CN116330757A - High-strength laminated carbon-carbon composite material and preparation method thereof - Google Patents
High-strength laminated carbon-carbon composite material and preparation method thereof Download PDFInfo
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Images
Classifications
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- B32B5/00—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/028—Net structure, e.g. spaced apart filaments bonded at the crossing points
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B32B37/10—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the pressing technique, e.g. using action of vacuum or fluid pressure
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- B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
- B32B5/12—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer characterised by the relative arrangement of fibres or filaments of different layers, e.g. the fibres or filaments being parallel or perpendicular to each other
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- B32B5/22—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by the presence of two or more layers which are next to each other and are fibrous, filamentary, formed of particles or foamed
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- B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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Abstract
The invention discloses a high-strength laminated carbon-carbon composite material and a preparation method thereof. The carbon-carbon composite material comprises a carbon fiber unidirectional cloth layer and a carbon fiber net tire layer, wherein the carbon fiber unidirectional cloth in the carbon fiber unidirectional cloth layer is paved in a staggered way by 90 degrees, the carbon fiber net tire is added between the layers, and the carbon fiber unidirectional cloth is integrally needled and formed. Firstly, drawing and paving carbon fiber filaments to prepare carbon fiber unidirectional cloth; chopping carbon fiber filaments, and performing needling to prepare a carbon fiber net tyre; then, the carbon fiber unidirectional cloth is staggered and paved according to 90 degrees, a carbon fiber net tire is added between the layers, and the carbon fiber unidirectional cloth is integrally needled to prepare a carbon fiber preform; finally, the carbon fiber preform is impregnated with resin, and then is cured under high temperature and pressure, and then carbonized and graphitized to prepare the carbon-carbon composite material. The carbon-carbon composite material has the advantages of the net-tire needle-punched laminated carbon-carbon composite material and the carbon cloth-type laminated carbon-carbon composite material, overcomes the defects of the net-tire needle-punched laminated carbon-carbon composite material and the carbon cloth-type laminated carbon-carbon composite material, and has higher cost performance and usability.
Description
Technical Field
The invention relates to the technical field of carbon-carbon composite materials, in particular to a high-strength laminated carbon-carbon composite material and a preparation method thereof.
Background
The existing laminated carbon-carbon composite materials in the market at present mainly have two main types: the first type is a net tire needling type laminated carbon-carbon composite material, which is characterized in that carbon fiber filaments are chopped, a carbon fiber net tire is manufactured through needling, then the net tire is laid layer by layer, part of carbon fiber unidirectional cloth or carbon fiber bidirectional cloth can be laid when the net tire is laid for strength enhancement, and then the carbon fiber prefabricated body is manufactured through integral needling. Impregnating the needled carbon fiber preform such as: phenolic aldehyde, furan, epoxy and other resins, laminating and curing the resins, and then carbonizing and graphitizing to prepare the net tyre needling type laminated carbon-carbon composite material; the other type is a carbon cloth type laminated carbon-carbon composite material, which is prepared by laminating carbon fiber unidirectional cloth layer by layer after resin treatment, laminating and solidifying, and then carbonizing and graphitizing.
The net tyre needling type laminated carbon-carbon composite material has the advantages that the material is needled and punctured, carbon fibers are distributed in the horizontal direction in the structure, and are also distributed in the vertical direction, and the carbon fibers in the vertical direction penetrate through a plurality of net tyre layers and the carbon cloth layers, so that the overall structure is more compact and is not easy to delaminate. If the density is increased by carburizing in the later stage, the needling process can lead the whole material to leave a large number of needling holes, the needling holes are easier to penetrate resin or gas in the liquid phase or gas phase infiltration process, the density is easy to promote, and the uniformity is higher. The net tire is made of carbon fiber short fibers, the strength of the net tire is not as good as that of carbon fiber long fibers, in addition, in the needling process, the needling needles can puncture the carbon fibers, a large number of needling holes are left, the material strength can be affected, and the compressive strength and the bending strength are poor especially under the condition of thinner thickness. Because of the need of integral needling process, especially when making certain cylindrical or crucible products, the production time is relatively long and the production period of the products is long.
