CN105176484A - Potting adhesive for power electronic devices, and preparation method thereof - Google Patents
Potting adhesive for power electronic devices, and preparation method thereof Download PDFInfo
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- CN105176484A CN105176484A CN201510557449.2A CN201510557449A CN105176484A CN 105176484 A CN105176484 A CN 105176484A CN 201510557449 A CN201510557449 A CN 201510557449A CN 105176484 A CN105176484 A CN 105176484A
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Abstract
The invention relates to a potting adhesive for power electronic devices, and a preparation method thereof. The potting adhesive is prepared by mixing a component A with a component B, and the component A comprises, by weight, 100 parts of vinyl silicone oil, 600-850 parts of an inorganic mixed heat conduction filler, 5-10 parts of a plasticizer and 30-40 parts of a strengthening agent; and the component B comprises, by weight, 17-48 parts of a catalyst system and 2-4 parts of the plasticizer. The catalyst system is composed of 0.2-2.1% of a platinum-containing catalyst, 96.2-98.6% of a cross-linking agent and 1.2-1.7% of a silane coupling agent. The inorganic heat conduction filler is a micro-nano composite AlN and BN mixture or a AlN and Al2O3 mixture. The preparation method of the potting adhesive comprises the following steps: respectively preparing the component A and the component B, weighing the component A and the component B according to a weight ratio of (6-10):(1.0-1.5), uniformly mixing, and defoaming under a vacuum degree of 103Pa.
Description
Technical field
The present invention relates to a kind of joint sealant and preparation method thereof, particularly a kind of joint sealant for power electronic devices and preparation method thereof.
Background technology
Along with power device is towards high frequency, high-power, high current density future development, the miniaturization of device, unfailing performance and life requirements are improved constantly, require that embedding part must run under the conditions such as high frequency, high temperature, high speed rotating simultaneously, therefore not only require that Embedding Material has excellent heat conductivility and dielectric properties, also need to possess the performances such as excellent high and low temperature resistance, mechanical property, flame retardant properties and sulfuration resistant reduction simultaneously simultaneously.The more Embedding Material of current use is various synthetic polymers, as: epoxy resin, urethane resin and acrylic resin.The matrix materials such as epoxy resin show the easily shortcoming such as aging, easy to change, easy to crack under high temperature, high radiation condition, affect power device bulk life time; And silicon rubber has excellent uv-resistant aging, high/low temperature chemical stability, elasticity can be kept for a long time in wide temperature range, low volumetric shrinkage, low internal stress, coordinate inorganic thermally conductive material, can obtain that there is thermal conductive resin, be the first-selected Embedding Material of power device, all adopt organosilicon as packaged material of new generation at present both at home and abroad.But, in order to obtain the electronic encapsulation material of better thermal conductivity, needing to carry out silicon rubber a large amount of filling-modified, thus the viscosity of electronic encapsulation material increased greatly, affecting the mechanical property after its mobility and solidification and electric property.As Chinese patent CN101054057A discloses a kind of high heat conduction organosilicon filling and sealing gum, CN101407635A discloses a kind of heat-conducting anti-flaming liquid silicon rubber, although this silicon rubber has higher thermal conductivity and flame retardant properties, but because its viscosity is at more than 10000mPas, mobility is not good enough, tensile strength and Resisting fractre extensibility deficiency, should not be used as electron pouring sealant.Chinese patent 200810035243.3, discloses a kind of nano heat conductive transparent embedding glue composite material and preparation method thereof, also there is the problem of illiquidity and shock resistance difference.Chinese patent CN103419346A etc. individually discloses a kind of technology of preparing of heat conductive silica gel, but all belongs to moisture condensed type, and have a large amount of small molecules polycondensate to discharge in solidification process, volumetric shrinkage is high, and curing depth is not enough, there is reversion when being heated; Patent CN103834352A proposes a kind of " two component height heat conduction joint sealants of excellent in mechanical performance and preparation method thereof " of filling with ball-aluminium oxide, the colloid mixing viscosity 1800cp when filler content is about 67%, thermal conductivity is only 0.75w/m.k, is difficult to meet the demand of high current density power device to high heat conduction joint sealant.In addition, patent CN104479623A discloses the organic joint sealant of a kind of high heat conduction ambient cure, heat conductive filler used is difform alumina powder jointed for being broken for, there is the uneven and too high levels of mineral filler dispersion, cause poor mechanical property, simultaneously due to problems such as the capacity effect of ceramic packing cause electric property before and after embedding inconsistent; Patent CN103865271A discloses organosilicon heat conductive electronic pouring sealant of a kind of nano-hybrid material modification and preparation method thereof, heat conductive filler used is AlN, AlB of 0.6 ~ 105 μm and the mixture of oxide ceramics, product thermal conductivity is only 0.6 ~ 0.85w/m.k, particle diameter is large in addition, not strong with silica gel avidity, mechanical property is unstable.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, propose a kind of joint sealant for power electronic devices and preparation method thereof.Organic silicon potting adhesive Uniform Doped prepared by the present invention inorganic hybrid conductive filler of micro-nano compound size.
