CN101974302A - Low-viscosity and high-heat conduction epoxy resin electronic potting adhesive - Google Patents
Low-viscosity and high-heat conduction epoxy resin electronic potting adhesive Download PDFInfo
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Abstract
The invention relates to a low-viscosity and high-heat conduction epoxy resin electronic potting adhesive which is formed by mixing a component A with an amine curing agent according to the weight ratio of 100:5-12, wherein the component A comprises the following raw materials in weight ratio: 70-85 parts of spherical alumina powder, 10-20 parts of epoxy resin, 2-4 parts of active thinner, 2.5-5 parts of toughening agent and 0.1-0.5 parts of coupling agent. The invention has the advantages that the spherical alumina of the potting adhesive has higher filling amount compared with non-spherical alumina, the viscosity is less affected, the fluidity is favorable and the construction is convenient; the potting adhesive has good dispersibility and is difficult to sedimentate; a condensate has high heat conductivity and can quickly dissipate accumulated heat of heating parts and components; a high-filling filler can reduce a thermal expansion coefficient and a volumetric shrinkage rate and is very suitable for potting parts and components; and the price is cheaper compared with boron nitride and aluminum nitride, and the cost is low.
Description
Technical field
The present invention relates to a kind of joint sealant, relate in particular to a kind of low viscosity high-thermal-conductivity epoxy resin electron pouring sealant, belong to the joint sealant technical field.
Background technology
Thermal conductive adhesive is used for bonding and the encapsulation under the electrical isolation occasion of electronic apparatus components and parts more.Development along with unicircuit in the electronic industry and package technique, the volume trend miniaturization of electronic devices and components and logical circuit, it is to multifunction and integrated direction development, certainly will cause the significantly increase of thermal value, this just proposes very high requirement to the heat conductivility of bonding and packaged material, and therefore improving thermal conductivity is the problem of demanding urgently day by day.
The approach that improves the polymkeric substance heat conductivility has two kinds: 1, synthetic structural polymer with high thermal conductivity coefficient, as have polyacetylene, polyaniline, polypyrrole of good heat conductive performance etc., main by electronics heat conduction mechanism realization heat conduction, or have complete crystallinity, realize the polymkeric substance of heat conduction by phonon; 2, by adding high heat conduction inorganics polymkeric substance is filled preparation polymer/inorganic thing heat-conductive composite material.Because good heat conductive performance organic polymer costs an arm and a leg, filling heat conduction inorganic filler is the method that extensively adopts at present, now adopts many inorganic heat conductive fillers to mainly contain aluminum oxide, boron nitride, aluminium nitride etc.
Boron nitride (BN) has high thermal conductivity, high disruptive strength is arranged, but because BN density less (2.25g/cm3), when the BN consumption surpass resin system 30% the time, resin viscosity increase, skewness, mixed glue is difficulty very, and the complicated process of preparation cost is too high.
Aluminium nitride (ALN) is as a kind of new packing, and domestic just the beginning in recent years produced in enormous quantities, and quality product and stability need to investigate, and price is more expensive, and use can make cost too high separately.
Non-ball-aluminium oxide (AL
2O
3) electrical insulation capability is good, the manufacturing process maturation, low price is used the most general.But its thermal conductivity is too low, needs high the filling could improve thermal conductivity.But high filling can cause negative impact, increase seriously as gelatin viscosity, and mobile the reduction, thus influence processing characteristics; Mechanical property also can be influenced in addition.
So the kind of mineral filler, shape and usage quantity thereof are the key points of the high heat conductive electronic pouring sealant of preparation.Therefore, by changing the kind of mineral filler, invention designs a kind of heat conductivility height, and viscosity is low, the loading level height, and preparation technology is simple, and the joint sealant that cost is low becomes a kind of inexorable trend.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of low viscosity high-thermal-conductivity epoxy resin electron pouring sealant is provided, to reach the heat conductivility height, viscosity is low, and the loading level height prepares simple purpose.
The technical scheme that the present invention solves the problems of the technologies described above is as follows: a kind of low viscosity high-thermal-conductivity epoxy resin electron pouring sealant, mixed by 100: 5～12 weight ratio by A component and amine curing agent, described A component is made up of each raw material of following weight ratio: 0.1～0.5 part of 70～85 parts in ball-aluminium oxide powder, 10～20 parts of Resins, epoxy, 2～4 parts of reactive thinners, 2.5～5 parts of toughner and coupling agent.
