CN112341819B - Preparation method of insulating graphene heat-conducting gasket - Google Patents
Preparation method of insulating graphene heat-conducting gasket Download PDFInfo
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- CN112341819B CN112341819B CN202011337284.5A CN202011337284A CN112341819B CN 112341819 B CN112341819 B CN 112341819B CN 202011337284 A CN202011337284 A CN 202011337284A CN 112341819 B CN112341819 B CN 112341819B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000000945 filler Substances 0.000 claims abstract description 99
- 239000007788 liquid Substances 0.000 claims abstract description 38
- 239000006185 dispersion Substances 0.000 claims abstract description 29
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 20
- 239000004945 silicone rubber Substances 0.000 claims abstract description 17
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 238000005520 cutting process Methods 0.000 claims abstract description 13
- 238000006722 reduction reaction Methods 0.000 claims abstract description 13
- 239000003607 modifier Substances 0.000 claims abstract description 11
- 238000013329 compounding Methods 0.000 claims abstract description 8
- 238000000707 layer-by-layer assembly Methods 0.000 claims abstract description 7
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 27
- 238000003756 stirring Methods 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 10
- 230000009467 reduction Effects 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 238000005507 spraying Methods 0.000 claims description 9
- 238000004073 vulcanization Methods 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 8
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 8
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 6
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 6
- 239000008103 glucose Substances 0.000 claims description 6
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 5
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 4
- 229910052582 BN Inorganic materials 0.000 claims description 4
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 4
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 claims description 4
- 125000005842 heteroatom Chemical group 0.000 claims description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 4
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims description 4
- 229910000043 hydrogen iodide Inorganic materials 0.000 claims description 4
- 239000000395 magnesium oxide Substances 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 239000000377 silicon dioxide Substances 0.000 claims description 4
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 239000004408 titanium dioxide Substances 0.000 claims description 4
- 239000011782 vitamin Substances 0.000 claims description 4
- 229940088594 vitamin Drugs 0.000 claims description 4
- 229930003231 vitamin Natural products 0.000 claims description 4
- 235000013343 vitamin Nutrition 0.000 claims description 4
- 239000011787 zinc oxide Substances 0.000 claims description 4
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 125000002791 glucosyl group Chemical group C1([C@H](O)[C@@H](O)[C@H](O)[C@H](O1)CO)* 0.000 claims description 3
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 3
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims description 3
- 235000010265 sodium sulphite Nutrition 0.000 claims description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 8
- 150000001875 compounds Chemical class 0.000 description 12
- 239000002131 composite material Substances 0.000 description 11
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N Alumina Chemical compound [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 3
- 229920001971 elastomer Polymers 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010008 shearing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 125000000623 heterocyclic group Chemical group 0.000 description 2
- 238000004806 packaging method and process Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- KHDSWONFYIAAPE-UHFFFAOYSA-N silicon sulfide Chemical compound S=[Si]=S KHDSWONFYIAAPE-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 230000017525 heat dissipation Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- -1 heterocyclic quaternary ammonium salt Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- JVBXVOWTABLYPX-UHFFFAOYSA-L sodium dithionite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])=O JVBXVOWTABLYPX-UHFFFAOYSA-L 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C08J5/18—Manufacture of films or sheets
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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Abstract
The invention discloses a preparation method of an insulated graphene heat-conducting gasket, which comprises the following steps: preparing a dispersion liquid by using a modifier with amino, and modifying an insulating filler by using the dispersion liquid to obtain a modified insulating filler with positive charges covered on the surface; modifying the graphene oxide by using the modified insulating filler according to the electrostatic self-assembly principle to obtain the insulating heat-conducting filler coated with the graphene oxide; carrying out chemical reduction on the insulating heat-conducting filler by using a reducing agent to obtain a hybrid insulating heat-conducting filler; and step three, compounding the hybrid insulating heat-conducting filler with liquid vulcanized silicone rubber, defoaming and orienting by using an orienter after compounding, vulcanizing, and cutting along the direction vertical to the orientation direction after vulcanizing to obtain the heat-conducting gasket. The invention aims to further improve the heat-conducting property and the insulating property of the product.
