CN111648128A - Quasi-isotropic high-thermal-conductivity C/C composite material and preparation method thereof - Google Patents
Quasi-isotropic high-thermal-conductivity C/C composite material and preparation method thereof Download PDFInfo
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- CN111648128A CN111648128A CN202010612639.0A CN202010612639A CN111648128A CN 111648128 A CN111648128 A CN 111648128A CN 202010612639 A CN202010612639 A CN 202010612639A CN 111648128 A CN111648128 A CN 111648128A
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- 239000002131 composite material Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000000835 fiber Substances 0.000 claims abstract description 39
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 32
- 239000004917 carbon fiber Substances 0.000 claims abstract description 32
- 239000004745 nonwoven fabric Substances 0.000 claims abstract description 32
- 238000003763 carbonization Methods 0.000 claims abstract description 28
- 238000005470 impregnation Methods 0.000 claims abstract description 19
- 239000010426 asphalt Substances 0.000 claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 16
- 238000000576 coating method Methods 0.000 claims abstract description 16
- 238000005087 graphitization Methods 0.000 claims abstract description 16
- 238000000280 densification Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 238000000197 pyrolysis Methods 0.000 claims abstract description 11
- 239000000126 substance Substances 0.000 claims abstract description 10
- 238000003475 lamination Methods 0.000 claims abstract description 8
- 230000003647 oxidation Effects 0.000 claims abstract description 8
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 8
- 230000001681 protective effect Effects 0.000 claims description 16
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 13
- 239000008103 glucose Substances 0.000 claims description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 12
- 230000004048 modification Effects 0.000 claims description 5
- 238000012986 modification Methods 0.000 claims description 5
- 239000004744 fabric Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 29
- 239000000463 material Substances 0.000 abstract description 5
- 230000004888 barrier function Effects 0.000 abstract description 4
- 230000004927 fusion Effects 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 description 60
- 239000007789 gas Substances 0.000 description 25
- 239000000243 solution Substances 0.000 description 18
- 239000011302 mesophase pitch Substances 0.000 description 15
- 238000009987 spinning Methods 0.000 description 12
- 239000007864 aqueous solution Substances 0.000 description 10
- 239000012299 nitrogen atmosphere Substances 0.000 description 9
- 239000011295 pitch Substances 0.000 description 9
- 239000002184 metal Substances 0.000 description 8
- 229910052751 metal Inorganic materials 0.000 description 8
- 239000012298 atmosphere Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 5
- 238000010000 carbonizing Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 239000002296 pyrolytic carbon Substances 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000012300 argon atmosphere Substances 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000008595 infiltration Effects 0.000 description 3
- 238000001764 infiltration Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000011301 petroleum pitch Substances 0.000 description 3
- 238000009941 weaving Methods 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000003208 petroleum Substances 0.000 description 2
- 125000001140 1,4-phenylene group Chemical group [H]C1=C([H])C([*:2])=C([H])C([H])=C1[*:1] 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 239000007770 graphite material Substances 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 230000016507 interphase Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002074 melt spinning Methods 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
Classifications
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/15—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from coal pitch
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/155—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from petroleum pitch
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4209—Inorganic fibres
- D04H1/4242—Carbon fibres
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/44—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling
- D04H1/46—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres
- D04H1/498—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties the fleeces or layers being consolidated by mechanical means, e.g. by rolling by needling or like operations to cause entanglement of fibres entanglement of layered webs
-
- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/58—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives
- D04H1/593—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties by applying, incorporating or activating chemical or thermoplastic bonding agents, e.g. adhesives to layered webs
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06C—FINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
- D06C7/00—Heating or cooling textile fabrics
- D06C7/04—Carbonising or oxidising
-
- G—PHYSICS
- G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
- G21B—FUSION REACTORS
- G21B1/00—Thermonuclear fusion reactors
- G21B1/05—Thermonuclear fusion reactors with magnetic or electric plasma confinement
- G21B1/057—Tokamaks
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/10—Nuclear fusion reactors
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Plasma & Fusion (AREA)
- General Engineering & Computer Science (AREA)
- High Energy & Nuclear Physics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Mechanical Engineering (AREA)
- Inorganic Chemistry (AREA)
- Nonwoven Fabrics (AREA)
- Inorganic Fibers (AREA)
Abstract
The invention relates to the technical field of barrier materials for nuclear fusion, in particular to a quasi-isotropic high-thermal-conductivity C/C composite material and a preparation method thereof. The method comprises the steps of forming a web of asphalt fibers, and then sequentially carrying out pre-oxidation treatment and carbonization treatment to obtain carbon fiber non-woven fabrics; coating a carbon quantum dot modified solution on the carbon fiber non-woven fabric, drying, and performing lamination and needling to obtain a modified carbon fiber non-woven fabric; and sequentially carrying out chemical combination, gas-phase permeation, precursor impregnation pyrolysis densification, carbonization treatment and graphitization treatment on the modified carbon fiber non-woven fabric to obtain the quasi-isotropic high-thermal-conductivity C/C composite material. The quasi-isotropic high-thermal-conductivity C/C composite material prepared by the method not only has a good interface bonding state, but also obviously improves the anisotropic characteristic of the composite material, and has good strength and thermal conductivity.
