CN112852165A - Single-component addition type high-temperature-resistant high-heat-conductivity silicone gel and preparation method thereof - Google Patents
Single-component addition type high-temperature-resistant high-heat-conductivity silicone gel and preparation method thereof Download PDFInfo
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- 229920001296 polysiloxane Polymers 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title abstract description 10
- 238000001879 gelation Methods 0.000 title description 2
- 239000001257 hydrogen Substances 0.000 claims abstract description 61
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 61
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229920002545 silicone oil Polymers 0.000 claims abstract description 54
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 38
- -1 polysiloxane Polymers 0.000 claims abstract description 36
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 31
- 239000003054 catalyst Substances 0.000 claims abstract description 27
- 239000000049 pigment Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 25
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 13
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 239000002245 particle Substances 0.000 claims description 59
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 22
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 22
- 238000003756 stirring Methods 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 12
- 238000011049 filling Methods 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229910017052 cobalt Inorganic materials 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical group [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 claims description 4
- 239000006229 carbon black Substances 0.000 claims description 3
- 239000011231 conductive filler Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 150000001335 aliphatic alkanes Chemical class 0.000 claims description 2
- CJOBVZJTOIVNNF-UHFFFAOYSA-N cadmium sulfide Chemical compound [Cd]=S CJOBVZJTOIVNNF-UHFFFAOYSA-N 0.000 claims description 2
- 239000003575 carbonaceous material Substances 0.000 claims description 2
- 239000013522 chelant Substances 0.000 claims description 2
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 claims description 2
- 230000007774 longterm Effects 0.000 abstract description 5
- 230000032683 aging Effects 0.000 abstract description 3
- 239000004519 grease Substances 0.000 abstract description 2
- 239000000499 gel Substances 0.000 description 37
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 12
- 239000011787 zinc oxide Substances 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000011256 inorganic filler Substances 0.000 description 5
- 229910003475 inorganic filler Inorganic materials 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 239000002131 composite material Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 3
- 230000017525 heat dissipation Effects 0.000 description 3
- 239000003921 oil Substances 0.000 description 3
- 239000000741 silica gel Substances 0.000 description 3
- 229910002027 silica gel Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910052581 Si3N4 Inorganic materials 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 2
- 229910052582 BN Inorganic materials 0.000 description 1
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000009795 derivation Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004100 electronic packaging Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000003112 inhibitor Substances 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000012782 phase change material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
-
- 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
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
- C08K2201/005—Additives being defined by their particle size in general
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
-
- 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
-
- 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
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention provides a single-component addition type high-temperature-resistant high-heat-conductivity silicone gel and a preparation method thereof; the single-component addition type high-temperature-resistant high-heat-conductivity silicone gel comprises the following raw materials in parts by weight: 80-100 parts of vinyl silicone oil, 0.1-5 parts of cross-linking agent hydrogen-containing silicone oil, 500-2000 parts of heat-conducting filler, 1-20 parts of treating agent, 1-4 parts of catalyst and 1-8 parts of pigment, wherein the hydrogen-containing silicone oil comprises at least one of terminal hydrogen-containing polysiloxane and side hydrogen-containing polysiloxane; the hydrogen content of the terminal hydrogenpolysiloxane is 0.16-3.00mmoles/g, and the hydrogen content of the lateral hydrogenpolysiloxane is 0.9-9 mmoles/g. Compared with the currently used silicone grease and silicone gasket, the single-component addition type high-temperature-resistant high-heat-conductivity silicone gel provided by the invention has the advantages of higher heat conductivity coefficient, higher bearing temperature, almost unchanged long-time aging thermal resistance and the like, thereby ensuring that the heat-conducting interface material always keeps high heat-conducting efficiency in the long-term use process.
Description
Technical Field
The invention relates to the technical field of heat-conducting interface materials, in particular to a single-component addition type high-temperature-resistant high-heat-conductivity silicone gel and a preparation method thereof.
Background
Along with the development of rapid manufacturing technology and the popularization of 5G technology, the electronic components, circuit modules, integrated circuits and other fields develop towards three major trends of high performance, miniaturization and integration, the electronic heat dissipation problem is more and more prominent, because the untimely derivation of heat can reduce the service life and the reliability of electronic devices, and the safety performance of equipment can be influenced. Effective thermal management is therefore critical to ensure its high performance and reliability. However, thermal management of many electronic devices still relies on basic passive cooling systems: internal heat sink and external natural convection. Relying on passive cooling techniques for high power, high density electronic devices cannot guarantee the internal temperature required for their proper operation.
