CN111155331A - Preparation method of 3D graphene cross-linked conductive cloth composite material, electromagnetic shielding material and application - Google Patents
Preparation method of 3D graphene cross-linked conductive cloth composite material, electromagnetic shielding material and application Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N7/00—Flexible sheet materials not otherwise provided for, e.g. textile threads, filaments, yarns or tow, glued on macromolecular material
- D06N7/0094—Fibrous material being coated on one surface with at least one layer of an inorganic material and at least one layer of a macromolecular material
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
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- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/0002—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate
- D06N3/0015—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof characterised by the substrate using fibres of specified chemical or physical nature, e.g. natural silk
- D06N3/0022—Glass fibres
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- D06N—WALL, FLOOR, OR LIKE COVERING MATERIALS, e.g. LINOLEUM, OILCLOTH, ARTIFICIAL LEATHER, ROOFING FELT, CONSISTING OF A FIBROUS WEB COATED WITH A LAYER OF MACROMOLECULAR MATERIAL; FLEXIBLE SHEET MATERIAL NOT OTHERWISE PROVIDED FOR
- D06N3/00—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof
- D06N3/12—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins
- D06N3/128—Artificial leather, oilcloth or other material obtained by covering fibrous webs with macromolecular material, e.g. resins, rubber or derivatives thereof with macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. gelatine proteins with silicon polymers
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- D06N2209/00—Properties of the materials
- D06N2209/04—Properties of the materials having electrical or magnetic properties
- D06N2209/048—Electromagnetic interference shielding
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- D06N2209/00—Properties of the materials
- D06N2209/10—Properties of the materials having mechanical properties
- D06N2209/103—Resistant to mechanical forces, e.g. shock, impact, puncture, flexion, shear, compression, tear
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- D06N2209/00—Properties of the materials
- D06N2209/14—Properties of the materials having chemical properties
- D06N2209/143—Inert, i.e. inert to chemical degradation, corrosion resistant
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- D06N2209/00—Properties of the materials
- D06N2209/16—Properties of the materials having other properties
- D06N2209/1685—Wear resistance
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- D06N2209/00—Properties of the materials
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Abstract
The invention discloses a preparation method of a 3D graphene crosslinked conductive fabric composite material, an electromagnetic shielding material and application thereof, wherein the composite material is of a sandwich structure, the bottom layer of the composite material is conductive fabric, the middle layer of the composite material is an electromagnetic shielding layer, the outer layer of the composite material is a corrosion-resistant and wear-resistant thin protective layer, and the electromagnetic shielding layer is formed by mutually crosslinking multi-walled carbon nanotubes through iron nanoparticles loaded on thin graphene to form a 3D graphene structure. The electromagnetic shielding material prepared by the invention has the performances of 150 ℃ high temperature resistance, corrosion resistance, flexibility, high electromagnetic shielding efficiency (30 MHz-20GHz, frequency band 60-90 dB), high heat conduction and the like, can realize heat dissipation and electromagnetic shielding in electronic equipment, and has wide application.
Description
Technical Field
The invention relates to a preparation method of a heat-conducting and electromagnetic shielding material, in particular to a preparation method and application of a 3D graphene cross-linked conductive cloth composite material, and belongs to the field of production technology and application of heat-conducting and electromagnetic shielding materials.
Background
With the development of electronic information technology, electromagnetic wave communication, detection, interference and other technologies are commonly applied, which facilitates our lives on one hand, but on the other hand, it also causes serious electromagnetic wave pollution. In order to meet the rapid development of electronic instruments in recent years, the industries such as aerospace, medical care and the like put higher demands on efficient microwave shielding materials. With the coming of the 5G era, the power consumption of consumer electronics products is getting larger and higher, and the requirements for heat dissipation are also getting higher and higher, especially the electronic devices are developing towards light weight, the weight and thickness are decreasing, the requirements for heat conduction materials are increasing, and the current heat dissipation problem has become a bottleneck restricting the development of high-power electronic devices, electric automobiles and large-scale integrated circuits. Therefore, the film material has wide application as a film material which gives consideration to both heat dissipation and electromagnetic shielding.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a thin film material which is light and thin and has electromagnetic shielding and heat dissipation functions and a preparation method thereof, thereby overcoming the defects in the prior art.
