CN108117811B - Graphene-silicon electromagnetic shielding filler and electromagnetic shielding coating - Google Patents
Graphene-silicon electromagnetic shielding filler and electromagnetic shielding coating Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
- C09D133/04—Homopolymers or copolymers of esters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- 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
- C08K3/02—Elements
- C08K3/04—Carbon
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- 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
Abstract
The invention belongs to the field of electromagnetic shielding materials, and discloses a graphene-silicon electromagnetic shielding filler and an electromagnetic shielding coating. Adding ethyl orthosilicate into an ethanol aqueous solution, adding ammonia water as a catalyst, reacting at the temperature of 30-60 ℃ to obtain nano silicon dioxide sol, adding graphene, ultrasonically stirring and uniformly dispersing to obtain a mixed solution, and drying to obtain a nano silicon dioxide-graphene compound; and uniformly mixing the obtained nano silicon dioxide-graphene composite with magnesium powder, heating to 500-1000 ℃ for high-temperature thermal reduction reaction, washing and drying to obtain the graphene-silicon electromagnetic shielding filler. According to the invention, the graphene and the semiconductor silicon are doped and compounded, so that the conductivity of the compound is obviously improved, the electromagnetic shielding performance of the compound is further enhanced, and the adverse effect of a compound matrix in the existing composite material on the conductivity of the graphene is avoided.
Description
Technical Field
The invention belongs to the field of electromagnetic shielding materials, and particularly relates to a graphene-silicon electromagnetic shielding filler and an electromagnetic shielding coating.
Background
The electromagnetic shielding coating has a conductivity of 10-10s·cm-1Above, a coating having the ability to conduct electrical current and dissipate accumulated static charge. The coating generally contains a matrix resin, a solvent and a conductive filler, and can form an electromagnetic shielding coating on a substrate. On one hand, the electromagnetic shielding coating can prevent electromagnetic wave radiation in the environment from interfering signals of the electronic product, so that the signals of the electronic product are fidelity and stable; on the other hand, the electromagnetic wave radiation pollution of the electronic product to the environment can be prevented, and the signal of the electronic product is kept secret. The coating is used as a fluid material, has simple preparation method and low cost, can be conveniently sprayed or brushed on the surfaces of plastic products with various shapes to form conductive electromagnetic shielding coatings, thereby achieving the purpose of electromagnetic shielding and being widely applied to the fields of electronic elements and circuit board printing, building industry, transportation, military, aerospace and the like. The key component of the electromagnetic shielding coating is conductive filler, so that the development of the conductive filler with good conductivity and magnetism is the key of the high-performance electromagnetic shielding coating.
Graphene has good electromagnetic shielding performance as a carbon material with high specific surface area and high conductivity, but the graphene alone serving as a filler often cannot achieve good effect, and is generally modified or compounded. For example, patent CN 106185905A discloses a pure graphene composite electromagnetic shielding film and a preparation method thereof, and the pure graphene composite electromagnetic shielding film is obtained by assembling graphene solid microspheres, hollow microspheres and lamellar graphene oxide. Through the high-temperature annealing process, the defects of the graphene are repaired, a perfect large conjugated structure is formed, and smoothness of a graphene conductive path is guaranteed. And simultaneously, functional groups on the graphene oxide fall off to form gas in a high-temperature annealing process, and the graphene sheet layer is peeled off under the synergistic action of the graphene microspheres to form a multi-stage porous structure. The graphene base with high conductivity and the multi-stage porous structure enable the graphene film to have extremely strong electromagnetic shielding performance. But has the defects of complex preparation method and high requirement on preparation conditions. Patent CN 104169213 a discloses a metal-flake graphene powder and an electromagnetic wave shielding coating composition containing the same. This patent binds metal to the graphene flake powder to reduce contact resistance. However, metals have the defect of poor oxidation resistance, and the shielding performance is often reduced in the using process. Patent CN 105111913 a discloses a graphene/nano ferrite-based aqueous electromagnetic shielding coating and a preparation method thereof. The graphene/ferrite nanocomposite material with ferrite nanoparticles loaded on the surface of flake graphene is used as a filler. However, ferrite has poor corrosion resistance, and ferrite as an oxide has poor conductivity, and the excellent conductivity of graphene is adversely affected although the magnetic properties of the nanostructure ferrite are combined. Patent CN 105062064A discloses a graphene/polypyrrole electromagnetic shielding film and a preparation method thereof. According to the preparation method, reduction of graphene oxide and polymerization of pyrrole are achieved through reaction of pyrrole and graphene oxide, ferric trichloride is added to continue reaction and suction filtration, so that the composite material has a 'brick and mortar' structure, graphene sheets are highly ordered and uniformly dispersed in a matrix, and the conductivity is greatly improved. But the coating is a complete film layer structure and cannot be used as a specific filler to be added into other different types of shielding coatings. Patent CN 105819710A discloses a graphene/basalt composite material, and discloses that the graphene/basalt composite material can be applied to the fields of static resistance and electromagnetic shielding. But basalt has poor conductivity and has adverse effect on the excellent conductivity of graphene.