Thermal Interface Materials (TIM) is a material commonly used for IC packaging and electronic heat dissipation, and is mainly used for filling up micro-gaps and holes with uneven surfaces generated when two Materials are jointed or contacted, reducing heat transfer contact resistance and improving heat dissipation performance of devices. The air thermal conductivity is 0.024W/mK, a poor conductor of heat, and heat conduction is seriously hindered. The high thermal conductivity TIM fills the gap, removes air, establishes an effective heat transmission channel, greatly reduces thermal resistance, and fully plays a role of a radiator. Therefore, thermally conductive interface materials are essential in electronic packaging. The heat conducting interface material mainly comprises heat conducting grease, heat conducting gel, a heat conducting gasket and a phase change material. The heat-conducting gel is widely applied to heat-conducting interface materials by virtue of the characteristics of high heat conductivity coefficient, strong material cohesion, shape restorability, difficult oil bleeding, long-term storage stability and the like. At present, the traditional heat-conducting silica gel has the problems of poor heat-conducting property, no high temperature resistance, rise in heat resistance of the heat-conducting silica gel after a long time, harsh storage conditions and the like, so that research on the traditional heat-conducting silica gel is needed.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a single-component addition type high-temperature-resistant high-heat-conductivity silicone gel and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
on one hand, the invention provides a single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following raw materials in parts by weight: 80-100 parts of vinyl silicone oil, 0.1-5 parts of cross-linking agent hydrogen-containing silicone oil, 2000 parts of heat-conducting filler, 1-20 parts of treating agent, 1-4 parts of catalyst and 1-8 parts of pigment.
Further, the vinyl silicone oil comprises one or more of vinyl-terminated polydimethylsiloxane, polymethylphenyl-methylvinylsiloxane and methyl-terminated polysiloxane with vinyl-containing side chains; the vinyl silicone oil has a vinyl content of 0.015 to 3.00mmoles/g and a viscosity at 25 ℃ in the range of 6 to 10000 cSt.
Further preferably, the vinyl silicone oil has a viscosity at 25 ℃ in the range of 30 to 1000 cSt.
Further, the cross-linking agent hydrogen-containing silicone oil is at least one of terminal hydrogen-containing silicone oil and side hydrogen-containing silicone oil, and the viscosity is 40-100 cSt.
Further, the cross-linking agent hydrogen-containing silicone oil comprises at least one of terminal hydrogen-containing polysiloxane and side hydrogen-containing polysiloxane; wherein the hydrogen content of the terminal hydrogenpolysiloxane is 0.16-3.00mmoles/g, and the hydrogen content of the lateral hydrogenpolysiloxane is 0.9-9 mmoles/g.
Further, the cross-linking agent hydrogen-containing silicone oil comprises end hydrogen-containing polysiloxane and side hydrogen-containing polysiloxane, and the mass ratio of the end hydrogen-containing polysiloxane to the side hydrogen-containing polysiloxane is 1: 1.
Further, the thermally conductive filler includes at least one of a metal filler, a carbon material, and inorganic thermally conductive particles.
Further preferably, the metal filler includes at least one of gold particles, silver particles, copper particles, aluminum particles, iron particles, zinc particles, nickel particles, and liquid alloy.
Further preferably, the carbon filler includes at least one of diamond, graphite, carbon black, carbon fiber, carbon nanotube, graphene, and graphdine.
Further preferably, the inorganic heat conductive particles include at least two of aluminum oxide, aluminum nitride, silicon nitride, boron nitride, silicon nitride, aluminum hydroxide, silicon carbide, magnesium oxide, zinc oxide, and silicon dioxide.
Further, the heat-conducting filler is spherical or spheroidal heat-conducting particles with the particle size of 0.3-150 microns, wherein the spherical or spheroidal heat-conducting particles with the particle size of 0.3-5 microns account for 1-30% of the total amount, the spherical or spheroidal heat-conducting particles with the particle size of 10-30 microns account for 10-30% of the total amount, and the spherical or spheroidal heat-conducting particles with the particle size of 70-150 microns account for 20-50% of the total amount.
