CN113736266A - Double-component heat-conducting gel and preparation method and application thereof - Google Patents

Double-component heat-conducting gel and preparation method and application thereof Download PDF

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CN113736266A
CN113736266A CN202111133630.2A CN202111133630A CN113736266A CN 113736266 A CN113736266 A CN 113736266A CN 202111133630 A CN202111133630 A CN 202111133630A CN 113736266 A CN113736266 A CN 113736266A
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heat
component
parts
conducting
filler
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CN113736266B (en
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刘廷铸
胡国新
陈柏富
赵志垒
黄永军
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Guangzhou Jointas Chemical Co Ltd
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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
    • H—ELECTRICITY
    • H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K7/00—Constructional details common to different types of electric apparatus
    • H05K7/20—Modifications to facilitate cooling, ventilating, or heating
    • H05K7/2039—Modifications to facilitate cooling, ventilating, or heating characterised by the heat transfer by conduction from the heat generating element to a dissipating body
    • 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
    • C08K2003/2217—Oxides; Hydroxides of metals of magnesium
    • C08K2003/222—Magnesia, i.e. magnesium oxide
    • 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
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/38—Boron-containing compounds
    • C08K2003/382—Boron-containing compounds and nitrogen
    • C08K2003/385—Binary compounds of nitrogen with boron
    • 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
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a two-component heat-conducting gel and a preparation method and application thereof. The two-component heat-conducting gel comprises a component A and a component B; the component A comprises the following components in parts by weight: 10-40 parts of monovinyl-terminated polydimethylsiloxane, 5-10 parts of methylhydrogen polydimethylsiloxane and 100-200 parts of heat-conducting filler A; the component B comprises the following components in parts by weight: 10-40 parts of alkoxy end-capped vinyl polydimethylsiloxane, 100-200 parts of heat-conducting filler B and 0.1-2 parts of catalyst. The preparation method comprises the following steps: firstly, mixing all the components in the component A to obtain premix A; mixing all the components in the component B to obtain a premix B; and then mixing the premix A and the premix B to obtain the bi-component heat-conducting gel. The double-component heat-conducting gel provided by the invention has the advantages of higher heat conductivity coefficient, better high temperature resistance and lower oil yield.

Description

Double-component heat-conducting gel and preparation method and application thereof
Technical Field
The invention belongs to the field of heat conduction materials, and particularly relates to a two-component heat conduction gel, and a preparation method and application thereof.
Background
In the heat dissipation process of the electronic component, heat is transferred from the inside of the device to the heat sink, and then is dissipated to the outside environment through the heat sink. Thermal resistance analysis shows that the device and the radiator are in hard contact, actual contact of the device and the radiator only accounts for 1-5% of the apparent area due to the fact that the microscopic surface of a solid is rough and uneven, and the rest part of the device and the radiator is provided with tiny pores filled with air, so that interface thermal resistance between the device and the radiator is large, an effective radiating channel is difficult to form, and the radiating effect is poor. Therefore, how to reduce the thermal interface resistance between the electronic component and the heat sink is one of the key technologies for improving the heat dissipation efficiency of the electronic component. The heat-conducting gel is a composite material prepared by mixing heat-conducting filler with organic polymer materials such as silicone oil and the like, is a novel heat-conducting interface material, combines the advantages of a heat-conducting gasket and heat-conducting paste, can keep a fixed shape like the heat-conducting gasket, and does not easily flow out of an interface like the heat-conducting paste, so that the heat-conducting gel is widely concerned by people.
CN111171571A discloses a high-elasticity heat-conducting gel and a preparation method thereof, wherein the high-elasticity heat-conducting gel comprises the following components in parts by weight: 100 parts of alpha, omega-alkoxy end-capped polydimethylsiloxane, 15-35 parts of simethicone, 5-10 parts of chain extender, 0.1-0.5 part of catalyst, 1-3 parts of surface treating agent and 700-1100 parts of heat-conducting filler. The preparation method comprises the following steps: uniformly mixing alpha, omega-alkoxy end-capped polydimethylsiloxane, simethicone, a surface treating agent and a heat conducting filler, heating to 120-130 ℃, then carrying out vacuum dehydration for 2-4 h, cooling to obtain a mixture, uniformly mixing a chain extender and a catalyst with the mixture under the protection of nitrogen, and discharging to obtain the high-elasticity heat conducting gel. Although the heat-conducting gel prepared by the technical scheme has the advantage of high resilience, the dimethyl silicone oil is easy to separate out and the oil yield is high in the preparation process of the heat-conducting gel.
CN111876135A discloses a heat-conducting gel and a preparation method thereof, wherein the heat-conducting gel comprises the following components in parts by weight: the heat-conducting filler comprises 10-60 parts of a component A, 10-60 parts of a component B and 200-700 parts of a heat-conducting filler; wherein the component A consists of vinyl silicone oil and a catalyst according to the mass ratio of (1000-6000) to 1; the component B is composed of vinyl silicone oil and hydrogen-containing silicone oil according to the mass ratio of 1 (2-3); the heat-conducting filler consists of modified heat-conducting ceramic powder and auxiliary heat-conducting filler, the heat-conducting filler accounts for more than 90% of the total mass of the heat-conducting gel, and the average particle size of the heat-conducting filler is 0.1-100 mu m; the modified heat-conducting ceramic powder is obtained by moving aluminum powder in a plasma atmosphere under a vacuum condition to modify the surface of aluminum powder. The heat-conducting gel prepared by the technical scheme has higher hardness and poorer high-temperature resistance.
CN108504108A discloses an addition type two-component organic silicon heat-conducting gel and a preparation method thereof. The organic silicon heat-conducting gel comprises two components A and B, wherein the component A comprises the following components: : 100 parts by weight of vinyl-containing silicone oil, 2-20 parts by weight of hydrogen-containing silicone oil, 200-3000 parts by weight of high-thermal-conductivity inorganic filler, 0-200 parts by weight of anti-settling filler, 0.1-2 parts by weight of surfactant and pigment; the component B comprises the following materials: 100 parts by weight of vinyl-containing silicone oil, 200-3000 parts by weight of high-thermal-conductivity inorganic filler, 0-200 parts by weight of anti-settling filler, 0.1-2 parts by weight of surfactant and 0.5-5 parts by weight of catalyst. The vinyl-containing silicone oil used in the technical scheme is polysiloxane containing more than two vinyl groups, and the prepared organic silicon heat-conducting gel has higher hardness and higher oil yield.
