CN115558241A - High-thermal-conductivity carbon fiber fabric composite material and preparation method thereof - Google Patents

High-thermal-conductivity carbon fiber fabric composite material and preparation method thereof Download PDF

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Publication number
CN115558241A
CN115558241A CN202211265242.4A CN202211265242A CN115558241A CN 115558241 A CN115558241 A CN 115558241A CN 202211265242 A CN202211265242 A CN 202211265242A CN 115558241 A CN115558241 A CN 115558241A
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carbon fiber
heat
conducting
fiber fabric
composite material
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张学骜
程书建
郭晓晓
林明源
蔡加法
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Jiujiang Research Institute Of Xiamen University
Xiamen University
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Jiujiang Research Institute Of Xiamen University
Xiamen University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L63/00Compositions of epoxy resins; Compositions of derivatives of epoxy resins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L79/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
    • C08L79/04Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
    • C08L79/08Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
    • C08L79/085Unsaturated polyimide precursors
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
    • C08L83/04Polysiloxanes

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  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Reinforced Plastic Materials (AREA)

Abstract

A high-thermal-conductivity carbon fiber fabric composite material and a preparation method thereof are disclosed, and the composite material comprises the following raw materials in percentage by mass: 35-60% of carbon fiber fabric, 10-45% of polymer matrix, 5-35% of heat-conducting chopped carbon fiber, 5-40% of curing agent and 5-15% of film-forming agent. The invention leads the heat-conducting short carbon fiber to be evenly and stably dispersed in the polyvinyl alcohol solution by mechanical stirring. The heat-conducting chopped carbon fiber solution is placed in a magnetic field, and is rotated in the magnetic field due to the Langchant diamagnetism, the heat-conducting chopped carbon fiber solution is converted from a high energy state to a low energy state until the axis of the heat-conducting chopped carbon fiber is parallel to the direction of the external magnetic field, the energy reaches the lowest state, and the heat-conducting chopped carbon fiber is directionally arranged in the polyvinyl alcohol solution; the heat-conducting chopped carbon fibers are vertically implanted into the carbon fiber fabric through vacuum filtration, the axial high-heat-conductivity characteristic of the heat-conducting chopped carbon fibers is fully utilized, and the heat-conducting chopped carbon fibers are vertically and directionally arranged through implantation, so that the heat-conducting performance of the carbon fiber fabric composite material in the thickness direction is improved.

