CN117264426A - Insulating heat-conducting gasket and preparation method thereof - Google Patents
Insulating heat-conducting gasket and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical class [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical class C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000945 filler Substances 0.000 claims abstract description 28
- 239000003054 catalyst Substances 0.000 claims abstract description 20
- 229920002545 silicone oil Polymers 0.000 claims abstract description 20
- 239000003112 inhibitor Substances 0.000 claims abstract description 12
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 11
- 239000001257 hydrogen Substances 0.000 claims abstract description 11
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 11
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 11
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 229910052582 BN Inorganic materials 0.000 claims description 25
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 25
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 24
- 239000004917 carbon fiber Substances 0.000 claims description 24
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 21
- 239000002041 carbon nanotube Substances 0.000 claims description 21
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 18
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 10
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- 229910052697 platinum Inorganic materials 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 8
- 229960001760 dimethyl sulfoxide Drugs 0.000 claims description 8
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 229920001213 Polysorbate 20 Polymers 0.000 claims description 6
- 238000003490 calendering Methods 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 claims description 6
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- MQWFLKHKWJMCEN-UHFFFAOYSA-N n'-[3-[dimethoxy(methyl)silyl]propyl]ethane-1,2-diamine Chemical compound CO[Si](C)(OC)CCCNCCN MQWFLKHKWJMCEN-UHFFFAOYSA-N 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 4
- -1 alkynyl cyclic alcohol compounds Chemical class 0.000 claims description 4
- 238000012986 modification Methods 0.000 claims description 4
- 230000004048 modification Effects 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910003460 diamond Inorganic materials 0.000 claims description 3
- 239000010432 diamond Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 238000005507 spraying Methods 0.000 claims description 3
- 229910052763 palladium Inorganic materials 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
- 239000011261 inert gas Substances 0.000 claims 2
- 238000000034 method Methods 0.000 claims 2
- 239000002131 composite material Substances 0.000 claims 1
- 239000004020 conductor Substances 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000000463 material Substances 0.000 description 12
- 239000011159 matrix material Substances 0.000 description 10
- 230000002411 adverse Effects 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical group C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 239000003575 carbonaceous material Substances 0.000 description 3
- 239000011231 conductive filler Substances 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- 238000011161 development Methods 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
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- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
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- 239000002270 dispersing agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- 239000002109 single walled nanotube Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
- C08J2383/07—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2483/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2483/04—Polysiloxanes
- C08J2483/05—Polysiloxanes containing silicon bound to hydrogen
-
- 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
- C08K3/28—Nitrogen-containing compounds
- C08K2003/282—Binary compounds of nitrogen with aluminium
-
- 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
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- 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
- C08K3/041—Carbon nanotubes
-
- 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
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
-
- 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
- C08K9/04—Ingredients treated with organic substances
-
- 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
Abstract
The invention belongs to the field of heat conducting materials, and particularly relates to an insulating heat conducting gasket and a preparation method thereof. The insulating heat-conducting gasket is prepared from the following raw materials in parts by weight: 90-100 parts by weight of vinyl silicone oil, 1-3 parts by weight of hydrogen-containing silicone oil, 0.01-0.03 part by weight of inhibitor, 0.1-0.2 part by weight of catalyst and 600-900 parts by weight of modified heat-conducting filler; the modified heat conducting filler consists of modified carbon fiber, modified carbon nano tube and basic filler. The insulating heat-conducting gasket has the characteristics of high heat conduction, high insulation and good mechanical property, and can meet the requirements of practical application.
Description
Technical Field
The invention belongs to the field of heat conducting materials, and particularly relates to an insulating heat conducting gasket and a preparation method thereof.
Background
With the vigorous development of electronic information technology, miniaturized, highly integrated and high-performance electronic devices have become the mainstream of development. These devices have significant heat generation under high efficiency operation, and if they do not dissipate heat effectively, they will cause risks such as circuit failure, component damage, and electrical breakdown, and therefore the need for thermal management is more stringent.