Disclosure of Invention
Aiming at the defects and shortcomings of the prior art, the invention mainly aims to provide a preparation method of a graphene-silicon electromagnetic shielding filler.
Another object of the present invention is to provide a graphene-silicon electromagnetic shielding filler prepared by the above method.
The invention also aims to provide an electromagnetic shielding coating containing the graphene-silicon electromagnetic shielding filler.
The purpose of the invention is realized by the following technical scheme:
a preparation method of a graphene-silicon electromagnetic shielding filler comprises the following preparation steps:
(1) adding ethyl orthosilicate into an ethanol aqueous solution, then adding ammonia water as a catalyst, and reacting at the temperature of 30-60 ℃ to obtain nano silicon dioxide sol;
(2) adding graphene into the nano-silica sol obtained in the step (1), ultrasonically stirring and uniformly dispersing to obtain a mixed solution, and drying to obtain a nano-silica-graphene compound;
(3) and (3) uniformly mixing the nano silicon dioxide-graphene compound obtained in the step (2) with magnesium powder, heating to 500-1000 ℃ for high-temperature thermal reduction reaction, washing and drying to obtain the graphene-silicon electromagnetic shielding filler.
Preferably, in the step (1), the mass fraction of ethanol in the ethanol aqueous solution is 60-95%, the adding amount of the ethyl orthosilicate is 2-42% of the mass of the ethanol aqueous solution, and the adding amount of the ammonia water is 0.3-6% of the mass of the ethanol aqueous solution.
Preferably, the addition amount of the graphene in the step (2) is 5-35% of the addition amount of the tetraethoxysilane.
Preferably, the drying in step (2) is freeze-drying.
Preferably, the time of the high-temperature thermal reduction reaction in the step (3) is 1-6 h.
Preferably, the washing and drying in the step (3) are acid washing, distilled water washing and vacuum drying at 50-120 ℃.
The graphene-silicon electromagnetic shielding filler is prepared by the method.
An electromagnetic shielding coating containing the graphene-silicon electromagnetic shielding filler comprises the following components in parts by weight:
preferably, the film-forming resin is acrylic resin, polyurethane resin or epoxy resin, and the solvent is one or a mixture of more than two of water, ethanol, isopropanol, acetone and ethyl acetate.
Preferably, the auxiliary agent comprises at least one of a dispersing agent, a coupling agent and a defoaming agent.
The preparation method and the obtained electromagnetic shielding filler and coating have the following advantages and beneficial effects:
(1) according to the invention, the nano-silica sol is prepared by a sol-gel method, then graphene is added for compounding, and then magnesium powder is used for high-temperature thermal reduction, so that on one hand, silica is reduced into silicon, on the other hand, the silicon and the compounded graphene form a doped structure, and the non-conductive silica is converted into a silicon semiconductor, so that the conductivity of the compound is obviously improved, the electromagnetic shielding performance of the compound is further enhanced, and the adverse effect of a compound matrix in the existing composite material on the conductivity of the graphene is avoided.
