CN115433434A - Three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material and preparation method thereof - Google Patents

Three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material and preparation method thereof Download PDF

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CN115433434A
CN115433434A CN202211000423.4A CN202211000423A CN115433434A CN 115433434 A CN115433434 A CN 115433434A CN 202211000423 A CN202211000423 A CN 202211000423A CN 115433434 A CN115433434 A CN 115433434A
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epoxy resin
composite material
electromagnetic shielding
mxene
carbon fiber
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权震震
沈萌迪
王黎明
覃小红
俞建勇
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Donghua University
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    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00—Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073—Shielding materials
    • H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract

The invention relates to a three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material and a preparation method thereof. The composite material takes porous three-dimensional woven carbon fiber as a reinforcement, MXene as filling particles and epoxy resin as a matrix. The preparation method comprises the following steps: preparing three-dimensional woven carbon fibers by using the carbon fibers through a weaving process; dissolving epoxy resin in a thinner, adding MXene, dispersing to obtain an electromagnetic shielding filler dispersion liquid, stirring and carrying out ultrasonic treatment, heating, adding a curing agent, defoaming to obtain a resin mixed liquid, and carrying out resin infusion and curing on the three-dimensional woven carbon fiber by using the resin mixed liquid by using a forming process. The electromagnetic shielding composite material prepared by the preparation method has the advantages of excellent mechanical property, electromagnetic shielding property, stability and the like.

