CN102212269B - Insulative potting composite material with high thermal conductivity and preparation method thereof - Google Patents
Insulative potting composite material with high thermal conductivity and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an insulative potting composite material with high thermal conductivity and a preparation method thereof. The insulative potting composite material is prepared by mixing a component A with a component B at a weight ratio of 1:1 and solidifying at the temperature of 50-150 DEG C for 20-50 minutes. The insulative potting composite material has the advantages that the thermal conductivity reaches 3.5 W/m.K (ASTM D5470, HotDish method) and the electrical insulation property and mechanical properties are excellent. According to the invention, the insulative potting composite material with high thermal conductivity is prepared by using vinyl silicone oil as a base adhesive and hydrogen-containing silicone oil as a solidifying agent, using spherical, flaky, acicular and prismatical heat-conducting fillers to fill, and forming plenty of heat conducting channels by virtue of the reasonable combination of the heat-conducting fillers of different shapes; and the solidified insulative potting composite material has excellent electrical properties and mechanical properties.
Description
Technical field
The present invention relates to a kind of high heat conductive insulating embedding matrix material and preparation method thereof, this matrix material is mainly used in the encapsulation of high-power electronic device.
Background technology
Along with the high speed development of microelectronics integrated technology, packing density improves rapidly, and the operating frequency of electronic component sharply increases, and the heat that is produced also increases thereupon.2 ℃ of the every risings of electronic devices and components temperature, its reliability decrease 10% (Macromolecules, 1996,29 (10): 3376-3383).Therefore, heat radiation becomes influences the electronic devices and components important factor in work-ing life.High heat conductive insulating embedding matrix material can not only provide safe and reliable heat radiation approach for electronic component, and plays insulation, damping, protection against the tide and etch-proof effect.The thermal conducting path that heat conductive filler forms in heat conduction embedding matrix material influences the thermal conductivity of matrix material to a great extent.Kumlutas etc. have studied the matrix material that particulate state, bat wool fill with finite element method thermal conductivity and packing volume than between funtcional relationship (Journal of Thermoplastic Composite Materials; 2006,19 (4): 441-455); Usefulness such as Sanada are piled up simulation and finite element method has been inferred relation (Composites Part A:Applied Science and Manufacturing, 2009,40 (6-7): 724-730) between superpolymer effective thermal conductivity and the microtexture.
Chinese patent CN101418123A application discloses a kind of liquid embedding composition of bi-component addition type Zylox; The said composition environmentally safe; Stable performance is not ftractureed at low temperatures, and can play protection against the tide, dustproof, protection against corrosion, effect such as shockproof; Thermal conductivity reaches 0.4W/mK, can not satisfy the heat radiation requirement of large power, electrically sub-element.Chinese patent CN101054507A application discloses a kind of high heat conduction organosilicon filling and sealing gum; This joint sealant cured article has good mechanical performance and electric property, high-low temperature resistant, radiation hardness; Thermal conductivity can reach 1.1 W/mK, still can not satisfy the heat radiation requirement of large power, electrically sub-element.
Summary of the invention
The objective of the invention is deficiency, a kind of high heat conductive insulating embedding matrix material is provided to prior art.As basic glue, containing hydrogen silicone oil is as solidifying agent with vinyl silicone oil in the present invention, adopts the heat conductive filler of patterns such as spherical, sheet, needle-like, column to fill; Reasonably combined through the different-shape heat conductive filler makes that the different-shape heat conductive filler is tightly packed, forms a large amount of thermal conducting path, and preparation has the embedding matrix material of high thermal conductivity coefficient, and cured article has good electric property and mechanical property.
The present invention realizes that through following technical scheme high heat conductive insulating embedding matrix material comprises A component and B component.
A components in mass portion meter is mixed by following component: 100 parts of vinyl silicone oils, 50 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 50 ~ 200 parts of column heat conductive fillers, 2 ~ 10 parts of catalyzer;
B components in mass portion meter is mixed by following component: 100 parts of vinyl silicone oils, 50 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 50 ~ 200 parts of column heat conductive fillers, 2 ~ 10 parts in solidifying agent.
