CN104877612A - Heat-conducting insulating adhesive and preparation method thereof - Google Patents
Heat-conducting insulating adhesive and preparation method thereof Download PDFInfo
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- CN104877612A CN104877612A CN201510336601.4A CN201510336601A CN104877612A CN 104877612 A CN104877612 A CN 104877612A CN 201510336601 A CN201510336601 A CN 201510336601A CN 104877612 A CN104877612 A CN 104877612A
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- 230000001070 adhesive effect Effects 0.000 title claims abstract description 44
- 239000000853 adhesive Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 37
- 239000003822 epoxy resin Substances 0.000 claims abstract description 37
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 37
- 239000003921 oil Substances 0.000 claims abstract description 25
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 100
- 239000011231 conductive filler Substances 0.000 claims description 70
- -1 amido silicon Chemical compound 0.000 claims description 60
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 40
- 238000006243 chemical reaction Methods 0.000 claims description 40
- 238000009413 insulation Methods 0.000 claims description 40
- 239000004593 Epoxy Substances 0.000 claims description 39
- 238000004381 surface treatment Methods 0.000 claims description 39
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 30
- 229910052710 silicon Inorganic materials 0.000 claims description 24
- 239000010703 silicon Substances 0.000 claims description 24
- 239000002245 particle Substances 0.000 claims description 22
- 238000001291 vacuum drying Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- 229960000583 acetic acid Drugs 0.000 claims description 20
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 20
- 239000012362 glacial acetic acid Substances 0.000 claims description 20
- 230000007062 hydrolysis Effects 0.000 claims description 20
- 238000006460 hydrolysis reaction Methods 0.000 claims description 20
- 230000007935 neutral effect Effects 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 18
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 16
- 150000001412 amines Chemical class 0.000 claims description 16
- 239000004917 carbon fiber Substances 0.000 claims description 16
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 16
- 229910052582 BN Inorganic materials 0.000 claims description 15
- PZNSFCLAULLKQX-UHFFFAOYSA-N Boron nitride Chemical compound N#B PZNSFCLAULLKQX-UHFFFAOYSA-N 0.000 claims description 15
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 claims description 15
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- SJECZPVISLOESU-UHFFFAOYSA-N 3-trimethoxysilylpropan-1-amine Chemical compound CO[Si](OC)(OC)CCCN SJECZPVISLOESU-UHFFFAOYSA-N 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000377 silicon dioxide Substances 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910017083 AlN Inorganic materials 0.000 claims description 4
- PIGFYZPCRLYGLF-UHFFFAOYSA-N Aluminum nitride Chemical compound [Al]#N PIGFYZPCRLYGLF-UHFFFAOYSA-N 0.000 claims description 4
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 claims description 4
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 3
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 3
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract 2
- 238000004026 adhesive bonding Methods 0.000 abstract 1
- OBFQBDOLCADBTP-UHFFFAOYSA-N aminosilicon Chemical compound [Si]N OBFQBDOLCADBTP-UHFFFAOYSA-N 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000010292 electrical insulation Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000007822 coupling agent Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention discloses a heat-conducting insulating adhesive and a preparation method thereof. The heat-conducting insulating adhesive is composed of a component A and a component B; the component A is prepared from such raw materials in percentage by mass as 5%-20% of amino silicon oil, 2%-8% of silane coupling agent, 40%-70% of epoxy resin and 20%-40% of heat-conducting filler, and the total percentage of the raw materials is 100%; the component b is a curing agent; the mass ratio of the component A to the component B is (1-4) to 1. The heat-conducting insulating adhesive has relatively long working life and relatively high heat conductivity coefficient and volume resistivity, and is especially suitable for insulating heat-conducting packaging and gluing in the fields of electronics and electrical, and the like.
Description
Technical field
The present invention relates to a kind of tackiness agent and preparation method thereof, refer in particular to and a kind of there is tackiness agent of heat conduction and insulating property and preparation method thereof.
Background technology
Along with the continuous renewal of integrated technology in electronic industry and package technique develops, the volume trend miniaturization of electronic devices and components and logical circuit, operating frequency but sharply increases, the now heat run-up that produces of electronics, at environment for use temperature, for ensureing the normal work of electronic devices and components long-time high reliability, more and more higher requirement is proposed for the heat conduction of tackiness agent, the insulating property playing cohesive action.
