CN108947557A - A kind of carbon/carbon compound material and preparation method thereof - Google Patents
A kind of carbon/carbon compound material and preparation method thereof Download PDFInfo
- Publication number
- CN108947557A CN108947557A CN201811117812.9A CN201811117812A CN108947557A CN 108947557 A CN108947557 A CN 108947557A CN 201811117812 A CN201811117812 A CN 201811117812A CN 108947557 A CN108947557 A CN 108947557A
- Authority
- CN
- China
- Prior art keywords
- carbon
- compound material
- coat
- carbon compound
- silicon carbide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 217
- 239000000463 material Substances 0.000 title claims abstract description 130
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 128
- 150000001722 carbon compounds Chemical class 0.000 title claims abstract description 117
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 64
- 150000001875 compounds Chemical class 0.000 claims abstract description 47
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910010271 silicon carbide Inorganic materials 0.000 claims abstract description 39
- 238000000576 coating method Methods 0.000 claims description 48
- 239000011248 coating agent Substances 0.000 claims description 46
- 238000000034 method Methods 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 17
- 239000010439 graphite Substances 0.000 claims description 17
- 238000005245 sintering Methods 0.000 claims description 17
- 239000010410 layer Substances 0.000 claims description 14
- 239000011812 mixed powder Substances 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 11
- 239000000843 powder Substances 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 9
- ZOXJGFHDIHLPTG-UHFFFAOYSA-N Boron Chemical compound [B] ZOXJGFHDIHLPTG-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 229910018557 Si O Inorganic materials 0.000 claims description 9
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 9
- 238000003763 carbonization Methods 0.000 claims description 9
- 238000010438 heat treatment Methods 0.000 claims description 9
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Inorganic materials [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 claims description 9
- 239000011863 silicon-based powder Substances 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 8
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000007704 transition Effects 0.000 claims description 6
- 230000008569 process Effects 0.000 claims description 5
- 238000007598 dipping method Methods 0.000 claims description 4
- 239000002356 single layer Substances 0.000 claims description 4
- 239000002904 solvent Substances 0.000 claims description 4
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 4
- RELMFMZEBKVZJC-UHFFFAOYSA-N 1,2,3-trichlorobenzene Chemical class ClC1=CC=CC(Cl)=C1Cl RELMFMZEBKVZJC-UHFFFAOYSA-N 0.000 claims description 3
- 229910007948 ZrB2 Inorganic materials 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- 150000004816 dichlorobenzenes Chemical class 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000002791 soaking Methods 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 3
- 238000002679 ablation Methods 0.000 abstract description 13
- 239000003963 antioxidant agent Substances 0.000 abstract description 9
- 230000003078 antioxidant effect Effects 0.000 abstract description 9
- 235000006708 antioxidants Nutrition 0.000 abstract description 9
- 239000010408 film Substances 0.000 description 37
- 239000000243 solution Substances 0.000 description 22
- 239000002131 composite material Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 12
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 9
- 239000001301 oxygen Substances 0.000 description 9
- 229910052760 oxygen Inorganic materials 0.000 description 9
- 238000007254 oxidation reaction Methods 0.000 description 8
- 230000007547 defect Effects 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 230000009471 action Effects 0.000 description 5
- 238000005452 bending Methods 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 230000003026 anti-oxygenic effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 229920000049 Carbon (fiber) Polymers 0.000 description 2
- 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
- 229910052786 argon Inorganic materials 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 230000003139 buffering effect Effects 0.000 description 2
- 239000004917 carbon fiber Substances 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000005253 cladding Methods 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 210000000867 larynx Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910003465 moissanite Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
-
- 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
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Composite Materials (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The present invention relates to a kind of carbon/carbon compound materials and preparation method thereof.Specifically, the carbon/carbon compound material includes carbon/carbon compound material ontology, is formed with compound tie coat on the surface of the carbon/carbon compound material ontology；The compound tie coat includes the buffer coat being formed on carbon/carbon compound material body surface and the coat of silicon carbide that is formed on buffer coat surface；Wherein, the buffer coat is graphene film.The carbon/carbon compound material has preferable anti-oxidant ablation property and intensity and toughness.
Description
Technical field
The present invention relates to carbon/carbon compound material technical field more particularly to a kind of carbon/carbon compound material and its preparation sides
Method.
Background technique
Carbon/carbon compound material is the C-base composte material with fibre reinforced, has low-density, high intensity, high-termal conductivity
And the series of advantages such as low-expansion coefficient, and it is able to maintain higher mechanical property with temperature raising, it has been successfully applied to navigate
Its aircraft nose cone, rocket engine larynx lining, high thrust-weight ratio engine hot-end component.But carbon/carbon compound material is in hot environment
In anti-oxidant and ablation resistance it is poor, it is the bottleneck for being most difficult to break through in carbon/carbon compound material practical application that high temperature is oxidizable.
In order to meet the demand for development of Future Spacecraft, the resistance to ablation of carbon/carbon compound material and antioxygenic property must be further strengthened.
Stop contact of the oxygen-containing gas with matrix by the surface prepares coating in carbon/carbon compound material, is to realize carbon/carbon compound material
The inevitable choice of the anti-oxidant anti-ablation of high-temperature long life.