A component and the B component formula more optimized are respectively:
A components in mass portion meter is mixed by following component: 100 parts of vinyl silicone oils, 200 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 100 ~ 200 parts of column heat conductive fillers, 4 ~ 8 parts of catalyzer;
B components in mass portion meter is mixed by following component:
100 parts of vinyl silicone oils, 200 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 100 ~ 200 parts of column heat conductive fillers, 4 ~ 8 parts in solidifying agent.
During use, after A component and B component mixed by mass ratio 1:1,20 ~ 50min was heating and curing under 50 ~ 150 ℃.
High heat conductive insulating embedding matrix material of the present invention, its vinyl silicone oil is a straight chain type, contents of ethylene 0.5 ~ 2.5%wt; Hydrogen content 0.1～the 1.5%wt of solidifying agent containing hydrogen silicone oil; Catalyzer is a Platinic chloride.
High heat conductive insulating embedding matrix material of the present invention, its spherical heat conductive filler are the spherical Al of particle diameter 1 ~ 30 μ m
2O
3, AlN.
High heat conductive insulating embedding matrix material of the present invention, its sheet heat conductive filler is the Al of particle diameter 5 ~ 50 μ m
2O
3, AlN, BN.
High heat conductive insulating embedding matrix material of the present invention, its needle-like heat conductive filler are SiC, the ZnO of length-to-diameter ratio (being length-to-diameter, as follows) 20 ~ 100, diameter 0.1 ~ 1 μ m.
High heat conductive insulating embedding matrix material of the present invention, its column heat conductive filler are AlN, BN, the ZnO of length-to-diameter ratio 1 ~ 30, diameter 0.5 ~ 5 μ m.
Another object of the present invention provides the method for preparing heat conductive insulating embedding matrix material.This method is to use double planetary mixer; 100 parts of vinyl silicone oils and 2 ~ 10 parts of catalyzer are added in the feed inlet barrel; Open and stir, with 50 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 50 ~ 200 parts of column heat conductive fillers, add in the feed inlet barrel one by one then in batches; Continue to stir 20 ~ 100min, make the A component; 100 parts of vinyl silicone oils and 2 ~ 10 parts of solidifying agent are added in the feed inlet barrel; Open and stir; Then with 0 ~ 100 part of 0 ~ 100 part of 50 ~ 300 parts of spherical heat conductive fillers, needle-like heat conductive filler, sheet heat conductive filler, 50 ~ 200 parts of the column heat conductive fillers of drying treatment; Add one by one in the feed inlet barrel in batches, continue to stir 20 ~ 100min, make the B component.
Compare with currently available products, beneficial effect of the present invention is:
Prepared the high heat conductive insulating embedding matrix material of thermal conductivity up to 3.5 W/mK (ASTM D 5470, Hot Disk method), the heat radiation for the large power, electrically sub-element provides assurance.In addition, embedding matrix material viscosity 10000 ~ 50000mPas, free settling is not easy to operate, and row's bubble is easy, automatically levelling.After the curing, density 2.0 ~ 3.5g/cm
3, volume specific resistance 10
13~ 10
15Ω cm, dielectric strength 13 ~ 18kV/mm, tensile strength 1.5 ~ 5.0MPa can satisfy the embedding requirement of large power, electrically sub-element.
Embodiment
Use double planetary mixer, preparation A component and B component.
Embodiment 1
Take by weighing 100 parts of vinyl silicone oils by mass parts, 6 parts of chloroplatinic acid catalysts are put in double planetary mixer and mix 10 min.Slowly add filler: 200 part of 5 spherical Al of μ m in batches
2O
3, 200 parts of diameter 0.5 μ m column AlN (length-to-diameter ratio is 10), 100 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), mix 60 min, make the A component.Take by weighing 100 parts of vinyl silicone oils, 6 parts of containing hydrogen silicone oils are put in double planetary mixer and mix 10 min.Slowly add filler: 200 part of 5 spherical Al of μ m through drying treatment in batches
2O
3, 200 parts of diameter 0.5 μ m column AlN (length-to-diameter ratio is 10), 100 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), mix 60 min, make the B component.A component and B component are mixed by mass ratio 1:1, and the gained mixture viscosity is 28000 mPas, is put in 120 ℃ and solidifies 40min.Solidified sample thermal conductivity 2.5W/mK (ASTM D 5470, Hot Disk method), volume specific resistance 10
14Ω cm, dielectric strength 14.5 kV/m, tensile strength 2.6 MPa.