Further, the above-mentioned treating agent comprises long-chain alkane trimethoxy siloxane, vinyl trimethoxy siloxane, titanate or a novel treating agent; the novel treating agent has a molecular formula of CnH2n+1(SiMe2O)mSi(OR)3。
Further, the catalyst includes any one of platinum-vinylsiloxane, platinum-alkyne chelate, and chloroplatinic acid.
Further, the pigment is cobalt blue, iron red, carbon black or cadmium yellow.
In a second aspect, the invention provides a method for preparing the above single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following steps:
step one, weighing vinyl silicone oil, hydrogen-containing silicone oil, heat-conducting filler and treating agent according to a ratio, adding into a planetary mixer, stirring for 1-3 hours at room temperature, and uniformly mixing for later use;
weighing a proper amount of catalyst and pigment, adding the catalyst and the pigment into a planetary mixer, vacuumizing at 55-65 ℃ and under the pressure of-0.1 MPa, and stirring at 30rpm for 1-2 hours.
And step three, subpackaging, namely filling the mixed single-component gel into a single-component tube of 30 CC.
By adopting the technical scheme, compared with the prior art, the invention has the following technical effects:
according to the invention, the medium-low viscosity vinyl silicone oil, the hydrogen-containing silicone oil, the heat-conducting filler, the treating agent, the catalyst and the pigment are blended, and spherical alumina, aluminum nitride and zinc oxide with different particle sizes are optimally compounded, so that the system is compactly stacked, a heat-conducting passage is optimized, and the heat-conducting property of the heat-conducting gel is improved; in addition, after the powder is optimally stacked, the addition amount of the heat-conducting filler can be reduced, so that the viscosity of the heat-conducting gel component is reduced, and the body strength and toughness of the heat-conducting gel are also obviously improved; the mass part ratio of terminal hydrogen and side hydrogen in the cross-linking agent hydrogen-containing silicone oil is optimized, so that the extrusion performance of the heat-conducting gel can be improved, and the cohesion of the heat-conducting gel can be improved; finally, compared with the filler modified by the common treating agent, the heat-conducting filler modified by the novel treating agent has lower viscosity and lower oil absorption value, so that the powder is easier to fill and disperse, and the heat-conducting gel is difficult to separate oil in the long-term storage process and is difficult to crack in the high-temperature aging process. In addition, the gel is free of an inhibitor, so that the gel is crosslinked during mixing, thereby enabling long-term storage at room temperature. In conclusion, compared with the existing products in the market, the product of the invention has better extrusion performance, higher heat conductivity coefficient, better cohesion, higher bearing temperature and more excellent storage condition.
Detailed Description
The invention provides a single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel and a preparation method thereof, aiming at the problems of poor thermal conductivity, low high temperature resistance, high thermal resistance rise of the thermal-conductivity gel after a long time and the like of the traditional thermal-conductivity silicone gel. Specifically, the single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel comprises the following raw materials in parts by weight: 80-100 parts of vinyl silicone oil, 0.1-5 parts of cross-linking agent hydrogen-containing silicone oil, 2000 parts of heat-conducting filler, 1-20 parts of treating agent, 1-4 parts of catalyst and 1-8 parts of pigment.
The present invention will be described in detail and specifically with reference to the following examples to facilitate better understanding of the present invention, but the following examples do not limit the scope of the present invention.
In the examples, the conventional methods were used unless otherwise specified, and reagents used were those conventionally commercially available or formulated according to the conventional methods without specifically specified.
Example 1
The embodiment provides a single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following components in parts by weight: 80 parts of vinyl silicone oil, 2 parts of cross-linking agent hydrogen-containing silicone oil, 1900 parts of high-thermal-conductivity filler, 12 parts of treating agent, 4 parts of catalyst and 4 parts of pigment.