The introducing of coating can introduce new interface in composite inner, need to alleviate using transition zone thus coating with
The unmatched problem of carbon/carbon composite material base isolator CTE.Silicon carbide (SiC) coating due to carbon/carbon compound material
Physics, chemical compatibility are good and are widely used as transition zone use.But inventor has found under study for action, due to SiC and carbon/
The defects of difference between carbon composite thermal expansion coefficient can keep coating surface cracked.When forming external coating, if
These defects, which cannot be effectively controlled, to be fully populated with.It, can shape after outer layer is oxidized and is destroyed in high-temperature oxydation
At oxygen channel, lead to the rapid oxidation of carbon/carbon compound material ontology, reduces the oxidation resistance of coating.
In view of this, the present invention is specifically proposed.
Summary of the invention
(1) technical problems to be solved
The technical problem to be solved by the present invention is how to improve the anti-oxidant ablation resistance of existing carbon/carbon compound material.
(2) technical solution
In order to solve the above-mentioned technical problems, the present invention provides following technical solutions:
A kind of carbon/carbon compound material, including carbon/carbon compound material ontology, on the surface of the carbon/carbon compound material ontology
On be formed with compound tie coat；The compound tie coat includes the buffering being formed on carbon/carbon compound material body surface
Coating and the coat of silicon carbide being formed on buffer coat surface；Wherein, the buffer coat is graphene film.
Preferably, the compound tie coat also has by the buffer coat and the silicon carbide on coat of silicon carbide
Coating, which is repeated in, is formed by multilayered structure；Wherein, in multilayered structure, the buffer coat and the coat of silicon carbide
The number of plies is identical.
Preferably, the graphene film has 1~5 μm of thickness.
Preferably, the graphene for being used to form the graphene film is single-layer graphene and/or multi-layer graphene.
Preferably, the compound transition zone has 1~100 μm of thickness.
Preferably, the carbon/carbon compound material ontology has 1.70~1.85g/cm3Density.
Preferably, external coating is also formed on the surface of the compound tie coat；Preferably, the external coating is
Zr-Si-O coating, Y-Si-O coating, Yb-Si-O coating, ZrB2Any one of coating.
The present invention also provides a kind of preparation methods of carbon/carbon compound material described in any of the above-described, include the following steps:
(1) carbon/carbon compound material ontology is provided；
(2) the satisfactory graphene film of thickness is formed on carbon/carbon compound material body surface as buffer coat；
(3) coat of silicon carbide is formed on buffer coat surface, thus multiple on the carbon/carbon compound material body surface
It closes and forms the compound tie coat comprising buffer coat and coat of silicon carbide；
Preferably, also have by the buffer coat and the carbonization on coat of silicon carbide when the compound tie coat
Silicon coating is repeated in when being formed by multilayered structure, and the preparation method further includes step (4):
It is repeated in step (2) and step (3), until being compounded to form thickness on the carbon/carbon compound material body surface
Spend satisfactory compound tie coat.
Preferably, the step (2) carries out as follows:
(21) graphene is configured to graphene solution；
(22) graphene solution is carried out by dipping, the method brushed or sprayed and carbon/carbon compound material ontology compound；
(23) it is carbonized；
(24) step (22) and (23) are repeated in, until graphene film thickness meets the requirements；
Preferably, the concentration of the graphene solution is 1~10wt%；
Preferably, the graphene solution uses water, methanol, ethyl alcohol, isopropanol, chloroform, carbon tetrachloride, acetone, acetic acid
Ethyl ester, tetrahydrofuran, toluene, dimethylbenzene, dimethyl sulfoxide, chlorobenzene, dichloro-benzenes or any one or more of conduct of trichloro-benzenes
Solvent is formulated；
Preferably, the carbonization is carried out using sintering process, is preferably sintered at 500~1500 DEG C.
Preferably, the step (3) carries out as follows:
(31) silicon powder, graphite powder, boron powder and alumina powder are configured to mixed powder；
(32) then existed with the mixed powder to through step (2), treated that carbon/carbon compound material ontology embeds
It is sintered, makes on buffer coat surface with coat of silicon carbide under oxygen-free atmosphere；
Preferably, in mixed powder, the mass fraction of the silicon powder is 40~60%, the mass fraction of the graphite powder
Mass fraction for 20~30%, the boron powder is 10~15%, and the mass fraction of the alumina powder is 5~10%；
Preferably, the sintering carries out at 1600~1800 DEG C, and soaking time is 4~6 hours；
It is highly preferred that the sintering is carried out as follows heating:
1200~1300 DEG C are risen to the heating speed of 2~3 DEG C/min, then rises to 1600 with the heating rate of 1~2 DEG C/min
~1800 DEG C.
(3) beneficial effect
Above-mentioned technical proposal of the invention has the advantages that
(1) carbon/carbon compound material provided by the invention is formed with buffer layer between SiC coating and composite body,
Buffer layer uses the graphite dilute film good with composite body compatibility, improves the intensity and toughness of material, while significantly mentioning
High anti-oxidation ablation property；
(2) The present invention gives the preparation methods of the dilute composite coating of carbon/carbon compound material graphite, can be according to use environment need
The preparation of multi-cycle composite coating is carried out to required thickness, method is simple and feasible；
(3) present invention is coated using graphite weak solution to carbon/carbon compound material body surface, is formed by sintering continuous
The dilute film of graphite fits in carbon/carbon compound material body surface, the pit defect of carbon/carbon compound material body surface is carried out effective
Cladding, the quantity by reducing hole are reduced, and size reduces, and effectively prevents the inside diffusion of oxygen, improves antioxygenic property；
(4) present invention by prepare the thin film of graphite, film carbonization treatment, investment prepare SiC coating and etc. technique
Design, ensure that the efficient form compact and stable of composite coating.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, below in conjunction with the embodiment of the present invention, to this hair
Bright technical solution is clearly and completely described.Obviously, described embodiment is a part of the embodiments of the present invention, and
The embodiment being not all of.Based on the embodiments of the present invention, those of ordinary skill in the art are not making creative work
Under the premise of every other embodiment obtained, shall fall within the protection scope of the present invention.
