CN113956683B - Heat-conducting insulating filler, preparation method thereof and heat-conducting insulating composite material - Google Patents
Heat-conducting insulating filler, preparation method thereof and heat-conducting insulating composite material Download PDFInfo
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- CN113956683B CN113956683B CN202010706082.7A CN202010706082A CN113956683B CN 113956683 B CN113956683 B CN 113956683B CN 202010706082 A CN202010706082 A CN 202010706082A CN 113956683 B CN113956683 B CN 113956683B
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- 239000002131 composite material Substances 0.000 title claims abstract description 59
- 239000000945 filler Substances 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 8
- 239000011159 matrix material Substances 0.000 claims abstract description 62
- 239000011248 coating agent Substances 0.000 claims abstract description 23
- 238000000576 coating method Methods 0.000 claims abstract description 23
- 239000000758 substrate Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 28
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 28
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 23
- 239000000203 mixture Substances 0.000 claims description 19
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 18
- 229910002804 graphite Inorganic materials 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 12
- 229920005989 resin Polymers 0.000 claims description 11
- 239000011347 resin Substances 0.000 claims description 11
- 239000010439 graphite Substances 0.000 claims description 10
- 229920000092 linear low density polyethylene Polymers 0.000 claims description 10
- 239000004707 linear low-density polyethylene Substances 0.000 claims description 10
- 239000012752 auxiliary agent Substances 0.000 claims description 9
- 230000003647 oxidation Effects 0.000 claims description 9
- 238000007254 oxidation reaction Methods 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- 229920001684 low density polyethylene Polymers 0.000 claims description 8
- 239000004702 low-density polyethylene Substances 0.000 claims description 8
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 7
- 239000004917 carbon fiber Substances 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 239000011302 mesophase pitch Substances 0.000 claims description 7
- -1 polyethylene Polymers 0.000 claims description 7
- 239000004698 Polyethylene Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000011307 graphite pitch Substances 0.000 claims description 6
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229920000573 polyethylene Polymers 0.000 claims description 6
- 239000004952 Polyamide Substances 0.000 claims description 5
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 5
- 239000012298 atmosphere Substances 0.000 claims description 5
- 229920002647 polyamide Polymers 0.000 claims description 5
- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 5
- 229920001155 polypropylene Polymers 0.000 claims description 5
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- 239000004020 conductor Substances 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000004814 polyurethane Substances 0.000 claims description 3
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021529 ammonia Inorganic materials 0.000 claims description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical group [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- 239000002671 adjuvant Substances 0.000 claims 2
- 239000004593 Epoxy Substances 0.000 claims 1
- 238000013019 agitation Methods 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 claims 1
- 229920002635 polyurethane Polymers 0.000 claims 1
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 5
- 239000011147 inorganic material Substances 0.000 abstract description 5
- 230000000694 effects Effects 0.000 abstract description 3
- 230000017525 heat dissipation Effects 0.000 abstract description 3
- 239000011810 insulating material Substances 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000012360 testing method Methods 0.000 description 12
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 6
- 239000002994 raw material Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 229910052582 BN Inorganic materials 0.000 description 4
- 229920002292 Nylon 6 Polymers 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- TZCXTZWJZNENPQ-UHFFFAOYSA-L barium sulfate Chemical compound [Ba+2].[O-]S([O-])(=O)=O TZCXTZWJZNENPQ-UHFFFAOYSA-L 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000003245 coal Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 3
- 239000010117 shenhua Substances 0.000 description 3
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 3
- 229910010271 silicon carbide Inorganic materials 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000005995 Aluminium silicate Substances 0.000 description 2
- 229920010126 Linear Low Density Polyethylene (LLDPE) Polymers 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 235000012211 aluminium silicate Nutrition 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 239000000835 fiber Substances 0.000 description 2
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000005543 nano-size silicon particle Substances 0.000 description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000002518 antifoaming agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 239000000080 wetting agent Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/10—Encapsulated ingredients
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/46—Graphite
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
- C09C3/063—Coating
-
- 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
- C09K3/00—Materials not provided for elsewhere
- C09K3/16—Anti-static materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
- C01P2004/84—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases one phase coated with the other
- C01P2004/86—Thin layer coatings, i.e. the coating thickness being less than 0.1 time the particle radius
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/32—Thermal properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Polymers & Plastics (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Inorganic Insulating Materials (AREA)
Abstract
The invention relates to the field of heat dissipation materials, and discloses a heat-conducting insulating material and a preparation method thereof, a heat-conducting insulating composite material and a preparation method thereof, wherein the filler takes a heat-conducting substrate as a core, and an insulating shell layer is coated outside the heat-conducting substrate; the radial dimension D of the heat-conducting substrate is 5-100 mu m, and the coating thickness of the insulating shell layer is 2-2000nm. Compared with the prior art, the high-thermal-conductivity insulating filler with a specific coating structure is prepared by adopting the thermal-conductivity matrix with high thermal conductivity and the inorganic material with good insulating property, and the comprehensive effect of the thermal conductivity and the insulating property of the thermal-conductivity insulating composite material prepared by the thermal-conductivity insulating filler is better by limiting the coating thickness and the radial size of the thermal-conductivity matrix.