The invention has the beneficial effects as follows: the ball-aluminium oxide of joint sealant of the present invention has higher loading level than non-ball-aluminium oxide, and is little to the influence of viscosity, good fluidity, easy construction; Good dispersity is free settling not; Cured article thermal conductivity height, can disperse rapidly the heating components and parts heat accumulation; The high filling of filler can reduce thermal expansivity and volumetric shrinkage, and is very suitable for the embedding electronic devices and components; And price is cheap than boron nitride, aluminium nitride, and cost is low.
On the basis of technique scheme, the present invention can also do following improvement.
Further, described amine curing agent is a kind of or any several mixture in aliphatic amide, modified fatty amine, phenol aldehyde modified amine, polyetheramine or the polymeric amide.
Adopt the beneficial effect of above-mentioned further scheme to be, i.e. ambient temperature curable, heating curable again, the low viscosity of mixing makes easy construction, and gives good electric property of cured article and mechanical property.
Further, the median size of described ball-aluminium oxide powder is 5～50 μ m, can adopt a kind of particle diameter to fill or two kinds of composite fillings of particle diameter.
Adopt the beneficial effect of above-mentioned further scheme to be, this ball-aluminium oxide powder diameter is neat, spherical rule, and high filler loading capacity, high heat conduction has good dispersiveness and mobile.
Further, described Resins, epoxy is a kind of or any several mixture in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, glycidyl amine type epoxy resin, the cycloaliphatic epoxy resin.
Adopt the beneficial effect of above-mentioned further scheme to be, give characteristics such as system low-shrinkage, weathering resistance, thermotolerance.
Further, described reactive thinner can be n-butyl glycidyl ether (BGE), glycidyl allyl ether (AGE), phenyl glycidyl ether (PGE), 1, a kind of or any several mixture in the 4-butanediol diglycidyl ether (BDGE).
Adopt the beneficial effect of above-mentioned further scheme to be, reduce the joint sealant system viscosity, improve manufacturability, improve wetting property, increase filler loading.
Further, described toughner can be carboxyl end of the liquid acrylonitrile-butadiene rubber (CTBN), hydroxyl terminated butyl nitrile (HTBN) rubber (HTBN) or strange scholar's toughner.
Adopt the beneficial effect of above-mentioned further scheme to be, improve epoxy resin cured product fragility, improve the epoxy resin cured product anti-cracking performance.
Further, described coupling agent is organo-silicon coupling agent, titanate coupling agent or aluminate coupling agent.
Adopt the beneficial effect of above-mentioned further scheme to be, make more media-resistant, water-fast, ageing-resistant of splicing face.
Further, described coupling agent is preferably organo-silicon coupling agent.
Further, described organo-silicon coupling agent is γ-An Bingjisanyiyangjiguiwan, styryl Trimethoxy silane or phenyltrimethoxysila,e.
Adopt the beneficial effect of above-mentioned further scheme to be,, improve the cementability of material guaranteeing to make splicing face more on media-resistant, water-fast, the ageing-resistant basis.
Further, the pigment 0.3 and the wetting dispersing agent 0.1～0.5 that also contain parts by weight in the described A component.
Adopt the beneficial effect of above-mentioned further scheme to be, pigment is in order to satisfy the product appearance requirement; Wetting dispersing agent is in order to promote base-material (Resins, epoxy) for the wetting of pigment and dispersion.
Further, described pigment is carbon black, and described Ricinate is a stearate.
During use, the weight ratio by 100: 5～12 takes by weighing A component and amine curing agent, and is even in stirring at room, solidifies 24～48 hours or gets final product in 4 hours in 65 ℃ of curing in 25 ℃.
Embodiment
Below principle of the present invention and feature are described, institute gives an actual example and only is used to explain the present invention, is not to be used to limit scope of the present invention.
Embodiment 1
70 parts in ball-aluminium oxide powder (homemade median size is 40 μ m), 15 parts of bisphenol A type epoxy resins, 5 parts of bisphenol f type epoxy resins, 3.7 parts of glycidyl allyl ethers, 5 parts of hydroxyl terminated butyl nitrile (HTBN) rubber, 0.5 part of phenyltrimethoxysila,e, 0.3 part of carbon black, 0.5 part of stearate at room temperature stirs, and makes the A component; Kymene 00 and 1: 1 amine curing agent of polyetheramine D-400 weight ratio.A component and amine curing agent mixed by weight 100: 12, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 24 hours in 25 ℃.