Description
Technical Field
The invention relates to the technical field of barrier materials for nuclear fusion, in particular to a quasi-isotropic high-thermal-conductivity C/C composite material and a preparation method thereof.
Background
The low-clutter current driving is a main means for realizing the steady-state operation of tokamak internationally at present, and a low-clutter antenna adopts a phased multi-junction waveguide array form. The multi-junction waveguide array antenna is composed of 20 main waveguide units, each main waveguide is divided into 8 active sub-waveguides by a power divider dividing into eight parts, a passive sub-waveguide is inserted between two adjacent main waveguide units, and in order to protect an antenna port from plasma current ignition and high-energy particle bombardment, a protection limiter is arranged at the antenna port. The new generation of limiter barrier material adopts high heat conduction C/C composite material to replace the traditional graphite material, and optimizes the anti-sputtering capability and the heat conduction capability of the barrier material.
The existing high-thermal-conductivity C/C composite material system is generally high in anisotropy, the distribution of fibers and pyrolytic carbon on a welding surface and the direction of thermal conductivity are considered when the high-thermal-conductivity C/C composite material system is welded with copper, and the design and the manufacture of the high-thermal-conductivity C/C composite material system are different from those of a traditional three-dimensional C/C composite material. Meanwhile, the high-thermal-conductivity C/C composite material consists of high-thermal-conductivity mesophase pitch-based carbon fibers and matrix carbon and is a multi-component material system. Because the modulus of the high-thermal-conductivity mesophase pitch-based carbon fiber is far higher than that of PAN-based carbon fiber, the modulus is usually more than 800GPa, the weaving process performance is poor, and the mechanical property and the thermal conductivity of the final composite material are obviously reduced due to the fact that the fiber is easily damaged during the forming of a prefabricated body. Finally, the mesophase pitch-based carbon fiber has large surface inertness, and the interface state with matrixes such as pyrolytic carbon, pitch carbon and the like is different from that of the traditional PAN-based carbon fiber, so that special structure regulation and control are required and the interface structure characteristics in a good combination state are obtained.
Disclosure of Invention
The invention aims to provide a quasi-isotropic high-thermal-conductivity C/C composite material and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a quasi-isotropic high-thermal-conductivity C/C composite material, which comprises the following steps:
1) performing pre-oxidation treatment and carbonization treatment on the asphalt fibers after the asphalt fibers are formed into a net, so as to obtain carbon fiber non-woven fabric;
2) coating a carbon quantum dot modified solution on the carbon fiber non-woven fabric, drying, and performing lamination and needling to obtain a modified carbon fiber non-woven fabric;
3) and sequentially carrying out chemical combination, gas-phase permeation, precursor impregnation pyrolysis densification, carbonization treatment and graphitization treatment on the modified carbon fiber non-woven fabric to obtain the quasi-isotropic high-thermal-conductivity C/C composite material.
Preferably, the pre-oxidation treatment in the step 1) is carried out under the condition that the temperature is raised to 260-300 ℃ at a temperature raising rate of 0.5-1.5 ℃/min.