The thermally conductive gasket serves as an important constituent of the thermal interface material and plays an important role therein. The heat-conducting material can be filled in a tiny gap between the heating element and the heat-radiating element to remove air, so that interface contact thermal resistance is reduced, and efficient heat conduction is realized. In addition, the thermally conductive gasket can also provide additional functions of packaging, shock absorption, insulation, and the like. The heat-conducting insulating gasket has important application in the fields of electronics, power, automobiles, aerospace and the like, and provides key support in heat conduction and electric insulation for equipment and systems in the fields.
In order to further improve the thermal conductivity of the thermal interface material, for example, CN106634863A, CN106813226A, CN109354874a and the like are studied, and carbon materials such as graphene, carbon nanotubes, carbon fibers and the like with ultra-high thermal conductivity are used as a thermal conductive filler to be applied to a thermal conductive gasket, however, such carbon materials often have a certain electrical conductivity, are extremely unfavorable for electronic devices, are easy to short-circuit equipment, and are dangerous. Therefore, how to avoid the disadvantage of carbon materials while maintaining high thermal conductivity remains a research hotspot in the field of thermal interface materials.
Disclosure of Invention
In view of the defects existing in the prior art, the invention provides the insulating heat-conducting gasket, and the modified heat-conducting filler composed of the modified carbon fiber, the modified carbon nano tube and the basic filler is adopted, so that the high heat conductivity of the gasket can be ensured, the heat can be effectively conducted, and the insulating heat-conducting gasket has the advantages of good insulativity and good mechanical property. The invention also provides a preparation method of the insulating heat-conducting gasket.
An insulating heat-conducting gasket comprises the following raw materials in parts by weight:
90-100 parts by weight of vinyl silicone oil, 1-3 parts by weight of hydrogen-containing silicone oil, 0.01-0.03 part by weight of inhibitor, 0.1-0.2 part by weight of catalyst and 600-900 parts by weight of modified heat conducting filler.
The existing heat-conducting gasket is prepared by taking a polymer as a matrix and adding basic heat-conducting fillers such as aluminum nitride, aluminum oxide, silicon dioxide, hexagonal boron nitride, diamond and the like, but the problem of poor heat-conducting performance often exists. According to the invention, a small amount of carbon nanotubes with excellent mechanical properties and high thermal conductivity, carbon fibers and basic thermal conductive filler are added for combined use, so that the thermal conductivity of the gasket is remarkably improved, and the adverse effect caused by the electrical conductivity of the gasket is reduced while the high thermal conductivity and high strength of the gasket are maintained through modification treatment of the carbon nanotubes and the carbon fibers.
Preferably, the modified heat conducting filler consists of 1-2wt% of modified carbon fiber, 0.1-0.5wt% of modified carbon nano tube and the balance of basic filler.
According to the invention, the Tween-20 is used as a dispersing agent for pretreating the carbon fiber, and then the silica sol is coated on the surface of the carbon fiber through interfacial adsorption and calcined to form the silica coated insulating layer, so that the problems of poor wettability and weak interfacial bonding between the carbon fiber and a matrix can be solved, the carbon fiber and the matrix are orderly arranged in the matrix, the high thermal conductivity and mechanical property of the heat-conducting gasket are effectively improved, and the adverse effect of the electrical conductivity of the carbon fiber is avoided.
Preferably, the preparation method of the modified carbon fiber comprises the following steps:
adding 10-15 parts by weight of carbon fiber and 1-5 parts by weight of tween-20 into 80-90 parts by weight of dimethyl sulfoxide, uniformly mixing, reacting for 0.5-2 hours at 50-60 ℃, adding 1-5 parts by weight of silica sol, continuously reacting for 2-4 hours, centrifuging, drying for 30-60 minutes at 80-90 ℃, and calcining for 3-5 hours at 1100-1300 ℃ under nitrogen protection to obtain the modified carbon fiber.
