substances 0.000 claims description 18
- 238000000151 deposition Methods 0.000 claims description 17
- 239000003999 initiator Substances 0.000 claims description 13
- 229910052786 argon Inorganic materials 0.000 claims description 12
- 238000000498 ball milling Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 239000002296 pyrolytic carbon Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000005229 chemical vapour deposition Methods 0.000 claims description 10
- 238000004062 sedimentation Methods 0.000 claims description 10
- 239000003292 glue Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 9
- 239000012159 carrier gas Substances 0.000 claims description 8
- 239000003085 diluting agent Substances 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 8
- 238000007711 solidification Methods 0.000 claims description 8
- 230000008023 solidification Effects 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 239000003431 cross linking reagent Substances 0.000 claims description 7
- 239000002270 dispersing agent Substances 0.000 claims description 7
- 239000011863 silicon-based powder Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000000178 monomer Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- -1 agitated Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 229910003978 SiClx Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 238000010008 shearing Methods 0.000 claims description 4
- DWAWYEUJUWLESO-UHFFFAOYSA-N trichloromethylsilane Chemical compound [SiH3]C(Cl)(Cl)Cl DWAWYEUJUWLESO-UHFFFAOYSA-N 0.000 claims description 4
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical group NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 3
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- KWYHDKDOAIKMQN-UHFFFAOYSA-N N,N,N',N'-tetramethylethylenediamine Chemical group CN(C)CCN(C)C KWYHDKDOAIKMQN-UHFFFAOYSA-N 0.000 claims description 3
- 238000003763 carbonization Methods 0.000 claims description 3
- 238000005336 cracking 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
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical group [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims description 2
- 238000005520 cutting process Methods 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 10
- 238000005516 engineering process Methods 0.000 abstract description 8
- 230000002708 enhancing effect Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000005245 sintering Methods 0.000 abstract description 6
- 230000008901 benefit Effects 0.000 abstract description 5
- 238000001746 injection moulding Methods 0.000 abstract description 4
- 238000011049 filling Methods 0.000 abstract description 3
- 239000007791 liquid phase Substances 0.000 abstract description 3
- 229920001296 polysiloxane Polymers 0.000 abstract description 3
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000007788 liquid Substances 0.000 description 7
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical group [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 4
- 239000012298 atmosphere Substances 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000003960 organic solvent Substances 0.000 description 3
- 238000010422 painting Methods 0.000 description 3
- 239000012071 phase Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 208000037656 Respiratory Sounds Diseases 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 101710198474 Spike protein Proteins 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000003754 machining Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- SBEQWOXEGHQIMW-UHFFFAOYSA-N silicon Chemical compound [Si].[Si] SBEQWOXEGHQIMW-UHFFFAOYSA-N 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 101100373011 Drosophila melanogaster wapl gene Proteins 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 210000005056 cell body Anatomy 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 238000002513 implantation Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011268 mixed slurry Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000010943 off-gassing Methods 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 210000004483 pasc Anatomy 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000011208 reinforced composite material Substances 0.000 description 1
- 238000007634 remodeling Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009466 transformation Effects 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
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
- C04B35/573—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide obtained by reaction sintering or recrystallisation
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
- C04B2235/5248—Carbon, e.g. graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
- C04B2235/602—Making the green bodies or pre-forms by moulding
- C04B2235/6023—Gel casting
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- Manufacturing & Machinery (AREA)
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- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Ceramic Products (AREA)
Abstract
The preparation method of silicon carbide fiber reinforced composite material provided by the invention, silicon carbide fiber reinforced precast body is prepared using the characteristics of gel injection molding and forming technology in-situ solidifying, and after silicon carbide fiber reinforced precast body is dried, a part of liquid-phase silicone is reacted, which with the carbon in precast body, by reaction sintering technology generates silicon carbide, remaining hole in a part of silicon filling precast body, to obtain silicon carbide fiber reinforced composite material, tough effect is mended using the enhancing that silicon carbide fiber reinforced composite material prepared by this method can give full play to fiber, material density is high, also there is simple process, it is at low cost, the advantages that with short production cycle.
Description
Technical field
The present invention relates to technology field of ceramic matrix composite material, in particular to a kind of silicon carbide fiber reinforced composite material
Preparation method.