In order to achieve the purpose, the technical scheme of the invention is as follows:
a preparation method of a 3D graphene crosslinked conductive fabric composite material is characterized in that the composite material is of a sandwich structure, the bottom layer of the composite material is conductive fabric, the middle layer of the composite material is an electromagnetic shielding layer, the outer layer of the composite material is a corrosion-resistant and wear-resistant thin protective layer, the electromagnetic shielding layer is formed by mutually crosslinking multi-walled carbon nanotubes through iron nanoparticles loaded on the thin graphene to form a 3D graphene structure, the preparation method of the electromagnetic shielding layer comprises the steps of utilizing hydrothermal reaction functionalization modification of iron acetate on the thin graphene, then using a catalytic chemical deposition method to grow the crosslinked multi-walled carbon nanotube structure, then using nitrogen doping treatment to improve conductivity, and finally preparing uniform slurry through ultrasound.
Preferably, the thin protective layer uses 25-50% diluted polydimethylsiloxane ethyl acetate as the protective layer.
Preferably, the conductive cloth is 0.016TPI silver-plated conductive cloth or electroplated glass fiber cloth.
Preferably, the surface resistance of the conductive cloth is less than 0.03 ohm.
Preferably, the wear resistance of the thin protective layer meets 40000 times or more (ASTND 4966-98), the corrosion resistance is resistant to bending tests with the flexibility of 20000 times or more under weak acid and weak base environments, and the thickness dimension of the thin protective layer is not more than 0.01 mm; the wear-resistant and corrosion-resistant composite material has certain wear resistance, corrosion resistance, flexibility and light and thin characteristics.
Preferably, the thickness of the electromagnetic shielding layer is 0.1mm, the electromagnetic shielding layer is loaded by suction filtration, a protective layer is coated by a spin coating technology, and a finished product is finished by vacuum drying and final treatment, wherein the electromagnetic shielding layer has the characteristics of low density, high heat conductivity and high electric conductivity.
The 3D graphene cross-linked conductive cloth composite electromagnetic shielding material prepared by the preparation method has the thickness dimension of 0.15mm, the electromagnetic shielding frequency range of 30MHz-20GHz, the electromagnetic shielding efficiency of 60-90dB and the thermal conductivity of 500-750W/(m.K).
The electromagnetic shielding material can be applied to electromagnetic shielding in the fields of electronic product heat dissipation and electromagnetic shielding.
According to the technical scheme, the preparation method of the 3D graphene cross-linked conductive fabric composite material, the electromagnetic shielding material and the application of the electromagnetic shielding material are provided, the electromagnetic shielding material prepared by the method has the performances of 150 ℃ high temperature resistance, corrosion resistance, flexibility, high electromagnetic shielding efficiency (30 MHz-20GHz, frequency band 60-90 dB), high heat conduction and the like, and can realize heat dissipation and electromagnetic shielding in electronic equipment, and the application is wide.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a schematic structural view of the present invention;
FIG. 2 is a schematic structural view of an interlayer of the present invention.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention.
Example 1
As shown in fig. 1-2, a 3D graphene cross-linked structure was prepared: weighing 100ml of high-quality thin-layer graphene aqueous slurry (solid content is 10%), adding 2ml of ferric chloride, and adding concentrated ammonia water to adjust the pH = 10; uniformly stirring the mixed solution, putting the mixed solution into a Teflon-lined high-pressure kettle, and carrying out hydrothermal reaction for 9h at the temperature of 150 ℃ and 200 ℃; washed 3 times with suction and dried overnight in vacuo.
Adding the solid powder into a tube furnace, introducing 60sccm nitrogen gas to exhaust air, setting a heating curve at 20 ℃/min after 30min, and heating to 1000 ℃; introducing 30sccm nitrogen and 30sccm hydrogen for reduction treatment for 20 min; then introducing 10sccm methane, 20sccm hydrogen and 30sccm nitrogen to grow for 15min, and finally slowly cooling under the condition of introducing 60sccm nitrogen.
