CN104178076A - Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof - Google Patents
Heat-conducting electric-insulating epoxy resin potting adhesive and preparation method thereof Download PDFInfo
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- CN104178076A CN104178076A CN201410457717.9A CN201410457717A CN104178076A CN 104178076 A CN104178076 A CN 104178076A CN 201410457717 A CN201410457717 A CN 201410457717A CN 104178076 A CN104178076 A CN 104178076A
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Abstract
The invention discloses a heat-conducting electric-insulating epoxy resin potting adhesive which is composed of an epoxy resin, a curing agent, a toughener, a diluter, a filler, an accelerator and a defoaming agent. The component A is composed the following components in parts by weight: 100 parts of epoxy resin, 10-30 parts of diluter, 5-15 parts of filler, 0.5-1 part of defoaming agent and 3-5 parts of coupling agent. The component B is composed the following components in parts by weight: 78-145 parts of curing agent, 10-40 parts of toughener, 5-10 parts of filler, 0.1-3 parts of accelerator and 0.5-1 part of defoaming agent. The A/B weight ratio is 1:1. The toughener is epoxy hydroxyl-terminated polybutadiene acrylonitrile. The filler is composite powder composed of nano magnesium silicon nitride, nano silicon carbide, nano aluminum nitride, nano boron nitride, high-sphericity nano aluminum oxide and nano silicon nitride with different particle sizes, and the average particle size is 40-60nm. The potting adhesive has the advantages of favorable thermal conductivity and favorable electric insulating property.
Description
Technical field
The present invention relates to sizing agent preparing technical field, particularly heat conductive insulating epoxy resin embedding adhesive and preparation method.
Background technology
Epoxy resin embedding adhesive is the thermosetting polymer matrix material that a class has the performances such as good bonding, corrosion-resistant, electric insulation, high strength, has become electronics, electric, machinofacture, chemical anticorrosion, aerospace, ship and the indispensable base mateiral of other many industrial circles.
Along with microelectronics and unicircuit are to high-speed, high-density, miniaturization, lightweight future development, make electronic devices and components, logical circuit volume constantly compressed, the heat that electronics unit volume produces sharply increases, thereby heat conductivility will affect the life and reliability of electronic devices and components, electronics.For guaranteeing the normal operation of electronic devices and components, need material to possess high heat-sinking capability, to guarantee the quick transmission of heat.And traditional epoxy resin is hot poor conductor, thermal conductivity is 0.2Wm
-1k
-1left and right, is difficult to meet the timely heat radiation requirement of electronic devices and components; Insulating property also have material impact to the service efficiency of electronic component and life-span, and good electrical insulating property can improve the service efficiency of electrical element, increases the service life.Therefore, guaranteeing that the heat conductivility that how effectively to improve epoxy resin under the prerequisite of insulating property becomes one of emphasis of current research.
Improve joint sealant thermal conductivity and mainly contain two kinds of approach, a kind of approach is to add the polymkeric substance with thermal conductivity, but because synthetic thermal conductive polymer cost is high, the tactical rule of organic polymer material is poor, and heat conductivility is also not ideal, thereby seldom uses; Another kind of approach is by adding high heat conductive filler, and at present, filling heat conductive filler is the method extensively adopting.The heat conductive filler that existing epoxy resin embedding adhesive adds is generally metal (copper, aluminium, iron etc.) powder and mineral filler (graphite, carbon black, inorganic oxide, nitride etc.).Although metallic substance thermal conductivity is higher, also can be used as the filler of heat-conductivity polymer composite, because metallic substance has electroconductibility, finished product poor insulativity, easily puncture, affect efficiency and the life-span of electronic component.Silicon powder thermal conductivity conventional in inorganic heat conductive filler is lower, and the thermal conductivity of the potting compound that employing silicon powder is filled is also lower, is less than 0.6W/ (mK), is unfavorable for the heat radiation of electric elements.The thermal conductivity of the mineral fillers such as non-ball-aluminium oxide, boron nitride, aluminium nitride is higher, but granularity large (general 400 orders) is poor with resin affinity, skewness, easily precipitation.
