CN115160866A - Method for preparing surface modified electromagnetic shielding material by joule heat treatment - Google Patents
Method for preparing surface modified electromagnetic shielding material by joule heat treatment Download PDFInfo
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- CN115160866A CN115160866A CN202210512790.6A CN202210512790A CN115160866A CN 115160866 A CN115160866 A CN 115160866A CN 202210512790 A CN202210512790 A CN 202210512790A CN 115160866 A CN115160866 A CN 115160866A
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- 238000010438 heat treatment Methods 0.000 title claims abstract description 64
- 239000000463 material Substances 0.000 title claims abstract description 61
- 238000000034 method Methods 0.000 title claims abstract description 10
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 52
- 239000010935 stainless steel Substances 0.000 claims abstract description 52
- 239000002002 slurry Substances 0.000 claims abstract description 41
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000000758 substrate Substances 0.000 claims abstract description 17
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 11
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052721 tungsten Inorganic materials 0.000 claims abstract description 9
- 239000010937 tungsten Substances 0.000 claims abstract description 9
- 239000004744 fabric Substances 0.000 claims abstract description 8
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 claims description 52
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 39
- 239000011734 sodium Substances 0.000 claims description 39
- 239000000843 powder Substances 0.000 claims description 36
- 238000002156 mixing Methods 0.000 claims description 28
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 26
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 26
- 239000012498 ultrapure water Substances 0.000 claims description 26
- 238000004140 cleaning Methods 0.000 claims description 24
- 239000011248 coating agent Substances 0.000 claims description 24
- 238000000576 coating method Methods 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- 239000006229 carbon black Substances 0.000 claims description 13
- 239000012535 impurity Substances 0.000 claims description 13
- 239000011261 inert gas Substances 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 238000002791 soaking Methods 0.000 claims description 13
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 13
- PHIQPXBZDGYJOG-UHFFFAOYSA-N sodium silicate nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Na+].[Na+].[O-][Si]([O-])=O PHIQPXBZDGYJOG-UHFFFAOYSA-N 0.000 claims description 13
- ASTWEMOBIXQPPV-UHFFFAOYSA-K trisodium;phosphate;dodecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.[Na+].[Na+].[Na+].[O-]P([O-])([O-])=O ASTWEMOBIXQPPV-UHFFFAOYSA-K 0.000 claims description 12
- 229910052742 iron Inorganic materials 0.000 claims description 11
- 229920000642 polymer Polymers 0.000 claims description 11
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N iron oxide Inorganic materials [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 31
- 239000000203 mixture Substances 0.000 description 20
- 229940105289 carbon black Drugs 0.000 description 12
- 235000019241 carbon black Nutrition 0.000 description 12
- 229910052802 copper Inorganic materials 0.000 description 11
- 239000012459 cleaning agent Substances 0.000 description 10
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 230000002238 attenuated effect Effects 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000002800 charge carrier Substances 0.000 description 1
- 239000006255 coating slurry Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007669 thermal treatment Methods 0.000 description 1
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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
- C09D129/00—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 an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
-
- 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
- C09D5/23—Magnetisable or magnetic paints or lacquers
-
- 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
- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
-
- 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
-
- 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
- C08K2003/085—Copper
-
- 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
- C08K2003/0862—Nickel
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
-
- 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
Abstract
The invention relates to a method for preparing a surface modified electromagnetic shielding material by joule heat treatment, belonging to the technical field of material science and engineering. After the conductive and magnetic conductive slurry prepared by the method is coated on the surface of a substrate material, the electromagnetic wave absorption capacity of the conductive and magnetic conductive slurry can be remarkably improved through joule heat treatment, so that the electromagnetic shielding performance is effectively improved. The substrate material comprises stainless steel mesh, nickel mesh, tungsten mesh, carbon cloth and the like. The invention has the advantages of high efficiency, strong applicability and the like.
Description
Technical Field
The invention relates to a method for preparing a surface modified electromagnetic shielding material by joule heat treatment, belonging to the technical field of material science and engineering.
