CN109627781B - Organic silicon graphite composite thermal interface material and preparation method and application thereof - Google Patents
Organic silicon graphite composite thermal interface material and preparation method and application thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 121
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 74
- 239000010439 graphite Substances 0.000 title claims abstract description 74
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002131 composite material Substances 0.000 title claims abstract description 50
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 19
- 239000010703 silicon Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 28
- 239000002210 silicon-based material Substances 0.000 claims abstract description 8
- 239000003292 glue Substances 0.000 claims description 36
- 229920002554 vinyl polymer Polymers 0.000 claims description 36
- 239000003054 catalyst Substances 0.000 claims description 34
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 32
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 31
- -1 phthalate ester Chemical class 0.000 claims description 31
- 239000001257 hydrogen Substances 0.000 claims description 30
- 229910052739 hydrogen Inorganic materials 0.000 claims description 30
- 238000000034 method Methods 0.000 claims description 24
- 239000002994 raw material Substances 0.000 claims description 22
- 239000003431 cross linking reagent Substances 0.000 claims description 19
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 18
- 238000007731 hot pressing Methods 0.000 claims description 13
- 239000003112 inhibitor Substances 0.000 claims description 13
- 229910052697 platinum Inorganic materials 0.000 claims description 13
- 238000004026 adhesive bonding Methods 0.000 claims description 11
- 229920001721 polyimide Polymers 0.000 claims description 11
- 239000007822 coupling agent Substances 0.000 claims description 10
- 238000007598 dipping method Methods 0.000 claims description 10
- 238000007493 shaping process Methods 0.000 claims description 9
- 229920003235 aromatic polyamide Polymers 0.000 claims description 7
- 238000010030 laminating Methods 0.000 claims description 7
- 239000012756 surface treatment agent Substances 0.000 claims description 7
- 239000004642 Polyimide Substances 0.000 claims description 6
- 229920002545 silicone oil Polymers 0.000 claims description 6
- 229920002050 silicone resin Polymers 0.000 claims description 6
- 238000003763 carbonization Methods 0.000 claims description 5
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 5
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 4
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 238000010000 carbonizing Methods 0.000 claims description 4
- 150000004696 coordination complex Chemical class 0.000 claims description 4
- 150000002736 metal compounds Chemical class 0.000 claims description 4
- 239000004814 polyurethane Substances 0.000 claims description 4
- 229920002635 polyurethane Polymers 0.000 claims description 4
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 claims description 4
- 239000004760 aramid Substances 0.000 claims description 3
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical compound C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 claims description 2
- 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 2
- 239000004971 Cross linker Substances 0.000 claims description 2
- 239000004593 Epoxy Substances 0.000 claims description 2
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 2
- 125000001931 aliphatic group Chemical group 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- UJTGYJODGVUOGO-UHFFFAOYSA-N diethoxy-methyl-propylsilane Chemical compound CCC[Si](C)(OCC)OCC UJTGYJODGVUOGO-UHFFFAOYSA-N 0.000 claims description 2
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 2
- 229910052763 palladium Inorganic materials 0.000 claims description 2
- MOVRCMBPGBESLI-UHFFFAOYSA-N prop-2-enoyloxysilicon Chemical compound [Si]OC(=O)C=C MOVRCMBPGBESLI-UHFFFAOYSA-N 0.000 claims description 2
- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-UHFFFAOYSA-N 0.000 claims description 2
- 150000002909 rare earth metal compounds Chemical class 0.000 claims description 2
- 229910052703 rhodium Inorganic materials 0.000 claims description 2
- 239000010948 rhodium Substances 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- QBERHIJABFXGRZ-UHFFFAOYSA-M rhodium;triphenylphosphane;chloride Chemical compound [Cl-].[Rh].C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1.C1=CC=CC=C1P(C=1C=CC=CC=1)C1=CC=CC=C1 QBERHIJABFXGRZ-UHFFFAOYSA-M 0.000 claims description 2
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 claims description 2
- 239000011995 wilkinson's catalyst Substances 0.000 claims description 2
- 229920006335 epoxy glue Polymers 0.000 claims 2
- 125000004122 cyclic group Chemical group 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000000413 hydrolysate Substances 0.000 claims 1
- DQZNLOXENNXVAD-UHFFFAOYSA-N trimethoxy-[2-(7-oxabicyclo[4.1.0]heptan-4-yl)ethyl]silane Chemical compound C1C(CC[Si](OC)(OC)OC)CCC2OC21 DQZNLOXENNXVAD-UHFFFAOYSA-N 0.000 claims 1
- 238000012856 packing Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 8
- DBAMUTGXJAWDEA-UHFFFAOYSA-N Butynol Chemical compound CCC#CO DBAMUTGXJAWDEA-UHFFFAOYSA-N 0.000 description 7
- 230000017525 heat dissipation Effects 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000011049 filling Methods 0.000 description 5
- 229910021389 graphene Inorganic materials 0.000 description 5
- 229920005989 resin Polymers 0.000 description 5
- 239000011347 resin Substances 0.000 description 5
- 239000003822 epoxy resin Substances 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000012299 nitrogen atmosphere Substances 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000004891 communication Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000007790 scraping Methods 0.000 description 3
