CN110241613B - Flexible ultrathin high-thermal-conductivity electromagnetic shielding film and preparation method thereof - Google Patents
Flexible ultrathin high-thermal-conductivity electromagnetic shielding film and preparation method thereof Download PDFInfo
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- 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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- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
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Abstract
The invention discloses a flexible ultrathin high-heat-conductivity electromagnetic shielding film and a preparation method thereof, wherein the preparation method comprises the following steps: (1) preparing porous carbon fiber non-woven fabric: (2) respectively placing graphene and resin in a solvent, heating and stirring in a water bath to obtain a graphene solution and a resin solution, mixing the graphene solution and the resin solution, and heating and ultrasonically treating to obtain a mixed solution; (3) and (3) putting the porous carbon fiber non-woven fabric prepared in the step (1) into the mixed solution in the step (2), and drying to obtain the flexible ultrathin high-heat-conductivity electromagnetic shielding film. The high-thermal-conductivity high-electromagnetic-shielding thin film provided by the invention has a three-dimensional mesh interconnection structure, and comprises a porous carbon fiber non-woven fabric and a graphene filler resin matrix, wherein the porous carbon fiber non-woven fabric is uniformly embedded in the graphene filler resin matrix. The film has excellent flexibility, light weight, ultra-thin property, excellent electromagnetic shielding property, high heat conduction capability and good mechanical property.
Description
Technical Field
The invention relates to the field of aerospace, wearable electronic equipment, flexible materials, electronic communication and the like which need electromagnetic protection, in particular to a high-heat-conductivity electromagnetic shielding film and a preparation method thereof.
Background
The development of science and technology is rapidly advanced, and various electronic and electrical devices such as cellular base stations, wireless devices, smart phones, palm computers and the like bring great convenience to the lives of people. However, these electronic and electrical devices also generate significant electromagnetic radiation, which not only interferes with the proper operation of the surrounding devices, but also causes high energy hot spots that can significantly reduce the useful life of the electronic components. With the increasing degree of digitalization and integration of electronic and electrical equipment, the sensitivity of electronic and electrical equipment to external electromagnetic interference is increasing to meet the requirements of high speed, light weight and miniaturization. In response to these challenges, there is an urgent need for lightweight, flexible, high electromagnetic shielding materials with good thermal conductivity and sufficient mechanical strength.
At present, metal-based shielding materials have the defects of high density, poor flexibility, poor corrosion resistance, complex process, limited electromagnetic shielding efficiency range and the like, and limit the application and popularization of the metal-based shielding materials in the fields of high-end electronic products, automobiles and aerospace. Foamed materials and non-woven materials are used as common flexible electromagnetic shielding materials, but the shielding performance of the materials is insufficient, the heat conduction capability is poor, and the mechanical strength of the materials cannot meet the requirements of most fields.
Disclosure of Invention
In order to overcome the defects that the electromagnetic shielding material in the prior art is difficult to have the comprehensive properties of high heat conduction and high shielding efficiency, ultrathin flexibility, light weight and good mechanical strength, the invention aims to provide a high heat conduction and high electromagnetic shielding film with simple and environment-friendly process and excellent performance and a preparation method thereof.
The purpose of the invention is realized by at least one of the following technical solutions.
The invention provides a preparation method of a flexible ultrathin high-heat-conductivity electromagnetic shielding film, which comprises the following steps:
(1) preparing porous carbon fiber non-woven fabric:
placing carbon fibers and ES fibers in the dispersion, stirring and mixing, standing, papermaking into a felt, drying to obtain a preformed porous carbon fiber non-woven fabric, and hot-pressing the preformed porous carbon fiber non-woven fabric to obtain the porous carbon fiber non-woven fabric;
(2) respectively placing graphene and resin in a solvent, heating and stirring in a water bath to obtain a graphene solution and a resin solution, mixing the graphene solution and the resin solution, and heating and ultrasonically treating to obtain a mixed solution;
(3) and (3) putting the porous carbon fiber non-woven fabric prepared in the step (1) into the mixed solution in the step (2), and drying to obtain the flexible ultrathin high-heat-conductivity electromagnetic shielding film.