Background
Along with the deepening of social modernization, the popularity of electronic equipment is continuously improved, the rapid advancement of the 5G era and the miniaturization of high-power equipment bring intelligent revolution to human beings, the living standard of people is greatly improved, and the electromagnetic pollution caused by the intelligent revolution is increasingly serious. In order to ensure that electronic equipment does not interfere with other equipment, is not influenced by other equipment, and simultaneously protects the personal safety of equipment operators, various equipment has good electromagnetic compatibility. Electromagnetic compatibility, as well as safety, is one of the most important indicators of product quality. Security relates to personal and property, while electromagnetic compatibility relates to personal and environmental protection. The electromagnetic wave will react with the electronic device to generate the interfered phenomenon.
Electromagnetic shielding in a region of space, measures to reduce the field strength caused by certain sources. When the electromagnetic wave reaches the surface of the shielding body, the incident wave is reflected due to the impedance discontinuity on the interface of the air and the metal; the energy that enters the shield without being reflected off the surface is attenuated by the shielding material during the forward propagation in the body, so-called absorption; when the remaining energy that has not been attenuated within the shield passes to another surface of the material, it encounters a metal-air impedance discontinuity interface, which causes it to re-reflect and return back into the shield. This reflection may be multiple reflections at the interface of the two metals. In summary, the electromagnetic attenuation of electromagnetic shielding is mainly based on the reflection of electromagnetic waves and the absorption of electromagnetic waves. The shielding materials can be classified into two types according to the electromagnetic shielding principle. One is the absorption of electromagnetic waves, primarily used by military aircraft and other equipment requiring covert detection, to reduce the detectability of targets by eliminating reflections of radar signals hitting the target surface. The other is mainly reflected electromagnetic waves; its main function is to reflect radiation using charge carriers that interact directly with electromagnetic fields, and can be used in commercial and scientific electronics, antenna systems, space exploration, medical devices and personal protection.
Disclosure of Invention
1. Objects of the invention
The invention aims to provide a method for preparing a novel electromagnetic shielding material, which is characterized in that metal and metal oxide are simply and efficiently attached to a substrate material by using coating slurry, the metal and the metal oxide are tightly combined by virtue of joule heat treatment, a magnetic conduction path and a conductive path are constructed, and the electromagnetic wave shielding effect is realized from the double angles of electric shielding and magnetic shielding. The optimal proportion is researched by adjusting the concentration of metal and metal oxide in the slurry to improve the electromagnetic shielding efficiency, and the influence of the current on the electromagnetic shielding performance during joule heat treatment is researched. Meanwhile, the applicant can obtain the electromagnetic shielding performance which is equivalent to or more advantageous than the expensive substrate material by the substrate material with low cost through the technical method of the patent, can meet the requirements of various electromagnetic shielding materials, and has higher universality.
2. The invention of the technology is characterized in that
The key points of the invention are as follows:
a method for preparing a surface modified electromagnetic shielding material by Joule heat treatment is characterized by comprising the following steps:
(1) Mixing sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g was sufficiently dissolved in 500mL of ultrapure water as a deoiling liquid (solution A);
(2) Putting a plurality of substrate materials with the size of 3cm multiplied by 6cm into the solution A, soaking for 5min to remove oil stains and other impurities on the surface of the substrate materials, taking out the substrate materials, and cleaning the substrate materials by using ultrapure water, wherein the substrate materials comprise: stainless steel mesh, nickel mesh, tungsten mesh, carbon cloth, and the like;
(3) Mixing polyvinyl butyral (PVB) with absolute ethyl alcohol, and stirring with a magnetic stirrer at 50 ℃ and 600rpm for 2 hours until the solution is clear and transparent to obtain a PVB solution (solution B), wherein the concentration of the solution A is 5wt.%, 10wt.% and 15wt.%;
(4) Mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry (solution C), cu, ni and Fe in solution B 3 O 4 The concentrations of (a) are calculated individually as 5wt.%, 10wt.%, 20wt.% and 50wt.%, respectively, and the concentration of C is 50wt.%, 60wt.% and 70wt.%, respectively;
(5) Flatly coating the solution C on a substrate material, and drying the coated solution C in a vacuum drying oven to obtain a material A;
(6) Performing joule heating treatment on the material A in a glove box in an inert gas environment, wherein the voltage of the joule heating treatment is 6V, the current is 15A, 20A and 25A, the heat treatment time is 15s, and a citric acid solution with pH =3 is continuously dripped during the joule heating treatment;
(7) And after the base material is cooled to room temperature after the Joule heat treatment, taking out the base material from the glove box for testing the electromagnetic shielding performance.