Description
Technical Field
The invention relates to the technical field of heat conduction materials, in particular to a preparation method of an insulating graphene heat conduction gasket.
Background
The introduction of high frequency in the 5G era, the upgrading of hardware parts, and the multiplication of the number of internet devices and antennas, which present new requirements and challenges for related materials in the industry chain. Along with the updating and upgrading of electronic products, the power consumption and the heat productivity of equipment are continuously increased, and in order to improve the heat conduction performance and prevent short circuit of the equipment caused by a heat conduction gasket, higher technical requirements are put forward on the heat conduction performance and the insulation performance of a thermal interface material.
Graphene has been attracting attention as a novel carbon material since it was discovered in 2004. The material is a quasi-two-dimensional crystal material which is composed of sp2 hybridized carbon atoms and has the thickness of only a single atomic layer or a plurality of single atomic layers, and has excellent performances of high light transmittance, electric conductivity, thermal conductivity, high specific surface area, high strength, flexibility and the like. The graphene has excellent heat conductivity which is 10 times that of copper as high as 5000W/(m.K), has ultrahigh specific surface area as high as 2600 m2/g and ultrahigh strength which is 100 times that of steel, and has good flexibility and extensibility. Therefore, graphene is an ideal light-weight and efficient heat management material in theory. However, the material has ultrahigh conductivity, so that the thermal interface material has conductivity; this is extremely disadvantageous for circuit packaging, and therefore, it is a difficult problem and challenge to overcome this drawback and make the carbon nanomaterial fully perform its thermal conductivity.
The document with publication number CN111171381A discloses a nano α -alumina-loaded thermal reduction graphene, a preparation method thereof, and a high thermal conductivity electrical insulation elastomer thermal interface material, and the scheme is as follows: mixing the graphene oxide slurry with the nano gamma-alumina dispersion liquid, carrying out ultrasonic stirring and electrostatic self-assembly for 0.5-5 h, and then carrying out centrifugal freeze drying to obtain nano alumina-loaded graphene oxide powder; and heating the obtained powder to 600-2000 ℃ under the protection of nitrogen and keeping the temperature for 0.5-2 hours to obtain the nano alpha-alumina loaded thermal reduction graphene. The obtained reduced hybrid filler and the micron filler are compounded and used to be filled into silicon rubber, and the obtained thermal interface material has high volume resistivity and thermal conductivity, can meet the performance requirements of integrated circuit packaging heat dissipation, but still has the following technical problems:
1. the surface of the graphene oxide is negatively charged, and the surface of the aluminum oxide is-OH, which is similar to the negative charge property, so that the electrostatic self-assembly effect is poor, and the product quality is influenced.
2. The technique is to mix Al 2 O 3 The coated graphene is directly filled in the organic silicon rubber, no orientation is carried out on the graphene, and the specification shows that the highest thermal conductivity is only 4.11W/(m.k), and the thermal conductivity is still poor.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of an insulated graphene heat conduction gasket, and the invention aims to further improve the heat conduction performance and the insulation performance of a product.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of an insulated graphene heat conduction gasket is characterized by comprising the following steps:
preparing a dispersion liquid by using a modifier with amino, and modifying an insulating filler by using the dispersion liquid to obtain a modified insulating filler with positive charges covered on the surface;
modifying the graphene oxide by using the modified insulating filler according to the electrostatic self-assembly principle to obtain the insulating heat-conducting filler coated with the graphene oxide; carrying out chemical reduction on the insulating heat-conducting filler by using a reducing agent to obtain a hybrid insulating heat-conducting filler;
and step three, compounding the hybrid insulating heat-conducting filler with liquid vulcanized silicone rubber, defoaming and orienting by using an orienter after compounding, vulcanizing, and cutting along the direction vertical to the orientation direction after vulcanizing to obtain the heat-conducting gasket.
The specific method of the first step comprises the following steps: uniformly stirring 0.1-5 parts by weight of modifier with amino, 10-50 parts by weight of absolute ethyl alcohol and 0.01-1 part by weight of concentrated hydrochloric acid to obtain hydrolyzed dispersion liquid; and adding the dispersion into 100 parts by weight of insulating filler in a spraying manner, and drying at the temperature of 80 ℃ for 1-2h to obtain the modified insulating filler with the surface covered with positive charges.
