CN107903067A - A kind of growth in situ SiC nanowire enhancing SiC ceramic based composites and preparation method thereof - Google Patents
A kind of growth in situ SiC nanowire enhancing SiC ceramic based composites and preparation method thereof Download PDFInfo
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- 239000002070 nanowire Substances 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 30
- 239000000919 ceramic Substances 0.000 title claims abstract description 27
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims description 13
- 230000002708 enhancing effect Effects 0.000 title claims description 12
- 239000000835 fiber Substances 0.000 claims abstract description 43
- 239000012783 reinforcing fiber Substances 0.000 claims abstract description 24
- 239000011159 matrix material Substances 0.000 claims abstract description 21
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 15
- 230000002787 reinforcement Effects 0.000 claims description 11
- 229920003257 polycarbosilane Polymers 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 10
- 239000004744 fabric Substances 0.000 claims description 9
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- 230000008595 infiltration Effects 0.000 claims description 8
- 238000001764 infiltration Methods 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 6
- 238000000498 ball milling Methods 0.000 claims description 5
- 239000012700 ceramic precursor Substances 0.000 claims description 4
- KTWOOEGAPBSYNW-UHFFFAOYSA-N ferrocene Chemical compound [Fe+2].C=1C=C[CH-]C=1.C=1C=C[CH-]C=1 KTWOOEGAPBSYNW-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 238000000197 pyrolysis Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000005336 cracking Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 238000004080 punching Methods 0.000 claims description 3
- 238000005245 sintering Methods 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 230000008901 benefit Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 5
- 238000005728 strengthening Methods 0.000 description 5
- SICLLPHPVFCNTJ-UHFFFAOYSA-N 1,1,1',1'-tetramethyl-3,3'-spirobi[2h-indene]-5,5'-diol Chemical compound C12=CC(O)=CC=C2C(C)(C)CC11C2=CC(O)=CC=C2C(C)(C)C1 SICLLPHPVFCNTJ-UHFFFAOYSA-N 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical group [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000011204 carbon fibre-reinforced silicon carbide Substances 0.000 description 2
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- 238000004132 cross linking Methods 0.000 description 2
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- 239000002904 solvent Substances 0.000 description 2
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011153 ceramic matrix composite Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- HPNSNYBUADCFDR-UHFFFAOYSA-N chromafenozide Chemical compound CC1=CC(C)=CC(C(=O)N(NC(=O)C=2C(=C3CCCOC3=CC=2)C)C(C)(C)C)=C1 HPNSNYBUADCFDR-UHFFFAOYSA-N 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
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- 239000003863 metallic catalyst Substances 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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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
- C04B35/571—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 from Si-containing polymer precursors or organosilicon monomers
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/628—Coating the powders or the macroscopic reinforcing agents
- C04B35/62844—Coating fibres
- C04B35/62857—Coating fibres with non-oxide ceramics
- C04B35/62865—Nitrides
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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
- C04B2235/5216—Inorganic
- C04B2235/524—Non-oxidic, e.g. borides, carbides, silicides or nitrides
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- 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
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Abstract
The present invention relates to a kind of growth in situ SiC nanowire to strengthen SiC ceramic based composites, by reinforcing fiber, SiC nanowire, boundary layer and SiC matrix composition；It is characterized in that SiC nanowire growth in situ, in reinforcing fiber, boundary layer is coated on reinforcing fiber and SiC nanowire surface, SiC matrix is filled in the gap that reinforcing fiber and SiC nanowire surround；The reinforcing fiber is fiber C or SiC fibers；A diameter of 50 ~ the 200nm of the SiC nanowire, length are 0.5 ~ 3mm；The boundary layer is PyC or BN, and thickness is 0.02 ~ 0.1 μm.Present invention efficiently solves SiC nanowire in fibre preforms body more difficult the problem of being uniformly distributed, while SiC nanowire has been given full play to advantage of SiC ceramic based composites etc. by growth in situ SiC nanowire.
Description
Technical field
It is growth in situ SiC nanometers more particularly to a kind of the present invention relates to a kind of ceramic matric composite and preparation method thereof
Line enhancing SiC ceramic based composites and preparation method thereof.
Background technology
SiC ceramic based composites have structure light wt, height than strong Gao Bimo, high temperature resistant, good thermal shock, low thermal expansion
The features such as coefficient and oxidation and corrosion, be widely used in aero-engine hot arc structural member, rocket engine
The aerospace fields such as jet pipe, combustion chamber.As these high-end fields put forward higher requirements material property, as engine will
Ask material can to bear bigger air-flow more resistant to high temperature and wash away, jet pipe position requires material to be also subjected to bigger pressure, due to environment
Temperature and pressure greatly improves, and SiC ceramic based composites are more difficult to meet requirement, because can be destroyed under high temperature and pressure
The structure of composite material, SiC matrix is extruded between reinforcing fiber, causes material destructive failure phenomenon occur, so necessary
Further Strengthening and Toughening SiC ceramic based composites.