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 150000004645 aluminates Chemical class 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000010354 integration Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000010295 mobile communication Methods 0.000 description 2
- 239000009719 polyimide resin Substances 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 229920006231 aramid fiber Polymers 0.000 description 1
- 238000013473 artificial intelligence Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- SBRXLTRZCJVAPH-UHFFFAOYSA-N ethyl(trimethoxy)silane Chemical compound CC[Si](OC)(OC)OC SBRXLTRZCJVAPH-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-L phthalate(2-) Chemical compound [O-]C(=O)C1=CC=CC=C1C([O-])=O XNGIFLGASWRNHJ-UHFFFAOYSA-L 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions 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; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Laminated Bodies (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
本发明提供了一种有机硅石墨复合热界面材料及其制备方法和应用，所述有机硅石墨复合热界面材料包括具有蜂窝结构的石墨骨架以及填充在蜂窝结构内的有机硅材料。本发明的热界面材料包括有机硅与蜂窝状石墨骨架，既保留了有机硅柔软的贴合性又具有石墨骨架良好的导热性，有机硅材料填充在石墨骨架的蜂窝结构内，使本发明的热界面材料在较低的填充密度下具有较高的纵向导热性能，并且蜂窝结构可以进一步提高有机硅材料的抗拉强度，以及延长在恶劣环境下的使用寿命。The present invention provides an organosilicon-graphite composite thermal interface material and a preparation method and application thereof. The organosilicon-graphite composite thermal interface material includes a graphite skeleton with a honeycomb structure and an organosilicon material filled in the honeycomb structure. The thermal interface material of the present invention includes organic silicon and honeycomb graphite skeleton, which not only retains the soft fit of organic silicon but also has good thermal conductivity of the graphite skeleton. The organic silicon material is filled in the honeycomb structure of the graphite skeleton, so that the Thermal interface materials have higher longitudinal thermal conductivity at lower packing densities, and the honeycomb structure can further improve the tensile strength of silicone materials and prolong the service life in harsh environments.
Description
Technical Field
The invention belongs to the technical field of thermal interface materials, and relates to an organic silicon graphite composite thermal interface material, and a preparation method and application thereof.
Background
The fifth generation mobile communication (5G) is a new generation mobile communication system oriented to the demand of the information society in 2020, has the characteristics of high frequency spectrum utilization rate, large data traffic, low network energy consumption, high reliability, short time delay and the like, and is the basis of application and innovation of new generation information technologies such as Internet of things, unmanned driving, telemedicine, artificial intelligence and the like. Breakthrough of the 5G communication technology and expansion of application scenes promote revolutionary development of the intelligent terminal, and bring new opportunities for development of the thermal interface material industry. Particularly, as the intelligent terminal is continuously developed to ultra-high system integration, miniaturization and high density, the electronic device (especially a power device) generates high-density heat in the working process, which causes the rapid temperature rise and the rapid reliability decrease of the electronic product. According to the Arrhenius formula, the lifetime of the device decreases by 50% for every 10 ℃ rise in temperature. Therefore, the heat dissipation problem has become a critical issue to be solved urgently in the new generation of electronic products.
The thermal interface material plays a very important role in thermal management as an effective heat dissipation solution, becomes one of key technologies influencing the future development of thermal management technology, and attracts people's extensive attention. The silicone thermal interface material is a mainstream material for transferring energy between a heating part and a radiating part, has good flexibility, electrical insulation and ductility, and is an ideal choice for a heat transfer material in electronic equipment. However, the silicone heat conductive material in the prior art is filled with high heat conductive ceramic particles such as alumina, zinc oxide, quartz powder, aluminum nitride, boron nitride, silicon carbide and the like in silicone, and has low heat conductivity (longitudinal heat conductivity is difficult to exceed 8W · m)-1·K-1) High density and high hardness.
CN102746670A discloses a heat dissipation interface material for high-power LED lamp packaging and a preparation method thereof, the heat dissipation interface material is prepared by taking flexible AB two-component condensation type room temperature curing organic silicon resin as a matrix, adding dimethyl silicone oil and functionalized graphene micro-sheets as heat conducting fillers and fully mixing, and the functionalized graphene micro-sheets and the silicon resin are fully mixed on a double-roller mill during preparation, so that the functionalized graphene is uniformly dispersed in the silicon resin matrix, thereby preparing the heat dissipation interface material with excellent performance. CN107686699A discloses a heat-conducting interface material and a preparation method thereof, the heat-conducting interface material includes: the method comprises the following steps of (1) preparing a graphene composite interface material gasket, spraying resin and heat-conducting and insulating powder; spraying a mixture of resin and heat-conducting insulating powder, and covering the mixture on the graphene composite interface material gasket; the insulation of the heat-conducting interface material is increased, but the heat conductivity of the material is still low and the density of the material is too high, so that the application requirements cannot be met.
