CN114517014B - Heat-conducting shielding rubber, preparation method thereof and electronic equipment containing heat-conducting shielding rubber - Google Patents
Heat-conducting shielding rubber, preparation method thereof and electronic equipment containing heat-conducting shielding rubber Download PDFInfo
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- CN114517014B CN114517014B CN202011296533.0A CN202011296533A CN114517014B CN 114517014 B CN114517014 B CN 114517014B CN 202011296533 A CN202011296533 A CN 202011296533A CN 114517014 B CN114517014 B CN 114517014B
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- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical group CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 3
- XDLMVUHYZWKMMD-UHFFFAOYSA-N 3-trimethoxysilylpropyl 2-methylprop-2-enoate Chemical compound CO[Si](OC)(OC)CCCOC(=O)C(C)=C XDLMVUHYZWKMMD-UHFFFAOYSA-N 0.000 claims description 3
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/06—Reinforcing macromolecular compounds with loose or coherent fibrous material using pretreated fibrous materials
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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
- H05K7/00—Constructional details common to different types of electric apparatus
- H05K7/20—Modifications to facilitate cooling, ventilating, or heating
- H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
-
- 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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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
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- 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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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention provides a heat-conducting shielding rubber, a preparation method thereof and electronic equipment containing the heat-conducting shielding rubber. The preparation method of the heat-conducting shielding rubber comprises the following steps: adopting graphite fibers containing metal plating layers to construct a three-dimensional framework; preparing liquid vulcanized silicone rubber mixed with heat conducting filler; and filling the three-dimensional framework with liquid vulcanized silicone rubber mixed with the heat-conducting filler, and carrying out vacuum treatment and room temperature vulcanization treatment to obtain the heat-conducting shielding rubber. Compared with the existing method, the method for preparing the heat-conducting shielding rubber is beneficial to reducing the consumption of filler, improving the electromagnetic field shielding capacity and mechanical property of the heat-conducting shielding rubber, greatly improving the heat dissipation performance of electronic components in the application process, prolonging the service life of electronic equipment and widening the application range of the electronic equipment.
Description
Technical Field
The invention relates to the field of communication, in particular to heat conduction shielding rubber, a preparation method thereof and electronic equipment containing the heat conduction shielding rubber.
Background
The volume of electronic components in the communication field is continuously reduced, the working frequency is continuously improved, and the mutual interference phenomenon between electronic devices and the produced heat are rapidly accumulated. The reliability and stability of the electronic components are reduced by 10% every 2 ℃ of the temperature of the electronic components. In order to ensure that electronic components can operate with high reliability for a long time, heat dissipation becomes an important factor affecting the service life of the electronic components, and therefore, development of electromagnetic shielding materials with high heat conductivity is urgently required.
As a novel electromagnetic shielding material, the conductive silicon rubber has good flexibility, sealing performance and weather resistance, has excellent electromagnetic shielding performance, and can effectively solve the problems. For conductive silicone rubber, the conductivity of the filler and its dispersion and connectivity in the silicone rubber are important factors that limit its overall conductive and electromagnetic shielding properties. The traditional blending preparation method can not realize even distribution and efficient penetration of the filler in the matrix material, so that the material has the problems of large filler consumption, poor electromagnetic shielding effect and the like.
In view of the above, there is a need to develop a silicone rubber composite material having a low filler content and a high shielding effectiveness.
Disclosure of Invention
The invention mainly aims to provide a heat-conducting shielding rubber, a preparation method thereof and electronic equipment containing the heat-conducting shielding rubber, so as to solve the problems that the existing method cannot realize uniform distribution and efficient penetration of filler in a matrix material, and the silicone rubber composite material has large filler consumption and poor electromagnetic shielding effect.
In order to achieve the above object, according to an aspect of the present invention, there is provided a method for preparing a heat conductive shielding rubber, the method comprising: adopting graphite fibers containing metal plating layers to construct a three-dimensional framework; preparing liquid vulcanized silicone rubber mixed with heat conducting filler; and filling the three-dimensional framework with liquid vulcanized silicone rubber mixed with the heat-conducting filler, and carrying out vacuum treatment and room temperature vulcanization treatment to obtain the heat-conducting shielding rubber.
Further, the step of constructing a three-dimensional skeleton includes: constructing at least two alternative three-dimensional models; analyzing the influence of each alternative three-dimensional model on mechanical properties, and taking the alternative three-dimensional model with the optimal mechanical properties as a target three-dimensional skeleton structure when the consumption of graphite fibers containing metal plating layers is the minimum; and taking graphite fibers containing the metal plating layers as raw materials, and modeling according to a target three-dimensional framework structure to obtain a three-dimensional framework.
