CN114105529A - High-thermal-conductivity wave-absorbing composite material, preparation method thereof and wave-absorbing heat-conducting gasket - Google Patents
High-thermal-conductivity wave-absorbing composite material, preparation method thereof and wave-absorbing heat-conducting gasket Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 55
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 claims abstract description 71
- 229920005989 resin Polymers 0.000 claims abstract description 47
- 239000011347 resin Substances 0.000 claims abstract description 47
- 239000007788 liquid Substances 0.000 claims abstract description 46
- 229910001338 liquidmetal Inorganic materials 0.000 claims abstract description 39
- 238000003756 stirring Methods 0.000 claims abstract description 38
- 239000002245 particle Substances 0.000 claims abstract description 32
- 239000000945 filler Substances 0.000 claims abstract description 31
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 29
- 238000001723 curing Methods 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 9
- 238000003825 pressing Methods 0.000 claims abstract description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 35
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 25
- 229910003460 diamond Inorganic materials 0.000 claims description 24
- 239000010432 diamond Substances 0.000 claims description 24
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 239000002041 carbon nanotube Substances 0.000 claims description 17
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 17
- 229920002545 silicone oil Polymers 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 15
- -1 phenyl vinyl Chemical group 0.000 claims description 15
- 239000002994 raw material Substances 0.000 claims description 15
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 15
- 229920002554 vinyl polymer Polymers 0.000 claims description 15
- 229920002050 silicone resin Polymers 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 12
- 229910000846 In alloy Inorganic materials 0.000 claims description 9
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 9
- 239000011231 conductive filler Substances 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 230000008018 melting Effects 0.000 claims description 5
- 229910000519 Ferrosilicon Inorganic materials 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 229910001152 Bi alloy Inorganic materials 0.000 claims description 3
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 3
- JWVAUCBYEDDGAD-UHFFFAOYSA-N bismuth tin Chemical compound [Sn].[Bi] JWVAUCBYEDDGAD-UHFFFAOYSA-N 0.000 claims description 3
- YZZNJYQZJKSEER-UHFFFAOYSA-N gallium tin Chemical compound [Ga].[Sn] YZZNJYQZJKSEER-UHFFFAOYSA-N 0.000 claims description 3
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004408 titanium dioxide Substances 0.000 claims description 2
- 239000000084 colloidal system Substances 0.000 abstract description 27
- 230000017525 heat dissipation Effects 0.000 abstract description 8
- 239000011248 coating agent Substances 0.000 abstract description 3
- 238000000576 coating method Methods 0.000 abstract description 3
- 238000000465 moulding Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 21
- 238000004132 cross linking Methods 0.000 description 11
- 238000006243 chemical reaction Methods 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 230000010354 integration Effects 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000011358 absorbing material Substances 0.000 description 6
- 238000000748 compression moulding Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- UJYZRMROGXVXFD-UHFFFAOYSA-N 1-hex-1-ynylcyclohexan-1-ol Chemical group CCCCC#CC1(O)CCCCC1 UJYZRMROGXVXFD-UHFFFAOYSA-N 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000003475 lamination Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical group [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 239000003340 retarding agent Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000011888 foil Substances 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001465 metallisation Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
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- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B26/00—Compositions of mortars, concrete or artificial stone, containing only organic binders, e.g. polymer or resin concrete
- C04B26/30—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Other silicon-containing organic compounds; Boron-organic compounds
- C04B26/32—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Other silicon-containing organic compounds; Boron-organic compounds containing silicon
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/34—Metals, e.g. ferro-silicon
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
- C09K5/14—Solid materials, e.g. powdery or granular
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01Q—ANTENNAS, i.e. RADIO AERIALS
- H01Q17/00—Devices for absorbing waves radiated from an antenna; Combinations of such devices with active antenna elements or systems
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00241—Physical properties of the materials not provided for elsewhere in C04B2111/00
- C04B2111/00258—Electromagnetic wave absorbing or shielding materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Thermal Sciences (AREA)
- Physics & Mathematics (AREA)
- Structural Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Combustion & Propulsion (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
Abstract
The application relates to the field of heat-conducting wave-absorbing composite materials, and particularly discloses a high-heat-conducting wave-absorbing composite material, a preparation method thereof and a wave-absorbing heat-conducting gasket. The high-thermal-conductivity wave-absorbing composite material comprises: liquid resin, heat-conducting filler, liquid metal, wave-absorbing powder, a retarder, a curing agent and a catalyst. The preparation method comprises the following steps: mixing the heat-conducting filler with liquid metal, and then coating the liquid metal on the surfaces of the heat-conducting filler particles by heating and stirring; adding liquid resin and wave absorbing powder, and further stirring until the mixture is uniformly mixed; cooling to room temperature, sequentially adding a delay agent and a curing agent, stirring, adding a catalyst, and continuously stirring until the mixture is uniformly mixed to obtain a colloid of the high-thermal-conductivity wave-absorbing composite material; and pressing and molding the colloid to obtain the wave-absorbing heat-conducting gasket. The wave-absorbing heat-conducting gasket prepared from the high-heat-conduction wave-absorbing composite material has high heat-conducting performance and excellent wave-absorbing performance, and can effectively improve the heat dissipation problem and the electromagnetic interference problem of electronic products.