According to the invention, the carbon nano tube is modified, so that the problems that the dispersibility of the carbon nano tube is poor due to the high aspect ratio and the large specific surface area, the compatibility with a matrix is poor, the thermal resistance of a large interface is high, the effective conduction cannot be realized, and the thermal conductivity of the gasket is not obviously improved can be solved. According to the invention, the characteristic that the surface of the carbon nano tube is negatively charged is utilized, and the 3- (2-amino ethyl amino) propyl methyl dimethoxy silane is adopted to modify the hexagonal boron nitride so that the surface of the hexagonal boron nitride is covered with positive charges, and self-assembly occurs between the hexagonal boron nitride and the hexagonal boron nitride through electrostatic action and chemical bonding, so that the surface of the carbon nano tube is covered with a layer of firm insulating heat conducting filler, thus not only improving the compatibility and the dispersibility with a matrix, but also further improving the heat conducting property and reducing the adverse effect caused by the conductivity of the hexagonal boron nitride.
Preferably, the preparation method of the modified carbon nano tube comprises the following steps:
adding 0.1-0.5 weight part of 3- (2-amino ethyl amino) propyl methyl dimethoxy silane and 0.01-0.03 weight part of 35-37 weight percent hydrochloric acid into 20-50 weight parts of absolute ethyl alcohol, and uniformly mixing to obtain a modified liquid; uniformly spraying a modifying solution into hexagonal boron nitride, wherein the weight ratio of the modifying solution to the hexagonal boron nitride is 1:7-10, and drying at 70-80 ℃ for 60-90min to obtain surface modified hexagonal boron nitride; adding 10-20 parts by weight of carbon nano tube and 3-6 parts by weight of surface modified hexagonal boron nitride into 150-200 parts by weight of methyl sulfoxide, uniformly mixing, reacting for 2-5 hours at 30-35 ℃, centrifuging, drying for 30-60 minutes at 80-90 ℃, and calcining for 1-3 hours at 1500-1600 ℃ under nitrogen protection to obtain the modified carbon nano tube.
Preferably, the base filler is at least one of aluminum nitride, aluminum oxide, silicon dioxide, hexagonal boron nitride and diamond. Further preferably, the base filler is aluminum nitride.
Preferably, the inhibitor is any one of alkynyl cyclic alcohol compounds and alkenyl cyclic siloxane compounds. Further preferably, the inhibitor is 1-ethynyl cyclohexanol.
Preferably, the catalyst is any one of rhodium catalyst, platinum catalyst and palladium catalyst. Further preferably, the catalyst is a platinum catalyst.
In a specific embodiment, the vinyl silicone oil has a vinyl content of 0.65% and a viscosity of 1000mpa.s.
In a specific embodiment, the hydrogen-containing silicone oil has a terminal hydrogen content of 0.32% and a viscosity of 500mpa.s.
In a specific embodiment, pitch-based carbon fibers are used for the carbon fibers, and have a diameter of 7 μm and a length of 200. Mu.m.
In a specific embodiment, the silica sol has a solids content of 50wt%, a pH of 9.5 to 10.5 and an average particle size of 80 to 120nm.
In a specific embodiment, the carbon nano tube adopts a single-wall carbon nano tube which is not modified, aminated and carboxylated, the tube diameter is 1-5nm, and the length is 20-50 mu m.
In a specific embodiment, hexagonal boron nitride is 100nm hexagonal boron nitride.
In a specific embodiment, 30 μm aluminum nitride is used as the aluminum nitride.
In a specific embodiment, the platinum catalyst has a platinum content of 3000ppm.
The invention also provides a preparation method of the insulating heat-conducting gasket, which comprises the following steps:
adding 90-100 parts by weight of vinyl silicone oil, 1-3 parts by weight of hydrogen-containing silicone oil, 0.01-0.03 part by weight of inhibitor and 0.1-0.2 part by weight of catalyst into a kneader, and stirring until the mixture is uniform; then adding 600-900 parts by weight of modified heat conducting filler, and stirring until the materials are uniformly mixed; vacuumizing and calendaring; and heating and solidifying at 120-130 ℃ and cooling to obtain the insulating heat-conducting gasket.
The invention has the beneficial effects that:
according to the invention, the carbon nano tube and the carbon fiber with excellent mechanical and heat conducting properties are combined with the basic heat conducting filler, so that the heat conductivity of the gasket is obviously improved, and the adverse effect caused by the electric conductivity of the gasket is reduced while the high heat conductivity and the high strength of the gasket are maintained through modification treatment of the carbon nano tube and the carbon fiber.