Organic joint sealant of the present invention comprises component A and B component, and the mass ratio of component A and B component is (6 ~ 10): (1.0 ~ 1.5).
Described component A comprises vinyl silicone oil, inorganic mixing heat conductive filler, strengthening agent and softening agent, is by weight: vinyl silicone oil 100 parts, inorganic mixing heat conductive filler 600 ~ 850 parts, strengthening agent 30 ~ 40 parts, 5 ~ 10 parts, softening agent.
Described B component comprises catalyst system and softening agent, and by weight, catalyst system 17 ~ 48 parts, softening agent is 2 ~ 4 parts.Described catalyst system is made up of catalyst made from platonic, linking agent and silane coupling agent, and wherein the content of catalyst made from platonic in catalyst system is 0.2 ~ 2.1%, and linking agent is 96.2 ~ 98.6%, and silane coupling agent is 1.2 ~ 1.7%.
Described vinyl silicone oil is divinyl polydimethylsiloxane, two vinyl are wherein end chain or intermediate chain, or one in end chain intermediate chain or two kinds of mixing, the contents of ethylene of vinyldimethicone is 0.3 ~ 0.45wt.%, and when 25 DEG C, viscosity is 300 ~ 475mPas.
Described inorganic mixing heat conductive filler is AlN and BN mixture through coupling agent surface oleophylic process or AlN and Al
2o
3mixture, wherein, the content of AlN in inorganic mixing heat conductive filler is 20 ~ 60wt.%, Al
2o
3be 40 ~ 80wt.%; AlN particle diameter is 0.6 ~ 0.8 μm, BN or Al
2o
3particle diameter be 10 ~ 100 μm.In component A, the content of inorganic mixing heat conductive filler used in organic joint sealant is 60 ~ 85wt%.
Described strengthening agent is the thermal silica through hydrophobic treatment.
The end-vinyl polydimethylsiloxane solution of described platinum catalyst to be Pt massfraction the be platinum-vinyl siloxane title complex of 1%.
Described silane coupling agent is one or more the mixture in KH530, KH540, KH550, KH560, and when for two or more mixtures, each component proportion is decile ratio.
The described softening agent epoxy hydroxyl terminated butadiene acrylonitrile copolymer that to be molecule segment be with epoxy group(ing), cyano group, molecular weight 1800 ~ 2000, oxirane value is 0.7 ~ 1.0mmol/g, and acrylonitrile content is 4 ~ 6%.
Described linking agent is Methyl Hydrogen Polysiloxane Fluid, and the viscosity of silicone oil linking agent is 320 ~ 480mPas at 25 DEG C.
The method that the present invention prepares described organic silicon potting adhesive comprises the steps:
1) component A is prepared:
Under normal temperature, get mixed fillers AlN and the Al that AlN content is 20 ~ 60wt.%
2o
3or AlN and BN600 ~ 850 part mixing, stirs 10 ~ 30 minutes, obtained inorganic mixing heat conductive filler; In 100 parts of vinyl silicone oils, add the inorganic mixing heat conductive filler of 8 ~ 15 parts of softening agent and 30 ~ 40 portions of strengthening agents and 600 ~ 850 parts, fully stir 20 ~ 50 minutes, obtained component A;
2) B component is prepared
Under normal temperature, be add 0.04 ~ 1.00 part of platinum catalyst that platinum content is 1500 ~ 4500ppm in 16.80 ~ 45.20 parts of silicone oil linking agents of 0.3 ~ 1.8wt% at hydrogen content, and 0.20 ~ 0.80 part of silane coupling agent and 2 ~ 4 parts of softening agent, fully stir 20 ~ 50 minutes, obtained B component;
3) joint sealant is prepared:
Under normal temperature, according to (6 ~ 10): the weight ratio of (1.0 ~ 1.5) takes component A and B component, mixes, in vacuum tightness 10
3deaeration 15 ~ 20 minutes under Pa, obtains bubble-free joint sealant of the present invention.
