CN114539783B - High-heat-conductivity high-insulation gasket and preparation method thereof - Google Patents
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- 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
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- 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
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- C09K5/14—Solid materials, e.g. powdery or granular
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
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- C08K2003/382—Boron-containing compounds and nitrogen
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- C08K2201/003—Additives being defined by their diameter
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- C08K2201/004—Additives being defined by their length
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Abstract
The invention discloses a high-heat-conductivity high-insulation gasket and a preparation method thereof. The main body of the heat conducting filler is h-BN with good heat conducting property and excellent insulativity, and is compounded with asphalt-based chopped carbon fiber with excellent heat conducting property, and the two are combined together in an electrostatic self-assembly mode. After being oriented by liquid nitrogen, the high-heat-conductivity high-insulation gasket filler shows excellent heat conduction and insulation performance in a direction parallel and consistent with a heat conduction direction under extremely low filling quantity (20 wt%). The high-heat-conductivity high-insulation gasket is tested according to the ISO 22007-2 standard, the heat conductivity coefficient of the high-heat-conductivity high-insulation gasket is more than or equal to 3W/m.K, the breakdown voltage UD of the high-heat-conductivity high-insulation gasket is more than or equal to 13kV according to the ASTM D149 standard, and excellent heat conductivity and electric insulation performance are shown.
Description
Technical Field
The invention relates to a high-heat-conductivity high-insulation gasket and a preparation method thereof, and belongs to the field of thermal interface materials.
Background
As electronic devices are being miniaturized, highly integrated, and powered, heat dissipation issues are becoming more and more pronounced. Meanwhile, occasions such as 5G communication and large-scale integrated circuits require not only a heat dissipation material having high heat conduction properties but also good insulation properties. Polymer-based thermally conductive materials are receiving attention because of their low cost and good processing characteristics. The polymer-based thermally conductive material is generally composed of a thermally conductive filler and a polymer matrix. At present, a large number of documents report polymer composite heat conducting materials using carbon-based materials such as carbon nanotubes and the like as fillers, such as nano silver particles-reduced graphene oxide (rGO) fillers, pressed graphite paper, pure graphene, graphene foam graphene/cellulose fillers and the like.
However, the application of the composite material in insulation occasions is severely limited because the carbon materials such as graphene and the like have high conductivity. And Boron Nitride (BN) is a material having good heat conductive properties, high mechanical strength and excellent insulating properties. Therefore, in the occasion of heat dissipation with high requirement on insulating property, the boron nitride polymer composite heat conducting material has very broad application prospect.
The main heat conducting function for the heat conducting composite material is the heat conducting filler, and the most important is the construction of a heat conducting path for the heat conducting filler. The construction of the heat conduction path is beneficial to the maximum play of the heat conduction filler, so that the heat conduction filler has excellent heat conduction performance. The heat conducting filler is arranged in the matrix in a disordered way in a simple blending way, and a heat conducting passage cannot be formed effectively. By constructing a large number of effective heat conduction passages in a directional orientation mode, the composite material can achieve extremely high heat conduction performance (the heat conduction coefficient is more than or equal to 3W/m.K) under extremely low filling quantity (15 wt%) and has breakdown voltage UD more than or equal to 13kV, and excellent heat conduction and electric insulation performances are shown.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention discloses a high-heat-conductivity high-insulation gasket and a preparation method thereof, and the prepared high-heat-conductivity high-insulation gasket can realize extremely high heat-conductivity (the heat conductivity coefficient is more than or equal to 3W/m.K) under extremely low filling amount (15 wt%) and has breakdown voltage UD of more than or equal to 13kV, and the heat-conductivity gasket has excellent heat conductivity and electric insulation performance, so that the heat-conductivity gasket can be widely applied to the fields with 5G heat conductivity and higher requirements on insulativity.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: the utility model provides a high heat conduction high insulation gasket and preparation method thereof, high heat conduction high insulation gasket, includes liquid silicone rubber and heat conduction filler main part, its characterized in that: the liquid silicone rubber in the high-heat-conductivity high-insulation gasket comprises vinyl-terminated silicone oil, hydrogen-containing silicone oil, an inhibitor and an accelerator; the main body of the heat-conducting filler is h-BN with good heat-conducting property and excellent insulativity, and is compounded with asphalt-based chopped carbon fiber with excellent heat-conducting property, and the two are combined together in an electrostatic self-assembly mode;
preferably, the mass ratio of the vinyl-terminated silicone oil to the hydrogen-containing silicone oil to the inhibitor to the accelerator is 100: (15-25): (3-8): (5-10).