Preferably, the carbonization treatment in the step 1) is carried out under protective gas at the temperature of 600-1000 ℃ for 10-60 min, and the density of the carbon fiber non-woven fabric surface is 10-40 g/m2。
Preferably, the carbon quantum dot modified solution in the step 2) is prepared by performing a hydrothermal reaction on an aqueous glucose solution, wherein the concentration of the aqueous glucose solution is 0.8-1.6 g/L, the temperature of the hydrothermal reaction is 160-200 ℃, and the time is 12-36 h.
Preferably, the coating amount of the coating in the step 2) is 0.8-1.2L/m2The drying treatment temperature is 80-100 ℃, and the drying treatment time is 1-5 h.
Preferably, the chemical bonding in the step 3) is carried out under a protective gas, the air pressure is a positive pressure condition, the temperature is 400-500 ℃, and the time is 1-2 h; the gas phase permeation is carried out at the pressure of 1-3 kPa, the temperature of 800-1050 ℃ and the time of 100-500 h.
Preferably, the impregnation, pyrolysis and densification of the precursor in the step 3) are carried out under a protective gas, the pressure is 5-10 MPa, the impregnation temperature is 200-280 ℃, and the time is 0.5-1 h.
Preferably, the pressure of the carbonization treatment in the step 3) is 40-100 MPa, the temperature is 800-1000 ℃, and the time is 10-60 min.
Preferably, the graphitization treatment in the step 3) is performed under a protective gas, the air pressure is a positive pressure condition, the temperature is 2500-3000 ℃, and the time is 10-60 min.
The invention also provides the quasi-isotropic high-thermal-conductivity C/C composite material prepared by the preparation method.
The invention has the beneficial effects that:
1) starting from mesophase pitch melt spinning, constructing a planar isotropic fiber network, carbonizing to endow the strength to a preform, performing needling treatment to form a quasi-isotropic fiber preform, enabling the fiber preform to be in a delayed initiation heat conduction state, performing CVI (chemical vapor infiltration) and PIP (poly-p-phenylene) densification, and then performing heat conduction through heat treatment at 2500-3000 ℃, wherein the conventional high-heat-conduction fiber preform is designed in a directional weaving mode, so that the prepared composite material has high anisotropy; and the distribution state of the fibers is difficult to control by means of continuous fiber chopping, net forming and fixing, the steps are complicated and the fibers cannot be organically fused with the densification of the composite material.
2) Aiming at the characteristic of large surface inertia of the mesophase pitch-based carbon fiber, the carbon quantum dots are introduced on the surface of the fiber by spraying a carbon quantum solution, the carbon quantum dots are solidified on the surface of the carbon fiber by combining heat treatment, and then the combination state between the carbon fiber and pyrolytic carbon is improved during chemical vapor infiltration, so that the defect of an interface structure caused by the mismatch of thermal behaviors of the fiber and a matrix in the multi-round heat treatment process of the composite material is greatly reduced. Compared with the C/C composite material without carbon quantum dot modification, the interlayer strength of the two-dimensional C/C composite material is improved from 6-8 MPa to 12-14 MPa.
Detailed Description
The invention provides a preparation method of a quasi-isotropic high-thermal-conductivity C/C composite material, which comprises the following steps:
1) performing pre-oxidation treatment and carbonization treatment on the asphalt fibers after the asphalt fibers are formed into a net, so as to obtain carbon fiber non-woven fabric;
2) coating a carbon quantum dot modified solution on the carbon fiber non-woven fabric, drying, and performing lamination and needling to obtain a modified carbon fiber non-woven fabric;
3) and sequentially carrying out chemical combination, gas-phase permeation, precursor impregnation pyrolysis densification, carbonization treatment and graphitization treatment on the modified carbon fiber non-woven fabric to obtain the quasi-isotropic high-thermal-conductivity C/C composite material.
In the invention, the web formation is preferably carried out by spraying mesophase pitch, pitch fibers are formed into the web under the condition of reciprocating motion in the direction of the metal mesh belt X, Y, and the reciprocating motion speed of the metal mesh belt is preferably 0.5-5 m/min, and more preferably 1-3 m/min.
In the invention, the coal-based or petroleum-based asphalt is preferably sprayed, the softening point of the asphalt is preferably 240-290 ℃, more preferably 250-280 ℃, the content of the mesophase is preferably 80-100%, more preferably 90-95%, the ash content is preferably less than or equal to 200ppm, more preferably less than or equal to 180ppm, and the QI content is preferably 40-60%, more preferably 50-55%.