Embodiment 2
75 parts in ball-aluminium oxide powder (homemade median size is 40 μ m), 14 parts of bisphenol A type epoxy resins, 3.5 parts of bisphenol f type epoxy resins, 2.9 parts of n-butyl glycidyl ethers, 3.7 parts of hydroxyl terminated butyl nitrile (HTBN) rubber, 0.3 part of phenyltrimethoxysila,e, 0.3 part of carbon black, 0.3 part of stearate at room temperature stirs, and makes the A component; Polyamide 6 51 and 1: 1 amine curing agent of polyetheramine D-400 weight ratio.A component and amine curing agent mixed by weight 100: 9.8, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 36 hours in 25 ℃.
Embodiment 3
80 parts in ball-aluminium oxide powder (homemade median size is 40 μ m), 11 parts of bisphenol A type epoxy resins, 3 parts of bisphenol f type epoxy resins, 2.3 parts of phenyl glycidyl ethers, 3 parts of hydroxyl terminated butyl nitrile (HTBN) rubber, 0.2 part of phenyltrimethoxysila,e, 0.3 part of carbon black, 0.2 part of stearate at room temperature stirs, and makes the A component; The amine curing agent of D-400.A component and amine curing agent mixed by weight 100: 7.7, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 48 hours in 25 ℃.
Embodiment 4
80 parts in ball-aluminium oxide powder (Japanese median size is 25 μ m), 10 parts of bisphenol A type epoxy resins, 2 parts of cycloaliphatic epoxy resins, 2 parts of glycidyl amine type epoxy resins, 1,2.3 parts of 4-butanediol diglycidyl ethers, 3 parts of carboxyl end of the liquid acrylonitrile-butadiene rubber, 0.2 part of styryl Trimethoxy silane, 0.3 part of carbon black, 0.2 part of stearate at room temperature stirs, and makes the A component; Polyamide 6 51 and 1: 1 amine curing agent of polyetheramine D-400 weight ratio.A component and amine curing agent mixed by weight 100: 7.2, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 4 hours in 65 ℃.
Embodiment 5
80 parts of (Japanese 50 μ m: 5 μ m=6: 4 (weight ratios)) of ball-aluminium oxide powder, 12 parts of bisphenol A type epoxy resins, 2 parts of novolac epoxys, 1,2.3 parts of 4-butanediol diglycidyl ethers, 3 parts of carboxyl end of the liquid acrylonitrile-butadiene rubber, 0.2 part of styryl Trimethoxy silane, 0.3 part of carbon black, 0.2 part of stearate, at room temperature stir, make the A component; Kymene 00 and 1: 1 amine curing agent of polyetheramine D-400 weight ratio.A component and amine curing agent mixed by weight 100: 7.2, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 4 hours in 65 ℃.
Embodiment 6
85 parts of (Japanese 50 μ m: 5 μ m=6: 4 (weight ratios)) of ball-aluminium oxide powder, 9 parts of bisphenol A type epoxy resins, 1 part of novolac epoxy, 2.0 parts of n-butyl glycidyl ethers, 2.5 parts of strange scholar's toughner, 0.1 part of γ-An Bingjisanyiyangjiguiwan, 0.3 part of carbon black, 0.1 part of stearate at room temperature stirs, and makes the A component; The amine curing agent of D-400.A component and amine curing agent mixed by weight 100: 5, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 4 hours in 65 ℃.
The comparative example 1
70 parts in non-ball-aluminium oxide powder (Japanese A-42-6), 18 parts of bisphenol A type epoxy resins, 2 parts of cycloaliphatic epoxy resins, 3.7 parts of n-butyl glycidyl ethers, 5 parts of strange scholar's toughner, 0.5 part of γ-An Bingjisanyiyangjiguiwan, 0.3 part of carbon black, 0.5 part of stearate at room temperature stirs, and makes the A component; Kymene 00 and 1: 1 amine curing agent of polyetheramine D-400 weight ratio.A component and amine curing agent mixed by weight 100: 12, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 48 hours in 25 ℃.