Wherein the vinyl silicone oil is vinyl-terminated polydimethylsiloxane, the vinyl content is 0.22mmoles/g, and the viscosity is 250 cSt;
according to the total mass of the silicone gel, the hydrogen-containing silicone oil comprises 1 part of hydrogen-terminated polydimethylsiloxane and 1 part of lateral hydrogen-containing polydimethylsiloxane; the Si-H content in the hydrogen-terminated polydimethylsiloxane is 1.37mmoles/g, the viscosity is 14cSt, the Si-H content in the lateral hydrogen-containing polydimethylsiloxane is 3mmoles/g, and the viscosity is 50 cSt;
the high heat conduction filler comprises aluminum oxide and zinc oxide and is spherical or sphere-like heat conduction particles with the particle size of 0.5-90 microns, wherein the spherical or sphere-like heat conduction particles with the particle size of 70-90 microns account for 50% of the total amount, the spherical or sphere-like heat conduction particles with the particle size of 10-30 microns account for 20% of the total amount, and the spherical or sphere-like heat conduction particles with the particle size of 0.5-5 microns account for 30% of the total amount;
the treating agent is a novel treating agent; the catalyst is platinum-vinyl siloxane; the pigment is cobalt blue.
The embodiment also provides a preparation method of the single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following steps:
step one, weighing vinyl silicone oil, hydrogen-containing silicone oil, heat-conducting filler and treating agent according to a ratio, adding into a planetary mixer, stirring for 2 hours at room temperature, and uniformly mixing for later use;
weighing a proper amount of catalyst and pigment, adding the catalyst and the pigment into a planetary mixer, vacuumizing the planetary mixer at the temperature of 60 ℃ and the pressure of-0.1 MPa, and stirring the mixture for 1 hour at the speed of 30 rpm.
And step three, subpackaging, namely filling the mixed single-component gel into a single-component tube of 30 CC.
Example 2
The embodiment provides a single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following components in parts by weight: 80 parts of vinyl silicone oil, 3 parts of cross-linking agent hydrogen-containing silicone oil, 1900 parts of heat-conducting filler, 12 parts of treating agent, 4 parts of catalyst and 4 parts of pigment.
Wherein the vinyl silicone oil is vinyl-terminated polydimethylsiloxane, the vinyl content is 0.22mmoles/g, and the viscosity is 250 cSt;
according to the total mass of the silicon gel, the hydrogen-containing silicone oil comprises 1.5 parts of hydrogen-containing terminated polydimethylsiloxane and 1.5 parts of lateral hydrogen-containing polydimethylsiloxane, wherein the Si-H content in the hydrogen-containing terminated polydimethylsiloxane is 1.37mmoles/g, the viscosity is 14cSt, the Si-H content in the lateral hydrogen-containing polydimethylsiloxane is 3mmoles/g, and the viscosity is 50 cSt;
the high heat conduction filler comprises aluminum oxide and zinc oxide; the high heat conduction compound inorganic filler is spherical or sphere-like heat conduction particles with the particle size of 0.5-90 microns, wherein the spherical or sphere-like heat conduction particles with the particle size of 70-90 microns account for 50% of the total amount, the spherical or sphere-like heat conduction particles with the particle size of 10-30 microns account for 20% of the total amount, and the spherical or sphere-like heat conduction particles with the particle size of 0.5-5 microns account for 30% of the total amount;
the powder treating agent is a novel treating agent; the catalyst is platinum-vinyl siloxane; the pigment is cobalt blue.
The embodiment also provides a preparation method of the single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following steps:
step one, weighing vinyl silicone oil, hydrogen-containing silicone oil, heat-conducting filler and treating agent according to a ratio, adding into a planetary mixer, stirring for 2 hours at room temperature, and uniformly mixing for later use;
weighing a proper amount of catalyst and pigment, adding the catalyst and the pigment into a planetary mixer, vacuumizing the planetary mixer at the temperature of 60 ℃ and the pressure of-0.1 MPa, and stirring the mixture for 1 hour at the speed of 30 rpm.
And step three, subpackaging, namely filling the mixed single-component gel into a single-component tube of 30 CC.
Example 3
The embodiment provides a single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following components in parts by weight: 80 parts of vinyl silicone oil, 2 parts of cross-linking agent hydrogen-containing silicone oil, 1900 parts of heat-conducting filler and 12 parts of treating agent; 4 parts of catalyst and 4 parts of pigment.