Preparing 3D graphene cross-linked conductive cloth: dispersing the prepared 3D graphene cross-linked structure by using methanol, and performing suction filtration and coating on a conductive fabric; then, polydimethylsiloxane was diluted with ethyl acetate at a ratio of 25-50%, spin-coated on a conductive cloth, and the resulting conductive cloth was dried overnight at 70 ℃.
Example 2
As shown in fig. 1-2, a 3D graphene cross-linked structure was prepared: weighing 100ml of high-quality thin-layer graphene aqueous slurry (solid content is 10%), adding 2ml of nickel nitrate, and adding concentrated ammonia water to adjust the pH = 10; uniformly stirring the mixed solution, putting the mixed solution into a Teflon-lined high-pressure kettle, and carrying out hydrothermal reaction for 9h at the temperature of 150 ℃ and 200 ℃; washed 3 times with suction and dried overnight in vacuo.
Adding the solid powder into a tube furnace, introducing 60sccm nitrogen gas to exhaust air, setting a heating curve at 20 ℃/min after 30min, and heating to 1000 ℃; introducing 30sccm nitrogen and 30sccm hydrogen for reduction treatment for 20 min; then introducing 10sccm methane, 20sccm hydrogen and 30sccm nitrogen to grow for 15min, and finally slowly cooling under the condition of introducing 60sccm nitrogen.
Preparing 3D graphene cross-linked conductive cloth: dispersing the prepared 3D graphene cross-linked structure by using methanol, and performing suction filtration and coating on a conductive fabric; then, the polydimethylsiloxane is diluted by ethyl acetate with the proportion of 25% -50%, the polydimethylsiloxane is coated on the conductive cloth in a spinning mode, and the obtained conductive cloth is dried at 70 ℃ overnight.
Example 3
As shown in fig. 1-2, a 3D graphene cross-linked structure was prepared: weighing 100ml of high-quality thin-layer graphene aqueous slurry (solid content is 10%), adding 2ml of ferric chloride, and adding concentrated ammonia water to adjust the pH = 10; the mixed solution is evenly stirred and put into a Teflon-lined high-pressure kettle, hydrothermal reaction is carried out for 9h at the temperature of 150 ℃ and 200 ℃, suction filtration and washing are carried out for 3 times, and vacuum drying is carried out overnight.
Adding the solid powder into a tube furnace, introducing argon of 60sccm to exhaust air, setting a heating curve at 20 ℃/min after 30min, and heating to 1000 ℃; introducing 30sccm argon and 30sccm hydrogen for reduction treatment for 20 min; then introducing 10sccm methane, 20sccm hydrogen and 30sccm argon to grow for 15min, and finally slowly cooling under the condition of introducing 60sccm argon.
Preparing 3D graphene cross-linked conductive cloth: dispersing the prepared 3D graphene cross-linked structure by using methanol, and performing suction filtration and coating on a conductive fabric; then, polydimethylsiloxane was diluted with ethyl acetate at a ratio of 25-50%, spin-coated on a conductive cloth, and the resulting conductive cloth was dried overnight at 70 ℃.
Example 4
As shown in fig. 1-2, a 3D graphene cross-linked structure was prepared: weighing 100ml of high-quality thin-layer graphene oxide aqueous slurry (solid content is 10%), adding 2ml of ferric nitrate, adding concentrated ammonia water to adjust the pH to be =10, and adding hydrazine hydrate; the mixed solution is uniformly stirred, heated and refluxed for 12 hours, washed for many times and dried for 24 hours for later use.
Adding the solid powder into a tube furnace, introducing 60sccm nitrogen gas to exhaust air, setting a heating curve at 20 ℃/min after 30min, and heating to 1000 ℃; introducing 30sccm nitrogen and 30sccm hydrogen for reduction treatment for 20 min; then introducing 10sccm methane, 20sccm hydrogen and 30sccm nitrogen to grow for 15min, and finally slowly cooling under the condition of introducing 60sccm nitrogen.
Preparing 3D graphene cross-linked conductive cloth: dispersing the prepared 3D graphene cross-linked structure by using methanol, and performing suction filtration and coating on a conductive fabric; then, polydimethylsiloxane was diluted with ethyl acetate at a ratio of 25-50%, spin-coated on a conductive cloth, and the resulting conductive cloth was dried overnight at 70 ℃.