Therefore, how to provide a heat conductive gel with better high temperature resistance and lower oil yield is a technical problem to be solved urgently at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a two-component heat-conducting gel and a preparation method and application thereof. According to the invention, through the matching use of the components and the further use of the monovinyl end-capped polydimethylsiloxane and the alkoxy end-capped vinyl polydimethylsiloxane, the prepared two-component heat-conducting gel has better high temperature resistance, lower oil yield and higher heat conductivity coefficient, and is suitable for the preparation of electronic components.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the present invention provides a two-component thermally conductive gel comprising a component a and a component B;
the component A comprises the following components in parts by weight:
10-40 parts of monovinyl-terminated polydimethylsiloxane;
5-10 parts of methyl hydrogen polydimethylsiloxane;
100-200 parts of a heat-conducting filler A;
the component B comprises the following components in parts by weight:
10-40 parts of alkoxy end-capped vinyl polydimethylsiloxane;
100-200 parts of a heat-conducting filler B;
0.1-2 parts of a catalyst.
According to the invention, through the matching use of the components and the use of alkoxy end-capped vinyl polydimethylsiloxane, the two-component heat-conducting gel has better high temperature resistance and lower oil yield, and through the use of the monovinyl end-capped polydimethylsiloxane, the steric hindrance generated during the reaction of the monovinyl end-capped polydimethylsiloxane, the alkoxy end-capped vinyl polydimethylsiloxane and the methyl hydrogen polydimethylsiloxane is reduced, and the oil yield of the two-component heat-conducting gel is further reduced.
In the present invention, the weight parts of the monovinyl-terminated polydimethylsiloxane may be 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 23 parts, 25 parts, 27 parts, 30 parts, 33 parts, 36 parts, 38 parts, 40 parts, or the like.
The parts by weight of the methylhydrogen polydimethylsiloxane can be 5 parts, 5.5 parts, 6 parts, 6.5 parts, 7 parts, 7.5 parts, 8 parts, 8.5 parts, 9 parts, 9.5 parts, 10 parts and the like.
The weight parts of the thermally conductive filler a may be 100 parts, 110 parts, 120 parts, 130 parts, 140 parts, 150 parts, 160 parts, 170 parts, 180 parts, 190 parts, 200 parts, or the like.
The weight portion of the alkoxy-terminated vinyl polydimethylsiloxane may be 10 parts, 12 parts, 15 parts, 18 parts, 20 parts, 23 parts, 25 parts, 27 parts, 30 parts, 33 parts, 36 parts, 38 parts, 40 parts, or the like.
The weight parts of the thermally conductive filler B may be 100 parts, 110 parts, 120 parts, 130 parts, 140 parts, 150 parts, 160 parts, 165 parts, 180 parts, 190 parts, 200 parts, or the like.
The weight portion of the catalyst can be 0.1 portion, 0.2 portion, 0.4 portion, 0.6 portion, 0.8 portion, 1 portion, 1.2 portions, 1.4 portions, 1.6 portions, 1.8 portions, 2 portions and the like.
The following is a preferred technical solution of the present invention, but not a limitation to the technical solution provided by the present invention, and the object and advantageous effects of the present invention can be better achieved and achieved by the following preferred technical solution.
In a preferred embodiment of the present invention, the viscosity of the monovinyl-terminated polydimethylsiloxane is 100 to 5000cps (for example, 100cps, 500cps, 1000cps, 1500cps, 2000cps, 2500cps, 3000cps, 3500cps, 4000cps, 4500cps, 5000cps, etc.), and more preferably 100 to 1000 cps.
Preferably, the monovinyl-terminated polydimethylsiloxane has the structural formula of (CH)3)3SiO[R1R2SiO1/2]p[(R1)2SiO1/2]qSi(CH3)2CH＝CH2；
Wherein R is1Is selected from-CH3、-CH2CH3or-C6H5Any one of the above;
R2is selected from-H, -CH3or-C6H5Any one of the above;
p and q are each independently selected from integers greater than 0.
The methylhydrogen polydimethylsiloxane preferably has a viscosity of 50 to 1000cps (for example, 50cps, 100cps, 150cps, 200cps, 300cps, 400cps, 500cps, 600cps, 700cps, 800cps, 900cps, 1000cps, etc.), and more preferably 50 to 150 cps.
Preferably, the methyl hydrogen polydimethylsiloxane has a structural formula of H (CH)3)2Si[SiMeR3O]m[SiR3HO3/2]n[SiO2]sSi(R4)2H；
Wherein R is3Is selected from C1～C5Any one of straight chain or branched chain alkyl and phenyl;
R4is selected from C1～C5Any one of linear or branched alkyl;
in the present invention, said C1～C5The linear or branched alkyl group includes C1, C2, C3, C4, or C5, illustratively including but not limited to: methyl, ethyl, n-propyl, isopropyl, n-butyl, isobutyl, tert-butyl, n-pentyl, isopentyl, or neopentyl, and the like.
m, n and s are each independently selected from integers greater than zero.
In a preferred embodiment of the present invention, the viscosity of the alkoxy-terminated vinyl polydimethylsiloxane is 100 to 5000cps (for example, 100cps, 500cps, 1000cps, 1500cps, 2000cps, 2500cps, 3000cps, 3500cps, 4000cps, 4500cps, 5000cps, etc.), and more preferably 100 to 1000 cps.
Preferably, the alkoxy-terminated vinyl polydimethylsiloxane has the structural formula of (CH)3)2CH3OSiO[CH2＝CHR5SiO1/2]u[(R6)2SiO1/2]vSiOCH3(CH3)2；
Wherein R is5Is selected from-H, -CH3or-C6H5Any one of the above;
R6is selected from-CH3、-CH2CH3or-C6H5Any one of the above;
u and v are each independently selected from integers greater than 0.
Preferably, the catalyst is a platinum catalyst.
Preferably, the platinum catalyst is selected from the group consisting of a platinum divinyl tetramethyl disiloxane complex or/and a chloroplatinic acid-octanol complex.
As a preferred embodiment of the present invention, the heat conductive filler a and the heat conductive filler B are each independently selected from any one of alumina, boron nitride, magnesium oxide, zinc oxide, or silicon carbide, or a combination of at least two of them.
Preferably, the thermally conductive filler a and the thermally conductive filler B each independently include a combination of a first thermally conductive filler, a second thermally conductive filler, and a third thermally conductive filler.
Preferably, the particle size of the D90 of the first heat conductive filler is 30 to 50 μm, and may be 30 μm, 32 μm, 34 μm, 36 μm, 38 μm, 40 μm, 42 μm, 44 μm, 46 μm, 48 μm, or 50 μm, for example.