Summary of the invention
First technical problem that the present invention will solve is to provide a kind of heat conductive insulating epoxy resin embedding adhesive, and this joint sealant not only has good thermal conductivity, and good insulation preformance.
Second technical problem that the present invention will solve is to provide a kind of preparation method of this heat conductive insulating epoxy resin embedding adhesive.
Heat conductive insulating epoxy resin embedding adhesive of the present invention, is comprised of epoxy resin, solidifying agent, toughner, thinner, filler, promotor and defoamer, and the weight ratio of each composition is as follows:
A component:
B component:
A/B weight ratio 1: 1.
Be suitable for preferably one or more in liquid bisphenol A type epoxy resin, bisphenol f type epoxy resin, cycloaliphatic epoxy resin, aliphatic epoxy resin etc. of epoxy resin of the present invention, as E-51, E-44, E-42, E-54 or EP828 etc.; Applicable solidifying agent is as liquid anhydride, be selected from hexahydrophthalic anhydride, methyl carbic anhydride, hydrogenation methyl carbic anhydride any one or multiple; Applicable toughner is as endurable active toughener, and its molecule segment is the epoxy hydroxyl terminated butadiene acrylonitrile copolymer with epoxy group(ing), cyano group, and preferred molecular weight is 1800～2000, and oxirane value is 0.6～1mmol/g, and acrylonitrile content is 3%～7%; Applicable thinner is reactive thinner, be selected from polypropylene glycol 2-glycidyl, diglycidylether aniline, glycerin triglycidyl ether any one or multiple; Applicable filler is the composite powder that varigrained nano-silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride, high sphericity nano aluminium oxide and nano-silicon nitride form, its mean particle size 40～60nm, is not particularly limited composite powder component concentration; Applicable promotor is liquid imidazole class promotor, be selected from 2-ethyl-4-methylimidazole, 1 benzyl 2 methyl imidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole any one or multiple; Applicable coupling agent is silane coupling agent, be selected from γ aminopropyltriethoxy silane, gamma-amino propyl trimethoxy silicane, γ-glycidoxy Trimethoxy silane any one or multiple; Applicable defoamer is as tributyl phosphate etc.
The method of preparing heat conductive insulating epoxy resin embedding adhesive of the present invention, comprises the following steps:
(1) A component preparation:
Epoxy resin, thinner, filler, defoamer, coupling agent are added in stirring tank, under heating condition, be fully uniformly mixed, obtain A component;
(2) B component preparation:
Solidifying agent, toughner, filler, promotor, defoamer are added in stirring tank, under heating condition, be fully uniformly mixed, obtain B component;
(3) A component and B component are joined in mix and blend still by weight at 1: 1, be warming up to 85 ℃, vacuum tightness is greater than 0.095MPa, continues 30min, vacuumizes and removes bubble;
(4) compound is joined in mould, 90 ℃ of curing 1h, 110 ℃ of curing 2h, 180 ℃ of curing 3h, are down to room temperature naturally.
The endurable active toughener epoxy hydroxyl terminated butadiene acrylonitrile copolymer molecule segment that the present invention introduces is with epoxy group(ing), cyano group and hydroxyl, good and viscosity is low with liquid bisphenol A epoxy resin compatibility, improved the fragility of epoxy resin cured product and eliminated crack performance, can obviously improve epoxy resin embedding adhesive impact resistance and insulating property; The filler that the present invention introduces, multiple super-high heat-conductive media assemblage by different-grain diameter, good with resin affinity, be evenly distributed, be difficult for precipitation, can make to form between filler the degree of piling up of maximum, make to the full extent the heat conduction network that epoxy pouring sealant System forming is good, thereby reach effective thermal conduction and insulation, obtain high heat conductive insulating system, and water-intake rate is low.Product of the present invention can be widely used in electronics, electric, machinofacture, chemical anticorrosion, aerospace, ship and other many industrial circles, has a extensive future.The preparation method of heat conductive insulating epoxy resin embedding adhesive of the present invention, filler is added in respectively in A, B component, and dispersion effect is good, and the joint sealant heat conductive insulating performance of preparation is good, and technique is simple.
