CN113860900A - Rapid preparation method of high-performance carbon fiber composite material plate - Google Patents
Rapid preparation method of high-performance carbon fiber composite material plate Download PDFInfo
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- CN113860900A CN113860900A CN202111266391.8A CN202111266391A CN113860900A CN 113860900 A CN113860900 A CN 113860900A CN 202111266391 A CN202111266391 A CN 202111266391A CN 113860900 A CN113860900 A CN 113860900A
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- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 48
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 46
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 25
- 239000004744 fabric Substances 0.000 claims abstract description 20
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 15
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000005011 phenolic resin Substances 0.000 claims abstract description 14
- 229920001568 phenolic resin Polymers 0.000 claims abstract description 14
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 11
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 238000004080 punching Methods 0.000 claims abstract description 3
- 239000010409 thin film Substances 0.000 claims abstract description 3
- 238000007731 hot pressing Methods 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 6
- 238000007711 solidification Methods 0.000 claims description 4
- 230000008023 solidification Effects 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 3
- 238000007723 die pressing method Methods 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 238000001723 curing Methods 0.000 description 16
- 239000000047 product Substances 0.000 description 14
- 238000003763 carbonization Methods 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000005087 graphitization Methods 0.000 description 5
- 238000003754 machining Methods 0.000 description 4
- 238000005470 impregnation Methods 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005229 chemical vapour deposition Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001721 carbon Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/71—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
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
- C04B35/522—Graphite
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- 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
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
- C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
- C04B2235/6567—Treatment time
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/74—Physical characteristics
- C04B2235/77—Density
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Abstract
The invention relates to the technical field of carbon fiber composite material production, and discloses a rapid preparation method of a high-performance carbon fiber composite material plate, aiming at the problems of long production period, high cost and low efficiency of the carbon fiber composite material plate in the prior art, the following scheme is proposed, which comprises the following steps: s1, performing flat needling on the prefabricated part, cutting three carbon cloths of plain cloth, twill cloth and laid cloth and a net tire into required sizes, alternately stacking and layering, performing needling on a flat needling machine, and performing needling flat prefabricated part with the density of 0.45g/cm through thin film needle punching; and S2, impregnating resin, namely impregnating the flat plate preform needled in the S1 with phenolic resin, wherein a curing agent and graphite powder are added into the phenolic resin. The method can prepare the carbon fiber composite flat plate with high density in a short time, effectively improves the production efficiency, and can flexibly control the thickness of the carbon fiber preform and the ratio of the resin to the graphite powder to prepare the carbon fiber composite flat plate with the corresponding density.
Description
Technical Field
The invention relates to the technical field of carbon fiber composite material production, in particular to a rapid preparation method of a high-performance carbon fiber composite material plate.
Background
Carbon/carbon composites are carbon matrix composites reinforced with carbon fibers and fabrics thereof. The high-strength high-thermal-conductivity high-expansion-coefficient high-friction-performance high-thermal-shock-resistance high-dimensional stability high-performance high-thermal-stability high-performance high-.
The traditional preparation process of the carbon/carbon composite material mainly comprises a chemical vapor deposition process and a liquid phase impregnation process, wherein the chemical vapor deposition process has a good effect on preparing small carbon/carbon composite materials such as crucibles, but for products with thick walls, flat plates and the like, the problems of uneven product density, deformation of the products and the like caused by deposition and densification are solved; the liquid phase impregnation process is more beneficial to products with thick wall size, but has the deformation problem for products of flat plate type; and the two processes have the defects of long production period, high production cost and low efficiency.
Disclosure of Invention
The invention provides a rapid preparation method of a high-performance carbon fiber composite plate, which solves the problems of long production cycle, high cost and low efficiency of the carbon fiber composite plate in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
a rapid preparation method of a high-performance carbon fiber composite plate comprises the following steps:
s1, performing flat needling on the prefabricated part, cutting three carbon cloths of plain cloth, twill cloth and laid cloth and a net tire into required sizes, alternately stacking and layering, performing needling on a flat needling machine, and performing needling flat prefabricated part with the density of 0.45g/cm through thin film needle punching;
s2, impregnating resin, namely impregnating the flat plate preform needled in the S1 with phenolic resin, wherein a curing agent and graphite powder are added into the phenolic resin, and the phenolic resin is fully permeated into the flat plate preform after being uniformly stirred;
s3, performing flat plate die pressing, wrapping the prefabricated body flat plate soaked in the S2 in the tetrafluoro cloth for hot pressing and solidification, and putting a pressing block with corresponding thickness between hot press dies according to the thickness of the required plate;
s4, carbonizing the carbon fiber flat plate solidified in the S3 at the temperature of 600-1000 ℃;
s5, performing high-temperature treatment on the carbonized product in the step S4, wherein the high-temperature treatment temperature is 2000-2500 ℃, and the highest temperature heat preservation time is 2-4 h;
and S6, processing the product subjected to high-temperature treatment in the S5 into a required finished product size according to the requirements of a drawing.