Description
Technical Field
The application relates to the field of heat-conducting wave-absorbing composite materials, in particular to a high-heat-conducting wave-absorbing composite material, a preparation method thereof and a wave-absorbing heat-conducting gasket.
Background
With the rapid popularization of the internet, various electronic products are gradually developing toward miniaturization, refinement and high power, resulting in a great increase in the integration density of transistors on an electronic chip. The greatly increased integration of electronic transistors means that more heat is generated by the electronic components packaged in the circuit board. If the heat generated in the operation process of the electronic components is not conducted in time, the heat in the electronic product can be rapidly accumulated, the working temperature of the electronic components is rapidly increased, and the normal operation of the electronic equipment is influenced. Meanwhile, due to the integration development of electronic components, the distances among various elements in the electronic product are reduced, so that electromagnetic wave interference is easily generated among the electronic components, and the normal work of the electronic equipment is influenced.
In order to solve the problems of heat dissipation and electromagnetic interference caused by high integration of electronic devices, the conventional means at present is to adopt conductive foam, copper foil, aluminum foil or rubber wave-absorbing materials on electronic products to conduct heat and play a role in heat dissipation while solving the problem of electromagnetic interference. In addition, some electronic products are adhered with heat-conducting gaskets and wave-absorbing materials to achieve the double functions of heat conduction and wave absorption of the electronic products.
However, the heat conduction coefficient of the wave-absorbing material on the market is generally below 1W/(m.K), the heat conduction effect is limited, and the good heat dissipation effect cannot be achieved; and the mode of realizing the double functions of heat conduction and wave absorption through the lamination of the heat conduction gasket and the wave absorption material can influence the thickness of the electronic product on one hand, and on the other hand, two layers of interface thermal resistances exist after the lamination, so that the heat conduction effect in practical application can be reduced.
Disclosure of Invention
In order to solve the problems of heat dissipation and electromagnetic interference of electronic products caused by high integration of electronic components, the application provides a high-thermal-conductivity wave-absorbing composite material, a preparation method thereof and a wave-absorbing heat-conducting gasket.
In a first aspect, the present application provides a high thermal conductivity wave-absorbing composite material, which adopts the following technical scheme:
a high-thermal-conductivity wave-absorbing composite material is prepared from the following raw materials in parts by weight:
by adopting the technical scheme, the heat-conducting filler and the wave-absorbing powder are uniformly dispersed in the liquid resin to play the roles of heat conduction and electromagnetic interference reduction. The heat-conducting filler has good heat-conducting property, the wave-absorbing powder can absorb electromagnetic waves, the liquid resin is used as a carrier, the heat-conducting filler, the wave-absorbing powder and the liquid resin are mixed, and the liquid resin is crosslinked and cured to obtain the composite material with good wave-absorbing property and excellent heat-conducting property.
In the process of mixing the heat-conducting filler, the wave-absorbing powder and the liquid resin, the uniformity of mixing can be improved by adding the liquid metal. The liquid metal and the liquid resin have good compatibility, and the liquid metal is used as a bridging agent between the powder (mainly the heat-conducting filler) and the colloid (the liquid resin), so that the liquid metal is uniformly coated on the surface of the powder to improve the compatibility between the powder and the liquid resin, further improve the dispersion uniformity of the heat-conducting filler in the liquid resin, and further improve the heat conduction performance. Meanwhile, the liquid metal has certain heat conduction performance, so that the heat conduction effect of the composite material can be further improved.
The addition of the curing agent and the catalyst can promote the crosslinking reaction of the liquid resin, and facilitate the curing and molding of the liquid resin to prepare a required product. In the process of curing the liquid resin, in order to allow sufficient working time for the raw materials to be mixed, a retarder is also added to retard the crosslinking curing of the liquid resin. The retarder can inhibit the crosslinking rate of the liquid resin at normal temperature, and allow enough time for the mixing operation to ensure that all raw materials are uniformly mixed.
In the technical scheme, the heat-conducting filler and the wave-absorbing powder are simultaneously dispersed and mixed in the liquid resin, and the liquid metal is added to improve the compatibility between the powder and the colloid, so that the prepared high-heat-conducting wave-absorbing composite material has high heat-conducting property and excellent electromagnetic wave absorption property. The composite material is applied to electronic products, and can effectively solve the problems of heat dissipation and electromagnetic interference caused by high integration of electronic devices.