In the invention, the pressure of the jet spinning is preferably 0.3-5 MPa, more preferably 1-3 MPa, the spinning temperature is preferably 260-310 ℃, more preferably 280-300 ℃, the air knife speed is preferably 5-20 m/s, more preferably 10-15 m/s, and the diameter of the asphalt fiber is preferably 12-20 μm, more preferably 15-18 μm.
In the invention, the atmosphere of the pre-oxidation treatment in the step 1) is air, the temperature of the pre-oxidation treatment is preferably raised to 260-300 ℃ at a heating rate of 0.5-1.5 ℃/min, more preferably raised to 270-280 ℃ at a heating rate of 0.8-1.2 ℃/min, and the temperature is not required to be kept after the temperature is raised.
In the invention, the carbonization treatment in the step 1) is preferably carried out under protective gas, the temperature is preferably 600-1000 ℃, the further preferred is 700-900 ℃, the time is preferably 10-60 min, the further preferred is 30-50 min, and the preferred density of the carbon fiber non-woven fabric surface is 10-40 g/m2More preferably 20 to 30g/m2。
In the invention, the protective gas for carbonization treatment is preferably nitrogen, the heating rate of heating to the carbonization treatment temperature is preferably 5-15 ℃/min, and more preferably 8-12 ℃/min, and the fibers in the carbon fiber non-woven fabric are randomly arranged in a plane.
In the invention, the carbon quantum dot modified solution in the step 2) is preferably prepared by carrying out hydrothermal reaction on an aqueous glucose solution, after the reaction, the aqueous glucose solution is preferably subjected to filtration and centrifugation to obtain an aqueous solution of the carbon quantum dots, the concentration of the aqueous glucose solution is preferably 0.8-1.6 g/L, more preferably 1.0-1.4 g/L, the temperature of the hydrothermal reaction is preferably 160-200 ℃, more preferably 170-190 ℃, the time is preferably 12-36 h, and more preferably 18-24 h.
In the invention, the coating amount of the coating in the step 2) is preferably 0.8-1.2L/m2More preferably 0.9 to 1.1L/m2The temperature of the drying treatment is preferably 80-100 ℃, further preferably 85-90 ℃, and the time is preferably 1-5 hours, further preferably 2-4 hours.
In the invention, the drying treatment is preferably followed by lamination needling, and the fiber volume density of the mesophase pitch-based carbon fiber integral felt is adjusted to be 0.15-0.3 g/cm3The bulk density of the Z-direction fiber is 0.03-0.06 g/cm3Further preferably, the fiber volume density of the mesophase pitch-based carbon fiber integral felt is adjusted to be 0.2-0.25 g/cm3The bulk density of the Z-direction fiber is 0.04-0.05 g/cm3。
In the invention, the chemical bonding in the step 3) is preferably carried out under a protective gas, the gas pressure is preferably a positive pressure condition, the temperature is preferably 400-500 ℃, the time is preferably 420-460 ℃, and the time is preferably 1-2 hours, and the time is preferably 1.5 hours.
In the present invention, the positive pressure refers to a gas state higher than the gas pressure of the normal pressure (i.e., usually, one atmosphere).
In the invention, the chemically combined protective gas is preferably nitrogen, and the heating rate in the process of heating to 400-500 ℃ is preferably 1-5 ℃/min, and more preferably 2-4 ℃/min.
In the invention, the gas phase permeation pressure is preferably 1 to 3kPa, more preferably 2kPa, the temperature is preferably 800 to 1050 ℃, more preferably 850 to 1000 ℃, more preferably 900 to 950 ℃, and the time is preferably 100 to 500 hours, more preferably 200 to 400 hours.
In the invention, the heating rate of the gas phase permeation heating to 800-1050 ℃ is preferably 3-10 ℃/min, and more preferably 5-8 ℃/min.
In the invention, the impregnation, pyrolysis and densification of the precursor in the step 3) are preferably carried out under a protective gas, the protective gas is preferably nitrogen, the pressure is preferably 5-10 MPa, more preferably 6-9 MPa, even more preferably 7-8 MPa, the impregnation temperature is preferably 200-280 ℃, more preferably 220-260 ℃, and the time is preferably 0.5-1 h, even more preferably 0.75 h.