Background technique
Critical component of the reflecting mirror as large space optical sensor, it is necessary to meet that specific stiffness is high, thermal stability is good, can
Realize the performance requirements such as ultra lightweighting.Silicon carbide ceramics has high specific stiffness, good thermal stability, gradually substitutes glass
Glass, metal become the preferred material of large caliber reflecting mirror.But silicon carbide ceramics is most important as large caliber reflecting mirror one
Problem is its biggish brittleness, realizes that ultra lightweighting difficulty is larger.The carbon fiber of excellent in mechanical performance, silicon carbide fibre are added
Enter into silicon carbide ceramics matrix and silicon carbide fiber reinforced composite material is made, keeps material de- by fiber in fracture process
The mechanism such as viscous, crack deflection, fibrous fracture, spike protein gene, can largely improve the brittleness of silicon carbide ceramics, be real
The ultra lightweighting of existing reflecting mirror provides a practicable technological approaches.
Silicon carbide fiber reinforced composite material is prepared at present there are mainly three types of method, precursor infiltration and pyrolysis method (PIP method),
Chemical vapor infiltration (CVI method) and reaction sintering (RB method), PIP method and CVI method prepare composite material of silicon carbide temperature phase
To lower, be conducive to the high-temperature damage for avoiding fiber, but since preparation process limits, manufactured silicon carbide fiber reinforced composite wood
Material relative density can only achieve 90% or so, and the defects of stomata, crackle is more in composite material, and the presence of hole and crackle is not only
The mechanical property of material is influenced, mirror optics processing performance also will receive a degree of influence.With PIP method and CVI method phase
Than reaction sintering, which prepares silicon carbide fiber reinforced composite material, to be had consistency height, can prepare complex-shaped part, production cycle
Advantage short, at low cost.
It is German ECM company, ginseng that it is most representational, which to prepare silicon carbide fiber reinforced composite material, for reaction sintering
See M.G.S.Kutter, Cesic --- engineering material for optomechanical
Applications, SPIE, 2003, Vol.5179.The said firm develops the short carbon fiber reinforced that the commercial trade mark is CeSiC and is carbonized
Silicon composite is applied to optical mirror and its structural member.CeSiC prepares carbon fiber/carbon precast body using compression molding, it
Reaction-sintered prepares silicon carbide fiber reinforced composite material afterwards.But due in preparation process Carbon Fiber Damage it is serious, part carbon
Fiber and pasc reaction generate silicon carbide, and the composite material of silicon carbide toughness of preparation is about 4.6MPam1/2, toughness improves unknown
It is aobvious.Therefore there is an urgent need to one kind can either realize that high tenacity is able to achieve the silicon carbide fiber reinforced composite material of high-compactness again
Preparation method.
Summary of the invention
Have in view of that, it is necessary in view of the defects existing in the prior art, provide the fiber increasing of a kind of high tenacity, high-compactness
The preparation method of strong composite material of silicon carbide.
To achieve the above object, the present invention adopts the following technical solutions:
A kind of preparation method of silicon carbide fiber reinforced composite material, the fiber are carbon fiber, are included the following steps:
Chopped strand or 3 D weaving body is made in carbon fiber；
The fiber surface of the chopped strand or 3 D weaving body is deposited into composite coating, the composite coating internal layer is to split
Carbon coating is solved, outer layer is coat of silicon carbide；
The chopped strand that surface is deposited with composite coating is prepared into short fiber reinforced silicon carbide precast body, or will be fine
The 3 D weaving body that dimension table face is deposited with composite coating is prepared into continuous fiber reinforcement silicon carbide precast body；
The short fiber reinforced silicon carbide precast body or the continuous fiber reinforcement silicon carbide precast body are dried；
It will be on the short fiber reinforced silicon carbide precast body or the continuous fiber reinforcement silicon carbide precast body after drying
High-purity silicon powder is placed on surface, and 1450-1550 DEG C of reaction-sintered is heated in vacuum environment, then be cooled to room temperature and obtain fiber
Enhance composite material of silicon carbide.
In some preferred embodiments, in the step of carbon fiber is made to chopped strand or 3 D weaving body,
Using carbon fiber as raw material, shear to obtain the chopped strand by shearing equipment, the length of the chopped strand exists
Between 0.5-5mm；
Using carbon fiber as raw material, the 3 D weaving body, the 3 D weaving body are obtained by three-dimensional four-way weaving
The volume content of middle fiber is between 40%-60%.