The insulating filler is one or a plurality of materials mixed according to any proportion of silicon dioxide, boron nitride, silicon carbide, zinc oxide, magnesium oxide, aluminum nitride and titanium dioxide, and the size of the insulating filler is 50nm-500 nm.
The modifier with amino is one or more of 3-aminopropyl trimethoxy silane, quaternary ammonium salt with alkyl, quaternary ammonium salt containing hetero atom, quaternary ammonium salt containing benzene ring and quaternary ammonium salt containing heterocycle in any proportion.
The specific method of the second step is as follows: firstly, ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 0.5-1h, then adding 0.1-10 parts by weight of modified insulating filler and stirring for 2-6h, then adjusting the pH to 7.5-9 by using a pH regulator, and finally adding a reducing agent for reduction and washing to obtain the hybrid insulating heat-conducting filler.
The pH regulator is one or more of ammonia water, triethanolamine and AMP95 mixed according to any proportion.
The reducing agent is glucose, vitamins, hydrogen iodide, hydrazine hydrate, NaBH 4 One or more of sodium bisulfite and sodium sulfite mixed according to any proportion.
The third step is specifically as follows: firstly, stirring and mixing 1-100 parts by weight of hybrid insulating heat-conducting filler and 1-100 parts by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 5-100Pa.s, then grinding for 10-100 times by using a three-roll grinder, then adding into an orienter for defoaming and orientation, then vulcanizing, and cutting along the direction vertical to the orientation direction after vulcanization to obtain the heat-conducting gasket.
The orientation device comprises a first orientation piece and a second orientation piece which are fixedly connected, wherein an annular feeding hole and a rectangular discharging hole are respectively formed in two ends of the first orientation piece, and a first orientation channel with an inner cavity gradually changed into a rectangle from an annular shape is arranged in the first orientation piece; and a second orientation channel is arranged in the second orientation piece, one end of the second orientation channel is communicated with the rectangular discharge hole as a material inlet, the other end of the second orientation channel is used as a material outlet, and orientation convex columns are uniformly distributed on the inner wall of the second orientation channel.
The second orientation piece comprises a groove body, a cover plate and a fastener, the groove body is fixed at the rectangular discharge port of the first orientation piece, and the orientation convex columns are uniformly distributed on the groove body; one side of the cover plate is hinged with the groove body, and the other side of the cover plate is fixedly connected with the groove body through a fastener; the second orientation channel is formed by fixing the cover plate on the groove body.
The orientation convex columns are arranged in multiple rows, and two adjacent rows of orientation convex columns are distributed in a staggered mode.
The orientation convex column is in a water drop shape and is contacted with the cover plate.
The rectangular discharge port is of a rectangular structure, and the second orientation channel is of a rectangular structure.
The annular feed inlet is of a circular structure or an oval structure.
The invention has the advantages that:
1. according to the invention, the modifier with amino is used for preparing the dispersion liquid, and the dispersion liquid is used for modifying the insulating filler, so that the modified insulating filler with positive charges covered on the surface can be obtained. Through the modified insulating filler with positive charges, the modified insulating filler can be subjected to electrostatic self-assembly and chemical generation with negative charges on the surface of graphene to form electrostatic action and chemical bonding, so that de-coating cannot occur in the subsequent processing process, and the heat conducting property and the insulating property of a product can be further improved.
2. The insulating filler with a specific structure is adopted, the density is lower, and the graphene sheet can bear more quantity, so that the insulating property is improved more. Meanwhile, the strength of the silicon rubber can be increased, so that the mechanical property of the product is superior to that of a conventional heat-conducting product.
3. The orientation product provided by the invention is provided with two orientation pieces with specific channels, and compared with the prior art, the orientation product is simpler in structure and can effectively reduce energy consumption. Furthermore, the first orientation channel is gradually changed from a ring shape to a rectangle shape, so that when the composite material passes through the first orientation channel of the specific structure, the composite material can generate an internal shearing force due to different internal and external flow rates caused by the change of the inner diameter of the inner cavity, and the internal shearing force can perform first orientation on the composite material in the flow direction. When the composite material passes through the second orientation channel, the composite material can be oriented for the second time in the flowing direction due to the obstruction of the orientation convex columns. The degree of orientation of the composite material can be further improved by the cooperation of the two orientations.