Description

High-thermal-conductivity carbon fiber fabric composite material and preparation method thereof
Technical Field
The invention relates to the field of heat-conducting composite materials, in particular to a high-heat-conducting carbon fiber fabric composite material and a preparation method thereof.
Background
As the density of electronic devices increases, the heat generated by electronic equipment builds up rapidly. In order to ensure reliable operation of an electronic device for a long period of time, it is necessary to prevent the operating temperature of the device from rising, and therefore, the heat dissipation capability becomes an important factor affecting the service life of the electronic device.
The carbon fiber fabric composite material has the advantages of high strength, low density and the like, and is widely applied. However, the carbon fiber fabric composite material has poor heat conductivity in the thickness direction, so that the preparation of the high-heat-conductivity carbon fiber fabric composite material with excellent comprehensive performance becomes a research hotspot in the field in order to meet the development requirements of various manufacturing industries and high-tech fields of electronics, aerospace, military equipment and the like, and is receiving more and more attention.
At present, the research on the high-thermal-conductivity carbon fiber fabric composite materials at home and abroad focuses on filling high-thermal-conductivity particles, and the fillers mainly adopted are copper, diamond, graphene, carbon fibers, aluminum oxide and the like. However, the prior art does not solve the problem of ordering of fillers, has poor heat conduction performance in the thickness direction, and has heat conductivity of only 0.7 to 1W/(m.K). Thermally conductive chopped carbon fiber (mesophase pitch-based carbon fiber) as a fiber consisting of carbon atoms in sp 2 The carbon material with the hexagonal honeycomb lattice structure formed by the hybrid tracks has high orientation degree and excellent heat conduction performance, the axial heat conductivity reaches 900W/(m.K), and the carbon material is common heat conductionTens of times the material. However, thermally conductive chopped carbon fibers have high axial thermal conductivity and low radial thermal conductivity. Therefore, the heat-conducting chopped carbon fibers vertically and directionally arranged in the carbon fiber fabric are expected to remarkably improve the heat-conducting performance of the carbon fiber fabric composite material in the thickness direction.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a high-thermal-conductivity carbon fiber fabric composite material and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the high-thermal-conductivity carbon fiber fabric composite material comprises, by mass, 35% -60% of carbon fiber fabrics, 10% -45% of a polymer matrix, 5% -35% of thermal-conductivity chopped carbon fibers, 5% -40% of a curing agent and 5% -15% of a film forming agent.
The carbon fiber fabric is high-strength carbon fiber and has a thickness of 0.2-1 mm.
The polymer matrix is at least one of epoxy resin, bismaleimide resin, cyanate ester resin and silicon rubber.
The heat-conducting short carbon fibers are mesophase pitch-based carbon fibers, the diameter of the mesophase pitch-based carbon fibers can be 5-10 microns, and the length of the mesophase pitch-based carbon fibers can be 25-200 microns.
The film former may be selected from polyvinyl alcohol and glycerol.
The curing agent can be at least one selected from dicyandiamide, methylhexahydrophthalic anhydride and hydrogen-containing silicone oil.
The preparation method of the high-thermal-conductivity carbon fiber fabric composite material comprises the following steps:
1) Adding polyvinyl alcohol into deionized water, stirring and heating to obtain a polyvinyl alcohol solution.
2) Adding the heat-conducting short carbon fibers into a polyvinyl alcohol solution, dropwise adding glycerol, mechanically stirring, and performing ultrasonic dispersion to obtain a dispersion;
3) Placing the carbon fiber fabric on a vacuum pumping filter membrane, adding the heat-conducting short-cut carbon fiber dispersion liquid, and applying a magnetic field;
4) Starting a vacuum pump, pumping water in the dispersion liquid into a filter flask, arranging the heat-conducting short carbon fibers in order under the action of a magnetic field, and vertically implanting the heat-conducting short carbon fibers into the carbon fiber fabric by vacuum negative pressure;
5) And transferring the carbon fiber fabric mixture subjected to suction filtration to an electric heating constant temperature air blast drying oven, and heating, drying and curing.
