CN115895264B - Electromagnetic shielding composite material and preparation method and application thereof - Google Patents
Electromagnetic shielding composite material and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 64
- 239000002086 nanomaterial Substances 0.000 claims abstract description 51
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 31
- 239000012046 mixed solvent Substances 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 7
- 238000004891 communication Methods 0.000 claims abstract description 5
- 230000007123 defense Effects 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 42
- 239000004945 silicone rubber Substances 0.000 claims description 33
- 235000012239 silicon dioxide Nutrition 0.000 claims description 28
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 18
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 10
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 229910052710 silicon Inorganic materials 0.000 claims description 6
- 239000010703 silicon Substances 0.000 claims description 6
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 4
- 239000008096 xylene Substances 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 32
- 239000011229 interlayer Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 238000009422 external insulation Methods 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 239000002105 nanoparticle Substances 0.000 abstract 1
- 239000002344 surface layer Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 25
- 239000010410 layer Substances 0.000 description 20
- 239000002245 particle Substances 0.000 description 13
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- -1 polydimethylsiloxane Polymers 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229920001296 polysiloxane Polymers 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000000945 filler Substances 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002070 nanowire Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000002082 metal nanoparticle Substances 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
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Abstract
The invention discloses an electromagnetic shielding composite material, and a preparation method and application thereof, and belongs to the technical field of electromagnetic shielding. The invention carries out high-temperature treatment on the low-dimensional nano material in high-concentration alkali liquor, then carries out in-situ loading of silica nano particles on the surface and interlayer of the low-dimensional nano material to obtain a SiO 2 @low-dimensional nano material, then mixes the SiO 2 @low-dimensional nano material with a mixed solvent and silicon rubber, and obtains the silicon rubber/silica@low-dimensional nano material electromagnetic shielding composite material with insulated surface and wide use temperature range through a variable-temperature heating process; the obtained composite material shows a sandwich structure with external insulation and internal conduction. The electromagnetic shielding composite material has the advantages of stable mechanical property, wide use temperature range and excellent electromagnetic shielding performance, and can be used in the fields of manufacturing components and sealing equipment with electromagnetic shielding requirements in the fields of aerospace, military national defense, ships and warships and information communication.
Description
Technical Field
The invention relates to an electromagnetic shielding composite material, a preparation method and application thereof, and belongs to the technical field of electromagnetic shielding.
Background
In recent years, the high-speed development of the electronic technology field brings great trouble to the human society, and is derived from the problem of electromagnetic interference (EMI) caused by electronic equipment, and the intangible electromagnetic radiation can affect the health of human beings on one hand, and the electromagnetic waves emitted between the electronic equipment can affect the operation of precision equipment on the other hand. In addition, in the fields of aerospace, military national defense, ships and warships, information communication, high-temperature workstations and the like, not only is the material required to have excellent electromagnetic shielding (EMI SE) capability, but also the requirement in a severe environment and the long-term durability in a special environment are more important. Therefore, the development of electromagnetic shielding materials that can be applied in extreme environments is a current problem of research.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention provides an electromagnetic shielding silicone rubber/silicon dioxide@low-dimensional nanomaterial composite material with insulated surface and wide use temperature range, and a preparation method and application thereof.
During the preparation of the composite material, the composite material shows a three-layer structure with the volatilization of the mixed solvent, and comprises an insulating outer layer and a conductive middle layer
The invention provides a surface-insulated silicon rubber/silicon dioxide@low-dimensional nanomaterial electromagnetic shielding composite material with a wide use temperature range, wherein the composite material surface is provided with a three-layer structure and comprises an insulating outer layer and a conductive middle layer; the outer layer is made of a silicone rubber material, and the middle layer is made of a silicone rubber-silicon dioxide-low-dimensional nano material composite; the silicon rubber-silicon dioxide-low-dimensional nanomaterial composite is of a bicontinuous phase structure of silicon rubber and silicon dioxide@low-dimensional nanomaterial, and the silicon dioxide@low-dimensional nanomaterial is uniformly dispersed in the silicon rubber.