The comparative example 2
75 parts in non-ball-aluminium oxide powder (Japanese A-42-6), 16 parts of bisphenol A type epoxy resins, 1.5 parts of cycloaliphatic epoxy resins, 2.9 parts of n-butyl glycidyl ethers, 3.7 parts of strange scholar's toughner, 0.3 part of γ-An Bingjisanyiyangjiguiwan, 0.3 part of carbon black, 0.3 part of stearate at room temperature stirs, and makes the A component; Kymene 00 and 1: 1 amine curing agent of polyetheramine D-400 weight ratio.A component and amine curing agent mixed by weight 100: 9.8, at room temperature stirred, and measured viscosity; Mixture solidified survey cured article thermal conductivity 48 hours in 25 ℃.Test the performance of Resins, epoxy electron pouring sealant of the present invention by following test experiments.
Test experiments 1: viscosity test
Use rich reining in to fly (Brookfield RV) viscometer, the sample that sample that embodiment 1～6 is made according to GB/T2794-1995 and comparative example 1～2 make carries out viscosity test.
Test experiments 2: thermal conductivity test
Use the TPS 2500S type thermal conductivity measuring apparatus of Hot Disk company, the sample that sample that embodiment 1～6 is made according to ASTM E1530 and comparative example 1～2 make carries out the thermal conductivity test.
The result is as shown in table 1 for the test gained.
Table 1 test gained result
From The above results as can be seen, the Resins, epoxy heat conductive electronic joint sealant with ball-aluminium oxide is filled has higher loading level than non-ball-aluminium oxide, and is little to the influence of viscosity, cured article thermal conductivity height.Low and the high thermal conductivity coefficient of viscosity can satisfy embedding the requirements small and electronic devices and components that thermal value is big, this be the non-ball-aluminium oxide Resins, epoxy heat conductive electronic joint sealant of filling can not accomplish.
The high heat conductive electronic pouring sealant of low viscosity of the present invention is mainly used in the perfusion and the sealing of the small electronic devices and components that need heat conduction and heat radiation, and the mixed viscosity of its pair component is 8000～18000cp, and glue density is 2.1～2.4g/cm
3, thermal conductivity is 1.2～1.8W/mK, thermal expansivity 35ppm/ ℃, and volumetric shrinkage＜0.5%, water-intake rate＜0.1%, bending strength 90～110MPa, ultimate compression strength 100～150MPa, volume specific resistance＞10
15Ω cm; With its embedding temperature sensor, can play that heat conduction, insulation, bonding are fixed, the effect of moistureproof, cold-resistant thermal shocking.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant, it is characterized in that, mixed by 100: 5～12 weight ratio by A component and amine curing agent, described A component is made up of each raw material of following weight ratio: 0.1～0.5 part of 70～85 parts in ball-aluminium oxide powder, 10～20 parts of Resins, epoxy, 2～4 parts of reactive thinners, 2.5～5 parts of toughner and coupling agent.
2. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 1 is characterized in that, described amine curing agent is a kind of or any several mixture in aliphatic amide, modified fatty amine, phenol aldehyde modified amine, polyetheramine or the polymeric amide.
3. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 1 is characterized in that, the median size of described ball-aluminium oxide powder is 5～50 μ m.
4. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 1, it is characterized in that described Resins, epoxy is a kind of or any several mixture in bisphenol A type epoxy resin, bisphenol f type epoxy resin, novolac epoxy, glycidyl amine type epoxy resin, the cycloaliphatic epoxy resin.
5. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 1, it is characterized in that, described reactive thinner is n-butyl glycidyl ether, glycidyl allyl ether, phenyl glycidyl ether or 1, a kind of or any several mixture in the 4-butanediol diglycidyl ether.
6. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 1 is characterized in that, described toughner is carboxyl end of the liquid acrylonitrile-butadiene rubber, hydroxyl terminated butyl nitrile (HTBN) rubber or strange scholar's toughner.
7. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 1 is characterized in that described coupling agent is organo-silicon coupling agent, titanate coupling agent or aluminate coupling agent.
8. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 1, it is characterized in that, described coupling agent is an organo-silicon coupling agent, and described organo-silicon coupling agent is γ-An Bingjisanyiyangjiguiwan, styryl Trimethoxy silane, phenyltrimethoxysila,e.
9. according to each described low viscosity high-thermal-conductivity epoxy resin electron pouring sealant of claim 1 to 8, it is characterized in that, also contain the pigment 0.3 and the wetting dispersing agent 0.1～0.5 of parts by weight in the described A component.
10. low viscosity high-thermal-conductivity epoxy resin electron pouring sealant according to claim 9 is characterized in that described pigment is carbon black, and described Ricinate is a stearate.
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