Step 1) described in vinyl silicone oil be divinyl polydimethylsiloxane, two vinyl are wherein end chain or intermediate chain, or one in end chain intermediate chain or two kinds of mixing, the contents of ethylene of vinyldimethicone is 0.3 ~ 0.45wt.%, and when 25 DEG C, viscosity is 300 ~ 475mPas.
Step 2) described in Silicon Containing Hydrogen oil viscosity be 320 ~ 480mPas at 25 DEG C.
Step 1) described in inorganic mixing heat conductive filler be AlN and BN mixture through coupling agent surface oleophylic process or AlN and Al
2o
3mixture, wherein, the content of AlN in inorganic mixing heat conductive filler is 20 ~ 60wt.%, Al
2o
3be 40 ~ 80wt.%; AlN particle diameter is 0.6 ~ 0.8 μm, BN or Al
2o
3particle diameter be 10 ~ 100 μm.In component A, the content of inorganic mixing heat conductive filler used in organic joint sealant is 60 ~ 85wt%.
The end-vinyl polydimethylsiloxane solution of described catalyzer to be Pt massfraction the be platinum-vinyl siloxane title complex of 1%.
Described strengthening agent is the thermal silica through hydrophobic treatment.
Described silane coupling agent is one or more the mixture in KH530, KH540, KH550, KH560, and when for two or more mixtures, each component proportion is decile ratio.
Joint sealant of the present invention has efficient heat dispersion, AlN and the BN introduced or AlN and Al
2o
3mixed fillers is made up of micro-nano different-grain diameter super-high heat-conductive filler, good with silica gel avidity, is evenly distributed, not easily precipitate, can make to form maximum contact between filler, reduce interface contact heat resistance to greatest extent, thus reach effective thermal conduction and insulation, obtain the insulation system of high heat conduction.Simultaneously partial filler has electro-magnetic screen function, can the electromagnetic shielding efficiency of effective boost device.
Product of the present invention can be applicable to, in the power electronic devices of different capacity density, also can be applicable to microelectronic industry.The organic joint sealant preparation technology of heat conductive insulating of the present invention is simple, with low cost, superior performance, and production process no coupling product, safety and environmental protection.
Accompanying drawing explanation
The element line distribution of the joint sealant different positions prepared by Fig. 1 a embodiment 1;
The element line distribution of the joint sealant different positions prepared by Fig. 1 b embodiment 6;
In the inorganic heat conductive filler of Fig. 2 a prepared by embodiment 1, AlN content is the thermal diffusivity of the joint sealant of 20%;
In the inorganic heat conductive filler of Fig. 2 b prepared by embodiment 2, AlN content is thermal diffusivity and the thermal conductivity of the joint sealant of 40%;
In the inorganic heat conductive filler of Fig. 2 c prepared by embodiment 3, AlN content is thermal diffusivity and the thermal conductivity of the joint sealant of 60%.
Embodiment
Embodiment 1
1) AlN400 weight part is taken, add in high speed planetary ball mill, under high-speed stirring condition, slowly drip 1 weight part in advance with the Union carbide A-162 of ethanolic soln dilution, after dropwising, be warming up to 65 DEG C, continue high-speed stirring 2 hours, high speed centrifugation is separated.Be placed in vacuum drying oven by gained filler after solid-liquid separation, after removing residual water and ethanol, the i.e. obtained particle diameter that sieves is the AlN surface-treated through silane coupling agent of 0.6 μm.