Detailed Description
The above summary of the present invention is described in further detail below in conjunction with the detailed description, but it should not be understood that the scope of the above-described subject matter of the present invention is limited to the following examples.
Example 1
The preparation method of the insulating heat-conducting gasket comprises the following steps:
adding 98 parts by weight of vinyl silicone oil, 2 parts by weight of hydrogen-containing silicone oil, 0.02 part by weight of inhibitor 1-ethynyl cyclohexanol and 0.18 part by weight of platinum catalyst into a kneader, and stirring until the materials are uniformly mixed; then 700 parts by weight of modified heat conducting filler is added and stirred until the materials are uniformly mixed; vacuumizing and calendaring; and heating, solidifying and cooling at 125 ℃ to obtain the insulating heat-conducting gasket.
The modified heat conduction filler consists of 1.6wt% of modified carbon fiber, 0.4wt% of modified carbon nano tube and the balance of aluminum nitride.
The preparation method of the modified carbon fiber comprises the following steps:
adding 12 parts by weight of carbon fiber and 3 parts by weight of Tween-20 into 82 parts by weight of dimethyl sulfoxide, uniformly mixing, reacting for 1h at 55 ℃, then adding 3 parts by weight of silica sol, continuously reacting for 2.5h, centrifuging, drying for 50min at 85 ℃, and calcining for 3.5h at 1250 ℃ under nitrogen protection to obtain the modified carbon fiber.
The preparation method of the modified carbon nano tube comprises the following steps:
adding 0.25 weight part of 3- (2-amino ethyl amino) propyl methyl dimethoxy silane and 0.012 weight part of 36 weight percent hydrochloric acid into 30 weight parts of absolute ethyl alcohol, and uniformly mixing to obtain a modified liquid; uniformly spraying a modifying solution into hexagonal boron nitride, wherein the weight ratio of the modifying solution to the hexagonal boron nitride is 1:8, and drying at 78 ℃ for 80min to obtain surface modified hexagonal boron nitride; adding 15 parts by weight of carbon nano tube and 5 parts by weight of surface modified hexagonal boron nitride into 180 parts by weight of methyl sulfoxide, uniformly mixing, reacting for 2.5 hours at 32 ℃, centrifuging, drying for 50 minutes at 85 ℃, and calcining for 1.5 hours at 1550 ℃ under the protection of nitrogen to obtain the modified carbon nano tube.
Example 2
The preparation method of the insulating heat-conducting gasket comprises the following steps:
adding 98 parts by weight of vinyl silicone oil, 2 parts by weight of hydrogen-containing silicone oil, 0.02 part by weight of inhibitor 1-ethynyl cyclohexanol and 0.18 part by weight of platinum catalyst into a kneader, and stirring until the materials are uniformly mixed; then 700 parts by weight of modified heat conducting filler is added and stirred until the materials are uniformly mixed; vacuumizing and calendaring; and heating, solidifying and cooling at 125 ℃ to obtain the insulating heat-conducting gasket.
The modified heat conduction filler consists of 1.6wt% of modified carbon fiber, 0.4wt% of carbon nano tube and the balance of aluminum nitride.
The preparation method of the modified carbon fiber comprises the following steps:
adding 12 parts by weight of carbon fiber and 3 parts by weight of Tween-20 into 82 parts by weight of dimethyl sulfoxide, uniformly mixing, reacting for 1h at 55 ℃, then adding 3 parts by weight of silica sol, continuously reacting for 2.5h, centrifuging, drying for 50min at 85 ℃, and calcining for 3.5h at 1250 ℃ under nitrogen protection to obtain the modified carbon fiber.
Example 3
The preparation method of the insulating heat-conducting gasket comprises the following steps:
adding 98 parts by weight of vinyl silicone oil, 2 parts by weight of hydrogen-containing silicone oil, 0.02 part by weight of inhibitor 1-ethynyl cyclohexanol and 0.18 part by weight of platinum catalyst into a kneader, and stirring until the materials are uniformly mixed; then 700 parts by weight of modified heat conducting filler is added and stirred until the materials are uniformly mixed; vacuumizing and calendaring; and heating, solidifying and cooling at 125 ℃ to obtain the insulating heat-conducting gasket.