Embodiment
Below in conjunction with embodiment, the invention will be further described.The following stated umber is weight part.
Each embodiment heat conductive insulating epoxy resin embedding adhesive is prepared by the following method, and gained joint sealant performance is in Table 1.
(1) A component preparation:
Each composition is added in stirring tank, and then heated and stirred still to 85 ℃ is fully uniformly mixed under heating condition, obtains A component;
(2) B component preparation:
Each composition is added in stirring tank, and then heated and stirred still is 85 ℃, is fully uniformly mixed, and obtains B component;
(3) A component and B component are joined in mix and blend still by weight at 1: 1, be warming up to 85 ℃, vacuum tightness is greater than 0.095MPa, continues 30min, vacuumizes and removes bubble;
(4) compound is joined in mould, 90 ℃ of curing 1h, 110 ℃ of curing 2h, 180 ℃ of curing 3h, are down to room temperature naturally.
Filler is the composite powder that varigrained nano-silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride, high sphericity nano aluminium oxide and nano-silicon nitride six components form, its mean particle size 50nm.
EP828 is Dutch shell company product.
Embodiment 1
A component:
B component:
Embodiment 2:
A component:
B component:
Embodiment 3:
A component:
B component:
Comparative example
Each embodiment joint sealant performance of table 1
| Project | Comparative example | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Thermal conductivity, W/ (mk) | 0.35 | 4.31 | 4.46 | 5.15 |
| Volume specific resistance, Ω cm | 2.57×10 15 | 3.24×10 16 | 4.18×10 16 | 5.18×10 16 |
| Shock strength, kJ/m 2 | 1.7 | 18.80 | 21.03 | 25.62 |
| Water-intake rate, % (in 20 ℃ of invasion waters 50 days) | 0.28 | 0.30 | 0.32 | 0.35 |
Claims (9)
1. a heat conductive insulating epoxy resin embedding adhesive, is comprised of epoxy resin, solidifying agent, toughner, thinner, filler, promotor and defoamer, and the weight ratio of each composition is as follows:
A component:
B component:
A/B weight ratio 1: 1
Described toughner is epoxy hydroxyl terminated butadiene acrylonitrile copolymer; Filler is the composite powder that varigrained nano-silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride, high sphericity nano aluminium oxide and nano-silicon nitride form, its mean particle size 40～60nm.
2. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described epoxy resin is one or more in liquid bisphenol A type epoxy resin, bisphenol f type epoxy resin, cycloaliphatic epoxy resin, aliphatic epoxy resin etc.
3. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described solidifying agent be selected from hexahydrophthalic anhydride, methyl carbic anhydride, hydrogenation methyl carbic anhydride any one or multiple.
4. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described toughner molecular weight is 1800～2000, and its oxirane value is 0.6～1mmol/g, and its acrylonitrile content is 3%～7%.
5. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described thinner be selected from polypropylene glycol 2-glycidyl, diglycidylether aniline, glycerin triglycidyl ether any one or multiple.
6. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described promotor be selected from 2-ethyl-4-methylimidazole, 1 benzyl 2 methyl imidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole any one or multiple.
7. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described coupling agent be selected from γ aminopropyltriethoxy silane, gamma-amino propyl trimethoxy silicane, γ-glycidoxy Trimethoxy silane any one or multiple.
8. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described defoamer is tributyl phosphate.
9. a method of preparing the described heat conductive insulating epoxy resin embedding adhesive of one of claim 1～8, comprises the following steps:
(1) A component preparation
Epoxy resin, thinner, filler, defoamer, coupling agent are added in stirring tank, under heating condition, be fully uniformly mixed, obtain A component;
(2) B component preparation
Solidifying agent, toughner, filler, promotor, defoamer are added in stirring tank, under heating condition, be fully uniformly mixed, obtain B component;
(3) A component and B component are joined in mix and blend still by weight at 1: 1, be warming up to 85 ℃, vacuum tightness is greater than 0.095MPa, continues 30min, vacuumizes and removes bubble;
(4) compound is joined in mould, 90 ℃ of curing 1h, 110 ℃ of curing 2h, 180 ℃ of curing 3h, are down to room temperature naturally.