Therefore, it is urgently needed to develop a high thermal conductivity organic silicon thermal interface material to ensure the stable and continuous operation and the application popularization of 5G communication terminal equipment.
Disclosure of Invention
The invention aims to provide an organic silicon-graphite composite thermal interface material and a preparation method and application thereof, and the organic silicon-graphite composite thermal interface material provided by the invention has the advantages of high thermal conductivity, light density and better strength, and is particularly suitable for application requirements of light weight and high thermal conductivity of new energy automobiles, 5G communication equipment and the like.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a silicone-graphite composite thermal interface material, which includes a graphite skeleton having a honeycomb structure and a silicone material filled in the honeycomb structure.
The thermal interface material disclosed by the invention comprises the organic silicon and the honeycomb-shaped graphite framework, the soft attaching property of the organic silicon is kept, the thermal conductivity of the graphite framework is good, and the organic silicon material is filled in the honeycomb structure of the graphite framework, so that the thermal interface material disclosed by the invention has higher longitudinal thermal conductivity under lower filling density, and the honeycomb structure can further improve the tensile strength of the organic silicon material and prolong the service life of the thermal interface material, especially the service life of the thermal interface material under severe environments.
The graphite with the honeycomb structure is used as the framework, the integration of the heat conduction paths is realized by the graphite framework with the honeycomb structure, the thermal contact resistance of heat conduction network channels among powder in the traditional technology can be obviously reduced, the vertical arrangement of the heat conduction paths is realized, and the using amount of heat conduction materials is greatly reduced, so that the light high-heat-conduction organic silicon graphite thermal interface material is obtained, and the heat dissipation problem of an application product can be effectively solved.
Preferably, the raw materials for preparing the organosilicon material comprise polyvinyl siloxane, a crosslinking agent and a catalyst.
Preferably, the mass ratio of the polyvinyl siloxane, the crosslinking agent and the catalyst is 100 (1-25): 0.01-2.5, such as 100:2:0.05, 100:5:0.1, 100:8:0.5, 100:10:1, 100:15:1.5, 100:20:2 and the like.
Preferably, the polyvinyl siloxane is a linear polyvinyl siloxane, a branched polyvinyl siloxane, a dendritic polyvinyl siloxane, or a slightly crosslinked polyvinyl siloxane.
Preferably, the molecular structure of the polyvinyl siloxane contains at least two aliphatic unsaturated double bonds.
Preferably, the molecular structure of the polyvinyl siloxane contains at least two vinyl groups.
Preferably, the viscosity of the polyvinyl siloxane is 300-500000 mPas, such as 400 mPas, 500 mPas, 1000 mPas, 5000 mPas, 10000 mPas, 50000 mPas, 100000 mPas, 400000 mPas, etc.
Preferably, the cross-linking agent is any one of linear hydrogen-containing silicone oil, annular hydrogen-containing silicone resin or branched cross-linked hydrogen-containing silicone resin or a combination of at least two of the linear hydrogen-containing silicone oil, the annular hydrogen-containing silicone resin and the branched cross-linked hydrogen-containing silicone resin.
Preferably, the molecular structure of the cross-linking agent contains at least two silicon-hydrogen bonds.
Preferably, the crosslinking agent has a viscosity of 10 to 10000 mPas, for example, 50 mPas, 100 mPas, 120 mPas, 150 mPas, 200 mPas, 250 mPas, 400 mPas, 500 mPas, 800 mPas, 1000 mPas, 1200 mPas, 1500 mPas, 1800 mPas, 2000 mPas, 2500 mPas, 2800 mPas, and the like, and more preferably 100 and 3000 mPas.
Preferably, the crosslinker has a hydrogen content of 0.02 to 1.52%, e.g., 0.05%, 0.08%, 0.1%, 0.2%, 0.5%, 0.8%, 1.0%, 1.2%, 1.4%, 1.5%, etc.
Preferably, the catalyst is any one or a combination of at least two of a rare earth metal compound, a group VIII metal compound or metal complex, a group VII metal compound or metal complex, more preferably any one or a combination of at least two of a platinum-based catalyst, a rhodium-based catalyst or a palladium-based catalyst, still more preferably any one or a combination of at least two of a Speier catalyst, a Karstedt catalyst or a Wilkinson catalyst, and most preferably a Speier catalyst.
Preferably, the Speier catalyst has a Pt content of 100-5000ppm, such as 200ppm, 300 ppm, 500ppm, 800ppm, 1000ppm, 2000ppm, 3000ppm, 4000ppm, and the like.
Preferably, the raw materials for preparing the organosilicon material also comprise an inhibitor and a surface treating agent.
Preferably, the mass ratio of the inhibitor and surface treatment agent to the polyvinyl siloxane is (0.2-3.0): 0.5-8.0):100, e.g., 0.5:1:100, 1:2:100, 1.5:3:100, 2:4:100, 2.5:6:100, etc.
Preferably, the inhibitor is an alkynol compound and/or a polyvinyl silicone oil.