Preferably, the thickness of the prefabricated panel in the step S1 is 2-3 times of the thickness of the required finished panel.
Preferably, in the step S2, the ratio of the resin, the curing agent and the graphite powder is 10:1:1, and the ratio can be adjusted according to a temperature rise process during curing, and the carbon residue rate of the resin is 40% to 60%.
Preferably, the process temperature of the carbon fiber resin board in the step S3 is 100 ℃, the pressure is 10-25MPa, and the process time is 2-3 h.
Preferably, the curing agent is a NL type curing agent.
In the invention:
1. compared with the existing deposition and impregnation carbonization process, the method has the advantages that the high-density carbon fiber composite material flat plate can be prepared in a short time, and the production efficiency is improved well.
2. In the invention S2, resin curing and graphite powder mixing are mentioned, and the preparation method is used for penetrating a preform flat plate, so that the defect of low densification speed caused by low residual carbon rate of the resin is effectively reduced.
3. The method can flexibly control the thickness of the carbon fiber preform and the proportion of the resin and the graphite powder according to the required density of the finished carbon fiber composite flat plate to prepare the carbon fiber composite flat plate with the corresponding density, and the density range of the carbon fiber composite flat plate prepared by the method is 1.0-1.6g/cm for carrying out labor.
4. The invention can also flexibly control the process of carbon fiber preform layering according to the strength required by the finished carbon fiber composite material flat plate, adjust the proportion of the carbon cloth and the net tire according to the strength required by the finished product, and flexibly and effectively provide the preparation process according to the requirement.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Referring to fig. 1, a method for rapidly preparing a high-performance carbon fiber composite material plate includes the following steps:
s1, needling the carbon fiber flat plate preform, cutting three carbon fabrics of plain cloth, twill cloth and weftless cloth and a net tire into required sizes, alternately stacking and laying, needling on a flat needle machine by applying a carbon fiber needling technology to make the needled flat plate preform with the density of 0.45g/cm, wherein the proportion of the carbon cloth layer and the net tire layer can be changed according to the density and strength requirements of a finished product, and finally needling is carried out to obtain the carbon fiber flat plate preform with the required size of the finished product;
s2, impregnating resin, namely impregnating phenolic resin into the flat plate preform needled in the S1, wherein a curing agent and graphite powder are added into the phenolic resin, uniformly stirring the phenolic resin and the graphite powder to fully permeate the flat plate preform, uniformly mixing the phenolic resin with high carbon residue rate, an NL type curing agent and the graphite powder, uniformly stirring the mixture and permeating the mixture into a flat plate of the needled preform, wherein the ratio of the curing agent to the resin can be adjusted according to a heating process, and the general ratio range is 7-12%;
s3, performing flat plate mould pressing, namely hot-pressing solidification, namely, wrapping the impregnated prefabricated body flat plate in the S2 in the tetrafluoro cloth for hot-pressing solidification, and putting a pressing block with corresponding thickness between hot press moulds according to the thickness of the required plate, wherein the hot-pressing temperature is 80-100 ℃, the time is 1-3h, and the pressure is 10-25 MPa;
s4, carbonizing, namely, putting the carbon fiber composite flat plate subjected to hot-pressing curing in the S3 into a carbonization furnace for carbonization, wherein the carbonization process comprises the following steps: the carbonization time is 20-30h, the carbonization temperature is 800-1000 ℃, and the highest temperature is kept for 2-4 h;
s5, high-temperature graphitization, namely placing the carbonized carbon fiber composite material flat plate in a high-temperature furnace for high-temperature graphitization treatment, wherein the treatment process comprises the following steps: the high temperature time is 10-20h, the temperature is 2000-;
and S6, machining, namely machining the carbon fiber composite material subjected to high-temperature graphitization treatment in the S5 according to the size of a finished product to obtain a final high-performance carbon fiber composite material flat plate.
