CN114539781A - Heat-conducting gel and preparation method thereof - Google Patents
Heat-conducting gel and preparation method thereof Download PDFInfo
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- CN114539781A CN114539781A CN202011340888.5A CN202011340888A CN114539781A CN 114539781 A CN114539781 A CN 114539781A CN 202011340888 A CN202011340888 A CN 202011340888A CN 114539781 A CN114539781 A CN 114539781A
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- heat
- coupling agent
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000001879 gelation Methods 0.000 title description 2
- 239000000945 filler Substances 0.000 claims abstract description 32
- 239000007788 liquid Substances 0.000 claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 229910045601 alloy Inorganic materials 0.000 claims abstract description 12
- 239000000956 alloy Substances 0.000 claims abstract description 12
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 96
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 50
- 238000003756 stirring Methods 0.000 claims description 31
- 238000006459 hydrosilylation reaction Methods 0.000 claims description 30
- 239000003607 modifier Substances 0.000 claims description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 23
- 229920001296 polysiloxane Polymers 0.000 claims description 20
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 claims description 19
- 238000006243 chemical reaction Methods 0.000 claims description 19
- 229910052733 gallium Inorganic materials 0.000 claims description 19
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 17
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 17
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 17
- 229910001128 Sn alloy Inorganic materials 0.000 claims description 13
- 239000007809 chemical reaction catalyst Substances 0.000 claims description 12
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 12
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 10
- RHZWSUVWRRXEJF-UHFFFAOYSA-N indium tin Chemical compound [In].[Sn] RHZWSUVWRRXEJF-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002683 reaction inhibitor Substances 0.000 claims description 10
- CEBKHWWANWSNTI-UHFFFAOYSA-N 2-methylbut-3-yn-2-ol Chemical compound CC(C)(O)C#C CEBKHWWANWSNTI-UHFFFAOYSA-N 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 9
- 239000000654 additive Substances 0.000 claims description 8
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 claims description 8
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 8
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 8
- 238000004381 surface treatment Methods 0.000 claims description 8
- NMEPHPOFYLLFTK-UHFFFAOYSA-N trimethoxy(octyl)silane Chemical compound CCCCCCCC[Si](OC)(OC)OC NMEPHPOFYLLFTK-UHFFFAOYSA-N 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 239000011231 conductive filler Substances 0.000 claims description 7
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 7
- 229910000846 In alloy Inorganic materials 0.000 claims description 6
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 6
- 230000000996 additive effect Effects 0.000 claims description 6
- KQAHMVLQCSALSX-UHFFFAOYSA-N decyl(trimethoxy)silane Chemical compound CCCCCCCCCC[Si](OC)(OC)OC KQAHMVLQCSALSX-UHFFFAOYSA-N 0.000 claims description 6
- 229910052755 nonmetal Inorganic materials 0.000 claims description 6
- CLSUSRZJUQMOHH-UHFFFAOYSA-L platinum dichloride Chemical compound Cl[Pt]Cl CLSUSRZJUQMOHH-UHFFFAOYSA-L 0.000 claims description 6
- -1 rhodium metal compounds Chemical class 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- FBEIPJNQGITEBL-UHFFFAOYSA-J tetrachloroplatinum Chemical compound Cl[Pt](Cl)(Cl)Cl FBEIPJNQGITEBL-UHFFFAOYSA-J 0.000 claims description 5
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims description 4
- KSLSOBUAIFEGLT-UHFFFAOYSA-N 2-phenylbut-3-yn-2-ol Chemical compound C#CC(O)(C)C1=CC=CC=C1 KSLSOBUAIFEGLT-UHFFFAOYSA-N 0.000 claims description 4
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims description 4
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 4
- 239000003086 colorant Substances 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- YGUFXEJWPRRAEK-UHFFFAOYSA-N dodecyl(triethoxy)silane Chemical compound CCCCCCCCCCCC[Si](OCC)(OCC)OCC YGUFXEJWPRRAEK-UHFFFAOYSA-N 0.000 claims description 4
- 239000003063 flame retardant Substances 0.000 claims description 4
- 230000001788 irregular Effects 0.000 claims description 4
- 229910001338 liquidmetal Inorganic materials 0.000 claims description 4
- 229910044991 metal oxide Inorganic materials 0.000 claims description 4
- 150000004706 metal oxides Chemical class 0.000 claims description 4
- 150000004767 nitrides Chemical class 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229910052763 palladium Inorganic materials 0.000 claims description 4
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 claims description 4
- 239000004014 plasticizer Substances 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 229910052703 rhodium Inorganic materials 0.000 claims description 4
- 239000010948 rhodium Substances 0.000 claims description 4
- 239000004094 surface-active agent Substances 0.000 claims description 4
- 239000002562 thickening agent Substances 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 3
- 229910052582 BN Inorganic materials 0.000 claims description 2
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052581 Si3N4 Inorganic materials 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 150000001343 alkyl silanes Chemical class 0.000 claims description 2
