CN115558304B - Preparation method of ultra-light composite electromagnetic shielding material based on carbon fiber solid waste modification and insulating coating - Google Patents
Preparation method of ultra-light composite electromagnetic shielding material based on carbon fiber solid waste modification and insulating coating Download PDFInfo
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 70
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 70
- 239000000463 material Substances 0.000 title claims abstract description 22
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- 238000000576 coating method Methods 0.000 title claims abstract description 20
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 37
- 239000000243 solution Substances 0.000 claims description 35
- 238000003756 stirring Methods 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
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- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 238000009210 therapy by ultrasound Methods 0.000 claims description 10
- 239000004793 Polystyrene Substances 0.000 claims description 9
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 9
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- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 6
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 5
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims description 5
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- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 5
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 4
- KAESVJOAVNADME-UHFFFAOYSA-N Pyrrole Chemical compound C=1C=CNC=1 KAESVJOAVNADME-UHFFFAOYSA-N 0.000 claims description 4
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000006250 one-dimensional material Substances 0.000 claims description 4
- 229930040373 Paraformaldehyde Natural products 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 3
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- JRKICGRDRMAZLK-UHFFFAOYSA-L persulfate group Chemical group S(=O)(=O)([O-])OOS(=O)(=O)[O-] JRKICGRDRMAZLK-UHFFFAOYSA-L 0.000 claims description 3
- 229920002647 polyamide Polymers 0.000 claims description 3
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229920006324 polyoxymethylene Polymers 0.000 claims description 3
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 3
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- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- 229910021417 amorphous silicon Inorganic materials 0.000 claims description 2
- 229910021486 amorphous silicon dioxide Inorganic materials 0.000 claims description 2
- 238000009826 distribution Methods 0.000 claims description 2
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- 125000000524 functional group Chemical group 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 239000004417 polycarbonate Substances 0.000 claims description 2
- 229920000515 polycarbonate Polymers 0.000 claims description 2
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- 229930192474 thiophene Natural products 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 229920000747 poly(lactic acid) Polymers 0.000 claims 1
- 229920000915 polyvinyl chloride Polymers 0.000 claims 1
- 239000002699 waste material Substances 0.000 abstract description 2
- 229920000767 polyaniline Polymers 0.000 description 23
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 229910001870 ammonium persulfate Inorganic materials 0.000 description 6
- 239000010410 layer Substances 0.000 description 6
- 239000012188 paraffin wax Substances 0.000 description 6
- 239000011162 core material Substances 0.000 description 5
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CYGKLLHTPPFPHH-UHFFFAOYSA-N aniline;hydrate Chemical compound O.NC1=CC=CC=C1 CYGKLLHTPPFPHH-UHFFFAOYSA-N 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical group C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
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- OHVLMTFVQDZYHP-UHFFFAOYSA-N 1-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-2-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]ethanone Chemical compound N1N=NC=2CN(CCC=21)C(CN1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)=O OHVLMTFVQDZYHP-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- 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
Abstract
The invention discloses a preparation method of an ultra-light composite electromagnetic shielding material based on carbon fiber solid waste modification and insulating coating, which is based on one-dimensional characteristics of chopped carbon fiber waste, and combines an insulating outer coating scheme through modulation of carbon fiber surface conductivity, so that the eddy current size of the carbon fiber surface is reduced, the reverse magnetic field shielding capability is improved, and macroscopic conductive connection caused by overlapping of one-dimensional carbon fibers is avoided. The material of the invention can be directly fused with a polymer matrix used by a device, and the overall resistivity can still be kept at 10 9 ‑10 20 Higher levels of Ω·m can ensure electrical safety and performance of surrounding connectors and circuits. The invention can be applied to electromagnetic wave shielding of DC-42.5 GHz frequency band in various devices and products.
Description
Technical Field
The invention belongs to the field of electromagnetic functional materials, and particularly relates to a preparation method of an ultra-light composite electromagnetic shielding material based on carbon fiber solid waste modification and insulating coating.