The carbon cloth type laminated carbon-carbon composite material has the advantages that the material is formed by laminating and bonding a layer of carbon cloth layers, carbon fibers in the material are basically long fibers, and the fibers are continuous and have no fracture, so that the compressive strength and the bending strength are higher, and the strength advantage is obvious especially in materials with thinner thickness. And because no needling is needed, the production efficiency is higher, and the production period of the product is shorter. The disadvantage is that lamination and lamination of carbon cloth are simple, and delamination and cracking are easy to occur. If the density is increased by carburizing in the later stage, the surface of the carbon cloth is too dense, the difficulty of improving the density by liquid phase or gas phase infiltration is high, and uneven density distribution is easy to occur, so that uneven mechanical strength distribution of the material is caused.
Disclosure of Invention
The invention aims to solve the technical problems and provides a high-strength laminated carbon-carbon composite material and a preparation method thereof.
In a first aspect, the present invention provides a high strength laminated carbon-carbon composite material, which is realized by adopting the following technical scheme.
A high-strength laminated carbon-carbon composite material comprises a carbon fiber unidirectional cloth layer and a carbon fiber net tire layer, wherein the carbon fiber unidirectional cloth in the carbon fiber unidirectional cloth layer is paved in a staggered way by 90 degrees, and the carbon fiber net tire is added between the layers, so that the carbon fiber unidirectional cloth is integrally needled and formed.
Further, the interlayer density of the carbon fiber unidirectional cloth and the carbon fiber net tire is 15-25 layers/cm.
Further, the carbon fiber net tire in the carbon-carbon composite material accounts for less than or equal to 20 percent.
In a second aspect, the invention provides a method for preparing a high-strength laminated carbon-carbon composite material, which is realized by adopting the following technical scheme.
The preparation method of the high-strength laminated carbon-carbon composite material comprises the following steps:
s1, preparing carbon fiber unidirectional cloth by drawing and paving carbon fiber filaments; chopping carbon fiber filaments, and performing needling to prepare a carbon fiber net tyre;
s2, the carbon fiber unidirectional cloth is paved in a staggered way according to 90 degrees, a carbon fiber net tire is added between the layers, and the carbon fiber unidirectional cloth is integrally needled to prepare a carbon fiber preform;
s3, impregnating the carbon fiber preform with resin, pressurizing and curing at high temperature, and then carbonizing and graphitizing to prepare the carbon-carbon composite material.
Further, in the step S2, the interlayer density of the carbon fiber unidirectional cloth and the carbon fiber net tire is 15-25 layers/cm.
Further, in the step S2, the carbon fiber unidirectional cloth and the carbon fiber net are of which the proportion is less than or equal to 20 percent.
Further, in step S2, the needling density is 10-20 needles/cm 2 。
Further, in step S3, the curing conditions are: and high-temperature pressurizing and curing at 100-300 deg.c and pressure over 10 MPa.
Further, in the step S3, the carbonization temperature is 800-1600 ℃, the carbonization heating rate is 5-15 ℃/min, the heat preservation time from the highest temperature to the highest temperature is 30-100min, and the natural cooling is carried out after the power-off when the temperature is reduced; the graphitization temperature is 1700-2800 ℃, the graphitization heating rate is 5-15 ℃/min, the heat preservation time to the highest temperature is 30-100min, and the natural cooling is performed after power off when the temperature is reduced.
Further, liquid-phase infiltration or vapor deposition is carried out on the prepared carbon-carbon composite material blank, carbonization and graphitization are carried out again after the density is increased by liquid-phase infiltration or vapor deposition, and finally machining forming is carried out.
The invention has the following beneficial effects.
1. The needling density of the carbon-carbon composite material is lower, the carbon fiber net tire is small in ratio, the carbon fiber unidirectional cloth is larger in ratio, and the interlayer density is extremely high due to the fact that the carbon fiber unidirectional cloth is thinner (the thickness of the carbon fiber unidirectional cloth is smaller than that of the carbon fiber bidirectional cloth and the carbon fiber net tire), so that the volume density is higher, and the material also has higher mechanical strength;
2. the carbon-carbon composite material is subjected to needling processing, carbon fibers exist in the three-dimensional direction, and the material is strong in integrity and not easy to delaminate;
3. the process mainly comprises the steps of laying carbon fiber unidirectional cloth, relatively less needling process, relatively higher production efficiency and relatively shorter production period of products;
4. if the density is increased by carburizing later, the needling process in the application can leave more needling holes in the whole material, the needling holes can be easier for resin or gas to permeate in the liquid phase or gas phase permeation process, the density is relatively easy to promote, and the uniformity is relatively high.