Example 1
Carrying out flat needling on 1500 × 1500mm carbon cloth and a net tire according to a layering ratio of 1:3, finally needling to obtain a 28mm thick carbon fiber preform flat plate, putting the 1500 × 1500 × 28 thick carbon fiber preform flat plate on a hot press platform, weighing 30kg of phenolic resin and 2.4kg of NL type curing agent, repeatedly stirring uniformly, adding 3kg of graphite powder, stirring uniformly, uniformly permeating the prepared solution into the carbon fiber flat plate preform, carrying out hot pressing on the carbon fiber preform flat plate after permeation by using the hot press, increasing the temperature from room temperature to 90 ℃ at 1h, increasing the pressure from normal pressure to 10MPa, increasing the temperature from 90 ℃ to 120 ℃ at 1h, increasing the pressure from 10MPa to 20MPa at constant pressure, keeping the constant pressure for 1h to finish hot pressing and curing, pressing to obtain a 1500 × 1500 × 15mm fibrous composite material flat plate, putting the plate into a nitrogen carbonization furnace for carbonization treatment after curing, increasing the temperature to 950 ℃ under the protection of nitrogen, and keeping the temperature for 4 hours. Placing the carbonized plate into a high-temperature furnace, raising the temperature to 2300 ℃, preserving the heat for 2 hours, carrying out high-temperature graphitization treatment, carrying out high-temperature treatment, carrying out high-density ethanol distillation on the plate, and finally carrying out machining treatment on the graphitized product according to a drawing;
example 2:
carrying out flat needling on 1300 x 1400mm carbon cloth and a mesh tire according to a layering ratio of 1:5, finally needling to obtain a carbon fiber preform flat plate with the thickness of 23mm, putting the carbon fiber preform flat plate with the thickness of 1300 x 1400 x 23 on a hot press platform, weighing 20kg phenolic resin and 2kg NL type curing agent, repeatedly stirring uniformly, adding 1kg graphite powder, stirring uniformly, uniformly permeating the prepared solution into the carbon fiber flat plate preform, carrying out hot pressing on the carbon fiber preform flat plate after permeation by using the hot press, increasing the temperature to 90 ℃ from room temperature for 1h, increasing the pressure to 10MPa from normal pressure, increasing the temperature to 110 ℃ from 1h, increasing the pressure to 20MPa from 10MPa, keeping the constant pressure for 1h, completing hot-pressing and curing, pressing to obtain a 1300 x 1400 x 10mm fibrous composite material flat plate, putting the plate into a carbonization furnace for carbonization treatment after curing, increasing the temperature to 950 ℃ under the protection of nitrogen, and preserving heat for 4 hours, putting the carbonized plate into a high-temperature furnace, heating to 2300 ℃, preserving heat for 2 hours, carrying out high-temperature graphitization treatment, carrying out high-temperature treatment, carrying out density of 1.6g/cm, and finally carrying out machining treatment on the graphitized product according to a drawing.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (5)
1. A rapid preparation method of a high-performance carbon fiber composite plate is characterized by comprising the following steps:
s1, performing flat needling on the prefabricated part, cutting three carbon cloths of plain cloth, twill cloth and laid cloth and a net tire into required sizes, alternately stacking and layering, performing needling on a flat needling machine, and performing needling flat prefabricated part with the density of 0.45g/cm through thin film needle punching;
s2, impregnating resin, namely impregnating the flat plate preform needled in the S1 with phenolic resin, wherein a curing agent and graphite powder are added into the phenolic resin, and the phenolic resin is fully permeated into the flat plate preform after being uniformly stirred;
s3, performing flat plate die pressing, wrapping the prefabricated body flat plate soaked in the S2 in the tetrafluoro cloth for hot pressing and solidification, and putting a pressing block with corresponding thickness between hot press dies according to the thickness of the required plate;
s4, carbonizing the carbon fiber flat plate solidified in the S3 at the temperature of 600-1000 ℃;
s5, performing high-temperature treatment on the carbonized product in the step S4, wherein the high-temperature treatment temperature is 2000-2500 ℃, and the highest temperature heat preservation time is 2-4 h;
and S6, processing the product subjected to high-temperature treatment in the S5 into a required finished product size according to the requirements of a drawing.