Preferably, the heat conducting filler is one or more of diamond micropowder, carbon nanotubes and spherical aluminum nitride. Further preferably, the heat conducting filler is a combination of three of diamond micro powder, carbon nanotubes and spherical aluminum nitride.
Preferably, the particle size of the diamond micro powder is 150-350 μm; the length of the carbon nano tube is 10-100 mu m; the particle size of the spherical aluminum nitride is 40-100 mu m.
By adopting the technical scheme, the diamond micro powder, the carbon nano tube and the spherical aluminum nitride are all substances with good heat conductivity, and play a main heat conducting role in a composite material mixed system. The particle size of the heat-conducting filler needs to be kept in a proper range, the heat-conducting filler is easy to agglomerate when the particle size is too small, and the heat-conducting filler is difficult to disperse uniformly in liquid resin planting; when the particle size of the heat conductive filler is too large, it is difficult to disperse the heat conductive filler in the liquid resin, and the coating of the liquid metal is also affected.
Preferably, the wave absorbing powder is one of carbonyl iron powder, ferrosilicon aluminum powder, ferrosilicon nickel powder and titanium dioxide powder. Further preferably, the wave absorbing powder is carbonyl iron powder.
Preferably, the particle size of the wave-absorbing powder is 2-10 μm.
By adopting the technical scheme, the wave absorbing powder mainly plays a role in absorbing electromagnetic waves in a composite material system so as to weaken electromagnetic interference. The wave-absorbing powder is uniformly dispersed in the liquid resin and is matched with the heat-conducting filler to play double functions of wave absorption and heat conduction. When the particle size of the wave-absorbing powder is too small, the wave-absorbing powder is easy to agglomerate and is difficult to disperse uniformly; when the particle size of the wave-absorbing powder is too large, the wave-absorbing powder is not easy to be mixed and dispersed with liquid resin, and the performance of the composite material for absorbing electromagnetic waves is influenced.
Preferably, the liquid metal is one of gallium-indium alloy, gallium-tin alloy, indium-tin alloy, tin-bismuth alloy and gallium-indium-tin alloy. More preferably, the liquid metal is a gallium indium alloy.
Preferably, the melting point of the liquid alloy is not higher than 120 ℃.
By adopting the technical scheme, the liquid metal plays a role in connecting the powder and the colloid in the composite material mixed system. The alloy such as gallium-indium alloy, gallium-tin alloy, indium-tin alloy, tin-bismuth alloy, gallium-indium-tin alloy and the like has a low melting point, is solid at normal temperature, can be melted at a low temperature, has good heat-conducting property, has good compatibility with resin materials, and can be stably connected with liquid resin. After the liquid metal is added, the liquid metal is coated on the surface of the powder particles, so that the compatibility between the powder and the colloid can be enhanced. The liquid metal needs to be completely melted into a molten state when being added, so the melting point of the liquid metal is not too high, the energy consumption during heating and melting is reduced, and the influence on other raw materials caused by too high temperature during mixing and heating is avoided.
Preferably, the liquid resin is one or two of vinyl silicone oil and phenyl vinyl silicone resin. More preferably, the liquid resin is a combination of vinyl silicone oil and phenyl vinyl resin, and the viscosity is 300-5000 mpa-s.
Preferably, the catalyst is a platinum catalyst; the retarder is hexynyl cyclohexanol; the curing agent is hydrogen-containing silicone oil.
In a second aspect, the application provides a preparation method of a high thermal conductivity wave-absorbing composite material, which adopts the following technical scheme: a preparation method of a high-thermal-conductivity wave-absorbing composite material comprises the following steps:
s1, mixing a heat-conducting filler with liquid metal, and then heating and stirring to enable the liquid metal to be coated on the surfaces of heat-conducting filler particles;
s2, adding the liquid resin and the wave absorbing powder into the mixture obtained in the step S1, and further stirring until the mixture is uniformly mixed;
and S3, cooling the mixture obtained in the step S2 to room temperature, sequentially adding a delay agent and a curing agent, stirring and mixing uniformly, adding a catalyst, and continuously stirring until the mixture is uniformly mixed to obtain the high-thermal-conductivity wave-absorbing composite material.
Preferably, the heating temperature in step S1 is 100-.
By adopting the technical scheme, when mixing materials, the liquid metal is melted in a molten state by heating, and then the liquid metal is coated on the surface of the heat-conducting filler powder under the action of centrifugal force by stirring. The liquid metal is heated to 100-120 ℃ to ensure that the liquid metal is completely melted to a molten state and has good fluidity, so that the surface of the heat-conducting filler powder can be better coated. A certain stirring speed needs to be kept during stirring, and when the stirring speed is lower than 3500r/min, the centrifugal force is too small, so that the liquid metal cannot be completely coated on the surface of the heat-conducting filler powder; when the stirring speed is higher than 5000r/min, the centrifugal force is too large, and the liquid metal is easy to be thrown away from the surface of the heat-conducting filler powder in the stirring process, so that the liquid metal coated on the surface of the heat-conducting filler powder is too thin and even can not be coated.