Embodiment 2
Take by weighing 100 parts of vinyl silicone oils by mass parts, 6 parts of chloroplatinic acid catalysts are put in double planetary mixer and mix 10 min.Slowly add filler: 200 part of 5 spherical Al of μ m in batches
2O
3, 200 parts of diameter 0.5 μ m column AlN (length-to-diameter ratio is 10), 100 parts of diameter 10 μ m sheet BN, mix 60 min, make the A component.Take by weighing 100 parts of vinyl silicone oils, 6 parts of containing hydrogen silicone oils are put in double planetary mixer and mix 10 min.Slowly add filler: 200 part of 5 spherical Al of μ m through drying treatment in batches
2O
3, 200 parts of diameter 0.5 μ m column AlN (length-to-diameter ratio is 10), 100 parts of diameter 10 μ m sheet BN, mix 60 min, make the B component.A component and B component are mixed by mass ratio 1:1, and the gained mixture viscosity is 25000 mPas, is put in 120 ℃ and solidifies 40min.Solidified sample thermal conductivity 2.8 W/mK (ASTM D 5470, Hot Disk method), volume specific resistance 10
14Ω cm, dielectric strength 13.8 kV/m, tensile strength 2.9 MPa.
Embodiment 3
Take by weighing 100 parts of vinyl silicone oils by mass parts, 6 parts of chloroplatinic acid catalysts are put in double planetary mixer and mix 10 min.Slowly add filler: 300 part of 5 spherical Al of μ m in batches
2O
3, 200 parts of diameter 0.5 μ m column AlN (length-to-diameter ratio is 10), 50 parts of diameter 10 μ m sheet BN, 50 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), mix 60 min, make the A component.Take by weighing 100 parts of vinyl silicone oils, 6 parts of containing hydrogen silicone oils are put in double planetary mixer and mix 10 min.Slowly add filler: 300 part of 5 spherical Al of μ m through drying treatment in batches
2O
3, 200 parts of diameter 0.5 μ m column AlN (length-to-diameter ratio is 10), 50 parts of diameter 10 μ m sheet BN, 50 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), mix 60 min, make the B component.A component and B component are mixed by mass ratio 1:1, and the gained mixture viscosity is 38000 mPas, is put in 110 ℃ and solidifies 50min.Solidified sample thermal conductivity 3.3W/mK (ASTM D 5470, Hot Disk method), volume specific resistance 10
14Ω cm, dielectric strength 16.3 kV/m, tensile strength 3.6 MPa.
Embodiment 4
Take by weighing 100 parts of vinyl silicone oils by mass parts, 6 parts of chloroplatinic acid catalysts are put in double planetary mixer and mix 10 min.Slowly add filler: 300 part of 10 spherical AlN of μ m, 200 parts of diameter 0.5 μ m column ZnO (length-to-diameter ratio is 10), 50 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), 50 parts of diameter 10 μ m sheet Al in batches
2O
3, mix 60 min, make the A component.Take by weighing 100 parts of vinyl silicone oils, 6 parts of containing hydrogen silicone oils are put in double planetary mixer and mix 10 min.Slowly add filler: 300 part of 10 spherical AlN of μ m, 200 parts of diameter 0.5 μ m column ZnO (length-to-diameter ratio is 10), 50 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), 50 parts of diameter 10 μ m sheet Al through drying treatment in batches
2O
3, mix 60 min, make the B component.A component and B component are mixed by mass ratio 1:1, and the gained mixture viscosity is 41000 mPas, is put in 110 ℃ and solidifies 50min.Solidified sample thermal conductivity 3.1W/mK (ASTM D 5470, Hot Disk method), volume specific resistance 10
13Ω cm, dielectric strength 15.3 kV/m, tensile strength 3.9MPa.
