CN116082052A - Graphene-based carbon/carbon composite material and precursor thereof - Google Patents
Graphene-based carbon/carbon composite material and precursor thereof Download PDFInfo
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- CN116082052A CN116082052A CN202211731633.0A CN202211731633A CN116082052A CN 116082052 A CN116082052 A CN 116082052A CN 202211731633 A CN202211731633 A CN 202211731633A CN 116082052 A CN116082052 A CN 116082052A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 198
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 110
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 97
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 239000002243 precursor Substances 0.000 title claims abstract description 28
- 239000011347 resin Substances 0.000 claims abstract description 46
- 229920005989 resin Polymers 0.000 claims abstract description 46
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 38
- 239000004917 carbon fiber Substances 0.000 claims abstract description 38
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000004744 fabric Substances 0.000 claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 5
- 239000001301 oxygen Substances 0.000 claims abstract description 5
- 238000010000 carbonizing Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 2
- 229910021397 glassy carbon Inorganic materials 0.000 claims description 2
- 238000007598 dipping method Methods 0.000 claims 1
- 238000005087 graphitization Methods 0.000 abstract description 17
- 238000003763 carbonization Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 8
- 230000008569 process Effects 0.000 abstract description 8
- 239000011521 glass Substances 0.000 abstract description 4
- 239000010410 layer Substances 0.000 description 31
- 239000011159 matrix material Substances 0.000 description 11
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000010586 diagram Methods 0.000 description 7
- 239000000017 hydrogel Substances 0.000 description 7
- 238000002360 preparation method Methods 0.000 description 5
- 239000000126 substance Substances 0.000 description 4
- 239000011203 carbon fibre reinforced carbon Substances 0.000 description 3
- 238000000465 moulding Methods 0.000 description 3
- 238000005457 optimization Methods 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 230000001680 brushing effect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- 229910021385 hard carbon Inorganic materials 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 239000013081 microcrystal Substances 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 239000011295 pitch Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
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- 238000011282 treatment Methods 0.000 description 2
- 239000004593 Epoxy Chemical group 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000012790 adhesive layer Substances 0.000 description 1
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- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 239000011304 carbon pitch Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 239000000805 composite resin Substances 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- XLJMAIOERFSOGZ-UHFFFAOYSA-M cyanate Chemical compound [O-]C#N XLJMAIOERFSOGZ-UHFFFAOYSA-M 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
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- 239000002861 polymer material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000002296 pyrolytic carbon Substances 0.000 description 1
- 238000011946 reduction process Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—Ceramic products containing macroscopic reinforcing agents
- C04B35/78—Ceramic products containing macroscopic reinforcing agents containing non-metallic materials
- C04B35/80—Fibres, filaments, whiskers, platelets, or the like
- C04B35/83—Carbon fibres in a carbon matrix
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
- C04B2235/422—Carbon
- C04B2235/425—Graphite
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/48—Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
- C04B2235/52—Constituents or additives characterised by their shapes
- C04B2235/5208—Fibers
- C04B2235/5252—Fibers having a specific pre-form
- C04B2235/5256—Two-dimensional, e.g. woven structures
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- 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
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a graphene-based carbon/carbon composite material and a precursor thereof. The precursor comprises a plurality of carbon fiber fabric layers which are arranged in a stacked mode, wherein the carbon fiber fabric layers are filled with resin and graphene, a graphene bonding layer is arranged between adjacent carbon fiber fabric layers, and the oxygen content of the graphene is 0% -50%. The carbon fiber fabric layer of the precursor is filled with resin and graphene base materials, so that the enhancement in the carbon fiber fabric layer is realized, and the graphitization degree of the glass carbon formed by resin carbonization of the composite material precursor in the carbonization and graphitization processes is improved due to the existence of graphene, so that the carbon/carbon composite material based on graphene with optimized performance is obtained.
Description
Technical Field
The invention belongs to the technical field of carbon/carbon composite materials, and particularly relates to a graphene-based carbon/carbon composite material and a precursor thereof.