- 150000004645 aluminates Chemical class 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 2
- 150000001412 amines Chemical class 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- YZZNJYQZJKSEER-UHFFFAOYSA-N gallium tin Chemical compound [Ga].[Sn] YZZNJYQZJKSEER-UHFFFAOYSA-N 0.000 claims description 2
- ORTRWBYBJVGVQC-UHFFFAOYSA-N hexadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCS ORTRWBYBJVGVQC-UHFFFAOYSA-N 0.000 claims description 2
- RSKGMYDENCAJEN-UHFFFAOYSA-N hexadecyl(trimethoxy)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OC)(OC)OC RSKGMYDENCAJEN-UHFFFAOYSA-N 0.000 claims description 2
- 239000003112 inhibitor Substances 0.000 claims description 2
- 230000002401 inhibitory effect Effects 0.000 claims description 2
- 230000000977 initiatory effect Effects 0.000 claims description 2
- 239000000395 magnesium oxide Substances 0.000 claims description 2
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 claims description 2
- 239000002923 metal particle Substances 0.000 claims description 2
- QJAOYSPHSNGHNC-UHFFFAOYSA-N octadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCS QJAOYSPHSNGHNC-UHFFFAOYSA-N 0.000 claims description 2
- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 2
- 150000002894 organic compounds Chemical class 0.000 claims description 2
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 claims description 2
- 229910052707 ruthenium Inorganic materials 0.000 claims description 2
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 claims description 2
- 239000012798 spherical particle Substances 0.000 claims description 2
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 2
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 claims description 2
- OYGYKEULCAINCL-UHFFFAOYSA-N triethoxy(hexadecyl)silane Chemical compound CCCCCCCCCCCCCCCC[Si](OCC)(OCC)OCC OYGYKEULCAINCL-UHFFFAOYSA-N 0.000 claims description 2
- MTPVUVINMAGMJL-UHFFFAOYSA-N trimethyl(1,1,2,2,2-pentafluoroethyl)silane Chemical compound C[Si](C)(C)C(F)(F)C(F)(F)F MTPVUVINMAGMJL-UHFFFAOYSA-N 0.000 claims description 2
- 229920002554 vinyl polymer Polymers 0.000 claims description 2
- 239000011787 zinc oxide Substances 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 50
- 239000000843 powder Substances 0.000 description 16
- 239000007822 coupling agent Substances 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 150000002258 gallium Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K5/00—Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
- C09K5/08—Materials not undergoing a change of physical state when used
-
- 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
- C08K3/08—Metals
- C08K2003/0806—Silver
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- 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
- C08K3/08—Metals
- C08K2003/0812—Aluminium
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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Abstract
The invention discloses a heat-conducting gel and a preparation method thereof, wherein the heat-conducting gel comprises a second-phase liquid, and the second-phase liquid is low-melting-point elemental metal or alloy with a melting point of 10-60 ℃. According to the invention, a small amount of second-phase liquid is introduced into the system, and a heat-conducting liquid bridge is built among the heat-conducting fillers by utilizing capillary force, so that the interface thermal resistance among the fillers is reduced, and the high heat conductivity coefficient of the heat-conducting gel is realized. Meanwhile, the heat-conducting gel prepared by the invention has low viscosity and moderate thixotropy, is more suitable for being operated in a continuous dispensing mode, saves labor and improves the production efficiency; and the use amount of the filler can be reduced, so that the heat-conducting gel is endowed with better flexibility. The preparation method is simple and feasible, and is a novel heat-conducting gel with large-scale industrial production prospect.
Description
Technical Field
The invention belongs to the technical field of high-molecular heat-conducting composite materials, and particularly relates to a heat-conducting gel and a preparation method thereof.
Background
With the rapid development of the electronic communication industry and the automobile industry, the heat dissipation requirements of 5G communication equipment, handheld electronic equipment, new energy automobile parts and the like are higher and higher. Therefore, it is particularly important to utilize thermal interface materials for heat dissipation purposes. At present, the thermal interface materials which are commonly used mainly comprise heat-conducting silicone grease, heat-conducting silicone gaskets, heat-conducting gel and the like, and the heat-conducting gel is concerned as a novel thermal interface material. The heat-conducting silicone grease has no crosslinking reaction, so that the defects of oil leakage, drying and the like are easily caused; the heat-conducting silica gel gasket generally adopts a die cutting method to obtain a film with a certain thickness in a regular shape, and is difficult to fill interfaces with irregular shapes and different joint filling thicknesses; and the heat-conducting gel avoids oil leakage and drying phenomena through a certain degree of cross-linking, can quickly realize automatic operation through dispensing equipment, and can well fill irregular interfaces to achieve the purpose of heat dissipation.