The present invention provides a kind of carbon/carbon compound material in first aspect, has the following structure:
The carbon/carbon compound material includes carbon/carbon compound material ontology, and in the carbon/carbon compound material ontology
Compound tie coat is formed on surface；The compound tie coat includes being formed on carbon/carbon compound material body surface
Buffer coat and the coat of silicon carbide being formed on buffer coat surface；Wherein, the buffer coat is graphene film.
Inventor has found under study for action, although coat of silicon carbide has and the good physics of carbon/carbon compound material, chemical phase
Capacitive and similar linear expansion coefficient, but still coating surface can be made often to go out in difference present on linear expansion coefficient between the two
The defects of existing crackle, when forming external coating on coat of silicon carbide, if cannot be effectively controlled will be by for these defects
It is fully populated with.In high-temperature oxydation, after outer layer is oxidized and is destroyed, oxygen channel will form, lead to carbon/carbon compound material sheet
The rapid oxidation of body reduces the oxidation resistance of coating.
Based on above-mentioned discovery, inventor is provided with buffer coat between coat of silicon carbide and carbon/carbon compound material ontology,
And using graphene film as buffer coat.Experiments verify that graphene film and composite body have better compatibility,
Not only effectively overcome the appearance of crackle in coating, but also the continuous dilute film of graphite fits in composite body surface, it will be compound
The pit defect on material body surface is effectively coated, and by reducing the quantity and its size of hole, effectively prevents oxygen
Inwardly diffusion, improves the anti-oxidant ablation property of material.
In addition, the preferable toughness of graphene and intensity can also greatly improve the mechanical property of material, composite material is improved
Intensity and toughness.
Inventors have found that the thickness of graphene film has anti-oxidant ablation property, toughness and the intensity of carbon/carbon compound material
It influences.In the identical situation of other situations, thicker graphene film can lack the pit of carbon/carbon compound material body surface
It is trapped into the significantly more efficient cladding of row, can preferably stop the infiltration of extraneous oxygen, while the raising journey of the toughness of material and intensity
Degree is also more significant.But the excessive graphene film that also results in of thickness is the same as of carbon/carbon compound material ontology and coat of silicon carbide
It is reduced with property.Graphene film is preferably with a thickness of 1~5 μm.The graphene for being used to form the graphene film can be single layer stone
Black alkene and/or multi-layer graphene.
The satisfactory graphene film of a layer thickness can be formed on carbon/carbon compound material ontology and a layer thickness meets
It is required that coat of silicon carbide.But inventor has found under study for action, in the case where carbon/carbon compound material bulk density is identical, graphene
The increase of film and the coat of silicon carbide number of plies influences the performance of final composite material so that the thickness of compound tie coat increases
It is larger.Therefore, carbon/carbon compound material provided by the invention can also be formed on coat of silicon carbide by the buffer coat and institute
It states coat of silicon carbide and is repeated in and be formed by multilayered structure；Wherein, in multilayered structure, the buffer coat and the carbonization
The number of plies of silicon coating is identical.This design can suitably increase compound mistake under the premise of being no more than graphene film optimum thickness
The thickness of coating is crossed, to improve the anti-oxidant ablation property and mechanical property of composite material.It is verified, compound tie coat
Thickness is preferably 1~100 μm, for example, the thickness of the compound tie coat can within the scope of this all numerical value or
Subrange, for example, can be 1 μm, 2 μm, 3 μm, 4 μm, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μ
M, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, 100 μm, it is described
Subrange can for 1~10 μm, 5~15 μm, 20~30 μm, 25~40 μm, 45~60 μm, 50~70 μm, 40~80 μm, 60~
90 μm, 65~100 μm or 80~100 μm.On this basis, the number of plies of multilayered structure can be according to the thickness of compound tie coat
It determines.
It should be noted that the present invention is not defined the preparation method of carbon/carbon compound material ontology, it can be using existing
There is method to prepare carbon/carbon compound material ontology, such as chemical vapour deposition technique, presoma carbonization treatment technique etc., but the present invention
Higher to the density requirements of carbon/carbon compound material ontology, density is preferably in 1.70~1.85g/cm3, can be within the scope of this
All numerical value or subrange, for example, can be 1.70g/cm3、1.71g/cm3、1.72g/cm3、1.73g/cm3、1.74g/cm3、
1.75g/cm3、1.76g/cm3、1.77g/cm3、1.78g/cm3、1.79g/cm3、1.80g/cm3、1.81g/cm3、1.82g/cm3、
1.83g/cm3、1.84g/cm3Or 1.85g/cm3。
Inventor has found that the density of carbon/carbon compound material ontology is too small under study for action, carbon/carbon compound material short texture,
Though the preparation for follow-up coating provides enough reaction infiltration spaces, the composite materials property finally obtained is poor,
Mainly due to carbon/carbon material density too eutectic seep when fiber it is easily damaged.When carbon/carbon compound material density becomes within the above range
Change, final product material mechanical performance and antioxygenic property is influenced unobvious.