Description
Technical Field
The invention relates to the technical field of heat dissipation materials, in particular to a heat conduction insulating filler, a preparation method thereof and a heat conduction insulating composite material.
Background
With the increasing number of high-power electronic devices, such as mobile phone 5G technology, the problem of heat generation is more and more prominent, and the problem of heat dissipation is urgently needed to be solved. When the power of the electronic equipment is higher, heat accumulation is generated, so that the performance of the equipment is reduced, and the service life is reduced, for example, the performance of the electronic equipment is reduced by 10 percent every time the temperature of the electronic equipment is increased by 2 ℃. However, if heat is dissipated through a heat conducting material to lower its temperature by 10 ℃, the service life will be doubled.
The addition of heat-conducting fillers in the high polymer material is a main method for preparing the heat-conducting composite material at present. The existing heat-conducting insulating composite material is mainly prepared by adding insulating inorganic materials such as boron nitride, aluminum nitride, magnesium oxide and the like, but the thermal conductivity of the aluminum oxide and the silicon oxide is low, and the price of the boron nitride is high.
CN110218449A discloses a preparation method of a heat-conducting insulating composite material, which comprises the steps of loading simple substance silver on the surface of graphite fiber, taking the silver-loaded fiber and hexagonal boron nitride as fillers, and modifying the surfaces of the fillers by adopting a silane coupling agent.
CN105198436A discloses an insulating and heat-conducting inorganic nano composite ceramic, which is composed of the following raw materials in parts by mass: silicon carbide: silicon dioxide: filling material: auxiliary agent: solvent =30% -45%:10% -15%:15% -30%:1% -10%:10% -30%; the filler is composed of the following raw materials in parts by mass: aluminum nitride: precipitating barium sulfate: kaolin =70%:25%:5 percent, wherein the precipitated barium sulfate and the kaolin are sieved by a sieve with more than 6000 meshes; the auxiliary agent comprises the following substances in parts by mass: rheological aid: defoaming agent: wetting agent: a flattening auxiliary agent: thickening agent: film-forming aid =15% -30%:20% -30%:15% -30%:20% -30%:15% -30%: 15-30 percent of the additive, and the sum of the mass percentage of the additives is 100 percent.
CN109880355A discloses an insulating heat-conducting modified nylon 6 composite material, which is prepared by the following method: 1) Mixing PA6, high sphericity alumina, nano silicon carbide and nano boron nitride serving as raw materials in a high-speed mixer for 3min; 2) Extruding and granulating by a double-screw extruder; fully drying the granules to obtain the insulating heat-conducting modified nylon 6 composite material; in the step 1), the obtained mixture contains the following raw materials: 40-50 parts of PA6, 45-55 parts of high-sphericity alumina, 5-10 parts of nano silicon carbide and 5-10 parts of nano boron nitride.
Disclosure of Invention
The invention aims to overcome the defects of low thermal conductivity and high cost caused by adding insulating inorganic materials such as boron nitride, aluminum nitride, magnesium oxide and the like to prepare a heat-conducting insulating material in the prior art, and provides a heat-conducting insulating filler, a preparation method thereof and a heat-conducting insulating composite material. The heat-conducting insulating filler has the advantages of high heat conductivity and relatively low cost.