The existing heat-conducting gel mainly realizes high heat conductivity coefficient by adding high-content heat-conducting filler to form a heat-conducting passage, but the increase of the filler content will influence the integral mechanical property of the material, so that the hardness and viscosity of the material are increased, and the implementation of a dispensing process is influenced.
In view of the above analysis, the present invention aims to provide a thermal conductive gel that achieves a high thermal conductivity at a low filler loading content, and that has a low viscosity and good flexibility.
Disclosure of Invention
In order to solve the problems of the background art, the present invention provides a thermally conductive gel and a method for preparing the same. According to the invention, a small amount of second-phase liquid is introduced into the system, and a heat-conducting liquid bridge is built among the heat-conducting fillers by utilizing capillary force, so that the interface thermal resistance among the fillers is reduced, and the high heat conductivity coefficient of the heat-conducting gel is realized.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: on one hand, the invention provides a heat-conducting gel which is prepared from the following raw materials in parts by mass:
(A) 100 parts of organopolysiloxane containing at least 2 vinyl groups;
(B) 10-90 parts of polyorganosiloxane having at least 2 silicon-bonded hydrogen atoms;
(C) 0.1-10 parts of a hydrosilylation catalyst;
(D) 0.1-0.5 part of hydrosilylation inhibitor;
(E) 100 portions and 1200 portions of modified heat-conducting filler;
(F) 0.001-50 parts of second-phase liquid;
the second phase liquid is low-melting point elemental metal or alloy with the melting point between 10 and 60 ℃.
Further, the organopolysiloxane containing at least 2 vinyl groups has the following structural formula:
preferably, the organopolysiloxane having at least 2 vinyl groups has a viscosity of 20 to 1000mpa.s at 25 ℃.
Further, the polyorganosiloxane having at least 2 silicon-bonded hydrogen atoms has the following structural formula:
preferably, the polyorganosiloxane having at least 2 silicon-bonded hydrogen atoms has a viscosity of 20 to 100mPa.s at 25 ℃.
Further, the hydrosilylation reaction catalyst is a hydrosilylation reaction catalyst capable of initiating a hydrosilylation reaction of components (a) and (B);
preferably, the hydrosilylation reaction catalyst is at least one selected from the group consisting of platinum black, rhodium, ruthenium, palladium, platinum metal compounds and organic complexes thereof, rhodium metal compounds and organic complexes thereof, ruthenium metal compounds and organic complexes thereof, palladium metal compounds and organic complexes thereof;
still preferably, the hydrosilylation reaction catalyst is at least one selected from the group consisting of platinum black, a platinum metal compound, and an organic complex thereof;
more preferably, the platinum metal compound comprises platinum dichloride, platinum tetrachloride, chloroplatinic acid; the platinum metal compound organic compound comprises a compound of chloroplatinic acid, olefin and vinyl siloxane.
Further, the hydrosilylation reaction inhibitor is a hydrosilylation reaction inhibitor capable of inhibiting the hydrosilylation reaction of components (a) and (B);
preferably, the hydrosilylation reaction inhibitor is selected from at least one of alkynol, enyne compound, amine and maleate;
preferably, the alkynol comprises at least one of 2-methyl-3-butyn-2-ol, 3-methyl-1-butyn-3-ol, 2-phenyl-3-butyn-2-ol, 1-dimethyl-2-propynyloxytrimethylsilane.
Further, the modified heat-conducting filler is a silane coupling agent modified heat-conducting filler;
preferably, the heat conducting filler is at least one of simple metal, metal oxide, non-metal carbide and non-metal nitride; more preferably, the metal simple substance is at least one selected from aluminum powder, silver powder and copper powder; more preferably, the metal oxide is selected from at least one of alumina, magnesia, zinc oxide, and silica; more preferably, the non-metallic carbide is selected from at least one of silicon carbide and titanium carbide; more preferably, the non-metal nitride is selected from at least one of silicon nitride and boron nitride;
preferably, the heat conductive filler is regular spherical particles, flaky particles or irregular particles;
preferably, the particle size of the heat conductive filler is 0.4-30 μm;
preferably, the silane coupling agent is a long-chain alkyl silane coupling agent, more preferably, the silane coupling agent comprises octyl trimethoxy silane coupling agent, decyl trimethoxy silane coupling agent, dodecyl triethoxy silane coupling agent, hexadecyl trimethoxy silane coupling agent, hexadecyl triethoxy silane coupling agent;
preferably, the preparation method of the silane coupling agent modified heat-conducting filler comprises the following steps: adding a heat-conducting filler into ethanol, water or an ethanol/water solution of a silane coupling agent for surface treatment, stirring in the reaction process, and after complete reaction, washing with alcohol and drying in vacuum to obtain the silane coupling agent modified heat-conducting filler; more preferably, the reaction temperature is 40-80 ℃, the reaction time is 0.5-3h, and the mass of the silane coupling agent is 0.01-3% of that of the heat-conducting filler.