Background
The carbon/carbon composite material is a composite material prepared by taking pyrolytic carbon as a matrix and taking carbon fiber as a reinforcing material, has the advantages of low density, high heat conduction, ultra-high temperature mechanical property, small thermal expansion coefficient, small friction coefficient, flexible structural designability and the like, is an important thermal structural material in the aerospace field, gradually extends to the fields of mechanical braking, biomedical and the like, and has very wide application space in the industrial fields of semiconductors, chemical industry, metallurgy, atomic energy and the like.
The formation of matrix carbon in carbon/carbon composites is largely accomplished in two ways: (1) Asphalt or resin is used as a precursor and carbonized at high temperature to form the asphalt or resin. (2) The carbon source gas is deposited on the surface of the preform by controlling the temperature and the pressure. The preparation of the carbon/carbon composite material by using pitch or resin as a precursor requires the preparation of a carbon fiber/pitch-based or carbon fiber/resin-based reinforcement, followed by carbonization at high temperature to convert the pitch phase or resin phase into a carbon matrix, thereby obtaining the carbon fiber-reinforced carbon (carbon/carbon) composite material. And then, the densification of the composite material is realized through repeated impregnation and carbonization treatments. Finally, the carbon/carbon composite material with the density reaching the standard is obtained through high-temperature graphitization treatment.
The basic structure of the carbon/carbon composite material is mostly a disordered graphite structure or a transition structure between the disordered graphite structure and a graphite crystal structure. Under the action of heat treatment, the interplanar spacing of carbon is reduced, the size of graphite microcrystals is increased, and the process of converting the disordered graphite structure into the polycrystalline graphite structure is called graphitization. Graphitization can influence the material performance, the deepening of graphitization degree can obviously strengthen the fracture toughness and the heat conductivity of the composite material, however, the glass carbon formed by resin pyrolysis is an amorphous carbon material (hard carbon) formed by disordered arrangement of carbon microcrystals, the microcrystalline structure of the glass carbon is not arranged according to a certain direction, and long ribbon-shaped laminates on the carbon layer surface form disordered network structures, so that graphitization is difficult, and further the thermophysical performance, mechanical performance, frictional wear performance and the like of the carbon/carbon composite material are directly influenced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provides a graphene-based carbon/carbon composite material and a precursor thereof, and aims to improve the overall graphitization degree of the carbon/carbon composite material by constructing a specific material layer structure and utilizing a high graphitization structure of graphene, induce the graphitization degree of matrix carbon to be improved, solve the problem of low graphitization degree of the carbon/carbon composite material prepared by a resin precursor method and realize the performance optimization of the composite material.
One of the technical schemes adopted for solving the technical problems is as follows: the carbon/carbon composite material precursor based on the graphene comprises a plurality of carbon fiber fabric layers which are stacked, wherein the carbon fiber fabric layers are filled with resin and graphene, a graphene bonding layer is arranged between adjacent carbon fiber fabric layers, and the oxygen content of graphene in the graphene bonding layer is 0% -50%.
In a preferred embodiment of the present invention, the carbon fiber fabric layer is impregnated with a mixed solution of graphene and resin to achieve the internal filling of the resin and graphene.
In a preferred embodiment of the present invention, the mass ratio of graphene to resin in the mixed solution of graphene and resin is 5%.
In a preferred embodiment of the present invention, the resin content of the carbon fiber fabric layer is 40-50%.
In a preferred embodiment of the present invention, the resin includes, but is not limited to, phenolic resin, cyanate resin.
In a preferred embodiment of the present invention, the graphene in the graphene bonding layer and the graphene filled in the carbon fiber fabric layer include graphene, graphene oxide or reduced graphene oxide.
In a preferred embodiment of the present invention, the number of layers of the graphene bonding layer is 1-20.