In some preferred embodiments, the fiber surface of the chopped strand or 3 D weaving body is being deposited into compound painting
In the step of layer, specifically include the following steps:
The chopped strand or fibrage body are placed in chemical vapor deposition stove, are heated to 400-800 after vacuumizing
It DEG C carries out handling except glue；
Except the chopped strand or fibrage body pass through chemical vapor deposition manner in the chopped strand after glue processing
Or the fiber surface of fibrage body deposits the composite coating；
It is carbon source that methane, ethylene or propylene are selected when depositing the Pyrolytic carbon coating, and high pure nitrogen is diluent gas and load
Gas, depositing temperature are 900-1100 DEG C, and sedimentation time is 10-100 hours, and gas pressure is in 500-2000Pa；Deposit the carbon
Using trichloromethyl silane as silicon carbide source when SiClx coating, for hydrogen as carrier gas and catalyst, high-purity argon gas is diluent gas, is sunk
Accumulated temperature degree is 1000-1200 DEG C, and sedimentation time is 10-100 hours, and gas pressure is in 500-2000Pa.
In some preferred embodiments, staple fiber is prepared into the chopped strand that surface is deposited with composite coating
The 3 D weaving body that fiber surface is deposited with composite coating is prepared into continuous fiber reinforcement by enhancing silicon carbide precast body
In the step of silicon carbide precast body, specifically include the following steps:
When the chopped strand that surface is deposited with composite coating is prepared into short fiber reinforced silicon carbide precast body, packet
Include following step:
One silicon carbide slurry is provided；
The chopped strand that surface is deposited with composite coating is added in the silicon carbide slurry, is uniformly mixed laggard
Row froth in vacuum, wherein the mass ratio of the chopped strand and silicon carbide micro-powder is 0.1-0.4:1；
The silicon carbide slurry is maintained between 20-30 DEG C, then catalyst and initiation is added in the silicon carbide slurry
Agent, and it is cured after obtain the short fiber reinforced silicon carbide precast body；
When to be prepared into continuous fiber reinforcement silicon carbide pre- for the 3 D weaving body that fiber surface is deposited with composite coating
When body processed, include the following steps:
One silicon carbide slurry is provided；
By the silicon carbide slurry froth in vacuum, and it is maintained at slurry temperature between 20-30 DEG C, then in the silicon carbide
Catalyst and initiator is added in slurry；
The 3 D weaving body that fiber surface is deposited with composite coating is placed in mold, is placed in vacuum drying oven together
Vacuumize process is carried out, is passed through the slurry in the mold later；
It is passed through high-pressure inert gas in the vacuum drying oven, so that the silicon carbide slurry is sufficiently impregnated into fibre by high pressure
It ties up inside knitted body, continuous fiber reinforcement silicon carbide precast body is obtained after solidification.
In some preferred embodiments, then in the silicon carbide slurry catalyst and initiator are added, and it is cured after
In the step of obtaining the short fiber reinforced silicon carbide precast body, the catalyst is N, N, N ', N '-tetramethylethylenediamine, institute
Stating initiator is ammonium persulfate.
In some preferred embodiments, in a step of silicon carbide slurry is provided, specifically include the following steps:
In proportion for 5-10:0.1-0.5:1-3:100 by deionized water, organic monomer, crosslinking agent and dispersant
Obtain mixed solution；
Silicon carbide micro-powder is added in the mixed solution, agitated, dispersion and ball milling obtain silicon carbide slurry.
In some preferred embodiments, it is passed through high-pressure inert gas in the vacuum drying oven, the carbon is made by high pressure
The step of SiClx slurry is sufficiently impregnated into inside fibrage body, and continuous fiber reinforcement silicon carbide precast body is obtained after solidification
In, the high pressure gas is high-purity argon gas, and the gas pressure of the high-purity argon gas is between 5-30atm.
In some preferred embodiments, the organic monomer is acrylamide, and the crosslinking agent is N, N '-di-2-ethylhexylphosphine oxide
Acrylamide, the dispersing agent are sodium cellulose glycolate.
The present invention by adopting the above technical scheme the advantages of be:
The preparation method of silicon carbide fiber reinforced composite material provided by the invention, using gel injection molding and forming technology original position
The characteristics of solidification, prepares silicon carbide fiber reinforced precast body, and by after the drying process of silicon carbide fiber reinforced precast body, passes through
Reaction sintering technology makes a part of liquid-phase silicone react generation silicon carbide with the carbon in precast body, remains in a part of silicon filling precast body
Remaining hole, so that silicon carbide fiber reinforced composite material is obtained, the silicon carbide fiber reinforced composite wood prepared using this method
Tough effect is mended in the enhancing that material can give full play to fiber, and material density is high, also has simple process, at low cost, production cycle
The advantages that short.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
Other attached drawings are obtained according to these attached drawings.