(2) The graphene-silicon electromagnetic shielding filler disclosed by the invention is good in oxidation resistance and corrosion resistance.
(3) The graphene-silicon electromagnetic shielding filler can be suitable for electromagnetic shielding coating formulas of various systems.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
The preparation method of the graphene-silicon electromagnetic shielding filler provided by the embodiment comprises the following specific preparation steps:
(1) adding 10g of tetraethoxysilane into 100g of ethanol water solution with the ethanol mass fraction of 90%, then adding 0.5g of ammonia water as a catalyst, and carrying out ultrasonic stirring reaction at the temperature of 40 ℃ to obtain nano silicon dioxide sol;
(2) adding 1g of graphene into the nano-silica sol obtained in the step (1), ultrasonically stirring and uniformly dispersing to obtain a mixed solution, and freeze-drying to obtain a nano-silica-graphene compound;
(3) and (3) uniformly mixing the nano silicon dioxide-graphene compound obtained in the step (2) with magnesium powder, placing the mixture in a carbonization furnace, heating to 700 ℃ for carrying out high-temperature thermal reduction reaction for 4 hours, washing the product with hydrochloric acid and deionized water in sequence, and then drying in vacuum at 80 ℃ to obtain the graphene-silicon electromagnetic shielding filler.
Example 2
The preparation method of the graphene-silicon electromagnetic shielding filler provided by the embodiment comprises the following specific preparation steps:
(1) adding 10g of tetraethoxysilane into 50g of ethanol water solution with the ethanol mass fraction of 75%, then adding 0.5g of ammonia water as a catalyst, and carrying out ultrasonic stirring reaction at the temperature of 50 ℃ to obtain nano silicon dioxide sol;
(2) adding 3g of graphene into the nano-silica sol obtained in the step (1), ultrasonically stirring and uniformly dispersing to obtain a mixed solution, and freeze-drying to obtain a nano-silica-graphene compound;
(3) and (3) uniformly mixing the nano silicon dioxide-graphene compound obtained in the step (2) with magnesium powder, placing the mixture in a carbonization furnace, heating to 600 ℃ for carrying out high-temperature thermal reduction reaction for 6 hours, washing the product with hydrochloric acid and deionized water in sequence, and then drying in vacuum at 80 ℃ to obtain the graphene-silicon electromagnetic shielding filler.
Example 3
The preparation method of the graphene-silicon electromagnetic shielding filler provided by the embodiment comprises the following specific preparation steps:
(1) adding 10g of tetraethoxysilane into 200g of ethanol water solution with the ethanol mass fraction of 95%, then adding 2.0g of ammonia water as a catalyst, and carrying out ultrasonic stirring reaction at the temperature of 50 ℃ to obtain nano silicon dioxide sol;
(2) adding 0.5g of graphene into the nano-silica sol obtained in the step (1), ultrasonically stirring and uniformly dispersing to obtain a mixed solution, and freeze-drying to obtain a nano-silica-graphene compound;
(3) and (3) uniformly mixing the nano silicon dioxide-graphene compound obtained in the step (2) with magnesium powder, placing the mixture in a carbonization furnace, heating to 800 ℃ for carrying out high-temperature thermal reduction reaction for 2 hours, washing the product with hydrochloric acid and deionized water in sequence, and then drying in vacuum at 100 ℃ to obtain the graphene-silicon electromagnetic shielding filler.
Example 4
The electromagnetic shielding coating comprises the following components in parts by weight:
adding the water-based acrylic acid film-forming resin into water for high-speed dispersion, then adding the graphene-silicon electromagnetic shielding filler, carrying out mechanical blending through high-speed dispersion, and then adding the silane coupling agent for high-speed dispersion and uniform mixing to obtain the electromagnetic shielding coating.