Further, the step of preparing the liquid vulcanized silicone rubber mixed with the heat conductive filler comprises the following steps: carrying out surface modification on the heat-conducting filler by adopting a coupling agent to obtain a surface-modified heat-conducting filler; premixing and vacuum kneading the surface modified heat conducting filler, room temperature vulcanized silicone rubber and a mixture of a catalyst in sequence to obtain a pretreatment product; crosslinking reaction is carried out on the pretreated product and a crosslinking agent, so as to obtain liquid vulcanized silicone rubber mixed with the heat conducting filler; preferably, the coupling agent is selected from gamma-aminopropyl triethoxysilane and/or methacryloxypropyl trimethoxysilane; preferably, the thermally conductive filler is selected from one or more of the group consisting of boron nitride, aluminum oxide, silicon nitride, aluminum nitride; more preferably, the particle diameter of the heat conductive filler is 50 to 150nm, and still more preferably, the particle diameter of the heat conductive filler is 90 to 110nm.
Further, the surface modification process includes: mixing a coupling agent with an organic solvent to obtain a first solution; mixing the first solution, the heat-conducting filler and water, and sequentially performing ultrasonic dispersion, solvent evaporation and drying treatment to obtain a surface-modified heat-conducting filler; preferably, the weight ratio of the coupling agent to the heat conducting filler to the water is (1-5): (120-180): (2-10).
Further, after the first solution, the heat conducting filler and the water are mixed, the pH of the reaction system is 3-5, the time of the ultrasonic dispersion treatment process is 20-60 min, the temperature of the solvent evaporation process is 60-90 ℃, the temperature of the drying process is 100-130 ℃, and the drying time is 12-24 h.
Further, the graphite fibers containing the metal plating layer are selected from one or more of the group consisting of silver-plated graphite fibers, copper-plated graphite fibers and nickel-plated graphite fibers; preferably, the monofilament diameter of the graphite fiber containing the metal plating layer is 6-10 μm, the plating thickness is 0.1-0.3 μm, and the addition amount of the graphite fiber containing the metal plating layer is 10-30% based on 100 parts by weight of the heat conductive shielding rubber.
Further, in the step of preparing the liquid vulcanized silicone rubber mixed with the heat-conducting filler, the weight of the mixture of the room temperature vulcanized silicone rubber and the catalyst is calculated as 100 parts, the weight of the heat-conducting filler with surface modification is 20-40 parts, the dosage of the catalyst is 0.01-0.3 part, the dosage of the cross-linking agent is 0.1-0.5 part, and the premixing time is 1-2 hours; the time of the vacuum kneading process is 4 to 8 hours.
Further, the room temperature vulcanized silicone rubber is linear, branched or micro-crosslinked polysiloxane, and any one molecular structure at least comprises two or more aliphatic unsaturated double bonds, the viscosity range is 300-500000 mPa.s, and the chain end or side chain of the room temperature vulcanized silicone rubber at least comprises two vinyl groups, preferably alpha, omega-dihydroxy polydimethylsiloxane-based rubber; the catalyst is one or more selected from the group consisting of platinum compounds, organotin compounds and organotin compounds; the cross-linking agent is selected from one or more of the group consisting of alkoxysilane, hydrosilane, hydroxyaminosilane, amidosilane and silanol.
Further, the temperature of the room temperature vulcanization treatment is 10-35 ℃ and the vulcanization time is 24-72 h.
The application also provides a heat-conducting shielding rubber which is prepared by the preparation method.
Still another aspect of the present application provides an electronic device including an electronic component and a thermally conductive electromagnetic shielding material dispersed around the electronic component, the thermally conductive electromagnetic shielding material including the thermally conductive shielding rubber provided by the present application.
By applying the technical scheme of the invention, the graphite fiber with better electric conductivity and containing the metal plating layer is used for replacing the traditional carbon fiber, carbon nano tube, graphene and the like, so that the electric conductivity of the heat conduction shielding rubber can be greatly improved, and a better shielding effect can be obtained. Meanwhile, due to the designability of the three-dimensional framework, the constructed electric conduction and heat conduction path is quicker and more complete, so that the electric conduction capacity and the shielding performance of the heat conduction shielding rubber are further improved, and the efficient heat conduction shielding rubber material is prepared. Compared with the existing method, the method for preparing the heat-conducting shielding rubber is beneficial to reducing the consumption of filler, improving the electromagnetic field shielding capacity and mechanical property of the heat-conducting shielding rubber, greatly improving the heat dissipation performance of electronic components in the application process, prolonging the service life of electronic equipment and widening the application range of the electronic equipment.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this specification, illustrate embodiments of the application and together with the description serve to explain the application. In the drawings:
FIG. 1 is a schematic view showing the structure of a three-dimensional skeleton constructed in example 1 of the present invention;
fig. 2 is a cross-sectional view showing a three-dimensional skeleton constructed in example 1 of the present invention.