Epoxy resin is the macromolecule matrix being commonly used for Heat Conductive Insulation Adhesive, it has excellent physical and mechanical properties, electrical insulation capability and adhesive property, simultaneously its solidification value wide ranges, and cross-linking density is easy to control, solidification process does not produce small molecule by-product, and thus shrinking percentage is low.And while epoxy resin exists many excellent properties, still have its weak point, rear internal stress is large, matter is crisp as solidified, and thermotolerance, shock-resistance and humidity resistance are poor, greatly limit its application in high-tech sector.
Simultaneously, resin thermal conductivity is low, significantly improve the thermal conductivity of tackiness agent, main path fills heat conduction component exactly in polymkeric substance, as patent CN 102719210 A describes a kind of super low temperature insulation heat conduction sizing agent, heat conductive filler is made up of metal powder and nonmetallic heat conductive powder, though the Heat Conductive Insulation Adhesive of preparation has good electrical insulating property, thermal conductivity is no more than 1W/mk.Though existing method can prepare high heat conductive material, material is on-insulated.
Therefore, how effectively to improve the toughness of epoxy resin, improve the heat conductive insulating performance of tackiness agent simultaneously, this Heat Conductive Insulation Adhesive for research, exploitation superperformance is very important.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, there is provided a kind of thermal conductivity high, there is the Heat Conductive Insulation Adhesive of excellent electrical insulation capability simultaneously, this Heat Conductive Insulation Adhesive is made up of component A and B component, described component A by mass percentage be 5% ~ 20% amido silicon oil, the silane coupling agent of 2% ~ 8%, the epoxy resin of 40% ~ 70% and 20% ~ 40% heat conductive filler form, the summation of above-mentioned composition is 100%; B component is solidifying agent.
Described component A and the mass ratio of B component are 1 ~ 4: 1.
Described amido silicon oil is containing amino polydimethylsiloxane in side chain or end group, and amino value is 0.5 ~ 0.8g/100g, and its structure meets following general formula:
Wherein R
1for methyl or hydroxyl, R
2for ammonia alkyl or R
1for ammonia alkyl, R
2for methyl.
Described silane coupling agent is one or more mixing in 3-aminopropyl triethoxysilane, 3-glycydoxy Trimethoxy silane, 3-aminopropyl trimethoxysilane, aminophenyl triethoxy silica alkane.
Described epoxy resin is one or both mixing in bisphenol A type epoxy resin, glycidyl ester type epoxy resin.
Described heat conductive filler is one or more mixing in boron nitride, aluminium nitride, silicon carbide, aluminum oxide, carbon fiber, and the particle diameter of described heat conductive filler is 0.05 μm ~ 200 μm.
Described solidifying agent is one or both mixing in modified amine curing agent, modification aliphatic cyclic amine solidifying agent.
Another object of the present invention is to provide a kind of preparation method of Heat Conductive Insulation Adhesive, it is characterized in that, comprises the following steps:
(1) 50ml ~ 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 4 ~ 6, the heat conductive filler of 20% ~ 40% and the coupling agent of 0 ~ 1% that particle diameter is 0.05 μm ~ 200 μm is added under stirring, and regulate temperature 50 C ~ 60 DEG C, after stirring 20min ~ 30min, put into ultrasonic cleaner ultrasonic disperse 40min ~ 50min, and constant temperature hydrolysis 1h ~ 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C ~ 60 DEG C dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil of 5% ~ 20% is placed in beaker with 2% ~ 8% silane coupling agent by mixing, stirring reaction 4h ~ 6h at temperature is 60 DEG C ~ 80 DEG C, the epoxy resin of 40% ~ 70% is added again in beaker, stirring reaction 2h ~ 2.5h, obtain modified epoxy, join in modified epoxy by the heat conductive filler after above-mentioned surface treatment, stirring at room temperature 20min ~ 30min, obtains component A.
(3) ratio being 1 ~ 4: 1 in mass ratio by component A and B component coordinates, and obtains Heat Conductive Insulation Adhesive.
Excellent effect of the present invention is:
Adopt A, B two-pack composition Heat Conductive Insulation Adhesive, substantially prolongs working life, adopt amino-modified silicone epoxy resin simultaneously, improve the shortcomings such as conventional thermal conductive glue poor toughness, poor heat resistance, add surface-treated heat conductive filler, the Heat Conductive Insulation Adhesive of preparation has excellent electrical insulating property and high thermal conductivity simultaneously.Heat Conductive Insulation Adhesive preparation technology of the present invention is simple, and cost is low, and using value is high.
Embodiment
Below in conjunction with embodiment, the invention will be further described, but embodiments of the present invention are not limited thereto.