Wherein the vinyl silicone oil is vinyl-terminated polydimethylsiloxane, the vinyl content is 0.19mmoles/g, and the viscosity is 400 cSt;
according to the total mass of the silicone gel, the hydrogen-containing silicone oil comprises 2 parts of hydrogen polydimethylsiloxane and 2 parts of lateral hydrogen-containing polydimethylsiloxane, the Si-H content in the terminal hydrogen-containing polydimethylsiloxane is 1.37mmoles/g, the viscosity is 14cSt, the Si-H content in the lateral hydrogen-containing polydimethylsiloxane is 3mmoles/g, and the viscosity is 50 cSt;
the high-thermal-conductivity composite inorganic filler comprises aluminum oxide and zinc oxide, and the high-thermal-conductivity composite inorganic filler is spherical or spheroidal thermal-conductivity particles with the particle size of 0.5-90 micrometers, wherein the spherical or spheroidal thermal-conductivity particles with the particle size of 70-90 micrometers account for 50% of the total amount, the spherical or spheroidal thermal-conductivity particles with the particle size of 10-30 micrometers account for 20% of the total amount, and the spherical or spheroidal thermal-conductivity particles with the particle size of 0.5-5 micrometers account for 30% of the total amount;
the powder treating agent is a novel treating agent; the catalyst is platinum-vinyl siloxane; the pigment is cobalt blue.
The embodiment also provides a preparation method of the single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following steps:
step one, weighing vinyl silicone oil, hydrogen-containing silicone oil, heat-conducting filler and treating agent according to a ratio, adding into a planetary mixer, stirring for 2 hours at room temperature, and uniformly mixing for later use;
weighing a proper amount of catalyst and pigment, adding the catalyst and the pigment into a planetary mixer, vacuumizing the planetary mixer at the temperature of 60 ℃ and the pressure of-0.1 MPa, and stirring the mixture for 1 hour at the speed of 30 rpm.
And step three, subpackaging, namely filling the mixed single-component gel into a single-component tube of 30 CC.
Example 4
The embodiment provides a single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following components in parts by weight: 80 parts of vinyl silicone oil, 2 parts of cross-linking agent hydrogen-containing silicone oil, 2000 parts of heat-conducting filler, 12 parts of treating agent, 4 parts of catalyst and 4 parts of pigment.
Wherein the vinyl silicone oil is vinyl-terminated polydimethylsiloxane, the vinyl content is 0.19mmoles/g, and the viscosity is 400 cSt;
according to the total mass of the silicone gel, the hydrogen-containing silicone oil comprises 2.5 parts of hydrogen-containing polydimethylsiloxane and 2.5 parts of lateral hydrogen-containing polydimethylsiloxane; the Si-H content in the hydrogen-terminated polydimethylsiloxane is 1.37mmoles/g, the viscosity is 14cSt, the Si-H content in the lateral hydrogen-containing polydimethylsiloxane is 3mmoles/g, and the viscosity is 50 cSt;
the high-thermal-conductivity composite inorganic filler comprises aluminum oxide and zinc oxide, and the high-thermal-conductivity composite inorganic filler is spherical or spheroidal thermal-conductivity particles with the particle size of 0.5-90 micrometers, wherein the spherical or spheroidal thermal-conductivity particles with the particle size of 90-120 micrometers account for 50% of the total amount, the spherical or spheroidal thermal-conductivity particles with the particle size of 10-30 micrometers account for 20% of the total amount, and the spherical or spheroidal thermal-conductivity particles with the particle size of 0.5-5 micrometers account for 30% of the total amount;
the powder treating agent is a novel treating agent; the catalyst is platinum-vinyl siloxane; the pigment is cobalt blue.
The embodiment also provides a preparation method of the single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel, which comprises the following steps:
step one, weighing vinyl silicone oil, hydrogen-containing silicone oil, heat-conducting filler and treating agent according to a ratio, adding into a planetary mixer, stirring for 2 hours at room temperature, and uniformly mixing for later use;
weighing a proper amount of catalyst and pigment, adding the catalyst and the pigment into a planetary mixer, vacuumizing the planetary mixer at the temperature of 60 ℃ and the pressure of-0.1 MPa, and stirring the mixture for 1 hour at the speed of 30 rpm.
And step three, subpackaging, namely filling the mixed single-component gel into a single-component tube of 30 CC.