Fig. 1 is the step flow chart of the preparation method for the silicon carbide fiber reinforced composite material that the embodiment of the present invention 1 provides.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts all other
Embodiment shall fall within the protection scope of the present invention.
Referring to Fig. 1, be the preparation method of silicon carbide fiber reinforced composite material provided in an embodiment of the present invention, including under
State step:
Step S110: chopped strand or 3 D weaving body is made in carbon fiber；
In some preferred embodiments, chopped strand or 3 D weaving body is made in carbon fiber by the present embodiment, including under
State step:
Using carbon fiber as raw material, shear to obtain the chopped strand by shearing equipment, the length of the chopped strand exists
Between 0.5-5mm；
Using carbon fiber as raw material, the 3 D weaving body is obtained by three-dimensional four-way weaving, to guarantee three-dimensional volume
The isotropism of body is knitted, the volume content of fiber is between 40%-60% in the 3 D weaving body.
Step S120: the fiber surface of the chopped strand or 3 D weaving body is deposited into composite coating, the compound painting
Layer internal layer is Pyrolytic carbon coating, and outer layer is coat of silicon carbide；
In some preferred embodiments, the fiber surface of the chopped strand or 3 D weaving body is being deposited into compound painting
In the step of layer, specifically include the following steps:
Step S121: the chopped strand or fibrage body are placed in chemical vapor deposition stove, are heated after vacuumizing
Handle except glue to 400-800 DEG C；
Step S122: except the chopped strand or fibrage body pass through chemical vapor deposition manner described after glue processing
Chopped strand or fibrage body fiber surface deposit the composite coating.
It is carbon source that methane, ethylene or propylene are selected when depositing the Pyrolytic carbon coating, and high pure nitrogen is diluent gas and load
Gas, depositing temperature are 900-1100 DEG C, and sedimentation time is 10-100 hours, and gas pressure is in 500-2000Pa；Deposit the carbon
Using trichloromethyl silane as silicon carbide source when SiClx coating, for hydrogen as carrier gas and catalyst, high-purity argon gas is diluent gas, is sunk
Accumulated temperature degree is 1000-1200 DEG C, and sedimentation time is 10-100 hours, and gas pressure is in 500-2000Pa.
It is appreciated that working out body fiber surface deposition cracking carbon in chopped strand or fiber by chemical vapor deposition process
And silicon carbide compound coating.The presence of Pyrolytic carbon coating can form suitably weak binding, material fracture between fiber and matrix
The bending strength and fracture toughness of material can be improved by mechanism such as crack deflection, spike protein gene, fibrous fractures in the process；Carbonization
The presence of silicon coating can also be effectively protected fiber from damage during reaction-sintered, therefore can give full play to fiber
Enhancing mend tough effect, the silicon carbide fiber reinforced composite material of preparation has better room-temperature mechanical property.
Step S130: it is prefabricated that the chopped strand that surface is deposited with composite coating is prepared into short fiber reinforced silicon carbide
Body, or the 3 D weaving body that fiber surface is deposited with composite coating is prepared into continuous fiber reinforcement silicon carbide precast body.
In some preferred embodiments, staple fiber is prepared into the chopped strand that surface is deposited with composite coating
The 3 D weaving body that fiber surface is deposited with composite coating is prepared into continuous fiber reinforcement by enhancing silicon carbide precast body
In the step of silicon carbide precast body, specifically include the following steps:
When the chopped strand that surface is deposited with composite coating is prepared into short fiber reinforced silicon carbide precast body, packet
Include following step:
Step S131: a silicon carbide slurry is provided；
Step S132: the chopped strand that surface is deposited with composite coating is added in the silicon carbide slurry, is mixed
It is poured out after closing uniformly, carries out froth in vacuum, wherein the mass ratio of the chopped strand and silicon carbide micro-powder is 0.1-0.4:1.It can
To understand, in actual operation, if fruit fiber additional amount is very little, the composite material strength of preparation, toughness improve unobvious；And it is fine
It is too high to tie up additional amount, can generate " bridge formation effect ", increases the porosity of short carbon fiber reinforced silicon carbide precast body, makes sintered
The content of free silica increases in material, will lead to the bending strength and fracture toughness decline of composite material instead, and when described short
When the mass ratio for cutting fiber and silicon carbide micro-powder is 0.1-0.4:1, the defect of above-mentioned appearance can avoid.