Description

Three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material and preparation method thereof
Technical Field
The invention belongs to the field of electromagnetic shielding materials and preparation thereof, and particularly relates to a three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material and a preparation method thereof.
Background
With the rapid development of 5G mobile signals, various electronic devices have been widely used, which improve people's living standard, but also bring about serious electromagnetic interference (EMI) and radiation. These miniaturized devices can generate electromagnetic waves, which can affect the normal use of electronic systems and even cause leakage of electromagnetic information. In addition, if the human body is exposed to electromagnetic radiation for a long time, it may have harmful effects on human health, such as nausea, headache, eye problems, cancer, and adverse effects on brain development of infants. Some medical implants or devices (e.g., hearing aids, insulin pumps, and hearts) are also prone to failure in alternating electric fields, and therefore, there is a strong need for a good shield to limit the electromagnetic contamination to a certain extent and to reduce its ability to diffuse out.
The composite material is artificially compounded by two or more than two artificially selected components (or constituent components) in a certain quantity ratio, and each component has an obvious interface and a certain special function. The laminated composite material has wide application in the fields of aerospace, ships, sports equipment and the like, but the laminated composite material serving as a main bearing structure is easy to be layered and damaged after being stressed and cannot meet the requirements of engineering application. The three-dimensional woven composite material is almost free from layering when being damaged by external force due to the integrity of the three-dimensional woven composite material, and the three-dimensional woven composite material gradually replaces the traditional composite material to become the first choice for engineering application in recent years.
In recent years, attention has been paid to three-dimensional woven composite materials in more and more engineering fields, and three-dimensional woven composite materials with integrated structural functions have been proposed. The three-dimensional braided composite material with integrated structure and function meets the requirement of electromagnetic shielding performance, has good mechanical property, and can be widely applied to places requiring light weight, high strength and stable electromagnetic shielding performance of materials, such as shielding chamber shells, airplane skins, equipment cabins and the like.
Disclosure of Invention
The invention aims to solve the technical problem of providing a three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material and a preparation method thereof.
The invention provides an electromagnetic shielding composite material, which takes porous three-dimensional woven carbon fibers as a reinforcement, MXene as filling particles and epoxy resin as a matrix, wherein the MXene is communicated with circuits between adjacent carbon fiber filaments to form a three-dimensional network channel in the epoxy resin.
Preferably, the three-dimensional woven carbon fiber structure comprises three-dimensional four-direction, three-dimensional five-direction, three-dimensional six-direction or three-dimensional seven-direction.
Preferably, the MXene comprises Ti 3 C 2 T x 、V 2 CT x 、Nb 2 CT x 、Mo 2 CT x 、Nb 4 C 3 Tx、V 4 C 3 T x One or more of them.
Preferably, the epoxy resin comprises one or more of resorcinol epoxy resin, glycerol epoxy resin and novolac epoxy resin.
The invention also provides a preparation method of the electromagnetic shielding composite material, which comprises the following steps:
(1) Preparing three-dimensional woven carbon fibers by using the carbon fibers through a weaving process;
(2) Dissolving epoxy resin in a thinner, adding MXene, and dispersing to obtain an electromagnetic shielding filler dispersion liquid;
(3) Stirring the electromagnetic shielding filler dispersion liquid in the step (2), carrying out ultrasonic treatment, heating and volatilizing the thinner, then adding a curing agent, and defoaming to obtain a resin mixed liquid;
(4) And (3) performing resin infusion on the three-dimensional woven carbon fiber in the step (1) by using the resin mixed solution in the step (3) by using a molding process, and curing to obtain the electromagnetic shielding composite material.
Preferably, the carbon fiber in the step (1) is 6-24K carbon fiber.
Preferably, the knitting process in the step (1) is as follows: the knitting yarns are interwoven through a four-step or two-step knitting process.
Preferably, the diluent in the step (2) comprises one or more of acetone, ethanol, ethylene glycol, toluene, xylene, ethyl acetate and dioxane.
Preferably, the resin mixed liquor in the step (3) comprises the following components in percentage by weight: 2 to 15 percent of MXene, 40 to 50 percent of epoxy resin, 34 to 42.5 percent of curing agent and 5 to 15 percent of thinner.
Preferably, the curing agent in the step (3) comprises one or more of aliphatic amine/modified aliphatic amine curing agent, alicyclic amine/modified alicyclic amine curing agent, polyamide curing agent, aromatic amine/modified aromatic amine curing agent and phenolic aldehyde amine curing agent.