After the liquid metal is uniformly coated on the surface of the heat-conducting filler powder, the liquid metal is mixed with the liquid resin and the wave-absorbing powder, and the heat-conducting filler powder coated on the surface of the liquid metal has good compatibility with the liquid resin, so that the wave-absorbing powder is easily dispersed in the liquid resin. Therefore, the uniform dispersion of the heat-conducting filler and the wave-absorbing powder in the liquid resin can be realized, and all the heat-conducting filler and the wave-absorbing powder have good connection strength with the liquid resin.
In order to promote the crosslinking and curing of the liquid resin and facilitate the preparation of products by later-stage compression molding, a curing agent and a catalyst are also required to be added, the curing agent can promote the crosslinking reaction of the liquid resin, the liquid resin is easy to cure and mold, and the catalyst plays a role in catalyzing the crosslinking reaction. Meanwhile, in order to avoid that the liquid resin cannot be mixed due to too high crosslinking reaction speed, a delay agent can be added to delay the time of the liquid resin crosslinking reaction. The retarder can inhibit the crosslinking reaction rate of the liquid resin at normal temperature, and sufficient time is reserved for the mixing operation to ensure the uniformity of mixing; meanwhile, after the retarder is added, the self-crosslinking curing speed of the composite material colloid is greatly inhibited at normal temperature, and the normal-temperature storage time of the composite material colloid can be prolonged.
In a third aspect, the present application provides a wave-absorbing heat-conducting gasket, which adopts the following technical scheme:
a wave-absorbing heat-conducting gasket is made of the high-heat-conduction wave-absorbing composite material provided by the technical scheme. Specifically, the colloid of the high-thermal-conductivity wave-absorbing composite material prepared in the technical scheme is pressed and molded in a vacuum environment, and then is heated, dried and cured to obtain the wave-absorbing heat-conducting gasket.
Preferably, the curing temperature after the compression molding is 80-120 ℃, and the curing time is 15-30 min.
By adopting the technical scheme, the wave-absorbing heat-conducting gasket prepared by using the colloid of the high-heat-conducting wave-absorbing composite material provided by the technical scheme has high heat-conducting property and high wave-absorbing property, and can effectively improve the heat dissipation problem and the electromagnetic interference problem of electronic equipment caused by high integration of electronic components.
The high-thermal-conductivity wave-absorbing composite material provided by the technical scheme is colloidal at normal temperature, and the wave-absorbing heat-conducting gasket with the specified thickness and size can be prepared by compression molding. And vacuumizing treatment is carried out before compression molding, and air doped in the colloid is pumped out, so that the influence of bubbles in the wave-absorbing heat-conducting gasket after compression molding on the strength and the heat-conducting effect of the wave-absorbing heat-conducting gasket is avoided.
After compression molding, the reaction between the curing agent and the liquid resin is promoted by heating, the catalytic efficiency of the catalyst is improved, the inhibition effect of the retarder on the crosslinking reaction is reduced, the liquid resin is further accelerated to crosslink and cure, and the prepared wave-absorbing heat-conducting gasket achieves certain strength and hardness.
In summary, the present application has the following beneficial effects:
1. in the application, the heat-conducting filler with ultrahigh heat-conducting effect and the wave-absorbing powder with excellent wave-absorbing performance are uniformly dispersed in the liquid resin to prepare the high-heat-conducting wave-absorbing composite material, so that the high-heat-conducting performance and the excellent wave-absorbing performance are integrated. And the liquid metal is added as a bridging agent between the powder raw material and the colloid raw material, so that the compatibility and the connection strength between the powder raw material and the colloid raw material are improved. The wave-absorbing heat-conducting gasket prepared from the high-heat-conduction wave-absorbing composite material has the characteristics of high heat conduction and high wave-absorbing capacity, can simultaneously solve the problems of heat dissipation and electromagnetic interference of electronic equipment, and has wide application prospect in the field of Yunnan West products.
2. The wave-absorbing powder can be selected to be matched with wave-absorbing powders of different types and particle sizes, so that the absorption frequency band of the product to electromagnetic waves can be widened, the absorption capacity of the electromagnetic waves can be improved, and the application range of the product can be further expanded.
Detailed Description
The present application will be described in further detail with reference to examples and comparative examples. The following examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer; the starting materials used in the following examples are all those conventionally commercially available except where specifically noted.