Preferably, the surface treatment agent comprises any one or a combination of at least two of a vinyl silane coupling agent, an epoxy coupling agent, an acryloxy silane coupling agent, a phthalate coupling agent, a zirconate coupling agent, an aluminate coupling agent or an aluminate coupling agent hydrolysate, further preferably any one or a combination of at least two of gamma-methacryloxypropyl trimethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3- (2, 3-glycidoxy) propylmethyldiethoxysilane, 2- (3, 4-epoxycyclohexylalkyl) ethyltrimethoxysilane, isopropyl tristearate, n-butyl titanate, bis (acetylacetonate) ethoxyisopropoxytitanate, bis (triethanolamine) diisopropyl titanate or tetra-n-propyl zirconate, 3-glycidoxypropyltrimethoxysilane is more preferable.
In a second aspect, the present invention provides a method of making the silicone graphite composite thermal interface material according to the first aspect, the method comprising: dipping the graphite framework with the honeycomb structure in an organic silicon material glue solution and curing to obtain the organic silicon graphite composite thermal interface material.
Preferably, the preparation method of the graphite skeleton with the honeycomb structure comprises the following steps:
(1) gluing, laminating and hot-pressing the raw material paper to obtain a honeycomb laminated block;
(2) and stretching and shaping the honeycomb stacked block, and then carbonizing to obtain the graphite framework with the honeycomb structure.
Preferably, the raw paper comprises any one of meta-aramid paper, para-aramid paper, or polyimide film, or a combination of at least two of them.
Preferably, the raw paper has a thickness of 15-500 μm, such as 20 μm, 25 μm, 30 μm, 40 μm, 50 μm, 80 μm, 100 μm, 150 μm, 200 μm, 300 μm, 400 μm, 450 μm, and the like.
Preferably, said gluing is carried out on a glue roll.
Preferably, the glue solution used for gluing is any one of epoxy resin glue, polyurethane glue, acrylate glue or polyimide glue or a combination of at least two of the epoxy resin glue, the polyurethane glue, the acrylate glue and the polyimide glue.
Preferably, the honeycomb core cell diameter of the honeycomb stack is 0.5-10mm, such as 1mm, 2mm, 3mm, 4mm, 5mm, 6mm, 7mm, 8mm, 9mm, and the like.
Preferably, the honeycomb core cell thickness of the honeycomb stack is 5-50mm, such as 10mm, 15mm, 20mm, 25mm, 30mm, 35mm, 40mm, 45mm, and the like.
Preferably, the temperature for the shaping is 280-350 ℃, such as 290 ℃, 300 ℃, 310 ℃, 320 ℃, 330 ℃, 340 ℃ and the like.
Preferably, the setting time is 0.5-1h, such as 0.6h, 0.7h, 0.8h, 0.9h, etc.
Preferably, the carbonization is performed in a tube furnace.
Preferably, the temperature of the carbonization is 1200-3000 ℃, such as 1500 ℃, 2000 ℃, 2500 ℃, 2800 ℃ and the like.
Preferably, the carbonization time is 2-3h, such as 2.2h, 2.4h, 2.5h, 2.6h, 2.8h, etc.
Preferably, the gumming is performed in a gumming machine.
Preferably, the curing temperature is 140-160 ℃, such as 142 ℃, 145 ℃, 147 ℃, 150 ℃, 152 ℃, 155 ℃, 157 ℃ and the like.
Preferably, the curing time is 20-40min, such as 22min, 25min, 27min, 30min, 32min, 35min, 37min, and the like.
In a third aspect, the invention provides an application of the organosilicon graphite composite thermal interface material according to the first aspect in new energy automobiles or electronic components.
Compared with the prior art, the invention has the following beneficial effects:
(1) the thermal interface material disclosed by the invention comprises organic silicon and a honeycomb-shaped graphite framework, the soft attaching property of the organic silicon is kept, the thermal interface material also has good thermal conductivity of the graphite framework, and the organic silicon material is filled in a honeycomb structure of the graphite framework, so that the thermal interface material disclosed by the invention has higher longitudinal thermal conductivity under lower filling density, and the honeycomb structure can further improve the tensile strength of the organic silicon material and prolong the service life under severe environment;
(2) the light high-thermal-conductivity organic silicon graphite thermal interface material has the advantages of high thermal conductivity and low density, wherein the maximum thermal conductivity can reach more than 10W/m.K, and the minimum density is 1.2g/cm3The following.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
An organosilicon-graphite composite thermal interface material is composed of a graphite skeleton with a honeycomb structure and an organosilicon material filled in the honeycomb structure.
Wherein, the raw material for preparing the organosilicon material consists of 100 weight parts of polyvinyl siloxane, 5.5 weight parts of methyl hydrogen-containing polysiloxane cross-linking agent, 0.3 weight part of platinum catalyst, 0.2 weight part of butynol inhibitor and 1.5 weight parts of KH-560 surface treating agent.