Further, the second phase liquid is selected from at least one of metal gallium, gallium-indium alloy, gallium-indium-tin alloy, indium-tin alloy and gallium-tin alloy;
preferably, the second phase liquid is a low-melting point elemental metal or alloy modified by a surface modifier; more preferably, the surface modifying agent comprises a titanate, an aluminate, cetyl mercaptan, stearyl mercaptan;
preferably, the preparation method of the surface modifier modified low-melting point elemental metal or alloy comprises the following steps: adding low-melting-point elemental metal or alloy into an organic solvent containing a surface modifier, and performing ultrasonic dispersion to obtain liquid metal particles coated by the surface modifier; more preferably, the organic solvent comprises ethanol, ethanol/water, toluene, tetrahydrofuran; the ultrasonic time is 0.1-2h, and the ultrasonic frequency is 25-130 KHZ; the mass of the surface modifier is 0.01-1% of the mass of the low-melting-point alloy.
Further, the additive also comprises a raw material component (G);
preferably, the additives include a thickener, a plasticizer, a surfactant, a flame retardant, and a colorant;
preferably, the additive comprises 0-1 part of thickening agent, 0-20 parts of plasticizer, 0-2 parts of surfactant, 0-1 part of flame retardant and 0-0.5 part of colorant, wherein the parts are parts by mass.
Further, the heat conductivity coefficient of the heat-conducting gel is 3.0-12W/mK, and the viscosity is 100-500 Pa.s; preferably, the thermal conductivity of the thermal conductive gel is 6-12W/mK, and the viscosity is 100-350 Pa.s.
In another aspect, the present invention provides a method for preparing any one of the above thermal conductive gels, including the following steps:
mixing organopolysiloxane containing at least 2 vinyl groups, polyorganosiloxane with at least 2 silicon-bonded hydrogen atoms, hydrosilylation reaction catalyst, hydrosilylation reaction inhibitor and modified heat-conducting filler at 25-100 ℃ under vacuum stirring for 0.5-2h, then adding second phase liquid, stirring again for 0.5-1h, and obtaining the heat-conducting gel;
or mixing organopolysiloxane containing at least 2 vinyl groups, polyorganosiloxane with at least 2 silicon-bonded hydrogen atoms, hydrosilylation reaction catalyst, hydrosilylation reaction inhibitor, modified heat-conducting filler and additive at 25-100 ℃ under vacuum stirring for 0.5-2h, then adding second phase liquid, stirring again for 0.5-1h, and obtaining the heat-conducting gel;
preferably, the stirring rate is 500-.
In another aspect, the present invention provides a heat conductive gel layer, wherein the heat conductive gel layer is obtained by curing the prepared heat conductive gel;
preferably, the curing temperature is 100-150 ℃, and the curing time is 0.5-1 h.
The invention has the beneficial effects that: according to the invention, a small amount of second-phase liquid is introduced into the system, and a heat-conducting liquid bridge is built among the heat-conducting fillers by utilizing capillary force, so that the interface thermal resistance among the fillers is reduced, and the high heat conductivity coefficient of the heat-conducting gel is realized. Meanwhile, the heat-conducting gel prepared by the invention has low viscosity and moderate thixotropy, is more suitable for being operated in a continuous dispensing mode, saves labor and improves the production efficiency; and the use amount of the filler can be reduced, so that the heat-conducting gel is endowed with better flexibility. The preparation method is simple and feasible, and is a novel heat-conducting gel with large-scale industrial production prospect.
Drawings
FIG. 1 is a flow chart of the preparation of the thermally conductive gel of the present invention.
Detailed Description
The preparation flow diagram of the heat-conducting gel is shown in figure 1, and a liquid bridge can be spontaneously formed between heat-conducting fillers in the mixing process due to the addition of a small amount of second-phase liquid, so that a heat-conducting path is formed between the fillers, and the interface thermal resistance between the fillers can be simultaneously reduced due to the high heat conductivity of low-melting-point alloy or simple substance metal, so that the heat-conducting gel has high heat conductivity coefficient.