Preferably, the dispersion liquid in the step (1) is hydroxyethyl cellulose solution, and is obtained by dissolving hydroxyethyl cellulose powder in deionized water, and the density is 0.01-0.15 g/cm3(ii) a The mass ratio of the carbon fibers to the ES fibers is 0.65-1.5.
Preferably, the ratio of the total mass of the carbon fibers and the ES fibers to the volume of the dispersion in the step (1) is 0.006 to 0.008 g/ml.
Preferably, the length of the carbon fiber and the ES fiber in the step (1) is 6-10 mm.
Preferably, the stirring speed in the step (1) is 600-700 rpm; stirring for 5-10 min; standing for 5-10 min; the drying temperature is 60-80 ℃; the drying time is 0.8-1 h; the hot pressing time is 10-15 min, the hot pressing temperature is 150-170 ℃, and the hot pressing pressure is 6-10 MPa.
Preferably, the resin in step (2) is PVDF powder; the solvent is DMF.
Preferably, the temperature for heating the water bath in the step (2) is 50-60 ℃; stirring for 2-3 h; heating at 50-60 ℃ during ultrasonic treatment; the ultrasonic time is 20-24 h.
Preferably, the mass-to-volume ratio of the graphene to the solvent in the step (2) is 0.02-0.05 g/ml; the mass volume ratio of the resin to the solvent is 0.05-0.1 g/ml; the mass ratio of the graphene to the resin is 0.06-0.78.
Preferably, the drying temperature in the step (3) is 80-90 ℃; the drying time is 12-18 h; the ratio of the total mass of the graphene and the resin to the total mass of the carbon fibers and the ES fibers is 6.37 to 10.67.
The invention also provides the flexible ultrathin high-thermal-conductivity electromagnetic shielding film prepared by the preparation method.
The high-thermal-conductivity high-electromagnetic-shielding thin film provided by the invention has a three-dimensional mesh interconnection structure, and comprises a porous carbon fiber non-woven fabric and a graphene filler resin matrix, wherein the porous carbon fiber non-woven fabric is uniformly embedded in the graphene filler resin matrix. The porous carbon fiber non-woven fabric is manufactured by carbon fiber and ES fiber through papermaking and hot pressing. The nanoscale two-dimensional graphene and the macroscale one-dimensional carbon fiber are combined to form a three-dimensional frame, and a high-efficiency conductive path is provided. The effect of the content of two-dimensional graphene on the crystallinity of the resin varies the high efficiency of the conductive path. The porous carbon fiber non-woven fabric is firmly bonded by hot-pressing nodes formed between the ES fibers and hot-pressing nodes formed between the ES fibers and the carbon fibers. In order to prevent the porous carbon fiber non-woven fabric from being bonded on a programmed tablet press through hot-pressing nodes in the hot-pressing process, release paper needs to be laid on two surfaces of the porous carbon fiber non-woven fabric before hot pressing.
The dispersion of the graphene is completed by two steps, namely, Van der Waals force among the graphene is destroyed through ultrasonic oscillation; secondly, introducing carbonyl on the surface of the graphene through DMF (dimethyl formamide) to be uniformly combined with fluorine groups in PVDF (polyvinylidene fluoride).
Different dosages of graphene can cause differences in the crystallinity of PVDF, thereby affecting the microstructure inside the shielding film.
Compared with the prior art, the invention has the following beneficial effects and advantages:
1) according to the porous carbon fiber non-woven fabric prepared by the papermaking hot-pressing two-step method, the ES fiber shells are mutually pressed to form hot-pressing nodes by controlling the temperature in the hot-pressing process, so that the uniform dispersion morphology of carbon fibers is kept fixed, the carbon fibers are not easily damaged after being embedded into the graphene filler resin matrix, and the efficiency and the quality are improved.
