CN104178076B - A kind of heat conductive insulating epoxy resin embedding adhesive and preparation method - Google Patents
A kind of heat conductive insulating epoxy resin embedding adhesive and preparation method Download PDFInfo
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- CN104178076B CN104178076B CN201410457717.9A CN201410457717A CN104178076B CN 104178076 B CN104178076 B CN 104178076B CN 201410457717 A CN201410457717 A CN 201410457717A CN 104178076 B CN104178076 B CN 104178076B
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Abstract
The invention discloses a kind of heat conductive insulating epoxy resin embedding adhesive, being made up of epoxy resin, firming agent, toughener, diluent, filler, accelerator and defoamer, the weight ratio of each composition is: component A: epoxy resin 100 parts, diluent 10～30 parts, filler 5～15 parts, defoamer, 0.5～1 part, coupling agent 3～5 parts；B component: 78～145 parts of firming agent, toughener 10～40 parts, filler 5～10 parts, accelerator 0.1～3 part, defoamer 0.5～1 part；A/B weight ratio 1: 1。Described toughener is epoxy hydroxyl terminated butadiene acrylonitrile copolymer；Filler is the composite powder of varigrained nano-silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride, high sphericity nano aluminium oxide and nano-silicon nitride composition, its particle mean size 40～60nm。This casting glue not only has a good heat conductivity, and good insulation preformance。
Description
Technical field
The present invention relates to adhesive preparing technical field, particularly to heat conductive insulating epoxy resin embedding adhesive and preparation method。
Background technology
Epoxy resin embedding adhesive is the thermosetting polymer composite that a class has the performance such as good bonding, corrosion-resistant, electric insulation, high intensity, it has also become electronics, electrically, machine-building, chemical anticorrosion, Aero-Space, Shipping and other indispensable basic materials of many industrial circles。
Along with microelectronics and integrated circuit develop to high speed, high density, miniaturization, lightweight direction, electronic devices and components, logic circuit volume are constantly compressed, heat produced by electronic equipment unit volume sharply increases, thus heat conductivility will affect the life and reliability of electronic devices and components, electronic equipment。For guaranteeing the properly functioning of electronic devices and components, it is necessary to material possesses high heat-sinking capability, to ensure the quick transmission of heat。And traditional epoxy resin is the non-conductor of heat, heat conductivity is 0.2W m-1·K-1Left and right, is difficult to meet the timely cooling requirements of electronic devices and components；The service efficiency of electronic component and life-span are also had material impact by insulating properties, and good electrical insulating property can improve the service efficiency of electrical equipment, increases the service life。Therefore, one of heat conductivility emphasis becoming research at present how being effectively improved epoxy resin under the premise ensureing insulating properties。
Improving casting glue heat conductivity and mainly have two kinds of approach, a kind of approach is the polymer adding and having heat conductivity, but owing to synthesis thermal conductive polymer cost is high, the tactical rule of high-molecular organic material is poor, and heat conductivility is also not ideal, thus is rarely employed；Another kind of approach is by adding high heat filling, and at present, filling heat filling is widely used method。The heat filling that existing epoxy resin embedding adhesive adds is generally metal (copper, aluminum, ferrum etc.) powder and inorganic filler (graphite, white carbon black, inorganic oxide, nitride etc.)。Although metal material heat conductivity is higher, it is possible to as the filler of heat-conductivity polymer composite, but owing to metal material has electric conductivity, manufactured goods poor insulativity, easily puncture, affect efficiency and the life-span of electronic component。Silicon powder heat conductivity conventional in inorganic heat filling is relatively low, adopts the heat conductivity of the potting compound of silicon powder filling to be relatively low, less than 0.6W/ (m K), is unfavorable for the heat radiation of electric elements。The heat conductivity of the inorganic fillers such as aspherical aluminium oxide, boron nitride, aluminium nitride is higher, but granularity relatively big (general 400 orders), poor with resin affinity, skewness, it is easy to precipitation。
Summary of the invention