Carbon/carbon compound material provided by the invention is applied in addition to forming compound transition on carbon/carbon compound material body surface
Layer is outer, can also form external coating on the surface of compound tie coat.External coating can select temperature resistant grade height, oxygen diffusion system
Number is low, coatings that heat emissivity coefficient is high, improves service performance of the carbon/carbon compound material under superhigh temperature aerobic environment and uses the longevity
Life.The external coating can be Zr-Si-O coating, Y-Si-O coating, Yb-Si-O coating, ZrB2Any one of coating.When
So, the coating that existing other temperature resistant grades are high, diffusion coefficient is low, heat emissivity coefficient is high can also be used as outer painting of the invention
Layer.The preparation method of above-mentioned several coatings can be prepared using existing method, it is no longer described in detail in the present invention.
The present invention provides a kind of preparation method of any of the above-described kind of carbon/carbon compound material in second aspect, including
Following steps:
(1) carbon/carbon compound material ontology is provided；
As described in foregoing teachings, carbon/carbon compound material ontology can be prepared using existing preparation method, such as chemistry
Vapour deposition process, presoma carbonization treatment technique etc..The structure of carbon/carbon compound material ontology is also the prior art, can be served as reasons
The structure of carbon fiber and matrix composition.But.In order to obtain preferably effect, the density of carbon/carbon compound material ontology can be controlled
System is in 1.70~1.85g/cm3。
(2) the satisfactory graphene film of thickness is formed on carbon/carbon compound material body surface as buffer coat；
In some embodiments, the graphene film can be prepared as follows:
(21) graphene is configured to graphene solution；Preferably, the concentration of the graphene solution is 1~10wt%,
Can be all numerical value or subrange within the scope of this, for example, can for 1wt%, 2wt%, 3wt%, 4wt%, 5wt%,
6wt%, 7wt%, 8wt%, 9wt%, 10wt%, the subrange can be 1~5wt%, 3~8wt%, 5~10wt% or 6
~10wt%.
The ratio of graphene and solvent is appropriate in graphene solution with above-mentioned concentration, solution have suitable concentration and
Adhesive force, can easily be adhered to component surface, while will not there is a phenomenon where flow.
In some embodiments, the graphene solution can use water, methanol, ethyl alcohol, isopropanol, chloroform, four chlorinations
Any in carbon, acetone, ethyl acetate, tetrahydrofuran, toluene, dimethylbenzene, dimethyl sulfoxide, chlorobenzene, dichloro-benzenes or trichloro-benzenes
It plants or a variety of conduct solvents is formulated.
(22) graphene solution is carried out by dipping, the method brushed or sprayed and carbon/carbon compound material ontology compound；
In this step, graphene solution and the compound of carbon/carbon compound material ontology can be using dipping, brushing or sprayings
Method carry out.For dip time, there is no particular limitation, and inventor has found under study for action, as long as determining graphene solution
Concentration is in above-mentioned suitable range, and the factors such as dip time, spraying uniformity are to the dilute film thickness of the graphite of formation and subsequent packet
Burying reaction influences unobvious, therefore the present invention is to compound specific process parameter (such as dip time) that there is no particular limitation, in reality
In the operation of border, it can be determined according to the actual situation.
(23) it is carbonized；
In this step, carbonization is carried out by the way of sintering, makes graphene carbonization in carbon/carbon compound material ontology
The graphene film of compact structure is formed on surface.More expediently, the temperature control of sintering is at 500~1500 DEG C, sintering temperature
It can be any subrange within the scope of all numerical value within the scope of this either this, for example, can be 500 DEG C, 550 DEG C, 600
℃、650℃、700℃、750℃、800℃、850℃、900℃、950℃、1000℃、1050℃、1100℃、1150℃、1200
DEG C, 1250 DEG C, 1300 DEG C, 1350 DEG C, 1400 DEG C, 1450 DEG C or 1500 DEG C, the subrange can be 500~600 DEG C, 700
~900 DEG C, 900~1200 DEG C, 1000~1300 or 1200~1500 DEG C.
For sintering time, the present invention is not particularly limited this, can required sintering determines according to actual conditions
Time.
(24) step (22) and (23) are repeated in, until graphene film thickness meets the requirements；
(3) coat of silicon carbide is formed on buffer coat surface, thus multiple on the carbon/carbon compound material body surface
It closes and forms the compound tie coat comprising buffer coat and coat of silicon carbide；
Coat of silicon carbide in the present invention is prepared using investment, and specifically, the coat of silicon carbide can be according to
As under type carries out:
(31) silicon powder, graphite powder, boron powder and alumina powder are configured to mixed powder；
Preferably, in mixed powder,
The mass fraction of the silicon powder is 40~60%, for example, can for 40%, 41%, 42%, 43%, 44%,
45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59% or
60%；
The mass fraction of the graphite powder is 20~30%, for example, can for 20%, 21%, 22%, 23%, 24%,
25%, 26%, 27%, 28%, 29% or 30%；
The mass fraction of the boron powder is 10~15%, for example, can for 10%, 11%, 12%, 13%, 14% or
15%；
The mass fraction of the alumina powder is 5~10%, for example, can be 5%, 6%, 7%, 8%, 9% or 10%.
When preparing mixed powder, in order to obtain the preferable mixed powder of granularity, can by silicon powder, graphite powder, boron powder and
Alumina powder be put into using agate ball as ball milling in the planetary ball mill in abrasive media for a period of time (for example, 2~4 hours),
To obtain the mixed powder for embedding carbon/carbon compound material ontology.