Detailed Description
It should be noted that, without conflict, the embodiments of the present application and features of the embodiments may be combined with each other. The present application will be described in detail with reference to examples.
As described in the background art, the existing method can not realize uniform distribution and efficient penetration of the filler in the matrix material, so that the silicone rubber composite material has the problems of large filler dosage and poor electromagnetic shielding effectiveness. In order to solve the technical problems, the application provides a preparation method of heat-conducting shielding rubber, which comprises the following steps: adopting graphite fibers containing metal plating layers to construct a three-dimensional framework; preparing liquid vulcanized silicone rubber mixed with heat conducting filler; and filling the three-dimensional framework with liquid vulcanized silicone rubber mixed with the heat-conducting filler, and carrying out vacuum treatment and room temperature vulcanization treatment to obtain the heat-conducting shielding rubber.
The graphite fiber with better electric conductivity and containing the metal plating layer is used for replacing the traditional carbon fiber, carbon nano tube, graphene and the like, so that the electric conductivity of the heat conduction shielding rubber can be greatly improved, and a better shielding effect is obtained. Meanwhile, due to the designability of the three-dimensional framework, the constructed heat and electric conduction path is quicker and more complete, so that the heat and electric conduction capacity and the shielding performance of the heat and electric conduction shielding rubber are further improved, and the efficient heat and electric conduction shielding rubber material is prepared. Compared with the existing method, the method for preparing the heat-conducting shielding rubber is beneficial to reducing the consumption of filler, improving the electromagnetic field shielding capacity and mechanical property of the heat-conducting shielding rubber, greatly improving the heat dissipation performance of electronic components in the application process, prolonging the service life of electronic equipment and widening the application range of the electronic equipment.
In order to further improve the mechanical properties of the heat conductive shielding rubber, in a preferred embodiment, the step of constructing a three-dimensional skeleton includes: constructing at least two alternative three-dimensional models; analyzing the influence of each alternative three-dimensional model on mechanical properties, and taking the alternative three-dimensional model with the optimal mechanical properties as a target three-dimensional skeleton structure when the consumption of graphite fibers containing metal plating layers is the minimum; and taking graphite fibers containing the metal plating layers as raw materials, and modeling according to a target three-dimensional framework structure to obtain a three-dimensional framework.
More preferably, a rapier loom is used to construct a three-dimensional framework of metal-plated graphite fibers. The three-dimensional framework of the graphite fiber containing the metal coating is constructed by utilizing the rapier loom, and then the room temperature vulcanized rubber is injected to prepare the light and efficient shielding rubber material.
Conventional heat conducting filler powder is easy to delaminate in matrix rubber, so that the mechanical property and shielding property of the shielding rubber material are affected to a certain extent. In a preferred embodiment, the step of preparing a liquid, thermally conductive filler-mixed vulcanized silicone rubber comprises: carrying out surface modification on the heat-conducting filler by adopting a coupling agent to obtain a surface-modified heat-conducting filler; premixing and vacuum kneading the surface modified heat conducting filler, room temperature vulcanized silicone rubber and a mixture of a catalyst in sequence to obtain a pretreatment product; and (3) carrying out a crosslinking reaction on the pretreated product and a crosslinking agent to obtain the liquid vulcanized silicone rubber mixed with the heat conducting filler.
Compared with unmodified heat conducting filler, the silane coupling agent is adopted to pretreat the heat conducting filler powder, so that the dispersibility of the heat conducting filler powder in the matrix rubber is enhanced, and the mechanical property of the shielding rubber material is further improved.
In a preferred embodiment, the coupling agent includes, but is not limited to, gamma-aminopropyl triethoxysilane and/or methacryloxypropyl trimethoxysilane. Compared with other coupling agents, the coupling agents have more excellent coupling performance, so that the coupling agents are beneficial to further improving the dispersion performance of the surface modified heat conducting filler in the matrix resin.
In a preferred embodiment, the thermally conductive filler includes, but is not limited to, one or more of the group consisting of boron nitride, aluminum oxide, silicon nitride, aluminum nitride. The heat-conducting filler is selected to replace the traditional white carbon black to be used as the reinforcing agent of the silicon rubber, and the mechanical property of the heat-conducting shielding rubber has a certain influence, but the influence of the nickel-coated graphite skeleton is considered, so that the influence on the mechanical property is almost negligible. And the heat conductivity coefficient of the heat conducting filler powder is far higher than that of the white carbon black, so that the addition of the heat conducting filler is beneficial to greatly improving the heat conducting capacity of the heat conducting shielding rubber. More preferably, the particle diameter of the heat conductive filler is 50 to 150nm, and still more preferably, the particle diameter of the heat conductive filler is 90 to 110nm.