Wherein the viscosity of the polyvinyl siloxane is 1000 mPa.s; the viscosity of the methyl hydrogen-containing polysiloxane cross-linking agent is 100 mPa.s, and the hydrogen content is 0.8%; the Pt content of the platinum catalyst was 2000 ppm.
The preparation method comprises the following steps:
(1) using para-aramid fiber paper with the thickness of 50 mu m as raw material paper, gluing by using a glue spreader stained with core strip glue, laminating a plurality of layers of glued raw material paper in staggered layers, and finally hot-pressing by using a hot press to prepare a honeycomb laminated block with the hole size of 1.83mm and the thickness of 6 mm.
Wherein the core strip glue is high-temperature epoxy resin glue, and the viscosity is 20s/50 mL; when hot pressing, preheating at 80 deg.C for 10min, gelling at 150 deg.C for 30min, and curing at 170 deg.C for 2 hr under 5 MPa.
(2) And (3) stretching the honeycomb stacked block at a stretching speed of 5mm/min by using a stretcher to form a regular hexagonal honeycomb cell, then shaping at a high temperature of 280 ℃/30min, and then transferring to a 1200 ℃ tubular furnace to carbonize for 240min under a nitrogen atmosphere to prepare the graphite framework with the honeycomb structure.
(3) Dipping the graphite framework with the honeycomb structure in a dipping machine, and curing at 150 ℃/30min to obtain the organic silicon-graphite composite thermal interface material.
Example 2
An organosilicon-graphite composite thermal interface material is composed of a graphite skeleton with a honeycomb structure and an organosilicon material filled in the honeycomb structure.
Wherein, the raw material for preparing the organosilicon material consists of 100 weight parts of polyvinyl siloxane, 2.5 weight parts of methyl hydrogen-containing polysiloxane cross-linking agent, 0.05 weight part of platinum catalyst, 0.25 weight part of butynol inhibitor and 3.0 weight parts of KH-560 surface treating agent.
Wherein the viscosity of the polyvinyl siloxane is 400 mPa.s; the viscosity of the methyl hydrogen-containing polysiloxane cross-linking agent is 50 mPa.s, and the hydrogen content is 1.5%; the Pt content of the platinum catalyst was 3000 ppm.
The preparation method comprises the following steps:
(1) the method comprises the following steps of taking meta-aramid fiber paper with the thickness of 25 mu m as raw material paper, gluing by using a glue spreader stained with core strip glue, laminating a plurality of layers of glued raw material paper in a staggered manner, and finally hot-pressing by using a hot press to prepare a honeycomb laminated block with the hole size of 1.0mm and the thickness of 10 mm.
Wherein the core strip glue is high-temperature epoxy resin glue, and the viscosity is 20s/50 mL; when hot pressing, preheating at 80 deg.C for 10min, gelling at 150 deg.C for 30min, and curing at 170 deg.C for 2 hr under 5 MPa.
(2) And (3) stretching the honeycomb stacked block at a stretching speed of 5mm/min by using a stretcher to form a regular hexagonal honeycomb cell, then shaping at a high temperature of 280 ℃/30min, and then transferring to a 1500 ℃ tubular furnace to carbonize for 180min under a nitrogen atmosphere to prepare the graphite framework with the honeycomb structure.
(3) Dipping the graphite framework with the honeycomb structure in a dipping machine, and curing at 150 ℃/30min to obtain the organic silicon-graphite composite thermal interface material.
Example 3
An organosilicon-graphite composite thermal interface material is composed of a graphite skeleton with a honeycomb structure and an organosilicon material filled in the honeycomb structure.
Wherein, the raw material for preparing the organosilicon material consists of 100 weight parts of polyvinyl siloxane, 3.5 weight parts of methyl hydrogen-containing polysiloxane cross-linking agent, 0.5 weight part of platinum catalyst, 0.2 weight part of butynol inhibitor and 2.0 weight parts of KH-560 surface treating agent.
Wherein the viscosity of the polyvinyl siloxane is 500000 mPas; the viscosity of the methyl hydrogen-containing polysiloxane cross-linking agent is 1000 mPa.s, and the hydrogen content is 1.0 percent; the Pt content of the platinum catalyst was 5000 ppm.
The preparation method comprises the following steps:
(1) using polyimide fiber paper with the thickness of 30 mu m as raw material paper, gluing by using a glue spreader stained with core strip glue, laminating a plurality of layers of glued raw material paper in staggered layers, and finally hot-pressing by using a hot press to prepare a honeycomb laminated block with the hole size of 0.5mm and the thickness of 5 mm.
Wherein the core strip glue is high-temperature polyimide resin glue, and the viscosity is 15s/50 mL; when hot pressing, preheating at 100 ℃ for 30min, then gelling at 150 ℃ for 60min, and finally curing at 200 ℃ for 2h, wherein the hot pressing pressure is 7 MPa.
(2) And (3) stretching the honeycomb stacked block at a stretching speed of 5mm/min by using a stretcher to form a regular hexagonal honeycomb cell, then shaping at a high temperature of 350 ℃/60min, and then transferring to a 3000 ℃ tubular furnace to carbonize for 120min under a nitrogen atmosphere to prepare the graphite framework with the honeycomb structure.