In order to achieve the above object, a first aspect of the present invention provides a heat conducting insulating filler, which takes a heat conducting substrate as a core, and an insulating shell layer is coated outside the heat conducting substrate; the radial dimension D of the heat-conducting substrate is 5-100 mu m, and the coating thickness of the insulating shell layer is 2-2000nm.
A second aspect of the present invention provides a method for preparing a thermally conductive insulating filler, comprising: preparing a mixture of a heat-conducting matrix and sol-gel, wherein the sol-gel is coated on the surface of the heat-conducting matrix, and then filtering and drying the mixture to enable the sol-gel to form an insulating shell layer, so as to obtain a heat-conducting insulating filler;
wherein the radial dimension D of the heat-conducting matrix is 10-100 μm; the coating thickness of the insulating shell layer is 10-200nm.
The third aspect of the invention provides a heat-conducting insulating filler prepared by the method.
A fourth aspect of the present invention provides a heat conductive and insulating composite material comprising a resin matrix and the heat conductive and insulating filler of the first or third aspect described above.
According to the invention, the high-thermal-conductivity insulating filler with a specific coating structure is prepared by adopting the thermal-conductivity matrix with high thermal conductivity and the inorganic material with good insulating property, and the comprehensive effect of the thermal conductivity and the insulating property of the thermal-conductivity insulating composite material prepared by the thermal-conductivity insulating filler is better by limiting the coating thickness and the radial size of the thermal-conductivity matrix; the thermal conductivity of the preferred heat-conducting insulating composite material is 2-7W/mk, and the electric resistance is 10 3 -10 13 Ω。
Additional advantages and features of the present invention will be set forth in the detailed description which follows.
Detailed Description
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a heat-conducting insulating filler, which takes a heat-conducting matrix as a core, and an insulating shell layer is coated outside the heat-conducting matrix; the radial dimension D of the heat-conducting substrate is 5-100 mu m, and the coating thickness of the insulating shell layer is 2-2000nm.
The inventor of the invention finds that the high-heat-conductivity insulating filler with a specific coating structure is prepared by adopting a heat-conductivity matrix with high heat conductivity and an inorganic material with good insulating property, and the heat-conductivity insulating filler with good comprehensive performance of heat conductivity and insulating property can be obtained by limiting the coating thickness and the radial dimension of the heat-conductivity matrix. Preferably, the radial dimension D of the heat-conducting matrix is 10-100 μm; the coating thickness of the insulating shell layer is 10-200nm.
Preferably, the weight ratio of the insulating shell layer to the heat-conducting matrix is (4-20): (80-96).
The present invention particularly defines the material of the heat conducting matrix, and preferably, the heat conducting matrix comprises at least one of carbon powder, graphite, expanded graphite and mesophase pitch carbon fiber which are subjected to oxidation treatment, specifically, the heat conducting matrix is obtained by at least one of carbon powder, graphite, expanded graphite and mesophase pitch carbon fiber which are subjected to oxidation treatment, and the materials have the advantages of high heat conductivity, wide sources and low cost, and can enable the heat conducting insulating filler to obtain excellent heat conductivity and insulating property. In the present invention, the carbon powder, graphite, expanded graphite and mesophase pitch carbon fiber are all commercially available, for example, the expanded graphite is available from Qingdao rock-ocean carbon materials, inc.; the mesophase pitch carbon fibers can be purchased from Liaoning Nuo carbon materials Co.
Preferably, the insulating shell layer comprises silicon oxide and/or aluminum oxide.
A second aspect of the present invention provides a method of preparing a thermally conductive insulating filler, comprising: preparing a mixture of a heat-conducting matrix and sol-gel, wherein the sol-gel is coated on the surface of the heat-conducting matrix, and then filtering and drying the mixture to enable the sol-gel to form an insulating shell layer, so as to obtain a heat-conducting insulating filler;
wherein the radial dimension D of the heat-conducting matrix is 5-100 μm; the coating thickness of the insulating shell layer is 2-2000nm.
In a preferred embodiment of the present invention, the method further comprises: oxidizing the heat conducting material at 450-650 ℃ to obtain the heat conducting matrix; the heat conducting material comprises at least one of carbon powder, graphite, expanded graphite and mesophase pitch carbon fiber.
Preferably, the conditions of the oxidation treatment include: the atmosphere is an oxygen-containing gas, preferably air, at a temperature of 500-650 deg.C for a period of 1-10h, more preferably 3-7h.
