CN112012007A - Preparation method of flexible electromagnetic protection material with meridian-shaped bionic skin - Google Patents
Preparation method of flexible electromagnetic protection material with meridian-shaped bionic skin Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- 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
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
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Abstract
The invention discloses a preparation method of a flexible electromagnetic protection material with meridian-shaped bionic skin, belonging to the technical field of electromagnetic protection materials and comprising the following steps: carbon fiber degumming treatment, carbon fiber corona activation treatment, carbon fiber wrapping of silver nanowires and wrapping of MXene materials to obtain the carbon fiber-silver nanowires-MXene composite material, wherein the outer silver nanowire-MXene wrapping layer is the vein-shaped bionic skin. The corona method is adopted to activate the surface of the carbon fiber, so that structural damage can not be generated, and C-C bonds can be broken, so that the surface activation uniformity of the carbon fiber is better; the venous silver nanowire conductive network is attached to the surface of the carbon fiber, and the carbon fiber and the silver nanowires are laminated and wrapped by the MXene two-dimensional material with excellent conductivity to form a leaf surface shape, so that the obtained carbon fiber-silver nanowire-MXene composite material is the flexible electromagnetic protection material with the meridian bionic skin, and the overall conductivity is greatly improved while the flexibility is good.
Description
Technical Field
The invention belongs to the technical field of electromagnetic protection materials, and particularly relates to a preparation method of a flexible electromagnetic protection material with meridian-shaped bionic skin.
Background
With the development of electronic devices such as flexible displays, portable electronic devices, and large-scale integrated circuits, the electromagnetic compatibility problem and the human health problem caused by electromagnetic radiation and interference are particularly prominent while convenience is brought to the life of people. High performance electromagnetic shielding materials are an effective means to solve these problems. For the fields of future unmanned aerial vehicles, novel flexible electronic equipment and power systems, the mechanical flexibility of the material is crucial to practical application besides high electromagnetic shielding effectiveness.
At present, metals and metal alloys having high conductivity and shallow skin effect are widely used in the field of electromagnetic shielding. Despite its high shielding effectiveness, metals or alloys have the disadvantages of high density, poor flexibility, susceptibility to corrosion, etc. In recent years, conductive polymer composite materials based on fillers such as Carbon Fibers (CF), Carbon Nanotubes (CNT), Graphene (Graphene), and transition metal carbide/carbonitride (MXene) have been widely used in the field of electromagnetic shielding materials because of their advantages such as light weight, good processability, and corrosion resistance. The composite material has the difficulties of high shielding effectiveness, high strength, good flexibility and the like, which limits the practical application of the composite material in the aerospace field and integrated circuit packaging communication equipment.
Disclosure of Invention
The invention aims to provide a preparation method of a flexible electromagnetic protection material with meridian-shaped bionic skin, and aims to solve the problems that metal and metal alloy protection materials in the prior art have the defects of high shielding performance, poor flexibility and easiness in corrosion, and a conductive polymer composite material with light weight, good processability and corrosion resistance is difficult to have high shielding efficiency, high strength, good flexibility and the like.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a flexible electromagnetic protection material with a meridian-shaped bionic skin comprises the following steps:
s1: carbon fiber degumming treatment
Soaking the carbon fiber in a container filled with an acetone solution, taking out the carbon fiber, cleaning the carbon fiber with water, and drying the carbon fiber to obtain the degumming carbon fiber A1;
s2: carbon fiber corona activation treatment
Performing corona treatment on the degumming carbon fiber A1 cleaned in the step S1 to obtain a carbon fiber A2;
s3: carbon fiber-wrapped silver nanowire
Uniformly dispersing silver nanowires in an isopropanol solution, wherein the mass ratio of the silver nanowires to the isopropanol is 1-5:1000 to obtain a mixture B1, soaking the carbon fiber A2 obtained in the step S2 in the mixture B1, and drying; repeating the soaking-drying process for 1-5 times to obtain carbon fiber C1 with leaf vein structure silver nanowires attached to the surface;
s4: uniformly dispersing MXene materials in water under inert protective gas, wherein the mass ratio of MXene to water is 1-5:1000 to obtain a mixture D1, and then soaking the carbon fibers C1 obtained in the step S3 in the mixture D1 and drying; the process of soaking and drying is repeated for 1-5 times to obtain the carbon fiber-silver nanowire-MXene composite material, and the external silver nanowire-MXene coating layer is the vein-shaped bionic skin.
Preferably, step S1, step S3 and step S4 are all mixed and soaked under ultrasonic wave regulation.