The modified heat-conducting filler consists of 2wt% of modified carbon fiber and the balance of aluminum nitride.
The preparation method of the modified carbon fiber comprises the following steps:
adding 12 parts by weight of carbon fiber and 3 parts by weight of Tween-20 into 82 parts by weight of dimethyl sulfoxide, uniformly mixing, reacting for 1h at 55 ℃, then adding 3 parts by weight of silica sol, continuously reacting for 2.5h, centrifuging, drying for 50min at 85 ℃, and calcining for 3.5h at 1250 ℃ under nitrogen protection to obtain the modified carbon fiber.
Example 4
The preparation method of the insulating heat-conducting gasket comprises the following steps:
adding 98 parts by weight of vinyl silicone oil, 2 parts by weight of hydrogen-containing silicone oil, 0.02 part by weight of inhibitor 1-ethynyl cyclohexanol and 0.18 part by weight of platinum catalyst into a kneader, and stirring until the materials are uniformly mixed; then 700 parts by weight of modified heat conducting filler is added and stirred until the materials are uniformly mixed; vacuumizing and calendaring; and heating, solidifying and cooling at 125 ℃ to obtain the insulating heat-conducting gasket. The modified heat conducting filler consists of 2 weight percent of carbon fiber and the balance of aluminum nitride.
Test example 1
The thermal pads of the above examples were tested for tensile strength using a universal tensile machine, with reference to the ASTM D412 standard method.
TABLE 1 tensile Strength of thermally conductive gasket
| Tensile strength, mpa | |
| Example 1 | 0.90 |
| Example 3 | 0.78 |
Test example 2
The thermal conductivity of the thermal pads of the above examples was tested using a thermal conductivity tester, with reference to the ASTM D5470 standard method. The thermal pads of the above examples were tested for breakdown voltage using a withstand voltage tester, with reference to the ASTM D149 standard method.
TABLE 2 thermal conductivity and breakdown Voltage resistance of thermal conductive pads
| Thermal conductivity, W/(m.k) | Breakdown voltage, V/cm | |
| Example 1 | 5.8 | 1100 |
| Example 2 | 5.1 | 500 |
| Example 3 | 3.3 | 1200 |
| Example 4 | 2.7 | 700 |
It can be seen that the thermal conductivity of the gasket is remarkably improved by adding a small amount of carbon nanotubes and carbon fibers with excellent mechanical properties and high thermal conductivity and combining the carbon nanotubes and the carbon fibers with the basic thermal conductive filler, and adverse effects caused by the electrical conductivity of the gasket are reduced while the high thermal conductivity and the high strength of the gasket are maintained by modifying the carbon nanotubes and the carbon fibers. Compared with the embodiment 4, the embodiment 3 adopts the modified carbon fiber, the silica sol is coated on the surface of the carbon fiber through interfacial adsorption and is calcined to form the silica coated insulating layer, so that the problems of poor wettability and weak interfacial bonding between the carbon fiber and the matrix can be solved, the carbon fiber and the matrix are orderly arranged in the matrix, the high thermal conductivity and mechanical property of the heat conduction gasket are effectively improved, and meanwhile, the heat conduction gasket has good insulativity. Compared with the embodiment 2, the embodiment 1 adopts the modified carbon nano tube, utilizes the characteristic that the surface of the carbon nano tube is negatively charged, adopts the 3- (2-amino ethyl amino) propyl methyl dimethoxy silane to modify the hexagonal boron nitride to cover the surface of the hexagonal boron nitride with positive charges, and self-assembles the hexagonal boron nitride by electrostatic action and chemical bonding, so that the surface of the carbon nano tube is covered with a layer of firm insulating heat conducting filler, thereby not only improving and solving the adverse effects of poor dispersibility and poor compatibility with a matrix caused by high diameter ratio and large specific surface area of the carbon nano tube, but also having the problems that the heat conductivity of a gasket cannot be effectively conducted due to larger interface thermal resistance, further improving the heat conducting property and reducing the electric conductivity of the carbon nano tube.