In one embodiment of the invention, the silica has a particle size of 5-300nm.
In one embodiment of the present invention, the low-dimensional nanomaterial is at least one of a one-dimensional nanomaterial and/or a two-dimensional nanomaterial.
In one embodiment of the present invention, the low-dimensional nanomaterial is specifically selected from at least one of carbon quantum dots, metal nanoparticles, carbon nanotubes/nanowires, metal nanowires, graphene oxide, 2D perovskite, and two-dimensional layered metal carbon/nitride (MXene).
In one embodiment of the present invention, the silicone rubber is at least one of an alpha, omega-dihydroxy polydimethylsiloxane, a trifluoropropyl methyl polysiloxane, a methyl vinyl polysiloxane, and a methyl vinyl phenyl polysiloxane.
In one embodiment of the invention, the electromagnetic shielding silicone rubber/silica @ low dimensional nanomaterial composite is used at a temperature in the range of-80 ℃ to 300 ℃.
The second object of the invention is to provide a preparation method of a surface-insulated silicon rubber/silicon dioxide@low-dimensional nanomaterial electromagnetic shielding composite material with a wide use temperature range, which comprises the following steps:
(a) Adding the low-dimensional nano material into alkali liquor, uniformly mixing, and purifying to obtain an activated low-dimensional nano material;
(b) Adding the activated low-dimensional nano material into a mixed solution of water and ethanol with the pH value of 8-10, adding an ethanol solution of tetraethyl orthosilicate, fully and uniformly mixing, collecting solids, and purifying to obtain a silicon dioxide@low-dimensional nano material compound;
(c) Adding the silicon dioxide@low-dimensional nano material compound obtained in the step (b) into a mixture of silicon rubber and a mixed solvent, and uniformly mixing;
(d) Pouring the homogeneous liquid obtained in the step (c) into a mold, and performing variable-temperature heating treatment to obtain the silicone rubber/silicon dioxide@low-dimensional nano material composite material.
In one embodiment of the invention, in step (a), the lye is at least one of sodium hydroxide and potassium hydroxide solution.
In one embodiment of the invention, in step (a), the concentration of the low dimensional nanomaterial relative to the lye is between 0.01 and 0.05g/mL. Specifically, 0.02g/mL is selected.
In one embodiment of the invention, in step (a), the mass fraction of lye is 10% -50%.
In one embodiment of the invention, in step (a), the mixture is stirred for 6 to 18 hours.
In one embodiment of the invention, in step (a), the temperature of the stirring is from 90 ℃ to 160 ℃.
In one embodiment of the invention, in step (b), the concentration of the activated low-dimensional nanomaterial relative to the mixed liquor is from 0.001 to 0.05g/mL.
In one embodiment of the invention, in step (b), the mass ratio of tetraethyl orthosilicate to the low-dimensional nanomaterial is in the range of 0.1:1 to 5.0:1. Specifically, 0.1:1, 2:1 and 5:1 are selected.
In one embodiment of the invention, in step (b), the concentration of the ethanol solution of tetraethyl orthosilicate is 0.01-0.5g/mL.
In one embodiment of the invention, in step (b), the mixture is thoroughly mixed by stirring for 3 to 16 hours.
In one embodiment of the invention, in step (c), the mass ratio of silica @ low dimensional nanomaterial complex to silicone rubber is from 0.05:1 to 0.5:1. Specifically, the ratio of the components is 0.1:1.
In one embodiment of the invention, in step (c), the concentration of silicone rubber relative to the mixed solvent is between 5% and 40%.
In one embodiment of the present invention, in the step (c), the mixed solvent is at least two of xylene, chloroform, ethanol, isopropanol, diethyl ether, acetone, tetrahydrofuran, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
In one embodiment of the present invention, in step (c), the mixed solvent is specifically selected from a mixed system of xylene and tetrahydrofuran, and the volume ratio of the two is 2:3.