Preferably, the molding process in the step (4) includes a vacuum assisted resin transfer process, a resin transfer molding process or a vacuum infusion molding process.
The invention also provides application of the electromagnetic shielding composite material in an airplane framework, a skin, electronic equipment and various functional components.
Advantageous effects
(1) The invention has high temperature resistance, the long-term working temperature of the carbon fiber can reach about 300 ℃, the mechanical property is not reduced (strength super steel) and the invention can be applied to extreme conditions of aerospace and military.
(2) The three-dimensional woven carbon fiber multidirectional yarn is conductive to improve the electromagnetic shielding performance, and the three-dimensional woven multidirectional yarn forms a conductive path in each direction, so that the movement of electrons in an alternating electric field is facilitated, the ohmic loss is increased, and the electromagnetic shielding performance is improved.
(3) The three-dimensional woven preform fiber is quasi-isotropic, absorbs electromagnetic waves in all directions, has more than four orientations compared with a single-layer laying layer or a conductive filler composite material, and can realize the absorption of the electromagnetic waves in all directions.
(4) The invention has excellent mechanical property, the three-dimensional woven carbon fiber/epoxy resin keeps the excellent mechanical property of a three-dimensional woven piece, and the three-dimensional woven carbon fiber/epoxy resin is not easy to layer under the action of external force; has high specific strength and specific modulus; the fatigue resistance is good; the vibration damping capacity is strong, and the vibration absorption performance is good; excellent ablation resistance; the designability is strong, and the forming process is simple; good safety performance in overload and the like.
(5) The electromagnetic shielding material has stable electromagnetic shielding performance, and MXene can be effectively protected and prevented from being oxidized by taking the resin as the outermost layer material, so that the performance reliability and the stability of the composite material are ensured.
Drawings
Fig. 1 is a schematic structural diagram of a three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material of the present invention, wherein 1 is a carbon fiber three-dimensional woven preform; 2 is MXene; and 3 is surface layer epoxy resin.
Fig. 2 shows the shielding effectiveness of the carbon fiber/MXene/epoxy resin electromagnetic shielding composite material prepared in example 1.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention can be made by those skilled in the art after reading the teaching of the present invention, and these equivalents also fall within the scope of the claims appended to the present application.
Example 1
A three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material takes a three-dimensional four-way carbon fiber three-dimensional woven prefabricated part as a reinforcement, and resin mixed liquid comprises the following components in percentage by weight: 15% of MXene, 40% of epoxy resin, 34% of curing agent and 11% of thinner; wherein MXene is MulD-Ti 3 C 2 T x 。
Specifically, in the present embodiment, the ringThe oxygen resin is JC-02A produced by the firm Kaffir chemical company, the curing agent is JC-02B produced by the firm Kaffir chemical company, the MXene is organ-shaped MulD-Ti produced by the North Korea science and technology company Limited of Suzhou 3 C 2 T x The carbon fiber is T300 carbon fiber produced by Dongli in Japan.
The embodiment also provides a preparation method of the three-dimensional braided carbon fiber/MXene/epoxy resin electromagnetic shielding composite material, which comprises the following steps:
(1) Preparing a woven three-dimensional four-way prefabricated member by using a four-step weaving process;
(2) 40g of epoxy resin was diluted with 22g of acetone;
(3) Adding 15g of MulD-Ti into the diluted epoxy resin obtained in the step (2) 3 C 2 T x Filling and uniformly dispersing to obtain an electromagnetic shielding filling dispersion liquid;
(4) Performing constant-temperature magnetic stirring at 25 ℃ on the electromagnetic shielding filler dispersion liquid obtained in the step (3), and performing ultrasonic treatment with the frequency of 40KHz and the time of 30 min;
(5) Heating the ultrasonic electromagnetic shielding filler dispersion liquid obtained in the step (4) to volatilize most of the thinner, adding 34g JC-02B curing agent, and uniformly mixing;
(6) Placing the electromagnetic shielding filler dispersion liquid obtained in the step (5) after the curing agent is added into a vacuum drying oven at 60 ℃ for defoaming for 1.5h;
(7) Maintaining the temperature of the dispersion liquid at 60 ℃ and the vacuum degree at 0.1MPa, and performing resin infusion on the braided prefabricated member obtained in the step (1) by using the defoamed electromagnetic shielding filler dispersion liquid obtained in the step (6) through a vacuum-assisted resin transfer molding process;
(8) And (3) curing the woven prefabricated member which is subjected to resin infusion and obtained in the step (7) in an oven, baking for 2 hours at the temperature of 90 ℃, baking for 1 hour at the temperature of 110 ℃, and baking for 4 hours at the temperature of 130 ℃ to obtain the carbon fiber/MXene/epoxy resin electromagnetic shielding composite material.