(3) Dipping the graphite framework with the honeycomb structure in a dipping machine, and curing at 150 ℃/30min to obtain the organic silicon-graphite composite thermal interface material.
Example 4
An organosilicon-graphite composite thermal interface material is composed of a graphite skeleton with a honeycomb structure and an organosilicon material filled in the honeycomb structure.
Wherein, the raw material for preparing the organosilicon material consists of 100 weight parts of polyvinyl siloxane, 25 weight parts of methyl hydrogen-containing polysiloxane cross-linking agent, 2.5 weight parts of platinum catalyst, 3 weight parts of butynol inhibitor and 3.0 weight parts of KH-560 surface treating agent.
Wherein the polyvinyl siloxane is a mixture of 80 parts of vinyl terminated polysiloxane with the viscosity of 500 mPas and 20 parts of vinyl terminated polysiloxane with the viscosity of 30000 mPas; the methyl hydrogen-containing polysiloxane cross-linking agent is prepared from 20 parts of hydrogen-containing polysiloxane (viscosity is 3000mPa & s, hydrogen content is 0.05%) and 5 parts of hydrogen-containing polysiloxane (viscosity is 50mPa & s, hydrogen content is 0.8%); the Pt content of the platinum catalyst was 100 ppm.
The preparation method comprises the following steps:
(1) using polyimide fiber paper with the thickness of 400 mu m as raw material paper, gluing by using a glue spreader stained with core strip glue, laminating a plurality of layers of glued raw material paper in staggered layers, and finally hot-pressing by using a hot press to prepare a honeycomb laminated block with the hole size of 10mm and the thickness of 50 mm.
Wherein the core strip glue is high-temperature polyimide resin glue, and the viscosity is 15s/50 mL; when in hot pressing, the steel is preheated at 100 ℃ for 30min, then 180 ℃/60min, 230 ℃/60min and the hot pressing pressure is 7 MPa.
(2) And (3) stretching the honeycomb stacked block at a stretching speed of 5mm/min by using a stretcher to form a regular hexagonal honeycomb cell, then shaping at a high temperature of 350 ℃/60min, and then transferring to a 3000 ℃ tubular furnace to carbonize for 120min under a nitrogen atmosphere to prepare the graphite framework with the honeycomb structure.
(3) Dipping the graphite framework with the honeycomb structure in a dipping machine, and curing at 150 ℃/30min to obtain the organic silicon-graphite composite thermal interface material.
Comparative example 1
A thermal interface material is prepared by the preparation method provided by the prior art, and the method comprises the following steps:
(1) adding 50 parts by weight of 1000 mPas vinyl terminated polysiloxane into a reaction kettle, then sequentially adding 1.2 parts by weight of methyl hydrogenpolysiloxane, 3 parts by weight of vinyl trimethoxy silane, 650 parts by weight of alumina with the particle size of 30 micrometers, 350 parts by weight of alumina with the particle size of 3.5 micrometers, 0.3 part by weight of platinum catalyst and 0.005 part by weight of butynol inhibitor, and stirring the materials in a vacuum manner for 30min by a high-speed power mixer to obtain a uniformly mixed material.
(2) And filling the mixed material after stirring and mixing into a frame-shaped mold with the thickness of 2mm, wherein the frame-shaped mold is an upper open mold, so that the upper surface of the material is convenient to cure and mold. After the material filled into the frame-shaped die is leveled, scraping out the redundant material by using a scraper; and (3) putting the mould filled with the mixed material into an oven, curing for 15min at the temperature of 100 ℃, and curing and forming to obtain the thermal interface material with the thickness of 2 mm.
Comparative example 2
The preparation method provided by the prior art is used for preparing the organic silicon graphite composite thermal interface material, and comprises the following steps:
(1) adding 100 parts by weight of 500mPa s polyvinyl siloxane into a reaction kettle, and then sequentially adding 22 parts by weight of methyl hydrogen polysiloxane, 3 parts by weight of vinyl trimethoxy silane, 1900 parts by weight of alumina with the particle size of 30 micrometers, 600 parts by weight of alumina with the particle size of 3.5 micrometers, 0.3 part by weight of platinum catalyst and 0.005 part by weight of butynol inhibitor, and stirring the materials in a high-speed power mixer for 30min in vacuum to obtain a uniformly mixed material;
(2) and filling the mixed material after stirring and mixing into a frame-shaped mold with the thickness of 2mm, wherein the frame-shaped mold is an upper open mold, so that the upper surface of the material is convenient to cure and mold. After the material filled into the frame-shaped die is leveled, scraping out the redundant material by using a scraper; and (3) putting the mould filled with the mixed material into an oven, curing for 15min at the temperature of 100 ℃, and curing and forming to obtain the thermal interface material with the thickness of 2 mm.