(32) then existed with the mixed powder to through step (2), treated that carbon/carbon compound material ontology embeds
It is sintered, makes on buffer coat surface with coat of silicon carbide under oxygen-free atmosphere；
Preferably, it is described sintering carried out at 1600~1800 DEG C, for example, can for 1600 DEG C, 1650 DEG C, 1700 DEG C,
1750 DEG C or 1800 DEG C, soaking time is 4~6 hours, for example, can be 4 hours, 5 hours or 6 hours；
It is highly preferred that the sintering is carried out as follows heating:
With 2~3 DEG C/min (for example, can for 2 DEG C/min, 2.1 DEG C/min, 2.2 DEG C/min, 2.3 DEG C/min, 2.4 DEG C/
Min, 2.5 DEG C/min, 2.6 DEG C/min, 2.7 DEG C/min, 2.8 DEG C/min, 2.9 DEG C/min or 3 DEG C/min) heating speed rise to
1200~1300 DEG C (for example, can be 1200 DEG C, 1210 DEG C, 1220 DEG C, 1230 DEG C, 1240 DEG C, 1250 DEG C, 1260 DEG C, 1270
DEG C, 1280 DEG C, 1290 DEG C or 1300 DEG C), then with 1~2 DEG C/min (for example, can for 1 DEG C/min, 1.1 DEG C/min, 1.2 DEG C/
Min, 1.3 DEG C/min, 1.4 DEG C/min, 1.5 DEG C/min, 1.6 DEG C/min, 1.7 DEG C/min, 1.8 DEG C/min, 1.9 DEG C/min or 2
DEG C/min) heating rate rise to 1600~1800 DEG C.
When the compound tie coat also has by the buffer coat and the coat of silicon carbide on coat of silicon carbide
It is repeated in when being formed by multilayered structure, the preparation method further includes step (4):
It is repeated in step (2) and step (3), until being compounded to form thickness on the carbon/carbon compound material body surface
Spend satisfactory compound tie coat.
It is the embodiment that the present invention enumerates below.
Embodiment 1
(1) carbon/carbon compound material ontology is prepared
Carbon fiber precast body is packed into CVI-C furnace, under the conditions of vacuum condition and 1020 DEG C of temperature, is passed through C3H8With
Ar mixed gas, deposition are come out of the stove for 600 hours, and acquisition density is 1.70g/cm3Carbon/carbon compound material ontology.
(2) buffer layer is compound
(21) it takes 1g mono-layer graphite is dilute to be added in 100g aqueous solution, carries out ultrasonic treatment 30min, it is molten to obtain graphene
Liquid.
(22) carbon/carbon compound material ontology is placed in graphite weak solution and is impregnated 2 hours.
(23) drying is sintered after taking out the carbon/carbon compound material ontology in step (22), sintering temperature 500
DEG C, sintering time is 6 hours, to form the dilute film of graphite with a thickness of 1 μm on carbon/carbon compound material ontology as buffering
Layer.
(3) coat of silicon carbide is compound
(31) silicon powder, graphite powder, boron powder, alumina powder is taken to be mixed evenly；In mixed material, the quality point of silicon powder
Number content is 55%, and the mass fraction content of graphite powder is 25%, and the mass fraction content of boron powder is 15%, the matter of alumina powder
Measuring fractional content is 5%；Mixed material is placed in using agate ball as ball milling 2 hours in the planetary ball mill in abrasive media,
It obtains embedding required mixed powder.
(32) above-mentioned mixed powder half is placed in graphite crucible, place into be formed with graphene film carbon/carbon it is compound
Material body is subsequently placed into the other half embedding powder and covers above-mentioned ontology；Graphite crucible is put into high-temperature atmosphere sintering furnace,
Vacuumizing makes vacuum degree reach -0.1MPa, fidelity sky 30min, after vacuum meter instruction is stablized, takes out again after logical argon gas to normal pressure true
Sky repeats this process 3 times, and whole process leads to argon gas protection, to make in furnace for oxygen-free atmosphere.Furnace temperature is risen to 1700 from room temperature
DEG C, 4 hours are kept the temperature, power supply cooled to room temperature is finally closed, to form coat of silicon carbide in graphene membrane surface.
(4) it is repeated in step (2), step (3), is repeated 2 times, the carbon/carbon with the compound tie coat of 10 μ m-thicks is obtained
Composite material.
Carbon/carbon compound material made from embodiment 1 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 0.8%.
Embodiment 2
That the preparation method is the same as that of Example 1 is substantially the same for embodiment 2, the difference is that:
Circulation repeatedly, obtains the carbon/carbon compound material with the compound tie coat of 20 μ m-thicks in step (4).
Carbon/carbon compound material made from embodiment 2 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 0.5%.
Embodiment 3
That the preparation method is the same as that of Example 1 is substantially the same for embodiment 3, the difference is that:
Circulation repeatedly, obtains the carbon/carbon compound material with the compound tie coat of 100 μ m-thicks in step (4).
Carbon/carbon compound material made from embodiment 3 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 0.4%.
Embodiment 4
That the preparation method is the same as that of Example 1 is substantially the same for embodiment 4, the difference is that:
In step (2), it is repeated in step (22) and (23) repeatedly, until being formed on carbon/carbon compound material ontology
With a thickness of the dilute film of 5 μm of graphite.
Carbon/carbon compound material made from embodiment 4 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 0.6%.
Embodiment 5
That the preparation method is the same as that of Example 1 is substantially the same for embodiment 5, the difference is that:
The density of carbon/carbon compound material ontology is 1.85g/cm3。
Carbon/carbon compound material made from embodiment 5 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 0.8%.
Comparative example 1
That the preparation method is the same as that of Example 1 is substantially the same for comparative example 1, the difference is that:
Circulation repeatedly, obtains the carbon/carbon compound material with the compound tie coat of 130 μ m-thicks in step (4).
Carbon/carbon compound material made from comparative example 1 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 0.9%.