Specifically, the chopped strand that surface is deposited with composite coating is added in silicon carbide slurry, ball-milling treatment
1-2 hours, carry out froth in vacuum.
Step S133: the silicon carbide slurry is maintained between 20-30 DEG C, then is added and is catalyzed in the silicon carbide slurry
Agent and initiator, and it is cured after obtain the short fiber reinforced silicon carbide precast body.
Further, the catalyst is N, N, N ', N '-tetramethylethylenediamine, the initiator is ammonium persulfate.
Specifically, catalyst and initiator is added in the silicon carbide slurry, is finally injected into after solidifying in mold and obtains
The short fiber reinforced silicon carbide precast body.
When to be prepared into continuous fiber reinforcement silicon carbide pre- for the 3 D weaving body that fiber surface is deposited with composite coating
When body processed, include the following steps:
Step S131 ': a silicon carbide slurry is provided；
Step S132 ': by the silicon carbide slurry froth in vacuum, and being maintained at slurry temperature between 20-30 DEG C, then
Catalyst and initiator is added in the silicon carbide slurry；
Step S133 ': the 3 D weaving body that fiber surface is deposited with composite coating is placed in mold, a juxtaposition
In carrying out vacuumize process in vacuum drying oven.
Step S134 ': being passed through high-pressure inert gas in the vacuum drying oven, keeps the silicon carbide slurry abundant by high pressure
It is impregnated into inside fibrage body, continuous fiber reinforcement silicon carbide precast body is obtained after solidification.
Preferably, the high pressure gas is high-purity argon gas, and the gas pressure of the high-purity argon gas is between 5-30atm.
Further, silicon carbide slurry described in S131, S131 ' is prepared especially by following step:
In proportion for 5-10:0.1-0.5:1-3:100 by deionized water, organic monomer, crosslinking agent and dispersant
Obtain mixed solution；Silicon carbide micro-powder is added in the mixed solution, is carried out after tentatively being dispersed by churned mechanically mode
Ball milling, abrading-ball select silicon carbide abrading-ball, and silicon carbide slurry, the carbonization is made in Ball-milling Time control after 3-6 hours, ball milling
Silicon slurry viscosity is about 2Pas.
It is appreciated that the silicon carbide fiber reinforced precast body preparation that the above embodiment of the present invention provides, uses gel and infuses
Mould moulding process, for short fiber reinforced composite material of silicon carbide, due to gel injection-moulding in-situ solidifying process characteristic, it can be achieved that
Staple fiber being uniformly distributed in silicon carbide substrate；It can by the way of pressurization for continuous fiber reinforcement composite material of silicon carbide
So that slurry is sufficiently infiltrated up in fiber preform.
Step S140: by the short fiber reinforced silicon carbide precast body or the prefabricated soma of continuous fiber reinforcement silicon carbide
Dry processing；
It is appreciated that contain a certain amount of moisture in the silicon carbide fiber reinforced precast body of gel casting forming, it need to be by dry
Drying process discharge.The present embodiment selects the compatible with water and immiscible organic solvent of gel rubber system to be configured to dry liquid, in room temperature
It is lower to set short fiber reinforced silicon carbide precast body described in step S140 or the continuous fiber reinforcement silicon carbide precast body
In dry liquid, dry liquid is slowly diffused to by moisture and realizes that precast body is slowly dried, due to the inside and outside drying of green body
Rate is equal, and the defects of cracking can be effectively avoided.Specific drying process is in the existing public affairs of patent CN102887711B
It opens.
It is appreciated that silicon carbide fiber reinforced precast body moderate strength after drying, precast body machining property are excellent
It is different, precast body can be processed into required shape, it, can be to a certain extent compared with carrying out machining after reaction-sintered again
Production cost is reduced, the manufacturing cycle of material is shortened.
Step S150: by the short fiber reinforced silicon carbide precast body or the continuous fiber reinforcement silicon carbide after drying
High-purity silicon powder is placed in precast body upper surface, and 1450-1550 DEG C of reaction-sintered is heated in vacuum, then be cooled to room temperature and obtain
Silicon carbide fiber reinforced composite material.