Preferably, the mass percentage of the first heat conductive filler in the heat conductive filler a and the heat conductive filler B is 50 to 80%, for example, 50%, 52%, 55%, 57%, 60%, 63%, 66%, 68%, 70%, 73%, 75%, 77%, 80%, or the like.
Preferably, the particle size of the D90 of the second heat conductive filler is 5 to 20 μm, and may be, for example, 5 μm, 6 μm, 7 μm, 8 μm, 9 μm, 10 μm, 11 μm, 12 μm, 13 μm, 14 μm, 15 μm, 16 μm, 17 μm, 18 μm, 19 μm, or 20 μm.
Preferably, the mass percentage of the second heat conductive filler in the heat conductive filler a and the heat conductive filler B is 5 to 30%, for example, 5%, 7%, 10%, 12%, 15%, 18%, 20%, 23%, 25%, 27%, or 30%.
Preferably, the particle size of the D90 of the third heat conductive filler is 0.1 to 2 μm, and may be, for example, 0.1 μm, 0.2 μm, 0.4 μm, 0.6 μm, 0.8 μm, 1 μm, 1.2 μm, 1.4 μm, 1.6 μm, 1.8 μm, or 2 μm.
Preferably, the mass percentage of the third heat conductive filler in the heat conductive filler a and the heat conductive filler B is 1 to 20%, for example, 1%, 2%, 4%, 6%, 8%, 10%, 12%, 14%, 16%, 18%, 20%, or the like.
According to the invention, the heat-conducting fillers with different particle sizes are used, so that the stacking structure of the two-component thermal gel is denser, and the prepared two-component heat-conducting gel has lower viscosity, higher heat conductivity coefficient and better extrudability.
In a preferred embodiment of the present invention, the component a further comprises 0.1 to 2 parts of a first powder treatment agent, which may be, for example, 0.1 part, 0.2 part, 0.4 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, or the like.
Preferably, the first powder treatment agent is selected from any one or a combination of at least two of hexadecyl trimethoxy silane, n-decyl trimethoxy silane, hexamethyl disilazane, methyl trimethoxy silane, ethyl trimethoxy silane, methyl triethoxy silane, or ethyl triethoxy silane, and further preferably is hexadecyl trimethoxy silane and/or n-decyl trimethoxy silane.
Preferably, the component A also comprises 0.1-2 parts of tackifier, such as 0.1 part, 0.2 part, 0.4 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts or 2 parts.
Preferably, the adhesion promoter is selected from any one or a combination of at least two of vinyltrimethoxysilane, methyltrimethoxysilane, aminopropyltrimethoxysilane, aminopropyltriethoxysilane, vinyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane or N-beta-aminoethyl-gamma-aminopropyltrimethoxysilane.
Preferably, the component A also comprises 0.01-0.1 part of inhibitor, such as 0.01 part, 0.02 part, 0.03 part, 0.04 part, 0.05 part, 0.06 part, 0.07 part, 0.08 part, 0.09 part or 0.1 part and the like.
Preferably, the inhibitor is selected from any one or a combination of at least two of tetramethyldivinyldisiloxane, ethynylcyclohexanol, diallyl formamide, tetramethyltetravinylcyclotetrasiloxane or diallyl fumarate, and is further preferably tetramethyldivinyldisiloxane and/or tetramethyltetravinylcyclotetrasiloxane.
In a preferred embodiment of the present invention, the component B further comprises 0.1 to 2 parts of a second powder treatment agent, which may be, for example, 0.1 part, 0.2 part, 0.4 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts, 2 parts, or the like.
Preferably, the second powder treatment agent is selected from any one or a combination of at least two of hexadecyl trimethoxy silane, n-decyl trimethoxy silane, hexamethyl disilazane, methyl trimethoxy silane, ethyl trimethoxy silane, methyl triethoxy silane or ethyl triethoxy silane, and further preferably hexadecyl trimethoxy silane and/or n-decyl trimethoxy silane.
Preferably, the component B also comprises 0.1-2 parts of antioxidant, such as 0.1 part, 0.2 part, 0.4 part, 0.6 part, 0.8 part, 1 part, 1.2 parts, 1.4 parts, 1.6 parts, 1.8 parts or 2 parts.
Preferably, the antioxidant is selected from any one of or a combination of at least two of pentaerythritol tetrakis [ beta-propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, dinonyldiphenylamine or 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanurate.
Preferably, the component B also comprises 0.1-1 part of heat-resistant auxiliary agent, such as 0.1 part, 0.2 part, 0.3 part, 0.4 part, 0.5 part, 0.6 part, 0.7 part, 0.8 part, 0.9 part or 1 part and the like.
Preferably, the heat-resisting auxiliary agent is selected from any one of or a combination of at least two of octadecyl trimethyl ammonium chloride, methyl methacrylate copolymer or polyaromatic hydrocarbon mineral oil.
In a second aspect, the present invention provides a method for preparing a two-component thermal conductive gel according to the first aspect, including the following steps:
(1) mixing monovinyl-terminated polydimethylsiloxane, methylhydrogen polydimethylsiloxane, a heat-conducting filler A, an optional first powder treating agent, an optional tackifier and an optional inhibitor to obtain a premix A;
mixing alkoxy end-capped vinyl polydimethylsiloxane, a heat-conducting filler B, a catalyst, an optional second powder treating agent, an optional antioxidant and an optional heat-resisting auxiliary agent to obtain a premix B;
(2) and (2) mixing the premix A and the premix B obtained in the step (1) to obtain the bi-component heat-conducting gel.
As a preferred technical scheme of the invention, the premix A in the step (1) is mixed under vacuum condition.
Preferably, the degree of vacuum under the vacuum condition is 0.08 to 0.1MPa, and may be, for example, 0.08MPa, 0.085MPa, 0.09MPa, 0.095MPa, or 0.1 MPa.
Preferably, the mixing time of the premix A in the step (1) is 20-60 min, for example, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min or 60 min.
As a preferred technical scheme of the invention, the premix B in the step (1) is mixed under vacuum condition.
Preferably, the degree of vacuum under the vacuum condition is 0.08 to 0.1MPa, and may be, for example, 0.08MPa, 0.085MPa, 0.09MPa, 0.095MPa, or 0.1 MPa.
Preferably, the mixing time of the premix B in the step (1) is 20-60 min, for example, 20min, 25min, 30min, 35min, 40min, 45min, 50min, 55min or 60 min.