Preferably, the power of the corona treatment machine in the step S2 is 100-3000W, and the corona discharge time is 30-600S.
Preferably, in step S3, the carbon fiber a2 is soaked in the mixture B1 for 10 to 100 seconds before each drying, and then is dried.
Preferably, in step S4, the carbon fiber C1 is soaked in the mixture D1 for 10 to 100 seconds before being dried each time, and then is dried.
Preferably, the inert shielding gas in step S4 is argon.
Adopt the produced beneficial effect of above-mentioned technical scheme to lie in: the method adopts a corona method to carry out activation treatment on the surface of the carbon fiber, belongs to a plasma treatment technology, and compared with the traditional roughening treatment by a liquid phase oxidation method, the corona treatment can not generate structural damage and can break C-C bonds, and the surface of the carbon fiber can be better activated by forming uniform active sites; the one-dimensional silver nanowires are uniformly attached to the surface of the carbon fiber to form a meridian-shaped conductive network, and then the carbon fiber and the silver nanowires are laminated and wrapped by the two-dimensional MXene material with excellent conductive performance to form a leaf surface shape. The CF-AgNWs-MXene composite material obtained by the method is a flexible electromagnetic protection material with meridian-like bionic skin, and has good flexibility and greatly improved integral conductivity.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is an SEM photograph of a columnar carbon fiber used in the present invention;
FIG. 2 is a schematic view of the outer shape of a columnar carbon fiber;
FIG. 3 is an SEM photograph of silver nanowires used in the present invention;
FIG. 4 is a schematic view of the shape of a columnar carbon fiber with silver nanowires attached to the surface;
FIG. 5 is an SEM photograph of a vein-like CF-AgNWs-MXene composite material of leaves in an embodiment of the present invention;
in the figure: 1-carbon fiber and 2-silver nanowire.
Detailed Description
The technical solutions in the embodiments of the present invention are 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.
Example 1:
firstly, soaking carbon fibers (shown in figure 1) in acetone under the ultrasonic vibration condition to remove photoresist, taking out the carbon fibers, washing the carbon fibers with water, and drying the carbon fibers to obtain the photoresist-removed carbon fibers A1 (shown in figure 2). Carrying out corona treatment on the cleaned carbon fiber A1 by adopting a common corona treatment machine with the power of 100W to obtain carbon fiber A2, wherein the corona discharge time is 600 s; dispersing commercial silver nanowires (shown in figure 3) in an isopropanol solution, performing ultrasonic dispersion (the mass ratio of AgNWs to isopropanol is 1:1000) to obtain a mixture B1, soaking a carbon fiber A2 in the mixture B1 for 100s, then drying, and repeating the soaking-drying process for 5 times to obtain a carbon fiber C1 with silver nanowires attached to the surface, as shown in figure 4; the method comprises the steps of dispersing commercial MXene in an aqueous solution under the inert protection atmosphere of argon through ultrasonic waves (the mass ratio of MXene to water is 1:1000) to obtain a mixture D1, soaking carbon fiber C1 in the mixture D1 for 100s, drying, repeating the process of soaking and drying for 1 time to obtain the carbon fiber-silver nanowire-MXene composite material (shown in figure 5), and obtaining the carbon fiber-silver nanowire-MXene composite material which is the flexible electromagnetic protection material with the vein-shaped bionic skin through an outer silver nanowire-MXene wrapping layer.
Example 2:
firstly, soaking carbon fibers in acetone under the ultrasonic vibration condition to remove glue, taking out the carbon fibers, washing the carbon fibers with water, and drying the carbon fibers to obtain the carbon fibers A1 with the glue removed. Carrying out corona treatment on the cleaned carbon fiber A1 by using a common corona treatment machine at the power of 500W to obtain carbon fiber A2, wherein the corona discharge time is 450 s; dispersing commercial silver nanowires in isopropanol solution, performing ultrasonic dispersion (the mass ratio of AgNWs to isopropanol is 2:1000) to obtain a mixture B1, soaking a carbon fiber A2 in the mixture B1 for 80s, drying, and repeating the soaking-drying process for 4 times to obtain a carbon fiber C1 with silver nanowires attached to the surface; ultrasonically dispersing commercial MXene in an aqueous solution (the mass ratio of MXene to water is 2:1000) under an argon inert protective atmosphere to obtain a mixture D1, then soaking carbon fiber C1 in the mixture D1 for 80s, drying, and repeating the process of soaking-drying for 2 times to obtain the carbon fiber-silver nanowire-MXene composite material, wherein the external silver nanowire-MXene coating layer is the vein-shaped bionic skin.