The surface modification process may be carried out by a method commonly used in the art. In a preferred embodiment, the surface modification process comprises: mixing a coupling agent with an organic solvent to obtain a first solution; and mixing the first solution, the heat-conducting filler and water, and sequentially performing ultrasonic dispersion, solvent evaporation and drying treatment to obtain the surface-modified heat-conducting filler.
In order to further improve the dispersion property of the heat conductive filler in the matrix rubber and the mechanical property of the shielding rubber material, preferably, the weight ratio of the coupling agent to the heat conductive filler to the water is (1-5): (120-180): (2-10).
In the surface modification process, the organic solvent may be one or more selected from the group consisting of absolute ethyl alcohol, ethylene glycol, n-butanol and petroleum ether.
The surface modification process may be carried out by a process commonly used in the art. In a preferred embodiment, after the first solution, the heat conductive filler and the water are mixed, the pH of the reaction system is 3-5, the time of the ultrasonic dispersion treatment process is 20-60 min, the temperature of the solvent evaporation process is 60-90 ℃, the temperature of the drying process is 100-130 ℃, and the drying time is 12-24 h.
In a preferred embodiment, the monofilament diameter of the graphite fiber containing the metal plating layer is 6 to 10 μm, the plating thickness is 0.1 to 0.3 μm, and the addition amount of the graphite fiber containing the metal plating layer in the heat conductive shielding rubber is 10 to 30% based on 100 parts by weight of the heat conductive shielding rubber. The graphite fiber containing the metal plating layer with the specification is selected, and the dosage of the graphite fiber containing the metal plating layer is limited in the range, so that the mechanical property and the electric conductivity of the heat conduction shielding rubber are improved, and the density of the heat conduction shielding rubber is smaller under the same electric conductivity and heat conduction conditions.
In a preferred embodiment, in the step of preparing the liquid vulcanized silicone rubber mixed with the heat-conducting filler, the mixture of the room temperature vulcanized silicone rubber and the catalyst is prepared by taking 100 parts by weight of the mixture, 20-40 parts by weight of the surface-modified heat-conducting filler, 0.01-0.3 part by weight of the catalyst, 0.1-0.5 part by weight of the cross-linking agent and 1-2 hours of premixing; the time of the vacuum kneading process is 4 to 8 hours.
The room temperature vulcanizing silicone rubber, the catalyst and the crosslinking agent may be of the kind commonly used in the art. For example, the room temperature vulcanized silicone rubber is linear, branched or micro-crosslinked polysiloxane, and any molecular structure at least comprises two or more aliphatic unsaturated double bonds, the viscosity range is 300-500000 mPa.s, and the chain end or side chain of the room temperature vulcanized silicone rubber at least comprises two vinyl groups, preferably comprises but is not limited to alpha, omega-dihydroxy polydimethylsiloxane-based rubber; the catalyst includes, but is not limited to, one or more of the group consisting of platinum-based compounds, organotin-based compounds, and organotitanium-based compounds; in a preferred embodiment, the cross-linking agent includes, but is not limited to, one or more of the group consisting of alkoxysilanes, hydrosilanes, hydroxyaminosilanes, amidosilanes, and silanol.
In a preferred embodiment, the temperature of the room temperature vulcanization process is 10 to 35℃and the vulcanization time is 24 to 72 hours. The temperature and the vulcanizing time in the room temperature vulcanizing process are limited in the above range, which is favorable for further improving the vulcanizing degree of the heat-conducting shielding rubber, and further improving the comprehensive properties of elasticity, weather resistance and the like.
The application also provides a heat-conducting shielding rubber which is prepared by the preparation method.
The graphite fiber with better electric conductivity and containing the metal plating layer is used for replacing the traditional carbon fiber, carbon nano tube, graphene and the like, so that the electric conductivity of the heat conduction shielding rubber can be greatly improved, and a better shielding effect is obtained. Meanwhile, due to the designability of the three-dimensional framework, the constructed electric conduction and heat conduction path is quicker and more complete, so that the electric conduction capacity and the shielding performance of the heat conduction shielding rubber are further improved, and the efficient heat conduction shielding rubber material is prepared. Compared with the existing method, the method for preparing the heat-conducting shielding rubber is beneficial to reducing the consumption of filler, improving the electromagnetic field shielding capacity and mechanical property of the heat-conducting shielding rubber, greatly improving the heat dissipation performance of electronic components in the application process, prolonging the service life of electronic equipment and widening the application range of the electronic equipment.