Drawings
FIG. 1 is a cross-sectional view of the carbon-carbon composite of the present invention.
1, a material body; 2. the needle is punched.
Detailed Description
The present invention will be further described with reference to examples.
A method for preparing a high-strength laminated carbon-carbon composite material, comprising the following steps:
1. selecting 1-12K carbon fiber filaments, and performing wiredrawing and laying to prepare carbon fiber unidirectional cloth; cutting carbon fiber filaments (with cutting length of 20-50 mm), and needling (with needling density of 20-50 needles/cm) 2 ) Making a carbon fiber net tyre;
2. then each layer of carbon fiber unidirectional cloth is paved at 90 degrees in a staggered way, a small amount of carbon fiber net tyre (the carbon fiber unidirectional cloth and the carbon fiber net tyre with the carbon fiber net tyre ratio less than or equal to 20 percent and the interlayer density of the carbon fiber unidirectional cloth and the carbon fiber net tyre of 15-25 layers/cm) is added between the layers, and then the needling density is 10-20 needles/cm 2 Integrally needling to prepare a carbon fiber preform;
3. impregnating carbon fiber preform with resin (phenolic resin, furan resin, epoxy resin, etc.), pressurizing at 100-300 deg.C under 10MPa or more for solidification, carbonizing and graphitizing (carbonization temperature 800-1600 deg.C, graphitization temperature 1700-2800 deg.C, and regulating actual temperature rise and fall curve and heat preservation time according to actual condition) to obtain density of 1.6-1.9g/cm 3 Carbon-carbon recombination of (2)And (5) synthesizing materials.
4. If the density is required to be increased, the strength of the material can be further increased by a liquid phase infiltration (impregnating a blank with resin (phenolic, furan, epoxy and other resins) under vacuum in an impregnating pressure furnace, then charging inert gas such as nitrogen or argon, pressurizing by gas, wherein the pressure is 1-10Mpa, impregnating the resin, then curing the resin at a high temperature of 100-300 ℃ for 2-24 hours) or vapor deposition (in a vapor deposition furnace, taking gas such as helium, hydrogen, argon or nitrogen as carrier gas, taking methane, propane or propylene and other hydrocarbon gases with low relative molecular mass as carbon sources, infiltrating hydrocarbon gases between fibers under the environmental pressure of 0.1-10Kpa, performing pyrolysis at the high temperature of 500-1200 ℃ to generate carbon to deposit in gaps of the carbon fibers and on the surfaces of the carbon fibers), further increasing the density, improving the strength, and completing the process in the order of increasing the density, carbonizing and graphitizing.
Example 1
A method for preparing a high-strength laminated carbon-carbon composite material, comprising the following steps:
1. spreading: 3K carbon fiber filaments of Zhongfushenying hawk 49s are selected, are manufactured into carbon fiber unidirectional cloth through wiredrawing and paving, and then each layer of unidirectional cloth is paved and laminated in a staggered way according to 90 degrees; adding a small amount of carbon fiber net tyres (carbon fiber unidirectional cloth and carbon fiber net tyres, wherein the carbon fiber net tyres account for 15% of the carbon fiber unidirectional cloth and carbon fiber net tyres, and the interlayer density of the carbon fiber unidirectional cloth and the carbon fiber net tyres is 20 layers/cm) which are prepared by chopping 12K carbon fiber filaments of Chinese godet hawk 49s and then lapping and needling;
2. needling: the needling density is 15 needles/cm 2 Integrally needling to prepare a carbon fiber preform;
3. and (3) dipping and curing: impregnating the preform with phenolic epoxy resin, and then pressurizing and curing the resin at a high temperature of 200 ℃ and a pressure of 50 Mpa;
4. carbonizing and graphitizing: carbonizing and graphitizing the resin-impregnated preform (carbonization temperature 1000 deg.C, graphitization temperature 2000 deg.C, wherein the heating rate of the carbonization furnace is 10-15 deg.C/min, the holding time to the highest temperature is 200min, and naturally cooling down when cooling down, graphitization furnace heating up)The temperature rate is 10-15 ℃/min, the heat preservation time from the highest temperature to the highest temperature is 300min, and the natural cooling is carried out when the temperature is reduced by power off), and the density is 1.6-1.9g/cm 3 Carbon-carbon composite material of (a).