Example 3:
firstly, soaking carbon fibers in acetone under the ultrasonic vibration condition to remove glue, taking out the carbon fibers, washing the carbon fibers with water, and drying the carbon fibers to obtain the carbon fibers A1 with the glue removed. Carrying out corona treatment on the cleaned carbon fiber A1 by adopting a common corona treatment machine with the power of 1000W to obtain carbon fiber A2, wherein the corona discharge time is 300 s; dispersing commercial silver nanowires in isopropanol solution, performing ultrasonic dispersion (the mass ratio of AgNWs to isopropanol is 3:1000) to obtain a mixture B1, soaking carbon fibers A2 in the mixture B1 for 60s, drying, and repeating the soaking-drying process for 3 times to obtain carbon fibers C1 with silver nanowires attached to the surfaces; the method comprises the steps of dispersing commercial MXene in an aqueous solution under the inert protection atmosphere of argon through ultrasonic waves (the mass ratio of MXene to water is 3:1000) to obtain a mixture D1, soaking carbon fiber carbon fibers C1 in the mixture D1 for 60s, drying, and repeating the soaking-drying process for 3 times to obtain the carbon fiber-silver nanowire-MXene composite material, wherein the external silver nanowire-MXene coating layer is the vein-shaped bionic skin.
Example 4:
firstly, soaking carbon fibers in acetone under the ultrasonic vibration condition to remove glue, taking out the carbon fibers, washing the carbon fibers with water, and drying the carbon fibers to obtain the carbon fibers A1 with the glue removed. Carrying out corona treatment on the cleaned carbon fiber A1 by adopting a common corona treatment machine with the power of 2000W to obtain carbon fiber A2, wherein the corona discharge time is 100 s; dispersing commercial silver nanowires in isopropanol solution, performing ultrasonic dispersion (the mass ratio of AgNWs to isopropanol is 4:1000) to obtain a mixture B1, soaking the carbon fiber A2 in the mixture B1 for 35s, drying, and repeating the soaking-drying process for 4 times to obtain a carbon fiber C1 with silver nanowires attached to the surface; ultrasonically dispersing commercial MXene in an aqueous solution (the mass ratio of MXene to water is 4:1000) under an argon inert protective atmosphere to obtain a mixture D1, then soaking carbon fiber C1 in the mixture D1 for 40s, drying, and repeating the process of soaking-drying for 4 times to obtain the carbon fiber-silver nanowire-MXene composite material, wherein the external silver nanowire-MXene coating layer is the vein-shaped bionic skin.
Example 5:
firstly, soaking carbon fibers in acetone under the ultrasonic vibration condition to remove glue, taking out the carbon fibers, washing the carbon fibers with water, and drying the carbon fibers to obtain the carbon fibers A1 with the glue removed. Carrying out corona treatment on the cleaned carbon fiber A1 by adopting a common corona treatment machine at the power of 3000W to obtain carbon fiber A2, wherein the corona discharge time is 30 s; dispersing commercial silver nanowires in isopropanol solution, performing ultrasonic dispersion (the mass ratio of AgNWs to isopropanol is 5:1000) to obtain a mixture B1, soaking the carbon fiber A2 in the mixture B1 for 10s, drying, and repeating the soaking-drying process for 5 times to obtain a carbon fiber C1 with silver nanowires attached to the surface; ultrasonically dispersing commercial MXene in an aqueous solution (the mass ratio of MXene to water is 5:1000) under an argon inert protective atmosphere to obtain a mixture D1, then soaking carbon fiber C1 in the mixture D1 for 10s, drying, and repeating the process of soaking-drying for 1 time to obtain the carbon fiber-silver nanowire-MXene composite material, wherein the external silver nanowire-MXene coating layer is the vein-shaped bionic skin.
Through test comparison, the conductivity of the carbon fiber, the carbon fiber with the silver nanowire attached to the surface and the carbon fiber-silver nanowire-MXene composite material is shown in the following table:
the test data in the table show that the carbon fiber-silver nanowire-MXene composite material is obtained after activation treatment, silver nanowire wrapping and MXene material treatment, so that the overall conductivity is greatly improved, and the composite material has excellent conductivity.