The application also provides electronic equipment, which comprises electronic components and the heat-conducting electromagnetic shielding material dispersed around the electronic components, wherein the heat-conducting electromagnetic shielding material comprises the heat-conducting shielding rubber provided by the application.
The heat conduction shielding rubber prepared by the method has better electromagnetic field shielding capability and mechanical property. The electronic equipment containing the heat conduction shielding material has good heat radiation performance and shielding performance, so that the service life of the electronic equipment can be greatly prolonged, and the application range of the electronic equipment is widened.
The application is described in further detail below in connection with specific examples which are not to be construed as limiting the scope of the application as claimed.
Example 1
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) Nickel-plated graphite fibers (RTP EMI 383FR, monofilament diameter 8.4 μm, plating thickness 0.2 μm, nickel-plated graphite fibers 20%) were used to construct a three-dimensional skeleton using a rapier loom, and the three-dimensional skeleton is shown in FIG. 1. Within one weave cycle, the three-dimensional sandwich fabric comprises 6 warp yarns (numbered 1 to 6) and 20 weft yarns (numbered ① ) Wherein warp yarn 1 and warp yarn 3 weave together an upper surface layer, warp yarn 2 and warp yarn 4 weave together a lower surface layer, warp yarn 5 and warp yarn 6 weave together a middle sandwich layer, the sandwich layer height of the three-dimensional fabric sandwich composite material is 10mm, the sandwich layer spacing is 24mm, and the warp sectional view is shown in figure 2.
(2) 3 Parts by weight of silane coupling agent KH550 is dissolved by using absolute ethyl alcohol of an organic solvent, 150 parts by weight of boron nitride powder (with the particle size of 90-100 nm) is added under the stirring state, the PH value of the mixed solution is adjusted to be 4, 6 parts by weight of deionized water is added, after ultrasonic dispersion is carried out for 40min, heating is carried out to 70 ℃ for stirring, when the solvent is evaporated, the product is dried, and the boron nitride micro powder with the surface treated is obtained.
(3) And (2) premixing 100 parts by weight of room temperature vulcanized silicone rubber base rubber, 0.1 part by weight of titanate and 30 parts by weight of the boron nitride powder micro powder subjected to the surface treatment obtained in the step (2) for 1.5 hours by using mechanical stirring, transferring into a vacuum kneader, repeatedly kneading for 6 hours until uniform, adding the component B in the room temperature vulcanized silicone rubber containing 0.3 part by weight of hydrosilane, and uniformly mixing to obtain the liquid room temperature vulcanized rubber.
(4) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Example 2
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) The nickel-plated graphite fiber was structured into a three-dimensional skeleton using a rapier loom (this step is the same as in example 1).
(2) 3 Parts by weight of silane coupling agent KH550 is dissolved by using absolute ethyl alcohol of an organic solvent, 150 parts by weight of boron nitride powder is added under the stirring state, the PH value of the mixed solution is adjusted to be 4, 6 parts by weight of deionized water is added, ultrasonic dispersion is carried out for 40min, heating is carried out to 70 ℃ for stirring, after solvent evaporation is completed, and the product is dried to obtain the boron nitride micro powder subjected to surface treatment.
(3) And (2) premixing 100 parts by weight of room temperature vulcanized silicone rubber base rubber, 0.1 part by weight of titanate and 30 parts by weight of the boron nitride powder micro powder subjected to the surface treatment obtained in the step (2) by using mechanical stirring for 1.5 hours, transferring into a vacuum kneader for repeated kneading for 6 hours until the mixture is uniform, adding the component B in the room temperature vulcanized silicone rubber containing 0.3 part by weight of hydroxyamino silane, and uniformly mixing to obtain the liquid room temperature vulcanized rubber.
(4) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Example 3
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) The nickel-plated graphite fiber was structured into a three-dimensional skeleton using a rapier loom (this step is the same as in example 1).
(2) 3 Parts by weight of a silane coupling agent KH550 is dissolved by using absolute ethyl alcohol of an organic solvent, boron nitride powder is added under the stirring state, the PH value of the mixed solution is adjusted to be 4, 6 parts by weight of deionized water is added, ultrasonic dispersion is carried out for 40min, heating is carried out to 70 ℃ for stirring, after solvent evaporation is completed, and the product is dried to obtain the boron nitride micro powder subjected to surface treatment.