5. And (3) forming: and machining and forming as required.
Performance detection
1. And (3) density detection: cutting 50mm square 50mm, and detecting density not less than 1.6g/cm 3 ；
2. Density uniformity detection: the error of the detection density is required to be within +/-5% according to the different square blocks with the cutting dimensions of 50mm and 50 mm;
3. bending strength test: according to the national standard GB/T40398.2-2021, the bending strength is tested to be more than or equal to 150Mpa (compared with the conventional carbon-carbon composite material, the conventional bending strength is more than or equal to 100Mpa, so that the bending strength is improved by 50 percent);
4. compressive strength test: the compressive strength is more than or equal to 220Mpa (compared with the conventional carbon-carbon composite material, the compressive strength is more than or equal to 150Mpa, and therefore, the bending strength is improved by more than 46 percent) according to the national standard GB/T34559-2017;
5. high temperature resistance test: processing 200mm by 100mm by 30mm, placing in a high-temperature furnace, cooling naturally to room temperature after heating to a maximum temperature of 2800 ℃ at 20 ℃/min and a heat preservation time of 200min, and taking out the material without cracking, layering and deformation.
The embodiments of the present invention are all preferred embodiments of the present invention, and are not intended to limit the scope of the present invention in this way, therefore: all equivalent changes in structure, shape and principle of the invention should be covered in the scope of protection of the invention.
Claims (10)
1. A high strength laminated carbon-carbon composite material characterized by: the carbon fiber unidirectional fabric comprises a carbon fiber unidirectional fabric layer and a carbon fiber net tire layer, wherein the carbon fiber unidirectional fabric in the carbon fiber unidirectional fabric layer is paved in a staggered way by 90 degrees, the carbon fiber net tire is added between the layers, and the carbon fiber unidirectional fabric is integrally needled and formed.
2. A high strength laminated carbon-carbon composite material according to claim 1, wherein: the interlayer density of the carbon fiber unidirectional cloth and the carbon fiber net tire is 15-25 layers/cm.
3. A high strength laminated carbon-carbon composite material according to claim 1, wherein: the carbon fiber net tyre in the carbon-carbon composite material accounts for less than or equal to 20 percent.
4. A method of making the high strength laminated carbon-carbon composite material of any one of claims 1-3, characterized by: the method comprises the following steps:
s1, preparing carbon fiber unidirectional cloth by drawing and paving carbon fiber filaments; chopping carbon fiber filaments, and performing needling to prepare a carbon fiber net tyre;
s2, the carbon fiber unidirectional cloth is paved in a staggered way according to 90 degrees, a carbon fiber net tire is added between the layers, and the carbon fiber unidirectional cloth is integrally needled to prepare a carbon fiber preform;
s3, impregnating the carbon fiber preform with resin, pressurizing and curing at high temperature, carbonizing and graphitizing to prepare a carbon-carbon composite material blank, and machining and forming the blank.
5. The method for producing a high-strength laminated carbon-carbon composite material according to claim 4, wherein: in the step S2, the interlayer density of the carbon fiber unidirectional cloth and the carbon fiber net tire is 15-25 layers/cm.
6. The method for producing a high-strength laminated carbon-carbon composite material according to claim 4, wherein: in the step S2, the carbon fiber unidirectional cloth and the carbon fiber net are of which the proportion is less than or equal to 20 percent.
7. The method for producing a high-strength laminated carbon-carbon composite material according to claim 4, wherein: in step S2, needling density is 10-20 needles/cm 2 。
8. The method for producing a high-strength laminated carbon-carbon composite material according to claim 4, wherein: in step S3, the curing conditions are: and high-temperature pressurizing and curing at 100-300 deg.c and pressure over 10 MPa.
9. The method for producing a high-strength laminated carbon-carbon composite material according to claim 4, wherein: in the step S3, the carbonization temperature is 800-1600 ℃, the carbonization heating rate is 5-15 ℃/min, the heat preservation time from the highest temperature to the highest temperature is 30-100min, and the natural cooling is performed; graphitization temperature is 1700-2800 ℃, graphitization heating rate is 5-15 ℃/min, heat preservation time to the highest temperature is 30-100min, and natural cooling is performed.
10. The method for producing a high-strength laminated carbon-carbon composite material according to claim 4, wherein: and (3) performing liquid-phase infiltration or vapor deposition on the prepared carbon-carbon composite material blank, performing carbonization and graphitization again after increasing the density by liquid-phase infiltration or vapor deposition, and finally performing machining forming.
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| 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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