In one embodiment of the present invention, in the step (d), the variable temperature heating treatment comprises two processes, one is to treat at a temperature of 20 ℃ to 80 ℃ for 6 to 48 hours, and the other is to treat at a temperature of 60 ℃ to 150 ℃ for 6 to 48 hours.
The invention also provides application of the silicon rubber/silicon dioxide@low-dimensional nanomaterial composite material, which comprises application in manufacturing components and sealing equipment with electromagnetic shielding requirements in the fields of aerospace, military national defense, ships and warships and information communication.
The invention has the beneficial effects that:
The electromagnetic shielding silicone rubber/silicon dioxide@low-dimensional nanomaterial composite material with a three-layer structure is prepared by a simple one-step molding method, and comprises an outer silicone rubber layer and a silicone rubber-silicon dioxide-low-dimensional nanomaterial composite layer in the middle layer, wherein the silicone rubber layer is insulating, and can effectively protect contacted electrical equipment from damage such as short circuit and the like, and the middle composite layer is used as a conductive layer to provide high electromagnetic shielding effect. The silicon rubber/silicon dioxide@low-dimensional nanomaterial composite material prepared by the method can be stably used for a long time in an extreme environment of-80 ℃ to 300 ℃, has electromagnetic shielding performance of more than 35dB, and has a huge application prospect in severe environments such as aerospace, military national defense, ships and warships, information communication and the like.
Drawings
FIG. 1 is an SEM image of the SiO 2 @MXene of examples 1-3 and comparative examples 1-2.
FIG. 2 is an SEM image of a cross-section of a silicone rubber/SiO 2 @ MXene composite of examples 1-3 and comparative examples 1-2.
Detailed Description
The embodiments disclosed herein are examples of the application, which may be embodied in different forms. Therefore, the disclosure's details, including specific structural and functional details, are not intended to limit the application, but merely to form the basis of the claims. It should be understood that the detailed description of the application is not intended to be limiting but is intended to cover all possible modifications, equivalents and alternatives falling within the scope of the application as defined by the appended claims. The word "may" is used throughout in a permissive sense rather than the mandatory sense. Similarly, unless otherwise indicated, the words "comprise", "comprising" and "consist of" mean "including but not limited to". The words "a" or "an" mean "at least one," and the word "plurality" means more than one. When abbreviations or technical terms are used, these terms represent commonly accepted meanings known in the art.
Example 1
An electromagnetic shielding silicon rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
(A) Adding 1g of MXene into 50ml of 30% potassium hydroxide solution, heating to 130 ℃ and stirring for 12 hours, and purifying to obtain activated MXene particles;
(b) Adding 1g of activated MXene particles into 200mL of a mixed solution of water and ethanol with the pH of 9 (volume ratio of water to ethanol is 1:1), adding 10mL of an ethanol solution of tetraethyl orthosilicate with the concentration of 0.01g/mL (the mass ratio of MXene to tetraethyl orthosilicate is 1:0.1), stirring for 8 hours, collecting a solid, and purifying to obtain SiO 2 @MXene;
(c) Adding the SiO 2 @ MXene (0.5 g) obtained in the step (b) into a mixture of 5g of silicon rubber and 20ml of dimethylbenzene/tetrahydrofuran (the volume ratio is 2:3) (the mass ratio of the SiO 2 @ MXene to the silicon rubber is 0.1:1), and uniformly mixing;
(d) Pouring the homogeneous liquid obtained in the step (c) into a mould, firstly placing for 24 hours at 50 ℃, then placing for 24 hours at 110 ℃ to remove all mixed solvent and solidify the silicon rubber, thus obtaining the silicon rubber/SiO 2 @MXene composite material.