In the invention, the precursor is impregnated with pyrolysis to increase the density, preferably impregnated pitch is used as the precursor, and the density after the increase is preferably>1.75g/cm3Further, it is preferable>1.9g/cm3。
In the present invention, the dipping asphalt is preferably isotropic petroleum asphalt, the softening point of the asphalt is preferably 90 to 140 ℃, more preferably 100 to 120 ℃, the ash content is preferably 200ppm or less, more preferably 180ppm or less, and the QI content is preferably 1% or less, more preferably 0.9% or less.
In the present invention, the heating rate in the process of heating the dipping temperature to 120 ℃ is preferably 1 to 5 ℃/min, more preferably 2 to 4 ℃/min, and the heating rate in the process of heating to the final temperature (200 to 280 ℃) is preferably 0.5 to 1 ℃/min, more preferably 0.6 to 0.8 ℃/min.
In the invention, the pressure of the carbonization treatment in the step 3) is preferably 40-100 MPa, more preferably 50-90 MPa, even more preferably 60-80 MPa, the temperature is preferably 800-1000 ℃, more preferably 850-900 ℃, the time is preferably 10-60 min, even more preferably 20-40 min, and the carbonization treatment is naturally cooled to room temperature.
In the invention, the heating rate in the process of raising the temperature of carbonization treatment to 260 ℃ is preferably 1-5 ℃/min, more preferably 2-4 ℃/min, the heating rate in the process of raising the temperature to 500 ℃ is preferably 0.1-1 ℃/min, more preferably 0.5-0.8 ℃/min, and the heating rate in the process of raising the temperature to the final temperature (800-1000 ℃) is preferably 3-10 ℃/min, more preferably 5-8 ℃/min.
In the invention, the graphitization treatment in the step 3) is preferably performed under a protective gas, the protective gas is preferably argon, the gas pressure is preferably positive pressure, the temperature is preferably 2500-3000 ℃, more preferably 2600-2800 ℃, the time is preferably 10-60 min, more preferably 20-40 min, and the graphitized product is naturally cooled to room temperature after the graphitization treatment.
In the present invention, the temperature increase rate in the temperature increase to 2000 ℃ in the graphitization treatment is preferably 5 to 10 ℃/min, more preferably 6 to 8 ℃/min, and the temperature increase rate in the temperature increase to the final temperature (2500 to 3000 ℃) is preferably 1 to 3 ℃/min, more preferably 2 ℃/min.
The invention also provides the quasi-isotropic high-thermal-conductivity C/C composite material prepared by the preparation method.
In the invention, the thermal conductivity of the quasi-isotropic high thermal conductivity C/C composite material in the direction of X, Y is 260-320W/m.K.
The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
1) In the coal seriesSpraying and spinning the interphase asphalt, wherein the pressure of spraying and spinning is 0.3MPa, the spinning temperature is 260 ℃, the air knife speed is 5m/s, and the diameter of the asphalt fiber is 12 mu m; forming a net by the asphalt fiber under the reciprocating motion condition of the metal mesh belt X, Y, wherein the reciprocating motion speed of the metal mesh belt is 0.5 m/min; then, carrying out preoxidation treatment and carbonization treatment in sequence, wherein the atmosphere of the preoxidation treatment is air, and the temperature is increased to 260 ℃ at the temperature increase rate of 0.5 ℃/min; the carbonization treatment is carried out in the nitrogen atmosphere, the temperature is 600 ℃, the time is 10min, the heating rate of the temperature which is heated to the carbonization treatment temperature is 6 ℃/min, and the density of the carbon fiber non-woven fabric surface is 10g/m2。
2) Coating carbon quantum dot modified solution on carbon fiber non-woven fabric, wherein the coating amount is 0.8L/m2Carrying out hydrothermal reaction preparation on the carbon quantum dot modified solution through a glucose aqueous solution, filtering and centrifuging after reaction to obtain an aqueous solution of the carbon quantum dots, wherein the concentration of the glucose aqueous solution is 0.8g/L, the temperature of the hydrothermal reaction is 160 ℃, and the time is 12 hours; drying at 80 deg.C for 1 hr; carrying out lamination needling to adjust the fiber volume density of the mesophase pitch-based carbon fiber integral felt to be 0.15g/cm3And the bulk density of the Z-direction fiber is 0.03g/cm3Obtaining modified carbon fiber non-woven fabric;