Embodiment 5
Take by weighing 100 parts of vinyl silicone oils by mass parts, 6 parts of chloroplatinic acid catalysts are put in double planetary mixer and mix 10 min.Slowly add filler in batches: 300 part of 10 spherical AlN of μ m, 200 parts of diameter 0.5 μ m column ZnO (length-to-diameter ratio is 10), 50 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), 50 parts of diameter 10 μ m sheet BN, mix 60 min, make the A component.Take by weighing 100 parts of vinyl silicone oils, 6 parts of containing hydrogen silicone oils are put in double planetary mixer and mix 10 min.Slowly add filler: 300 part of 10 spherical AlN of μ m, 200 parts of diameter 0.5 μ m column ZnO (length-to-diameter ratio is 10), 50 parts of diameter 0.1 μ m needle-like SiC whiskers (length-to-diameter ratio is 50), 50 parts of diameter 10 μ m sheet BN through drying treatment in batches; Mix 60 min, make the B component.A component and B component are mixed by mass ratio 1:1, and the gained mixture viscosity is 40000 mPas, is put in 110 ℃ and solidifies 50min.Solidified sample thermal conductivity 3.3W/mK (ASTM D 5470, Hot Disk method), volume specific resistance 10
13Ω cm, dielectric strength 15.7kV/m, tensile strength 4.0 MPa.
Embodiment 6
Take by weighing 100 parts of vinyl silicone oils by mass parts,, be put in double planetary mixer and mix 10 min.Slowly add filler: 300 part of 10 spherical AlN of μ m, 200 parts of diameter 0.5 μ m column BN (length-to-diameter ratio is 10), 50 parts of diameter 0.1 μ m needle-like ZnO length-to-diameter ratios are 50 in batches), 50 parts of diameter 10 μ m sheet Al
2O
3, mix 60 min, make the A component.Take by weighing 100 parts of vinyl silicone oils, 6 parts of containing hydrogen silicone oils are put in double planetary mixer and mix 10 min.Slowly add the filler through drying treatment: 300 part of 10 spherical AlN of μ m, 200 parts of diameter 0.5 μ m column BN (length-to-diameter ratio is 10), 50 parts of diameter 0.1 μ m needle-like ZnO length-to-diameter ratios are 50 in batches), 50 parts of diameter 10 μ m sheet Al
2O
3, mix 60 min, make the B component.A component and B component are mixed by mass ratio 1:1, and the gained mixture viscosity is 44000 mPas, is put in 110 ℃ and solidifies 50min.Solidified sample thermal conductivity 3.5W/mK (ASTM D 5470, Hot Disk method), volume specific resistance 10
14Ω cm, dielectric strength 17.8 kV/m, tensile strength 4.5 MPa.
Claims (5)
1. high heat conductive insulating embedding matrix material; Comprise A component and B component; It is characterized in that: said A components in mass portion meter is mixed by following component: 100 parts of vinyl silicone oils, 50 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 50 ~ 200 parts of column heat conductive fillers, 2 ~ 10 parts of catalyzer; Said B components in mass portion meter is mixed by following component: 100 parts of vinyl silicone oils, 50 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 50 ~ 200 parts of column heat conductive fillers, 2 ~ 10 parts in solidifying agent; Said spherical heat conductive filler is spherical Al
2O
3Or spherical AlN, said needle-like heat conductive filler is needle-like SiC whisker or needle-like ZnO, said sheet heat conductive filler is sheet BN or sheet Al
2O
3Or sheet AlN, the column heat conductive filler is column AlN or column ZnO or column BN; Wherein spherical heat conductive filler is the spherical Al of particle diameter 1 ~ 30 μ m
2O
3Or spherical AlN; The sheet heat conductive filler is the sheet Al of particle diameter 5 ~ 50 μ m
2O
3, sheet AlN or sheet BN; The needle-like heat conductive filler is needle-like SiC whisker or the needle-like ZnO of length-to-diameter ratio 20 ~ 100, diameter 0.1 ~ 1 μ m; Wherein the column heat conductive filler is column AlN, column BN or the column ZnO of length-to-diameter ratio 1 ~ 30, diameter 0.5 ~ 5 μ m.