The electromagnetic shielding coating obtained in the embodiment reaches 81dB through a shielding effect test. The test result of the shielding effect of the filler prepared from the existing pure silver nano powder (30 parts) under the same condition is 70dB, which shows that the shielding effect of the filler prepared by the invention is obviously improved compared with the shielding effect of the existing pure silver nano powder. Meanwhile, a comparison experiment of adding pure graphene is set, and a shielding effect test result under the condition of the same addition amount of the graphene (30 parts by 10% to 3 parts) is 54dB, which shows that the shielding effect is remarkably improved under the condition of the same addition amount of the graphene through compounding of silicon and the graphene.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (5)
1. A preparation method of a graphene-silicon electromagnetic shielding filler is characterized by comprising the following preparation steps:
(1) adding ethyl orthosilicate into an ethanol aqueous solution, then adding ammonia water as a catalyst, and reacting at the temperature of 30-60 ℃ to obtain nano silicon dioxide sol;
(2) adding graphene into the nano-silica sol obtained in the step (1), ultrasonically stirring and uniformly dispersing to obtain a mixed solution, and drying to obtain a nano-silica-graphene compound;
(3) uniformly mixing the nano silicon dioxide-graphene compound obtained in the step (2) with magnesium powder, heating to 500-1000 ℃ for high-temperature thermal reduction reaction, washing and drying to obtain graphene-silicon electromagnetic shielding filler;
in the step (1), the mass fraction of ethanol in the ethanol water solution is 60-95%, the adding amount of the ethyl orthosilicate is 2-42% of the mass of the ethanol water solution, and the adding amount of the ammonia water is 0.3-6% of the mass of the ethanol water solution; the addition amount of the graphene in the step (2) is 5-35% of the addition amount of the tetraethoxysilane; the drying in the step (2) is freeze drying; the time of the high-temperature thermal reduction reaction in the step (3) is 1-6 h; and (3) washing and drying in the step (3) are acid washing, distilled water washing and vacuum drying at the temperature of 50-120 ℃.
2. A graphene-silicon electromagnetic shielding filler is characterized in that: prepared by the method of claim 1.
3. An electromagnetic shielding coating containing the graphene-silicon electromagnetic shielding filler according to claim 2, wherein the electromagnetic shielding coating comprises the following components in parts by weight:
4. an electromagnetic shielding paint according to claim 3, wherein: the film-forming resin is acrylic resin, polyurethane resin or epoxy resin, and the solvent is one or a mixture of more than two of water, ethanol, isopropanol, acetone and ethyl acetate.
5. An electromagnetic shielding paint according to claim 3, wherein: the auxiliary agent comprises at least one of a dispersing agent, a coupling agent and a defoaming agent.
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| CN108882107B (en) * | 2018-09-03 | 2019-09-27 | 南安松茂贸易有限公司 | A kind of sound equipment of high tone quality |
| CN109246337B (en) * | 2018-09-03 | 2021-01-29 | 小巧精密科技(南通)有限公司 | Wafer-level lens module |
| CN109251513A (en) * | 2018-09-17 | 2019-01-22 | 深圳市心版图科技有限公司 | A kind of polyurethane foamed material and its processing method of counter infrared ray radiation |
| CN109320916A (en) * | 2018-10-22 | 2019-02-12 | 安阳师范学院 | A kind of silicon substrate graphene resin conductive composite material and preparation method and application |
| CN109370338A (en) * | 2018-10-29 | 2019-02-22 | 嘉兴市海德姆智能电气有限公司 | A kind of preparation method of lightweight electromagnetic screen coating |
| CN110312330A (en) * | 2019-06-27 | 2019-10-08 | 江阴暖烯石墨烯科技有限公司 | A kind of safety electric film and preparation method thereof |
| CN113936849B (en) * | 2021-10-15 | 2022-06-14 | 四川省新都美河线缆厂 | Corrosion-resistant cable for transmitting signals |
| CN115304391A (en) * | 2022-08-16 | 2022-11-08 | 三一集团有限公司 | Graphite felt-based composite material and preparation method thereof |
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| US9728777B2 (en) * | 2013-07-26 | 2017-08-08 | Nanoteck Instruments, Inc. | Methods for mass-producing silicon nano powder and graphene-doped silicon nano powder |
| CN105161696B (en) * | 2015-07-09 | 2017-11-14 | 上海交通大学 | A kind of preparation method of graphene silicon nano composite material |
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