CN109370226A - A kind of preparation method of electromagnetic shielding material - Google Patents
A kind of preparation method of electromagnetic shielding material Download PDFInfo
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- CN109370226A CN109370226A CN201811239601.2A CN201811239601A CN109370226A CN 109370226 A CN109370226 A CN 109370226A CN 201811239601 A CN201811239601 A CN 201811239601A CN 109370226 A CN109370226 A CN 109370226A
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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
- C08K13/00—Use of mixtures of ingredients not covered by one single of the preceding main groups, each of these compounds being essential
- C08K13/06—Pretreated ingredients and ingredients covered by the main groups C08K3/00 - C08K7/00
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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
- C08K3/042—Graphene or derivatives, e.g. graphene oxides
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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
- C08K3/08—Metals
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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
- C08K5/00—Use of organic ingredients
- C08K5/54—Silicon-containing compounds
- C08K5/541—Silicon-containing compounds containing oxygen
- C08K5/5415—Silicon-containing compounds containing oxygen containing at least one Si—O bond
- C08K5/5419—Silicon-containing compounds containing oxygen containing at least one Si—O bond containing at least one Si—C bond
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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
- C08K9/00—Use of pretreated ingredients
- C08K9/12—Adsorbed ingredients, e.g. ingredients on carriers
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- 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
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- 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
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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
- C08K3/08—Metals
- C08K2003/0806—Silver
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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
- C08K3/08—Metals
- C08K2003/0856—Iron
Abstract
The present invention provides a kind of preparation methods of electromagnetic shielding material, comprising the following steps: mixes graphene oxide, aniline monomer and dodecylbenzenesulfonic acid solution, ultrasonic disperse;Ammonium persulfate solution is slowly added dropwise, stirs;It filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is dry;Powder after collecting drying, is put into tube furnace and is heat-treated;Modified powder is handled to obtain on the ground electrode being equably laid in low-temperature plasma processing unit;Using the electrodeposition process of constant current, Ag particle, which is carried on modified powder, must shield powder;Silicon rubber, more alkoxy silanes, modified powder and iron wire mixing are taken, is kneaded on a mill uniform;Die-filling, press cure is at disc-shaped up to electromagnetic shielding material on vulcanizing press.Electromagnetic shielding material prepared by this law is light, has very high shield effectiveness, and electromagnetic shielding performance is fine, while having extraordinary mechanics row energy.
Description
Technical field
The present invention relates to a kind of preparation methods of electromagnetic shielding material.
Background technique
Electromagnetic radiation will lead to human organ physiological barrier or injury, and electromagnetic wave can also have an impact electronic instrument.Perhaps
The electromagnetism wave energy that the electronics that more works normally, electrical equipment generate makes neighbouring electronics, electrical equipment performance decline or even can not
Work, or even cause the accident and equipment damage.Electromagnetic pollution has become worldwide public hazards, and the World Health Organization has been classified as
The fourth-largest pollution after water pollution, atmosphere pollution, noise pollution, United Nations Conference on the Human Environment have also been classified as environment
One of protection project.Therefore carry out extremely important to the research of electromagnetic shielding material and its shield effectiveness.The harm of electromagnetic wave
Following several high-power transmitting equipment, such as radio broadcasting communication, TV, radar industry, science, medicine can be substantially divided into
The intense radiation high pressure of the radio-frequency apparatus used, the intense radiation of extra high voltage network and its corona discharge electric railway electric power supply
The electromagnetic interference of the intense radiation of electric line and its spark discharge and the generation of arc discharge computer system in the process of running, core
The electromagnetic exposure etc. that the electromagnetic leakage accident that all kinds of household electrical appliance such as electric pulse field caused by exploding generate generates.And electromagnetic screen
It covers silicon rubber to have important application in fields such as high-voltage technology, electronic technology and Medical Devices, how to improve shielding
Mechanical property is also improved while energy, becomes one of the hot spot of numerous researchers' researchs.
Summary of the invention
Technical problems to be solved: providing a kind of preparation method of electromagnetic shielding material, gained electromagnetic shielding material is light,
With very high shield effectiveness, electromagnetic shielding performance is fine, while having extraordinary mechanics row energy.