3) chemically combining the modified carbon fiber non-woven fabric in a nitrogen atmosphere, wherein the air pressure is a positive pressure condition, the temperature is 400 ℃, the time is 1h, and the heating rate in the process of heating to 400 ℃ is 2 ℃/min; carrying out gas phase permeation, wherein the gas pressure is 1kPa, the temperature is 800 ℃, the time is 100h, and the heating rate is 3 ℃/min in the process of heating to 800 ℃;
carrying out impregnation pyrolysis densification on the precursor in a nitrogen atmosphere, wherein the impregnation pitch is isotropic petroleum pitch, the impregnation pressure is 5MPa, the temperature is 200 ℃ (the temperature rise rate in the process of heating to 120 ℃ is 1 ℃/min, the temperature rise rate in the process of heating to the final temperature is 0.5 ℃/min), the time is 0.5h, and the densified density>1.75g/cm3；
Carbonizing at 40MPa and 800 deg.C (heating rate of 1 deg.C/min to 260 deg.C, heating rate of 0.1 deg.C/min to 500 deg.C, and heating rate of 3 deg.C/min to final temperature) for 10 min; and (2) carrying out graphitization treatment under the argon atmosphere, wherein the air pressure is a positive pressure condition, the temperature is 2500 ℃ (the heating rate in the process of heating to 2000 ℃ is 5 ℃/min, the heating rate in the process of heating to the final temperature is 1 ℃/min), the time is 10min, and cooling to the room temperature after the graphitization treatment is finished to obtain the quasi-isotropic high-thermal-conductivity C/C composite material.
Example 2
1) Carrying out jet spinning by using coal-series or petroleum-series mesophase pitch, wherein the jet spinning pressure is 2MPa, the spinning temperature is 280 ℃, the air knife speed is 10m/s, and the diameter of pitch fiber is 15 mu m; forming a net by the asphalt fiber under the reciprocating motion condition of the metal mesh belt X, Y, wherein the reciprocating motion speed of the metal mesh belt is 3 m/min; then, carrying out preoxidation treatment and carbonization treatment in sequence, wherein the atmosphere of the preoxidation treatment is air, and the temperature is increased to 280 ℃ at the temperature increase rate of 0.8 ℃/min; the carbonization treatment is carried out in the nitrogen atmosphere, the temperature is 800 ℃, the time is 30min, the heating rate of the temperature to the carbonization treatment temperature is 10 ℃/min, and the density of the carbon fiber non-woven fabric surface is 20g/m2。
2) Coating carbon quantum dot modified solution on carbon fiber non-woven fabric with the coating amount of 1.0L/m2Carrying out hydrothermal reaction preparation on the carbon quantum dot modified solution through a glucose aqueous solution, filtering and centrifuging after reaction to obtain an aqueous solution of the carbon quantum dots, wherein the concentration of the glucose aqueous solution is 1.2g/L, the temperature of the hydrothermal reaction is 180 ℃, and the time is 24 hours; drying at 90 deg.C for 3 hr; carrying out lamination needling to adjust the fiber volume density of the mesophase pitch-based carbon fiber integral felt to be 0.2g/cm3And the bulk density of the Z-direction fiber is 0.04g/cm3Obtaining modified carbon fiber non-woven fabric;
3) chemically combining the modified carbon fiber non-woven fabric in a nitrogen atmosphere, wherein the air pressure is a positive pressure condition, the temperature is 450 ℃, the time is 1.5h, and the heating rate in the process of heating to 450 ℃ is 2 ℃/min; carrying out gas phase permeation, wherein the gas pressure is 2kPa, the temperature is 900 ℃, the time is 300h, and the heating rate is 5 ℃/min in the process of heating to 900 ℃;
carrying out impregnation pyrolysis densification on the precursor in a nitrogen atmosphere, wherein the impregnation pitch is isotropic petroleum pitch, the impregnation pressure is 8MPa, the temperature is 260 ℃ (the temperature rise rate in the process of heating to 120 ℃ is 3 ℃/min, the temperature rise rate in the process of heating to the final temperature is 0.8 ℃/min), the time is 0.6h, and the densified density>1.75g/cm3；
Carbonizing at 60MPa and 900 deg.C (2 deg.C/min for heating to 260 deg.C, 0.5 deg.C/min for heating to 500 deg.C, and 5 deg.C/min for 30 min; and (2) carrying out graphitization treatment under the argon atmosphere, wherein the air pressure is a positive pressure condition, the temperature is 2800 ℃ (the heating rate in the process of heating to 2000 ℃ is 7 ℃/min, the heating rate in the process of heating to the final temperature is 2 ℃/min), the time is 30min, and after the graphitization treatment is finished, cooling to the room temperature to obtain the quasi-isotropic high-thermal-conductivity C/C composite material.