(3) And (2) premixing 100 parts by weight of room temperature vulcanized silicone rubber base rubber, 0.1 part by weight of titanate and 20 parts by weight of the boron nitride powder micro powder subjected to the surface treatment obtained in the step (2) for 1.5 hours by using mechanical stirring, transferring into a vacuum kneader, repeatedly kneading for 6 hours until uniform, adding the component B in the room temperature vulcanized silicone rubber containing 0.1 part by weight of hydrosilane, and uniformly mixing to obtain the liquid room temperature vulcanized rubber.
(4) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Example 4
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) The nickel-plated graphite fiber was structured into a three-dimensional skeleton using a rapier loom (this step is the same as in example 1).
(2) 3 Parts by weight of a silane coupling agent KH550 is dissolved by using absolute ethyl alcohol of an organic solvent, boron nitride powder is added under the stirring state, the PH value of the mixed solution is adjusted to be 4, 6 parts by weight of deionized water is added, ultrasonic dispersion is carried out for 40min, heating is carried out to 70 ℃ for stirring, after solvent evaporation is completed, and the product is dried to obtain the boron nitride micro powder subjected to surface treatment.
(3) And (2) premixing 100 parts by weight of room temperature vulcanized silicone rubber base rubber, 0.1 part by weight of titanate and 40 parts by weight of the boron nitride powder micro powder subjected to the surface treatment obtained in the step (2) by using mechanical stirring for 1.5 hours, transferring into a vacuum kneader for repeated kneading for 6 hours until the mixture is uniform, adding the component B in the room temperature vulcanized silicone rubber containing 0.5 part by weight of hydrosilane, and uniformly mixing to obtain the liquid room temperature vulcanized rubber.
(4) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Example 5
The difference from example 1 is that the weight ratio of coupling agent to boron nitride is 6:80 and the pH is 7.
Example 6
The difference from example 1 is that the weight ratio of coupling agent to boron nitride is 1:120, the pH is 3, and the ultrasound time is 20min.
Example 7
The difference from example 1 was that the monofilament diameter of the nickel-plated graphite fiber was 6 μm and the plating thickness was 0.1. Mu.m, and the use amount of the nickel-plated graphite fiber was 10% based on 100 parts by weight of the heat conductive shielding rubber.
Example 8
The difference from example 1 was that the monofilament diameter of the nickel-plated graphite fiber was 5 μm and the plating thickness was 0.05 μm, and the use amount of the nickel-plated graphite fiber was 5% based on 100 parts by weight of the heat conductive shielding rubber.
Example 9
The difference from example 1 is that the particle size of boron nitride is 190 to 210nm.
Comparative example 1
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) The nickel-plated graphite fiber was structured into a three-dimensional skeleton using a rapier loom (this step is the same as in example 1).
(2) 100 Parts by weight of room temperature vulcanized silicone rubber base rubber and 0.1 part by weight of titanate are added, and then component B in the room temperature vulcanized silicone rubber containing 0.1 part by weight of hydrosilane is added, and the mixture is uniformly mixed, so that the liquid room temperature vulcanized rubber is obtained.
(3) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Comparative example 2
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) The nickel-plated graphite fiber was structured into a three-dimensional skeleton using a rapier loom (this step is the same as in example 1).
(2) 3 Parts by weight of silane coupling agent KH550 is dissolved by using absolute ethyl alcohol of an organic solvent, 150 parts by weight of boron nitride powder is added under the stirring state, the PH value of the mixed solution is adjusted to be 4, 6 parts by weight of deionized water is added, ultrasonic dispersion is carried out for 40min, heating is carried out to 70 ℃ for stirring, after solvent evaporation is completed, and the product is dried to obtain the boron nitride micro powder subjected to surface treatment.
(3) And (2) premixing 100 parts by weight of room temperature vulcanized silicone rubber base rubber, 0.1 part by weight of titanate and 50 parts by weight of the boron nitride powder micro powder subjected to the surface treatment obtained in the step (2) by using mechanical stirring for 1.5 hours, transferring into a vacuum kneader for repeated kneading for 6 hours until the mixture is uniform, adding the component B in the room temperature vulcanized silicone rubber containing 0.3 part by weight of hydrosilane, and uniformly mixing to obtain the liquid room temperature vulcanized rubber.
(4) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Comparative example 3
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) The carbon fiber was structured into a three-dimensional skeleton using a rapier loom (this step is the same as in example 1).
(2) 3 Parts by weight of silane coupling agent KH550 is dissolved by using absolute ethyl alcohol of an organic solvent, 150 parts by weight of boron nitride powder is added under the stirring state, the PH value of the mixed solution is adjusted to be 4, 6 parts by weight of deionized water is added, ultrasonic dispersion is carried out for 40min, heating is carried out to 70 ℃ for stirring, after solvent evaporation is completed, and the product is dried to obtain the boron nitride micro powder subjected to surface treatment.