It is appreciated that by the short fiber reinforced silicon carbide precast body or the continuous fiber reinforcement silicon carbide after drying
High-purity silicon powder is placed in precast body upper surface, and 1450-1550 DEG C of reaction-sintered is heated in vacuum environment, silicon powder melt after
It is penetrated into precast body under capillarity, part silicon is reacted with the carbon in precast body generates silicon carbide, and part silicon fills green body
In remaining hole, thus cooling after available densification silicon carbide fiber reinforced composite material.
The preparation method of silicon carbide fiber reinforced composite material provided by the invention, using gel injection molding and forming technology original position
The characteristics of solidification, prepares silicon carbide fiber reinforced precast body, and by after the drying process of silicon carbide fiber reinforced precast body, passes through
Reaction sintering technology makes a part of liquid-phase silicone react generation silicon carbide with the carbon in precast body, remains in a part of silicon filling precast body
Remaining hole, so that silicon carbide fiber reinforced composite material is obtained, the silicon carbide fiber reinforced composite wood prepared using this method
Tough effect is mended in the enhancing that material can give full play to fiber, and material density is high, also has simple process, at low cost, production cycle
The advantages that short.
Above-mentioned technical proposal of the present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1
Step S1: it using carbon fiber as raw material, shears to obtain chopped strand by shearing equipment, chopped strand length is 2mm.
Step S2: chopped strand is placed in chemical vapor deposition stove, and 500 DEG C are heated to after vacuumizing and is carried out except Jiao Chu
Reason.Except in-furnace temperature is raised to 1050 DEG C after glue, using methane as carbon source, high pure nitrogen is diluent gas and carrier gas, utilizes chemistry
Gas-phase deposition deposits Pyrolytic carbon coating, atmosphere pressures 1000Pa on chopped strand surface, and sedimentation time is 15 hours；
After depositing Pyrolytic carbon coating, depositing silicon silicon coating on the basis of Pyrolytic carbon coating, with trichloromethyl silane
It (MTS) is precursor, hydrogen is as carrier gas and catalyst, MTS and H2The ratio of the amount of substance is 1:8, is dilution with high-purity argon gas
Gas, atmosphere pressures 800Pa, depositing temperature are 1100 DEG C, and sedimentation time is 20 hours.
Step S3: 90g monomer, 4g crosslinking agent, 15ml dispersing agent are added in 500g deionized water.It is added after completely dissolution
Silicon carbide micro-powder 1930g, ball milling 4 hours, obtain silicon carbide slurry after mixing evenly；Surface deposition is added in silicon carbide slurry
There is the chopped strand 480g of composite coating, continues ball milling 2 hours, ball milling takes out uniformly mixed slurry after completing,
De-bubble 15 minutes under vacuum environment, and slurry temperature is controlled at 25 DEG C, catalyst and initiator is added and is stirred, later
The slurry of homogenizing is injected into solidification in mold and obtains short carbon fiber reinforced silicon carbide precast body.
Step S4: various concentration organic solvent composition will be first placed on after the demoulding of short carbon fiber reinforced silicon carbide precast body
In dry liquid, the moisture diffusion in green body to dry liquid is gradually realized that slow flawless is dry, specific back tender at normal temperature
Skill is shown in CN102887711B.
Step S5: high-purity silicon powder is placed into the short carbon fiber reinforced silicon carbide precast body upper surface, heating in vacuum arrives
1500 DEG C of progress reaction-sintereds, liquid-state silicon penetrate into precast body through capillary action, and a part is reacted with carbon generates silicon carbide,
Another part fills remaining hole, and cooling obtains short carbon fiber reinforced composite material of silicon carbide after reaction.
Embodiment 2
Step S1: using carbon fiber as raw material, weave to obtain 3 D weaving body by three-dimensional four-way, in the 3 D weaving body
The volume content of fiber is 50%.
Step S2: the fibrage body in step S1 is placed in chemical vapor deposition stove, and 550 DEG C are heated to after vacuumizing
Handled except glue.Except in-furnace temperature is raised to 1050 DEG C after glue, using methane as carbon source, high pure nitrogen is diluent gas and load
Gas deposits Pyrolytic carbon coating, atmosphere pressures 1000Pa, sedimentation time on chopped strand surface using chemical vapor deposition process
It is 15 hours；
After depositing Pyrolytic carbon coating, depositing silicon silicon coating on the basis of depositing Pyrolytic carbon coating, with trichloromethyl silicon
Alkane (MTS) is precursor, and hydrogen is as carrier gas and catalyst, MTS and H2The ratio of the amount of substance is 1:8, is dilute with high-purity argon gas
Outgassing body and carrier gas, depositing temperature are 1100 DEG C, atmosphere pressures 800Pa, and sedimentation time is 20 hours.