Example 2
An electromagnetic shielding silicon rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
(A) Adding 1g of MXene into 50mL of 30% potassium hydroxide solvent, heating to 130 ℃ and stirring for 12 hours, and purifying to obtain activated MXene particles;
(b) Adding 1g of activated MXene particles into 200mL of a mixed solution of water and ethanol with the pH of 9 (volume ratio of water to ethanol is 1:1), adding 10mL of an ethanol solution of tetraethyl orthosilicate with the concentration of 0.2g/mL (the mass ratio of MXene to tetraethyl orthosilicate is 1:2), stirring for 8 hours, collecting a solid, and purifying to obtain SiO 2 @MXene;
(c) Adding the SiO 2 @ MXene (0.5 g) obtained in the step (b) into a mixture of 5g of silicon rubber and 20mL of dimethylbenzene/tetrahydrofuran (the volume ratio is 2:3) (the mass ratio of the SiO 2 @ MXene to the silicon rubber is 0.1:1), and uniformly mixing;
(d) Pouring the homogeneous liquid obtained in the step (c) into a mould, firstly placing for 24 hours at 50 ℃, then placing for 24 hours at 110 ℃ to remove all mixed solvent and solidify the silicon rubber, thus obtaining the silicon rubber/SiO 2 @MXene composite material.
Example 3
An electromagnetic shielding silicon rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
(A) Adding 1g of MXene into 50mL of 30% potassium hydroxide solvent, heating to 130 ℃ and stirring for 12 hours, and purifying to obtain activated MXene particles;
(b) Adding 1g of activated MXene particles into 200mL of a mixed solution of water and ethanol with the pH of 9 (volume ratio of water to ethanol is 1:1), adding 10mL of an ethanol solution of tetraethyl orthosilicate with the concentration of 0.5g/mL (the mass ratio of MXene to tetraethyl orthosilicate is 1:5), stirring for 8 hours, collecting a solid, and purifying to obtain SiO 2 @MXene;
(c) Adding the SiO 2 @ MXene (0.5 g) obtained in the step (b) into a mixture of 5g of silicon rubber and 20mL of dimethylbenzene/tetrahydrofuran (the volume ratio is 2:3) (the mass ratio of the SiO 2 @ MXene to the silicon rubber is 0.1:1), and uniformly mixing;
(d) Pouring the homogeneous liquid obtained in the step (c) into a mould, firstly placing for 24 hours at 50 ℃, then placing for 24 hours at 110 ℃ to remove all mixed solvent and solidify the silicon rubber, thus obtaining the silicon rubber/SiO 2 @MXene composite material.
Comparative example 1
In comparison with example 1, the tetraethyl orthosilicate solution was not added in step (b), but the same applies.
Comparative example 2
The concentration of the tetraethyl orthosilicate solution added in step (b) was 1g/mL (mass ratio of MXene to tetraethyl orthosilicate 1:10) compared to example 1, except that the solution was the same.
The layered structure characteristics, siO 2 particle size, sample thickness, electromagnetic shielding properties, tensile strength, etc. of the silicone rubber/SiO 2 @MXene composite materials obtained in examples 1-3 and comparative examples 1-2 were tested and characterized as shown in Table 1. SEM of SiO 2 @ MXene in examples 1-3 and comparative examples 1-2 is shown in FIG. 1. SEM of cross-section of the silicone rubber/SiO 2 @MXene composite material of examples 1-3 and comparative examples 1-2 is shown in FIG. 2.
The testing method comprises the following steps:
Electromagnetic shielding performance measurement:
the materials obtained in examples 1 to 3 and comparative examples 1 to 2 were tested for electromagnetic shielding performance by a waveguide method using a vector network analyzer in the range of X-band (8 to 12 GHz).
Tensile strength measurement:
the materials obtained in examples 1 to 3 and comparative examples 1 to 2 were tested for tensile strength and elongation at break according to GB/T1040.1 to 2018 using a universal tester at a tensile rate of 10mm/min.