2) And uniformly dispersing the graphene in the resin solution by adopting a solution casting technology, and then orderly arranging the graphene in a three-dimensional framework of the carbon fiber.
3) The preparation method provided by the invention introduces the carbon fiber non-woven fabric, and overcomes the problem of large brittleness of the graphene filler resin matrix.
4) The electromagnetic shielding film prepared by the invention has excellent flexibility, light weight, ultra-thin property, excellent electromagnetic shielding property, strong heat conductivity and high mechanical strength.
5) The method has the advantages of simple and environment-friendly technical means, economy and feasibility, and is convenient for popularization and application.
Drawings
FIG. 1 is a schematic structural diagram of a flexible ultrathin high thermal conductivity electromagnetic shielding film prepared by an embodiment;
fig. 2 is an SEM image of the flexible ultrathin high thermal conductivity electromagnetic shielding thin film with low content of graphene, medium content of graphene, and high content of graphene respectively prepared in embodiments 1 to 3 of the present invention;
in the figure: 1-graphene; 2-chopped carbon fibers; 3-chopped ES fibers; 4-PVDF.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to specific examples.
Example 1
The embodiment provides a preparation method of a flexible ultrathin high-thermal-conductivity electromagnetic shielding film with low graphene content (5 wt.%), which comprises the following steps:
(1) preparing porous carbon fiber non-woven fabric:
chopping 0.503 g of carbon fiber and 0.754 g of ES fiber filament bundle into 6 mm long to obtain chopped carbon fiber and chopped ES fiber, placing the chopped carbon fiber and chopped ES fiber in 170 ml of hydroxyethyl cellulose solution (the solvent in the hydroxyethyl cellulose solution is deionized water, the mass of the hydroxyethyl cellulose is 1.7 g, and the volume of the solvent is 169 ml), stirring and mixing at the speed of 600 rpm for 5 minutes, standing for 5 minutes, then making into felt by a paper forming machine, placing the felt into a constant temperature drying box, drying for 1 hour at the temperature of 60 ℃ to obtain preformed porous carbon fiber non-woven fabric, placing the preformed porous carbon fiber non-woven fabric into a programmed tablet press, and carrying out hot pressing for 10 minutes at the hot pressing temperature of 150 ℃ and the hot pressing pressure of 6 MPa to obtain the porous carbon fiber non-woven fabric;
(2) respectively placing 0.463 g of graphene and 7.542 g of PVDF powder into 20 ml and 80 ml of DMF, respectively mechanically stirring for 2 hours under the heating of water bath at 50 ℃ to obtain a graphene solution and a resin solution, then mixing the graphene solution and the PVDF solution, and carrying out ultrasonic treatment for 20 hours at 60 ℃ to obtain a mixed solution;
(3) and (3) putting the porous carbon fiber non-woven fabric prepared in the step (1) into the mixed solution in the step (2), and drying the porous carbon fiber non-woven fabric in an air-blowing drying oven at 80 ℃ for 12 hours to obtain the flexible ultrathin high-heat-conductivity electromagnetic shielding film with the graphene content of 5 wt.%.