4. According to the invention, a product with higher heat conductivity coefficient and insulation coefficient can be obtained through a specific preparation process, specifically, the highest heat conductivity coefficient of the obtained heat conduction gasket can reach 25W/(m.k), and the breakdown voltage resistance can reach 8kv @1 mm.
Drawings
FIG. 1 is an SEM photograph of the hybrid insulating and heat conducting filler obtained in step two of the present invention;
FIG. 2 is a diagram showing the effect of the present invention after step three;
FIG. 3 is a schematic plan view of the orienter cover of the present invention when open;
FIG. 4 is a schematic plan view of the orienter cover of the present invention when closed;
FIG. 5 is a schematic perspective view of an aligner according to the present invention;
labeled as: 1. the device comprises a first orientation piece, a second orientation piece, a ring-shaped feed inlet, a rectangular discharge outlet, a first orientation channel, a second orientation channel, a groove body, a cover plate, a second orientation channel, a cover plate, a first orientation convex column, a second orientation convex column, a cover plate, a fastening piece and a fastening piece.
Detailed Description
The invention provides a preparation method of an insulated graphene heat conduction gasket, which comprises the following steps:
step one, preparing a dispersion liquid by using a modifier with amino, and modifying the insulating filler by using the dispersion liquid to obtain the modified insulating filler with the surface covered with positive charges.
Preferably, the specific method of the step one is as follows: uniformly stirring 0.1-5 parts by weight of modifier with amino, 10-50 parts by weight of absolute ethyl alcohol and 0.01-1 part by weight of concentrated hydrochloric acid to obtain hydrolyzed dispersion liquid; and adding the dispersion into 100 parts by weight of insulating filler in a spraying manner, and drying at the temperature of 80 ℃ for 1-2h to obtain the modified insulating filler with the surface covered with positive charges.
The insulating filler is one or a plurality of materials mixed according to any proportion of silicon dioxide, boron nitride, silicon carbide, zinc oxide, magnesium oxide, aluminum nitride and titanium dioxide, and the size of the insulating filler is 50nm-500 nm.
The modifier with amino is one or more of 3-aminopropyl trimethoxy silane, quaternary ammonium salt with alkyl, quaternary ammonium salt containing hetero atom, quaternary ammonium salt containing benzene ring and quaternary ammonium salt containing heterocycle in any proportion.
Modifying the graphene oxide by using the modified insulating filler according to the electrostatic self-assembly principle to obtain the insulating heat-conducting filler coated with the graphene oxide; and chemically reducing the insulating heat-conducting filler by using a reducing agent to obtain the hybrid insulating heat-conducting filler.
Preferably, the specific method of the second step is as follows: firstly, ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 mu m in 100 parts by weight of N, N-dimethylformamide for 0.5-1h, then adding 0.1-10 parts by weight of modified insulating filler and stirring for 2-6h, then adjusting the pH to 7.5-9 by using a pH regulator, and finally adding a reducing agent for reduction and washing to obtain the hybrid insulating heat-conducting filler.
The pH regulator is one or more of ammonia water, triethanolamine and AMP95 mixed according to any proportion.
The reducing agent is glucose, vitamins, hydrogen iodide, hydrazine hydrate, NaBH 4 One or more of sodium bisulfite and sodium sulfite mixed according to any proportion.
And step three, compounding the hybrid insulating heat-conducting filler with liquid vulcanized silicone rubber, defoaming and orienting by using an orienter after compounding, vulcanizing, and cutting along the direction vertical to the orientation direction after vulcanizing to obtain the heat-conducting gasket.
Preferably, the specific method of the third step is as follows: firstly, stirring and mixing 1-100 parts by weight of hybrid insulating heat-conducting filler and 1-100 parts by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 5-100Pa.s, then grinding for 10-100 times by using a three-roll grinder, then adding into an orienter for defoaming and orientation, then vulcanizing, and cutting along the direction vertical to the orientation direction after vulcanization to obtain the heat-conducting gasket.