Embodiment 1
(1) 50ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 4, add boron nitride 8g and 3-aminopropyl triethoxysilane 0.15g that particle diameter is 50nm under stirring, and regulate temperature 50 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl triethoxysilane 2g is taken in beaker, 24g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 12g of getting 35g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 2
(1) 50ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, add under stirring particle diameter be 50nm aluminium nitride 8g and 3-aminopropyl triethoxysilane 0.2g, and regulate temperature 50 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl triethoxysilane 2g is taken in beaker, 24g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 12g of getting 36g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 3
(1) 50ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 6, add silicon carbide 8g and 3-aminopropyl triethoxysilane 0.25g that particle diameter is 50nm under stirring, and regulate temperature 50 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 45min, and constant temperature hydrolysis 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl triethoxysilane 2g is taken in beaker, 24g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is put into the epoxy resin of modification, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 12g of getting 36g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 4
(1) 50ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, add aluminum oxide 8g and 3-aminopropyl triethoxysilane 0.25g that particle diameter is 50nm under stirring, and regulate temperature 60 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl triethoxysilane 2g is taken in beaker, 24g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 12g of getting 37g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 5
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 8g and carbon fiber 2g and 3-aminopropyl triethoxysilane 0.3g that particle diameter is 50nm is added under stirring, and regulate temperature 60 C, after stirring 30min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 50 DEG C in dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl triethoxysilane 1g is taken in beaker, 20g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 15g of getting 33g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 6
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 6g, carbon fiber 2g and ball-aluminium oxide 2g and 3-aminopropyl triethoxysilane 0.3g that particle diameter is 50nm is added under stirring, and regulate temperature 60 C, after stirring 30min, put into ultrasonic cleaner ultrasonic disperse 50min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 50 DEG C in dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 3g, 3-aminopropyl triethoxysilane 1g is taken in beaker, 21g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 15g of getting 33g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 7
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 6, ball-aluminium oxide 6g, silicon carbide 2g and carbon fiber 2g and 3-aminopropyl triethoxysilane 0.35g that particle diameter is 50 μm is added under stirring, and regulate temperature 50 C, after stirring 25min, put into ultrasonic cleaner ultrasonic disperse 45min, and constant temperature hydrolysis 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 50 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl triethoxysilane 1g is taken in beaker, 20g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 15g of getting 33g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 8
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 6, boron nitride 6g, carbon fiber 2g and 3-glycydoxy Trimethoxy silane 0.25g that particle diameter is 50 μm is added under stirring, and regulate temperature 50 C, after stirring 25min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 45 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 5g, 3-glycydoxy Trimethoxy silane 1g is taken in beaker, 20g glycidyl ester type epoxy resin is added after stirring reaction 4h at temperature is 65 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 16g of getting 32g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 9
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 6, boron nitride 6g, carbon fiber 2g and 3-glycydoxy Trimethoxy silane 0.25g that particle diameter is 100 μm is added under stirring, and regulate temperature 45 C, after stirring 25min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 5g, 3-glycydoxy Trimethoxy silane 2g is taken in beaker, 20g glycidyl ester type epoxy resin is added after stirring reaction 4h at temperature is 70 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 17g of getting 32g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 10
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g, carbon fiber 2g and 3-glycydoxy Trimethoxy silane 0.3g that particle diameter is 100 μm is added under stirring, and regulate temperature 55 DEG C, after stirring 25min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 6g, 3-glycydoxy Trimethoxy silane 1g is taken in beaker, 20g glycidyl ester type epoxy resin is added after stirring reaction 4h at temperature is 65 DEG C, stirring reaction 2.5h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) modified amine curing agent (B component) of the component A and 11g of getting 38g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 11
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g and carbon fiber 2g and 3-aminopropyl trimethoxysilane 0.3g that particle diameter is 50nm is added under stirring, and regulate temperature 50 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C in dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl trimethoxysilane 1g is taken in beaker, 20g glycidyl ester type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 30min, obtains component A.