In a preferred embodiment of the present invention, the carbon fiber fabric layer and the graphene adhesive layer are laminated and compounded by a molding process, including compression molding, vacuum bagging, lamination, autoclave, or other molding processes.
The second technical scheme adopted by the invention for solving the technical problems is as follows: the carbon/carbon composite material based on the graphene is prepared by carbonizing and graphitizing a precursor of the carbon/carbon composite material based on the graphene.
In a preferred embodiment of the present invention, the graphene-based carbon/carbon composite precursor is carbonized, repeatedly immersed in a mixed solution of graphene and resin, cured and carbonized to form glassy carbon with the resin to fill the internal voids, and graphitized.
Compared with the background technology, the technical proposal has the following advantages:
1. graphene is a two-dimensional single-layer carbon material, has a thickness of only one atom, and has high structural regularity, and is equivalent to a two-dimensional high polymer material with very high graphitization degree. Graphene oxide is an oxide of graphene, and the surface of the graphene oxide contains abundant active groups such as hydroxyl, carboxyl, epoxy, carbonyl and the like, so that the graphene oxide can be well dispersed in solvents such as water, acetone, ethanol and the like. Graphene oxide is subjected to certain chemical or physical conditions, wherein oxygen-containing groups can be partially reduced into reduced graphene oxide (the structural schematic diagrams of several graphene-based materials are shown in figure 1); according to the invention, by constructing a specific material layer structure and utilizing a graphitized structure with regular graphene height, the integral graphitization degree of the carbon/carbon composite material is improved;
2. compared with graphene and reduced graphene oxide, the graphene oxide has better compatibility with a resin matrix due to the fact that a large number of oxygen-containing groups are contained in the structure of the graphene oxide, and can generate better chemical bonding and physical effects with the resin matrix. Through the high-temperature thermal reduction process, the graphene oxide can be changed into reduced graphene oxide, and has a regular structure and physical properties which are closer to those of graphene, so that the graphene oxide-resin system can be changed into a reduced graphene oxide-resin (graphene-resin) system through corresponding chemical or physical means. According to the invention, the graphitization degree of the matrix carbon is improved by graphene induction, so that the performance optimization of the carbon/carbon composite material is realized.
Drawings
Fig. 1 is a schematic structural diagram of several graphene-based materials, (a) graphene, (b) graphene oxide, (c) reduced graphene oxide, and (d) graphene oxide hydrogel film.
Fig. 2 is a schematic diagram of a composite precursor structure (a) and a schematic diagram of a molding structure (b), and a schematic diagram of a general carbon/carbon composite structure (c) in the embodiment.
Fig. 3 is an SEM photograph of the internal micro morphology of the composite material, (a) carbon fiber/carbon composite material, (b) graphene/carbon fiber/carbon composite material.
FIG. 4 is an SEM photograph of the internal microstructure of a composite material of example after multiple carbonization, (a) 1 time (b) 3 times (c) 5 times (d) 7 times (d) carbonization.
Fig. 5 is an SEM photograph of (a) XRD profile and (b) microscopic morphology of the composite material of the example.
Fig. 6 is a comparison of (a) electrical conductivity and (b) thermal conductivity of the example with a conventional carbon fiber/resin composite.
Fig. 7 is a schematic diagram of the preparation process of the example.
Detailed Description
Examples
The precursor of the graphene-based carbon/carbon composite material comprises a plurality of carbon fiber fabric layers which are stacked, wherein the carbon fiber fabric layers are filled with resin and graphene oxide, a graphene bonding layer is arranged between adjacent carbon fiber fabric layers, the graphene bonding layer is prepared from graphene oxide hydrogel, and the resin is phenolic resin.
The number of layers of the graphene bonding layer is 3, and the thickness of a single graphene bonding layer is 1mm.
The preparation method of the carbon/carbon composite material by adopting the precursor of the carbon/carbon composite material based on graphene comprises the following steps:
(1) Preparing graphene oxide-acetone solution and resin-acetone solution respectively, and uniformly mixing the graphene oxide-acetone solution and the resin-acetone solution to obtain graphene oxide-resin-acetone solution; the ratio of graphene oxide to resin was controlled to be 5%.