SiC nanowire is a kind of nanometer reinforcement of excellent performance, and tensile strength can reach 53.4GPa, fine much larger than SiC
Peacekeeping SiC whiskers, especially ultralong SiC nanowires can not only improve the interface cohesion of fiber and matrix, it is often more important that also
Fiber can firmly be pinned each other with fiber, fiber and matrix, make fiber be more difficult to slide, so as to greatly enhance SiC ceramic base
The intensity of composite material.By ultralong SiC nanowires growth in situ in reinforcing fiber, due to ultralong SiC nanowires part along
Fiber radial radial is grown to inside fibre bundle, in the gap of fibre bundle and fiber interfascicular, can be effectively by reinforcing fiber
Close connection, drastically increases the obdurability of SiC ceramic based composites, while improve the ratio surface in fibre preforms body
Product, easy to the attachment of ceramic precursor, so as to improve the consistency of SiC matrix；And ultralong SiC nanowires can also be by dividing
Dissipate the toughening mechanisms such as pressure, crack deflection and bridging, the interface that effectively Strengthening and Toughening fiber is combined with SiC matrix, so as to strengthen
SiC ceramic based composites.
The Chinese patent of application publication number CN106866148A discloses a kind of SiC of SiC nanowire In-sltu reinforcement f /SiC
Composite material and preparation method thereof, which includes SiC fiber preforms, SiC nanowire and SiC ceramic matrix, described
The mutually winding networking between the fiber surface of the SiC fiber preforms, the SiC nanowire of SiC nanowire growth in situ
Shape structure；The SiC ceramic matrix is filled in the hole of the SiC fiber preforms.Preparation method includes：（1）Come to the surface
Learn modification；（2）Loading catalyst；（3）Chemical vapor deposition；（4）Precursor infiltration and pyrolysis.The SiC nanowire is in situ to be increased
Strong SiC f / SiC ceramic matrix composite material have SiC nanowire be evenly distributed do not reunite and be well combined with SiC fibers, obdurability is good,
The advantages that consistency is high, preparation method technique is simple, equipment requirement is low, environmentally friendly, technique versatility is good, and SiC nanowire introduces body
Fraction is high and controllable.But SiC nanowire curtailment prepared by this method, interface can only be improved, can not real Strengthening and Toughening
SiC matrix, since this method is to first pass through impregnation catalyst agent solution, this can cause excessive metal catalytic particles to residue in fibre
Dimension table face, so that the performance of material under the high temperature conditions is reduced, and also this method is not prepared again after SiC nanowire is prepared
Protective boundary layer, this causes the compound middle SiC nanowire of the matrix to be below seriously damaged, prevent material property from
Effectively improve.
The Chinese patent of publication No. CN103553616B is authorized to disclose a kind of growth in situ SiC nanowire enhancing C/SiC
Composite material and preparation method thereof, the preparation method include：（1）It is prepared by slurry：Polycarbosilane, catalyst and solvent are mixed
Close ball milling and slurry is made, wherein the catalyst is iron, nickel, and/or ferrocene；（2）Vacuum high-pressure impregnates：Fiber C is prefabricated
Body is immersed in the slurry, when holding 0.1 ~ 1 is small under vacuum state, then passes to high-pressure inert gas to 1 ~ 10MPa, pressurize
1 ~ 4 it is small when；（3）Crosslinking curing：By impregnated fiber C precast body be put in air 6 it is small when more than carry out crosslinking curing and be made
Preform；And（4）Pintsch process：By the preform with 2 ~ 10 DEG C/min of heating rate liter under protective atmosphere
When warm to 1000 ~ 1300 DEG C insulations 1 ~ 4 are small, with the life in situ under metallic catalyst effect in the Polycarbosilane pyrolytic process
Long SiC nanowire, so that the growth in situ SiC nanowire enhancing C/SiC composite materials be made.But this method is directly by fibre
Dimension precast body is immersed in Polycarbosilane, catalyst and solvent mixing and ball milling and is made in slurry, is then pyrolyzed growth in situ SiC and receives
Rice noodles, since the decomposition of Polycarbosilane in pyrolytic process produces gas, and volume contraction can occurs in itself, this can cause SiC to receive
Nanowire growth is interfered, so that growth is uneven, and length is also insufficient, can not effectively strengthen composite material.