2. The method for rapidly manufacturing a high-performance carbon fiber composite board according to claim 1, wherein the thickness of the preform plate in the step S1 is 2-3 times of the thickness of the desired finished plate.
3. The method for rapidly preparing a high-performance carbon fiber composite board according to claim 1, wherein in the step S2, the ratio of the resin, the curing agent and the graphite powder is 10:1:1, and the ratio can be adjusted according to a temperature rise process during curing, and the carbon residue rate of the resin is 40% -60%.
4. The method for rapidly manufacturing a high-performance carbon fiber composite board according to claim 1, wherein the process temperature of the carbon fiber resin board in the step of S3 is 100 ℃, the pressure is 10-25MPa, and the process time is 2-3 h.
5. The method for rapidly manufacturing a high-performance carbon fiber composite board according to claim 1, wherein the curing agent is NL type curing agent.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN115872766A (en) * | 2022-11-14 | 2023-03-31 | 湖南碳谷新材料有限公司 | Preparation method of carbon-carbon material heat preservation device and heat preservation device |
| CN115974572A (en) * | 2022-12-28 | 2023-04-18 | 西安鑫垚陶瓷复合材料股份有限公司 | Low-cost short-period braking material and preparation method thereof |
| CN116178036A (en) * | 2023-02-24 | 2023-05-30 | 陕西美兰德炭素有限责任公司 | Carbon-carbon composite material supporting rod and preparation method thereof |
| CN116375488A (en) * | 2023-02-17 | 2023-07-04 | 贵州省紫安新材料科技有限公司 | Mould pressing manufacturing method of carbon-carbon crucible support |
| CN117623795A (en) * | 2024-01-26 | 2024-03-01 | 浙江星辉新材料科技有限公司 | Carbon-carbon plate and preparation method thereof |
| CN117644698A (en) * | 2023-12-25 | 2024-03-05 | 宜兴市新立织造有限公司 | Heterogeneous structure thermal protection needled composite material and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN115872766A (en) * | 2022-11-14 | 2023-03-31 | 湖南碳谷新材料有限公司 | Preparation method of carbon-carbon material heat preservation device and heat preservation device |
| CN115872766B (en) * | 2022-11-14 | 2024-01-02 | 湖南碳谷新材料有限公司 | Preparation method of carbon-carbon material heat preservation device and heat preservation device |
| CN115974572A (en) * | 2022-12-28 | 2023-04-18 | 西安鑫垚陶瓷复合材料股份有限公司 | Low-cost short-period braking material and preparation method thereof |
| CN115974572B (en) * | 2022-12-28 | 2023-11-17 | 西安鑫垚陶瓷复合材料股份有限公司 | Low-cost short-period braking material and preparation method thereof |
| CN116375488A (en) * | 2023-02-17 | 2023-07-04 | 贵州省紫安新材料科技有限公司 | Mould pressing manufacturing method of carbon-carbon crucible support |
| CN116178036A (en) * | 2023-02-24 | 2023-05-30 | 陕西美兰德炭素有限责任公司 | Carbon-carbon composite material supporting rod and preparation method thereof |
| CN116178036B (en) * | 2023-02-24 | 2024-04-05 | 陕西美兰德新材料股份有限公司 | Carbon-carbon composite material supporting rod and preparation method thereof |
| CN117644698A (en) * | 2023-12-25 | 2024-03-05 | 宜兴市新立织造有限公司 | Heterogeneous structure thermal protection needled composite material and preparation method thereof |
| CN117644698B (en) * | 2023-12-25 | 2024-05-03 | 宜兴市新立织造有限公司 | Heterogeneous structure thermal protection needled composite material and preparation method thereof |
| CN117623795A (en) * | 2024-01-26 | 2024-03-01 | 浙江星辉新材料科技有限公司 | Carbon-carbon plate and preparation method thereof |
| CN117623795B (en) * | 2024-01-26 | 2024-04-12 | 浙江星辉新材料科技有限公司 | Carbon-carbon plate and preparation method thereof |
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Application publication date: 20211231 |