Preferably, the mixing time in step (2) is 1-20 min, such as 1min, 2min, 4min, 6min, 8min, 10min, 12min, 14min, 16min, 18min or 20 min.
In a third aspect, the invention provides an application of the two-component thermal conductive gel in preparation of electronic components.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, through the matching use of the components, the weight parts of the alkoxy-terminated vinyl polydimethylsiloxane are further controlled within a specific range, and meanwhile, through the control of the use of the heat-conducting fillers with different particle sizes, the prepared two-component heat-conducting gel has good extrudability of 60-80 g/min, and the aging extrudability of the two-component heat-conducting gel after the two-component heat-conducting gel is placed at 90 ℃ for 21 days is 45-75 g/min; but also has lower oil yield of 0.6 to 1.3 percent; meanwhile, the high-temperature-resistant heat-conducting resin has good high temperature resistance, the heat conductivity coefficient is 4.0-6.0W/(m.K), the high-temperature-resistant heat-conducting resin is cured for 30min at the temperature of 100 ℃, and after the high-temperature-resistant heat-conducting resin is placed in a 180 ℃ oven for 72h, the thermal weight loss is small and is 0.6-1.2%.
Detailed Description
The technical solution of the present invention is further illustrated by the following specific examples. 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.
The sources of some of the components in the examples and comparative examples are as follows:
platinum divinyl tetramethyl disiloxane complex: anhui Eyota Silicone oil, Inc., IOTA-8100;
chloroplatinic acid-octanol complex: dongguan City Dong Cheng synthetic materials GmbH, DC-3000 ppm;
methyl methacrylate copolymer: denming wegian limited;
polyaromatic hydrocarbon mineral oil: the shinkansen chemical group, Vivatec 500, germany.
Example 1
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, wherein the two-component heat-conducting gel comprises a component A and a component B;
the component A comprises the following components in parts by weight:
Figure BDA0003281397840000101
the component B comprises the following components in parts by weight:
Figure BDA0003281397840000102
the viscosity of the monovinyl-terminated polydimethylsiloxane is 1000cps, and the structural formula is (CH)3)3SiO[R1R2SiO1/2]p[(R1)2SiO1/2]qSi(CH3)2CH＝CH2(ii) a Wherein R is1is-CH3，R2is-H, p is 20, q is 20;
the viscosity of the methyl hydrogen polydimethylsiloxane is 100cps, and the structural formula is H (CH)3)2Si[SiMeR3O]m[SiR3HO3/2]n[SiO2]sSi(R4)2H; wherein R is3Is methyl, R4Is ethyl, m is 10, n is 18, s is 20;
in the aluminum oxide, the particle size of the first heat-conducting filler is 40 micrometers, the mass percentage content of the first heat-conducting filler is 70%, the particle size of the second heat-conducting filler is 10 micrometers, the mass percentage content of the second heat-conducting filler is 20%, the particle size of the third heat-conducting filler is 1 micrometer, and the mass percentage content of the third heat-conducting filler is 10%;
the viscosity of the alkoxy end-capped vinyl polydimethylsiloxane is 1000cps, and the structural formula is (CH)3)2CH3OSiO[CH2＝CHR5SiO1/2]u[(R6)2SiO1/2]vSiOCH3(CH3)2(ii) a Wherein R is5is-H, R6is-CH3U is 16 and v is 27;
in the boron nitride, the particle size of the first heat-conducting filler is 30 microns, the mass percentage content of the first heat-conducting filler is 65%, the particle size of the second heat-conducting filler is 15 microns, the mass percentage content of the second heat-conducting filler is 25%, the particle size of the third heat-conducting filler is 1 micron, and the mass percentage content of the third heat-conducting filler is 10%.
The preparation method of the two-component heat-conducting gel comprises the following steps:
(1) under the condition that the vacuum degree is 0.08MPa, mono-vinyl end-capped polydimethylsiloxane, methyl hydrogen polydimethylsiloxane, alumina, hexadecyl trimethoxy silane, vinyl trimethoxy silane and tetramethyl divinyl disiloxane are mixed for 30min to obtain premix A;
under the condition that the vacuum degree is 0.08MPa, mixing alkoxy-terminated vinyl polydimethylsiloxane, boron nitride, n-decyltrimethoxysilane, tetra [ beta-propionic acid ] pentaerythritol ester, octadecyl trimethyl ammonium chloride and diethylene tetramethyl disiloxane platinum complex for 40min to obtain premix B;
(2) and (2) mixing the premix A and the premix B obtained in the step (1) for 2min to obtain the bi-component heat-conducting gel.
Example 2
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, wherein the two-component heat-conducting gel comprises a component A and a component B;
the component A comprises the following components in parts by weight:
Figure BDA0003281397840000121
the component B comprises the following components in parts by weight:
Figure BDA0003281397840000122
the viscosity of the monovinyl-terminated polydimethylsiloxane is 500cps, and the structural formula is (CH)3)3SiO[R1R2SiO1/2]p[(R1)2SiO1/2]qSi(CH3)2CH＝CH2(ii) a Wherein R is1is-CH2CH3，R2is-CH3P is 10 and q is 32;
the viscosity of the methyl hydrogen polydimethylsiloxane is 150cps, and the structural formula is H (CH)3)2Si[SiMeR3O]m[SiR3HO3/2]n[SiO2]sSi(R4)2H; wherein R is3Is ethyl, R4Is n-propyl, m is 17, n is 19, s is 26;
in the magnesium oxide, the particle size of the first heat-conducting filler is 50 μm and the mass percentage content is 50%, the particle size of the second heat-conducting filler is 5 μm and the mass percentage content is 30%, and the particle size of the third heat-conducting filler is 0.1 μm and the mass percentage content is 20%;
the viscosity of the alkoxy end-capped vinyl polydimethylsiloxane is 5000cps, and the structural formula is (CH)3)2CH3OSiO[CH2＝CHR5SiO1/2]u[(R6)2SiO1/2]vSiOCH3(CH3)2(ii) a Wherein R is5is-CH3，R6is-CH2CH3U is 32 and v is 40;
in the silicon carbide, the particle size of the first heat-conducting filler is 30 microns, the mass percentage content of the first heat-conducting filler is 60%, the particle size of the second heat-conducting filler is 25 microns, the mass percentage content of the second heat-conducting filler is 25%, the particle size of the third heat-conducting filler is 0.5 microns, and the mass percentage content of the third heat-conducting filler is 15%.