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The preparation method of the silane coupling agent modified Al powder comprises the following steps: 1000g of Al powder with the particle size of 30 mu m is added into an ethanol/water solution (30 g of the dodecyl triethoxy silane coupling agent, 100g of the ethanol/water solution and the volume ratio of ethanol to water of 90: 10) of the dodecyl triethoxy silane coupling agent for surface treatment, the reaction temperature is 80 ℃, and the reaction time is 2 hours. And after the reaction is completed, washing with ethanol and drying in vacuum to obtain the silane coupling agent modified Al powder.
The preparation method of the surface modifier modified metal gallium comprises the following steps: mixing 0.01g of titanate with 10mL of ethanol to obtain an ethanol solution of the titanate, then adding 1.0g of metal gallium into the ethanol solution of the titanate, and performing ultrasonic dispersion (ultrasonic frequency is 25KHZ, ultrasonic time is 1.0h) to obtain the liquid metal gallium particles coated by the surface modifier.
Preparing a heat conducting gel: organopolysiloxane containing two vinyl groups (model: Andisil VS 100, Nantong Limited, 100 parts), polyorganosiloxane containing 2 silicon-bonded hydrogen atoms (model: Andisil XL-13, Nantong Limited, 10 parts), platinum dichloride (10 parts), 2-methyl-3-butyn-2-ol (0.5 part), silane coupling agent modified Al powder (particle size 30 μm, 1200 parts) were mixed for 2 hours at 100 ℃ under vacuum stirring (stirring speed: 2000rpm), then surface modifier modified metal gallium (0.001 part) was added and mixed for 0.5 hours again (stirring speed: 500rpm), and the thermally conductive gel was obtained. And curing the prepared heat-conducting gel for 1h at 100 ℃ to obtain the heat-conducting gel layer.
Example 2
The preparation method of the silane coupling agent modified Al powder comprises the following steps: 1000g of Al powder with the particle size of 15 mu m is added into an ethanol/water solution of a decyltrimethoxysilane coupling agent (30 g of the decyltrimethoxysilane coupling agent, 100g of the ethanol/water solution and the volume ratio of ethanol to water of 90: 10) for surface treatment, the reaction temperature is 80 ℃, and the reaction time is 2 hours. And after the reaction is completed, washing with ethanol and drying in vacuum to obtain the silane coupling agent modified Al powder.
The preparation method of the gallium-indium alloy modified by the surface modifier comprises the following steps: mixing 0.05g of titanate with 50mL of ethanol to obtain an ethanol solution of the titanate, then adding 5.0g of gallium-indium alloy into the ethanol solution of the titanate, and performing ultrasonic dispersion (ultrasonic frequency is 25KHZ, and ultrasonic time is 1.0h) to obtain the liquid gallium-indium alloy particles coated with the surface modifier.
Preparing heat-conducting gel: organopolysiloxane containing two vinyl groups (model: Andisil VS 10, Nantong Limited, 100 parts), polyorganosiloxane containing 2 silicon-bonded hydrogen atoms (model: Andisil XL-17, Nantong Limited, 90 parts), platinum tetrachloride (0.1 part), 3-methyl-1-butyn-3-ol (0.1 part), silane coupling agent modified Al powder (particle size 15 μm, 100 parts) are mixed for 0.5h under vacuum stirring (stirring speed: 2000rpm) at 100 ℃, then surface modifier modified gallium-indium alloy (50 parts) is added and mixed for 0.5h again (stirring speed: 250rpm), and the heat-conducting gel is obtained. And curing the prepared heat-conducting gel at 150 ℃ for 0.5h to obtain the heat-conducting gel layer.
Example 3
The preparation method of the silane coupling agent modified silver powder comprises the following steps: 1000g of silver powder with the particle size of 15 mu m is added into an ethanol/water solution (30 g of decyl trimethoxy silane coupling agent, 100g of ethanol/water solution and the volume ratio of ethanol to water of 90: 10) of decyl trimethoxy silane coupling agent for surface treatment, the reaction temperature is 80 ℃, and the reaction time is 2 h. And after the reaction is completed, washing with ethanol, and drying in vacuum to obtain the silane coupling agent modified silver powder.
The preparation method of the gallium indium tin alloy modified by the surface modifier comprises the following steps: mixing 0.025g of titanate with 25mL of ethanol to obtain an ethanol solution of the titanate, then adding 2.5g of gallium indium tin alloy into the ethanol solution of the titanate, and performing ultrasonic dispersion (ultrasonic frequency is 25KHZ, ultrasonic time is 1.0h) to obtain the liquid gallium indium tin alloy particles coated with the surface modifier.