Comparative example 3
The preparation method provided by the prior art is used for preparing the organic silicon graphite composite thermal interface material, and comprises the following steps:
(1) adding 100 parts by weight of 1000 mPas vinyl-terminated polysiloxane into a reaction kettle, then sequentially adding 20 parts by weight of methyl hydrogen-containing polysiloxane, 3 parts by weight of vinyl trimethoxy silane, 150 parts by weight of crystalline flake graphite with the particle size of 30 micrometers, 0.3 part by weight of platinum catalyst and 0.005 part by weight of butynol inhibitor, and stirring the materials in a high-speed power mixer for 30min in vacuum to obtain a uniformly mixed material.
(2) And filling the mixed material after stirring and mixing into a frame-shaped mold with the thickness of 2mm, wherein the frame-shaped mold is an upper open mold, so that the upper surface of the material is convenient to cure and mold. After the material filled into the frame-shaped die is leveled, scraping out the redundant material by using a scraper; and (3) putting the mould filled with the mixed material into an oven, curing for 15min at the temperature of 100 ℃, and curing and forming to obtain the thermal interface material with the thickness of 2 mm.
Performance testing
The thermal interface materials provided in examples 1-4 and comparative examples 1-3 were tested for performance by the following methods:
(1) thermal conductivity: according to the ASTM D5470 standard, the heat conductivity coefficient tester LW-9389 of Taiwan Ruiz is adopted for testing, the sample size is 2.54 multiplied by 2.54cm, and the thickness is 2 mm;
(2) density: the density of the sample was measured by a DX-200F Density balance, Switzerland, according to ASTM D792 Standard;
(3) tensile strength: the test was carried out according to ASTM D412 using a universal tensile tester Zwick Allround Z050TEH, Germany.
The test results are shown in table 1:
TABLE 1
| Sample (I) | Thermal conductivity (W/m. K) | Density (g/cm)3) | Tensile Strength (KPa) |
| Example 1 | 4.51 | 1.12 | 1380 |
| Example 2 | 6.92 | 1.21 | 1530 |
| Example 3 | 10.75 | 1.27 | 1910 |
| Example 4 | 15.23 | 1.31 | 2560 |
| Comparative example 1 | 3.00 | 3.60 | 126 |
| Comparative example 2 | 6.05 | 3.75 | 86 |
| Comparative example 3 | 2.37 | 1.54 | 259 |
The embodiment and the performance test show that the thermal interface material provided by the invention has the advantages of high thermal conductivity and low density, wherein the thermal conductivity can reach more than 15W/m.K at most, and the density is 1.15g/cm at least3The following. As can be seen from the comparison between examples 1-4 and comparative examples 1-3, the honeycomb graphite skeleton and the organosilicon material are selected, so that the honeycomb graphite skeleton and the organosilicon material have the advantages of high heat conductivity and low density while the consumption of heat conductive materials is saved.
The applicant states that the present invention is illustrated by the above examples to show the silicone graphite composite thermal interface material of the present invention, its preparation method and application, but the present invention is not limited to the above detailed method, i.e. it does not mean that the present invention must be implemented by relying on the above detailed method. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
Claims (38)
1. The organic silicon-graphite composite thermal interface material is characterized by comprising a graphite framework with a honeycomb structure and an organic silicon material filled in the honeycomb structure;
the graphite skeleton with the honeycomb structure is prepared by adopting the following method, and the method comprises the following steps:
(1) gluing, laminating and hot-pressing the raw material paper to obtain a honeycomb laminated block;
(2) stretching and shaping the honeycomb stacked block, and then carbonizing to obtain the graphite framework with the honeycomb structure;
the raw material paper comprises any one or combination of at least two of meta-aramid paper, para-aramid paper or polyimide film.
2. The silicone-graphite composite thermal interface material of claim 1, wherein the silicone material is prepared from raw materials comprising a polyvinyl siloxane, a cross-linking agent, and a catalyst.
3. The silicone-graphite composite thermal interface material of claim 2, wherein the mass ratio of the polyvinyl siloxane to the cross-linking agent to the catalyst is 100 (1-25) to (0.01-2.5).
4. The silicone-graphite composite thermal interface material of claim 2, wherein the polyvinyl siloxane is a linear polyvinyl siloxane, a branched polyvinyl siloxane, a dendritic polyvinyl siloxane, or a micro-crosslinked polyvinyl siloxane.
5. The silicone-graphite composite thermal interface material of claim 2, wherein the molecular structure of the polyvinyl siloxane contains at least two aliphatic unsaturated double bonds.
6. The silicone-graphite composite thermal interface material of claim 5, wherein the molecular structure of the polyvinyl siloxane contains at least two vinyl groups.
7. The silicone-graphite composite thermal interface material of claim 2, wherein the polyvinyl siloxane has a viscosity of 300-500000 mPa-s.
8. The silicone-graphite composite thermal interface material of claim 2, wherein the cross-linking agent is any one of or a combination of at least two of linear hydrogen-containing silicone oil, cyclic hydrogen-containing silicone resin, or branched cross-linked hydrogen-containing silicone resin.