Background
Electromagnetic compatibility (EMC) of electrical products has become a mandatory market admission standard for countries around the world. In the field of increasingly growing electronics and communication, electromagnetic radiation generated outside and electromagnetic interference from outside in the operation of devices have become industry pain points affecting important factors such as product performance, reliability and safety, and the problems of the electromagnetic radiation and the electromagnetic interference are spread over a plurality of key fields such as new energy automobiles, consumer electronics, intelligent internet of things products, 5G and other communication products, wearable electronics, aviation, aerospace and the like. For example, in a new energy automobile, multiple frequency band electromagnetic waves generated by densely distributed three-electric systems are mutually overlapped, so that the failure of a vehicle driving system and a sensor is extremely easy to cause, and the driving safety is threatened; electromagnetic emission of electronic components in an aircraft can affect the operation of radar, communication and sensing systems, resulting in flight safety accidents; the intelligent internet of things system receives interference of external stray signals, so that the sensor and the receiver are distorted, linkage of multiple devices is affected, and even the internet of things collapses and the like. Therefore, the key technology of ultra-light high-efficiency electromagnetic shielding material is needed to be solved in response to the development of miniaturized integrated devices.
The electromagnetic shielding materials applied at present are mainly concentrated in the frequency band of 1-18GHz, particularly 8-12GHz (X-band) and 5G frequency band (C-band), and the electromagnetic shielding materials suitable for a wide frequency range are few. The electromagnetic shielding mode aiming at the microwave frequency band is mainly conductive shielding, namely, the reverse magnetic field generated by the electromagnetic induction effect of the conductor in the microwave counteracts the entry and influence of the external electromagnetic field. Related products and devices in industry mainly adopt a metal conductive shielding shell or conductive paint to perform external integral shielding. However, the shielding design difficulty of the miniaturized and miniaturized device is very high, and leakage waves still occur at key positions of connectors, connectors and the like, so that the current strict EMC standard and integration requirements cannot be met. The development of a novel insulating electromagnetic shielding material with high resistivity, which is seamlessly integrated with a device matrix, meets the requirements of electrical performance while ensuring electromagnetic performance, has been considered as a brand new solution to the EMC problem of future micro devices and special-shaped connectors.
Disclosure of Invention
Aiming at the problems of the current conductive shielding material in the application of small-sized and integrated devices, the invention aims to provide a preparation method of an ultra-light composite electromagnetic shielding material based on carbon fiber solid waste modification and insulating coating. The invention is based on the one-dimensional characteristic of the chopped carbon fiber waste, combines the modulation of the conductivity of the carbon fiber surface with the insulation outer layer coating scheme, reduces the eddy current size of the carbon fiber surface, improves the reverse magnetic field shielding capability, and avoids macroscopic conductive connection caused by the overlapping of the one-dimensional carbon fibers. The material of the invention can be directly fused with a polymer matrix used by a device, and the overall resistivity can still be kept at 10 9 -10 20 Higher levels of Ω·m can ensure electrical safety and performance of surrounding connectors and circuits. The invention can be applied to electromagnetic wave shielding of DC-42.5 GHz frequency band in various devices and products.