Preparing a heat conducting gel: organopolysiloxane containing two vinyl groups (model: Andisil VS 10, Nantong Co., Ltd., 100 parts), polyorganosiloxane containing 2 silicon-bonded hydrogen atoms (model: Andisil XL-17, Nantong Co., Ltd., 90 parts), platinum tetrachloride (0.2 part), 2-phenyl-3-butyn-2-ol (0.3 part), silane coupling agent modified silver powder (particle size 15 μm, 800 parts) were mixed at 70 ℃ under vacuum stirring (stirring speed: 1000rpm) for 1.0h, then surface modifier modified gallium indium tin alloy (25 parts) was added and mixed again (stirring speed: 500rpm) for 1.0h, and the thermal conductive gel was obtained. And curing the prepared heat-conducting gel at 125 ℃ for 0.75h to obtain the heat-conducting gel layer.
Example 4
The preparation method of the silane coupling agent modified silver powder comprises the following steps: 1000g of silver powder with the particle size of 15 mu m is added into an ethanol/water solution (30 g of octyl trimethoxy silane coupling agent, 100g of ethanol/water solution and the volume ratio of ethanol to water of 90: 10) of octyl trimethoxy silane coupling agent for surface treatment, the reaction temperature is 80 ℃, and the reaction time is 2 h. And after the reaction is completed, washing with ethanol, and drying in vacuum to obtain the silane coupling agent modified silver powder.
The preparation method of the gallium indium tin alloy modified by the surface modifier comprises the following steps: mixing 0.025g of titanate with 25mL of ethanol to obtain an ethanol solution of the titanate, then adding 2.5g of gallium indium tin alloy into the ethanol solution of the titanate, and performing ultrasonic dispersion (ultrasonic frequency is 25KHZ, ultrasonic time is 1.0h) to obtain the liquid gallium indium tin alloy particles coated with the surface modifier.
Preparing heat-conducting gel: organopolysiloxane containing two vinyl groups (model: Andisil VS 10, Nantong Limited, 100 parts), polyorganosiloxane containing 2 silicon-bonded hydrogen atoms (model: Andisil XL-17, Nantong Limited, 20 parts), platinum tetrachloride (0.2 part), 2-phenyl-3-butyn-2-ol (0.3 part), silane coupling agent modified silver powder (particle size 15 μm, 1000 parts) are mixed for 1.0h under vacuum stirring (stirring speed: 1000rpm) at 70 ℃, then gallium indium tin alloy modified by surface modifier (25 parts) is added and mixed for 1.0h again (stirring speed: 500rpm), and the heat-conducting gel is obtained. And curing the prepared heat-conducting gel at 150 ℃ for 1.0h to obtain the heat-conducting gel layer.
Example 5
The preparation method of the silane coupling agent modified Al powder comprises the following steps: 1000g of Al powder with the particle size of 30 mu m is added into an ethanol/water solution of an octyltrimethoxysilane coupling agent (30 g of the octyltrimethoxysilane coupling agent, 100g of the ethanol/water solution and the volume ratio of ethanol to water of 90: 10) for surface treatment, the reaction temperature is 80 ℃, and the reaction time is 2 h. And after the reaction is completed, washing with ethanol and drying in vacuum to obtain the silane coupling agent modified Al powder.
The preparation method of the surface modifier modified metal gallium comprises the following steps: 0.05g of titanate is mixed with 50mL of ethanol to obtain an ethanol solution of the titanate, and then 5.0g of metal gallium is added into the ethanol solution of the titanate to carry out ultrasonic dispersion (ultrasonic frequency is 25KHZ, ultrasonic time is 1.0h) to obtain the liquid metal gallium particles coated by the surface modifier.
Preparing a heat conducting gel: organopolysiloxane containing two vinyl groups (model: Andisil VS 100, Nantong Limited, 100 parts), polyorganosiloxane containing 2 silicon-bonded hydrogen atoms (model: Andisil XL-13, Nantong Limited, 10 parts), platinum dichloride (10 parts), 2-methyl-3-butyn-2-ol (0.5 part), silane coupling agent modified Al powder (particle size 30 μm, 800 parts) were mixed at 100 ℃ under vacuum stirring (stirring speed: 2000rpm) for 2h, then surface modifier modified metal gallium (50 parts) was added and mixed again (stirring speed: 500rpm) for 0.5h, and the thermally conductive gel was obtained. And curing the prepared heat-conducting gel for 1h at 100 ℃ to obtain the heat-conducting gel layer.
Comparative example 1
The preparation method of the silane coupling agent modified Al powder comprises the following steps: 1000g of Al powder with the particle size of 30 mu m is added into an ethanol/water solution of an octyltrimethoxysilane coupling agent (30 g of the octyltrimethoxysilane coupling agent, 100g of the ethanol/water solution and the volume ratio of ethanol to water of 90: 10) for surface treatment, the reaction temperature is 80 ℃, and the reaction time is 2 h. And after the reaction is completed, washing with ethanol and drying in vacuum to obtain the silane coupling agent modified Al powder.