Comparative example 2
That the preparation method is the same as that of Example 1 is substantially the same for comparative example 2, the difference is that:
In step (2), it is repeated in step (22) and (23) repeatedly, until being formed on carbon/carbon compound material ontology
With a thickness of the dilute film of 8 μm of graphite.
Carbon/carbon compound material made from comparative example 2 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 1.0%.
Comparative example 3
That the preparation method is the same as that of Example 1 is substantially the same for comparative example 3, the difference is that:
The density of carbon/carbon compound material ontology is 1.9g/cm3。
Carbon/carbon compound material made from comparative example 3 is placed in 1500 DEG C of air after aoxidizing 100h, sample mass loss late
It is 1.0%.
In addition, the present invention also to the fracture toughness of carbon/carbon compound material made from above-mentioned each embodiment and comparative example and
Bending strength is detected, and testing result is shown in Table 1.
From table 1 it follows that the anti-oxidant ablation property and bending strength of the composite material of embodiment 2 and fracture are tough
Property is superior to embodiment 1, this shows that the inoxidizability, resistance to of carbon/carbon compound material can be improved in compound tie coat thickness increase
Ablative and intensity and toughness.The performance test results of the material of embodiment 3 also further demonstrate this conclusion.But it compares
Compound tie coat in example 1 has 130 μm of thickness, and from the point of view of its testing result, the thickness of compound tie coat is not yet
It is to be the bigger the better, the binding ability that will cause between coating if blocked up reduces, and increases coating stripping in the environment of oxygen immerses
From speed.Based on this consideration, the thickness of compound tie coat of the invention is preferably selected as 1~100 μm, should using having
Anti-oxidant ablation property, bending strength and the fracture toughness of composite material can be improved as transition zone for the coating of thickness.
Embodiment 4 and difference of the embodiment 1 in preparation process are that graphene film thickness is different, the graphite of embodiment 4
The thickness of alkene film is greater than the thickness of the graphene film in embodiment.From the point of view of testing result, the composite material of embodiment 4 resists
Oxidation ablation performance and bending strength and fracture toughness are superior to embodiment 1, this shows that the increase of graphene film thickness can mention
Inoxidizability, ablation resistance and the intensity and toughness of high carbon/carbon compound material.But the graphene film in comparative example 2 has 8 μm
Thickness, the thickness than the graphene film of embodiment 1 is big, but from the point of view of its testing result, shows the thickness of graphene film also simultaneously
Non- is to be the bigger the better, and the excessive oxygen of thickness will increase contact area after penetrating into, and reduces inoxidizability, graphite dilute interlayer phase when fracture
Interreaction force decrease can be such that fracture toughness reduces.Based on this consideration, the thickness of graphene film of the invention is preferably selected as 1
~5 μm, more preferably 3 μm.
The difference of embodiment 5 and embodiment 1 in preparation process is the density of carbon/carbon compound material ontology used not
Together, the density of embodiment 5 is slightly larger than embodiment 1.From the point of view of the testing result of the two, the bending of the composite material of embodiment 5 is strong
Degree and fracture toughness are better than embodiment 1.If carbon/carbon compound material ontology has lower density, short texture, after being
The preparation of continuous coating provides enough reaction infiltration spaces, but the composite materials property finally obtained is poor, mainly
Since fiber is easily damaged when carbon/carbon material density too eutectic seeps.From the point of view of the testing result of comparative example 3, carbon/carbon compound material sheet
The density of body is also not the bigger the better, and density is bigger, and material can obtain better mechanical property, but sacrifices the anti-of material
Oxidation susceptibility.Comprehensively consider, the density of carbon/carbon compound material ontology used in the present invention is preferably selected as 1.7~1.85g/
cm3。
Finally, it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
Present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: it still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features；
And these are modified or replaceed, technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution spirit and
Range.
Claims (10)
1. a kind of carbon/carbon compound material, including carbon/carbon compound material ontology, which is characterized in that in the carbon/carbon compound material
Compound tie coat is formed on the surface of ontology；The compound tie coat includes being formed in this body surface of carbon/carbon compound material
Buffer coat on face and the coat of silicon carbide being formed on buffer coat surface；Wherein, the buffer coat is graphene film.
2. carbon/carbon compound material according to claim 1, which is characterized in that the compound tie coat is applied in silicon carbide
Also have on layer and is repeated in by the buffer coat and the coat of silicon carbide and is formed by multilayered structure；Wherein, in multilayer
In structure, the buffer coat is identical with the number of plies of the coat of silicon carbide.
3. carbon/carbon compound material according to claim 1, which is characterized in that the graphene film has 1~5 μm of thickness
Degree.
4. carbon/carbon compound material according to claim 1, which is characterized in that be used to form the graphite of the graphene film
Alkene is single-layer graphene and/or multi-layer graphene.
5. carbon/carbon compound material according to claim 1 or 2, which is characterized in that the compound transition zone has 1~100
μm thickness.
6. carbon/carbon compound material according to claim 1, which is characterized in that the carbon/carbon compound material ontology has
1.70~1.85g/cm3Density.
7. carbon/carbon compound material according to any one of claims 1 to 6, which is characterized in that in the compound tie coat
Surface on be also formed with external coating；Preferably, the external coating be Zr-Si-O coating, Y-Si-O coating, Yb-Si-O coating,
ZrB2Any one of coating.