Diamond micropowder and spherical aluminum nitride used in the embodiment of the application are powder subjected to surface modification. Wherein, the surface of the diamond micropowder is subjected to metallization pretreatment to improve the compatibility with liquid metal, and the spherical aluminum nitride is subjected to hydrolysis-resistant surface coating treatment to enhance the hydrolysis resistance of the spherical aluminum nitride. The following examples are given for the purpose of illustration and are carried out under conventional conditions or conditions recommended by the manufacturer, and the starting materials used in the following examples are all commercially available from ordinary sources except for the specific ones.
In the embodiment and the comparative example, the liquid metal is gallium-indium alloy, and the wave absorbing powder is carbonyl iron powder.
Some of the raw material sources used in the examples and comparative examples of the present application are shown in table 1 below:
table 1: part of raw material sources in the examples and comparative examples of the application
| Raw materials | Type (B) | Manufacturer(s) | Model number |
| Vinyl silicone oil | / | Guangzhou Xin thick chemical industry | / |
| Phenyl vinyl silicone resin | / | Guangzhou Xin thick chemical industry | AM-8071 |
| Retarding agent | Hexynylcyclohexanols | Middle-mountain jun | PH |
| Curing agent | Hydrogen-containing silicone oil | Guangzhou Chen Si (silicon of Guangzhou) | CX-350 |
Examples
Examples 1 to 7
The wave-absorbing heat-conducting gasket is prepared by the following method:
according to the dosage in the table 2, putting the diamond micro powder, the spherical aluminum nitride and the gallium-indium alloy into a stirrer with a heating function, heating to 120 ℃, and stirring at a constant speed of 4000r/min for 30 min; then adding vinyl silicone oil, phenyl vinyl silicone resin and carbonyl iron powder, continuing stirring for 15min, and cooling to room temperature; sequentially adding a delay agent and a curing agent, stirring for 5min at the rotating speed of 2500r/min, adding a catalyst, and continuously stirring for 5min to obtain a finally uniformly mixed high-thermal-conductivity wave-absorbing composite material;
pressing colloid of the high-heat-conduction wave-absorbing composite material on a forming machine to a specified thickness and size under a vacuum environment of-0.1 MPa to obtain a preliminarily formed wave-absorbing heat-conducting gasket;
and (3) moving the preliminarily molded wave-absorbing heat-conducting gasket into an oven, and drying at the temperature of 100-120 ℃ for 30min to obtain the finally stably molded wave-absorbing heat-conducting gasket.
Wherein the average grain diameter of the diamond micro powder is 180 μm, the average grain diameter of the spherical aluminum nitride is 80 μm, the average length of the carbon nano tube is 60 μm, and the average grain diameter of the carbonyl iron powder is 5 μm.
The viscosity of the vinyl silicone oil was 300 mPas, and the viscosity of the phenyl vinyl silicone resin was 2000 mPas.
Table 2: EXAMPLES 1-7 amount of raw Material (unit: g)
Example 8
The difference between this example and example 7 is that carbonyl iron powder with an average particle size of 2 μm and carbonyl iron powder with an average particle size of 7.8 μm were selected and mixed, wherein 300g of carbonyl iron powder with an average particle size of 2 μm and 350g of carbonyl iron powder with an average particle size of 7.8 μm were selected as carbonyl iron powder.
Example 9
This example differs from example 8 in that 200g of 2 μm carbonyl iron powder and 450g of 7.8 μm carbonyl iron powder.
Example 10
This example differs from example 8 in that 500g of 2 μm carbonyl iron powder and 150g of 7.8 μm carbonyl iron powder.
Example 11
This example is different from example 7 in that the amount of vinyl silicone oil added was 75g, and the amount of phenyl vinyl silicone resin added was 0.
Example 12
This example is different from example 11 in that the amount of diamond fine powder added was 530g, and the amounts of spherical aluminum nitride and carbon nanotubes added were both 0.
Example 13
The present example is different from example 11 in that the amount of addition of the diamond fine powder was 300g, the amount of addition of the spherical aluminum nitride was 230g, and the amount of addition of the carbon nanotube was 0.
Example 14
This example is different from example 7 in that the average particle diameter of the diamond fine powder was 100 μm, the average particle diameter of the spherical aluminum nitride was 20 μm, and the average length of the carbon nanotube was 5 μm.
Example 15
This example is different from example 14 in that the average particle diameter of the diamond fine powder was 500 μm, the average particle diameter of the spherical aluminum nitride was 150 μm, and the average length of the carbon nanotube was 150 μm.