Preferably, the h-BN particle diameter is (10 to 30) μm.
Preferably, the pitch-based carbon fiber has a diameter of 7 μm and a length of (0.1 to 0.3) mm.
Preferably, the h-BN is treated by using a cationic surfactant, wherein the cationic surfactant is one or more of cetyl trimethyl ammonium bromide, octadecyl trimethyl discourager and dodecyl dimethyl amine oxide, and the concentration of the cationic surfactant aqueous solution is (0.1-20) g/L.
Preferably, the pitch-based chopped carbon fiber is sulfonated with H2SO4 to negatively charge the pitch-based chopped carbon fiber, and the concentration of H2SO4 is (2-4) mol/L.
Preferably, the preparation process comprises the following steps:
1) Placing the h-BN in a cationic surfactant water solution with a certain concentration, stirring the mixture for (3-6) h, controlling the concentration of the h-BN at (10-50) g/L, carrying out suction filtration on the treated h-BN, and then placing the treated h-BN in a 50 ℃ oven for drying for 24h for later use;
2) Placing the chopped asphalt-based carbon fiber into an H2SO4 water solution with a certain concentration, stirring the chopped asphalt-based carbon fiber for 2 to 6 hours, controlling the concentration of the asphalt-based chopped carbon fiber to be (5 to 25) g/L, carrying out suction filtration on the chopped asphalt-based carbon fiber, and placing the chopped asphalt-based carbon fiber in a 50 ℃ oven for baking for 24 hours for later use;
3) Weighing the treated h-BN and the chopped asphalt-based carbon according to a proportion to prepare an aqueous solution, controlling the total concentration of the filler to be 15-50 g/L, stirring for 5-15 min, standing for 10-30 min, combining the two materials together in a static self-assembly mode, and placing the two materials in a 50 ℃ oven for baking for 24 hours for later use after suction filtration;
4) Preparing the filler and the carboxymethyl cellulose into an aqueous solution, wherein the filler accounts for (15-20) weight percent, the concentration of the carboxymethyl cellulose is (1-3) weight percent, and the prepared solution is placed in a liquid nitrogen freezing platform for directional freezing to prepare ice cubes;
5) Placing the prepared ice cubes into a freeze dryer for cold drying (3-5) d to prepare aerogel;
6) Weighing vinyl-terminated silicone oil, hydrogen-containing silicone oil and inhibitor according to a proportion, then carrying out vacuum defoaming mixing at the rotating speed of (500-1000) rpm, weighing accelerator according to a proportion, carrying out vacuum defoaming mixing at the rotating speed of (1000-2000) rpm after uniform mixing, immersing aerogel in prepared silicone rubber solution, heating to the temperature of (80-120) ℃ and curing for (5-30) min.
7) Slicing the solidified block into slices with the thickness of 2mm, and coating PET films on the two sides to obtain the gasket with high heat conductivity and high insulation.