90g monomer, 4g crosslinking agent, 10ml dispersing agent is added in step S3. in 500g deionized water, is added after completely dissolution
Silicon carbide micro-powder 2770g, is sufficiently stirred rear ball milling 5 hours, pours out slurry after ball milling, de-bubble 15 divides under vacuum conditions
Clock, and slurry temperature is controlled at 25 DEG C, catalyst and initiator is added and is stirred, the silicon carbide slurry being homogenized；
The 3 D weaving body that fiber surface is deposited with composite coating is placed in mold, one is placed in vacuum drying oven
Interior, after vacuumizing, implantation silicon carbide slurry in a mold, slurry coats the high-purity argon that charged pressure after knitted body is 20atm
Gas is infiltrated up to slurry sufficiently in fibrage body under high pressure effect, it is prefabricated that continuous fiber reinforcement silicon carbide is obtained after solidification
Body.
Step S4: various concentration organic solvent composition will be successively put into after the demoulding of continuous fiber reinforcement silicon carbide precast body
Drying liquid in, at normal temperature gradually by the moisture diffusion in precast body to dry liquid, realize that flawless is dry, specific back tender
Skill is shown in patent CN102887711B.
Step S5: after high-purity silicon powder is placed in the precast body upper surface, heating in vacuum carries out reaction burning to 1500 DEG C
Knot, liquid-state silicon penetrate into precast body through capillary action, and a part is reacted with the carbon in precast body generates silicon carbide, another portion
Divide remaining hole in packing material, is cooled to room temperature after reaction and obtains continuous carbon fibre enhancing composite material of silicon carbide.
Certainly the preparation method of silicon carbide fiber reinforced composite material of the invention can also have a variety of transformation and remodeling, and
It is not limited to the specific structure of above embodiment.In short, protection scope of the present invention should include that those are common for this field
It obviously converts or substitutes and retrofit for technical staff.
Claims (8)
1. a kind of preparation method of silicon carbide fiber reinforced composite material, it is characterised in that the fiber is carbon fiber, including under
State step:
Chopped strand or 3 D weaving body is made in carbon fiber；
The fiber surface of the chopped strand or 3 D weaving body is deposited into composite coating, the composite coating internal layer is cracking carbon
Coating, outer layer are coat of silicon carbide；
The chopped strand that surface is deposited with composite coating is prepared into short fiber reinforced silicon carbide precast body, or by fiber table
The 3 D weaving body that face is deposited with composite coating is prepared into continuous fiber reinforcement silicon carbide precast body；
The short fiber reinforced silicon carbide precast body or the continuous fiber reinforcement silicon carbide precast body are dried；
By after drying the short fiber reinforced silicon carbide precast body or the continuous fiber reinforcement silicon carbide precast body upper surface
High-purity silicon powder is placed, and is heated to 1450-1550 DEG C of reaction-sintered in vacuum environment, then be cooled to room temperature and obtain fiber reinforcement
Composite material of silicon carbide.
2. the preparation method of silicon carbide fiber reinforced composite material as described in claim 1, which is characterized in that by carbon fiber
In the step of chopped strand or 3 D weaving body is made,
Using carbon fiber as raw material, shear to obtain the chopped strand by shearing equipment, the length of the chopped strand is in 0.5-
Between 5mm；
Using carbon fiber as raw material, the 3 D weaving body, fibre in the 3 D weaving body are obtained by three-dimensional four-way weaving
The volume content of dimension is between 40%-60%.
3. the preparation method of silicon carbide fiber reinforced composite material as described in claim 1, which is characterized in that will be described short
In the step of cutting the fiber surface deposition composite coating of fiber or 3 D weaving body, specifically include the following steps:
The chopped strand or fibrage body are placed in chemical vapor deposition stove, be heated to after vacuumizing 400-800 DEG C into
Row is handled except glue；
Except the chopped strand or fibrage body pass through chemical vapor deposition manner in the chopped strand or fibre after glue processing
The fiber surface for tieing up knitted body deposits the composite coating；
It is carbon source that methane, ethylene or propylene are selected when depositing the Pyrolytic carbon coating, and high pure nitrogen is diluent gas and carrier gas, is sunk
Accumulated temperature degree is 900-1100 DEG C, and sedimentation time is 10-100 hours, and gas pressure is in 500-2000Pa；The silicon carbide is deposited to apply
Using trichloromethyl silane as silicon carbide source when layer, for hydrogen as carrier gas and catalyst, high-purity argon gas is diluent gas, depositing temperature
It is 1000-1200 DEG C, sedimentation time is 10-100 hours, and gas pressure is in 500-2000Pa.