Example 3
1) Carrying out jet spinning by using coal-series or petroleum-series mesophase pitch, wherein the jet spinning pressure is 5MPa, the spinning temperature is 310 ℃, the air knife speed is 20m/s, and the diameter of pitch fiber is 20 mu m; forming a net by the asphalt fiber under the reciprocating motion condition of the metal mesh belt X, Y, wherein the reciprocating motion speed of the metal mesh belt is 5 m/min; then, carrying out preoxidation treatment and carbonization treatment in sequence, wherein the atmosphere of the preoxidation treatment is air, and the temperature is increased to 300 ℃ at the temperature increase rate of 1.5 ℃/min; the carbonization treatment is carried out in the nitrogen atmosphere, the temperature is 1000 ℃, the time is 60min, the heating rate of the temperature which is heated to the carbonization treatment temperature is 15 ℃/min, and the density of the carbon fiber non-woven fabric surface is 40g/m2。
2) Coating carbon quantum dot modified solution on carbon fiber non-woven fabric with the coating amount of 1.2L/m2Carrying out hydrothermal reaction preparation on the carbon quantum dot modified solution through a glucose aqueous solution, filtering and centrifuging after reaction to obtain an aqueous solution of the carbon quantum dots, wherein the concentration of the glucose aqueous solution is 1.6g/L, the temperature of the hydrothermal reaction is 200 ℃, and the time is 36 h; drying at 100 deg.C for 5 hr; carrying out lamination needling to adjust the mesophase pitch-based carbon fiber wholeThe fiber bulk density of the felt was 0.3g/cm3And the bulk density of the Z-direction fiber is 0.06g/cm3Obtaining modified carbon fiber non-woven fabric;
3) chemically combining the modified carbon fiber non-woven fabric in a nitrogen atmosphere, wherein the air pressure is a positive pressure condition, the temperature is 500 ℃, the time is 2 hours, and the heating rate in the process of heating to 500 ℃ is 5 ℃/min; carrying out gas phase permeation, wherein the gas pressure is 3kPa, the temperature is 1050 ℃, the time is 500h, and the heating rate is 10 ℃/min in the process of heating to 1050 ℃;
carrying out impregnation pyrolysis densification on the precursor in a nitrogen atmosphere, wherein the impregnation pitch is isotropic petroleum pitch, the impregnation pressure is 10MPa, the temperature is 280 ℃ (the temperature rise rate in the process of heating to 120 ℃ is 5 ℃/min, the temperature rise rate in the process of heating to final temperature is 1 ℃/min), the time is 1h, and the densified density>1.75g/cm3；
Carbonizing at 100MPa and 1000 deg.C (heating rate of 5 deg.C/min to 260 deg.C, heating rate of 1 deg.C/min to 500 deg.C, and heating rate of 10 deg.C/min to final temperature) for 60 min; and (2) carrying out graphitization treatment under the argon atmosphere, wherein the air pressure is a positive pressure condition, the temperature is 3000 ℃ (the heating rate in the process of heating to 2000 ℃ is 10 ℃/min, the heating rate in the process of heating to the final temperature is 3 ℃/min), the time is 60min, and cooling to the room temperature after the graphitization treatment is finished to obtain the quasi-isotropic high-heat-conductivity C/C composite material.
The strength and the heat-conducting property of the quasi-isotropic high-heat-conductivity C/C composite material obtained in the examples 1 to 3 are verified, and specific results are shown in Table 1.