The foregoing describes in detail preferred embodiments of the present invention. It should be understood that numerous modifications and variations can be made in accordance with the concepts of the invention by one of ordinary skill in the art without undue burden. Therefore, all technical solutions which can be obtained by logic analysis, reasoning or limited experiments based on the prior art by the person skilled in the art according to the inventive concept shall be within the scope of protection defined by the claims.
Claims (8)
1. An insulating heat conduction gasket, characterized in that: the composite material is prepared from the following raw materials in parts by weight:
90-100 parts by weight of vinyl silicone oil, 1-3 parts by weight of hydrogen-containing silicone oil, 0.01-0.03 part by weight of inhibitor, 0.1-0.2 part by weight of catalyst and 600-900 parts by weight of modified heat-conducting filler;
the modified heat conducting filler consists of modified carbon fiber, modified carbon nano tube and basic filler.
2. The insulating and thermally conductive gasket of claim 1, wherein: the base filler is at least one of aluminum nitride, aluminum oxide, silicon dioxide, hexagonal boron nitride and diamond.
3. The insulating and thermally conductive gasket of claim 1, wherein: the preparation method of the modified carbon fiber comprises the following steps:
adding 10-15 parts by weight of carbon fiber and 1-5 parts by weight of tween-20 into 80-90 parts by weight of dimethyl sulfoxide, uniformly mixing, heating for reaction, adding 1-5 parts by weight of silica sol for continuous reaction, centrifuging and drying after the reaction is finished, and calcining under the protection of inert gas to obtain the modified carbon fiber.
4. The insulating and thermally conductive gasket of claim 1, wherein: the preparation method of the modified carbon nano tube comprises the following steps:
adding 0.1-0.5 part by weight of 3- (2-amino ethyl amino) propyl methyl dimethoxy silane and 0.01-0.03 part by weight of hydrochloric acid into 20-50 parts by weight of absolute ethyl alcohol, and uniformly mixing to obtain a modified liquid; uniformly spraying the modification liquid into hexagonal boron nitride, and drying to obtain surface modified hexagonal boron nitride; adding 10-20 parts by weight of carbon nano tube and 3-6 parts by weight of surface modified hexagonal boron nitride into 150-200 parts by weight of methyl sulfoxide, uniformly mixing, heating for reaction, centrifuging after the reaction is finished, drying, and calcining under the protection of inert gas to obtain the modified carbon nano tube.
5. The insulating and thermally conductive gasket of claim 4, wherein: the weight ratio of the modifying liquid to the hexagonal boron nitride is 1:7-10.
6. The insulating and thermally conductive gasket of claim 1, wherein: the inhibitor is any one of alkynyl cyclic alcohol compounds and alkenyl cyclic siloxane compounds.
7. The insulating and thermally conductive gasket of claim 1, wherein: the catalyst is any one of rhodium catalyst, platinum catalyst and palladium catalyst.
8. The method for preparing the insulating and heat conducting gasket according to any one of claims 1 to 7, wherein: the method comprises the following steps:
adding vinyl silicone oil, hydrogen-containing silicone oil, inhibitor and catalyst into a kneader, and stirring until the mixture is uniform; and then adding the modified heat conducting filler, stirring until the mixture is uniform, vacuumizing, calendaring, heating, solidifying and cooling to obtain the insulating heat conducting gasket.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117603660A (en) * | 2024-01-24 | 2024-02-27 | 北京泰派斯特电子技术有限公司 | Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof |
| CN117603660B (en) * | 2024-01-24 | 2024-04-26 | 北京泰派斯特电子技术有限公司 | Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof |
-
2023
- 2023-10-19 CN CN202311354216.3A patent/CN117264426A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117603660A (en) * | 2024-01-24 | 2024-02-27 | 北京泰派斯特电子技术有限公司 | Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof |
| CN117603660B (en) * | 2024-01-24 | 2024-04-26 | 北京泰派斯特电子技术有限公司 | Ultrathin breakdown voltage-resistant heat-conducting insulating gasket and preparation method thereof |
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