In this example, the electrical conductivity, electromagnetic shielding effectiveness, flexibility, stretchability, and thermal conductivity of the flexible ultrathin high thermal conductivity electromagnetic shielding film with a graphene content of 5 wt.% were evaluated. Finally, as shown in fig. 1 and fig. 2 (a), the fibers inside the electromagnetic shielding film are uniformly dispersed, and the fibers are not pulled by the matrix flow caused by the hot pressing process to tear the carbon fiber non-woven fabric due to the connection effect of the hot pressing nodes. The film had a density of 1.5 g/cm3The thickness is 185 mu m, the material can be bent and curled randomly, the electric conductivity sigma = 6.25S/cm, the shielding effectiveness reaches 25 dB in the frequency range of 30-1500 MHz, the tensile strength can reach 53 MPa, and the thermal conductivity is about 3.75W ∙ m-1∙K-1. The results show that the flexible ultrathin high-thermal-conductivity electromagnetic shielding film with low graphene content prepared by the method has extremely high mechanical strength and excellent flexibility, but the electromagnetic shielding and thermal conductivity of the electromagnetic shielding film is even lower than that of the electromagnetic shielding film without graphene due to the weak connection interface between the fiber and the graphene resin matrix in the electromagnetic shielding film, and the electromagnetic shielding film cannot meet higher use requirements.
Example 2
The embodiment provides a preparation method of a flexible ultrathin high-thermal-conductivity electromagnetic shielding film containing medium-content graphene (about 20 wt.%), which comprises the following steps:
(1) preparing porous carbon fiber non-woven fabric:
chopping 0.503 g of carbon fiber and 0.754 g of ES fiber filament bundle into 6 mm long to obtain chopped carbon fiber and chopped ES fiber, placing the chopped carbon fiber and chopped ES fiber in 170 ml of hydroxyethyl cellulose solution (the solvent in the hydroxyethyl cellulose solution is deionized water, the mass of the hydroxyethyl cellulose is 1.7 g, and the volume of the solvent is 169 ml), stirring and mixing at the speed of 600 rpm for 5 minutes, standing for 5 minutes, then making into felt by a paper forming machine, placing the felt into a constant temperature drying box, drying for 1 hour at the temperature of 60 ℃ to obtain preformed porous carbon fiber non-woven fabric, placing the preformed porous carbon fiber non-woven fabric into a programmed tablet press, and carrying out hot pressing for 10 minutes at the hot pressing temperature of 150 ℃ and the hot pressing pressure of 6 MPa to obtain the porous carbon fiber non-woven fabric;
(2) respectively placing 2.2 g of graphene and 7.542 g of PVDF powder in 50 ml and 150 ml of DMF, respectively mechanically stirring for 2 hours under the heating of water bath at 50 ℃ to obtain a graphene solution and a resin solution, then mixing the graphene solution and the PVDF solution, and carrying out ultrasonic treatment for 22 hours at 60 ℃ to obtain a mixed solution;
(3) and (3) putting the porous carbon fiber non-woven fabric prepared in the step (1) into the mixed solution in the step (2), and drying the porous carbon fiber non-woven fabric in an air-blowing drying oven at 80 ℃ for 15 hours to obtain the flexible ultrathin high-heat-conductivity electromagnetic shielding film with the graphene content of 20 wt.%.
In this example, the electrical conductivity, electromagnetic shielding effectiveness, flexibility, stretchability, and thermal conductivity of the flexible ultrathin high thermal conductivity electromagnetic shielding film with a content of 20wt.% graphene were evaluated. Finally, as shown in fig. 1 and (b) of fig. 2, the fibers inside the electromagnetic shielding film are uniformly dispersed, and the fibers are not pulled by the matrix flow caused by the hot pressing process to tear the carbon fiber non-woven fabric due to the connection effect of the hot pressing node. The density of the electromagnetic shielding film is 1.5 g/cm3The thickness is 223 mu m, the material can be bent and curled, the electric conductivity sigma = 10.5S/cm, the shielding effectiveness can reach 32 dB in the frequency range of 30-1500 MHz, the tensile strength can reach 28 MPa, and the thermal conductivity is about 10W ∙ m-1∙K-1. The results show that the flexible ultrathin high-thermal-conductivity electromagnetic shielding film containing the graphene prepared by the method has good flexibility and mechanical properties, and the graphene resin matrix presents a porous network structure, so that the connection of the contact interface of the fiber and the graphene resin matrix is improved due to the structure, the flexible ultrathin high-thermal-conductivity electromagnetic shielding film has good electromagnetic shielding property and thermal conductivity, and is an excellent shielding material with light weight and low price.