(3) the modification aliphatic cyclic amine solidifying agent (B component) of the component A and 13g of getting 35g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 12
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g, carbon fiber 2g and 3-aminopropyl trimethoxysilane 0.2g that particle diameter is 50nm is added under stirring, and regulate temperature 60 C, after stirring 30min, put into ultrasonic cleaner ultrasonic disperse 50min, and constant temperature hydrolysis 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C in dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, 3-aminopropyl trimethoxysilane 2g is taken in beaker, 18g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2.5h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) the modification aliphatic cyclic amine solidifying agent (B component) of the component A and 14g of getting 33g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 13
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, the aluminium nitride 8g of particle diameter 100 μm, carbon fiber 2g and aminophenyl triethoxy silica alkane 0.25g is added under stirring, and regulate temperature 60 C, after stirring 30min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C in dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 4g, aminophenyl triethoxy silica alkane 1g is taken in beaker, 19g bisphenol A type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2.5h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) the modification aliphatic cyclic amine solidifying agent (B component) of the component A and 16g of getting 32g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 14
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g and carbon fiber 2g and aminophenyl triethoxy silica alkane 0.15g that particle diameter is 50nm is added under stirring, and regulate temperature 55 DEG C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 5g, aminophenyl triethoxy silica alkane 2g is taken in beaker, 18g glycidyl ester type epoxy resin is added after stirring reaction 4h at temperature is 60 DEG C, stirring reaction 2h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) the modification aliphatic cyclic amine solidifying agent (B component) of the component A and 18g of getting 35g coordinates, and namely obtains Heat Conductive Insulation Adhesive.
Embodiment 15
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g and carbon fiber 2g and 3-glycydoxy Trimethoxy silane 0.1g that particle diameter is 50nm is added under stirring, 3-aminopropyl trimethoxysilane 0.1g, and regulate temperature 50 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain surface-treated heat conductive filler.
(2) amido silicon oil 4g, 3-glycydoxy Trimethoxy silane 1g, 3-aminopropyl trimethoxysilane 1g is taken in beaker, 20g bisphenol A type epoxy resin is added after stirring reaction 4.5h at temperature is 60 DEG C, stirring reaction 2.5h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 30min, obtains component A.
(3) component A of getting 35g coordinates with 10g modified amine curing agent, 10g modification aliphatic cyclic amine solidifying agent (B component), namely obtains Heat Conductive Insulation Adhesive.
Embodiment 16
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g and carbon fiber 2g and 3-glycydoxy Trimethoxy silane 0.1g that particle diameter is 50nm is added under stirring, 3-aminopropyl triethoxysilane 0.15g, and regulate temperature 60 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 50 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 5g, 3-glycydoxy Trimethoxy silane 0.5g, 3-aminopropyl triethoxysilane 0.5g is taken in beaker, 10g bisphenol A type epoxy resin and 10g glycidyl ester type epoxy resin is added after stirring reaction 4.5h at temperature is 60 DEG C, stirring reaction 2.5h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) component A of getting 33g coordinates with 11g modified amine curing agent, 11g modification aliphatic cyclic amine solidifying agent (B component), namely obtains Heat Conductive Insulation Adhesive.
Embodiment 17
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g and carbon fiber 2g and 3-glycydoxy Trimethoxy silane 0.3g that particle diameter is 50nm is added under stirring, and regulate temperature 60 C, after stirring 20min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 5g, 3-glycydoxy Trimethoxy silane 0.5g, aminophenyl triethoxy silica alkane 0.5g is taken in beaker, 10g bisphenol A type epoxy resin and 8g glycidyl ester type epoxy resin is added after stirring reaction 4.5h at temperature is 60 DEG C, stirring reaction 2.5h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) component A of getting 30g coordinates with 12g modified amine curing agent, 11g modification aliphatic cyclic amine solidifying agent (B component), namely obtains Heat Conductive Insulation Adhesive.
Embodiment 18
(1) 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 5, boron nitride 10g and carbon fiber 2g and 3-aminopropyl trimethoxysilane 0.3g that particle diameter is 50nm is added under stirring, and regulate temperature 60 C, after stirring 30min, put into ultrasonic cleaner ultrasonic disperse 40min, and constant temperature hydrolysis 1h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C of dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil 5g, 3-glycydoxy Trimethoxy silane 0.5g, 3-aminopropyl trimethoxysilane 0.5g is taken in beaker, 10g bisphenol A type epoxy resin and 8g glycidyl ester type epoxy resin is added after stirring reaction 4.5h at temperature is 60 DEG C, stirring reaction 2.5h, obtain modified epoxy, heat conductive filler after above-mentioned surface treatment is joined in modified epoxy, stirring at room temperature 20min, obtains component A.
(3) component A of getting 30g coordinates with 13g modified amine curing agent, 13g modification aliphatic cyclic amine solidifying agent (B component), namely obtains Heat Conductive Insulation Adhesive.
Component A and B component in above specific embodiment are fully mixed, after being placed in vacuum drying oven vacuumizing and defoaming 30min, pour mould (the diameter 50mm scribbling remover of preheating into, thickness 3mm) in, in 90 DEG C of baking 1h in vacuum drying oven, obtain shaping heat-conducting insulation material.Carry out thermal conductivity and insulating property test to this material, its concrete test result is in table 1.