(2) Immersing a single-layer carbon fiber fabric in graphene oxide-resin-acetone solution, airing at room temperature, and drying the solvent; preparing a carbon fiber-graphene oxide-resin prepreg sheet according to a general fiber prepreg process; the resin content in the prepreg was controlled to 45%.
(3) Preparing graphene oxide hydrogel with mass concentration of 2%; brushing graphene oxide hydrogel on the carbon fiber-graphene oxide-resin prepreg sheet prepared in the step (2), and carrying out multi-layer bonding and drying on the carbon fiber-graphene oxide-resin prepreg sheet coated with the graphene oxide hydrogel.
(4) And (3) brushing the carbon fiber-graphene oxide-resin prepreg sheet coated with the graphene oxide hydrogel in the step (3), and adopting a corresponding forming process of a general fiber resin matrix composite material, such as mould pressing, vacuum bagging, lamination, autoclave and the like, to form, thereby obtaining the graphene oxide/carbon fiber/resin matrix composite material.
(5) And (3) carbonizing the graphene oxide/carbon fiber/resin matrix composite material by adopting a preparation process of a general resin precursor carbon/carbon composite material, then soaking and carbonizing the graphene oxide/carbon fiber/resin matrix composite material in the graphene oxide-resin-acetone solution in the step (1), and obtaining the graphene-based carbon/carbon composite material through graphitization after repeated soaking and carbonizing for a plurality of times.
According to the carbon/carbon composite material structure based on graphene, graphene-based material hydrogel is used as a bonding layer to bond carbon fiber fabrics, so that carbon fiber fabric layers in a precursor of the composite material are formed by graphene substrate layers, a structure formed by resin among carbon fiber fabric layers in a traditional carbon/carbon composite material precursor is replaced, the effect of enhancing the graphene structure among the composite material precursor layers is achieved, a structural comparison schematic diagram is shown in fig. 2, and the internal microscopic morphology of the graphene/carbon fiber/carbon composite material formed through repeated impregnation and carbonization processes is shown in fig. 3 and fig. 4. The carbon fiber fabric layer in the carbon/carbon composite material precursor structure is filled with resin and graphene, so that not only is the enhancement in the carbon fiber fabric layer realized, but also the graphitization degree of glass carbon (hard carbon) formed by resin carbonization of the composite material precursor in carbonization and graphitization processes is improved due to the existence of the graphene (figure 5), and the performance optimization of the carbon/carbon composite material is realized (figure 6).
The above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (5)
1. A graphene-based carbon/carbon composite precursor, characterized in that: the carbon fiber fabric comprises a plurality of carbon fiber fabric layers which are stacked, wherein the carbon fiber fabric layers are filled with resin and graphene, a graphene bonding layer is arranged between every two adjacent carbon fiber fabric layers, and the oxygen content of graphene in the carbon fiber fabric layers and the graphene bonding layers is 0% -50%.
2. A graphene-based carbon/carbon composite precursor according to claim 1, wherein: the carbon fiber fabric layer is impregnated in a mixed solution of graphene and resin to realize the internal filling of the resin and the graphene.
3. A graphene-based carbon/carbon composite precursor according to claim 1, wherein: the graphene in the graphene bonding layer and the graphene filled in the carbon fiber fabric layer comprise graphene, graphene oxide or reduced graphene oxide.
4. A graphene-based carbon/carbon composite material, characterized in that: a graphene-based carbon/carbon composite precursor according to any one of claims 1 to 3, which is carbonized and graphitized.
5. The graphene-based carbon/carbon composite material according to claim 4, wherein: repeatedly dipping a graphene-based carbon/carbon composite material precursor into a mixed solution of graphene and resin, carbonizing to enable glassy carbon formed by the resin to fill an internal gap, and graphitizing.
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