TABLE 1 Properties of quasi-isotropic highly thermally conductive C/C composites
The conventional high-thermal-conductivity fiber preform is designed in a directional weaving mode, the prepared composite material has high anisotropy, the strength of the composite material in the directions of 0 degrees and 90 degrees is the highest, 180MPa, the thermal conductivity is 350W/m.K, the strength in the direction of 45 degrees is only 65MPa, the thermal conductivity is 210W/m.K, the mechanical property of the composite material is an obvious mechanical short plate, and the uniformity of the thermal conductivity is poor. The strength of the quasi-isotropic high-thermal-conductivity C/C composite material prepared by the invention in all directions of a plane is basically about 152MPa, the thermal conductivity is 280W/m.K, and the anisotropic characteristic of the composite material is obviously improved.
According to the embodiments, the quasi-isotropic high thermal conductivity C/C composite material and the preparation method thereof are provided, the method aims at the characteristics of high anisotropy, poor interface bonding state and the like of the high thermal conductivity C/C composite material, a quasi-isotropic fiber preform is constructed in the melting and spraying spinning process of mesophase pitch, surface modification and needling treatment of carbon quantum dots are performed after carbonization, then the interface bonding state between mesophase pitch-based carbon fiber and pyrolytic carbon is regulated and controlled through heat treatment and chemical vapor infiltration, and ultrahigh temperature graphitization treatment is performed after continuous densification of pitch to obtain the quasi-isotropic high thermal conductivity C/C composite material.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a quasi-isotropic high-thermal-conductivity C/C composite material is characterized by comprising the following steps:
1) performing pre-oxidation treatment and carbonization treatment on the asphalt fibers after the asphalt fibers are formed into a net, so as to obtain carbon fiber non-woven fabric;
2) coating a carbon quantum dot modified solution on the carbon fiber non-woven fabric, drying, and performing lamination and needling to obtain a modified carbon fiber non-woven fabric;
3) and sequentially carrying out chemical combination, gas-phase permeation, precursor impregnation pyrolysis densification, carbonization treatment and graphitization treatment on the modified carbon fiber non-woven fabric to obtain the quasi-isotropic high-thermal-conductivity C/C composite material.
2. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material as claimed in claim 1, wherein the pre-oxidation treatment in step 1) is performed under a temperature rise rate of 0.5-1.5 ℃/min to 260-300 ℃.
3. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material according to claim 1 or 2, wherein the carbonization treatment in the step 1) is performed under a protective gas at a temperature of 600-1000 ℃ for 10-60 min, and the cloth cover density of the carbon fiber non-woven fabric is 10-40 g/m2。
4. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material according to claim 1, wherein the carbon quantum dot modification solution in the step 2) is prepared by performing a hydrothermal reaction on an aqueous glucose solution, the concentration of the aqueous glucose solution is 0.8-1.6 g/L, the temperature of the hydrothermal reaction is 160-200 ℃, and the time is 12-36 hours.
5. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material as claimed in claim 1 or 4, wherein the coating amount of the coating in the step 2) is 0.8-1.2L/m2The drying treatment temperature is 80-100 ℃, and the drying treatment time is 1-5 h.
6. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material according to claim 1, wherein the chemical bonding in the step 3) is performed under a protective gas, the gas pressure is a positive pressure condition, the temperature is 400-500 ℃, and the time is 1-2 h; the gas phase permeation is carried out at the pressure of 1-3 kPa, the temperature of 800-1050 ℃ and the time of 100-500 h.
7. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material according to claim 1 or 6, wherein the impregnation, pyrolysis and densification of the precursor in the step 3) are performed under a protective gas, the pressure is 5-10 MPa, the impregnation temperature is 200-280 ℃, and the time is 0.5-1 h.
8. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material according to claim 1 or 6, wherein the pressure of the carbonization treatment in the step 3) is 40-100 MPa, the temperature is 800-1000 ℃, and the time is 10-60 min.
9. The preparation method of the quasi-isotropic high thermal conductivity C/C composite material according to claim 1 or 6, wherein the graphitization treatment in the step 3) is performed under a protective gas, the pressure is positive pressure, the temperature is 2500-3000 ℃, and the time is 10-60 min.
10. The quasi-isotropic high thermal conductive C/C composite material prepared by the preparation method of the quasi-isotropic high thermal conductive C/C composite material according to any one of claims 1 to 9.
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