The preparation method of the two-component heat-conducting gel comprises the following steps:
(1) under the condition that the vacuum degree is 0.085MPa, mono-vinyl end-capped polydimethylsiloxane, methyl hydrogen polydimethylsiloxane, magnesium oxide, n-decyl trimethoxy silane, methyl trimethoxy silane and acetylene cyclohexanol are mixed for 60min to obtain premix A;
under the condition that the vacuum degree is 0.085MPa, mixing alkoxy-terminated vinyl polydimethylsiloxane, silicon carbide, hexadecyl trimethoxy silane, tris (2, 4-di-tert-butylphenyl) phosphite, a methyl methacrylate copolymer and a chloroplatinic acid-octanol complex for 30min to obtain a premix B;
(2) and (2) mixing the premix A and the premix B obtained in the step (1) for 5min to obtain the bi-component heat-conducting gel.
Example 3
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, wherein the two-component heat-conducting gel comprises a component A and a component B;
the component A comprises the following components in parts by weight:
Figure BDA0003281397840000131
Figure BDA0003281397840000141
the component B comprises the following components in parts by weight:
Figure BDA0003281397840000142
the viscosity of the monovinyl-terminated polydimethylsiloxane is 5000cps, and the structural formula is (CH)3)3SiO[R1R2SiO1/2]p[(R1)2SiO1/2]qSi(CH3)2CH＝CH2(ii) a Wherein R is1is-C6H5，R2is-H, p is 35, q is 40;
the viscosity of the methyl hydrogen polydimethylsiloxane is 1000cps, and the structural formula is H (CH)3)2Si[SiMeR3O]m[SiR3HO3/2]n[SiO2]sSi(R4)2H; wherein R is3Is n-butyl, R4Is n-propyl; m is 36, n is 42, s is 18;
in the zinc oxide, the particle size of the first heat-conducting filler is 30 micrometers, the mass percentage content of the first heat-conducting filler is 80%, the particle size of the second heat-conducting filler is 5 micrometers, the mass percentage content of the second heat-conducting filler is 5%, the particle size of the third heat-conducting filler is 0.1 micrometers, and the mass percentage content of the third heat-conducting filler is 15%;
the viscosity of the alkoxy-terminated vinyl polydimethylsiloxane is 100cps, and the structural formula is (CH)3)2CH3OSiO[CH2＝CHR5SiO1/2]u[(R6)2SiO1/2]vSiOCH3(CH3)2(ii) a Wherein R is5is-C6H5，R6is-CH2CH3，uIs 18, v is 26;
in the aluminum oxide, the particle size of the first heat-conducting filler is 40 μm and the mass percentage content is 50%, the particle size of the second heat-conducting filler is 12 μm and the mass percentage content is 30%, and the particle size of the third heat-conducting filler is 2 μm and the mass percentage content is 20%.
The preparation method of the two-component heat-conducting gel comprises the following steps:
(1) under the condition that the vacuum degree is 0.09MPa, mono-vinyl end-capped polydimethylsiloxane, methyl hydrogen polydimethylsiloxane, zinc oxide, hexamethyldisilazane, aminopropyltrimethoxysilane and diallyl formamide are mixed for 50min to obtain premix A;
under the condition that the vacuum degree is 0.089MPa, mixing alkoxy end-capped vinyl polydimethylsiloxane, alumina, ethyltrimethoxysilane, dinonyldiphenylamine, polyolefin mineral oil and a divinyl tetramethyl disiloxane platinum complex for 20min to obtain premix B;
(2) and (2) mixing the premix A and the premix B obtained in the step (1) for 10min to obtain the bi-component heat-conducting gel.
Example 4
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, wherein the two-component heat-conducting gel comprises a component A and a component B;
the component A comprises the following components in parts by weight:
Figure BDA0003281397840000151
the component B comprises the following components in parts by weight:
Figure BDA0003281397840000152
Figure BDA0003281397840000161
the monovinyl end-cappingThe polydimethylsiloxane has a viscosity of 100cps and a simple structure formula of (CH)3)3SiO[R1R2SiO1/2]p[(R1)2SiO1/2]qSi(CH3)2CH＝CH2(ii) a Wherein R is1is-C6H5，R2is-CH3or-C6H5P is 8 and q is 12;
the viscosity of the methyl hydrogen polydimethylsiloxane is 1000cps, and the structural formula is H (CH)3)2Si[SiMeR3O]m[SiR3HO3/2]n[SiO2]sSi(R4)2H; wherein R is3Is phenyl, R4Is methyl; m is 72, n is 54, s is 18;
the particle size of the first heat-conducting filler in the boron nitride is 45 microns, the mass percentage content of the first heat-conducting filler is 70%, the particle size of the second heat-conducting filler is 15 microns, the mass percentage content of the second heat-conducting filler is 29%, the particle size of the third heat-conducting filler is 2 microns, and the mass percentage content of the third heat-conducting filler is 1%;
the viscosity of the alkoxy end-capped vinyl polydimethylsiloxane is 4000cps, and the structural formula is (CH)3)2CH3OSiO[CH2＝CHR5SiO1/2]u[(R6)2SiO1/2]vSiOCH3(CH3)2(ii) a Wherein R is5is-CH3，R6is-C6H5U is 48 and v is 36;
in the aluminum oxide, the particle size of the first heat-conducting filler is 50 μm and the mass percentage content is 80%, the particle size of the second heat-conducting filler is 20 μm and the mass percentage content is 5%, and the particle size of the third heat-conducting filler is 0.1 μm and the mass percentage content is 15%.
The preparation method of the two-component heat-conducting gel comprises the following steps:
(1) under the condition that the vacuum degree is 0.095MPa, mono-vinyl end-capped polydimethylsiloxane, methyl hydrogen polydimethylsiloxane, boron nitride, methyl triethoxysilane, vinyl trimethoxysilane and tetramethyl tetravinylcyclotetrasiloxane are mixed for 20min to obtain premix A;
under the condition that the vacuum degree is 0.095MPa, mixing alkoxy-terminated vinyl polydimethylsiloxane, alumina, ethyltriethoxysilane, 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanuric acid, octadecyl trimethyl ammonium chloride and a divinyl tetramethyl disiloxane platinum complex for 50min to obtain a premix B;
(2) and (2) mixing the premix A and the premix B obtained in the step (1) for 15min to obtain the bi-component heat-conducting gel.