(5) Attached drawings of the invention
FIG. 1 is a photograph of a Joule heat-treated stainless steel mesh coated with an electrically and magnetically conductive paste
FIG. 2 electromagnetic absorption Properties of Joule thermal treatment at different Current intensities after coating stainless Steel mesh
Examples of the invention
The following describes embodiments of the method of the invention:
example 1
And (4) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and is used for cleaning oil stains and other impurities on the surface of a stainless steel net; soaking a plurality of stainless steel meshes with the size of 3cm multiplied by 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 Is 5wt.%, the concentration of C is 50wt.%, respectively; flatly coating the slurry on a stainless steel net, and drying after coating; then, the mixture was subjected to joule heating treatment in a glove box under an inert gas atmosphere, and a citric acid solution having a pH of =3 was continuously added dropwise during the joule heating treatment, and joule heating was performedThe heat treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the stainless steel net is cooled to room temperature, the stainless steel net can be taken out from the glove box, namely the novel electromagnetic shielding material of the target.
Example 2
And (4) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and is used for cleaning oil stains and other impurities on the surface of a stainless steel net; soaking a plurality of stainless steel meshes with the size of 3cm × 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 The concentration of C is 10wt.% and the concentration of C is 60wt.%, respectively; flatly coating the slurry on a stainless steel net, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, continuously dropwise adding a citric acid solution with pH =3 during the joule heating treatment, wherein the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the stainless steel net is cooled to room temperature, the stainless steel net can be taken out from the glove box, namely the target novel electromagnetic shielding material.
Example 3
And (3) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of Joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, dodecahydrateSodium phosphate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and used for cleaning oil stains and other impurities on the surface of a stainless steel net; soaking a plurality of stainless steel meshes with the size of 3cm × 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 Respectively at a concentration of 15wt.% and a concentration of C of 70wt.%; flatly coating the slurry on a stainless steel net, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, continuously dropwise adding a citric acid solution with pH =3 during the joule heating treatment, wherein the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the stainless steel net is cooled to room temperature, the stainless steel net can be taken out from the glove box, namely the target novel electromagnetic shielding material.
Example 4
And (4) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and is used for cleaning oil stains and other impurities on the surface of a stainless steel net; soaking a plurality of stainless steel meshes with the size of 3cm multiplied by 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a 10wt.% PVB solution is prepared, and the mixture is stirred for 2 hours at the temperature of 50 ℃ and the speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 The concentration of C is 5wt.% and the concentration of C is 50wt.%, respectively; flatly coating the slurry on a stainless steel net, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, wherein a citric acid solution with the pH =3 is continuously dripped during the joule heating treatment, the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the stainless steel net is cooled to room temperature, the stainless steel net can be taken out from the glove box, namely the novel electromagnetic shielding material of the target.
Example 5
And (3) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of Joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and used for cleaning oil stains and other impurities on the surface of a stainless steel net; soaking a plurality of stainless steel meshes with the size of 3cm × 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 The concentration of C is 5wt.% and the concentration of C is 50wt.%, respectively; flatly coating the slurry on a stainless steel mesh, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, continuously dropwise adding a citric acid solution with pH =3 during the joule heating treatment, wherein the joule heating treatment voltage is 6V, the current is 20A, and the time is 15s; finally, wait for the stainless steel netAfter cooling to room temperature, the material can be taken out from the glove box, namely the target novel electromagnetic shielding material.