Preferably, the orientation device comprises a first orientation piece 1 and a second orientation piece 2 which are fixedly connected, wherein both ends of the first orientation piece 1 are respectively provided with an annular feeding hole 3 and a rectangular discharging hole 4, and a first orientation channel 5 with an inner cavity gradually changed into a rectangle from an annular shape is arranged in the first orientation piece 1; the first orientation channel 5 can generate an internal shearing force on the composite material due to the change of the inner diameter and the shape, so that the composite material is oriented in the flowing direction. A second orientation channel 6 is arranged in the second orientation piece 2, one end of the second orientation channel 6 is used as a material inlet and is communicated with the rectangular discharge hole 4, and the size of the material inlet is consistent with that of the rectangular discharge hole 4; the other end is used as a material outlet. In addition, the inner wall of the second orientation channel 6 is uniformly distributed with orientation convex columns 9, and the orientation convex columns 9 block the composite material, so that the composite material is oriented in the flowing direction again.
Since the first orientation member 1 has a specific structure, the first orientation member 1 can be prepared by using two rectangular sheets and two arc-shaped sheets. Specifically, the one end of two arc pieces remains unchanged for the arc, changes gradually the other end of two arc pieces into the plane earlier gradually, welds two rectangle pieces between two arc pieces again, can obtain the first orientation piece 1 that both ends have annular feed inlet 3 and rectangle discharge gate 4 respectively.
The second orientation piece 2 is preferably set to be an openable and closable structure, and specifically comprises a groove body 7, a cover plate 8 and a fastening piece 10, wherein the groove body 7 can be fixed at the rectangular discharge port 4 of the first orientation piece 1 in a welding manner, one side of the cover plate 8 is hinged to the groove body 7, and the other side of the cover plate 8 is fixedly connected with the groove body 7 through the fastening piece 10, so that the cover plate 8 can be opened on the groove body 7. The second orientation channel 6 is formed by a cover plate 8 fixed to the housing 7. Namely, after the cover plate 8 is covered, the second orientation channel 6 is formed between the cover plate 8 and the groove body 7. Of course, a corresponding sealing element can be provided between the cover plate 8 and the housing 7 to ensure a better sealing effect of the second orientation element 2.
Furthermore, the orientation convex columns 9 are uniformly distributed on the groove body 7 in multiple rows, and the adjacent two rows of orientation convex columns 9 are distributed in a staggered manner. Preferably, the orientation convex column 9 is in a water drop shape, and after the cover plate 8 is covered, the section surface of the orientation convex column 9 is contacted with the cover plate 8, so that the orientation effect of the composite material is better.
Furthermore, the annular feed inlet 3 is of a circular structure or an oval structure, the rectangular discharge outlet 4 is of a rectangular structure, the second orientation piece 2 is of a cuboid structure, and the second orientation channel 6 is of a rectangular structure.
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited thereto.
Example 1
The embodiment provides a preparation method of an insulating graphene heat conduction gasket, which comprises the following steps:
firstly, adding 100 parts by weight of silicon dioxide into a high-speed stirrer, and uniformly stirring 0.1 part by weight of 3-aminopropyltrimethoxysilane, 10 parts by weight of absolute ethyl alcohol and 0.01 part by weight of concentrated hydrochloric acid to prepare hydrolyzed dispersion liquid; and then adding the dispersion into the insulating filler in a spraying mode, and drying at the temperature of 80 ℃ for 1h to obtain the modified insulating filler with the surface covered with positive charges.
Ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 0.5h, adding 0.1 part by weight of modified insulating filler, stirring for 2h, modifying the graphene oxide, and obtaining the insulating heat-conducting filler coated with the graphene oxide; and then adjusting the pH value to 7.5-9 by using ammonia water, finally adding glucose for reduction and washing to obtain the hybrid insulating heat-conducting filler.