The electromagnetic wave absorption efficiency test adopts an Agilent PAN-LN523B vector network analyzer to test the three-dimensional woven carbon fiber/MXene/epoxy resin composite material according to a waveguide method. And testing the absorption and reflection power values of the material in the frequency range of 8.2-12.4 GHz. Specific test data are shown in table 1:
table 1 electromagnetic wave absorption efficiency test
Test frequency/GHz R A
8.2 0.44 0.56
8.8 0.32 0.67
9.4 0.24 0.76
10.0 0.17 0.83
10.6 0.13 0.87
11.2 0.10 0.89
11.8 0.08 0.91
12.4 0.08 0.92
As can be seen from Table 1, the addition of acetone greatly reduced the viscosity of the epoxy resin, promoting the uniform dispersion of MXene in the resin system. MXene is communicated with circuits between adjacent carbon fiber filaments, so that an efficient electromagnetic transmission three-dimensional network channel is formed in a resin matrix, the conductivity of the electromagnetic transmission three-dimensional network channel and the electromagnetic wave absorption performance of a composite material are remarkably improved, and more electromagnetic waves are absorbed by the material. In addition, the three-dimensional woven prefabricated member contains more gaps, electromagnetic waves are continuously reflected on the hole wall when passing through the three-dimensional woven prefabricated member, the transmission distance of the electromagnetic waves is increased, and therefore the electromagnetic wave energy is subjected to multiple reflection in an electromagnetic field and is finally lost in the form of heat energy. Example 1 the material prepared had a density of 1.82g/cm 3 And the development requirement of light weight of the electromagnetic shielding material is met.
The mechanical test adopts an Instron Dynatup 9250 drop hammer type impact tester, the impact head is a square impact plate of 7.2550kg, the impact compression energy is 15J, and data are collected every 25 ms. Specific test data are shown in table 2:
TABLE 2 impact test
Figure BDA0003807222040000041
Figure BDA0003807222040000051
As can be seen from the table 2, the material can reach 10.34kN under the impact of 15J energy and the maximum load of 0.46ms, and the material does not delaminate under the impact action and has excellent impact resistance.
Example 2
A three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material takes a three-dimensional five-direction carbon fiber three-dimensional woven prefabricated part as a reinforcement, and resin mixed liquid comprises the following components in percentage by weight: MXene 2%, epoxy resin 50%, curing agent 42.5%, and ethanol 5.5%; wherein MXene is V 2 CT x 。
Specifically, in this example, the epoxy resin was JC-02A from MIFARE CHEMICAL CO., LTD, the curing agent was JC-02B from MIFARE CHEMICAL CO., LTD, MXene was a monolayer V from North Korea Sourchin science CO., LTD 2 CT x The carbon fiber is a T300 carbon fiber produced by Dongli, japan.
The embodiment also provides a preparation method of the three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material, which comprises the following steps:
(1) Preparing a woven three-dimensional five-way prefabricated member by using a four-step weaving process;
(2) Diluting 50g of epoxy resin with 15g of ethanol solution;
(3) Adding 2g of V into the diluted epoxy resin obtained in the step (2) 2 CT x Filling and uniformly dispersing to obtain an electromagnetic shielding filling dispersion liquid;
(4) Performing constant-temperature magnetic stirring on the electromagnetic shielding filler dispersion liquid obtained in the step (3) at 25 ℃, and performing ultrasonic treatment with the frequency of 40KHz and the time of 30 min;
(5) Heating the ultrasonic electromagnetic shielding filler dispersion liquid obtained in the step (4) to volatilize most of the thinner, and adding 42.5g of JC-02B curing agent into the thinner to be uniformly mixed;
(6) Placing the electromagnetic shielding filler dispersion liquid obtained in the step (5) after the curing agent is added into a vacuum drying oven at 60 ℃ for defoaming for 1.5h;
(7) Maintaining the temperature of the dispersion liquid at 60 ℃ and the vacuum degree at 0.1MPa, and performing resin infusion on the braided prefabricated member obtained in the step (1) by using the defoamed electromagnetic shielding filler dispersion liquid obtained in the step (6) through a vacuum-assisted resin transfer molding process;
(8) And (3) curing the woven prefabricated member which is subjected to resin infusion and obtained in the step (7) in an oven, baking for 2 hours at the temperature of 90 ℃, baking for 1 hour at the temperature of 110 ℃, and baking for 4 hours at the temperature of 130 ℃ to obtain the carbon fiber/MXene/epoxy resin electromagnetic shielding composite material.
An Agilent PAN-LN523B vector network analyzer is adopted to test the three-dimensional woven carbon fiber/MXene/epoxy resin composite material according to the waveguide method, as shown in Table 3. In the frequency range of 8.2-12.4GHZ, the maximum absorption power of the electromagnetic wave shielding can reach 0.83. In the impact test with an impact energy of 15J, the test pieces showed good impact resistance up to a maximum load of 6.67kN, as shown in Table 4.
TABLE 3 electromagnetic wave absorption Performance test
Test frequency/GHz R A
8.2 0.58 0.42
8.8 0.49 0.51
9.4 0.40 0.59
10.0 0.32 0.67
10.6 0.26 0.73
11.2 0.21 0.78
11.8 0.19 0.81
12.4 0.17 0.83
TABLE 4 impact test
Time/ms load/kN
0.00 0
0.23 6.25
0.46 6.67
0.69 5.52
0.92 5.25
1.15 5.15
1.38 5.06
1.61 4.46
1.84 4.45