Verification examples
In this example, partial performance tests were performed on the thermally conductive gels provided in examples 1 to 4, and corresponding performance tests were performed on the similar products existing in the market as comparative examples, and the test results are shown in the following table:
from the above table, compared with the existing like products in the market, the product provided by the embodiment of the invention has the advantages of better extrusion performance, higher heat conductivity coefficient, higher bearing temperature, almost unchanged long-time aging thermal resistance and the like, and further ensures that the heat-conducting interface material always keeps high heat-conducting efficiency in the long-term use process.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.
Claims (10)
1. The single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel is characterized by comprising the following raw materials in parts by weight: 80-100 parts of vinyl silicone oil, 0.1-5 parts of cross-linking agent hydrogen-containing silicone oil, 2000 parts of heat-conducting filler, 1-20 parts of treating agent, 1-4 parts of catalyst and 1-8 parts of pigment.
2. The single-component addition type high-temperature-resistant high-thermal-conductivity silicone gel according to claim 1, wherein the vinyl silicone oil comprises one or more of vinyl-terminated polydimethylsiloxane, polymethylphenyl-methylvinylsiloxane and methyl-terminated polysiloxane containing vinyl in a side chain; the vinyl silicone oil has a vinyl content of 0.015 to 3.00mmoles/g and a viscosity at 25 ℃ in the range of 6 to 10000 cSt.
3. The one-component addition type high temperature resistant high thermal conductive silicone gel according to claim 1, wherein the cross-linking agent hydrogen-containing silicone oil is at least one of terminal hydrogen-containing silicone oil and side hydrogen-containing silicone oil, and has a viscosity of 40-100 cSt.
4. The one-component addition-type high temperature-resistant high thermal conductive silicone gel according to claim 3, wherein the cross-linking agent hydrogen-containing silicone oil comprises at least one of terminal hydrogen-containing polysiloxane and side hydrogen-containing polysiloxane; wherein the hydrogen content of the terminal hydrogenpolysiloxane is 0.16-3.00mmoles/g, and the hydrogen content of the terminal hydrogenpolysiloxane is 0.9-9 mmoles/g.
5. The one-component addition-type high temperature-resistant high thermal-conductive silicone gel according to claim 1, wherein the thermal-conductive filler comprises at least one of a metal filler, a carbon material, and inorganic thermal-conductive particles.
6. The single-component addition-type high temperature-resistant high thermal-conductive silicone gel according to claim 1, wherein the thermal-conductive filler is spherical or spheroidal thermal-conductive particles having a particle size of 0.3 to 150 μm, wherein the spherical or spheroidal thermal-conductive particles having a particle size of 0.3 to 5 μm account for 1 to 30% of the total amount, the spherical or spheroidal thermal-conductive particles having a particle size of 10 to 30 μm account for 10 to 30% of the total amount, and the spherical or spheroidal thermal-conductive particles having a particle size of 70 to 150 μm account for 20 to 50% of the total amount.
7. The one-component addition-type high temperature resistant high thermal conductive silicone gel according to claim 1, wherein the treatment agent comprises long chain alkane trimethoxy siloxane, vinyl trimethoxy siloxane, titanate, or a novel treatment agent; the molecular formula of the novel treating agent is CnH2n+1(SiMe2O)mSi(OR)3。
8. The one-component addition-type high temperature-resistant high thermal conductive silicone gel according to claim 1, wherein the catalyst comprises any one of platinum-vinylsiloxane, platinum-alkyne chelate, and chloroplatinic acid.
9. The one-component addition-type high temperature resistant high thermal conductive silicone gel according to claim 1, wherein the pigment is cobalt blue, iron red, carbon black or cadmium yellow.
10. A method for preparing the one-component addition type high temperature resistant high thermal conductive silicone gel according to any one of claims 1 to 9, comprising the steps of:
step one, weighing the vinyl silicone oil, the hydrogen-containing silicone oil, the heat-conducting filler and the treating agent according to a ratio, adding the materials into a planetary mixer, stirring the materials at room temperature for 1 to 3 hours, and uniformly mixing the materials for later use;
weighing a proper amount of catalyst and pigment, adding the catalyst and the pigment into the planetary mixer, vacuumizing at 55-65 ℃ and under the pressure of-0.1 MPa, and stirring at 30rpm for 1-2 hours.
And step three, subpackaging, namely filling the mixed single-component gel into a single-component tube of 30 CC.
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