In conclusion, the method adopts the corona method to activate the surface of the carbon fiber, and belongs to the plasma treatment technology compared with the traditional roughening treatment by the liquid phase oxidation method, and the plasma treatment has the advantages that the plasma treatment cannot generate structural damage, can break C-C bonds and form uniform active sites on the surface. The coarsening treatment by the traditional liquid-phase oxidation method is that the coarsening treatment by the oxidation method is generally that a coarsening liquid is prepared by ammonium persulfate and concentrated sulfuric acid according to a certain proportion, and the carbon fiber after degumming is coarsened in the coarsening liquid for different time under a constant-temperature water bath. This liquid phase oxidation treatment causes corrosion of the carbon fiber surface, resulting in a rough hollow structure. These hollow structures can become stress concentration points under the action of mechanical force, seriously attenuate the yield strength and elastic modulus of the material, and cause the reduction of mechanical properties. The invention adopts surface corona treatment, only carries out activation treatment on the molecular layer surface to the carbon fiber surface, enhances the interaction force between the carbon fiber surface and the matrix by breaking the carbon-carbon bond to form an unsaturated coordination dangling bond, and can lead the surface activation uniformity to be better, while the concentration gradient in the traditional chemical or electrochemical liquid phase treatment can cause the surface activation to be not uniform enough.
In order to further improve the conductivity of the carbon fiber, the MXene/AgNWs (silver nanowire)/carbon fiber multilayer composite material is successfully prepared on the surface of the carbon fiber substrate by a controllable synthesis and multilayer assembly method. The invention introduces the bionic structure concept into the carbon fiber surface coating technology, considering that the leaves have the meridian-like structure and show higher flexibility and mechanical strength. The invention uniformly attaches the one-dimensional silver nanowires on the surface of the carbon fiber to form meridians, and then the two-dimensional MXene material with excellent conductivity is used for laminating and wrapping the carbon fiber and the silver nanowires to form a leaf surface shape, wherein the wrapping layer is similar to the meridian-shaped bionic skin. The leaf channel-shaped structure can protect the silver nanowire conductive network and successfully introduce the MXene two-dimensional material with excellent conductivity into the composite material. By adopting the structure and the process, the CF-AgNWs-MXene composite material (namely the carbon fiber-silver nanowire-MXene composite material) has good flexibility, the integral conductivity is greatly improved, and the composite material can be widely applied to the field of electromagnetic protection.
In the description above, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and thus the present invention is not limited to the specific embodiments disclosed above.
Claims (6)
1. A preparation method of a flexible electromagnetic protection material with a meridian-shaped bionic skin is characterized by comprising the following steps:
s1: carbon fiber degumming treatment
Soaking the carbon fiber in a container filled with an acetone solution, taking out the carbon fiber, cleaning the carbon fiber with water, and drying the carbon fiber to obtain the degumming carbon fiber A1;
s2: carbon fiber corona activation treatment
Performing corona treatment on the degumming carbon fiber A1 cleaned in the step S1 to obtain a carbon fiber A2;
s3: carbon fiber-wrapped silver nanowire
Uniformly dispersing silver nanowires in an isopropanol solution, wherein the mass ratio of the silver nanowires to the isopropanol is 1-5:1000 to obtain a mixture B1, soaking the carbon fiber A2 obtained in the step S2 in the mixture B1, and drying; repeating the soaking-drying process for 1-5 times to obtain carbon fiber C1 with leaf vein structure silver nanowires attached to the surface;
s4: uniformly dispersing MXene materials in water under inert protective gas, wherein the mass ratio of MXene to water is 1-5:1000 to obtain a mixture D1, and then soaking the carbon fibers C1 obtained in the step S3 in the mixture D1 and drying; the process of soaking and drying is repeated for 1-5 times to obtain the carbon fiber-silver nanowire-MXene composite material, and the external silver nanowire-MXene coating layer is the vein-shaped bionic skin.
2. The method for preparing a flexible electromagnetic shielding material with a meridian-like bionic skin as claimed in claim 1, wherein step S1, step S3 and step S4 are all mixed and soaked under ultrasonic regulation.
3. The method for preparing a flexible electromagnetic shielding material with a simulated skin having a vein shape as claimed in claim 1, wherein the power of the corona treatment machine in step S2 is 100-3000W, and the corona discharge time is 30-600S.
4. The method for preparing a flexible electromagnetic shielding material with a meridian-like bionic skin as claimed in claim 1, wherein in step S3, the carbon fiber a2 is soaked in the mixture B1 for 10-100S before being dried each time, and then is dried.
5. The method for preparing a flexible electromagnetic shielding material with a simulated skin having a vein shape according to claim 1, wherein in step S4, the carbon fiber C1 is soaked in the mixture D1 for 10-100S before being dried each time, and then is dried.
6. The method for preparing a flexible electromagnetic shielding material with a simulated skin having a vein shape according to claim 1, wherein the inert shielding gas in step S4 is argon.
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