TABLE 1 characteristics of layered structures, siO 2 particle diameters, film thicknesses, and electromagnetic shielding properties of examples and comparative examples
As can be seen from the combination of FIG. 1 and Table 1, for examples 1-3, the SiO 2 particles in the prepared SiO 2 @MXene had particle diameters of 5-15nm, 100-150nm and 200-250nm (as shown in Table 1), respectively, and were uniformly dispersed on the surface of the MXene and inside the sheet layer as the concentration of the tetraethyl orthosilicate/ethanol mixture increased. In comparative example 1, only the structure of MXene was found without adding tetraethyl orthosilicate/ethanol mixed solution, as shown in fig. 1. In contrast, the concentration of the tetraethyl orthosilicate/ethanol mixture in comparative example 2 was too high, which represented a particle size of 300-350nm for SiO 2, and this too large particle size also destroyed the original layer structure of MXene (FIG. 1).
As can be seen from fig. 2 and table 1, in the silicone rubber/SiO 2 @ MXene composite material prepared in examples 1-3, MXene-based filler was completely dispersed in the middle layer of the composite film, exhibiting a typical sandwich structure; in comparative example 1, the MXene-based filler was entirely dispersed in the bottom layer of the composite film; in comparative example 2, the MXene-based filler was uniformly dispersed throughout the composite film; the electromagnetic shielding properties of the composites prepared in examples 1-3 were significantly increased relative to comparative examples 1-2.
In conclusion, the analysis proves that the SiO 2 is successfully loaded on the surface and the interlayer of the MXene, and also proves that the layer structure of the prepared silicon rubber composite material is formed and the electromagnetic shielding performance of the silicon rubber composite material is improved.
Example 4
An application of electromagnetic shielding silicone rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
(A) The silicone rubber/SiO 2 @ MXene composite obtained in example 1 was subjected to a 50-cycle stretching experiment in an environment of-80 ℃;
(b) After step (a) is completed, the electromagnetic shielding performance of the sample is tested.
Example 5
An application of electromagnetic shielding silicone rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
(A) The silicone rubber/SiO 2 @ MXene composite obtained in example 1 was subjected to a 50 cycle stretch experiment in an environment at 300 ℃;
(b) After step (a) is completed, the electromagnetic shielding performance of the sample is tested.
Comparative example 3
An application of electromagnetic shielding silicone rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
The silicone rubber/SiO 2 @ MXene composite material obtained in comparative example 1 was subjected to 50-cycle stretching experiments in an environment of-80 ℃ and then tested for electromagnetic shielding performance.
Comparative example 4
An application of electromagnetic shielding silicone rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
The silicone rubber/SiO 2 @ MXene composite material obtained in comparative example 1 was subjected to a 50-cycle stretching experiment in an environment of 300 ℃ and then tested for electromagnetic shielding properties.
Comparative example 5
An application of electromagnetic shielding silicone rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
The silicone rubber/SiO 2 @ MXene composite material obtained in comparative example 2 was subjected to 50-cycle stretching experiments in an environment of-80 ℃ and then tested for electromagnetic shielding performance.
Comparative example 6
An application of electromagnetic shielding silicone rubber/silicon dioxide@MXene composite material with an insulated surface and a wide use temperature range.
The silicone rubber/SiO 2 @ MXene composite material obtained in comparative example 2 was subjected to a 50-cycle stretching experiment in an environment of 300 ℃ and then tested for electromagnetic shielding properties.
The percent mechanical strength remaining and the electromagnetic shielding performance after 50 times of cyclic stretching in examples 4 to 5 and comparative examples 3 to 4 were tested as shown in Table 2.