And step three, stirring and mixing 1 part by weight of hybrid insulating heat-conducting filler and 1 part by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 5Pa.s, grinding for 10 times by using a three-roll grinder to compound the hybrid insulating heat-conducting filler and the liquid vulcanized silicone rubber, then adding the compound into an orienter to defoam and orient, vulcanizing after orientation, and cutting in a direction perpendicular to the orientation direction after vulcanization to obtain the heat-conducting gasket.
Example 2
The embodiment provides a preparation method of an insulating graphene heat conduction gasket, which comprises the following steps:
firstly, 100 parts by weight of boron nitride is added into a high-speed stirrer, and then 5 parts by weight of quaternary ammonium salt with alkyl, 50 parts by weight of absolute ethyl alcohol and 1 part by weight of concentrated hydrochloric acid are uniformly stirred to prepare hydrolyzed dispersion liquid; and then adding the dispersion into the insulating filler in a spraying mode, and drying at the temperature of 80 ℃ for 2h to obtain the modified insulating filler with the surface covered with positive charges.
Ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 1h, adding 3 parts by weight of modified insulating filler, stirring for 6h, modifying the graphene oxide and obtaining the insulating heat-conducting filler coated with the graphene oxide; and regulating the pH value to 7.5-9 by using triethanolamine, finally adding vitamins for reduction and washing, and washing to obtain the hybrid insulating heat-conducting filler.
And step three, stirring and mixing 100 parts by weight of hybrid insulating heat-conducting filler and 100 parts by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 100Pa.s, grinding for 100 times by using a three-roll grinder to compound the hybrid insulating heat-conducting filler and the liquid vulcanized silicone rubber, then adding the compound into an orienter to defoam and orient, vulcanizing after orientation, and cutting in a direction perpendicular to the orientation direction after vulcanization to obtain the heat-conducting gasket.
Example 3
The embodiment provides a preparation method of an insulating graphene heat conduction gasket, which comprises the following steps:
firstly, adding 100 parts by weight of silicon carbide into a high-speed stirrer, and uniformly stirring 3 parts by weight of quaternary ammonium salt containing heteroatoms, 30 parts by weight of absolute ethyl alcohol and 0.5 part by weight of concentrated hydrochloric acid to prepare hydrolyzed dispersion liquid; and then adding the dispersion into the insulating filler in a spraying mode, and drying at the temperature of 80 ℃ for 1.5h to obtain the modified insulating filler with the surface covered with positive charges.
Ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 0.5h, adding 10 parts by weight of modified insulating filler, stirring for 4h, modifying the graphene oxide and obtaining the insulating heat-conducting filler coated with the graphene oxide; and then, adjusting the pH value to 7.5-9 by using AMP95, finally adding hydrogen iodide for reduction and washing, and obtaining the hybrid insulating heat-conducting filler after washing.
And step three, stirring and mixing 50 parts by weight of hybrid insulating heat-conducting filler and 50 parts by weight of liquid silicon sulfide rubber in a double-planet stirrer until the viscosity is 50Pa.s, grinding for 55 times by using a three-roll grinder to compound the hybrid insulating heat-conducting filler and the liquid silicon sulfide rubber, then adding the compound into an orienter to defoam and orient, vulcanizing after orientation, and cutting in a direction perpendicular to the orientation direction after vulcanization to obtain the heat-conducting gasket.
Example 4
The embodiment provides a preparation method of an insulating graphene heat conduction gasket, which comprises the following steps:
firstly, adding 100 parts by weight of a mixture of zinc oxide and magnesium oxide into a high-speed stirrer, and uniformly stirring 2 parts by weight of heterocyclic quaternary ammonium salt, 40 parts by weight of absolute ethyl alcohol and 0.7 part by weight of concentrated hydrochloric acid to prepare hydrolyzed dispersion liquid; and then adding the dispersion into the insulating filler in a spraying mode, and drying at the temperature of 80 ℃ for 1h to obtain the modified insulating filler with the surface covered with positive charges.
Ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 1h, adding 8 parts by weight of modified insulating filler, stirring for 3h, modifying the graphene oxide and obtaining the insulating heat-conducting filler coated with the graphene oxide; then adjusting the pH to 7.5-9 by using a mixed solution of ammonia water and triethanolamine, and finally adding hydrazine hydrate and NaBH 4 Reducing and washing the mixture of the sodium hydrosulfite to obtain impuritiesInsulating heat-conducting filler.