2) Al is taken
2o
3400 weight parts, add in high speed planetary ball mill, 1 weight part is slowly dripped in advance with the Union carbide A-162 of ethanolic soln dilution under high-speed stirring condition, 65 DEG C are warming up to after dropwising, continue high-speed stirring 2 hours, high speed centrifugation is separated, and is placed in vacuum drying oven by gained filler after removing residual water and ethanol after solid-liquid separation, and the i.e. obtained particle diameter that sieves is the Al surface-treated through silicone coupling agents of 10 μm
2o
3.
3) be 300mPas by viscosity, contents of ethylene is the end chain of 0.4wt% and vinyldimethicone 100 weight part of intermediate chain mixing, step 1) the AlN400 weight part that processed, step 2) Al that processed
2o
3400 weight parts, PVC softening agent 5 weight part, white carbon black strengthening agent 30 weight part adds in vacuum drying oven, and in temperature 110 DEG C, vacuum tightness is 10
3under Pa, dewater blended 60 minutes obtained component A.
4) by Union carbide A-162 coupling agent 0.20 ~ 0.80 weight part, catalyst made from platonic 0.04 ~ 1.00 weight part, softening agent 2 ~ 4 weight part adds that viscosity is 320mPas, hydrogen content is in the 15 part by weight of liquid silicone oil linking agents of 0.3%, is fully uniformly mixed 30 minutes, obtains B component.
5) 6:1 takes component A and B component in mass ratio, at room temperature blended evenly after, be 10 in vacuum tightness
3deaeration 5 minutes under Pa, obtains joint sealant of the present invention.The performance test results of this joint sealant is as shown in table 1.Can find out, this joint sealant has excellent thermal conductivity, electrical property and mechanical property.
The preparation method of embodiment 2,3,4,5 and 6 is with embodiment 1.In each embodiment, processing parameter is as shown in table 1 each composition, ratio, consumption, particle diameter and technique vacuum tightness, time etc.:
The material composition of each embodiment of table 1, ratio and processing parameter
Note: " mixing heat conductive filler content " refers to the ratio of mixing heat conductive filler in whole joint sealant prepared by component A.
Organic joint sealant prepared by the present invention, by GB/T10247-2008 tested viscosity; By GB/T528-1998 test tensile strength and elongation at break; Shore A hardness is tested by GB/T531-2008; By GB/T1410-2006 test volume resistivity; Test thermal conductivity by GB/T11205-2009, the test result of above each embodiment is as shown in table 2:
The each embodiment performance test results of table 2
| Performance | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 |
| Viscosity (mPas) | 350 | 400 | 450 | 475 | 465 | 700 |
| Hardness (grams) | 85 | 113 | 300 | 450 | 500 | 600 |
| Thermal conductivity (W/m.k) | 2.8 | 3.1 | 3.5 | 2.9 | 3.0 | 3.2 |
| Volume specific resistance (10 15Ω·cm) | 2.75 | 9.5 | 4.7 | 2.0 | 4.8 | 6.4 |
| Specific inductivity (kv/mm) | 17 | 18 | 20 | 19 | 20 | 21 |
Fig. 1 and Fig. 2 adopts scanning electron microscope and laser conductometer to carry out quantitative scanning analysis and test to the composition of prepared joint sealant and thermal characteristics respectively.
Fig. 1 is the Surface scan of joint sealant composition prepared by the present invention, wherein, Fig. 1 a and Fig. 1 b is respectively the element Surface scan of embodiment 1 and the joint sealant any position prepared by embodiment 6, as seen from the figure in joint sealant except Silica hydrogel composition C and Si, also there is N, O and Al element, this mixes mineral filler Al just
2o
3with the principal element of AlN, in addition, also there is the conducting metal Au in electron microscopyc sample preparation process.
Fig. 2 is the test result such as thermal diffusivity and thermal conductivity of the heat conductive filler of different al N content.Joint sealant of the present invention has good fluidity, mechanical property, high thermal conductivity and low-dielectric energy as can be seen here, tensile strength and tension fracture rate high, meanwhile, before and after embedding, device has good electrical uniformity energy.