The preparation method of the ultra-light composite electromagnetic shielding material based on carbon fiber solid waste modification and insulating coating, disclosed by the invention, combines the insulation material coating and the chopped carbon fiber surface conductivity regulation, and cuts off macroscopic conductive transportation while enhancing microscopic electromagnetic shielding, and specifically comprises the following steps:
step 1: uniformly dispersing 0.05-3g of washed chopped carbon fiber solid waste in 20ml of absolute ethyl alcohol, adding a certain amount of dispersing agent into the solution, continuously carrying out ultrasonic treatment for 0.5-3 h, and improving the charge distribution on the surface through functional groups to uniformly disperse the carbon fiber solid waste; then carrying out suction filtration or centrifugal separation to obtain modified chopped carbon fiber powder with good polar solution dispersibility;
step 2: dispersing 0.05-3g of modified chopped carbon fiber powder obtained in the step 1 into 10-50 mL of conductive polymer monomer solution with the concentration of 0.0001-1 g/mL, stirring for 1h to be uniform, and regulating the pH value of the system to be less than or equal to 5 to obtain a precursor solution;
step 3: dropwise adding 3-10ml of initiator into the precursor solution obtained in the step (2) under continuous stirring, continuously stirring and reacting for 0.5-10 h under ice bath conditions, washing the obtained product by using distilled water and absolute ethyl alcohol, and carrying out suction filtration or centrifugal separation to obtain conductive polymer surface modified carbon fiber powder;
step 4: taking the conductive polymer surface modified carbon fiber powder obtained in the step 3, and respectively adopting the steps 4a or 4b to coat the particles with insulating amorphous silicon oxide or insulating polymer shells:
4a: uniformly dispersing the carbon fiber powder modified on the surface of the conductive polymer in a mixed solution composed of water, alcohol and ammonia water, stirring at room temperature for 0.5-2 h, slowly dripping tetraethyl orthosilicate (TEOS) into the system, and keeping the room temperature for continuous stirring reaction for 1-20 h; washing the reaction product with water and ethanol, suction filtering or centrifuging, and drying to obtain insulating amorphous SiO 2 Coated biomass carbon-based shielding material powder;
4b: uniformly dispersing carbon fiber powder modified on the surface of a conductive polymer in an insulating polymer monomer aqueous solution with the concentration of 0.05-8 mol/L, stirring for 0.5-5 h at room temperature, slowly adding an initiator into the system, continuously stirring for reaction for 1-20 h at the temperature of 0-90 ℃, washing the reaction product by water and ethanol, and carrying out suction filtration or centrifugal separation and drying to obtain the biomass carbon-based shielding material powder coated by the insulating polymer;
step 5: and (3) mixing the carbon fiber one-dimensional material coated by the insulating shell layer obtained in the step (4) with a device matrix, and forming to obtain the electromagnetic shielding material and the device with high-resistivity insulating coating.
The device matrix comprises resin, rubber, paint, colloid, paraffin and the like.
The added mass of the carbon fiber one-dimensional material coated by the insulating shell layer is 10-50% of the mass of the device matrix.
The mixing mode comprises direct mixing, banburying or open milling.
The molding method includes injection molding, extrusion molding, compression molding, blow molding, extrusion, rotational molding, coating, and the like.
In the step 1, the length of the chopped carbon fiber is 0.5-3mm, and the diameter is 2-5um.
In the step 1, the dispersing agent may be one or more of polyvinylpyrrolidone (PVP), sodium dodecyl benzene sulfonate (SDS), sodium Dodecyl Benzene Sulfonate (SDBS), KH550, polyethylene glycol (PEG), oleic acid, tween, and the like, or other types of carbon fiber surface affinity; the addition ratio of the dispersing agent is 0.001-3mol/L.
In step 2, reagents such as hydrochloric acid, nitric acid, sulfuric acid, phosphoric acid, acetic acid, etc. can be used for adjusting the pH value.
In the step 2, the conductive polymer monomer is one or more of aniline, thiophene and pyrrole.
In step 3, the initiator is a persulfate solution of 0.02 to 4mol/L, or other agent that can cause polymerization of the monomer.
In the step 4a, the volume ratio of ammonia water (the concentration is 25-28%) to water and alcohol in the mixed solution is 1: 2-30: 25 to 60.
In the step 4a, the proportion of the conductive polymer surface modified carbon fiber powder dispersed in the mixed solution is 0.01-0.075 g/mL.
In the step 4a, the addition volume of tetraethyl orthosilicate is 2-20% of the total solution volume.
In step 4b, the insulating polymer monomer is selected from monomers constituting a polymer having a high resistivity such as Polystyrene (PS), polymethyl methacrylate (PMMA), polyphenylene sulfide (PPS), polyamide (PA), polypropylene (PP), polybutylene terephthalate (PBT), polyimide (PI), polycarbonate (PC), polyoxymethylene (POM), polyethylene (PE), polyvinyl chloride (PVC), polylactic acid (PLA), and precursor monomers of doped or derivative thereof.
In the step 4b, the proportion of the conductive polymer surface modified carbon fiber powder dispersed in the insulating polymer monomer aqueous solution is 0.01-0.075 g/mL.