Table 1 Heat Conductive Insulation Adhesive performance
| Embodiment | Thermal conductivity (W/mk) | Volume specific resistance (Ω cm) | Dielectric strength (kV/mm) |
| 1 | 1.4 | 1.6×10 15 | 18 |
| 2 | 1.2 | 1.7×10 15 | 19 |
| 3 | 1.1 | 1.8×10 15 | 17 |
| 4 | 1.1 | 2.0×10 15 | 21 |
| 5 | 1.6 | 1.5×10 15 | 22 |
| 6 | 1.9 | 1.6×10 15 | 21 |
| 7 | 1.5 | 1.8×10 15 | 19 |
| 8 | 1.7 | 1.7×10 15 | 16 |
| 9 | 1.5 | 1.9×10 15 | 18 |
| 10 | 1.2 | 2.1×10 15 | 20 |
| 11 | 1.8 | 2.2×10 15 | 22 |
| 12 | 1.6 | 1.9×10 15 | 19 |
| 13 | 1.7 | 1.7×10 15 | 17 |
| 14 | 2.0 | 2.1×10 15 | 20 |
| 15 | 1.7 | 2.3×10 15 | 22 |
| 16 | 2.2 | 2.0×10 15 | 21 |
| 17 | 1.9 | 2.4×10 15 | 23 |
| 18 | 1.6 | 2.2×10 15 | 22 |
Claims (8)
1. a Heat Conductive Insulation Adhesive, it is characterized in that, be made up of component A and B component, described component A by mass percentage be 5% ~ 20% amido silicon oil, the silane coupling agent of 2% ~ 8%, the epoxy resin of 40% ~ 70% and 20% ~ 40% heat conductive filler form, the summation of above-mentioned composition is 100%; B component is solidifying agent.
2. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described component A and the mass ratio of B component are 1 ~ 4: 1.
3. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described amido silicon oil is containing amino polydimethylsiloxane in side chain or end group, and amino value is 0.5 ~ 0.8g/100g, and its structure meets following general formula:
Wherein R
1for methyl or hydroxyl, R
2for ammonia alkyl or R
1for ammonia alkyl, R
2for methyl.
4. a kind of Heat Conductive Insulation Adhesive according to claim 1, it is characterized in that, described silane coupling agent is one or more mixing in 3-aminopropyl triethoxysilane, 3-glycydoxy Trimethoxy silane, 3-aminopropyl trimethoxysilane, aminophenyl triethoxy silica alkane.
5. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described epoxy resin is one or both mixing in bisphenol A type epoxy resin, glycidyl ester type epoxy resin.
6. a kind of Heat Conductive Insulation Adhesive according to claim 1, it is characterized in that, described heat conductive filler is one or more mixing in boron nitride, aluminium nitride, silicon carbide, aluminum oxide, carbon fiber, and the particle diameter of described heat conductive filler is 0.05 μm ~ 200 μm.
7. a kind of Heat Conductive Insulation Adhesive according to claim 1, is characterized in that, described solidifying agent is one or both mixing in modified amine curing agent, modification aliphatic cyclic amine solidifying agent.
8. a preparation method for Heat Conductive Insulation Adhesive, is characterized in that, described preparation method carries out according to the following steps:
(1) 50ml ~ 60ml dehydrated alcohol is poured in 100ml beaker, adding Glacial acetic acid regulation system pH is 4 ~ 6, the heat conductive filler of 20% ~ 40% and the silane coupling agent of 0 ~ 1% that particle diameter is 0.05 μm ~ 200 μm is added under stirring, and regulate temperature 50 C ~ 60 DEG C, after stirring 20min ~ 30min, put into ultrasonic cleaner ultrasonic disperse 40min ~ 50min, and constant temperature hydrolysis 1h ~ 1.5h, after filtration, with deionized water wash to neutral, the heat conductive filler of finishing is put into vacuum drying oven in 40 DEG C ~ 60 DEG C dry 12h, obtain the heat conductive filler after surface treatment.
(2) amido silicon oil of 5% ~ 20% is mixed with 1% ~ 8% silane coupling agent be placed in beaker, stirring reaction 4h ~ 6h at temperature is 60 DEG C ~ 80 DEG C, the epoxy resin of 40% ~ 70% is added again in beaker, stirring reaction 2h ~ 2.5h, obtain modified epoxy, join in modified epoxy by the heat conductive filler after above-mentioned surface treatment, stirring at room temperature 20min ~ 30min, obtains component A.
(3) ratio being 1 ~ 4: 1 in mass ratio by component A and B component coordinates, and namely obtains described Heat Conductive Insulation Adhesive.
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