Claims (10)

1. The electromagnetic shielding composite material is characterized in that porous three-dimensional woven carbon fibers are used as a reinforcement, MXene is used as filling particles, epoxy resin is used as a matrix, the MXene is communicated with circuits between adjacent carbon fiber filaments, and a three-dimensional network channel is formed in the epoxy resin.
2. The composite material of claim 1, wherein the three-dimensional woven carbon fiber structure comprises three-dimensional four-way, three-dimensional five-way, three-dimensional six-way, or three-dimensional seven-way.
3. The composite material of claim 1, wherein the MXene comprises Ti 3 C 2 T x 、V 2 CT x 、Nb 2 CT x 、Mo 2 CT x 、Nb 4 C 3 T x 、V 4 C 3 T x One or more of the above; the epoxy resin comprises one or more of resorcinol epoxy resin, glycerol epoxy resin and novolac epoxy resin.
4. A method for preparing an electromagnetic shielding composite material comprises the following steps:
(1) Preparing three-dimensional woven carbon fibers by using the carbon fibers through a weaving process;
(2) Dissolving epoxy resin in a thinner, adding MXene, and dispersing to obtain an electromagnetic shielding filler dispersion liquid;
(3) Stirring the electromagnetic shielding filler dispersion liquid in the step (2), carrying out ultrasonic treatment, heating and volatilizing the thinner, then adding a curing agent, and defoaming to obtain a resin mixed liquid;
(4) And (3) performing resin infusion on the three-dimensional woven carbon fiber in the step (1) by using the resin mixed solution in the step (3) by using a molding process, and curing to obtain the electromagnetic shielding composite material.
5. The production method according to claim 4, wherein the carbon fiber in the step (1) is a 6-24K carbon fiber; the weaving process comprises the following steps: the knitting yarns are interwoven through a four-step or two-step knitting process.
6. The preparation method according to claim 4, wherein the diluent in the step (2) comprises one or more of acetone, ethanol, toluene, xylene, ethyl acetate and dioxane.
7. The preparation method according to claim 4, wherein the resin mixed liquid component in the step (3) comprises the following components in percentage by weight: 2 to 15 percent of MXene, 40 to 50 percent of epoxy resin, 34 to 42.5 percent of curing agent and 5 to 15 percent of thinner.
8. The preparation method according to claim 4, wherein the curing agent in the step (3) comprises one or more of aliphatic amine/modified aliphatic amine curing agent, alicyclic amine/modified alicyclic amine curing agent, polyamide curing agent, aromatic amine/modified aromatic amine curing agent and phenolic amine curing agent.
9. The method according to claim 4, wherein the forming process in the step (4) includes a vacuum assisted resin transfer process, a resin transfer molding process.
10. Use of the electromagnetically shielding composite material as claimed in claim 1 in aircraft frames, skins, electronic equipment and various functional components.
CN202211000423.4A 2022-08-19 2022-08-19 Three-dimensional woven carbon fiber/MXene/epoxy resin electromagnetic shielding composite material and preparation method thereof Pending CN115433434A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101531804A (en) * 2009-04-13 2009-09-16 天津大学 Electromagnetic shielding compound material made from three-dimensional braided nickel-plated carbon fiber and epoxy resin and method for preparing same
CN109897343A (en) * 2019-04-11 2019-06-18 西北工业大学 A kind of MXene aeroge/epoxy resin electromagnetic shielding nanocomposite and preparation method thereof
US20220225550A1 (en) * 2021-01-13 2022-07-14 Research & Business Foundation Sungkyunkwan University Electromagnetic interference shielding composite and electronic device including the same

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101531804A (en) * 2009-04-13 2009-09-16 天津大学 Electromagnetic shielding compound material made from three-dimensional braided nickel-plated carbon fiber and epoxy resin and method for preparing same
CN109897343A (en) * 2019-04-11 2019-06-18 西北工业大学 A kind of MXene aeroge/epoxy resin electromagnetic shielding nanocomposite and preparation method thereof
US20220225550A1 (en) * 2021-01-13 2022-07-14 Research & Business Foundation Sungkyunkwan University Electromagnetic interference shielding composite and electronic device including the same

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
唐婷婷等: "MXene及MXene改性以及在电磁屏蔽性能上的应用", 《现代盐化工》, no. 6, pages 35 - 36 *

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