6) And putting the cured carbon fiber fabric mixture into a mold, pouring a polymer and a curing agent, moving the mold to a vacuum oven, and heating and curing to obtain the high-thermal-conductivity carbon fiber fabric composite material.
In the step 3), the magnetic induction intensity of the external magnetic field is 0.1-1 Tesla, and the heat-conducting short carbon fibers need to be directionally arranged in the magnetic field.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1) According to the invention, the heat-conducting chopped carbon fibers are dispersed in the polyvinyl alcohol solution through mechanical stirring, can uniformly and stably exist in the polyvinyl alcohol solution, and do not need a dispersing agent.
2) The heat-conducting chopped carbon fiber solution is placed in a magnetic field, and is rotated in the magnetic field due to the Langchant diamagnetism, the heat-conducting chopped carbon fiber solution is converted from a high energy state to a low energy state until the axis of the heat-conducting chopped carbon fiber is parallel to the direction of the external magnetic field, the energy reaches the lowest state, and the heat-conducting chopped carbon fiber is directionally arranged in the polyvinyl alcohol solution; the heat-conducting chopped carbon fibers are vertically implanted into the carbon fiber fabric through vacuum filtration, the axial high-heat-conductivity characteristic of the heat-conducting chopped carbon fibers is fully utilized, and the heat-conducting chopped carbon fibers are vertically and directionally arranged through implantation, so that the heat-conducting performance of the carbon fiber fabric composite material in the thickness direction is improved.
3) The preparation method is simple and convenient and is easy to popularize.
Drawings
FIG. 1 is an optical microscope image of a carbon fiber fabric prepared in example 3 with vertically implanted directionally aligned thermally conductive chopped carbon fibers;
fig. 2 is a scanning electron microscope image of the cross section of the high thermal conductivity carbon fiber fabric composite material of example 3.
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. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A preparation method of a high-thermal-conductivity carbon fiber fabric composite material comprises 35-60% of carbon fiber fabric, wherein the carbon fiber fabric is high-strength carbon fiber and has the thickness of 0.2-1 mm; 5% -35% of heat-conducting chopped carbon fibers, wherein the diameter of each heat-conducting chopped carbon fiber is 5-10 mu m, and the length of each heat-conducting chopped carbon fiber is 25-200 nm;10% -45% of a polymer matrix, wherein the polymer matrix is at least one of epoxy resin, bismaleimide resin, cyanate ester resin and silicone rubber; 5 to 40 percent of curing agent, wherein the curing agent can be at least one of dicyandiamide, methylhexahydrophthalic anhydride and hydrogen-containing silicone oil; 5 to 15 percent of film forming agent, wherein the film forming agent can be selected from polyvinyl alcohol and glycerol, and a magnet (the magnetic induction intensity is 0.1 to 1 Tesla);
according to the materials in the ratio of the components by weight, firstly, dissolving polyvinyl alcohol by deionized water to obtain a polyvinyl alcohol solution, sequentially adding carbon fibers and glycerol into the polyvinyl alcohol solution, and carrying out mechanical stirring and ultrasonic dispersion. Secondly, placing the carbon fiber fabric on a filter membrane, applying a magnetic field, pouring a heat-conducting short carbon fiber solution, carrying out suction filtration, directionally arranging the heat-conducting short carbon fibers, vertically implanting the carbon fiber fabric, heating, drying and curing. And finally, compounding the cured carbon fiber fabric with a polymer matrix to obtain the high-thermal-conductivity carbon fiber fabric composite material. The high-thermal-conductivity carbon fiber fabric composite material adopts thermal-conductivity chopped carbon fibers as fillers, and can be prepared by adopting simple methods such as mechanical stirring and mixing, ultrasonic dispersion, magnetic field induced orientation, vacuum filtration and the like through a plurality of steps.
Specifically, the preparation process of the high thermal conductivity carbon fiber fabric composite material is as follows:
a. adding polyvinyl alcohol into deionized water, stirring and heating at 95 ℃ for 2 hours to obtain a polyvinyl alcohol solution;
b. adding the heat-conducting short-cut carbon fibers and glycerol into a polyvinyl alcohol solution, mechanically stirring, and ultrasonically dispersing;