The composition was the same as in example 1 except that the second phase liquid was not present. Organopolysiloxane containing two vinyl groups (model: Andisil VS 100, Nantong Co., Ltd., 100 parts), polyorganosiloxane containing 2 silicon-bonded hydrogen atoms (model: Andisil XL-13, Nantong Co., Ltd., 10 parts), platinum dichloride (10 parts), 2-methyl-3-butyn-2-ol (0.5 part), silane coupling agent modified Al powder (particle size 30 μm, 1200 parts) were mixed for 2 hours under vacuum stirring at 100 ℃ (stirring speed: 2000rpm), and a heat conductive gel was obtained.
Comparative example 2
The components were the same as in the examples except that there was no thermally conductive filler and no second phase liquid.
A heat-conductive gel was obtained by mixing an organopolysiloxane containing two vinyl groups (model: Andisil VS 100, Nantong Limited, 100 parts), a polyorganosiloxane containing 2 silicon-bonded hydrogen atoms (model: Andisil XL-13, Nantong Limited, 10 parts), platinum dichloride (10 parts), and 2-methyl-3-butyn-2-ol (0.5 part) at 100 ℃ for 2 hours under vacuum stirring (stirring speed: 2000 rpm).
(1) And (3) testing the heat conductivity coefficient:
the heat conductivity coefficient in the vertical direction is measured by adopting a standard test method ASTM D5470 steady state method, a tester is an LW-9389TIM thermal resistance and thermal conductivity measuring instrument, and the method comprises the following specific steps: placing a thermal interface material between the instrument bars, and establishing stable heat flow through the assembly; then monitoring the temperature in the strip at two or more points along its length; the temperature difference across the interface is calculated from the temperature readings obtained and used to determine the thermal conductivity of the interface.
(2) And (3) viscosity testing:
the viscosity value of the heat-conducting gel is tested by adopting a rheometer, and the specific steps are as follows: a small amount of gel was applied between parallel rotors 25mm in diameter, maintaining the spacing between the upper and lower parallel plates at 0.6mm, the shear rate sweep ranged from 0.5s-1 to 5.0s-1, and the test temperature was kept constant at room temperature, whereby the viscosity values were recorded as a function of shear rate.
The thermal conductivity and viscosity of the thermal conductive gels provided in examples 1 to 5 and comparative examples 1 to 2 were tested according to the above methods, and the test results are shown in table 1:
TABLE 1
The above description is only a specific embodiment of the present invention, and not all embodiments, and any equivalent modifications of the technical solutions of the present invention, which are made by those skilled in the art through reading the present specification, are covered by the claims of the present invention.
Claims (10)
1. The heat-conducting gel is characterized by being prepared from the following raw materials in parts by mass:
(A) 100 parts of organopolysiloxane containing at least 2 vinyl groups;
(B) 10-90 parts of polyorganosiloxane having at least 2 silicon-bonded hydrogen atoms;
(C) 0.1-10 parts of a hydrosilylation catalyst;
(D) 0.1-0.5 part of hydrosilylation inhibitor;
(E) 100 portions and 1200 portions of modified heat-conducting filler;
(F) 0.001-50 parts of second-phase liquid;
the second phase liquid is low-melting point elemental metal or alloy with the melting point between 10 and 60 ℃.
2. The thermally conductive gel of claim 1, wherein said organopolysiloxane having at least 2 vinyl groups has the following structural formula:
preferably, the organopolysiloxane having at least 2 vinyl groups has a viscosity of 20 to 1000mpa.s at 25 ℃.
3. The thermally conductive gel of claim 1, wherein said polyorganosiloxane having at least 2 silicon-bonded hydrogen atoms has the formula:
preferably, the polyorganosiloxane having at least 2 silicon-bonded hydrogen atoms has a viscosity of 20 to 100mPa.s at 25 ℃.
4. The thermally conductive gel of claim 1, wherein the hydrosilylation reaction catalyst is a hydrosilylation reaction catalyst capable of initiating a hydrosilylation reaction of components (a) and (B);
preferably, the hydrosilylation reaction catalyst is at least one selected from the group consisting of platinum black, rhodium, ruthenium, palladium, platinum metal compounds and organic complexes thereof, rhodium metal compounds and organic complexes thereof, ruthenium metal compounds and organic complexes thereof, palladium metal compounds and organic complexes thereof;
still preferably, the hydrosilylation reaction catalyst is at least one selected from the group consisting of platinum black, a platinum metal compound, and an organic complex thereof;
more preferably, the platinum metal compound comprises platinum dichloride, platinum tetrachloride, chloroplatinic acid; the platinum metal compound organic compound comprises a compound of chloroplatinic acid, olefin and vinyl siloxane.