In the step 4b, the initiator is persulfate or a reagent for polymerizing the monomers, and the addition volume is 1-12% of the total solution volume.
The invention has the advantages and beneficial effects that:
1. according to the invention, the carbon fiber is coated by amorphous or polymer with insulating property to form a conductive/insulating one-dimensional heterostructure, and the conductive connection outside is avoided while the effective electromagnetic shielding effect is formed inside, so that a novel insulating electromagnetic shielding matrix is constructed;
2. according to the invention, through the surface modification of the conductive polymer interlayer, the reverse magnetic fields of eddy currents in different frequency bands are modulated, so that the surface impedance and the electromagnetic shielding applicable frequency band are modulated, and the electromagnetic shielding of the DC-42.5 GHz wide application frequency band can be covered;
3. the high-resistivity composite material can be directly fused with a matrix material of a device and directly used as a product or a raw material for forming the device, so that an external metal shielding shell is replaced, the internal circuit connection is not influenced, and the mechanical property of the device can be greatly improved by the carbon fiber-based material;
4. the technology of the invention can lead the carbon fiber solid waste which is difficult to treat to obtain new application, saves the energy consumption of incineration, has extremely low process cost, saves energy, and is economical and environment-friendly.
Drawings
FIG. 1 is an SEM image of 1mm chopped carbon fibers/PANI/PS prepared in example 3; SEM morphology images show that the 0.5mm chopped carbon fiber/PANI/PS is cylindrical with the diameter of 5 mu m, the cylindrical surface is smooth and flat, the double-layer compact insulating coating of the PANI/PS is illustrated, and the notch of the shell layer can be used for coating the PANI on the surface of the carbon fiber.
FIG. 2 is a 0.5mm chopped carbon fiber/PANI/SiO prepared in example 4 2 SEM images of (2); SEM morphology image shows that 1mm chopped carbon fiber/PANI/SiO 2 The pillar shape with a diameter of 5 μm has a smooth and flat surface, which indicates PANI/SiO 2 The gap of the shell layer can be seen as PANI coated on the surface of the carbon fiber.
FIG. 3 shows the real parts of dielectric constants of samples in the frequency bands of (a) 1 to 18GHz, (b) 18 to 26.5GHz, and (c) 26.5 to 40GHz, respectively, in examples 1 to 5; examples 1-5 correspond to samples with epsilon' at a high level of 1-40GHz, where the fractional frequency range at 1-18GHz can be up to 20 or more, up to 30, indicating that there are a large number of dielectric dipoles in the biomass carbon and carbon fiber/PANI conductive cores despite the coating of the insulating shell.
FIG. 4 shows the imaginary parts of dielectric constants of the samples in the frequency bands of (a) 1 to 18GHz, (b) 18 to 26.5GHz, and (c) 26.5 to 40GHz, respectively, in examples 1-5; the values of epsilon' at 1-40GHz are also larger for the samples of examples 1-5, wherein the total frequency range reaches over 20 in the 1-40GHz frequency band, wherein the total frequency range reaches 200 and up to 500 in the 1-18GHz frequency band, indicating that the chopped carbon fibers and the chopped carbon fiber/PANI conductive cores have excellent dielectric loss performance despite the coating of the insulating shell, and the fact that the imaginary part is larger than the real part indicates that the conductive/insulating interface forms an effective shield to cause multiple reflection of electromagnetic waves inside the carbon fibers.
FIG. 5 shows the shielding effectiveness of the samples in the frequency bands of (a) 1 to 18GHz, (b) 18 to 26.5GHz, and (c) 26.5 to 40GHz, respectively, in examples 1 to 5. The SE of the high resistivity insulating samples in examples 1-5 had exceeded 10dB in the C-Ku band of 1-18GHz and the full band of 18-26.5GHz, and the SE in the partial band of 26.5-40GHz had exceeded 35dB, with the SE for example three being up to 70dB. Higher resistivity (greater than 10) in combination with the samples of examples 1-5 9 Omega.m), the biomass carbon and the biomass carbon/PANI conductive core have higher dielectric characteristics, so that excellent effective shielding for electromagnetic waves in the frequency range of 1-40GHz can be formed under the condition that the insulating shell is coated and no conductive connection exists between particles. In the graph (a), example 6 is the shielding effectiveness of carbon fiber without coating the conductive core and the insulating material, and comparing examples 1-5, it is known that the double coating of the conductive core/insulating material does not reduce the shielding effectiveness of the material.
