CN108117811A - A kind of graphene-silicon electromagnetic shielding filler and electromagnetic screen coating - Google Patents
A kind of graphene-silicon electromagnetic shielding filler and electromagnetic screen coating Download PDFInfo
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- CN108117811A CN108117811A CN201810071818.0A CN201810071818A CN108117811A CN 108117811 A CN108117811 A CN 108117811A CN 201810071818 A CN201810071818 A CN 201810071818A CN 108117811 A CN108117811 A CN 108117811A
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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
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Abstract
The invention belongs to electromagnetic shielding material fields, disclose a kind of graphene silicon electromagnetic shielding filler and electromagnetic screen coating.Ethyl orthosilicate is added in ethanol water, ammonium hydroxide is then added in as catalyst, nano silicon dioxide sol is obtained by the reaction at a temperature of 30~60 DEG C, then graphene is added in, ultrasonic agitation is uniformly dispersed, and obtains mixed liquor, it is dry, obtain nano silicon dioxide graphene complex;Gained nano silicon dioxide graphene complex with magnesium powder is uniformly mixed, 500~1000 DEG C of progress high temperature thermal reduction reactions is warming up to, washs drying, obtain graphene silicon electromagnetic shielding filler.Graphene is doped compound by the present invention with semiconductor silicon, significantly improves the electric conductivity of compound and further enhances its capability of electromagnetic shielding, avoids adverse effect of the complex matrix in existing composite material to graphene conductive.
Description
Technical field
The invention belongs to electromagnetic shielding material fields, and in particular to a kind of graphene-silicon electromagnetic shielding filler and electromagnetic screen
Cover coating.
Background technology
Electromagnetic screen coating is electrical conductivity 10-10s·cm-1More than, there is conduction electric current and exclude accumulation electrostatic charge ability
Coating.The coating typically contains matrix resin, solvent and conductive filler, and coating for EMI shielding can be formed on base material.Electricity
On the one hand magnetic screen coating can prevent interference of the electromagenetic wave radiation to electronic product signal in environment, make the signal of electronic product
Fidelity, stabilization;On the other hand it can prevent electronic product from being polluted to the electromagenetic wave radiation of environment, protect the signal of electronic product
It is close.The coating as a kind of fluent material, have preparation method it is simple, it is of low cost, can easily spray or brush in each
The surface of plastic products of kind shape, forms conductive coating for EMI shielding, so as to achieve the purpose that electromagnetic wave shielding, extensive use
In the fields such as electronic component and wiring board printing, construction industry, transport and military affairs, aerospace.Electromagnetic screen coating it is crucial into
Point be conductive filler, thus exploitation have both satisfactory electrical conductivity and magnetism conductive filler be High Performance Shielding coating pass
Key.
Graphene is as high-specific surface area and the carbon material of high conductivity, with good capability of electromagnetic shielding, but individually
Graphene as filler be to tend not to reach good effect, generally will be to modified or compound.Such as patent CN
106185905 A disclose a kind of pure graphene composite electromagnetic screen film and preparation method thereof, solid micro- by assembling graphene
Ball, hollow microsphere and lamella graphene oxide obtain pure graphene composite electromagnetic screen film.By high-temperature annealing process, repair
Multiple graphene defect forms perfect big conjugated structure, ensure that the unimpeded of graphene conductive access.High-temperature annealing process simultaneously
So that functional group comes off to form gas on graphene oxide, graphene sheet layer, shape are removed under the synergistic effect of graphene microballoon
Into multistage cavernous structure.Highly conductive graphene-based bottom adds multistage cavernous structure so that graphene film has extremely strong electromagnetism
Shielding properties.But there are the defects of preparation method is complicated, preparation condition requirement is high for it.104169213 A of patent CN disclose one
Kind metal-flake graphite alkene powder and the electromagnetic wave shielding coating composition containing it.Metal is incorporated into sheet by the patent
Graphene powder is to reduce contact resistance.But metal there are inoxidizability it is poor the defects of, often cause to shield in use
The problem of hydraulic performance decline.105111913 A of patent CN disclose a kind of aqueous electromagnetic shielding of graphene/nanometer ferrite base and apply
Material and preparation method thereof.Graphene/ferrite nano that it uses ferrite nanometer particle to be supported on flake graphite alkene surface is multiple
Condensation material is as filler.But ferrite corrosion resistance is poor, while its electric conductivity is poor as oxide for ferrite, although with reference to
The ferritic magnetic property of nanostructured, but can have a negative impact to the excellent electric conductivity of graphene.Patent CN
105062064 A disclose a kind of graphene/polypyrrole electromagnetic shielding film and preparation method thereof.The patent is first with pyrroles and oxygen
The reaction of graphite alkene realizes the reduction of graphene oxide and the polymerization of pyrroles, and then adding in ferric trichloride, the reaction was continued, takes out
Filter makes composite material have " brick and mortar " structure, and graphene sheet layer high-sequential in the base uniformly disperses,
Realize greatly improving for electric conductivity.But itself it is a kind of complete film layer structure, specific filler can not be used as to add in
Into other different types of shielding coatings.105819710 A of patent CN disclose a kind of graphene/basalt composite material,
And it discloses it and can be applied to antistatic, electromagnetic shielding field.But basalt self-conductive is poor, the conduction excellent to graphene
Performance adversely affects.