Example 5
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, wherein the two-component heat-conducting gel comprises a component A and a component B;
the component A comprises the following components in parts by weight:
40 parts of monovinyl-terminated polydimethylsiloxane;
6 parts of methyl hydrogen polydimethylsiloxane;
190 parts of aluminum oxide;
the component B comprises the following components in parts by weight:
10 parts of alkoxy-terminated vinyl polydimethylsiloxane;
180 parts of magnesium oxide;
1.3 parts of chloroplatinic acid-octanol complex;
the viscosity of the monovinyl-terminated polydimethylsiloxane is 4000cps, and the structural formula is (CH)3)3SiO[R1R2SiO1/2]p[(R1)2SiO1/2]qSi(CH3)2CH＝CH2(ii) a Wherein R is1is-CH3，R2is-C6H5P is 30 and q is 46;
the viscosity of the methyl hydrogen polydimethylsiloxane is 50cps, and the structural formula is H (CH)3)2Si[SiMeR3O]m[SiR3HO3/2]n[SiO2]sSi(R4)2H; wherein R is3Is phenyl, R4Is isobutyl, m is 18, n is 26, s is 14;
in the aluminum oxide, the particle size of the first heat-conducting filler is 35 μm and the mass percentage content is 65%, the particle size of the second heat-conducting filler is 10 μm and the mass percentage content is 25%, and the particle size of the third heat-conducting filler is 0.1 μm and the mass percentage content is 10%;
the viscosity of the alkoxy-terminated vinyl polydimethylsiloxane is 500cps, and the structural formula is (CH)3)2CH3OSiO[CH2＝CHR5SiO1/2]u[(R6)2SiO1/2]vSiOCH3(CH3)2(ii) a Wherein R is5is-CH3，R6is-C6H5U is 32 and v is 18;
in the magnesium oxide, the particle size of the first heat-conducting filler is 45 μm and the mass percentage content is 70%, the particle size of the second heat-conducting filler is 5 μm and the mass percentage content is 29%, and the particle size of the third heat-conducting filler is 2 μm and the mass percentage content is 1%.
The preparation method of the two-component heat-conducting gel comprises the following steps:
(1) under the condition that the vacuum degree is 0.1MPa, mixing monovinyl end-capped polydimethylsiloxane, methylhydrogen polydimethylsiloxane and alumina for 40min to obtain premix A;
under the condition that the vacuum degree is 0.1MPa, mixing alkoxy-terminated vinyl polydimethylsiloxane, magnesium oxide and chloroplatinic acid-octanol complex for 60min to obtain premix B;
(2) and (2) mixing the premix A and the premix B obtained in the step (1) for 20min to obtain the bi-component heat-conducting gel.
Example 6
This example provides a two-component thermal conductive gel and a method for preparing the same, which is different from example 1 only in that the part by weight of the alkoxy-terminated vinyl polydimethylsiloxane in the component B is 20 parts, and the other conditions are the same as example 1.
Example 7
This example provides a two-component thermal conductive gel and a method for preparing the same, which is different from example 1 only in that, in the component B, the alkoxy-terminated vinyl polydimethylsiloxane is 40 parts by weight, and the other conditions are the same as example 1.
Example 8
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, and the difference from embodiment 1 is only that in the component a, alumina does not contain a first heat-conducting filler, the particle size of a second heat-conducting filler is 10 μm, the mass percentage content of the second heat-conducting filler is 66.7%, the particle size of a third heat-conducting filler is 1 μm, and the mass percentage content of the third heat-conducting filler is 33.3%; in the component B, the boron nitride does not contain the first heat-conducting filler, the particle size of the second heat-conducting filler is 15 μm and the mass percentage content is 71.4%, the particle size of the third heat-conducting filler is 1 μm and the mass percentage content is 28.6%, and other conditions are the same as those in the embodiment 1.
Example 9
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, and the difference from embodiment 1 is only that in the component a, the alumina does not contain a second heat-conducting filler, the particle size of the first heat-conducting filler is 40 μm, the mass percentage content of the first heat-conducting filler is 87.5%, the particle size of the third heat-conducting filler is 1 μm, and the mass percentage content of the third heat-conducting filler is 12.5%; in the component B, the boron nitride does not contain the second heat-conducting filler, the particle size of the first heat-conducting filler is 30 μm and the mass percentage content of the first heat-conducting filler is 86.7%, the particle size of the third heat-conducting filler is 1 μm and the mass percentage content of the third heat-conducting filler is 13.3%, and other conditions are the same as those in the embodiment 1.
Example 10
The embodiment provides a two-component heat-conducting gel and a preparation method thereof, and the difference from embodiment 1 is only that in the component a, alumina does not contain a third heat-conducting filler, the particle size of the first heat-conducting filler is 40 μm, the mass percentage content of the first heat-conducting filler is 77.8%, the particle size of the second heat-conducting filler is 10 μm, and the mass percentage content of the second heat-conducting filler is 22.2%; in the component B, the boron nitride does not contain a third heat-conducting filler, the particle size of the first heat-conducting filler is 30 μm and the mass percentage content of the first heat-conducting filler is 72.2%, the particle size of the second heat-conducting filler is 15 μm and the mass percentage content of the second heat-conducting filler is 27.8%, and other conditions are the same as those in the embodiment 1.
Comparative example 1
The comparative example provides a two-component heat-conducting gel and a preparation method thereof, and is different from the example 1 only in that in the component B, the weight part of alkoxy-terminated vinyl polydimethylsiloxane is 7 parts, and other conditions are the same as those in the example 1.
Comparative example 2
The comparative example provides a two-component heat-conducting gel and a preparation method thereof, and is different from the example 1 only in that in the component B, the weight part of alkoxy-terminated vinyl polydimethylsiloxane is 45 parts, and other conditions are the same as those in the example 1.
Comparative example 3
This comparative example provides a two-component thermally conductive gel and a method of preparing the same, differing from example 1 only in that alkoxy-terminated vinyl polydimethylsiloxane was replaced with polydimethylsiloxane (available from dow corning corporation, silicone oil 201), and the other conditions were the same as in example 1.
Comparative example 4
The comparative example provides a two-component heat-conducting gel and a preparation method thereof, and is different from the example 1 only in that the single vinyl end-capped polydimethylsiloxane is replaced by polyvinyl polydimethylsiloxane (purchased from silicone material corporation, 206-.