The content of the invention
To solve the above problems, the present invention propose a kind of growth in situ SiC nanowire enhancing SiC ceramic based composites and
Its preparation method, gives full play to the advantage of SiC nanowire Strengthening and Toughening SiC ceramic based composites, it is compound to have widened SiC ceramic base
The application field of material.
A kind of growth in situ SiC nanowire strengthens SiC ceramic based composites, by reinforcing fiber, SiC nanowire, interface
Layer and SiC matrix composition；It is characterized in that SiC nanowire growth in situ, in reinforcing fiber, boundary layer is coated on reinforcing fiber
With SiC nanowire surface, SiC matrix is filled in the gap that reinforcing fiber and SiC nanowire surround；The reinforcing fiber is
Fiber C or SiC fibers；A diameter of 50 ~ the 200nm of the SiC nanowire, length are 0.5 ~ 3mm；The boundary layer is PyC
Or BN, thickness are 0.02 ~ 0.1 μm.
A kind of preparation method of growth in situ SiC nanowire enhancing SiC ceramic based composites, it is characterised in that including under
The step of stating order：
（1）By Polycarbosilane, ferrocene, activated carbon in mass ratio 1:0.01~0.05:Uniform powder is made in 3 ~ 6 mixing and ball millings
Precursor, is uniformly put into graphite crucible；
（2）Cloth of reinforcement fibers is covered in step（1）In be placed with the graphite crucible of powder precursor, be then put into togerther height
In warm sintering furnace, 1300 ~ 1500 DEG C, 1 ~ 5h of soaking time are warming up to the heating rate of 5 ~ 10 DEG C/min, and be passed through mobility
Ar；
（3）By step（2）Cloth of reinforcement fibers after processing is layered in graphite jig, and cloth of reinforcement fibers is made using needle-punching method
Fiber preform；
（4）Using chemical vapor infiltration in step（3）Deposited interfacial layer on the fiber preform prepared；
（5）Using the Polycarbosilane of liquid containing vinyl as ceramic precursor, by precursor infiltration and pyrolysis method in step（4）Prepare
The fiber preform of boundary layer prepares SiC matrix, and 1100 ~ 1300 DEG C of cracking temperature, obtains the enhancing of growth in situ SiC nanowire
SiC ceramic based composites.
Beneficial effect of the present invention：（1）Efficiently solve that SiC nanowire is more difficult in fibre preforms body equally distributed to ask
Topic, while advantage of the SiC nanowire to composite material Strengthening and Toughening has been given full play to by growth in situ SiC nanowire；（2）Pass through
Chemical vapor infiltration prepares an interfacial layer in SiC nanowire and reinforcing fiber surface, protects SiC nanowire, preferably
Beneficial to the densification of SiC matrix；（3）SiC ceramic based composites mechanical property is drastically increased, has widened its application neck
Domain.
Embodiment
A kind of growth in situ SiC nanowire strengthens SiC ceramic based composites, by reinforcing fiber, SiC nanowire, interface
Layer and SiC matrix composition；It is characterized in that SiC nanowire growth in situ, in reinforcing fiber, boundary layer is coated on reinforcing fiber
With SiC nanowire surface, SiC matrix is filled in the gap that reinforcing fiber and SiC nanowire surround；The reinforcing fiber is
Fiber C；The SiC nanowire a diameter of 100nm, length 1mm；The boundary layer is BN, and thickness is 0.05 μm.
A kind of preparation method of growth in situ SiC nanowire enhancing SiC ceramic based composites, it is characterised in that including under
The step of stating order：
（1）By Polycarbosilane, ferrocene, activated carbon in mass ratio 1:0.03:Uniform powder precursor is made in 5 mixing and ball millings,
Uniformly it is put into graphite crucible；
（2）Cloth of reinforcement fibers is covered in step（1）In be placed with the graphite crucible of powder precursor, be then put into togerther height
In warm sintering furnace, 1350 DEG C, soaking time 3h are warming up to the heating rate of 8 DEG C/min, and be passed through mobility Ar；
（3）By step（2）Cloth of reinforcement fibers after processing is layered in graphite jig, and cloth of reinforcement fibers is made using needle-punching method
Fiber preform；
（4）Using chemical vapor infiltration in step（3）BN boundary layers are deposited on the fiber preform prepared；
（5）Using the Polycarbosilane of liquid containing vinyl as ceramic precursor, by precursor infiltration and pyrolysis method in step（4）Prepare
The fiber preform of boundary layer prepares SiC matrix, and 1200 DEG C of cracking temperature, obtains growth in situ SiC nanowire enhancing SiC ceramic
Based composites.