TABLE 2
From Table 2, it can be seen that the silicone rubber/SiO 2 @MXene electromagnetic shielding composite material with a sandwich structure in examples 4-5 shows good mechanical properties and electromagnetic shielding property stability at-80 ℃ and 300 ℃; in comparative examples 3-6, the silicone rubber/SiO 2 @MXene composite material having a sandwich structure was poor in both mechanical properties and electromagnetic shielding property stability at-80℃and 300 ℃.
Those skilled in the art will appreciate that: the foregoing description of the embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (10)
1. The preparation method of the electromagnetic shielding composite material of the silicone rubber/silicon dioxide@low-dimensional nanomaterial is characterized by comprising the steps of forming a three-layer structure of the electromagnetic shielding composite material, wherein the electromagnetic shielding composite material comprises an outer layer and an intermediate layer; the outer layer is silicon rubber, and the middle layer is a compound of silicon rubber, silicon dioxide and low-dimensional nano materials; the silicon rubber-silicon dioxide-low-dimensional nanomaterial composite is of a bicontinuous phase structure of silicon rubber and silicon dioxide@low-dimensional nanomaterial, and the silicon dioxide@low-dimensional nanomaterial is uniformly dispersed in the silicon rubber;
the preparation method comprises the following steps:
(a) Adding the low-dimensional nano material into alkali liquor, uniformly mixing, and purifying to obtain an activated low-dimensional nano material;
(b) Adding the activated low-dimensional nano material into a mixed solution of water and ethanol with the pH value of 8-10, adding an ethanol solution of tetraethyl orthosilicate, fully and uniformly mixing, collecting solids, and purifying to obtain a silicon dioxide@low-dimensional nano material compound;
(c) Adding the silicon dioxide@low-dimensional nano material compound obtained in the step (b) into a mixture of silicon rubber and a mixed solvent, and uniformly mixing;
(d) Pouring the homogeneous liquid obtained in the step (c) into a mold, and performing variable-temperature heating treatment to obtain the silicone rubber/silicon dioxide@low-dimensional nano material composite material.
2. The method of claim 1, wherein in step (a), the concentration of the low-dimensional nanomaterial relative to the lye is 0.01-0.05g/mL.
3. The method of claim 1, wherein in step (b), the concentration of the activated low-dimensional nanomaterial relative to the mixed liquor is from 0.001 to 0.05g/mL.
4. The method of claim 1, wherein in step (b), the mass ratio of tetraethyl orthosilicate to the low-dimensional nanomaterial is 0.1:1 to 5.0:1.
5. The method according to claim 1, wherein in step (b), the concentration of the ethanol solution of tetraethyl orthosilicate is 0.01-0.5g/mL.
6. The method of claim 1, wherein in step (c), the mass ratio of silica @ low dimensional nanomaterial composite to silicone rubber is from 0.05:1 to 0.5:1.
7. The method according to claim 1, wherein the low dimensional nanomaterial is a one dimensional nanomaterial and/or a two dimensional nanomaterial.
8. The method according to any one of claims 1 to 7, wherein in step (c), the mixed solvent is at least two of xylene, chloroform, ethanol, isopropanol, diethyl ether, acetone, tetrahydrofuran, N-dimethylformamide, N-dimethylacetamide and N-methylpyrrolidone.
9. The silicone rubber/silicon dioxide@low-dimensional nanomaterial electromagnetic shielding composite material prepared by the method of claim 1.
10. The use of the silicone rubber/silica @ low-dimensional nanomaterial electromagnetic shielding composite of claim 9 in the fields of aerospace, military national defense, marine vessels, and information communication.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202211431732.7A CN115895264B (en) | 2022-11-16 | 2022-11-16 | Electromagnetic shielding composite material and preparation method and application thereof |
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| US20190352543A1 (en) * | 2017-02-14 | 2019-11-21 | 3M Innovative Properties Company | Composite compositions for electromagnetic interference shielding and articles including the same |
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| CN111438867A (en) * | 2020-03-16 | 2020-07-24 | 中北大学 | Method for preparing anisotropic conductive film by magnetic field induction method |
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