The invention particularly limits the radial size of the heat-conducting matrix and the coating thickness of the insulating shell layer, and is beneficial to improving the comprehensive performance of the heat-conducting insulating composite material; preferably, the radial dimension D of the heat-conducting matrix is 10-100 μm; the coating thickness of the insulating shell layer is 10-200nm.
The weight ratio of the insulating shell layer to the heat-conducting matrix is specially limited so as to improve the comprehensive performance of the heat-conducting insulating filler; preferably, the sol-gel is used in an amount such that the weight ratio of the insulating shell layer to the heat-conducting matrix is (4-20): (80-96).
The process of mixing the heat-conducting matrix and the sol-gel is particularly limited, the heat-conducting matrix can be mixed with the formed sol, the heat-conducting matrix can be added in the process of forming the sol to perform coating treatment while forming the sol, and the uniform and effective coating treatment can be better formed in the latter process.
Preferably, the sol-gel comprises a silica sol and/or an aluminum sol.
In a preferred embodiment of the present invention, the sol-gel is a silica sol, and the process of preparing the mixture of the thermally conductive substrate and the sol-gel includes: firstly, mixing a heat-conducting matrix with an ammonia organic solution for the first time to obtain a mixed solution, and then mixing tetraethoxysilane with the mixed solution for the second time.
The invention particularly limits the dosage of ammonia water and the content of tetraethoxysilane, and the dosage of the ammonia water and the tetraethoxysilane directly influences the coating thickness and the radial size and the content of the heat-conducting matrix. Preferably, the ammonia water organic solution contains ammonia water and an organic solvent, wherein the ammonia water accounts for 5-15vol% of the ammonia water organic solution; the tetraethoxysilane is 2-18vol% of the ammonia water organic solution; the dosage of the heat-conducting substrate is 5-15g relative to 180mL of the organic solvent in the ammonia water organic solution. In the present invention, the organic solvent is not particularly limited, and an organic solvent that is known in the art, for example, ethanol, can be used.
Preferably, the primary mixing is carried out under stirring for a period of time ranging from 0.5 to 3 hours at a speed ranging from 150 to 250 rpm, more preferably 200 rpm.
The invention particularly limits the time of the secondary mixing and stirring, and the stirring time directly influences the coating thickness and the radial size of the heat-conducting substrate; preferably, the second mixing is carried out under stirring for a period of time ranging from 0.5 to 20 hours, more preferably from 2 to 8 hours, at a speed ranging from 150 to 250 rpm, more preferably 200 rpm.
The third aspect of the invention provides a heat-conducting insulating filler prepared by the method. The heat-conducting insulating filler is completely the same as the heat-conducting insulating filler.
A fourth aspect of the present invention provides a thermally conductive and insulating composite material comprising a resin matrix and the thermally conductive and insulating filler of the first or third aspect.
The method for preparing the composite material is not particularly limited in the present invention, and the composite material can be prepared according to the methods existing in the field, for example, the heat-conducting and insulating filler is subjected to conventional banburying with the resin matrix and/or other auxiliary agents.
The weight ratio of the heat-conducting insulating filler to the resin matrix is particularly limited in the invention, so as to improve the comprehensive performance of the composite material. Preferably, the content of the thermally conductive and insulating filler is 20 to 90wt% and the content of the resin matrix is 10 to 80wt% with respect to the thermally conductive and insulating composite.
The resin matrix is not particularly limited in the present invention, and any resin existing in the art may be used; preferably, the resin matrix is selected from at least one of Polyethylene (PE), linear Low Density Polyethylene (LLDPE), low Density Polyethylene (LDPE), polypropylene (PP), polyamide (PA), polyphenylene Sulfide (PPs), polyurethane (PU), and epoxy resin. The properties of the Polyethylene (PE), linear Low Density Polyethylene (LLDPE), low Density Polyethylene (LDPE), polypropylene (PP), polyamide (PA), polyphenylene Sulfide (PPs), polyurethane (PU) and epoxy resin are not particularly limited, and those skilled in the art can freely select them according to actual requirements. Preferably, the low density polyethylene has a density of 92g/cm or less 2 Melt index at 190 ℃ and 2.16kg < 3g/10min, commercially available, e.g.LDPE (melt index at 190 ℃ and 2.16kg of 4g/10min, density 0.924 g/cm) 3 ) Purchased from Shenhua Baotou coal chemical industry, ltd., and having a brand number of 5220. Preferably, the linear low density polyethylene has a density of 0.93g/cm or less 2 The melt index at 190 ℃ and a load of 2.16kg is < 3g/10min. Commercially available, for example LLDPE (melt index at 190 ℃ and 2.16kg load of 2g/10min, density of 0.924 g/cm) 3 ) Purchased from Shenhua Baotou coal chemical industry, limited liability company under the trade name 7042.