Example 6
And (4) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and is used for cleaning oil stains and other impurities on the surface of a stainless steel net; soaking a plurality of stainless steel meshes with the size of 3cm multiplied by 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with the concentration of 5wt.% is prepared, and the solution is stirred for 2 hours by a magnetic stirrer at the temperature of 50 ℃ and the rpm of 600rpm until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymeric slurry of Cu, ni and Fe 3 O 4 Is 5wt.%, the concentration of C is 50wt.%, respectively; flatly coating the slurry on a stainless steel net, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, wherein a citric acid solution with the pH =3 is continuously dripped during the joule heating treatment, the joule heating treatment voltage is 6V, the current is 25A, and the time is 15s; and finally, after the stainless steel net is cooled to room temperature, the stainless steel net can be taken out from the glove box, namely the novel electromagnetic shielding material of the target.
Example 7
And (3) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of Joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g was sufficiently dissolved in500mL of ultrapure water is used for cleaning oil stains and other impurities on the surface of the stainless steel mesh; soaking a plurality of stainless steel meshes with the size of 3cm multiplied by 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with the concentration of 5wt.% is prepared, and the solution is stirred for 2 hours by a magnetic stirrer at the temperature of 50 ℃ and the rpm of 600rpm until the solution is clear and transparent; slowly pouring carbon black and Cu powder into a PVB solution in a stirring state, and uniformly mixing to obtain C/Cu/polymer slurry, wherein the concentrations of Cu and C in the slurry are respectively 5wt.% and 50wt.%; flatly coating the slurry on a stainless steel mesh, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, continuously dropwise adding a citric acid solution with pH =3 during the joule heating treatment, wherein the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the stainless steel net is cooled to room temperature, the stainless steel net can be taken out from the glove box, namely the novel electromagnetic shielding material of the target.
Example 8
And (3) preparing the electromagnetic shielding material with the surface of the stainless steel mesh coated with the conductive and magnetic conductive slurry by the aid of Joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and used for cleaning oil stains and other impurities on the surface of a stainless steel net; soaking a plurality of stainless steel meshes with the size of 3cm × 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; slowly pouring carbon black, cu powder and Ni powder into PVB solution in a stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Macromolecular slurry, wherein the concentrations of Cu and Ni in the slurry are respectively 5wt.%, and the concentration of C in the slurry is 50wt.%; the slurry is evenly coated on a stainless steel mesh, and drying is carried out after the coating is finishedDrying treatment; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, wherein a citric acid solution with the pH =3 is continuously dripped during the joule heating treatment, the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the stainless steel net is cooled to room temperature, the stainless steel net can be taken out from the glove box, namely the novel electromagnetic shielding material of the target.
Example 9
And (3) preparing the electromagnetic shielding material with the surface of the nickel screen coated with the conductive and magnetic conductive slurry by joule heat treatment assistance.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and used for cleaning oil stains and other impurities on the surface of a nickel net; soaking a plurality of nickel nets with the size of 3cm multiplied by 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 Is 5wt.%, the concentration of C is 50wt.%, respectively; flatly coating the slurry on a nickel screen, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, continuously dropwise adding a citric acid solution with pH =3 during the joule heating treatment, wherein the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the nickel screen is cooled to room temperature, the nickel screen can be taken out from the glove box, namely the target novel electromagnetic shielding material.
Example 10
And (3) preparing the electromagnetic shielding material with the surface of the tungsten mesh coated with the conductive and magnetic conductive slurry by the aid of Joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and is used for cleaning oil stains and other impurities on the surface of the tungsten mesh; soaking a plurality of tungsten nets with the size of 3cm multiplied by 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 The concentration of C is 5wt.% and the concentration of C is 50wt.%, respectively; flatly coating the slurry on a tungsten net, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, continuously dropwise adding a citric acid solution with pH =3 during the joule heating treatment, wherein the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the tungsten net is cooled to room temperature, the tungsten net can be taken out from the glove box, namely the target novel electromagnetic shielding material.