5. The thermally conductive gel of claim 1, wherein the hydrosilylation reaction inhibitor is a hydrosilylation reaction inhibitor capable of inhibiting the hydrosilylation reaction of components (a) and (B);
preferably, the hydrosilylation reaction inhibitor is selected from at least one of alkynol, enyne compound, amine and maleate;
preferably, the alkynol comprises at least one of 2-methyl-3-butyn-2-ol, 3-methyl-1-butyn-3-ol, 2-phenyl-3-butyn-2-ol, 1-dimethyl-2-propynyloxytrimethylsilane.
6. The thermally conductive gel of claim 1, wherein the modified thermally conductive filler is a silane coupling agent modified thermally conductive filler;
preferably, the heat conducting filler is at least one of simple metal, metal oxide, non-metal carbide and non-metal nitride; more preferably, the metal simple substance is at least one selected from aluminum powder, silver powder and copper powder; more preferably, the metal oxide is selected from at least one of alumina, magnesia, zinc oxide, and silica; more preferably, the non-metallic carbide is selected from at least one of silicon carbide and titanium carbide; more preferably, the non-metal nitride is selected from at least one of silicon nitride and boron nitride;
preferably, the heat conductive filler is regular spherical particles, flaky particles or irregular particles;
preferably, the particle size of the heat conductive filler is 0.4-30 μm;
preferably, the silane coupling agent is a long-chain alkyl silane coupling agent, more preferably, the silane coupling agent comprises octyl trimethoxy silane coupling agent, decyl trimethoxy silane coupling agent, dodecyl triethoxy silane coupling agent, hexadecyl trimethoxy silane coupling agent, hexadecyl triethoxy silane coupling agent;
preferably, the preparation method of the silane coupling agent modified heat-conducting filler comprises the following steps: adding a heat-conducting filler into ethanol, water or an ethanol/water solution of a silane coupling agent for surface treatment, stirring in the reaction process, and after complete reaction, washing with alcohol and drying in vacuum to obtain the silane coupling agent modified heat-conducting filler; more preferably, the reaction temperature is 40-80 ℃, the reaction time is 0.5-3h, and the mass of the silane coupling agent is 0.01-3% of that of the heat-conducting filler.
7. The thermally conductive gel of claim 1, wherein said second phase liquid is selected from at least one of metallic gallium, gallium indium alloy, gallium indium tin alloy, gallium tin alloy;
preferably, the second phase liquid is a low-melting point elemental metal or alloy modified by a surface modifier; more preferably, the surface modifying agent comprises a titanate, an aluminate, cetyl mercaptan, stearyl mercaptan;
preferably, the preparation method of the surface modifier modified low-melting point elemental metal or alloy comprises the following steps: adding low-melting-point elemental metal or alloy into an organic solvent containing a surface modifier, and performing ultrasonic dispersion to obtain liquid metal particles coated with the surface modifier; more preferably, the organic solvent comprises ethanol, ethanol/water, toluene, tetrahydrofuran; the ultrasonic time is 0.1-2h, and the ultrasonic frequency is 25-130 KHZ; the mass of the surface modifier is 0.01-1% of the mass of the low-melting-point alloy.
8. The thermally conductive gel of claim 1, further comprising a raw material component (G) additive;
preferably, the additives include a thickener, a plasticizer, a surfactant, a flame retardant, and a colorant;
preferably, the additive comprises 0-1 part of thickening agent, 0-20 parts of plasticizer, 0-2 parts of surfactant, 0-1 part of flame retardant and 0-0.5 part of colorant, wherein the parts are parts by mass.
9. The method of preparing a thermally conductive gel of any one of claims 1-8, comprising the steps of:
mixing organopolysiloxane containing at least one vinyl group, polyorganosiloxane with at least 2 silicon-bonded hydrogen atoms, hydrosilylation reaction catalyst, hydrosilylation reaction inhibitor and modified heat-conducting filler at 25-100 ℃ for 0.5-2h under vacuum stirring, then adding second phase liquid, stirring again for 0.5-1h, and obtaining the heat-conducting gel;
or mixing organopolysiloxane containing at least one vinyl group, polyorganosiloxane with at least 2 silicon-bonded hydrogen atoms, hydrosilylation reaction catalyst, hydrosilylation reaction inhibitor, modified heat-conducting filler and additive at 25-100 ℃ under vacuum stirring for 0.5-2h, then adding second phase liquid, stirring again for 0.5-1h, and obtaining the heat-conducting gel;
preferably, the stirring rate is 500-.
10. A thermally conductive gel layer, characterized in that the thermally conductive gel prepared in claim 9 is cured to obtain a thermally conductive gel layer;
preferably, the curing temperature is 100-150 ℃, and the curing time is 0.5-1 h.
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