Claims (9)
1. a power electronic devices joint sealant, is characterized in that: described joint sealant comprises component A and B component, and the mass ratio of component A and B component is (6 ~ 10): (1.0 ~ 1.5);
Described component A comprises vinyl silicone oil, inorganic mixing heat conductive filler, strengthening agent and softening agent, is by weight: vinyl silicone oil 100 parts, inorganic mixing heat conductive filler 600 ~ 850 parts, strengthening agent 30 ~ 40 parts, 5 ~ 10 parts, softening agent;
Described B component comprises catalyst system and softening agent, by weight, catalyst system 17 ~ 48 parts, softening agent is 2 ~ 4 parts; Described catalyst system is made up of catalyst made from platonic, linking agent and silane coupling agent, and wherein the content of catalyst made from platonic in catalyst system is 0.2 ~ 2.1%, and linking agent is 96.2 ~ 98.6%, and silane coupling agent is 1.2 ~ 1.7%.
2. power electronic devices joint sealant according to claim 1, it is characterized in that: described vinyl silicone oil is divinyl polydimethylsiloxane, two vinyl are wherein end chain or intermediate chain, or one in end chain intermediate chain or two kinds of mixing, the contents of ethylene of vinyldimethicone is 0.3 ~ 0.45wt.%, and when 25 DEG C, viscosity is 300 ~ 475mPas.
3. power electronic devices joint sealant according to claim 1, is characterized in that: described inorganic mixing heat conductive filler is mixture through AlN and the BN of coupling agent surface oleophylic process or AlN and Al
2o
3mixture, wherein, the content of AlN in inorganic mixing heat conductive filler is 20 ~ 60wt.%, Al
2o
3be 40 ~ 80wt.%; AlN particle diameter is 0.6 ~ 0.8 μm, BN or Al
2o
3particle diameter be 10 ~ 100 μm; The content of described inorganic mixing heat conductive filler in organic joint sealant is 60 ~ 85wt%.
4. power electronic devices joint sealant according to claim 1, is characterized in that: described strengthening agent is the thermal silica through hydrophobic treatment.
5. power electronic devices joint sealant according to claim 1, is characterized in that: the end-vinyl polydimethylsiloxane solution of described platinum catalyst to be Pt massfraction the be platinum-vinyl siloxane title complex of 1%.
6. power electronic devices joint sealant according to claim 1, is characterized in that: the described softening agent epoxy hydroxyl terminated butadiene acrylonitrile copolymer that to be molecule segment be with epoxy group(ing), cyano group.
7. power electronic devices joint sealant according to claim 1, is characterized in that: described linking agent is Methyl Hydrogen Polysiloxane Fluid, and the viscosity of silicone oil linking agent is 320 ~ 480mPas at 25 DEG C.
8. power electronic devices joint sealant according to claim 1, it is characterized in that: described silane coupling agent is one or more the mixture in KH530, KH540, KH550, KH560, when for two or more mixtures, each component proportion is decile ratio.
9. prepare the method for power electronic devices joint sealant according to claim 1, it is characterized in that: the step of described preparation method is as follows:
1) component A is prepared:
Under normal temperature, get mixed fillers AlN and the Al that AlN content is 20 ~ 60wt.%
2o
3or AlN and BN600 ~ 850 part mixing, stirs 10 ~ 30 minutes, obtained inorganic mixing heat conductive filler; In 100 parts of vinyl silicone oil linking agents, add the inorganic mixing heat conductive filler of 8 ~ 15 parts of softening agent and 30 ~ 40 portions of strengthening agents and 600 ~ 850 parts, fully stir 20 ~ 50 minutes, obtained component A;
2) B component is prepared
Under normal temperature, be add 0.04 ~ 1.00 part of platinum catalyst that platinum content is 1500 ~ 4500ppm in 16.80 ~ 45.20 parts of silicone oil linking agents of 0.3 ~ 1.8wt% at hydrogen content, and 0.20 ~ 0.80 part of silane coupling agent and 2 ~ 4 parts of softening agent, fully stir 20 ~ 50 minutes, obtained B component;
3) joint sealant is prepared:
Under normal temperature, according to (6 ~ 10): the weight ratio of (1.0 ~ 1.5) takes component A and B component, mixes, in vacuum tightness 10