8) The method for preparing the high-heat-conductivity high-insulation gasket according to claim 7, wherein the mass ratio of the chopped asphalt-based carbon fiber to the h-BN is (5-20): 100.
the invention discloses a high-heat-conductivity high-insulation gasket and a preparation method thereof, and the gasket has the following beneficial effects:
according to the high-heat-conductivity high-insulation gasket and the preparation method thereof, the high-heat-conductivity gasket is cut into a circular sheet with the diameter of 3cm by a cutter through a die, the heat conductivity coefficient of the circular sheet is tested by using a Hotdisk heat conduction tester according to the ISO 22007-2 standard, 6 sample sheets are tested, the average value is 3.1W/m.K, the test is performed according to the ASTM D149 standard, the breakdown voltage UD=13 kV of the high-heat-conductivity high-insulation gasket is achieved, and the high-heat-conductivity high-insulation gasket shows excellent heat conductivity and electrical insulation performance and can be applied to the field with high requirements on the heat conductivity coefficient and the insulation property.
Detailed Description
Example 1
The preparation method comprises the following steps:
1) Weighing 20g of h-BN, placing the h-BN in 1L of hexadecyl trimethyl ammonium bromide aqueous solution with the concentration of 1g/L, stirring the mixture in the cationic surfactant aqueous solution for 3 hours, performing suction filtration treatment on the treated h-BN, and placing the treated h-BN in a 50 ℃ oven for 24 hours for standby;
2) Placing 5g of chopped asphalt-based carbon fiber into 1L of H2SO4 water solution with the concentration of 2mol/L, stirring for 2 hours, carrying out suction filtration on the treated chopped asphalt-based carbon fiber, and placing the chopped asphalt-based carbon fiber into a 50 ℃ oven for drying for 24 hours for later use;
3) 15g of the treated h-BN and 1.5g of the chopped asphalt-based carbon fiber are weighed according to a proportion to prepare 1L of aqueous solution, the aqueous solution is stirred for 10min and then is kept stand for 30min, the two are combined together in an electrostatic self-assembly mode, and the aqueous solution is filtered by suction and then is placed in a 50 ℃ oven for drying for 24h for standby;
4) Preparing 20g of water solution of the filler and the carboxymethyl cellulose, wherein the filler accounts for 15wt% and the concentration of the carboxymethyl cellulose is 3wt%, and placing the prepared solution in a liquid nitrogen freezing platform for directional freezing to prepare ice cubes;
5) Placing the prepared ice cubes into a freeze dryer for cold drying for 5d to prepare aerogel;
6) Weighing vinyl-terminated silicone oil, hydrogen-containing silicone oil and inhibitor according to a proportion, then carrying out vacuum defoaming mixing at the rotating speed of (500-1000) rpm, weighing accelerator according to a proportion, carrying out vacuum defoaming mixing at the rotating speed of (1000-2000) rpm after uniform mixing, immersing aerogel in the prepared silicone rubber solution, heating to 80 ℃, and curing for 30min.
7) Slicing the solidified block into slices with the thickness of 2mm, and coating PET films on the two sides to obtain the gasket with high heat conductivity and high insulation.
The high heat conduction gasket is cut into a circular sheet with the diameter of 3cm by a cutter through a die, the heat conduction coefficient is tested by using a Hotdisk heat conduction tester according to the ISO 22007-2 standard, 6 sample sheets are tested, the average value is 3.1W/m.K, the test is carried out according to the ASTM D149 standard, the breakdown voltage UD=13 kV of the high heat conduction high insulation gasket shows excellent heat conduction performance and electric insulation performance, and the high heat conduction high insulation gasket can be applied to the field with high requirements on the heat conduction coefficient and the insulation performance.
Comparative example 1
This comparative example differs from example 1 in that the chopped strand pitch-based carbon fibers and h-BN were not treated and were directly frozen by liquid nitrogen.