First technical problem that the invention solves the problems that is to provide a kind of heat conductive insulating epoxy resin embedding adhesive, and this casting glue not only has a good heat conductivity, and good insulation preformance。
The preparation method that second technical problem that the invention solves the problems that is to provide this heat conductive insulating epoxy resin embedding adhesive a kind of。
Heat conductive insulating epoxy resin embedding adhesive of the present invention, is made up of epoxy resin, firming agent, toughener, diluent, filler, accelerator and defoamer, and the weight ratio of each composition is as follows:
Component A:
B component:
A/B weight ratio 1: 1。
Be suitable in the bisphenol A type epoxy resin of the preferred liquid of epoxy resin of the present invention, bisphenol f type epoxy resin, cycloaliphatic epoxy resin, aliphatic epoxy resin etc. one or more, such as E-51, E-44, E-42, E-54 or EP828 etc.；The firming agent being suitable for is such as liquid anhydride, in hexahydrophthalic anhydride, methylnadic anhydride, hydrogenating methyl carbic anhydride any one or multiple；The toughener such as endurable active toughener being suitable for, its molecule segment is the epoxy hydroxyl terminated butadiene acrylonitrile copolymer with epoxy radicals, cyano group, it is preferable that molecular weight is 1800～2000, and epoxide number is 0.6～1mmol/g, and acrylonitrile content is 3%～7%；Be suitable for diluent be reactive diluent, in polypropylene glycol diglycidyl, diglycidyl ether aniline, glycerin triglycidyl ether any one or multiple；The filler being suitable for is the composite powder of varigrained nano-silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride, high sphericity nano aluminium oxide and nano-silicon nitride composition, its particle mean size 40～60nm, is not specially limited composite powder constituent content；Be suitable for accelerator be liquid imidazole class accelerator, in 2-ethyl-4-methylimidazole, 1 benzyl 2 methyl imidazole, 1-cyanoethyl-2-ethyl-4-methylimidazole any one or multiple；Be suitable for coupling agent be silane coupler, in γ aminopropyltriethoxy silane, gamma-amino propyl trimethoxy silicane, γ-glycidoxy trimethoxy silane any one or multiple；The defoamer such as tributyl phosphate etc. being suitable for。
The method preparing heat conductive insulating epoxy resin embedding adhesive of the present invention, comprises the following steps:
(1) prepared by component A:
Epoxy resin, diluent, filler, defoamer, coupling agent are added in stirred tank, is sufficiently stirred for mix homogeneously in a heated condition, obtains component A；
(2) prepared by B component:
Firming agent, toughener, filler, accelerator, defoamer are added in stirred tank, is sufficiently stirred for mix homogeneously in a heated condition, obtains B component；
(3) component A and B component being joined in mix and blend still by weight 1: 1, be warming up to 85 DEG C, vacuum, more than 0.095MPa, continues 30min, evacuation elimination bubble；
(4) adding mixture in mould, 90 DEG C solidify 1h, and 110 DEG C solidify 2h, and 180 DEG C solidify 3h, are naturally down to room temperature。
The endurable active toughener epoxy hydroxyl terminated butadiene acrylonitrile copolymer molecule segment that present invention introduces is with epoxy radicals, cyano group and hydroxyl, good with liquid bisphenol A epoxy resin compatible and viscosity is low, improve the fragility of epoxy resin cured product and eliminate crack performance, epoxy resin embedding adhesive impact resistance and insulating properties can be significantly improved；The filler that present invention introduces, it is made up of the multiple super-high heat-conductive filler of different-grain diameter, good with resin affinity, it is evenly distributed, not easily precipitates, can make to be formed between filler maximum degree of piling up, make the heat conduction network that epoxy pouring sealant System forming is good to the full extent, thus reaching effective conduction of heat and insulation, it is thus achieved that high heat conductive insulating system, and water absorption rate is low。Product of the present invention can be widely applied to electronics, electrically, machine-building, chemical anticorrosion, Aero-Space, Shipping and other many industrial circles, have a extensive future。The preparation method of heat conductive insulating epoxy resin embedding adhesive of the present invention, filler is added in A, B component respectively, and dispersion effect is good, and the casting glue heat conductive insulating excellent performance of preparation, technique is simple。
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described。The following stated number is weight portion。