Technical solution: a kind of preparation method of electromagnetic shielding material, ingredient is by weight, comprising the following steps:
(1) 2-5 parts of graphene oxides, 1-2 parts of aniline monomers and 20-40 parts are contained into the molten of 10-12 parts of dodecyl benzene sulfonic acid
Liquid mixing, ultrasonic disperse 30-60min;
(2) it is slowly added dropwise ammonium persulfate solution, stirs 10-12h, wherein ammonium persulfate and distilled water in ammonium persulfate solution
Mass volume ratio are as follows: 2-3g:60-100mL;
(3) it filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is put into vacuum oven at 50-70 DEG C of temperature
Lower dry 24-36h;
(4) powder after drying is collected, is put into tube furnace, is heat-treated under the conditions of 700-750 DEG C;
(5) it is equably laid on the ground electrode in low-temperature plasma processing unit, in supply frequency 6-8kHz, operating voltage
6-9min is handled under the conditions of 20kV, discharge power 50-60W obtains modified powder;
(6) electrodeposition process of constant current is used, Ag particle, which is carried on modified powder, must shield powder, wherein with graphite electricity
Extremely to electrode, solution 0.001-0.003mol/LAgNO3, current density 0.20-0.25mA/cm2, time 30-
40min;(7) take 100-200 parts of silicon rubber, 5-10 parts of more alkoxy silanes, 50-60 parts of modified powders and 20-30 parts of iron wires mixed
It closes, is kneaded on a mill uniform;
(8) die-filling, press cure is electromagnetically shielded material at Φ 115mm, the disc-shaped of thick 2.0-2.2mm to obtain the final product on vulcanizing press
Material.
Further, the iron wire diameter is 3-5 μm, and length is 20-30 μm.
Further, heat treatment temperature is 730 DEG C in the step (4).
Further, in the step (5) supply frequency be 7kHz, discharge power 55W.
Further, AgNO in the step (6)3The concentration of solution is 0.002mol/L, current density 0.23mA/cm2.Have
Beneficial effect:
1. metallic weight can greatly reduce quality after graphene oxide microsphere surface is silver-plated.
2. the addition of iron wire can not only increase shielding properties, while can also improve mechanical property to a certain extent.
3. through low-temperature plasma processing unit processing after, powder hole more evenly, it is more dense.
4. there is very high shield effectiveness through electromagnetic shielding material prepared by the present invention, in 2.6GHz, 3.0GHz, 3.4GHz and
Shield effectiveness is up to -113.68dB, -116.27dB, -116.95dB and -115.93dB, electromagnetic shielding performance respectively under 3.8GHz
Very well, while its tensile strength and tearing strength have also respectively reached 3.2MPa and 11.4KN/m, have extraordinary mechanics row
Energy.
Specific embodiment
Embodiment 1
A kind of preparation method of electromagnetic shielding material, ingredient is by weight, comprising the following steps:
(1) solution by 2 parts of graphene oxides, 1 part of aniline monomer and 20 parts containing 10 parts of dodecyl benzene sulfonic acid mixes, ultrasound
Disperse 30min;
(2) ammonium persulfate solution is slowly added dropwise, stirs 10h, wherein the quality of ammonium persulfate and distilled water in ammonium persulfate solution
Volume ratio are as follows: 2g:60mL;
(3) it filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is put into vacuum oven under temperature 50 C
Drying is for 24 hours;
(4) powder after drying is collected, is put into tube furnace, is heat-treated under the conditions of 700 DEG C;
(5) it is equably laid on the ground electrode in low-temperature plasma processing unit, in supply frequency 6kHz, operating voltage
6min is handled under the conditions of 20kV, discharge power 50W obtains modified powder;
(6) electrodeposition process of constant current is used, Ag particle, which is carried on modified powder, must shield powder, wherein with graphite electricity
Extremely to electrode, solution 0.001mol/LAgNO3, current density 0.20mA/cm2, time 30min;
(7) 100 parts of silicon rubber, alkoxy silane more than 5 parts, 50 parts of modified powders and 20 parts of iron wire mixing are taken, are mixed on a mill
Refining is uniform;
(8) die-filling, press cure is at Φ 115mm on vulcanizing press, and the disc-shaped of thick 2.0mm is up to electromagnetic shielding material.