Detailed Description
Example 1:
(1) Washing and drying 0.3g of carbon fiber solid waste with the diameter of 5 mu m and the short cutting length of 0.5mm, uniformly dispersing in 20mL of absolute ethyl alcohol, adding 1g of PVP and 0.3g of PEG into the solid waste, continuously carrying out ultrasonic treatment for 0.5h, and then carrying out suction filtration and separation;
(2) Dispersing the modified carbon fiber obtained in the step (1) in 20mL of a styrene monomer aqueous solution with the concentration of 5mol/L, dropwise adding 0.5mL of a 0.15mol/L ammonium persulfate aqueous solution into the solution under the condition of water bath stirring at 70 ℃, and continuously stirring for 3 hours; washing the product with water and absolute ethyl alcohol, and then vacuum drying for 8 hours to obtain carbon fiber/PS powder;
(3) Mixing the carbon fiber/PS powder obtained in the step (2) with paraffin wax according to the proportion of 20%, and testing electromagnetic parameters and shielding effectiveness at 1-18GHz, 18-26.5GHz and 26.5-40 GHz.
Example 2:
(1) Washing and drying 0.3g of carbon fiber solid waste with the diameter of 5 mu m and the short cutting length of 1mm, uniformly dispersing in 20mL of absolute ethyl alcohol, adding 1g of PVP and 0.3g of PEG into the solid waste, continuously carrying out ultrasonic treatment for 0.5h, and then carrying out suction filtration and separation;
(2) Dispersing the modified carbon fiber obtained in the step (1) in 20mL of absolute ethyl alcohol, adding 0.2g of PVP and 0.8mL of ammonia water into the solution, and stirring for 0.5h to be uniform; then slowly dripping 0.3ml of tetraethyl orthosilicate (TEOS) into the solution, and continuously stirring for 5 hours; washing the product with water and absolute ethyl alcohol, and then vacuum drying for 8 hours to obtain carbon fiber/SiO 2 Powder;
(3) The carbon fiber/SiO obtained in the step (2) is treated 2 The powder is mixed with paraffin wax in a proportion of 20%, and electromagnetic parameters and shielding effectiveness of the powder at 1-18GHz, 18-26.5GHz and 26.5-40GHz are tested.
Example 3:
(1) Washing and drying 0.3g of carbon fiber solid waste with the diameter of 5 mu m and the short cutting length of 0.5mm, uniformly dispersing in 20mL of absolute ethyl alcohol, adding 1g of PVP and 0.3g of PEG into the solid waste, continuously carrying out ultrasonic treatment for 0.5h, and then carrying out suction filtration and separation;
(2) Adding the modified carbon fiber powder obtained in the step (1) into 30mL of 1mol/L aniline water solution, dropwise adding 5mL of 0.2mol/L hydrochloric acid solution into the solution, and continuously performing ultrasonic treatment for 1h;
(3) Slowly dropwise adding 5ml of ammonium persulfate aqueous solution with the concentration of 1mol/L into the precursor solution in the step (2) under continuous stirring, and continuously stirring for 5 hours; washing the reaction product with water and absolute ethyl alcohol, performing suction filtration, separating and drying for 8 hours to obtain carbon fiber/PANI powder;
(4) Dispersing the carbon fiber/PANI powder obtained in the step (3) in 20mL of absolute ethyl alcohol, adding 0.2g of PVP and 0.8mL of ammonia water into the solution, and uniformly stirring; then slowly dripping 0.3ml of tetraethyl orthosilicate (TEOS) into the solution, and continuously stirring for 5 hours; washing the product with water and absolute ethyl alcohol, and then vacuum drying for 8 hours to obtain the carbon fiber/PANI/SiO 2 Powder;
(5) The carbon fiber/PANI/SiO obtained in the step (4) is treated 2 The powder is mixed with paraffin wax in a proportion of 20%, and electromagnetic parameters and shielding effectiveness of the powder at 1-18GHz, 18-26.5GHz and 26.5-40GHz are tested.