2. want 1 described high heat conductive insulating embedding matrix material according to right; It is characterized in that: said A component and B component formula are respectively: A components in mass portion meter is mixed by following component: 100 parts of vinyl silicone oils, 200 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 100 ~ 200 parts of column heat conductive fillers, 4 ~ 8 parts of catalyzer; B components in mass portion meter is mixed by following component: 100 parts of vinyl silicone oils, 200 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 100 ~ 200 parts of column heat conductive fillers, 4 ~ 8 parts in solidifying agent.
3. high heat conductive insulating embedding matrix material according to claim 1 and 2 is characterized in that: after A component and B component mixed by mass ratio 1:1 during use, 20 ~ 50min was heating and curing under 50 ~ 150 ℃.
4. high heat conductive insulating embedding matrix material according to claim 1 and 2, therein ethylene base silicone oil is straight chain type, contents of ethylene 0.5 ~ 2.5%wt; Solidifying agent is a containing hydrogen silicone oil, hydrogen content 0.1～1.5%wt; Catalyzer is a Platinic chloride.
5. the method for preparing the described high heat conductive insulating embedding of claim 1 matrix material; It is characterized in that: use mixing tank, 100 parts of vinyl silicone oils and 2 ~ 10 parts of catalyzer are added in the feed inlet barrel, open and stir; Then with 50 ~ 300 parts of spherical heat conductive fillers, 0 ~ 100 part of needle-like heat conductive filler, 0 ~ 100 part of sheet heat conductive filler, 50 ~ 200 parts of column heat conductive fillers; Add one by one in the feed inlet barrel in batches, continue to stir 20 ~ 100min, make the A component; 100 parts of vinyl silicone oils and 2 ~ 10 parts of solidifying agent are added in the feed inlet barrel; Open and stir; Then with 0 ~ 100 part of 0 ~ 100 part of 50 ~ 300 parts of spherical heat conductive fillers, needle-like heat conductive filler, sheet heat conductive filler, 50 ~ 200 parts of the column heat conductive fillers of drying treatment; Add one by one in the feed inlet barrel in batches, continue to stir 20 ~ 100min, make the B component.
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| CN104151825A (en) * | 2014-08-06 | 2014-11-19 | 西南科技大学 | Thermally-conductive insulating polysulfone composite material and preparation method thereof |
| EP3150672B1 (en) * | 2015-10-02 | 2018-05-09 | Shin-Etsu Chemical Co., Ltd. | Thermal conductive silicone composition and semiconductor device |
| CN105315670A (en) * | 2015-11-24 | 2016-02-10 | 苏州盖德精细材料有限公司 | High-heat-conductivity electronic encapsulation composite and preparing method thereof |
| CN108841179A (en) * | 2018-05-18 | 2018-11-20 | 深圳市金菱通达电子有限公司 | A kind of liquid heat conductive formed body for electric vehicle component |
| CN109233287A (en) * | 2018-08-09 | 2019-01-18 | 张剑 | A kind of heat-conducting type electrically insulating silicone rubber gasket |
| JP7292941B2 (en) * | 2019-04-19 | 2023-06-19 | 株式会社トクヤマ | Aluminum nitride composite filler |
| CN110183853A (en) * | 2019-05-31 | 2019-08-30 | 宋远周 | A kind of fire-retardant high heat conduction organosilicon encapsulating composite material and preparation method |
| CN112608708A (en) * | 2021-01-05 | 2021-04-06 | 佛山市极威新材料有限公司 | Polyurethane heat-conducting insulating adhesive and preparation method thereof |
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