c. placing the carbon fiber fabric on a vacuum pumping filter membrane, applying a magnetic field, pouring a heat-conducting short-cut carbon fiber solution, vacuumizing, and vertically implanting the heat-conducting short-cut carbon fiber into the carbon fiber fabric;
d. the carbon fiber fabric is moved into an electric heating constant temperature blast drying oven, heated, dried and cured;
e. and (3) placing the cured carbon fiber fabric in a mold, pouring a polymer matrix and a curing agent, transferring to a vacuum drying oven, and further heating and curing.
Specific examples are given below.
Example 1
A high-thermal-conductivity carbon fiber fabric composite material comprises 35% of carbon fiber fabric, 5% of thermal-conductivity chopped carbon fibers, 10% of polyvinyl alcohol, 5% of glycerol, 35% of polymer and 10% of curing agent. The diameter of the heat-conducting chopped carbon fiber is 10 mu m, and the length of the heat-conducting chopped carbon fiber is 200um. The prepared product was subjected to thermal conductivity test, and the results are shown in table 1.
Example 2
A high-thermal-conductivity carbon fiber fabric composite material comprises 60% of carbon fiber fabric, 5% of thermal-conductivity chopped carbon fibers, 5% of polyvinyl alcohol, 5% of glycerol, 20% of polymer and 5% of curing agent. The heat-conducting chopped carbon fibers have the diameter of 5 mu m and the length of 25 mu m. The prepared product was subjected to thermal conductivity test, and the results are shown in table 1.
Example 3
A high-thermal-conductivity carbon fiber fabric composite material comprises 40% of carbon fiber fabric, 35% of thermal-conductivity chopped carbon fibers, 5% of polyvinyl alcohol, 5% of glycerol, 10% of polymer and 5% of curing agent. The diameter of the heat-conducting chopped carbon fiber is 10 mu m, and the length of the heat-conducting chopped carbon fiber is 25um. The prepared product was subjected to thermal conductivity test, and the results are shown in table 1.
As shown in fig. 1 to 2, in the product prepared in example 3, the thermally conductive chopped carbon fibers were regularly arranged to be perpendicular to the upper and lower surfaces of the carbon fiber fabric.
Example 4
A high-thermal-conductivity carbon fiber fabric composite material comprises 35% of carbon fiber fabric, 5% of thermal-conductivity chopped carbon fibers, 5% of polyvinyl alcohol, 5% of glycerol, 45% of polymer and 5% of curing agent. The diameter of the heat-conducting chopped carbon fiber is 10 mu m, and the length of the heat-conducting chopped carbon fiber is 150um. The prepared product was subjected to thermal conductivity test, and the results are shown in table 1.
Example 5
A high-thermal-conductivity carbon fiber fabric composite material comprises 35% of carbon fiber fabric, 10% of thermal-conductivity chopped carbon fiber, 7.5% of polyvinyl alcohol, 7.5% of glycerol, 20% of polymer and 20% of curing agent. The heat-conducting chopped carbon fibers have the diameter of 5 mu m and the length of 200 mu m. The prepared product was subjected to thermal conductivity test, and the results are shown in table 1.
TABLE 1
Examples Carbon fiber Fabric content (Wt%) Heat conductive chopped carbon fiber content (Wt%) Thermal conductivity W/(m K)
1 35% carbon fiber fabric 5% heat-conducting chopped carbon fiber 1.6
2 60% carbon fiber fabric 5% heat-conducting chopped carbon fiber 1.8
3 40% carbon fiber fabric 35% heat-conducting chopped carbon fiber 5.5
4 35% carbon fiber fabric 5% heat-conducting chopped carbon fiber 1.5
5 35% carbon fiber fabric 10% heat conductive chopped carbon fiber 2
According to the invention, the heat-conducting chopped carbon fibers and the glycerol are added into the PVA solution, and mechanical stirring and ultrasonic dispersion are carried out to obtain the heat-conducting chopped carbon fiber solution. And placing the carbon fiber fabric on a vacuum pumping membrane, applying a magnetic field, pouring a heat-conducting short carbon fiber solution, vacuumizing, and vertically implanting the heat-conducting short carbon fiber into the carbon fiber fabric. And putting the cured carbon fiber fabric mixture into a mold, pouring a polymer, moving the mold to a vacuum oven, and heating and curing to obtain the high-thermal-conductivity carbon fiber fabric composite material. The composite material adopts magnetic field to induce the orientation of the heat-conducting chopped carbon fibers, and the heat-conducting chopped carbon fibers are vertically implanted into the carbon fiber fabric by a vacuum filtration method, so that the high-heat-conducting carbon fiber fabric composite material can be prepared by simple steps.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.