The content of the invention
In place of above shortcoming and defect existing in the prior art, primary and foremost purpose of the invention is to provide a kind of graphite
The preparation method of alkene-silicon electromagnetic shielding filler.
Another object of the present invention is to provide a kind of graphene-silicon electromagnetic shielding being prepared by the above method to fill out
Material.
It is still another object of the present invention to provide a kind of electromagnetic shielding paintings containing above-mentioned graphene-silicon electromagnetic shielding filler
Material.
The object of the invention is achieved through the following technical solutions:
The preparation method of a kind of graphene-silicon electromagnetic shielding filler, including following preparation process:
(1) ethyl orthosilicate is added in ethanol water, then adds in ammonium hydroxide as catalyst, 30~60 DEG C of temperature
Under nano silicon dioxide sol is obtained by the reaction;
(2) graphene is added in into nano silicon dioxide sol obtained by step (1), ultrasonic agitation is uniformly dispersed, and is mixed
Liquid is closed, it is dry, obtain nano silicon dioxide-graphene complex;
(3) nano silicon dioxide-graphene complex obtained by step (2) is uniformly mixed with magnesium powder, it is warming up to 500~
1000 DEG C of progress high temperature thermal reduction reactions, wash drying, obtain graphene-silicon electromagnetic shielding filler.
Preferably, the mass fraction of ethyl alcohol is 60%~95% in ethanol water described in step (1), the positive silicic acid
The addition of ethyl ester is the 2%~42% of ethanol water quality, and the addition of the ammonium hydroxide is ethanol water quality
0.3%~6%.
Preferably, the addition of graphene described in step (2) adds in the 5%~35% of quality for ethyl orthosilicate.
Preferably, the drying described in step (2) refers to be freeze-dried.
Preferably, the time of high temperature thermal reduction reaction described in step (3) is 1~6h.
Preferably, the washing drying described in step (3) refers to successively through pickling, distillation water washing after 50~120 DEG C
At a temperature of be dried in vacuo.
A kind of graphene-silicon electromagnetic shielding filler, is prepared by the above method.
A kind of electromagnetic screen coating containing above-mentioned graphene-silicon electromagnetic shielding filler, the electromagnetic screen coating include
The component of following parts by weight:
Preferably, the film-forming resin is acrylic resin, polyurethane resin or epoxy resin, and the solvent is
Mixing more than one or both of water, ethyl alcohol, isopropanol, acetone, ethyl acetate.
Preferably, the auxiliary agent includes at least one of dispersant, coupling agent, antifoaming agent.
The preparation method of the present invention and gained electromagnetic shielding filler and coating has the following advantages that and advantageous effect:
(1) present invention prepares nano silicon dioxide sol by sol-gal process, and then addition graphene is compound, then passes through
Magnesium powder carries out high temperature thermal reduction, is on the one hand silicon by reducing silica, another aspect silicon is formed with compound graphene and adulterated
Nonconducting silica is converted into silicon semiconductor by structure, is significantly improved the electric conductivity of compound and is further enhanced
Its capability of electromagnetic shielding avoids adverse effect of the complex matrix in existing composite material to graphene conductive.