The performances of the two-component heat-conducting gel provided by the above examples and comparative examples were tested according to the following test standards:
extrudability: GB/T13477.3-2017;
oil yield: curing the two-component heat-conducting gel provided by the above examples and comparative examples at 100 ℃ for 30min to obtain a cured heat-conducting gel, then placing the cured heat-conducting gel in a 180 ℃ oven (Shanghai Jing electric heating constant temperature blast drying oven, DHG-9053A) for 72h, and removing silicone oil on the surface of the cured heat-conducting gel by using filter paper to obtain the heat-conducting gel
Oil yield is m2/m1×100％，
Wherein m is2For removing heat by curing through filter paperMass m of cured thermally conductive gel after silicone oil on gel surface1Mass of the cured thermally conductive gel;
coefficient of thermal conductivity: ASTM D5470;
aging and extrusion rate: after the two-component heat-conducting gel provided by the above examples and comparative examples is placed at 90 ℃ for 21 days, the extrudability of the two-component heat-conducting gel is measured according to GB/T13477.3-2017, namely the aging extrudability;
thermal weight loss: GB/T16776-.
The test results of the performance of the two-component thermal gel provided in the above examples and comparative examples are shown in table 1 below:
TABLE 1
Figure BDA0003281397840000211
Figure BDA0003281397840000221
As can be seen from Table 1, the two-component heat-conducting filler prepared by using the components in a matched manner, controlling the weight parts of the alkoxy-terminated vinyl polydimethylsiloxane within a specific range and controlling the use of the heat-conducting fillers with different particle sizes has good extrudability of 60-80 g/min, and the aging extrudability of the prepared two-component heat-conducting filler after the two-component heat-conducting filler is placed at 90 ℃ for 21 days is 45-75 g/min; but also has lower oil yield of 0.6 to 1.3 percent; meanwhile, the high-temperature-resistant heat-conducting resin has good high temperature resistance, the heat conductivity coefficient is 4.0-6.0W/(m.K), the high-temperature-resistant heat-conducting resin is cured for 30min at the temperature of 100 ℃, and after the high-temperature-resistant heat-conducting resin is placed in a 180 ℃ oven for 72h, the thermal weight loss is small and is 0.6-1.2%.
Compared with the example 1, if the heat-conducting filler A and the heat-conducting filler B do not contain the first heat-conducting filler (example 8), the prepared two-component heat-conducting gel has poor extrudability of 40g/min, and the aging extrudability of 34g/min after the two-component heat-conducting gel is placed at 90 ℃ for 21 days; if the particle sizes of the heat-conducting filler A and the heat-conducting filler B do not contain the second heat-conducting filler (example 9), the extrudability of the prepared two-component heat-conducting gel is poor and is 45g/min, and the aging extrudability of the two-component heat-conducting gel after the two-component heat-conducting gel is placed at 90 ℃ for 21 days is 42 g/min; if the particle sizes of the heat-conducting filler A and the heat-conducting filler B do not contain the third heat-conducting filler (example 9), the prepared two-component heat-conducting gel has poor extrudability of 55g/min, has an aged extrudability of 50g/min after being placed at 90 ℃ for 21 days, has poor heat conductivity and has a heat conductivity coefficient of 3.8W/(m.K). Therefore, the first heat-conducting filler, the second heat-conducting filler and the third heat-conducting filler have a synergistic effect, the heat-conducting fillers with different particle sizes are adopted, and the proportion relation of the first heat-conducting filler, the second heat-conducting filler and the third heat-conducting filler is further controlled within a specific range, so that the prepared two-component heat-conducting gel has good extrudability and heat conductivity.
Compared with example 1, if the weight part of the alkoxy-terminated vinyl polydimethylsiloxane is small (comparative example 1), the prepared two-component heat-conducting gel has poor extrudability of 30g/min, and the aging extrudability of the two-component heat-conducting gel after being placed at 90 ℃ for 21 days is 15 g/min; if the weight portion of the alkoxy-terminated vinyl polydimethylsiloxane is larger (comparative example 2), the prepared two-component heat-conducting gel has poor heat conductivity and the heat conductivity coefficient is 2.8W/(m.K) although the two-component heat-conducting gel has good extrudability. Therefore, when the weight parts of the alkoxy-terminated vinyl polydimethylsiloxane in the two-component heat-conducting gel are not in a specific range, the prepared two-component heat-conducting gel cannot have a high heat conductivity coefficient and good extrudability at the same time.
Compared with the example 1, if the alkoxy-terminated vinyl polydimethylsiloxane is replaced by other silicone oil (comparative example 3), the oil yield of the prepared two-component heat-conducting gel is higher by 3.2%, the high temperature resistance is poor, and the thermal weight loss is 2.0%; if the mono-vinyl end-capped polydimethylsiloxane is replaced by the poly-vinyl polydimethylsiloxane (comparative example 3), the oil yield of the prepared bi-component heat-conducting gel is 2.5%, the high temperature resistance is poor, and the thermal weight loss is 1.6%. Therefore, the bicomponent heat-conducting gel prepared by adopting the alkoxy end-capped vinyl polydimethylsiloxane and the monovinyl end-capped polydimethylsiloxane has lower oil yield and better heat-resistant weight loss.
In summary, the invention adopts alkoxy-terminated vinyl polydimethylsiloxane and monovinyl-terminated polydimethylsiloxane, further controls the weight part of the alkoxy-terminated vinyl polydimethylsiloxane in the two-component heat-conducting gel within a specific range, and controls the use of the heat-conducting fillers with different particle diameters in the heat-conducting filler A and the heat-conducting filler B, so that the prepared two-component heat-conducting gel has better extrudability, lower oil yield and higher high temperature resistance.
The applicant states that the present invention is illustrated by the detailed process flow of the present invention through the above examples, but the present invention is not limited to the above detailed process flow, that is, it does not mean that the present invention must rely on the above detailed process flow to be implemented. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.

Claims (10)

1. The two-component heat-conducting gel is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight:
10-40 parts of monovinyl-terminated polydimethylsiloxane;
5-10 parts of methyl hydrogen polydimethylsiloxane;
100-200 parts of a heat-conducting filler A;
the component B comprises the following components in parts by weight:
10-40 parts of alkoxy end-capped vinyl polydimethylsiloxane;
100-200 parts of a heat-conducting filler B;
0.1-2 parts of a catalyst.
2. The two-component heat-conducting gel according to claim 1, wherein the viscosity of the monovinyl-terminated polydimethylsiloxane is 100 to 5000cps, and more preferably 100 to 1000 cps;
preferably, the monovinyl-terminated polydimethylsiloxane has the structural formula of (CH)3)3SiO[R1R2SiO1/2]p[(R1)2SiO1/2]qSi(CH3)2CH＝CH2；
Wherein R is1Is selected from-CH3、-CH2CH3or-C6H5Any one of the above;
R2is selected from-H, -CH3or-C6H5Any one of the above;
p and q are each independently selected from integers greater than 0;
preferably, the viscosity of the methylhydrogen polydimethylsiloxane is 50 to 1000cps, and more preferably 50 to 150 cps;
preferably, the methyl hydrogen polydimethylsiloxane has a structural formula of H (CH)3)2Si[SiMeR3O]m[SiR3HO3/2]n[SiO2]sSi(R4)2H；
Wherein R is3Is selected from C1～C5Any one of straight chain or branched chain alkyl and phenyl;
R4is selected from C1～C5Any one of linear or branched alkyl;
m, n and s are each independently selected from integers greater than zero.