Embodiment 2
A kind of preparation method of electromagnetic shielding material, ingredient is by weight, comprising the following steps:
(1) solution by 3 parts of graphene oxides, 1.2 parts of aniline monomers and 25 parts containing 10.5 parts of dodecyl benzene sulfonic acid mixes,
Ultrasonic disperse 40min;
(2) ammonium persulfate solution is slowly added dropwise, stirs 10.5h, wherein the matter of ammonium persulfate and distilled water in ammonium persulfate solution
Measure volume ratio are as follows: 2g:70mL;
(3) it filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is put into vacuum oven at 55 DEG C of temperature
Dry 27h;
(4) powder after drying is collected, is put into tube furnace, is heat-treated under the conditions of 710 DEG C;
(5) it is equably laid on the ground electrode in low-temperature plasma processing unit, in supply frequency 6kHz, operating voltage
7min is handled under the conditions of 20kV, discharge power 55W obtains modified powder;
(6) electrodeposition process of constant current is used, Ag particle, which is carried on modified powder, must shield powder, wherein with graphite electricity
Extremely to electrode, solution 0.0015mol/LAgNO3, current density 0.22mA/cm2, time 35min;
(7) 120 parts of silicon rubber, alkoxy silane more than 6 parts, 52 parts of modified powders and 22 parts of iron wire mixing are taken, are mixed on a mill
Refining is uniform;
(8) die-filling, press cure is at Φ 115mm on vulcanizing press, and the disc-shaped of thick 2.1mm is up to electromagnetic shielding material.
Embodiment 3
A kind of preparation method of electromagnetic shielding material, ingredient is by weight, comprising the following steps:
(1) solution by 4 parts of graphene oxides, 1.5 parts of aniline monomers and 30 parts containing 11 parts of dodecyl benzene sulfonic acid mixes, and surpasses
Sound disperses 45min;
(2) ammonium persulfate solution is slowly added dropwise, stirs 11h, wherein the quality of ammonium persulfate and distilled water in ammonium persulfate solution
Volume ratio are as follows: 2.5g:80mL;
(3) it filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is put into vacuum oven under temperature 60 C
Dry 30h;
(4) powder after drying is collected, is put into tube furnace, is heat-treated under the conditions of 730 DEG C;
(5) it is equably laid on the ground electrode in low-temperature plasma processing unit, in supply frequency 7kHz, operating voltage
8min is handled under the conditions of 20kV, discharge power 55W obtains modified powder;
(6) electrodeposition process of constant current is used, Ag particle, which is carried on modified powder, must shield powder, wherein with graphite electricity
Extremely to electrode, solution 0.002mol/LAgNO3, current density 0.23mA/cm2, time 35min;
(7) 150 parts of silicon rubber, alkoxy silane more than 8 parts, 55 parts of modified powders and 25 parts of iron wire mixing are taken, are mixed on a mill
Refining is uniform;
(8) die-filling, press cure is at Φ 115mm on vulcanizing press, and the disc-shaped of thick 2.1mm is up to electromagnetic shielding material.
Embodiment 4
A kind of preparation method of electromagnetic shielding material, ingredient is by weight, comprising the following steps:
(1) solution by 4 parts of graphene oxides, 1.8 parts of aniline monomers and 35 parts containing 11.5 parts of dodecyl benzene sulfonic acid mixes,
Ultrasonic disperse 50min;
(2) ammonium persulfate solution is slowly added dropwise, stirs 11.5h, wherein the matter of ammonium persulfate and distilled water in ammonium persulfate solution
Measure volume ratio are as follows: 2.5g:90mL;
(3) it filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is put into vacuum oven at 65 DEG C of temperature
Dry 33h;
(4) powder after drying is collected, is put into tube furnace, is heat-treated under the conditions of 740 DEG C;
(5) it is equably laid on the ground electrode in low-temperature plasma processing unit, in supply frequency 7kHz, operating voltage
8min is handled under the conditions of 20kV, discharge power 55W obtains modified powder;
(6) electrodeposition process of constant current is used, Ag particle, which is carried on modified powder, must shield powder, wherein with graphite electricity
Extremely to electrode, solution 0.0025mol/LAgNO3, current density 0.24mA/cm2, time 35min;
(7) 180 parts of silicon rubber, alkoxy silane more than 8 parts, 57 parts of modified powders and 27 parts of iron wire mixing are taken, are mixed on a mill
Refining is uniform;
(8) die-filling, press cure is at Φ 115mm on vulcanizing press, and the disc-shaped of thick 2.1mm is up to electromagnetic shielding material.