(3) And (2) premixing 100 parts by weight of room temperature vulcanized silicone rubber base rubber, 0.1 part by weight of titanate and 30 parts by weight of the boron nitride powder micro powder subjected to the surface treatment obtained in the step (2) for 1.5 hours by using mechanical stirring, transferring into a vacuum kneader, repeatedly kneading for 6 hours until uniform, adding the component B in the room temperature vulcanized silicone rubber containing 0.3 part by weight of hydrosilane, and uniformly mixing to obtain the liquid room temperature vulcanized rubber.
(4) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Comparative example 4
A preparation method of a light high-efficiency shielding rubber sheet comprises the following steps:
(1) The nickel-plated graphite fiber was structured into a three-dimensional skeleton using a rapier loom (this step is the same as in example 1).
(3) And premixing 100 parts by weight of room temperature vulcanized silicone rubber base rubber, 0.1 part by weight of titanate and 30 parts by weight of boron nitride powder micro powder for 1.5 hours by using mechanical stirring, transferring into a vacuum kneader for repeated kneading for 6 hours until the mixture is uniform, adding the component B in the room temperature vulcanized silicone rubber containing 0.3 part by weight of hydrosilane, and uniformly mixing to obtain the liquid room temperature vulcanized rubber.
(4) Transferring the nickel-plated graphite skeleton into a flat plate mold, injecting the prepared liquid room temperature vulcanized rubber into the mold, carrying out vacuum treatment for 2 hours, and then placing the mold in air for room temperature vulcanization to obtain a finished product.
Performance test:
Volume resistivity testing used a Keithley model 2636B digital source table provided by gizzard. And (3) testing: the mode was two electrodes, the operating voltage was 10V, the diameter of the test specimen was about 13mm, the height was 14mm, TGCA and GCA cylinder, and the test was conducted as described in SJ20673-1998, and the average value of 5 tests was taken.
Tensile strength and elongation after break were measured according to GB/T528-2009.
And measuring the heat conductivity coefficient of the cured heat conducting shielding sheet by using a relaxation-resistant LFA457 type laser heat conductivity meter.
The shielding properties of the material were tested by EMC room according to the standard SJ 20524-1995. The sample sizes were 120mm by 2mm. Testing environmental conditions: the temperature is 22.5 ℃; humidity: 45% (RH). The flange coaxial method is adopted, and the test frequency range is 200 KHz-10 GHz. The results are shown in Table 1.
TABLE 1
From the above description, it can be seen that the above embodiments of the present invention achieve the following technical effects:
The graphite fiber with better electric conductivity and containing the metal plating layer is used for replacing the traditional carbon fiber, carbon nano tube, graphene and the like, so that the electric conductivity of the heat conduction shielding rubber can be greatly improved, and a better shielding effect is obtained. Meanwhile, due to the designability of the three-dimensional framework, the constructed electric conduction and heat conduction path is quicker and more complete, so that the electric conduction and heat conduction capability and shielding performance of the heat conduction shielding rubber are further improved, and the efficient heat conduction shielding rubber material is prepared. Compared with the existing method, the method for preparing the heat-conducting shielding rubber is beneficial to reducing the consumption of filler, improving the electromagnetic field shielding capacity and mechanical property of the heat-conducting shielding rubber, greatly improving the heat dissipation performance of electronic components in the application process, prolonging the service life of electronic equipment and widening the application range of the electronic equipment.
It should be noted that the terms "first," "second," and the like in the description and in the claims are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the terms so used are interchangeable under appropriate circumstances such that the embodiments of the application described herein are, for example, capable of operation in sequences other than those described herein.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (13)
1. The preparation method of the heat conduction shielding rubber is characterized by comprising the following steps of:
Adopting graphite fibers containing metal plating layers to construct a three-dimensional framework;
preparing liquid vulcanized silicone rubber mixed with heat conducting filler; and
Filling the three-dimensional framework with the liquid vulcanized silicone rubber mixed with the heat conducting filler, and carrying out vacuum treatment and room temperature vulcanization treatment to obtain the heat conducting shielding rubber;
The monofilament diameter of the graphite fiber containing the metal coating is 6-10 mu m, the coating thickness is 0.1-0.3 mu m, and the addition amount of the graphite fiber containing the metal coating is 10-30% based on 100 parts by weight of the heat conducting shielding rubber;
The preparation method of the liquid vulcanized silicone rubber mixed with the heat conducting filler comprises the following steps: carrying out surface modification on the heat conducting filler by adopting a coupling agent to obtain a surface modified heat conducting filler; the particle size of the heat conducting filler is 50-150 nm;
the surface modification process comprises: mixing the coupling agent with an organic solvent to obtain a first solution; mixing the first solution, the heat-conducting filler and water, and then sequentially performing ultrasonic dispersion, solvent evaporation and drying treatment to obtain the surface-modified heat-conducting filler; the weight ratio of the coupling agent to the heat conducting filler to the water is (1-5) (120-180) (2-10);
After the first solution, the heat conducting filler and water are mixed, the pH of a reaction system is 3-5;
In the step of preparing the liquid vulcanized silicone rubber mixed with the heat conducting filler, the weight of the mixture of the surface modified heat conducting filler, the vulcanized silicone rubber and the catalyst is calculated by 100 parts, the weight of the surface modified heat conducting filler is 20-40 parts, the dosage of the catalyst is 0.01-0.3 part, and the dosage of the cross-linking agent is 0.1-0.5 part.