(2) graphene-silicon electromagnetic shielding filler of the invention is anti-oxidant and corrosion resistance and good.
(3) graphene-silicon electromagnetic shielding filler of the invention is applicable to the electromagnetic screen coatings of various different systems and matches somebody with somebody
Side.
Specific embodiment
With reference to embodiment, the present invention is described in further detail, but the implementation of the present invention is not limited to this.
Embodiment 1
A kind of preparation method of graphene-silicon electromagnetic shielding filler of the present embodiment, specific preparation process are as follows:
(1) 10g ethyl orthosilicates are added in the ethanol water that 100g ethyl alcohol mass fraction is 90%, then added in
0.5g ammonium hydroxide is as catalyst, and nano silicon dioxide sol is obtained by the reaction in ultrasonic agitation at a temperature of 40 DEG C;
(2) 1g graphenes are added in into nano silicon dioxide sol obtained by step (1), ultrasonic agitation is uniformly dispersed, obtains
Mixed liquor, freeze-drying, obtains nano silicon dioxide-graphene complex;
(3) nano silicon dioxide-graphene complex obtained by step (2) is uniformly mixed with magnesium powder and is placed in retort,
700 DEG C of progress high temperature thermal reduction reaction 4h are warming up to, product is washed with hydrochloric acid and deionized water be dried in vacuo after 80 DEG C successively,
Obtain graphene-silicon electromagnetic shielding filler.
Embodiment 2
A kind of preparation method of graphene-silicon electromagnetic shielding filler of the present embodiment, specific preparation process are as follows:
(1) 10g ethyl orthosilicates are added in the ethanol water that 50g ethyl alcohol mass fraction is 75%, then added in
0.5g ammonium hydroxide is as catalyst, and nano silicon dioxide sol is obtained by the reaction in ultrasonic agitation at a temperature of 50 DEG C;
(2) 3g graphenes are added in into nano silicon dioxide sol obtained by step (1), ultrasonic agitation is uniformly dispersed, obtains
Mixed liquor, freeze-drying, obtains nano silicon dioxide-graphene complex;
(3) nano silicon dioxide-graphene complex obtained by step (2) is uniformly mixed with magnesium powder and is placed in retort,
600 DEG C of progress high temperature thermal reduction reaction 6h are warming up to, product is washed with hydrochloric acid and deionized water be dried in vacuo after 80 DEG C successively,
Obtain graphene-silicon electromagnetic shielding filler.
Embodiment 3
A kind of preparation method of graphene-silicon electromagnetic shielding filler of the present embodiment, specific preparation process are as follows:
(1) 10g ethyl orthosilicates are added in the ethanol water that 200g ethyl alcohol mass fraction is 95%, then added in
2.0g ammonium hydroxide is as catalyst, and nano silicon dioxide sol is obtained by the reaction in ultrasonic agitation at a temperature of 50 DEG C;
(2) 0.5g graphenes are added in into nano silicon dioxide sol obtained by step (1), ultrasonic agitation is uniformly dispersed, obtains
To mixed liquor, freeze-drying obtains nano silicon dioxide-graphene complex;
(3) nano silicon dioxide-graphene complex obtained by step (2) is uniformly mixed with magnesium powder and is placed in retort,
800 DEG C of progress high temperature thermal reduction reaction 2h are warming up to, product is washed with hydrochloric acid and deionized water done after 100 DEG C of vacuum successively
It is dry, obtain graphene-silicon electromagnetic shielding filler.
Embodiment 4
A kind of electromagnetic screen coating of the present embodiment, the electromagnetic screen coating are made of the component of following parts by weight:
Water soluble acrylic acid film-forming resin is added to the water high speed dispersion, then adds in graphene-silicon electromagnetic shielding filler,
Mechanical blending is carried out by high speed dispersion, silane coupling agent high speed dispersion is then added in and is uniformly mixed, obtain electromagnetic screen coating.