And step three, stirring and mixing 1-100 parts by weight of hybrid insulating heat-conducting filler and 1-100 parts by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 5-100Pa.s, grinding for 10-100 times by using a three-roll grinder to compound the hybrid insulating heat-conducting filler and the liquid vulcanized silicone rubber, then adding the compound into an orienter to defoam and orient, vulcanizing after orientation, and cutting along the direction vertical to the orientation direction after vulcanization to obtain the heat-conducting gasket.
Example 5
The embodiment provides a preparation method of an insulating graphene heat conduction gasket, which comprises the following steps:
firstly, adding 100 parts by weight of aluminum nitride into a high-speed stirrer, and uniformly stirring 5 parts by weight of a mixture of 3-aminopropyltrimethoxysilane and quaternary ammonium salt with alkyl, 10 parts by weight of absolute ethyl alcohol and 1 part by weight of concentrated hydrochloric acid to prepare hydrolyzed dispersion liquid; and then adding the dispersion into the insulating filler in a spraying mode, and drying at the temperature of 80 ℃ for 2h to obtain the modified insulating filler with the surface covered with positive charges.
Ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 1h, adding 6 parts by weight of modified insulating filler, stirring for 5h, and modifying the graphene oxide to obtain the insulating heat-conducting filler coated with the graphene oxide; and then adjusting the pH value to 7.5-9 by using ammonia water, finally adding glucose for reduction and washing to obtain the hybrid insulating heat-conducting filler.
And step three, stirring and mixing 80 parts by weight of hybrid insulating heat-conducting filler and 60 parts by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 80Pa.s, grinding for 40 times by using a three-roll grinder to compound the hybrid insulating heat-conducting filler and the liquid vulcanized silicone rubber, then adding the compound into an orienter to defoam and orient, vulcanizing after orientation, and cutting in a direction perpendicular to the orientation direction after vulcanization to obtain the heat-conducting gasket.
Example 6
The embodiment provides a preparation method of an insulating graphene heat conduction gasket, which comprises the following steps:
firstly, adding 100 parts by weight of titanium dioxide into a high-speed stirrer, and uniformly stirring 4 parts by weight of 3-aminopropyltrimethoxysilane, 25 parts by weight of absolute ethyl alcohol and 1 part by weight of concentrated hydrochloric acid to prepare hydrolyzed dispersion; and then adding the dispersion into the insulating filler in a spraying mode, and drying at the temperature of 80 ℃ for 1h to obtain the modified insulating filler with the surface covered with positive charges.
Ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 0.5h, adding 2 parts by weight of modified insulating filler, stirring for 2h, modifying the graphene oxide and obtaining the insulating heat-conducting filler coated with the graphene oxide; and then adjusting the pH value to 7.5-9 by using ammonia water, finally adding glucose for reduction and washing to obtain the hybrid insulating heat-conducting filler.
And step three, stirring and mixing 1-100 parts by weight of hybrid insulating heat-conducting filler and 1-100 parts by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 5-100Pa.s, grinding for 10-100 times by using a three-roll grinder to compound the hybrid insulating heat-conducting filler and the liquid vulcanized silicone rubber, then adding the compound into an orienter to defoam and orient, vulcanizing after orientation, and cutting along the direction vertical to the orientation direction after vulcanization to obtain the heat-conducting gasket.
Example 7
The performance of the heat-conducting gasket described in the above embodiments 1 to 6 was tested, and the testing method and the testing results are shown in table 1 below.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.