Example 4:
(1) Washing and drying 0.3g of carbon fiber solid waste with the diameter of 5 mu m and the short cutting length of 1mm, uniformly dispersing in 20mL of absolute ethyl alcohol, adding 1g of PVP and 0.3g of PEG into the solid waste, continuously carrying out ultrasonic treatment for 0.5h, and then carrying out suction filtration and separation;
(2) Adding the modified carbon fiber powder obtained in the step (1) into 30mL of 1mol/L aniline water solution, dropwise adding 5mL of 0.2mol/L hydrochloric acid solution into the solution, and continuously performing ultrasonic treatment for 1h;
(3) Slowly dropwise adding 5ml of ammonium persulfate aqueous solution with the concentration of 1mol/L into the precursor solution in the step (2) under continuous stirring, and continuously stirring for 5 hours; washing the reaction product with water and absolute ethyl alcohol, performing suction filtration, separating and drying for 8 hours to obtain carbon fiber/PANI powder;
(4) Dispersing the carbon fiber/PANI powder obtained in the step (3) in 20mL of 5mol/L styrene monomer aqueous solution, dropwise adding 0.5mL of 0.15mol/L ammonium persulfate aqueous solution into the solution under the condition of water bath stirring at 70 ℃, and continuously stirring for 3h; washing the product with water and absolute ethyl alcohol, and then vacuum drying for 58 hours to obtain carbon fiber/PANI/PS powder;
(5) Mixing the carbon fiber/PANI/PS powder obtained in the step (4) with paraffin wax in a proportion of 20% for molding, and testing electromagnetic parameters and shielding effectiveness at 1-18GHz, 18-26.5GHz and 26.5-40 GHz.
Example 5:
(1) Washing and drying 0.3g of carbon fiber solid waste with the diameter of 5 mu m and the short cutting length of 3mm, uniformly dispersing in 20mL of absolute ethyl alcohol, adding 1g of PVP and 0.3g of PEG into the solid waste, continuously carrying out ultrasonic treatment for 0.5h, and then carrying out suction filtration and separation;
(2) Adding the modified carbon fiber powder obtained in the step (1) into 30mL of 1mol/L aniline water solution, dropwise adding 5mL of 0.2mol/L hydrochloric acid solution into the solution, and continuously performing ultrasonic treatment for 1h;
(3) Slowly dropwise adding 5ml of ammonium persulfate aqueous solution with the concentration of 1mol/L into the precursor solution in the step (2) under continuous stirring, and continuously stirring for 5 hours; washing the reaction product with water and absolute ethyl alcohol, performing suction filtration, separating and drying for 8 hours to obtain carbon fiber/PANI powder;
(4) Dispersing the carbon fiber/PANI powder obtained in the step (3) in a mixed solution consisting of 2ml of MMA, 18ml of distilled water and 50ml of absolute ethyl alcohol, adding 0.052g of ammonium persulfate into the solution, continuously stirring for 10 hours in a water bath environment at 70 ℃, washing the product with water and the ethyl alcohol, and then drying in vacuum for 8 hours to obtain the carbon fiber/PANI/PMMA powder.
(5) Mixing the carbon fiber/PANI/PMMA powder obtained in the step (4) with paraffin wax according to the proportion of 20%, and testing electromagnetic parameters and shielding effectiveness at 1-18GHz, 18-26.5GHz and 26.5-40 GHz.