Example 11
And (3) preparing the electromagnetic shielding material with the conductive and magnetic conductive slurry coated on the surface of the carbon cloth by joule heat treatment.
Firstly, preparing deoiling liquid: sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g of the cleaning agent is fully dissolved in 500mL of ultrapure water and is used for cleaning oil stains and other impurities on the surface of the carbon cloth; soaking a plurality of carbon cloths with the size of 3cm multiplied by 6cm in the solution for 5min, taking out, cleaning with ultrapure water, and drying; then, polyvinyl butyral (PVB) and absolute ethyl alcohol are mixed, a PVB solution with a concentration of 5wt.% is prepared, and the mixture is stirred for 2 hours at a temperature of 50 ℃ and a speed of 600rpm by a magnetic stirrer until the solution is clear and transparent; mixing the carbonBlack, cu powder, ni powder and nano-iron sesquioxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry containing Cu, ni and Fe 3 O 4 Is 5wt.%, the concentration of C is 50wt.%, respectively; flatly coating the slurry on carbon cloth, and drying after coating; then, carrying out joule heating treatment on the mixture in a glove box in an inert gas environment, continuously dropwise adding a citric acid solution with pH =3 during the joule heating treatment, wherein the joule heating treatment voltage is 6V, the current is 15A, and the time is 15s; and finally, after the carbon cloth is cooled to room temperature, the carbon cloth can be taken out from the glove box, namely the target novel electromagnetic shielding material.
Claims (1)
1. A method for preparing a surface modified electromagnetic shielding material by Joule heat treatment is characterized by comprising the following steps:
(1) Mixing sodium carbonate (Na) 2 CO 3 ) 14g of sodium silicate nonahydrate (Na) 2 SiO 3 ·9H 2 O) 4g, sodium phosphate dodecahydrate (Na) 3 PO 4 ·12H 2 O) 11.5g was sufficiently dissolved in 500mL of ultrapure water as a deoiling liquid (solution A);
(2) Putting a plurality of substrate materials with the size of 3cm multiplied by 6cm into the solution A, soaking for 5min to remove oil stains and other impurities on the surface of the substrate materials, taking out the substrate materials, and cleaning the substrate materials by using ultrapure water, wherein the substrate materials comprise: stainless steel mesh, nickel mesh, tungsten mesh, carbon cloth, and the like;
(3) Mixing polyvinyl butyral (PVB) and absolute ethanol, and stirring with a magnetic stirrer at 50 ℃ and 600rpm for 2 hours until the solution is clear and transparent to obtain a PVB solution (solution B) with a concentration of 5wt.%, 10wt.% and 15wt.%;
(4) Mixing carbon black, cu powder, ni powder and nano-ferric oxide (Fe) 3 O 4 ) Slowly pouring the powder into PVB solution under stirring state, and uniformly mixing to obtain C/Cu/Ni/Fe 3 O 4 Polymer slurry (solution C), cu, ni and Fe in solution B 3 O 4 Is calculated separately, 5wt.%, 10wt.%, respectively20wt.% and 50wt.%, C concentrations 50wt.%, 60wt.% and 70wt.%, respectively;
(5) Flatly coating the solution C on a substrate material, and drying the coated solution C in a vacuum drying oven to obtain a material A;
(6) Performing Joule heat treatment on the material A in a glove box in an inert gas environment, wherein the voltage of the Joule heat treatment is 6V, the current is 15A, 20A and 25A, the heat treatment time is 15s, and a citric acid solution with the pH =3 is continuously dripped during the Joule heat treatment;
(7) And after the base material is cooled to room temperature after the Joule heat treatment, taking out the base material from the glove box for testing the electromagnetic shielding performance.
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