3deaeration 15 ~ 20 minutes under Pa, obtains bubble-free described joint sealant;
Described step 1) in:
Described vinyl silicone oil is divinyl polydimethylsiloxane, two vinyl are wherein end chain or intermediate chain, or one in end chain intermediate chain or two kinds of mixing, the contents of ethylene of vinyldimethicone is 0.3 ~ 0.45wt.%, and when 25 DEG C, viscosity is 300 ~ 475mPas;
Described inorganic mixing heat conductive filler is AlN and BN mixture through coupling agent surface oleophylic process or AlN and Al
2o
3mixture, wherein, the content of AlN in inorganic mixing heat conductive filler is 20 ~ 60wt.%, Al
2o
3be 40 ~ 80wt.%; AlN particle diameter is 0.6 ~ 0.8 μm, BN or Al
2o
3particle diameter be 10 ~ 100 μm; In component A, the content of inorganic mixing heat conductive filler used in organic joint sealant is 60 ~ 85wt%;
Described step 2) in:
The viscosity of described silicone oil linking agent is 320 ~ 480mPas at 25 DEG C;
The end-vinyl polydimethylsiloxane solution of described platinum catalyst to be Pt massfraction the be platinum-vinyl siloxane thing of 1%;
Described strengthening agent is the thermal silica through hydrophobic treatment;
Described silane coupling agent is one or more the mixture in KH530, KH540, KH550, KH560, and when for two or more mixtures, each component proportion is decile ratio;
The described softening agent epoxy hydroxyl terminated butadiene acrylonitrile copolymer that to be molecule segment be with epoxy group(ing), cyano group, molecular weight 1800 ~ 2000, oxirane value is 0.7 ~ 1.0mmol/g, and acrylonitrile content is 4 ~ 6%.
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| CN105969277A (en) * | 2016-05-31 | 2016-09-28 | 苏州市奎克力电子科技有限公司 | Heat-dissipating pouring sealant for packaging electronic devices |
| CN105969300A (en) * | 2016-05-31 | 2016-09-28 | 苏州市奎克力电子科技有限公司 | Pouring sealant for power electronic device |
| CN107987789A (en) * | 2017-12-21 | 2018-05-04 | 深圳市东成电子有限公司 | The composition and preparation method, application method of low rate of perviousness organic silicon potting adhesive |
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| CN105969300A (en) * | 2016-05-31 | 2016-09-28 | 苏州市奎克力电子科技有限公司 | Pouring sealant for power electronic device |
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| CN109082253A (en) * | 2018-06-25 | 2018-12-25 | 南亚新材料科技股份有限公司 | A kind of halogen-free adhesive of polymolecularity and preparation method thereof |
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| CN111423842A (en) * | 2020-03-30 | 2020-07-17 | 广州回天新材料有限公司 | Low-dielectric-constant organic silicon pouring sealant and preparation method thereof |
| CN111777985A (en) * | 2020-06-19 | 2020-10-16 | 台达电子企业管理（上海）有限公司 | Pouring sealant and heat dissipation device |
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| CN113462354A (en) * | 2021-07-20 | 2021-10-01 | 惠州市永卓科技有限公司 | Heat-conducting adhesive and preparation method thereof |
| CN115216267A (en) * | 2022-08-16 | 2022-10-21 | 西卡(江苏)工业材料有限公司 | Environment-friendly high-adhesion high-thermal-conductivity organic silicon pouring sealant and preparation method and application thereof |
| CN115287037A (en) * | 2022-08-16 | 2022-11-04 | 西卡(江苏)工业材料有限公司 | Environment-friendly single-component organic silicon high-thermal-conductivity adhesive and preparation method and application thereof |
| CN115287037B (en) * | 2022-08-16 | 2023-08-22 | 西卡(江苏)工业材料有限公司 | Environment-friendly single-component organic silicon high-heat-conductivity adhesive and preparation method and application thereof |
| CN115216267B (en) * | 2022-08-16 | 2023-08-22 | 西卡(江苏)工业材料有限公司 | Environment-friendly high-adhesion high-thermal-conductivity organic silicon pouring sealant and preparation method and application thereof |
| CN115622474A (en) * | 2022-12-15 | 2023-01-17 | 山西省机电设计研究院有限公司 | Sealed water-cooling motor controller |
| CN115622474B (en) * | 2022-12-15 | 2023-03-21 | 山西省机电设计研究院有限公司 | Sealed water-cooling motor controller |
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| CN105176484B (en) | 2018-12-18 |
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