Claims (8)

1. The high-thermal-conductivity carbon fiber fabric composite material is characterized by comprising the following raw materials in percentage by mass: 35-60% of carbon fiber fabric, 10-45% of polymer matrix, 5-35% of heat-conducting chopped carbon fiber, 5-40% of curing agent and 5-15% of film-forming agent.
2. A highly thermally conductive carbon fiber fabric composite material as claimed in claim 1, wherein: the carbon fiber fabric is high-strength carbon fiber and has a thickness of 0.2-1 mm.
3. A high thermal conductivity carbon fiber fabric composite material as claimed in claim 1, wherein: the polymer matrix is at least one of epoxy resin, bismaleimide resin, cyanate ester resin and silicon rubber.
4. A high thermal conductivity carbon fiber fabric composite material as claimed in claim 1, wherein: the heat-conducting short carbon fibers are mesophase pitch-based carbon fibers, the diameter of the mesophase pitch-based carbon fibers can be 5-10 microns, and the length of the mesophase pitch-based carbon fibers can be 25-200 microns.
5. A highly thermally conductive carbon fiber fabric composite material as claimed in claim 1, wherein: the film forming agent comprises polyvinyl alcohol and glycerol.
6. A high thermal conductivity carbon fiber fabric composite material as claimed in claim 1, wherein: the curing agent can be at least one selected from dicyandiamide, methylhexahydrophthalic anhydride and hydrogen-containing silicone oil.
7. The method for preparing a high-thermal-conductivity carbon fiber fabric composite material as claimed in any one of claims 1 to 6, characterized by comprising the following steps:
1) Adding polyvinyl alcohol into deionized water, stirring and heating to obtain a polyvinyl alcohol solution;
2) Adding the heat-conducting short carbon fibers into a polyvinyl alcohol solution, dropwise adding glycerol, mechanically stirring, and ultrasonically dispersing to obtain a heat-conducting short carbon fiber dispersion liquid;
3) Placing the carbon fiber fabric on a vacuum pumping filter membrane, adding the heat-conducting short-cut carbon fiber dispersion liquid, and applying a magnetic field;
4) Starting a vacuum pump, pumping water in the heat-conducting chopped carbon fiber dispersion liquid into a filter flask, arranging the heat-conducting chopped carbon fibers in an oriented manner under the action of a magnetic field, and vertically implanting the heat-conducting chopped carbon fibers into a carbon fiber fabric by vacuum negative pressure to obtain a carbon fiber fabric mixture;
5) Transferring the carbon fiber fabric mixture subjected to suction filtration to an electric heating constant-temperature air blast drying oven, and heating, drying and curing;
6) And putting the cured carbon fiber fabric mixture into a mold, pouring a polymer matrix and a curing agent, moving the polymer matrix and the curing agent to a vacuum oven, and heating and curing to obtain the high-thermal-conductivity carbon fiber fabric composite material.
8. The method of claim 7, wherein: in the step 3), the magnetic induction intensity of the external magnetic field is 0.1-1 Tesla.
CN202211265242.4A 2022-10-17 2022-10-17 High-thermal-conductivity carbon fiber fabric composite material and preparation method thereof Pending CN115558241A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170137561A1 (en) * 2014-05-09 2017-05-18 Jnc Corporation Composition for heat-dissipation members, heat-dissipation member, and electronic device
CN107323025A (en) * 2017-08-02 2017-11-07 北京航空航天大学 Vertical orientated composite of a kind of interlayer high heat conduction fine hair and preparation method thereof
CN110093033A (en) * 2019-05-27 2019-08-06 南京航空航天大学 A kind of induced by magnetic field fiber reinforced polyimide composite material and preparation method thereof
CN111978732A (en) * 2020-09-04 2020-11-24 广东思泉新材料股份有限公司 Thermal interface material with three-dimensional heat conduction network structure
CN113278259A (en) * 2021-05-14 2021-08-20 吉林大学 Preparation method of bionic carbon fiber reinforced epoxy resin composite material
CN113416420A (en) * 2021-06-25 2021-09-21 厦门大学 Preparation method of high-orientation-arrangement graphene sheet thermal interface material
CN114456603A (en) * 2022-01-27 2022-05-10 厦门大学 Magnetic field induction arrangement carbon fiber heat conduction material and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20170137561A1 (en) * 2014-05-09 2017-05-18 Jnc Corporation Composition for heat-dissipation members, heat-dissipation member, and electronic device
CN107323025A (en) * 2017-08-02 2017-11-07 北京航空航天大学 Vertical orientated composite of a kind of interlayer high heat conduction fine hair and preparation method thereof
CN110093033A (en) * 2019-05-27 2019-08-06 南京航空航天大学 A kind of induced by magnetic field fiber reinforced polyimide composite material and preparation method thereof
CN111978732A (en) * 2020-09-04 2020-11-24 广东思泉新材料股份有限公司 Thermal interface material with three-dimensional heat conduction network structure
CN113278259A (en) * 2021-05-14 2021-08-20 吉林大学 Preparation method of bionic carbon fiber reinforced epoxy resin composite material
CN113416420A (en) * 2021-06-25 2021-09-21 厦门大学 Preparation method of high-orientation-arrangement graphene sheet thermal interface material
CN114456603A (en) * 2022-01-27 2022-05-10 厦门大学 Magnetic field induction arrangement carbon fiber heat conduction material and preparation method thereof

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