Each embodiment heat conductive insulating epoxy resin embedding adhesive is prepared by the following method, and gained casting glue performance is in Table 1。
(1) prepared by component A:
Being added in stirred tank by each composition, then heated and stirred still is to 85 DEG C, is sufficiently stirred for mix homogeneously in a heated condition, obtains component A；
(2) prepared by B component:
Being added in stirred tank by each composition, then heated and stirred still 85 DEG C, are sufficiently stirred for mix homogeneously, obtain B component；
(3) component A and B component being joined in mix and blend still by weight 1: 1, be warming up to 85 DEG C, vacuum, more than 0.095MPa, continues 30min, evacuation elimination bubble；
(4) adding mixture in mould, 90 DEG C solidify 1h, and 110 DEG C solidify 2h, and 180 DEG C solidify 3h, are naturally down to room temperature。
Filler is the composite powder of 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 component composition, its particle mean size 50nm。
EP828 is Holland's shell Products。
Embodiment 1
Component A:
B component:
Embodiment 2:
Component A:
B component:
Embodiment 3:
Component A:
B component:
Comparative example
The each embodiment casting glue performance of table 1
| Project | Comparative example | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Heat conductivity, W/ (m k) | 0.35 | 4.31 | 4.46 | 5.15 |
| Specific insulation, Ω cm | 2.57×1015 | 3.24×1016 | 4.18×1016 | 5.18×1016 |
| Impact strength, kJ/m2 | 1.7 | 18.80 | 21.03 | 25.62 |
| Water absorption rate, % (in 20 DEG C of encroached waters 50 days) | 0.28 | 0.30 | 0.32 | 0.35 |
Claims (9)
1. a heat conductive insulating epoxy resin embedding adhesive, is made up of epoxy resin, firming agent, toughener, diluent, filler, accelerator, coupling agent and defoamer, and the weight ratio of each composition is as follows:
Component A:
B component:
Described toughener is epoxy hydroxyl terminated butadiene acrylonitrile copolymer；Filler is the composite powder of varigrained nano-silicon nitride magnesium, nanometer silicon carbide, nano aluminum nitride, nm-class boron nitride, high sphericity nano aluminium oxide and nano-silicon nitride composition, its particle mean size 40～60nm。
2. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described epoxy resin is one or more in the bisphenol A type epoxy resin of liquid, bisphenol f type epoxy resin, cycloaliphatic epoxy resin, aliphatic epoxy resin。
3. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described firming agent in hexahydrophthalic anhydride, methylnadic anhydride, the hydrogenating methyl carbic anhydride any one or multiple。
4. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described toughener molecular weight is 1800～2000, and its epoxide number 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 diluent in polypropylene glycol diglycidyl ether, diglycidyl ether aniline, the glycerin triglycidyl ether any one or multiple。
6. heat conductive insulating epoxy resin embedding adhesive according to claim 1, described accelerator in 2-ethyl-4-methylimidazole, 1 benzyl 2 methyl imidazole, the 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 in γ aminopropyltriethoxy silane, gamma-amino propyl trimethoxy silicane, the 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. the method preparing the described heat conductive insulating epoxy resin embedding adhesive of one of claim 1～8, comprises the following steps:
(1) prepared by component A
Epoxy resin, diluent, filler, defoamer, coupling agent are added in stirred tank, is sufficiently stirred for mix homogeneously in a heated condition, obtains component A；
(2) prepared by B component
Firming agent, toughener, filler, accelerator, defoamer are added in stirred tank, is sufficiently stirred for mix homogeneously in a heated condition, obtains B component；
(3) component A and B component being joined in mix and blend still by weight 1: 1, be warming up to 85 DEG C, vacuum, more than 0.095MPa, continues 30min, evacuation elimination bubble；
(4) adding mixture in mould, 90 DEG C solidify 1h, and 110 DEG C solidify 2h, and 180 DEG C solidify 3h, are naturally down to room temperature。
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Family Cites Families (3)
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| CN101508825B (en) * | 2009-03-30 | 2011-04-27 | 汕头市骏码凯撒有限公司 | Epoxy resin embedding glue and method for producing the same |
| MX2014005313A (en) * | 2011-11-01 | 2014-10-06 | Dow Global Technologies Llc | Liquid epoxy resin formulations. |
| CN102863936B (en) * | 2012-10-09 | 2014-07-02 | 株洲时代新材料科技股份有限公司 | Heating solidification type dual-component epoxy pouring sealant and preparation method thereof |
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