Comparative example
Comparative example 1
The wave-absorbing heat-conducting gasket is prepared by the following method:
putting 60g of vinyl silicone oil, 15g of phenyl vinyl silicone resin and 650g of carbonyl iron powder into a stirrer with a heating function, heating to 120 ℃, uniformly stirring for 15min at a rotating speed of 4000r/min, uniformly mixing, cooling to room temperature, sequentially adding 0.15g of retarder and 5.5g of curing agent, uniformly stirring for 5min at a rotating speed of 2500r/min, then adding 6g of catalyst, and continuously stirring for 5min at a uniform speed to obtain a colloid of the finally uniformly mixed high-thermal-conductivity wave-absorbing composite material;
pressing colloid of the high-heat-conduction wave-absorbing composite material on a forming machine to a specified thickness and size under a vacuum environment of-0.1 MPa to obtain a preliminarily formed wave-absorbing heat-conducting gasket;
and (3) moving the preliminarily molded wave-absorbing heat-conducting gasket into an oven, and drying at the temperature of 100-120 ℃ for 30min to obtain the finally stably molded wave-absorbing heat-conducting gasket.
Wherein the average grain diameter of the diamond micro powder is 180 μm, the average grain diameter of the spherical aluminum nitride is 80 μm, and the average length of the carbon nano tube is 60 μm;
the carbonyl iron powder is a combination of carbonyl iron powder with an average particle size of 2 mu m and carbonyl iron powder with an average particle size of 7.8 mu m, wherein 500g of the carbonyl iron powder with an average particle size of 2 mu m and 150g of the carbonyl iron powder with an average particle size of 7.8 mu m are selected as the carbonyl iron powder.
Comparative example 2
The wave-absorbing heat-conducting gasket is prepared by the following method:
putting 280g of diamond micro powder, 200g of spherical aluminum nitride and 50g of gallium-indium alloy into a stirrer with a heating function, heating to 120 ℃, and stirring at a constant speed of 4000r/min for 30 min; then adding 60g of vinyl silicone oil, 15g of phenyl vinyl silicone resin and 650g of carbonyl iron powder, continuing stirring for 15min, and cooling to room temperature; then, 0.15g of retarder and 5.5g of curing agent are sequentially added, the mixture is stirred for 5min at the rotating speed of 2500r/min, then 6g of catalyst is added, the mixture is continuously stirred for 5min, and finally the colloid of the high-thermal-conductivity wave-absorbing composite material which is uniformly mixed is obtained;
pressing colloid of the high-heat-conduction wave-absorbing composite material on a forming machine to a specified thickness and size under a vacuum environment of-0.1 MPa to obtain a preliminarily formed wave-absorbing heat-conducting gasket;
and (3) moving the preliminarily molded wave-absorbing heat-conducting gasket into an oven, and drying at the temperature of 100-120 ℃ for 30min to obtain the finally stably molded wave-absorbing heat-conducting gasket.
Wherein the average grain diameter of the diamond micro powder is 180 μm, the average grain diameter of the spherical aluminum nitride is 80 μm, and the average length of the carbon nano tube is 60 μm;
comparative example 3
The wave-absorbing heat-conducting gasket is prepared by the following method:
putting 280g of diamond micro powder and 200g of spherical aluminum nitride into a stirrer with a heating function, heating to 120 ℃, and stirring at a constant speed of 4000r/min for 30 min; then adding 60g of vinyl silicone oil, 15g of phenyl vinyl silicone resin and 650g of carbonyl iron powder, continuing stirring for 15min, and cooling to room temperature; then, 0.15g of retarder and 5.5g of curing agent are sequentially added, the mixture is stirred for 5min at the rotating speed of 2500r/min, then 6g of catalyst is added, the mixture is continuously stirred for 5min, and finally the colloid of the high-thermal-conductivity wave-absorbing composite material which is uniformly mixed is obtained;
pressing colloid of the high-heat-conduction wave-absorbing composite material on a forming machine to a specified thickness and size under a vacuum environment of-0.1 MPa to obtain a preliminarily formed wave-absorbing heat-conducting gasket;
and (3) moving the preliminarily molded wave-absorbing heat-conducting gasket into an oven, and drying at the temperature of 100-120 ℃ for 30min to obtain the finally stably molded wave-absorbing heat-conducting gasket.
Wherein the average grain diameter of the diamond micro powder is 180 μm, the average grain diameter of the spherical aluminum nitride is 80 μm, and the average length of the carbon nano tube is 60 μm.