The thermal conductivity of the composite material is 0.5-7W/mk, and the resistance is 100-10 13 Omega. The composite material prepared by the preferred scheme of the invention has the thermal conductivity of 2-7W/mk and the resistance of 10 3 -10 13 Ω。
Preferably, the composite material further comprises an auxiliary agent; more preferably, the assistant is a silane coupling agent, and the silane coupling agent may be used in at least one type selected from the group consisting of KH550, KH540, KH792, KH602, KH560, KH570 and KH 590.
The invention has special limitation on the dosage of the auxiliary agent so as to improve the comprehensive performance of the composite material; preferably, the addition agent is used in an amount of 0.5 to 2wt% with respect to the thermally conductive and insulating composite material.
The present invention will be described in detail below by way of examples. In the following examples, the thermal conductivity was measured by a relaxation resistant LF467 thermal conductivity tester and the electrical resistance was measured by a daily electrical resistance tester; the raw materials involved were all commercially available, except where stated otherwise, and were LLDPE (melt index at 190 ℃ and 2.16kg load of 2g/10min, density of 0.924 g/cm) 3 ) Purchased from Shenhua Baotou coal chemical industry, limited liability company under the trade name 7042.
Example 1
Firstly, 15g of carbon powder is taken to be oxidized for 3 hours at 550 ℃ in the air atmosphere to obtain the heat-conducting matrix. Measuring ammonia water, adding the ammonia water into 180mL of ethanol, and stirring for 5min to obtain an ammonia water ethanol solution with the ammonia water concentration of 15vol%; and weighing 15g of heat-conducting matrix, adding the heat-conducting matrix into the ammonia water ethanol solution, and stirring for 0.5h at 200 revolutions per minute to obtain a mixed solution. Measuring tetraethoxysilane, adding the tetraethoxysilane into the mixed liquid, wherein the volume concentration of the tetraethoxysilane in the mixed liquid is 8vol%, and stirring for 8 hours at 200 revolutions per minute. And filtering and drying to obtain the heat-conducting insulating filler.
The radial dimension D of the heat-conducting matrix is 20 mu m through testing; the coating thickness of the insulating shell layer is 100nm, and the weight ratio of the insulating shell layer to the heat-conducting matrix is 7.3.
And banburying and mixing the heat-conducting insulating filler and LLDPE at 180 ℃ to obtain a heat-conducting insulating composite material, wherein the content of the heat-conducting insulating filler is 65wt% and the content of the LLDPE is 35wt% relative to the heat-conducting insulating composite material.
The composite material is obtained by testing, the thermal conductivity is 6.2W/mk, and the resistance is 10 10 Ω。
Example 2
Firstly, 15g of carbon powder is taken to be oxidized for 3 hours at 550 ℃ in the air atmosphere to obtain the heat-conducting matrix. Measuring ammonia water, adding the ammonia water into 180mL of ethanol, and stirring for 5min to obtain an ammonia water ethanol solution with the ammonia water concentration of 15vol%; and weighing 15g of the heat-conducting matrix, adding the heat-conducting matrix into the ammonia water ethanol solution, and stirring for 0.5h at 200 revolutions per minute to obtain a mixed solution. Measuring tetraethoxysilane, adding the tetraethoxysilane into the mixed liquid, wherein the volume concentration of the tetraethoxysilane in the mixed liquid is 4vol%, and stirring for 2 hours at 200 revolutions per minute. And filtering and drying to obtain the heat-conducting insulating filler.
The radial dimension D of the heat-conducting matrix is 20 mu m through testing; the coating thickness of the insulating shell layer is 80nm, and the weight ratio of the insulating shell layer to the heat-conducting matrix is 4.4.