Electromagnetic screen coating obtained by the present embodiment has reached 81dB through shield effectiveness test.With existing fine silver under equal conditions
Nano powder (30 parts) is 70dB as the shield effectiveness test result of filler, illustrates that filler obtained by the present invention is received compared to existing fine silver
The shield effectiveness of rice flour significantly improves.Simultaneously the contrast experiment for adding in pure graphene is set, using the addition of equal graphene as
The shield effectiveness test result of condition (30 parts of 10%=3 parts of *) is 54dB, illustrates the present invention by the compound of silicon and graphene,
Under conditions of equal graphene addition, shield effectiveness has obtained significant raising.
Above-described embodiment is the preferable embodiment of the present invention, but embodiments of the present invention and from above-described embodiment
Limitation, other any Spirit Essences without departing from the present invention with made under principle change, modification, replacement, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (10)
1. the preparation method of a kind of graphene-silicon electromagnetic shielding filler, it is characterised in that including following preparation process:
(1) ethyl orthosilicate is added in ethanol water, then adds in ammonium hydroxide as catalyst, at a temperature of 30~60 DEG C instead
It should obtain nano silicon dioxide sol;
(2) graphene being added in into nano silicon dioxide sol obtained by step (1), ultrasonic agitation is uniformly dispersed, and obtains mixed liquor,
It is dry, obtain nano silicon dioxide-graphene complex;
(3) nano silicon dioxide-graphene complex obtained by step (2) with magnesium powder is uniformly mixed, is warming up to 500~1000 DEG C
High temperature thermal reduction reaction is carried out, drying is washed, obtains graphene-silicon electromagnetic shielding filler.
2. a kind of preparation method of graphene-silicon electromagnetic shielding filler according to claim 1, it is characterised in that:Step
(1) mass fraction of ethyl alcohol is 60%~95% in ethanol water described in, and the addition of the ethyl orthosilicate is ethyl alcohol
The 2%~42% of aqueous solution quality, the addition of the ammonium hydroxide are the 0.3%~6% of ethanol water quality.
3. a kind of preparation method of graphene-silicon electromagnetic shielding filler according to claim 1, it is characterised in that:Step
(2) addition of graphene described in adds in the 5%~35% of quality for ethyl orthosilicate.
4. a kind of preparation method of graphene-silicon electromagnetic shielding filler according to claim 1, it is characterised in that:Step
(2) drying described in refers to be freeze-dried.
5. a kind of preparation method of graphene-silicon electromagnetic shielding filler according to claim 1, it is characterised in that:Step
(3) time of high temperature thermal reduction reaction described in is 1~6h.
6. a kind of preparation method of graphene-silicon electromagnetic shielding filler according to claim 1, it is characterised in that:Step
(3) the washing drying described in refers to be dried in vacuo at a temperature of 50~120 DEG C through pickling, distillation water washing successively.
7. a kind of graphene-silicon electromagnetic shielding filler, it is characterised in that:Pass through claim 1~6 any one of them method system
It is standby to obtain.
A kind of 8. electromagnetic screen coating of the graphene containing described in claim 7-silicon electromagnetic shielding filler, it is characterised in that institute
State the component that electromagnetic screen coating includes following parts by weight:
9. a kind of electromagnetic screen coating according to claim 8, it is characterised in that:The film-forming resin is acrylic acid tree
Fat, polyurethane resin or epoxy resin, the solvent is water, ethyl alcohol, isopropanol, acetone, one kind in ethyl acetate or two
Kind or more mixing.
10. a kind of electromagnetic screen coating according to claim 8, it is characterised in that:The auxiliary agent includes dispersant, idol
Join at least one of agent, antifoaming agent.
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Cited By (8)
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CN108882107A (en) * | 2018-09-03 | 2018-11-23 | 佛山豆萁科技有限公司 | A kind of sound equipment of high tone quality |
CN109246337A (en) * | 2018-09-03 | 2019-01-18 | 佛山豆萁科技有限公司 | A kind of wafer-level lens mould group |
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 |
CN113936849A (en) * | 2021-10-15 | 2022-01-14 | 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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CN109246337A (en) * | 2018-09-03 | 2019-01-18 | 佛山豆萁科技有限公司 | A kind of wafer-level lens mould group |
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 |
CN113936849A (en) * | 2021-10-15 | 2022-01-14 | 四川省新都美河线缆厂 | Corrosion-resistant cable for transmitting signals |
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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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