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| CN104497491A (en) * | 2014-12-23 | 2015-04-08 | 安徽助成信息科技有限公司 | Method for improving thermal conductivity of epoxy resin based on nanometer silicon carbide |
| CN105419570A (en) * | 2016-01-18 | 2016-03-23 | 苏州法斯特信息科技有限公司 | High-adhesiveness and high-temperature endurable insulating paint composition for electrical machines and electrical apparatuses |
| CN105602485A (en) * | 2016-01-26 | 2016-05-25 | 河北工业大学 | High-infrared-radiance insulating heat conduction adhesive and preparing method thereof |
| CN105647120A (en) * | 2016-01-27 | 2016-06-08 | 西安交通大学 | Epoxy resin-based nonlinear self-adaptive nanocomposite insulating material and preparation method thereof |
| CN105907346A (en) * | 2016-05-26 | 2016-08-31 | 张学健 | Epoxy electronic pouring sealant and preparation method thereof |
| CN105950090A (en) * | 2016-06-08 | 2016-09-21 | 蚌埠市正园电子科技有限公司 | Waterproof epoxy resin pouring sealant filled and modified by composite beryllium oxide and used for LED display screen |
| CN105950091A (en) * | 2016-06-08 | 2016-09-21 | 蚌埠市正园电子科技有限公司 | Epoxy resin pouring sealant modified by composite silicon nitride thermal conductive filler and used for LED display screen |
| CN105969278A (en) * | 2016-06-08 | 2016-09-28 | 蚌埠高华电子股份有限公司 | Naleic anhydride toughened and modified composite heat-conduction epoxy pouring sealant for LED display screen |
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| CN108913076A (en) * | 2018-06-29 | 2018-11-30 | 佛山市高明区爪和新材料科技有限公司 | A kind of heat conductive insulating casting glue |
| CN109096933A (en) * | 2018-07-11 | 2018-12-28 | 常州澳弘电子有限公司 | A kind of aluminum-based copper-clad plate insulating heat-conductive glue film of low filling high thermal conductivity |
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| CN105419570A (en) * | 2016-01-18 | 2016-03-23 | 苏州法斯特信息科技有限公司 | High-adhesiveness and high-temperature endurable insulating paint composition for electrical machines and electrical apparatuses |
| CN105602485A (en) * | 2016-01-26 | 2016-05-25 | 河北工业大学 | High-infrared-radiance insulating heat conduction adhesive and preparing method thereof |
| CN105602485B (en) * | 2016-01-26 | 2017-06-23 | 河北工业大学 | A kind of insulating heat-conductive adhesive of high infrared radiance and preparation method thereof |
| CN105647120A (en) * | 2016-01-27 | 2016-06-08 | 西安交通大学 | Epoxy resin-based nonlinear self-adaptive nanocomposite insulating material and preparation method thereof |
| CN105907346A (en) * | 2016-05-26 | 2016-08-31 | 张学健 | Epoxy electronic pouring sealant and preparation method thereof |
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| CN114316869A (en) * | 2021-12-31 | 2022-04-12 | 江苏科化新材料科技有限公司 | Two-component thermosetting epoxy resin composition and application thereof, two-component thermosetting epoxy resin and preparation method and application thereof |
| CN114316869B (en) * | 2021-12-31 | 2024-06-11 | 江苏中科科化新材料股份有限公司 | Bi-component thermosetting epoxy resin composition and application thereof, bi-component thermosetting epoxy resin and preparation method and application thereof |
| CN114591597A (en) * | 2022-03-11 | 2022-06-07 | 西安理工大学 | Modified epoxy composite material and preparation method thereof |
| CN115960569A (en) * | 2023-02-03 | 2023-04-14 | 武汉楚辰新材料科技有限公司 | Epoxy resin pouring sealant |
| CN117736549A (en) * | 2024-02-02 | 2024-03-22 | 广东博汇新材料科技有限公司 | Preparation method of high-heat-conductivity epoxy resin compound |
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