And banburying and mixing the heat-conducting insulating filler and LLDPE at 180 ℃ to obtain the heat-conducting insulating composite material, wherein the content of the heat-conducting insulating filler is 55wt% and the content of the LLDPE is 45wt% relative to the heat-conducting insulating composite material.
The thermal conductivity of the composite material is 5.5W/mk through testing, and the resistance is 10 3 Ω。
Example 3
Firstly, taking 15g of carbon powder, and oxidizing for 3h at 550 ℃ in an air atmosphere to obtain the heat-conducting matrix. Measuring ammonia water, adding the ammonia water into 180mL of ethanol, and stirring for 5min to obtain an ammonia water ethanol solution with the ammonia water concentration of 15vol%; and weighing 15g of the heat-conducting matrix, adding the heat-conducting matrix into the ammonia water ethanol solution, and stirring for 0.5h at 200 revolutions per minute to obtain a mixed solution. Measuring tetraethoxysilane, adding the tetraethoxysilane into the mixed solution, wherein the volume concentration of the tetraethoxysilane in the mixed solution is 8vol%, and stirring for 8 hours at 200 revolutions per minute. And filtering and drying to obtain the heat-conducting insulating filler.
The radial dimension D of the heat-conducting matrix is 20 mu m through testing; the coating thickness of the insulating shell layer is 100nm, and the weight ratio of the insulating shell layer to the heat-conducting substrate is 7.3.
Banburying and mixing the heat-conducting insulating filler and LLDPE at 180 ℃ to obtain a heat-conducting insulating composite material; wherein, relative to the heat-conducting and insulating composite material, the content of the heat-conducting and insulating filler is 55wt%, and the content of LLDPE is 45wt%.
The composite material is obtained by testing, the thermal conductivity is 4W/mk, and the resistance is 10 10 Ω。
Example 4
Preparing a heat-conducting insulating filler and a heat-conducting insulating composite material according to the method of the embodiment 1 respectively, except that the carbon powder is replaced by graphite with the same amount, the volume concentration of the tetraethoxysilane in the obtained mixed solution is 10vol%, and the time of secondary mixing and stirring is 0.5h; the composite composition shown in table 1 was used instead of the corresponding composition in example 1, and the test results are shown in table 1.
Example 5
Preparing a heat-conducting insulating filler and a heat-conducting insulating composite material according to the method of example 1 respectively, except that the carbon powder is replaced by the same amount of expanded graphite, the temperature of the oxidation treatment is 500 ℃, and the time is 6 hours; the time for secondary mixing and stirring is 18 hours; the composite composition shown in table 1 was used instead of the corresponding composition in example 1, and the test results are shown in table 1.
Example 6
A heat conductive insulating filler and a heat conductive insulating composite material were prepared according to the methods of example 1, respectively, except that the temperature of the oxidation treatment was 600 ℃, and the rest was the same as example 1. The composite composition shown in table 1 was used instead of the corresponding composition in example 1, and the test results are shown in table 1.
Example 7
Preparing a heat-conducting insulating filler and a heat-conducting insulating composite material according to the method of the embodiment 1 respectively, except that the volume concentration of the tetraethoxysilane in the obtained mixed solution is 16vol%, and the time of secondary mixing and stirring is 4 hours; and an auxiliary agent KH550 is also added in the banburying mixing process, and the content of the auxiliary agent is 1wt% relative to the heat-conducting and insulating composite material. The corresponding test results are shown in table 1.
Comparative example 1
Preparing a heat-conducting insulating filler and a heat-conducting insulating composite material according to the method of the embodiment 1, except that the oxidation treatment temperature is 300 ℃ and the time is 1h; the composite composition shown in table 1 was used instead of the corresponding composition in example 1, and the test results are shown in table 1.
Comparative example 2
Preparing a heat-conducting insulating filler and a heat-conducting insulating composite material according to the method of example 1, except that the volume concentration of the tetraethoxysilane in the obtained mixed solution is 20vol%, the time for primary mixing and stirring is 2 hours, and the time for secondary mixing and stirring is 22 hours; the composite composition shown in table 1 was used instead of the corresponding composition in example 1, and the test results are shown in table 1.
TABLE 1
As can be seen from the results of table 1, examples 1 to 7 using the present invention have excellent thermal conductivity and insulating properties.