8. a kind of preparation method of any one of claim 1 to 7 carbon/carbon compound material, which is characterized in that including walking as follows
It is rapid:
(1) carbon/carbon compound material ontology is provided；
(2) the satisfactory graphene film of thickness is formed on carbon/carbon compound material body surface as buffer coat；
(3) coat of silicon carbide is formed on buffer coat surface, thus the complex on the carbon/carbon compound material body surface
At the compound tie coat comprising buffer coat and coat of silicon carbide；
Preferably, also have on coat of silicon carbide when the compound tie coat and applied by the buffer coat and the silicon carbide
Layer is repeated in when being formed by multilayered structure, and the preparation method further includes step (4):
It is repeated in step (2) and step (3), until being compounded to form thickness symbol on the carbon/carbon compound material body surface
Close desired compound tie coat.
9. preparation method according to claim 8, which is characterized in that the step (2) carries out as follows:
(21) graphene is configured to graphene solution；
(22) graphene solution is carried out by dipping, the method brushed or sprayed and carbon/carbon compound material ontology compound；
(23) it is carbonized；
(24) step (22) and (23) are repeated in, until graphene film thickness meets the requirements；
Preferably, the concentration of the graphene solution is 1~10wt%；
Preferably, the graphene solution using water, methanol, ethyl alcohol, isopropanol, chloroform, carbon tetrachloride, acetone, ethyl acetate,
Tetrahydrofuran, toluene, dimethylbenzene, dimethyl sulfoxide, chlorobenzene, dichloro-benzenes or any one or more of conduct solvent of trichloro-benzenes are matched
It makes；
Preferably, the carbonization is carried out using sintering process, is preferably sintered at 500~1500 DEG C.
10. preparation method according to claim 8, which is characterized in that the step (3) carries out as follows:
(31) silicon powder, graphite powder, boron powder and alumina powder are configured to mixed powder；
(32) with the mixed powder to through step (2), treated that carbon/carbon compound material ontology embeds, then in anaerobic
It is sintered, makes on buffer coat surface with coat of silicon carbide under atmosphere；
Preferably, in mixed powder, the mass fraction of the silicon powder is 40~60%, and the mass fraction of the graphite powder is 20
~30%, the mass fraction of the boron powder is 10~15%, and the mass fraction of the alumina powder is 5~10%；
Preferably, the sintering carries out at 1600~1800 DEG C, and soaking time is 4~6 hours；
It is highly preferred that the sintering is carried out as follows heating:
1200~1300 DEG C are risen to the heating speed of 2~3 DEG C/min, then 1600 are risen to the heating rate of 1~2 DEG C/min~
1800℃。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811117812.9A CN108947557B (en) | 2018-09-25 | 2018-09-25 | Carbon/carbon composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811117812.9A CN108947557B (en) | 2018-09-25 | 2018-09-25 | Carbon/carbon composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN108947557A true CN108947557A (en) | 2018-12-07 |
| CN108947557B CN108947557B (en) | 2021-05-14 |
Family
ID=64472223
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811117812.9A Active CN108947557B (en) | 2018-09-25 | 2018-09-25 | Carbon/carbon composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108947557B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110803941A (en) * | 2019-11-26 | 2020-02-18 | 航天特种材料及工艺技术研究所 | Carbon-silicon carbide composite material surface oxidation resistant coating and preparation method thereof |
| CN113024281A (en) * | 2021-02-28 | 2021-06-25 | 西北工业大学 | Silicon carbide/graphene bionic laminated coating and preparation method thereof |
| CN114773079A (en) * | 2022-05-10 | 2022-07-22 | 吉林联科特种石墨材料有限公司 | Preparation method of hard carbon fiber thermal insulation material with graphene efficient erosion-resistant layer |
| CN114920573A (en) * | 2022-06-06 | 2022-08-19 | 吉林联科特种石墨材料有限公司 | Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903791A (en) * | 2005-07-28 | 2007-01-31 | 西北工业大学 | Carbon/carbon composite material base silicon carbide coating layer and its preparation method |
| CN101462889A (en) * | 2009-01-16 | 2009-06-24 | 南开大学 | Graphene and carbon fiber composite material, and preparation thereof |
| CN101565328A (en) * | 2009-05-26 | 2009-10-28 | 西北工业大学 | Method for preparing carbon/carbon composite material antioxidation coating layer |
| CN103360124A (en) * | 2013-07-10 | 2013-10-23 | 航天材料及工艺研究所 | Composite coating and application thereof in carbon/carbon composite material |
| CN104211423A (en) * | 2014-09-17 | 2014-12-17 | 哈尔滨工业大学 | Preparation method of graphene modified carbon/carbon composite material |
| US20150140211A1 (en) * | 2013-11-19 | 2015-05-21 | Cvd Equipment Corporation | Scalable 2D-Film CVD Synthesis |
| CN105461357A (en) * | 2015-11-18 | 2016-04-06 | 中南大学 | A charcoal/charcoal composite material ablation-resisting coating and a preparing process thereof |
| CN105506579A (en) * | 2015-12-15 | 2016-04-20 | 南京工程学院 | Preparation method of graphene coated silicon carbide nanowire |
| EP3282038A2 (en) * | 2016-08-11 | 2018-02-14 | Goodrich Corporation | High temperature oxidation protection for composites |
| CN108530110A (en) * | 2018-06-08 | 2018-09-14 | 中南大学 | A kind of superhigh temperature ceramics coating of C/C composite materials and preparation method thereof |
-
2018
- 2018-09-25 CN CN201811117812.9A patent/CN108947557B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903791A (en) * | 2005-07-28 | 2007-01-31 | 西北工业大学 | Carbon/carbon composite material base silicon carbide coating layer and its preparation method |