Example 3
The embodiment provides a preparation method of a flexible ultrathin high-thermal conductivity electromagnetic shielding film with high graphene content (40 wt.%), which comprises the following steps:
(1) preparing porous carbon fiber non-woven fabric:
chopping 0.503 g of carbon fiber and 0.754 g of ES fiber filament bundle into 6 mm long to obtain chopped carbon fiber and chopped ES fiber, placing the chopped carbon fiber and chopped ES fiber in 170 ml of hydroxyethyl cellulose solution (the solvent in the hydroxyethyl cellulose solution is deionized water, the mass of the hydroxyethyl cellulose is 1.7 g, and the volume of the solvent is 169 ml), stirring and mixing at the speed of 600 rpm for 5 minutes, standing for 5 minutes, then making into felt by a paper forming machine, placing the felt into a constant temperature drying box, drying for 1 hour at the temperature of 60 ℃ to obtain preformed porous carbon fiber non-woven fabric, placing the preformed porous carbon fiber non-woven fabric into a programmed tablet press, and carrying out hot pressing for 10 minutes at the hot pressing temperature of 150 ℃ and the hot pressing pressure of 6 MPa to obtain the porous carbon fiber non-woven fabric;
(2) respectively placing 5.866 g of graphene and 7.542 g of PVDF powder in 150 ml of DMF and 150 ml of DMF, respectively mechanically stirring for 2 hours under the heating of water bath at 50 ℃ to obtain a graphene solution and a resin solution, mixing the graphene solution and the PVDF solution, and carrying out ultrasonic treatment for 24 hours at 60 ℃ to obtain a mixed solution;
(3) and (3) putting the porous carbon fiber non-woven fabric prepared in the step (1) into the mixed solution in the step (2), and drying the porous carbon fiber non-woven fabric in an air-blowing drying oven at 80 ℃ for 18 hours to obtain the flexible ultrathin high-heat-conductivity electromagnetic shielding film with the graphene content of 40 wt.%.
In this example, the electrical conductivity, electromagnetic shielding effectiveness, flexibility, stretchability, and thermal conductivity of the flexible ultrathin high thermal conductivity electromagnetic shielding film with 40 wt.% graphene content were evaluated. Finally, as shown in fig. 1 and fig. 2 (c), the fibers inside the electromagnetic shielding film are uniformly dispersed, and the fibers are not pulled by the matrix flow caused by the hot pressing process to tear the carbon fiber non-woven fabric due to the connection effect of the hot pressing nodes. The density of the electromagnetic shielding film is 1.5 g/cm3And a thickness of 284 μm. Because graphite alkene content is higher, graphite alkene resin base member fragility is great, and tiny crackle can appear on the film department surface of buckling, but inside because the existence of flexible carbon fiber non-woven fabrics, the brittle fracture can not take place for the film, still has certain flexibility. The electromagnetic shielding film has conductivity of sigma = 30S/cm, and has a frequency range of 30-1500 MHzThe shielding effectiveness reaches 48 dB, the tensile strength is more than 18 MPa, and the thermal conductivity is about 25W ∙ m-1∙K-1. The results show that the flexible ultrathin high-thermal-conductivity electromagnetic shielding film with high graphene content prepared by the method has certain flexibility and mechanical strength, and the graphene resin matrix presents a layered porous network structure, so that the connection between the fibers and the graphene resin matrix is improved to a certain extent, the graphene resin matrix has better electromagnetic shielding property and thermal conductivity, and the graphene resin matrix is an excellent shielding material with light weight and low price.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any equivalent alterations, modifications or improvements made by those skilled in the art to the above-described embodiments using the technical solutions of the present invention are still within the scope of the technical solutions of the present invention.