Embodiment 5
A kind of preparation method of electromagnetic shielding material, ingredient is by weight, comprising the following steps:
(1) solution by 5 parts of graphene oxides, 2 parts of aniline monomers and 40 parts containing 12 parts of dodecyl benzene sulfonic acid mixes, ultrasound
Disperse 60min;
(2) ammonium persulfate solution is slowly added dropwise, stirs 12h, wherein the quality of ammonium persulfate and distilled water in ammonium persulfate solution
Volume ratio are as follows: 3g:100mL;
(3) it filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is put into vacuum oven under temperature 70 C
Dry 36h;
(4) powder after drying is collected, is put into tube furnace, is heat-treated under the conditions of 750 DEG C;
(5) it is equably laid on the ground electrode in low-temperature plasma processing unit, in supply frequency 8kHz, operating voltage
9min is handled under the conditions of 20kV, discharge power 60W obtains modified powder;
(6) electrodeposition process of constant current is used, Ag particle, which is carried on modified powder, must shield powder, wherein with graphite electricity
Extremely to electrode, solution 0.003mol/LAgNO3, current density 0.25mA/cm2, time 40min;
(7) 200 parts of silicon rubber, alkoxy silane more than 10 parts, 60 parts of modified powders and 30 parts of iron wire mixing are taken, are mixed on a mill
Refining is uniform;
(8) die-filling, press cure is at Φ 115mm on vulcanizing press, and the disc-shaped of thick 2.2mm is up to electromagnetic shielding material.
Electromagnet shield effect test: the test macro formed using AV3618 vector network analyzer and rectangular waveguide, measurement frequency range are
2.6GHz-3.8GHz。
Mechanics Performance Testing: by the tensile strength of GB/T528-2009 test sample, by tearing for GB/T529-2008 test sample
Resistance to spalling.
The electromagnet shield effect and mechanical property of 1 electromagnetic screen coating of table
There is very high shield effectiveness through electromagnetic shielding material prepared by the present invention, in 2.6GHz, 3.0GHz, 3.4GHz and
Shield effectiveness is up to -113.68dB, -116.27dB, -116.95dB and -115.93dB, electromagnetic shielding performance respectively under 3.8GHz
Very well, while its tensile strength and tearing strength have also respectively reached 3.2MPa and 11.4KN/m, have extraordinary mechanics row
Energy.
Claims (5)
1. a kind of preparation method of electromagnetic shielding material, it is characterised in that: ingredient is by weight, comprising the following steps:
(1) 2-5 parts of graphene oxides, 1-2 parts of aniline monomers and 20-40 parts are contained into the molten of 10-12 parts of dodecyl benzene sulfonic acid
Liquid mixing, ultrasonic disperse 30-60min;
(2) it is slowly added dropwise ammonium persulfate solution, stirs 10-12h, wherein ammonium persulfate and distilled water in ammonium persulfate solution
Mass volume ratio are as follows: 2-3g:60-100mL;
(3) it filters, it is colourless to filtrate with distilled water, ethanol washing product respectively, it is put into vacuum oven at 50-70 DEG C of temperature
Lower dry 24-36h;
(4) powder after drying is collected, is put into tube furnace, is heat-treated under the conditions of 700-750 DEG C;
(5) it is equably laid on the ground electrode in low-temperature plasma processing unit, in supply frequency 6-8kHz, operating voltage
6-9min is handled under the conditions of 20kV, discharge power 50-60W obtains modified powder;
(6) electrodeposition process of constant current is used, Ag particle, which is carried on modified powder, must shield powder, wherein with graphite electricity
Extremely to electrode, solution 0.001-0.003mol/LAgNO3, current density 0.20-0.25mA/cm2, time 30-
40min;
(7) 100-200 parts of silicon rubber, 5-10 parts of more alkoxy silanes, 50-60 parts of modified powders and 20-30 parts of iron wire mixing are taken,
It is kneaded on a mill uniform;
(8) die-filling, press cure is electromagnetically shielded material at Φ 115mm, the disc-shaped of thick 2.0-2.2mm to obtain the final product on vulcanizing press
Material.
2. a kind of preparation method of electromagnetic shielding material according to claim 1, it is characterised in that: the iron wire diameter is
3-5 μm, length is 20-30 μm.
3. a kind of preparation method of electromagnetic shielding material according to claim 1, it is characterised in that: in the step (4)
Heat treatment temperature is 730 DEG C.
4. a kind of preparation method of electromagnetic shielding material according to claim 1, it is characterised in that: in the step (5)
Supply frequency is 7kHz, discharge power 55W.
5. a kind of preparation method of electromagnetic shielding material according to claim 1, it is characterised in that: in the step (6)
AgNO3The concentration of solution is 0.002mol/L, current density 0.23mA/cm2。
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112143236A (en) * | 2020-09-28 | 2020-12-29 | 刘涛 | Liquid silicone rubber electromagnetic shielding material |
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CN112143236A (en) * | 2020-09-28 | 2020-12-29 | 刘涛 | Liquid silicone rubber electromagnetic shielding material |
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