The invention provides electromagnetic shielding and heat dissipation by utilizing the excellent electrical conductivity and heat conductivity of the thin-layer graphene. In consideration of the problem of conductivity reduction among graphene sheets, thin-layer graphene is modified, then multi-walled carbon nanotubes which are mutually crosslinked among the thin-layer graphene grow through a Catalytic Chemical Vapor Deposition (CCVD) method, the multi-walled carbon nanotubes are loaded on conductive cloth through a suction filtration method after dispersion, and finally polydimethylsiloxane or other packaging agents are coated to finish the preparation of new materials.
The composite electromagnetic shielding material disclosed by the invention has excellent performances of 150 ℃ high temperature resistance, corrosion resistance, flexibility, high electromagnetic shielding efficiency (30 MHz-20GHz, frequency band 60-90 dB), high heat conduction and the like due to a complete interlayer structure, namely an outer protective layer, an intermediate layer shielding heat conduction layer and a bottom layer conductive layer, has a unique idea that a 3D graphene cross-linking structure of the intermediate shielding heat conduction layer enables the composite electromagnetic shielding material to have a high-conductivity network and a heat-conducting and heat-dissipating network, can realize both heat dissipation and electromagnetic shielding in electronic equipment, and has wide application.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (8)
1. The preparation method of the 3D graphene crosslinked conductive fabric composite material is characterized in that the composite material is of a sandwich structure, the bottom layer of the composite material is conductive fabric, the middle layer of the composite material is an electromagnetic shielding layer, the outer layer of the composite material is a corrosion-resistant and wear-resistant thin protective layer, the electromagnetic shielding layer is formed by mutually crosslinking multi-walled carbon nanotubes through iron nanoparticles loaded on thin graphene to form a 3D graphene structure, the preparation method of the electromagnetic shielding layer comprises the steps of utilizing hydrothermal reaction functionalization modification of iron acetate on the thin graphene, then using a catalytic chemical deposition method to grow the crosslinked multi-walled carbon nanotube structure, improving conductivity through nitrogen doping treatment, and finally preparing uniform slurry through ultrasound.
2. The method for preparing a 3D graphene crosslinked conductive fabric composite material according to claim 1, wherein the thin protective layer uses polydimethylsiloxane diluted by 25-50% of ethyl acetate as a protective layer.
3. The preparation method of the 3D graphene crosslinked conductive fabric composite material according to claim 1, wherein the conductive fabric is 0.016TPI silver-plated conductive fabric or electroplated glass fiber fabric.
4. The preparation method of the 3D graphene cross-linked conductive fabric composite material according to claim 3, wherein the surface resistance of the conductive fabric is less than 0.03 ohm.
5. The preparation method of the 3D graphene cross-linked conductive fabric composite material according to claim 1, wherein the wear resistance of the thin protective layer is more than 40000 times (ASTND 4966-98), the corrosion resistance is more than 20000 times of bending tests in weak acid and weak base resistance, and the thickness dimension is not more than 0.01 mm.
6. The preparation method of the 3D graphene cross-linked conductive fabric composite material according to claim 1, wherein the thickness of the electromagnetic shielding layer is 0.1mm, the electromagnetic shielding layer is loaded by suction filtration, a protective layer is coated by a spin coating technology, and a finished product is finished by vacuum drying and final treatment.
7. The 3D graphene cross-linked conductive cloth composite electromagnetic shielding material prepared by the preparation method of claims 1-6 is characterized in that the thickness of the material is 0.15mm, the electromagnetic shielding frequency range is 30MHz-20GHz, the electromagnetic shielding efficiency reaches 60-90dB, and the thermal conductivity is 500-.
8. The electromagnetic shielding material of claim 7 can be applied to electromagnetic shielding in the fields of electronic product heat dissipation and electromagnetic shielding.
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Cited By (1)
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CN111793435A (en) * | 2020-07-07 | 2020-10-20 | 苏州康丽达精密电子有限公司 | EMI shielding optimized coating and preparation method thereof |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111793435A (en) * | 2020-07-07 | 2020-10-20 | 苏州康丽达精密电子有限公司 | EMI shielding optimized coating and preparation method thereof |
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