As can be seen from comparison of example 1 and comparative examples 1 to 2, more excellent effects can be obtained by the scheme of the present invention.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.
Claims (18)
1. The preparation method of the heat-conducting insulating filler is characterized by preparing a mixture of a heat-conducting matrix and sol-gel, wherein the sol-gel is coated on the surface of the heat-conducting matrix, and then filtering and drying the mixture to enable the sol-gel to form an insulating shell layer to obtain the heat-conducting insulating filler;
the sol-gel is silica sol, and the process for preparing the mixture of the heat-conducting matrix and the sol-gel comprises the following steps: firstly, mixing a heat-conducting matrix with an ammonia organic solution for the first time to obtain a mixed solution, and then mixing tetraethoxysilane with the mixed solution for the second time;
the tetraethoxysilane is 2-18vol% of the ammonia water organic solution;
the primary mixing is carried out under stirring, and the stirring time is 0.5-3h;
the secondary mixing is carried out under stirring, and the stirring time is 0.5-20h;
the heat-conducting matrix comprises at least one of carbon powder, graphite, expanded graphite and mesophase pitch carbon fiber which are subjected to oxidation treatment;
the conditions of the oxidation treatment include: oxidizing the heat conducting material at 450-650 ℃;
the heat conduction material comprises at least one of carbon powder, graphite, expanded graphite and mesophase pitch carbon fiber;
the filler takes a heat-conducting matrix as a core, and an insulating shell layer is coated outside the heat-conducting matrix; the radial dimension D of the heat-conducting substrate is 5-100 mu m, and the coating thickness of the insulating shell layer is 2-2000nm; the weight ratio of the insulating shell layer to the heat-conducting base body is (4-20): (80-96).
2. The method of claim 1, wherein the thermally conductive matrix has a radial dimension D of 10-100 μ ι η and the insulating shell layer has a coating thickness of 10-200nm.
3. The method of claim 1, wherein the conditions of the oxidation treatment comprise: the atmosphere is oxygen-containing gas, the temperature is 500-650 ℃, and the time is 1-10h.
4. The method of claim 3, wherein the time is 3-7 hours.
5. The method of claim 1, wherein the aqueous ammonia organic solution comprises aqueous ammonia and an organic solvent, wherein the aqueous ammonia comprises 5-15vol% of the aqueous ammonia organic solution; the dosage of the heat-conducting matrix is 5-15g relative to 180mL of the organic solvent.
6. The process according to claim 1, wherein the primary mixing is carried out under stirring at a speed of from 150 to 250 rpm.
7. The process of claim 1 wherein the second mixing is conducted under agitation at a rate of 150 to 250 rpm.
8. The process according to claim 1, wherein the second mixing is carried out under stirring for a time ranging from 2 to 8h.
9. A thermally conductive and electrically insulating filler obtainable by the process according to any one of claims 1 to 8.
10. A heat conductive insulating composite material comprising a resin matrix and the heat conductive insulating filler according to claim 9.
11. The composite of claim 10, wherein the thermally conductive and insulating filler is present in an amount of 20-90wt% and the resin matrix is present in an amount of 10-80wt% relative to the thermally conductive and insulating composite.
12. The composite of claim 10, wherein the resin matrix is selected from at least one of polyethylene, polypropylene, polyamide, polyphenylene sulfide, polyurethane, and epoxy.
13. The composite of claim 12, wherein the polyethylene is a low density polyethylene.
14. The composite of claim 13, wherein the low density polyethylene is a linear low density polyethylene.
15. The composite of claim 10, wherein the composite has a thermal conductivity of 2-7W/mk and an electrical resistance of 10 3 -10 13 Ω。
16. The composite material according to any one of claims 10-15, wherein the composite material further comprises an auxiliary agent.
17. The composite of claim 16, wherein the adjuvant is a silane coupling agent.
18. The composite according to claim 16, wherein the adjuvant is used in an amount of 0.5-2wt% with respect to the thermally conductive and insulating composite.
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| US4546028A (en) * | 1982-04-27 | 1985-10-08 | Compagnie D'informatique Militaire Spatiale & Aeronautique | Composite substrate with high heat conduction |
| CN103183889A (en) * | 2013-03-21 | 2013-07-03 | 上海交通大学 | High-thermal-conductivity and insulating polymer composite material and preparation method thereof |
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