1) Weighing h-BN, chopped asphalt-based carbon fiber and carboxymethyl cellulose according to a proportion to prepare 20g of aqueous solution, wherein the filler accounts for 15wt% and the concentration of the carboxymethyl cellulose is 3wt%, and placing the prepared solution on a liquid nitrogen freezing platform for directional freezing to prepare ice cubes;
2) Placing the prepared ice cubes into a freeze dryer for cold drying for 5d to prepare aerogel;
3) Weighing vinyl-terminated silicone oil, hydrogen-containing silicone oil and inhibitor according to a proportion, then carrying out vacuum defoaming mixing at the rotating speed of (500-1000) rpm, weighing accelerator according to a proportion, carrying out vacuum defoaming mixing at the rotating speed of (1000-2000) rpm after uniform mixing, immersing aerogel in the prepared silicone rubber solution, heating to 80 ℃, and curing for 30min.
4) Slicing the solidified block into slices with the thickness of 2mm, and coating PET films on the two sides to obtain the gasket with high heat conductivity and high insulation.
The high heat conduction gasket is cut into a circular sheet with the diameter of 3cm by a cutter through a die, the heat conduction coefficient is tested by using a Hotdisk heat conduction tester according to the ISO 22007-2 standard, 6 sample sheets are tested, the average value is 1.6W/m.K, the breakdown voltage UD=2.5 kV of the gasket is tested according to the ASTM D149 standard, compared with the heat conduction performance and the electric insulation performance of the gasket in the embodiment 1, the gasket shows the general heat conduction performance and the poor electric insulation performance, and the gasket can be only applied to the field with low requirements on the heat conduction coefficient and the electric insulation performance.
Comparative example 2
This comparative example differs from example 1 in that the chopped pitch-based carbon fibers and h-BN were directly prepared into a thermally conductive gasket by blending.
The preparation method of the heat conduction gasket comprises the following steps:
1) Weighing vinyl-terminated silicone oil, hydrogen-containing silicone oil, inhibitor, chopped asphalt-based carbon fiber and h-BN in proportion (15% of total mass), then carrying out vacuum defoaming mixing at a rotating speed of 500rpm, weighing accelerator in proportion, and carrying out vacuum defoaming mixing at a rotating speed of 1000rpm after uniform mixing;
2) The evenly mixed slurry is coated on a PET film by using a coating machine, and the coating thickness is 2mm;
3) And (3) coating a layer of PET film on the upper part of the patch, and heating and curing for 30min at 80 ℃ to obtain the heat-conducting gasket.
The heat conducting gasket is cut into a circular sheet with the diameter of 3cm by a cutter through a die, the heat conducting coefficient is tested by using a Hotdisk heat conducting tester according to the ISO 22007-2 standard, 6 sample sheets are tested, the average value is 0.7W/m.K, the breakdown voltage UD=0.8 kV of the gasket is tested according to the ASTM D149 standard, the heat conducting property and the electric insulating property of the gasket are obviously reduced compared with those of the embodiment 1, and the gasket shows poor heat conducting property and poor electric insulating property and can be only applied to the field with very low requirements on the heat conducting coefficient and the electric insulating property.