4. the preparation method of silicon carbide fiber reinforced composite material as claimed in claim 2, which is characterized in that sink by surface
Product has the chopped strand of composite coating to be prepared into short fiber reinforced silicon carbide precast body or be deposited with fiber surface compound
In the step of 3 D weaving body of coating is prepared into continuous fiber reinforcement silicon carbide precast body, specifically include the following steps:
When the chopped strand that surface is deposited with composite coating is prepared into short fiber reinforced silicon carbide precast body, including under
State step:
One silicon carbide slurry is provided；
The chopped strand that surface is deposited with composite coating is added in the silicon carbide slurry, after mixing by slurry
It pours out, and carries out froth in vacuum, wherein the mass ratio of the chopped strand and silicon carbide micro-powder is 0.1-0.4:1；
The silicon carbide slurry after de-bubble is maintained between 20-30 DEG C, then catalyst is added in the silicon carbide slurry
And initiator, and it is cured after obtain the short fiber reinforced silicon carbide precast body；
When the 3 D weaving body that fiber surface is deposited with composite coating is prepared into continuous fiber reinforcement silicon carbide precast body
When, include the following steps:
One silicon carbide slurry is provided；
By the silicon carbide slurry froth in vacuum, and it is maintained at slurry temperature between 20-30 DEG C, then in the silicon carbide slurry
Middle addition catalyst and initiator；
The 3 D weaving body that fiber surface is deposited with composite coating is placed in mold, one is placed in progress in vacuum drying oven
The slurry is passed through in the mold by vacuumize process later；
It is passed through high-pressure inert gas in the vacuum drying oven, so that the silicon carbide slurry is sufficiently impregnated into fiber by high pressure and compiles
Internal portion is knitted, continuous fiber reinforcement silicon carbide precast body is obtained after solidification.
5. the preparation method of silicon carbide fiber reinforced composite material as claimed in claim 4, which is characterized in that in the carbonization
Catalyst and initiator is added in silicon slurry, and the catalyst is N, N, N ', N '-tetramethylethylenediamine, the initiator is over cure
Sour ammonium.
6. the preparation method of silicon carbide fiber reinforced composite material as claimed in claim 4, which is characterized in that providing a carbon
In the step of SiClx slurry, specifically include the following steps:
In proportion for 5-10:0.1-0.5:1-3:100 by deionized water, organic monomer, crosslinking agent and dispersant obtain
Mixed solution；
Silicon carbide micro-powder is added in the mixed solution, agitated, dispersion and ball milling obtain silicon carbide slurry.
7. the preparation method of silicon carbide fiber reinforced composite material as claimed in claim 4, which is characterized in that in the vacuum
It is passed through high-pressure inert gas in furnace, is impregnated into the silicon carbide slurry sufficiently inside fibrage body by high pressure, solidifies
After in the step of obtaining continuous fiber reinforcement silicon carbide precast body, the high pressure gas is high-purity argon gas, the high-purity argon gas
Gas pressure is between 5-30atm.
8. the preparation method of silicon carbide fiber reinforced composite material as claimed in claim 6, which is characterized in that organic list
Body is acrylamide, and the crosslinking agent is N, and N '-methylene-bisacrylamide, the dispersing agent is sodium cellulose glycolate.
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| CN113651618B (en) * | 2021-08-27 | 2022-07-05 | 西北工业大学 | Silicon carbide ceramic matrix composite reflector and preparation method and application thereof |
| CN113816754A (en) * | 2021-09-24 | 2021-12-21 | 南昌航空大学 | Preparation method of novel SiC/SiC micro composite material containing multilayer zirconium silicate interface phase |
| CN113698220A (en) * | 2021-09-26 | 2021-11-26 | 中国科学院长春光学精密机械与物理研究所 | Preparation method of fiber-reinforced silicon carbide composite material and fiber-reinforced silicon carbide composite material |
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