Comparative example 4
The wave-absorbing heat-conducting gasket is prepared by the following method:
putting 280g of diamond micro powder, 200g of spherical aluminum nitride and 50g of gallium-indium alloy into a stirrer, and stirring at a constant speed of 4000r/min for 30 min; then adding 60g of vinyl silicone oil and 15g of phenyl vinyl silicone resin, continuing stirring for 15min, and cooling to room temperature; then sequentially adding 0.15g of retarder and 5.5g of curing agent, stirring for 5min at the rotating speed of 2500r/min, then adding 6g of catalyst, and continuously stirring for 5min to obtain uniformly mixed heat conduction material colloid;
pressing colloid of the heat conduction material on a forming machine to a specified thickness and size under a vacuum environment of-0.1 MPa to obtain a preliminarily formed heat conduction gasket;
putting 60g of vinyl silicone oil, 15g of phenyl vinyl silicone resin and 650g of carbonyl iron powder into a stirrer, stirring at a constant speed of 4000r/min for 15min, then sequentially adding 0.15g of delay agent and 5.5g of curing agent, stirring at a speed of 2500r/min for 5min, then adding 6g of catalyst, and continuing stirring for 5min to obtain a colloid of the uniformly mixed wave-absorbing material;
pressing colloid of the wave-absorbing material on a forming machine to a specified thickness and size under a vacuum environment of-0.1 MPa to obtain a preliminarily formed wave-absorbing gasket;
bonding the heat-conducting gasket and the wave-absorbing gasket together on a bonding machine by utilizing self viscosity to obtain a bonded wave-absorbing heat-conducting gasket; and (4) moving the attached wave-absorbing heat-conducting gasket into an oven, and drying at the temperature of 100-120 ℃ for 30min to obtain the finally stably-formed wave-absorbing heat-conducting gasket.
Wherein the average grain diameter of the diamond micro powder is 180 μm, the average grain diameter of the spherical aluminum nitride is 80 μm, and the average length of the carbon nano tube is 60 μm.
The carbonyl iron powder is a combination of carbonyl iron powder with an average particle size of 2 μm and carbonyl iron powder with an average particle size of 7.8 μm, wherein 500g of the carbonyl iron powder with an average particle size of 2 μm and 150g of the carbonyl iron powder with an average particle size of 7.8 μm are selected as the carbonyl iron powder.
Comparative examples 5 to 8
The wave-absorbing heat-conducting gasket is prepared by the following method:
referring to the dosage in the table 3, the diamond micro powder, the spherical aluminum nitride and the gallium-indium alloy are put into a stirrer with a heating function, heated to 120 ℃, and stirred at a constant speed of 4000r/min for 30 min; then adding vinyl silicone oil, phenyl vinyl silicone resin and carbonyl iron powder, continuing stirring for 15min, and cooling to room temperature; sequentially adding a delay agent and a curing agent, stirring for 5min at the rotating speed of 2500r/min, adding a catalyst, and continuously stirring for 5min to obtain a finally uniformly mixed colloid of the high-thermal-conductivity wave-absorbing composite material;
pressing colloid of the high-heat-conduction wave-absorbing composite material on a forming machine to a specified thickness and size under a vacuum environment of-0.1 MPa to obtain a preliminarily formed wave-absorbing heat-conducting gasket;
and (3) moving the preliminarily molded wave-absorbing heat-conducting gasket into an oven, and drying at the temperature of 100-120 ℃ for 30min to obtain the finally stably molded wave-absorbing heat-conducting gasket.
Wherein the average grain diameter of the diamond micro powder is 180 μm, the average grain diameter of the spherical aluminum nitride is 80 μm, the average length of the carbon nano tube is 60 μm, and the average grain diameter of the carbonyl iron powder is 5 μm;
the viscosity of the vinyl silicone oil was 300 mPas, and the viscosity of the phenyl vinyl silicone resin was 2000 mPas.
Table 3: COMPARATIVE EXAMPLES 5 to 8 amount (unit: g) of raw materials
| Raw materials | Comparative example 5 | Comparative example 6 | Comparative example 7 | Comparative example 8 |
| Vinyl silicone oil | 60 | 60 | 60 | 60 |
| Phenyl vinyl silicone resin | 15 | 15 | 15 | 15 |
| Diamond micropowder | 80 | 450 | 280 | 280 |
| Carbon nanotube | 10 | 100 | 50 | 50 |
| Spherical aluminum nitride | 50 | 450 | 200 | 200 |
| Liquid metal | 50 | 50 | 50 | 50 |
| Carbonyl iron powder | 650 | 650 | 400 | 1000 |
| Retarding agent | 0.15 | 0.15 | 0.15 | 0.15 |
| Curing agent | 5.5 | 5.5 | 5.5 | 5.5 |
| Catalyst and process for preparing same | 6 | 6 | 6 | 6 |
Performance test
The performance of the wave-absorbing heat-conducting gaskets prepared in the embodiments 1 to 15 and the comparative examples 1 to 8 is tested.
Detection method
Testing the thermal conductivity of the product according to ASTM D5470;
testing the hardness of the product according to ASTM D2240 standard;
testing the tensile strength of the product according to ASTM D412;
testing the volume resistivity of the product according to ASTM D257 standard;
the absorption capacity of the product to electromagnetic waves is tested according to the GJB 2038A standard, and the interval with the reflection loss of the electromagnetic waves less than-5 dB/cm is taken as an effective absorption frequency band.
Performance testing data are shown in table 4 below.