| CN101462889A (en) * | 2009-01-16 | 2009-06-24 | 南开大学 | Graphene and carbon fiber composite material, and preparation thereof |
| CN101565328A (en) * | 2009-05-26 | 2009-10-28 | 西北工业大学 | Method for preparing carbon/carbon composite material antioxidation coating layer |
| CN103360124A (en) * | 2013-07-10 | 2013-10-23 | 航天材料及工艺研究所 | Composite coating and application thereof in carbon/carbon composite material |
| US20150140211A1 (en) * | 2013-11-19 | 2015-05-21 | Cvd Equipment Corporation | Scalable 2D-Film CVD Synthesis |
| CN104211423A (en) * | 2014-09-17 | 2014-12-17 | 哈尔滨工业大学 | Preparation method of graphene modified carbon/carbon composite material |
| CN105461357A (en) * | 2015-11-18 | 2016-04-06 | 中南大学 | A charcoal/charcoal composite material ablation-resisting coating and a preparing process thereof |
| CN105506579A (en) * | 2015-12-15 | 2016-04-20 | 南京工程学院 | Preparation method of graphene coated silicon carbide nanowire |
| EP3282038A2 (en) * | 2016-08-11 | 2018-02-14 | Goodrich Corporation | High temperature oxidation protection for composites |
| CN108530110A (en) * | 2018-06-08 | 2018-09-14 | 中南大学 | A kind of superhigh temperature ceramics coating of C/C composite materials and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| WEI YANG ET AL.: "Effect of Interface Modified by Graphene on the Mechanical and Frictional Properties of Carbon/Graphene/Carbon Composites", 《MATERIALS》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110803941A (en) * | 2019-11-26 | 2020-02-18 | 航天特种材料及工艺技术研究所 | Carbon-silicon carbide composite material surface oxidation resistant coating and preparation method thereof |
| CN110803941B (en) * | 2019-11-26 | 2022-02-01 | 航天特种材料及工艺技术研究所 | Carbon-silicon carbide composite material surface oxidation resistant coating and preparation method thereof |
| CN113024281A (en) * | 2021-02-28 | 2021-06-25 | 西北工业大学 | Silicon carbide/graphene bionic laminated coating and preparation method thereof |
| CN114773079A (en) * | 2022-05-10 | 2022-07-22 | 吉林联科特种石墨材料有限公司 | Preparation method of hard carbon fiber thermal insulation material with graphene efficient erosion-resistant layer |
| CN114920573A (en) * | 2022-06-06 | 2022-08-19 | 吉林联科特种石墨材料有限公司 | Sintering method for one-step coating process of asphalt-based hard carbon fiber thermal insulation material |
Also Published As
| Publication number | Publication date |
|---|---|
| CN108947557B (en) | 2021-05-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108947557A (en) | A kind of carbon/carbon compound material and preparation method thereof | |
| CN107814591B (en) | Preparation method of boride modified silicon-based antioxidant coating on surface of carbon material | |
| CN102964144B (en) | Method for improving oxidation resistance of surface coating layer of carbon/carbon composite material | |
| CN108530110A (en) | A kind of superhigh temperature ceramics coating of C/C composite materials and preparation method thereof | |
| CN105237039B (en) | The inoxidzable coating material of carbon/carbon brake material and the method for prepares coating | |
| CN108585897B (en) | Refractory metal high-temperature oxidation-resistant Si-Mo-YSZ coating and preparation method thereof | |
| US9259760B2 (en) | Method for coating oxidation protective layer for carbon/carbon composite, carbon heater, and cooker | |
| Zhou et al. | Microstructural evolution of SiC coating on C/C composites exposed to 1500° C in ambient air | |
| Chen et al. | Microstructure and anti-oxidation properties of Yb2Si2O7/SiC bilayer coating for C/SiC composites | |
| CN107032796A (en) | Self-healing SiC/ZrSi2‑MoSi2Coating material and preparation method | |
| CN112341233A (en) | Multi-element single-phase ultra-high temperature ceramic TaxHf1-xPreparation method of C modified carbon/carbon composite material | |
| CN102167623B (en) | Carbon material oxidation resistant coating and preparation method thereof | |
| CN106673710A (en) | HfC nanowire-toughened anti-ablation ceramic coating on surface of carbon/carbon composite material and preparation method | |
| CN113387724B (en) | High-temperature-resistant long-life composite coating on surface of carbon/carbon composite material and preparation method | |
| CN103980006A (en) | Self-healing environmental barrier coating on member surface and preparation method thereof | |
| CN106966699B (en) | Preparation method of high-temperature composite material full-temperature-section heat matching coating | |
| CN104945013B (en) | A kind of C/C composite and the preparation method of surface oxidation-resistant composite coating thereof | |
| CN108620298A (en) | Electrothermal silicon carbide element surface oxidation-resistant coating and preparation method thereof | |
| CN112624801A (en) | Preparation (SiC)NW) Method for modifying C/C composite material (ZrC matrix-coating integration) | |
| CN115894085B (en) | Composite ceramic coating material and preparation method and application thereof | |
| CN103806267A (en) | Method for preparing zirconium carbide ceramic boundary phase on surface of carbon fiber | |
| CN114315424B (en) | Preparation method of high-temperature-resistant coating and application of high-temperature-resistant coating in graphite product | |
| CN111155052A (en) | Er2O3Preparation method and application of coating | |
| CN115536413A (en) | Multilayer core-shell structure nanowire toughening chemical vapor deposition SiC coating and preparation method thereof | |
| CN108504980A (en) | A kind of high temperature resistant anti-ablation composite coating and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |