CN111636144A - Preparation process of carbon-carbon composite material flat plate - Google Patents

Preparation process of carbon-carbon composite material flat plate Download PDF

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CN111636144A
CN111636144A CN202010546992.3A CN202010546992A CN111636144A CN 111636144 A CN111636144 A CN 111636144A CN 202010546992 A CN202010546992 A CN 202010546992A CN 111636144 A CN111636144 A CN 111636144A
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net
net tire
needling
fiber
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曾国伟
甘晶晶
杨德森
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Zhejiang Xinghui New Material Technology Co ltd
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    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-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
    • D04H1/44Non-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
    • D04H1/46Non-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
    • DTEXTILES; PAPER
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    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-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
    • D04H1/44Non-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
    • D04H1/46Non-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
    • D04H1/498Non-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
    • DTEXTILES; PAPER
    • D04BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
    • D04HMAKING 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
    • D04H1/00Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
    • D04H1/40Non-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
    • D04H1/54Non-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 welding together the fibres, e.g. by partially melting or dissolving
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06CFINISHING, DRESSING, TENTERING OR STRETCHING TEXTILE FABRICS
    • D06C7/00Heating or cooling textile fabrics
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    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
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Abstract

The invention discloses a preparation process of a carbon-carbon composite material flat plate, which comprises the steps of short-cutting carbon fiber tows into threads, carding, lapping and needling to form a net body, cutting the net body according to the size of a product, and lapping; weighing a certain weight of chopped fiber bundles by using an electronic scale; then uniformly dispersing the weighed fiber bundles on a flat net tire; then covering a layer of net tire on the surface of the spread tows, introducing Z-direction fibers through a flat needle machine, continuously dispersing carbon fiber tows, covering the net tire, needling, and repeating the process until the product reaches the designed thickness, namely finishing the manufacture of the carbon fiber preform; then soaking resin, carrying out hot-pressing curing molding by a hot press, and carrying out carbonization, densification and high-temperature treatment on the carbon fiber resin plate subjected to hot-pressing curing molding to prepare a carbon-carbon composite material plate; the unit layer of the invention is composed of chopped fibers and a net tire, and then the chopped fibers and the net tire are compounded into a whole through needling.

Description

Preparation process of carbon-carbon composite material flat plate
Technical Field
The invention relates to the field of high-temperature heat treatment, in particular to a preparation process of a carbon-carbon composite material flat plate.
Background
Carbon/carbon composites are carbon matrix composites reinforced with carbon fibers and fabrics thereof. Has a low density of<2.0g/cm3) The material has the advantages of high strength, high specific modulus, high thermal conductivity, low expansion coefficient, good friction performance, good thermal shock resistance, high dimensional stability and the like, is a few of candidate materials applied above 1650 ℃ at present, and has the highest theoretical temperature as high as 2600 ℃, so the material is considered to be one of the high-temperature materials with the greatest development prospect.
The carbon-carbon composite material can be customized into plates, cylinders and various special-shaped structures according to requirements, and the manufacturing methods of materials with different structures are different. Of which flat plate shaped materials are the most used in production. The mainstream production process of the flat carbon-carbon composite material comprises the following steps:
weaving carbon fiber tows into carbon fiber cloth, and uniformly coating or infiltrating phenolic resin on the carbon fiber cloth to prepare carbon fiber prepreg cloth; and then cutting the carbon fiber into required specification and size, laminating to the designed thickness, and performing hot-pressing curing molding through a flat hot press to prepare a prefabricated body of the carbon-carbon composite material. Densifying the prefabricated body by a gas phase method or a liquid phase method to reach the required density, and finally performing high-temperature heat treatment once to finish the production of the 2D structure carbon-carbon composite material;
weaving carbon fiber tows into carbon fiber cloth (warp and weft cloth or non-weft cloth), then chopping and carding the carbon fiber tows into a carbon fiber net tire, alternately layering the net tire and the carbon fiber cloth, introducing Z-direction fibers by adopting a needling mode, and combining unit layers into a whole to prepare a carbon fiber preform; and (3) densifying the prefabricated body by a gas phase method or a liquid phase method to reach the required density, and finally performing high-temperature heat treatment once to finish the production of the 2.5D structure carbon-carbon composite material.
The problems of the two prior arts are as follows:
1. the adhesive force between the carbon fiber cloth unit layers is determined by resin, the adhesive force is poor, and the carbon fiber cloth unit layer is suitable for occasions with low requirements on the shearing strength between layers; the carbon fiber cloth woven by carbon fiber tows needs higher cost, and the carbon fiber cloth prepreg with evenly distributed resin needs higher production equipment requirements, so that the investment is huge.
2. Z-direction fibers are introduced between the unit layers through the net tire and the needling, so that the bonding strength between the layers is greatly enhanced; the carbon fiber tows need to be woven into the carbon fiber cloth, so the process is high in cost. Much very short fibre tow leftover material is also produced during the weaving process.
Disclosure of Invention
The present invention is directed to a carbon-carbon composite flat plate, which solves the above problems.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation process of a carbon-carbon composite flat plate comprises the following steps:
s1, cutting carbon fiber tows (3K,6K,12K,24K and 50K) into short shreds with the length of 30-120mm, and then carding, lapping and needling the shreds into a net blank; the gram weight of the net tire is 40-120g/m2
S2, short-cutting the carbon fiber tows (3K,6K,12K,24K and 50K) into short-cut fiber bundles with the length of 50-180 mm;
s3, selecting the gram weight of the net tire according to the technological requirements of the product, cutting the net tire according to the size of the product, and paving the net tire; weighing a certain weight of chopped fiber bundles by using an electronic scale; then uniformly dispersing the weighed fiber bundles on the flat net tire, wherein the dispersing method can be manual material scattering or mechanical material scattering, namely ensuring that the fiber bundles are uniformly and disorderly dispersed on the surface of the net tire;
s4, covering a layer of net tire on the surface of the spread tow, introducing Z-direction fibers through a flat needle machine, combining the two layers of net tires, and covering fiber bundles in the net tires to form a prefabricated unit layer; the special functional felting needles with barbs on edges are adopted for needling, fibers in the net tire layers are carried to the Z direction by means of the reverse direction barbed needling to generate vertical fiber clusters, so that the adjacent net tire layers are mutually entangled and restrained to form a quasi three-dimensional net structure prefabricated body with certain strength between flat layers, and the defect that the 2D carbon cloth laminated material layers are lack of connection is overcome;
s5, continuously dispersing carbon fiber tows on the unit layers, covering a net tire, needling, and repeating the process until the product reaches the designed thickness, namely, finishing the manufacture of the carbon fiber prefabricated body;
s6, cutting the prefabricated part into a designed size, then infiltrating resin (phenolic resin, furan resin, asphalt and the like), and performing hot-pressing curing molding through a hot press;
and S7, carbonizing, densifying and treating the carbon fiber resin plate subjected to hot-press curing molding at high temperature to prepare the carbon-carbon composite material plate with certain density required by people.
Further, in the step S6, the preform is infiltrated with asphalt; specifically, a container filled with a prefabricated body is placed into a vacuum tank for vacuumizing, and meanwhile, asphalt is placed into a melting tank for vacuumizing and is heated to 250 ℃, so that the asphalt is melted and the strength is reduced; and after the sample container is cooled, transferring the sample container into a pressure impregnation tank, heating to 250 ℃ for pressure infiltration, and further immersing the asphalt into the inner gap of the preform.
A carbon-carbon composite material flat plate prepared by the preparation process of the carbon-carbon composite material flat plate,
the net-shaped tire comprises a net-shaped tire layer, a chopped fiber layer and a carbonized matrix, wherein the net-shaped tire layer is formed by carding, lapping and needling of 30-120mm short-cut carbon fibers, the chopped fiber layer is composed of 50-180mm short-cut fiber bundles, the carbonized matrix is filled in a gap between the net-shaped tire layer and the chopped fiber layer, and the carbonized matrix is formed by carbonizing resin;
further, the carbonized matrix can be formed by carbonizing phenolic resin or furan resin.
Furthermore, the carbonized matrix can also be formed by carbonizing asphalt.
Compared with the prior art, the invention has the beneficial effects that:
the unit layer of the invention is composed of chopped fibers and a net tire, and then the chopped fibers and the net tire are compounded into a whole through needling. Therefore, the weaving process of the carbon fiber cloth is omitted in the whole process, and the cost is reduced; meanwhile, the chopped carbon fiber tows are short in length, some leftover carbon fibers can be utilized, the market purchase price is low, the cost is greatly saved, and the raw material cost and the process cost are greatly reduced through the design of the prefabricated body structure.
Drawings
Fig. 1 is a schematic structural diagram of a carbon-carbon composite flat plate.
Detailed Description
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
A preparation process of a carbon-carbon composite flat plate comprises the following steps:
s1, cutting carbon fiber tows (3K,6K,12K,24K and 50K) into short shreds with the length of 30-120mm, and then carding, lapping and needling the shreds into a net blank; the gram weight of the net tire is 40-120g/m2
S2, short-cutting the carbon fiber tows (3K,6K,12K,24K and 50K) into short-cut fiber bundles with the length of 50-180 mm;
s3, selecting the gram weight of the net tire according to the technological requirements of the product, cutting the net tire according to the size of the product, and paving the net tire; weighing a certain weight of chopped fiber bundles by using an electronic scale (the length of the fiber bundles and the weight of the fiber bundles are determined according to design requirements); then uniformly dispersing the weighed fiber bundles on the flat net tire, wherein the dispersing method can be manual material scattering or mechanical material scattering, namely ensuring that the fiber bundles are uniformly and disorderly dispersed on the surface of the net tire;
s4, covering a layer of net tire on the surface of the spread tow, introducing Z-direction fibers through a flat needle machine, combining the two layers of net tires, and covering fiber bundles in the net tires to form a prefabricated unit layer;
the special functional felting needles with barbs on edges are adopted for needling, fibers in the net tire layers are carried to the Z direction by means of the reverse direction barbed needling to generate vertical fiber clusters, so that the adjacent net tire layers are mutually entangled and restrained to form a quasi three-dimensional net structure prefabricated body with certain strength between flat layers, and the defect that the 2D carbon cloth laminated material layers are lack of connection is overcome;
s5, continuously dispersing carbon fiber tows on the unit layers, covering a net tire, needling, and repeating the process until the product reaches the designed thickness, namely, finishing the manufacture of the carbon fiber prefabricated body;
s6, cutting the prefabricated part into a designed size, then infiltrating resin (phenolic resin, furan resin, asphalt and the like), and performing hot-pressing curing molding through a hot press;
and S7, carbonizing, densifying and treating the carbon fiber resin plate subjected to hot-press curing molding at high temperature to prepare the carbon-carbon composite material plate with certain density required by people.
For example, the asphalt impregnation process usually employs coal pitch or petroleum pitch as an impregnant, and the impregnation is performed by vacuum impregnation and then pressure impregnation.
Specifically, a container filled with a prefabricated body is placed into a vacuum tank for vacuumizing, and meanwhile, asphalt is placed into a melting tank for vacuumizing and is heated to 250 ℃, so that the asphalt is melted and the strength is reduced; then injecting the melted asphalt into a container containing the prefabricated body from a melting tank to enable the asphalt to be immersed in the prefabricated body, after the sample container is cooled, moving the container into a pressure impregnation tank, heating to 250 ℃ to carry out pressure infiltration so as to enable the asphalt to be further immersed in the inner gap of the prefabricated body,
in order to make the carbon/carbon have good microstructure and performance, the growth process of the pitch mesophase is strictly controlled during pitch carbonization, and the growth, combination and growth of mesophase globules are controlled at the mesophase transition temperature (430-.
In the carbonization process, resin is pyrolyzed to form carbon residues, mass loss and size change are caused, and gaps are left in the preform.
The scheme has the following characteristics:
1. the cost is low; the carbon fiber tows are directly chopped, and carbon fiber cloth does not need to be woven, so that the cost of the weaving process is reduced; the carbon fiber tows are short in length, and the leftover materials of some carbon fiber tows generated in the production process can be used, so that the cost is reduced;
2. through reasonable interlayer density design, the carbon fiber tows can be dispersed more uniformly through multiple material scattering and layering;
3. the prepared product has good interlaminar shear strength and the mechanical property of the product reaches 2.5 d.
Referring to fig. 1, the carbon-carbon composite flat plate comprises a mesh layer 100, a chopped fiber layer 200 and a carbonized matrix 300, wherein the mesh layer 100 is formed by carding, lapping and needling chopped carbon fibers with the length of 30-120mm,
the chopped fiber layer 200 is composed of chopped fiber bundles having a length of 50-180mm,
the carbonized matrix 300 is filled in the gap between the net layer 100 and the chopped fiber layer 200, and the carbonized matrix 300 is formed by resin carbonization;
the carbonized substrate 300 may be formed by carbonizing phenolic resin or furan resin.
The carbonized matrix 300 may also be formed by carbonizing pitch.
The detection data of the carbon-carbon composite material flat plate prepared by the scheme are shown in the following table
Watch 1
Figure BDA0002541055710000061
The detection data of the carbon-carbon composite material flat plate prepared by the process 2 in the background art are shown in the following table two
Watch two
Figure BDA0002541055710000062
In conclusion, the tensile strength and the bending strength of the carbon-carbon composite flat plate prepared by the method are similar to those of the carbon-carbon composite flat plate prepared by the process 2 in the background art, and the Young modulus of the carbon-carbon composite flat plate is much higher than that of the carbon-carbon composite flat plate prepared by the process 2.
Although the preferred embodiments of the present patent have been described in detail, the present patent is not limited to the above embodiments, and various changes can be made without departing from the spirit of the present patent within the knowledge of those skilled in the art.

Claims (5)

1. A preparation process of a carbon-carbon composite material flat plate is characterized by comprising the following steps:
s1, short-cutting carbon fiber tows into short shreds with the length of 30-120mm, and then carding, lapping and needling the short shreds into a net blank; the gram weight of the net tire is 40-120g/m2
S2, short-cutting the carbon fiber tows into short fiber bundles with the length of 50-180 mm;
s3, selecting the gram weight of the net tire according to the technological requirements of the product, cutting the net tire according to the size of the product, and paving the net tire; weighing a certain weight of chopped fiber bundles by using an electronic scale; then uniformly dispersing the weighed fiber bundles on the flat net tire, wherein the dispersing method can be manual material scattering or mechanical material scattering, namely ensuring that the fiber bundles are uniformly and disorderly dispersed on the surface of the net tire;
s4, covering a layer of net tire on the surface of the spread tow, introducing Z-direction fibers through a flat needle machine, combining the two layers of net tires, and covering fiber bundles in the net tires to form a prefabricated unit layer; the special functional felting needles with barbs on edges are adopted for needling, fibers in the net tire layers are carried to the Z direction by means of the reverse direction barbed needling to generate vertical fiber clusters, so that the adjacent net tire layers are mutually entangled and restrained to form a quasi three-dimensional net structure prefabricated body with certain strength between flat layers, and the defect that the 2D carbon cloth laminated material layers are lack of connection is overcome;
s5, continuously dispersing carbon fiber tows on the unit layers, covering a net tire, needling, and repeating the process until the product reaches the designed thickness, namely, finishing the manufacture of the carbon fiber prefabricated body;
s6, cutting the prefabricated body into a designed size, then infiltrating resin, and carrying out hot-pressing curing molding through a hot press;
and S7, carbonizing, densifying and treating the carbon fiber resin plate subjected to hot-press curing molding at high temperature to prepare the carbon-carbon composite material plate with a certain density.
2. The process of claim 1, wherein the step S6 is performed by infiltrating the preform with pitch; specifically, a container filled with a prefabricated body is placed into a vacuum tank for vacuumizing, and meanwhile, asphalt is placed into a melting tank for vacuumizing and is heated to 250 ℃ so that the asphalt is melted and the strength is reduced; and after the sample container is cooled, transferring the sample container into a pressure impregnation tank, heating to 250 ℃ for pressure infiltration, and further immersing the asphalt into the inner gap of the preform.
3. The process for preparing a carbon-carbon composite flat plate according to claim 1, wherein the carbon-carbon composite flat plate comprises a net-shaped layer, a chopped fiber layer and a carbonized matrix, the net-shaped layer is formed by carding, lapping and needling 30-120mm long chopped filament carbon fibers, the chopped fiber layer is formed by 50-180mm long chopped fiber bundles, the carbonized matrix is filled in a gap between the net-shaped layer and the chopped fiber layer, and the carbonized matrix is formed by carbonizing resin.
4. The carbon-carbon composite flat plate according to claim 3, wherein the carbonized matrix is formed by carbonizing phenolic resin or furan resin.
5. The carbon-carbon composite flat plate according to claim 3, wherein the carbonized matrix is formed by carbonizing pitch.
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* Cited by examiner, † Cited by third party
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CN112553779A (en) * 2020-12-20 2021-03-26 西安美兰德新材料有限责任公司 Production process of needled carbon crucible support
CN112624779A (en) * 2020-12-26 2021-04-09 凯本(天津)新材料科技有限公司 Preparation method of carbon fiber plate prefabricated body with pure continuous carbon fiber structure
CN113186658A (en) * 2021-05-19 2021-07-30 浙江星辉新材料科技有限公司 Large-size carbon fiber cylinder prefabricated body wood mold
CN113564806A (en) * 2021-08-13 2021-10-29 因达孚先进材料(苏州)有限公司 Preparation method of needle-punched carbon fiber preform
CN114230358A (en) * 2022-01-07 2022-03-25 上海康碳复合材料科技有限公司 Preparation method of carbon-carbon composite material plate with long and short fiber structures simultaneously
CN114634368A (en) * 2022-05-13 2022-06-17 浙江星辉新材料科技有限公司 High-density carbon fiber plate and preparation method thereof
CN114645462A (en) * 2022-03-31 2022-06-21 西安航空制动科技有限公司 High-performance carbon fiber needling preform and preparation method thereof
CN114656272A (en) * 2022-05-23 2022-06-24 浙江星辉新材料科技有限公司 Modified carbon-carbon composite material for H/T type hollow plate and method for preparing H/T type hollow plate
CN115305643A (en) * 2022-07-11 2022-11-08 西安航空制动科技有限公司 Friction material preform and preparation method thereof
CN115353405A (en) * 2022-09-19 2022-11-18 陕西美兰德炭素有限责任公司 Preparation method of high-strength carbon/carbon fastener
CN117604717A (en) * 2023-12-08 2024-02-27 嘉兴睿创新材料有限公司 Large-wall-thickness tubular carbon-carbon composite material preform and cutting method thereof
CN117604717B (en) * 2023-12-08 2024-05-31 嘉兴睿创新材料有限公司 Large-wall-thickness tubular carbon-carbon composite material preform and cutting method thereof