Table 4: data for testing the Performance of examples 1-15 and comparative examples 1-8
By combining the data in the embodiments 1 to 15, the comparative examples 1 to 8 and the data in table 4, in the embodiment of the present application, the heat conductive filler and the wave absorbing powder are matched in the liquid resin system, and then the liquid metal is used to improve the compatibility between the heat conductive filler powder and the liquid resin, the high heat conductive wave absorbing composite material is prepared by reasonable proportioning, and then the wave absorbing heat conductive gasket prepared by the composite material has high heat conductive performance and excellent broadband wave absorbing characteristic.
The wave-absorbing heat-conducting gasket provided by the embodiment of the application has the advantages that the heat conductivity coefficient can reach 20W/(m.K), the effective wave-absorbing frequency band can reach 5-20GHz, the electromagnetic wave absorption peak value can be reached at 15GHz, and the absorption reflection loss at 15GHz can reach more than-40 dB/cm at most through tests. Meanwhile, the wave-absorbing heat-conducting gasket provided by the embodiment of the application has the tensile strength of more than 0.1MPa and the Shore C hardness of more than 40And a volume resistivity of 1010Omega cm, and has good mechanical strength and electrical insulation.
By combining the data in example 10, comparative example 3 and table 4, the heat conductivity of the wave-absorbing heat-conducting gasket can be further improved by adding liquid metal as a bridging agent between the heat-conducting filler powder and the liquid resin colloid, and the mechanical strength of the wave-absorbing heat-conducting gasket is also further improved.
By combining the data in examples 7-10, comparative example 2 and table 4, the wave-absorbing heat-conducting gasket has obvious absorption capacity due to the addition of the wave-absorbing powder, and the electromagnetic interference problem of electronic products can be effectively improved when the wave-absorbing heat-conducting gasket is applied to electronic equipment. Meanwhile, the absorption frequency band and the electromagnetic wave absorption capacity of the wave-absorbing heat-conducting gasket can be further widened by reasonably matching carbonyl iron powder with different particle sizes.
By combining the data in the embodiment 8, the comparative examples 3 to 4 and the data in the table 4, compared with the conventional wave-absorbing gasket or the wave-absorbing heat-conducting gasket manufactured by attaching the wave-absorbing material and the heat-conducting gasket, the wave-absorbing heat-conducting gasket provided by the embodiment of the application has obvious advantages in the aspects of heat-conducting property and wave-absorbing property.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (10)
1. The high-thermal-conductivity wave-absorbing composite material is characterized by being prepared from the following raw materials in parts by weight:
50-80 parts of liquid resin;
800 portions of heat-conducting filler;
50-200 parts of liquid metal;
800 portions of wave absorbing powder;
0.1-0.5 part of a retarder;
5-10 parts of a curing agent;
5-10 parts of a catalyst.
2. The composite material of claim 1, wherein the thermally conductive filler is one or more of diamond micropowder, carbon nanotubes, and spherical aluminum nitride.
3. The composite material as claimed in claim 2, wherein the diamond micro powder has a particle size of 150-350 μm; the length of the carbon nano tube is 10-100 mu m; the particle size of the spherical aluminum nitride is 40-100 mu m.
4. The composite material of claim 1 or 3, wherein the wave-absorbing powder is one of carbonyl iron powder, ferrosilicon aluminum powder, ferrosilicon nickel powder and titanium dioxide powder.
5. The composite material of claim 4, wherein the particle size of the absorbing powder is 2-10 μm.
6. The composite material of claim 1, wherein the liquid metal is one of gallium-indium alloy, gallium-tin alloy, indium-tin alloy, tin-bismuth alloy, and gallium-indium-tin alloy.
7. A high thermal conductivity and wave absorption composite material according to claim 6, wherein the melting point of the liquid metal is not higher than 120 ℃.
8. The composite material of claim 1, wherein the liquid resin is one or a combination of vinyl silicone oil and phenyl vinyl silicone resin.
9. The preparation method of the high-thermal-conductivity wave-absorbing composite material of any one of claims 1 to 8, which is characterized by comprising the following steps of:
s1, mixing the heat-conducting filler with liquid metal, heating to 120 ℃ at 100-;
s2, adding the liquid resin and the wave-absorbing powder into the mixture obtained in the step S1, and further stirring until the mixture is uniformly mixed;
and S3, cooling the mixture obtained in the step S2 to room temperature, sequentially adding a delay agent and a curing agent, stirring and mixing uniformly, adding a catalyst, and continuously stirring until the mixture is uniformly mixed to obtain the high-thermal-conductivity wave-absorbing composite material.
10. A wave-absorbing heat-conducting gasket is characterized in that: the high thermal conductivity wave-absorbing composite material prepared by the method of any one of claims 1 to 8 or the high thermal conductivity wave-absorbing composite material prepared by the method of claim 9 is prepared by vacuum pressing and heating and curing, wherein the heating temperature is 80-120 ℃, and the heating time is 15-30 min.
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