Claims (9)
1. A preparation method of a flexible ultrathin high-thermal-conductivity electromagnetic shielding film is characterized by comprising the following steps:
(1) preparing porous carbon fiber non-woven fabric:
placing carbon fibers and ES fibers in the dispersion, stirring and mixing, standing, papermaking into a felt, drying to obtain a preformed porous carbon fiber non-woven fabric, and hot-pressing the preformed porous carbon fiber non-woven fabric to obtain the porous carbon fiber non-woven fabric;
(2) respectively placing graphene and resin in a solvent, heating and stirring in a water bath to obtain a graphene solution and a resin solution, mixing the graphene solution and the resin solution, and heating and ultrasonically treating to obtain a mixed solution;
(3) putting the porous carbon fiber non-woven fabric prepared in the step (1) into the mixed solution in the step (2), and drying to obtain a flexible ultrathin high-heat-conductivity electromagnetic shielding film;
wherein the mass-volume ratio of the graphene to the solvent in the step (2) is 0.02-0.05 g/ml; the mass volume ratio of the resin to the solvent is 0.05-0.1 g/ml; the mass ratio of the graphene to the resin is 0.06-0.78.
2. The flexible ultra-thin member of claim 1The preparation method of the heat-conducting electromagnetic shielding film is characterized in that the dispersion liquid in the step (1) is hydroxyethyl cellulose solution, and the density is 0.01-0.15 g/cm3(ii) a The mass ratio of the carbon fibers to the ES fibers is 0.65-1.5.
3. The method for preparing a flexible ultrathin electromagnetic shielding film with high thermal conductivity as claimed in claim 1, wherein the ratio of the total mass of the carbon fibers and the ES fibers to the volume of the dispersion in step (1) is 0.006-0.008 g/ml.
4. The method for preparing the flexible ultrathin high-thermal-conductivity electromagnetic shielding film according to claim 1, wherein the length of the carbon fibers and the ES fibers in the step (1) is 6-10 mm.
5. The method for preparing the flexible ultrathin high-thermal-conductivity electromagnetic shielding film according to claim 1, wherein the stirring speed in the step (1) is 600-700 rpm; stirring for 5-10 min; standing for 5-10 min; the drying temperature is 60-80 ℃; the drying time is 0.8-1 h; the hot pressing time is 10-15 min, the hot pressing temperature is 150-170 ℃, and the hot pressing pressure is 6-10 MPa.
6. The method for preparing a flexible ultrathin high-thermal-conductivity electromagnetic shielding film according to claim 1, wherein the resin in the step (2) is PVDF powder; the solvent is DMF.
7. The method for preparing the flexible ultrathin high-thermal-conductivity electromagnetic shielding film according to claim 1, wherein the temperature of water bath heating in the step (2) is 50-60 ℃; stirring for 2-3 h; heating at 50-60 ℃ during ultrasonic treatment; the ultrasonic time is 20-24 h.
8. The method for preparing the flexible ultrathin high-thermal-conductivity electromagnetic shielding film according to claim 1, wherein the drying temperature in the step (3) is 80-90 ℃; the drying time is 12-18 h; the ratio of the total mass of the graphene and the resin to the total mass of the carbon fibers and the ES fibers is 6.37 to 10.67.
9. The flexible ultra-thin high thermal conductive electromagnetic shielding film prepared by the preparation method of any one of claims 1 to 8.
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| CN113583273B (en) * | 2021-08-23 | 2022-09-30 | 四川大学 | High absorption type electromagnetic shielding composite film |
| KR20230039353A (en) * | 2021-09-14 | 2023-03-21 | 전주대학교 산학협력단 | The manufacturing method of carbon paper including graphin and the electro-maganetic shielding sheet using the same |
| CN114773080A (en) * | 2022-05-10 | 2022-07-22 | 吉林联科特种石墨材料有限公司 | Preparation method of three-in-one heat-insulating material with graphene as heat reflecting layer |
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