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CN112553779A (en) * 2020-12-20 2021-03-26 西安美兰德新材料有限责任公司 Production process of needled carbon crucible support
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CN113186658A (en) * 2021-05-19 2021-07-30 浙江星辉新材料科技有限公司 Large-size carbon fiber cylinder prefabricated body wood mold
CN113564806A (en) * 2021-08-13 2021-10-29 因达孚先进材料(苏州)有限公司 Preparation method of needle-punched carbon fiber preform
CN114230358A (en) * 2022-01-07 2022-03-25 上海康碳复合材料科技有限公司 Preparation method of carbon-carbon composite material plate with long and short fiber structures simultaneously
CN114645462A (en) * 2022-03-31 2022-06-21 西安航空制动科技有限公司 High-performance carbon fiber needling preform and preparation method thereof
CN114645462B (en) * 2022-03-31 2024-04-09 西安航空制动科技有限公司 High-performance carbon fiber needled preform and preparation method thereof
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CN114656272A (en) * 2022-05-23 2022-06-24 浙江星辉新材料科技有限公司 Modified carbon-carbon composite material for H/T type hollow plate and method for preparing H/T type hollow plate
CN115305643A (en) * 2022-07-11 2022-11-08 西安航空制动科技有限公司 Friction material preform and preparation method thereof
CN115353405A (en) * 2022-09-19 2022-11-18 陕西美兰德炭素有限责任公司 Preparation method of high-strength carbon/carbon fastener
CN117604717A (en) * 2023-12-08 2024-02-27 嘉兴睿创新材料有限公司 Large-wall-thickness tubular carbon-carbon composite material preform and cutting method thereof
CN117604717B (en) * 2023-12-08 2024-05-31 嘉兴睿创新材料有限公司 Large-wall-thickness tubular carbon-carbon composite material preform and cutting method thereof

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