The foregoing has shown and described the basic principles and main features of the present invention and the advantages of the present invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. The utility model provides a high heat conduction high insulation gasket, includes liquid silicone rubber and heat conduction filler main part, its characterized in that: the liquid silicone rubber in the high-heat-conductivity high-insulation gasket comprises vinyl-terminated silicone oil, hydrogen-containing silicone oil, an inhibitor and an accelerator; the main body of the heat-conducting filler is h-BN with good heat-conducting property and excellent insulativity, and is compounded with asphalt-based chopped carbon fiber with excellent heat-conducting property, and the two are combined together in an electrostatic self-assembly mode;
the preparation steps of the high-heat-conductivity high-insulation gasket are as follows:
1) Placing the h-BN in a cationic surfactant aqueous solution with a certain concentration, stirring the mixture for (3-6) h, controlling the concentration of the h-BN at (10-50) g/L, carrying out suction filtration on the treated h-BN, and placing the treated h-BN in a 50 ℃ oven for drying for 24h for later use;
2) Placing chopped pitch-based carbon fiber at a certain concentration of H 2 SO 4 Stirring in an aqueous solution for 2-6 h, controlling the concentration of the pitch-based chopped carbon fibers to be (5-25) g/L, and placing the treated chopped pitch-based carbon fibers in a baking oven at 50 ℃ for 24h for standby after suction filtration;
3) Weighing the treated h-BN and the chopped asphalt-based carbon fiber according to a proportion to prepare an aqueous solution, controlling the total concentration of the filler to be (15-50) g/L, stirring for (5-15) min, standing for (10-30) min, combining the two materials together in a static self-assembly mode, and placing the mixture in a 50 ℃ oven for baking for 24 hours for later use after suction filtration;
4) Preparing the filler and the carboxymethyl cellulose into an aqueous solution, wherein the filler accounts for (15-20) weight percent, the concentration of the carboxymethyl cellulose is (1-3) weight percent, and the prepared solution is placed in a liquid nitrogen freezing platform for directional freezing to prepare ice cubes;
5) Placing the prepared ice cubes into a freeze dryer for cold drying (3-5) d to prepare aerogel;
6) Weighing vinyl-terminated silicone oil, hydrogen-containing silicone oil and inhibitor according to a proportion, then carrying out vacuum defoaming mixing at the rotating speed of (500-1000) rpm, weighing accelerator according to a proportion, carrying out vacuum defoaming mixing at the rotating speed of (1000-2000) rpm after uniform mixing, soaking aerogel in prepared silicone rubber solution, heating to the temperature of (80-120) ℃ and curing for (5-30) min;
7) Slicing the solidified block into slices with the thickness of 2mm, and coating PET films on the two sides to obtain the gasket with high heat conductivity and high insulation.
2. The high thermal conductivity and high insulation gasket as defined in claim 1, wherein: the mass ratio of the vinyl-terminated silicone oil to the hydrogen-containing silicone oil to the inhibitor to the accelerator is 100: (15-25): (3-8): (5-10).
3. The high thermal conductivity and high insulation gasket as defined in claim 1, wherein: the particle size of the h-BN is (10-30) mu m.
4. The high thermal conductivity and high insulation gasket as defined in claim 1, wherein: the pitch-based carbon fiber has a diameter of 7 μm and a length of (0.1-0.3) mm.
5. The high thermal conductivity and high insulation gasket as defined in claim 1, wherein: the h-BN is treated by using a cationic surfactant, wherein the cationic surfactant is one or more of hexadecyl trimethyl ammonium bromide and dodecyl dimethyl amine oxide, and the concentration of the cationic surfactant aqueous solution is (0.1-20) g/L.
6. The high thermal conductivity and high insulation gasket as defined in claim 1, wherein: the pitch-based chopped carbon fiber uses H 2 SO 4 Sulfonation to negatively charge H 2 SO 4 The concentration of (C) is (2-4) mol/L.
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| WO2017143625A1 (en) * | 2016-02-25 | 2017-08-31 | 深圳市欧姆阳科技有限公司 | High thermal conductive composite material, thermal conductive sheet prepared from material, and preparation method therefor |
| WO2021128895A1 (en) * | 2019-12-26 | 2021-07-01 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity insulating layer material, metal substrate, and preparation method |
| CN114426774A (en) * | 2022-03-19 | 2022-05-03 | 南京冠旭新材料科技有限公司 | High-thermal-conductivity gasket and preparation method thereof |
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| WO2017143625A1 (en) * | 2016-02-25 | 2017-08-31 | 深圳市欧姆阳科技有限公司 | High thermal conductive composite material, thermal conductive sheet prepared from material, and preparation method therefor |
| WO2021128895A1 (en) * | 2019-12-26 | 2021-07-01 | 苏州巨峰电气绝缘系统股份有限公司 | High-thermal-conductivity insulating layer material, metal substrate, and preparation method |
| CN114426774A (en) * | 2022-03-19 | 2022-05-03 | 南京冠旭新材料科技有限公司 | High-thermal-conductivity gasket and preparation method thereof |
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