2. The method of preparing a thermally conductive shielding rubber according to claim 1, wherein the step of constructing a three-dimensional skeleton comprises:
Constructing at least two alternative three-dimensional models;
Analyzing the influence of each alternative three-dimensional model on mechanical properties, and taking the alternative three-dimensional model with the optimal mechanical properties as a target three-dimensional skeleton structure when the consumption of the graphite fibers containing the metal plating layers is the minimum; and
And modeling according to the target three-dimensional framework structure by taking the graphite fiber containing the metal coating as a raw material to obtain the three-dimensional framework.
3. The method for preparing a heat conductive shielding rubber according to claim 1, wherein the step of preparing a liquid heat conductive filler-mixed vulcanized silicone rubber comprises:
Sequentially premixing and vacuum kneading the surface modified heat conducting filler, the vulcanized silicone rubber and the mixture of the catalyst to obtain a pretreated product;
and (3) carrying out a crosslinking reaction on the pretreatment product and the crosslinking agent to obtain the liquid vulcanized silicone rubber mixed with the heat conducting filler.
4. A method of preparing a thermally conductive barrier rubber as claimed in claim 3 wherein the coupling agent is selected from gamma-aminopropyl triethoxysilane and/or methacryloxypropyl trimethoxysilane.
5. The method for producing a heat conductive shielding rubber according to claim 3, wherein the heat conductive filler is one or more selected from the group consisting of boron nitride, aluminum oxide, silicon nitride, and aluminum nitride.
6. The method for producing a heat conductive shielding rubber according to claim 3, wherein the particle size of the heat conductive filler is 90 to 110nm.
7. The method of preparing a heat conductive shielding rubber according to claim 1, wherein after the first solution, the heat conductive filler and water are mixed, the pH of the reaction system is 3-5, the time of the ultrasonic dispersion treatment process is 20-60 min, the temperature of the solvent evaporation process is 60-90 ℃, the temperature of the drying process is 100-130 ℃, and the drying time is 12-24 h.
8. The method for producing a heat conductive shielding rubber according to any one of claims 1 to 7, wherein the graphite fibers containing a metal plating layer are one or more selected from the group consisting of silver-plated graphite fibers, copper-plated graphite fibers, and nickel-plated graphite fibers.
9. The method for preparing a heat conductive shielding rubber according to claim 3, wherein the premixing time is 1-2 hours; the time of the vacuum kneading process is 4-8 hours.
10. The method for producing a heat conductive shielding rubber according to claim 1 or 7, wherein the vulcanized silicone rubber is a linear, branched or micro-crosslinked polysiloxane, and any one of the molecular structures contains at least two or more aliphatic unsaturated double bonds, the viscosity ranges from 300 to 500000 mPa-s, and the chain ends or side chains thereof contain at least two vinyl groups, or α, ω -dihydroxypolydimethylsiloxane-based gums;
The catalyst is one or more selected from the group consisting of platinum compounds, organotin compounds and organotin compounds;
The cross-linking agent is selected from one or more of the group consisting of alkoxysilane, hydrosilane, hydroxyaminosilane, amidosilane and silanol.
11. The method for producing a heat conductive shielding rubber according to claim 1 or 7, wherein the temperature of the room temperature vulcanization treatment is 10 to 35 ℃ and the vulcanization time is 24 to 72 hours.
12. A heat conductive shielding rubber, characterized in that it is produced by the production method according to any one of claims 1 to 11.
13. An electronic device comprising an electronic component and a thermally conductive electromagnetic shielding material dispersed around the electronic component, the thermally conductive electromagnetic shielding material comprising the thermally conductive shielding rubber of claim 12.
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