9. The silicone-graphite composite thermal interface material of claim 2, wherein the cross-linking agent comprises at least two silicon-hydrogen bonds in its molecular structure.
10. The silicone-graphite composite thermal interface material of claim 2, wherein the cross-linking agent has a viscosity of 10 to 10000 mPa-s.
11. The silicone-graphite composite thermal interface material of claim 10, wherein the cross-linking agent has a viscosity of 100-3000 mPa-s.
12. The silicone-graphite composite thermal interface material of claim 2, wherein the crosslinker has a hydrogen content of 0.02-1.52%.
13. The silicone-graphite composite thermal interface material of claim 2, wherein the catalyst is any one of or a combination of at least two of a rare earth metal compound, a group VIII metal compound or metal complex, a group VII metal compound or metal complex.
14. The silicone-graphite composite thermal interface material of claim 2, wherein the catalyst is any one of a platinum-based catalyst, a rhodium-based catalyst, or a palladium-based catalyst, or a combination of at least two thereof.
15. The silicone-graphite composite thermal interface material of claim 2, wherein the catalyst is any one of a Speier catalyst, a Karstedt catalyst, or a Wilkinson catalyst, or a combination of at least two thereof.
16. The silicone-graphite composite thermal interface material of claim 15, wherein the catalyst is a Speier catalyst.
17. The silicone-graphite composite thermal interface material of claim 15 or 16, wherein the Speier catalyst has a Pt content of 100-5000 ppm.
18. The silicone-graphite composite thermal interface material of claim 2, wherein the raw materials for preparing the silicone material further comprise an inhibitor and a surface treatment agent.
19. The silicone-graphite composite thermal interface material of claim 18, wherein the mass ratio of the inhibitor and surface treatment agent to polyvinyl siloxane is (0.2-3.0): (0.5-8.0): 100.
20. The silicone graphite composite thermal interface material of claim 18, wherein the inhibitor is an alkynol compound and/or a polyvinyl silicone oil.
21. The silicone-graphite composite thermal interface material of claim 18, wherein the surface treatment agent comprises any one of or a combination of at least two of a vinyl silane coupling agent, an epoxy coupling agent, an acryloxy silane coupling agent, a phthalate ester coupling agent, a zirconate ester coupling agent, an aluminate ester coupling agent, or an aluminate ester coupling agent hydrolysate.
22. The silicone-graphite composite thermal interface material of claim 21, wherein the surface treatment agent is any one of γ -methacryloxypropyltrimethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3- (2, 3-glycidoxy) propylmethyldiethoxysilane, 2- (3, 4-epoxycyclohexyl) ethyltrimethoxysilane, isopropyl tristearate, n-butyl titanate, bis (acetylacetonate) ethoxyisopropoxytitanate, bis (triethanolamine) diisopropyl titanate, or tetra-n-propylzirconate, or a combination of at least two thereof.
23. The silicone-graphite composite thermal interface material of claim 22, wherein the surface treatment agent is 3-glycidoxypropyltrimethoxysilane.
24. The method of making the silicone graphite composite thermal interface material of any one of claims 1-23, comprising: dipping a graphite framework with a honeycomb structure in an organic silicon material glue solution and curing to obtain the organic silicon graphite composite thermal interface material;
the graphite framework of the honeycomb structure is prepared by adopting the following method, and the method comprises the following steps:
(1) gluing, laminating and hot-pressing the raw material paper to obtain a honeycomb laminated block;
(2) stretching and shaping the honeycomb stacked block, and then carbonizing to obtain a graphite framework with a honeycomb structure;
the raw material paper comprises any one or combination of at least two of meta-aramid paper, para-aramid paper or polyimide film.
25. The method of claim 24, wherein the raw paper has a thickness of 15 to 500 μm.
26. A method as claimed in claim 24, wherein said gluing is carried out on a glue roll.
27. The preparation method according to claim 24, wherein the glue solution for gluing is any one of epoxy glue, polyurethane glue, acrylate glue or polyimide glue or a combination of at least two of the epoxy glue, the polyurethane glue, the acrylate glue and the polyimide glue.
28. The method of claim 24, wherein the honeycomb stack has a honeycomb core cell diameter of 0.5 to 10 mm.
29. The method of claim 24, wherein the honeycomb stack has a honeycomb core cell thickness of 5-50 mm.
30. The method as claimed in claim 24, wherein the temperature for the shaping is 280-350 ℃.
31. The method of claim 24, wherein the setting time is 0.5 to 1 hour.
32. The method of claim 24, wherein the carbonizing is performed in a tube furnace.
33. The method as claimed in claim 24, wherein the carbonization temperature is 1200-3000 ℃.
34. The method of claim 24, wherein the carbonization time is 2-3 hours.
35. The method of claim 24, wherein the gumming is performed in a gumming machine.
36. The method as claimed in claim 24, wherein the curing temperature is 140-160 ℃.
37. The method of claim 24, wherein the curing time is 20-40 min.
38. The application of the silicone graphite composite thermal interface material according to any one of claims 1 to 23 in new energy automobiles or electronic components.
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