Claims (7)
1. A preparation method of an insulated graphene heat conduction gasket is characterized by comprising the following steps:
preparing a dispersion liquid by using a modifier, and modifying an insulating filler by using the dispersion liquid to obtain a modified insulating filler with a positive charge covered on the surface;
modifying the graphene oxide by using the modified insulating filler according to the electrostatic self-assembly principle to obtain the insulating heat-conducting filler coated with the graphene oxide; carrying out chemical reduction on the insulating heat-conducting filler by using a reducing agent to obtain a hybrid insulating heat-conducting filler;
step three, compounding the hybrid insulating heat-conducting filler with liquid vulcanized silicone rubber, defoaming and orienting by using an orienter after compounding, vulcanizing, and cutting along the direction vertical to the orientation direction after vulcanizing to obtain a heat-conducting gasket;
the modifier is one or a plurality of 3-aminopropyl trimethoxy silane, quaternary ammonium salt with alkyl, quaternary ammonium salt containing hetero atoms and quaternary ammonium salt containing benzene rings which are mixed according to any proportion;
the orientation device comprises a first orientation piece (1) and a second orientation piece (2) which are fixedly connected, wherein two ends of the first orientation piece (1) are respectively provided with an annular feeding hole (3) and a rectangular discharging hole (4), and a first orientation channel (5) with an inner cavity gradually changed into a rectangle from an annular shape is arranged in the first orientation piece (1); a second orientation channel (6) is arranged in the second orientation piece (2), one end of the second orientation channel (6) is used as a material inlet and communicated with the rectangular discharge hole (4), the other end of the second orientation channel is used as a material outlet, and orientation convex columns (9) are uniformly distributed on the inner wall of the second orientation channel (6);
the second orientation piece (2) comprises a groove body (7), a cover plate (8) and a fastener (10), the groove body (7) is fixed at the rectangular discharge port (4) of the first orientation piece (1), and orientation convex columns (9) are uniformly distributed on the groove body (7); one side of the cover plate (8) is hinged with the groove body (7), and the other side is fixedly connected with the groove body (7) through a fastener (10); the second orientation channel (6) is formed by fixing a cover plate (8) on the groove body (7).
2. The preparation method of the insulating graphene thermal pad according to claim 1, wherein the preparation method comprises the following steps: the specific method of the first step comprises the following steps: uniformly stirring 0.1-5 parts by weight of modifier, 10-50 parts by weight of absolute ethyl alcohol and 0.01-1 part by weight of concentrated hydrochloric acid to obtain hydrolyzed dispersion liquid; and adding the dispersion into 100 parts by weight of insulating filler in a spraying manner, and drying at the temperature of 80 ℃ for 1-2h to obtain the modified insulating filler with the surface covered with positive charges.
3. The preparation method of the insulating graphene thermal pad according to claim 1, wherein the preparation method comprises the following steps: the insulating filler is one or a plurality of materials mixed according to any proportion of silicon dioxide, boron nitride, silicon carbide, zinc oxide, magnesium oxide, aluminum nitride and titanium dioxide, and the size of the insulating filler is 50nm-500 nm.
4. The preparation method of the insulating graphene thermal pad according to claim 1, wherein the preparation method comprises the following steps: the specific method of the second step is as follows: firstly, ultrasonically dispersing 10 parts by weight of graphene oxide with the sheet diameter of 1-10 microns in 100 parts by weight of N, N-dimethylformamide for 0.5-1h, then adding 0.1-10 parts by weight of modified insulating filler and stirring for 2-6h, then adjusting the pH to 7.5-9 by using a pH regulator, and finally adding a reducing agent for reduction and washing to obtain the hybrid insulating heat-conducting filler.
5. The preparation method of the insulating graphene thermal pad according to claim 1, wherein the preparation method comprises the following steps: the reducing agent is glucose, vitamins, hydrogen iodide, hydrazine hydrate, NaBH 4 One or more of sodium bisulfite and sodium sulfite mixed according to any proportion.
6. The preparation method of the insulating graphene thermal pad according to claim 1, wherein the preparation method comprises the following steps: the third step is specifically as follows: firstly, stirring and mixing 1-100 parts by weight of hybrid insulating heat-conducting filler and 1-100 parts by weight of liquid vulcanized silicone rubber in a double-planet stirrer until the viscosity is 5-100Pa.s, then grinding for 10-100 times by using a three-roll grinder, then adding into an orienter for defoaming and orientation, then vulcanizing, and cutting along the direction vertical to the orientation direction after vulcanization to obtain the heat-conducting gasket.
7. The preparation method of the insulating graphene thermal pad according to claim 1, wherein the preparation method comprises the following steps: the annular feed inlet (3) is of a circular structure or an oval structure.
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