3. The two-component heat-conducting gel according to claim 1 or 2, wherein the viscosity of the alkoxy-terminated vinyl polydimethylsiloxane is 100 to 5000cps, and more preferably 100 to 1000 cps;
preferably, the alkoxy-terminated vinyl polydimethylsiloxane has the structural formula of (CH)3)2CH3OSiO[CH2＝CHR5SiO1/2]u[(R6)2SiO1/2]vSiOCH3(CH3)2；
Wherein R is5Is selected from-H, -CH3or-C6H5Any one of the above;
R6is selected from-CH3、-CH2CH3or-C6H5Any one of the above;
u and v are each independently selected from integers greater than 0;
preferably, the catalyst is a platinum catalyst;
preferably, the platinum catalyst is selected from the group consisting of a platinum divinyl tetramethyl disiloxane complex or/and a chloroplatinic acid-octanol complex.
4. The two-component thermally conductive gel according to any one of claims 1 to 3, wherein the thermally conductive filler A and the thermally conductive filler B are each independently selected from any one of alumina, boron nitride, magnesium oxide, zinc oxide, or silicon carbide or a combination of at least two thereof;
preferably, the thermally conductive filler a and the thermally conductive filler B each independently comprise a combination of a first thermally conductive filler, a second thermally conductive filler, and a third thermally conductive filler;
preferably, the D90 particle size of the first heat-conducting filler is 30-50 μm;
preferably, the mass percentage of the first heat-conducting filler in the heat-conducting filler A and the mass percentage of the first heat-conducting filler in the heat-conducting filler B are respectively and independently 50-80%;
preferably, the D90 particle size of the second heat-conducting filler is 5-20 μm;
preferably, the mass percentage of the second heat-conducting filler in the heat-conducting filler A and the mass percentage of the second heat-conducting filler in the heat-conducting filler B are respectively and independently 5-30%;
preferably, the D90 particle size of the third heat-conducting filler is 0.1-2 μm;
preferably, the mass percentage of the third heat-conducting filler in the heat-conducting filler A and the mass percentage of the third heat-conducting filler in the heat-conducting filler B are respectively and independently 1-20%.
5. The two-component heat-conducting gel according to any one of claims 1 to 4, wherein the component A further comprises 0.1-2 parts of a first powder treating agent;
preferably, the first powder treating agent is selected from any one or a combination of at least two of hexadecyl trimethoxy silane, n-decyl trimethoxy silane, hexamethyl disilazane, methyl trimethoxy silane, ethyl trimethoxy silane, methyl triethoxy silane or ethyl triethoxy silane, and further preferably is hexadecyl trimethoxy silane and/or n-decyl trimethoxy silane;
preferably, the component A also comprises 0.1-2 parts of a tackifier;
preferably, the adhesion promoter is selected from any one or a combination of at least two of vinyltrimethoxysilane, methyltrimethoxysilane, aminopropyltrimethoxysilane, aminopropyltriethoxysilane, vinyltrimethoxysilane, N-phenyl-3-aminopropyltrimethoxysilane or N-beta-aminoethyl-gamma-aminopropyltrimethoxysilane;
preferably, the component A also comprises 0.01-0.1 part of inhibitor;
preferably, the inhibitor is selected from any one or a combination of at least two of tetramethyldivinyldisiloxane, ethynylcyclohexanol, diallyl formamide, tetramethyltetravinylcyclotetrasiloxane or diallyl fumarate, and is further preferably tetramethyldivinyldisiloxane and/or tetramethyltetravinylcyclotetrasiloxane.
6. The two-component heat-conducting gel according to any one of claims 1 to 5, wherein the component B further comprises 0.1-2 parts of a second powder treating agent;
preferably, the second powder treating agent is selected from any one or a combination of at least two of hexadecyl trimethoxy silane, n-decyl trimethoxy silane, hexamethyl disilazane, methyl trimethoxy silane, ethyl trimethoxy silane, methyl triethoxy silane or ethyl triethoxy silane, and further preferably is hexadecyl trimethoxy silane and/or n-decyl trimethoxy silane;
preferably, the component B also comprises 0.1-2 parts of an antioxidant;
preferably, the antioxidant is selected from any one or a combination of at least two of pentaerythritol tetrakis [ beta-propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, dinonyldiphenylamine or 1,3, 5-tris (3, 5-di-tert-butyl-4-hydroxybenzyl) isocyanurate;
preferably, the component B also comprises 0.1-1 part of heat-resistant auxiliary agent;
preferably, the heat-resisting auxiliary agent is selected from any one of or a combination of at least two of octadecyl trimethyl ammonium chloride, methyl methacrylate copolymer or polyaromatic hydrocarbon mineral oil.
7. A method of preparing the two-component thermally conductive gel of any of claims 1-6, comprising the steps of:
(1) mixing monovinyl-terminated polydimethylsiloxane, methylhydrogen polydimethylsiloxane, a heat-conducting filler A, an optional first powder treating agent, an optional tackifier and an optional inhibitor to obtain a premix A;
mixing alkoxy end-capped vinyl polydimethylsiloxane, a heat-conducting filler B, a catalyst, an optional second powder treating agent, an optional antioxidant and an optional heat-resisting auxiliary agent to obtain a premix B;
(2) and (2) mixing the premix A and the premix B obtained in the step (1) to obtain the bi-component heat-conducting gel.
8. The method for preparing the premix according to claim 7, wherein the mixing of the premix A of step (1) is carried out under vacuum;
preferably, the vacuum degree under the vacuum condition is 0.08-0.1 MPa;
preferably, the mixing time of the premix A in the step (1) is 20-60 min.
9. The preparation method according to claim 7 or 8, wherein the mixing of premix B in step (1) is carried out under vacuum;
preferably, the vacuum degree under the vacuum condition is 0.08-0.1 MPa;
preferably, the mixing time of the premix B in the step (1) is 20-60 min;
preferably, the mixing time in the step (2) is 1-20 min.
10. Use of the two-component thermally conductive gel according to any one of claims 1 to 6 in the preparation of electronic components.
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