The embodiment of the present invention is above are only, but the design concept of the present invention is not limited thereto, it is all to utilize this
Conceive the change that unsubstantiality is carried out to the present invention, the behavior for invading the scope of protection of the invention should all be belonged to.In every case it is not de-
From the content of technical solution of the present invention, what the technical spirit according to the present invention made above example any type of simply repaiies
Change, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (2)
1. a kind of growth in situ SiC nanowire strengthens SiC ceramic based composites, by reinforcing fiber, SiC nanowire, boundary layer
Formed with SiC matrix；It is characterized in that SiC nanowire growth in situ is in reinforcing fiber, boundary layer be coated on reinforcing fiber and
SiC nanowire surface, SiC matrix are filled in the gap that reinforcing fiber and SiC nanowire surround；The reinforcing fiber is C
Fiber or SiC fibers；A diameter of 50 ~ the 200nm of the SiC nanowire, length are 0.5 ~ 3mm；The boundary layer for PyC or
BN, thickness are 0.02 ~ 0.1 μm.
2. a kind of preparation method of growth in situ SiC nanowire enhancing SiC ceramic based composites, it is characterised in that including following
The step of order：
（1）By Polycarbosilane, ferrocene, activated carbon in mass ratio 1:0.01~0.05:Uniform powder is made in 3 ~ 6 mixing and ball millings
Precursor, is uniformly put into graphite crucible；
（2）Cloth of reinforcement fibers is covered in step（1）In be placed with the graphite crucible of powder precursor, be then put into togerther height
In warm sintering furnace, 1300 ~ 1500 DEG C, 1 ~ 5h of soaking time are warming up to the heating rate of 5 ~ 10 DEG C/min, and be passed through mobility
Ar；
（3）By step（2）Cloth of reinforcement fibers after processing is layered in graphite jig, and cloth of reinforcement fibers is made using needle-punching method
Fiber preform；
（4）Using chemical vapor infiltration in step（3）Deposited interfacial layer on the fiber preform prepared；
（5）Using the Polycarbosilane of liquid containing vinyl as ceramic precursor, by precursor infiltration and pyrolysis method in step（4）Prepare
SiC matrix is prepared in the fiber preform of boundary layer, 1100 ~ 1300 DEG C of cracking temperature, obtains the enhancing of growth in situ SiC nanowire
SiC ceramic based composites.
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| CN108452590A (en) * | 2018-04-20 | 2018-08-28 | 苏州宏久航空防热材料科技有限公司 | A kind of high intensity SiC with high efficiency filterf/ SiC ceramic matrix composite material screen pipe |
| CN108484135A (en) * | 2018-04-17 | 2018-09-04 | 苏州宏久航空防热材料科技有限公司 | A kind of growth in situ ceramics reinforcing fiber resin composite materials |
| CN108585954A (en) * | 2018-06-01 | 2018-09-28 | 西北工业大学 | A kind of C/C-Si composite material surfaces grow radial nano wire and preparation method at normal temperatures |
| CN108754357A (en) * | 2018-05-29 | 2018-11-06 | 苏州宏久航空防热材料科技有限公司 | A kind of SiC nanowire enhancing aluminum silicon carbide composite material and preparation method thereof |
| CN109020628A (en) * | 2018-08-04 | 2018-12-18 | 南京航空航天大学 | A kind of SiC nanowire enhancing porous ceramic composite and preparation method thereof |
| CN109055874A (en) * | 2018-08-17 | 2018-12-21 | 苏州宏久航空防热材料科技有限公司 | A kind of boundary layer enhancing biradical fibrous composite of aluminium alloy-silicon carbide and preparation method thereof |
| CN109251049A (en) * | 2018-09-13 | 2019-01-22 | 中国科学院上海硅酸盐研究所 | A method of limitation matrices of composite material propagation of internal cracks |
| CN110256082A (en) * | 2019-05-17 | 2019-09-20 | 浙江理工大学 | Reaction-sintered prepares monocrystalline silicon carbide nanofiber/carbon/silicon carbide ceramic matrix composite method |
| CN110357647A (en) * | 2018-10-08 | 2019-10-22 | 湖南德智新材料有限公司 | A kind of ceramic matric composite and preparation method thereof of silicon carbide nanometer line enhancing |
| CN111039687A (en) * | 2019-12-13 | 2020-04-21 | 中国航空制造技术研究院 | A kind of continuous fiber reinforced ceramic matrix composite material without damage hole making method |
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| CN111647386A (en) * | 2020-06-17 | 2020-09-11 | 中国民航大学 | Preparation method of silicon carbide nanowire in-situ growth toughened ceramic precursor type high-temperature adhesive |
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