Claims (5)
1. The preparation method of the ultra-light composite electromagnetic shielding material based on carbon fiber solid waste modification and insulating coating is characterized by comprising the following steps:
step 1: uniformly dispersing 0.05-3g of washed chopped carbon fiber solid waste in 20ml of absolute ethyl alcohol, adding a dispersing agent into the solution, continuously carrying out ultrasonic treatment for 0.5-3 h, and improving the charge distribution of the surface through functional groups to uniformly disperse the carbon fiber solid waste; then carrying out suction filtration or centrifugal separation to obtain modified chopped carbon fiber powder with good polar solution dispersibility;
step 2: dispersing 0.05-3g of modified chopped carbon fiber powder obtained in the step 1 into 10-50 mL of conductive polymer monomer solution with the concentration of 0.0001-1 g/mL, stirring for 1-h until uniform, and regulating the pH value of the system to be less than or equal to 5 to obtain a precursor solution;
step 3: dropwise adding 3-10ml of initiator into the precursor solution obtained in the step (2) under continuous stirring, continuously stirring and reacting for 0.5-10 h under ice bath conditions, washing the obtained product by using distilled water and absolute ethyl alcohol, and carrying out suction filtration or centrifugal separation to obtain conductive polymer surface modified carbon fiber powder;
step 4: taking the conductive polymer surface modified carbon fiber powder obtained in the step 3, and coating the particles with insulating amorphous silicon oxide or insulating polymer shells by adopting the method of the step 4a or 4b:
4a: uniformly dispersing carbon fiber powder modified on the surface of a conductive polymer in a mixed solution composed of water, alcohol and ammonia water, stirring at room temperature for 0.5-2 h, slowly dripping tetraethyl orthosilicate into the system, and keeping the room temperature for continuous stirring reaction for 1-20 h; washing the reaction product with water and ethanol, suction filtering or centrifuging, and drying to obtain insulating amorphous SiO 2 Coated biomass carbon-based shielding material powder;
4b: uniformly dispersing carbon fiber powder modified on the surface of a conductive polymer in an insulating polymer monomer aqueous solution with the concentration of 0.05-8 mol/L, stirring for 0.5-5 h at room temperature, slowly adding an initiator into the system, continuously stirring for reaction for 1-20 h at the temperature of 0-90 ℃, washing the reaction product by water and ethanol, and carrying out suction filtration or centrifugal separation and drying to obtain the biomass carbon-based shielding material powder coated by the insulating polymer;
step 5: mixing the carbon fiber one-dimensional material coated by the insulating shell layer obtained in the step 4 with a device matrix, and forming to obtain an electromagnetic shielding material with high resistivity insulating coating;
in the step 1, the length of the chopped carbon fiber is 0.5-3mm, and the diameter is 2-5um;
in the step 2, the conductive polymer monomer is one or more of aniline, thiophene and pyrrole;
in the step 4a, the proportion of the conductive polymer surface modified carbon fiber powder dispersed in the mixed solution is 0.01-0.075 g/mL; the adding volume of the tetraethyl orthosilicate is 2-20% of the total solution volume;
in the step 4b, the proportion of the conductive polymer surface modified carbon fiber powder dispersed in the insulating polymer monomer aqueous solution is 0.01-0.075 g/mL;
in the step 5, the addition mass of the carbon fiber one-dimensional material coated by the insulating shell layer is 10-50% of the mass of the device matrix.
2. The method of manufacturing according to claim 1, characterized in that:
in the step 1, the dispersing agent is one or more of polyvinylpyrrolidone, sodium dodecyl benzene sulfonate, KH550, polyethylene glycol, oleic acid and tween; the addition ratio of the dispersing agent is 0.001-3mol/L.
3. The method of manufacturing according to claim 1, characterized in that:
in the step 3, the initiator is persulfate solution, and the addition amount is 0.02-4mol/L.
4. The method of manufacturing according to claim 1, characterized in that:
in the step 4a, the volume ratio of the ammonia water, the water and the alcohol in the mixed solution is 1: 2-30: 25-60.
5. The method of manufacturing according to claim 1, characterized in that:
in step 4b, the insulating polymer monomer is selected from the group consisting of polystyrene, polymethyl methacrylate, polyphenylene sulfide, polyamide, polypropylene, polybutylene terephthalate, polyimide, polycarbonate, polyoxymethylene, polyethylene, polyvinyl chloride, or polylactic acid.
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