CN103849356A - Electrical insulating phase-change heat conducting material and preparation method thereof - Google Patents

Electrical insulating phase-change heat conducting material and preparation method thereof Download PDF

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Publication number
CN103849356A
CN103849356A CN201410102937.XA CN201410102937A CN103849356A CN 103849356 A CN103849356 A CN 103849356A CN 201410102937 A CN201410102937 A CN 201410102937A CN 103849356 A CN103849356 A CN 103849356A
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phase
change
heat conduction
conductive material
conduction powder
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王执乾
王月祥
张恩贵
朱毅
张世麟
白翰林
张小刚
孟德文
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CETC 33 Research Institute
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CETC 33 Research Institute
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Abstract

The invention discloses an electrical insulating phase-change heat conducting material and a preparation method thereof. The electrical insulating phase-change heat conducting material is prepared from 4-12% of two-component molding liquid silicone rubber, 10-30% of paraffin-acrylic phase change microcapsules, 50-70% of heat-conducting powder, 1-2% of silane coupling agent, and 10-25% of ethenyl terminated silicon oil. The electrical insulating phase-change heat conducting material disclosed by the invention is high in heat conductivity coefficient, low in heat resistance, and good in electrical insulating property, is in a solid state at room temperature, can be conveniently attached to the surface of a cooling fin or an electronic component; the electrical insulating phase-change heat conducting material is subjected to phase change to become soft (but not become liquid) when the working temperature of the component is achieved, the electrical insulating phase-change heat conducting material plays an electric insulating effect when the contact thermal resistance is reduced and the heat-conducting property is improved, a short circuit of the electric component is not caused, and the safety and the reliability of the electronic component are improved.

Description

A kind of electric insulation phase-change heat conductive material and preparation method thereof
Technical field
The present invention relates to a kind of hot interfacial phase change thermally conductive material, particularly relate to a kind of electric insulation phase-change heat conductive material, and the preparation method of this thermally conductive material.
Background technology
High temperature will produce harmful effect to the stability of electronic devices and components, reliability and life-span, 2 DEG C of the every risings of electronic devices and components temperature, 1/6 when life-span when 10%, 50 DEG C of reliability decrease only has 25 DEG C.The raising of heat conductivility is accompanied by the optimization of heat dispersion conventionally.Visible heat radiation is for miniaturization, the densification of electronics and to improve its precision most important.In order to solve the heat dissipation problem of heating electronic component, conventionally use scatterer to dispel the heat to components and parts.But, be limited to existing industrial production technology, exist imperceptible rough interface gaps between electronic devices and components surface and scatterer, the air in interface gaps can increase interface resistance, obstruction heat conducts, and has a strong impact on the integral heat sink effect of electronic devices and components.
Hot interface thermally conductive material is a kind of generally for the material of cooling electronic component, is mainly used in filling up the microvoid of generation when electronic devices and components are surperficial to be contacted with scatterer and the hole of surface irregularity, reduces thermal contact resistance, improves device radiating efficiency.Phase-change heat conductive material is wherein main one.
Phase-change heat conductive material is that heat strengthens polymkeric substance, there is the feature such as high thermal conductivity, low thermal resistance, the thermal resistance value being designed between the radiator element that makes electronic devices and components and be attached thereto is reduced to minimum, the passage that this thermal resistance is little makes the performance of radiator element reach best, the effectively space between filling interface, dispel air between interface, scatterer effect is improved to more than 40%.
Traditional phase-change heat conductive material is to utilize polymer technology, is mixed with organic polymer material, heat conductive filler and wax phase change filler.Because material is on-insulated, at high temperature become mutually liquid, through repeatedly extruding, likely cause metal and metallic contact, be difficult to meet the insulating requirements between portions of electronics components and parts and scatterer, easily cause the short circuit of electronic devices and components.Therefore, traditional phase-change heat conductive material can not use as insulating material.
Summary of the invention
The object of this invention is to provide a kind of electric insulation phase-change heat conductive material and preparation method thereof, thermally conductive material of the present invention can directly fit on electronic devices and components plate while use, there is excellent electrical insulation properties, voltage breakdown can reach 6000Vac/mm, through repeatedly not causing electronic devices and components short circuit after extruding, can be used as insulating material and use.
Electric insulation phase-change heat conductive material of the present invention is a kind of polymer composite, its raw material by following weight per-cent prepares: dual composition addition type liquid silastic 4%~12%, paraffin-vinylformic acid phase-change microcapsule 10%~30%, heat conduction powder 50%~70%, silane coupling agent 1%~2%, ethenyl blocking silicone oil 10%~25%.
Wherein, described heat conduction powder is made up of according to the weight ratio of 6~7 ﹕ 2~3 ﹕ 1 the heat conduction powder of large, medium and small three kinds of particle diameters, the particle size of described large particle diameter heat conduction powder is 70 μ m~80 μ m, the particle size of middle particle diameter heat conduction powder is 30 μ m~40 μ m, and the particle size of small particle size heat conduction powder is 0.5 μ m~1 μ m.
Further, described heat conduction powder is one or more the arbitrary proportion mixture in aluminum oxide, aluminium nitride, silicon carbide.
In above-mentioned raw materials, the preferred KH-570 of described silane coupling agent.
The viscosity of described dual composition addition type liquid silastic is 120,000 cst, hardness 30(shore A), wherein the weight ratio of A, B component is 100 ﹕ 1.
Described paraffin-vinylformic acid phase-change microcapsule be taking paraffin as core, vinylformic acid is wall material, the phase-change microcapsule that adopts situ aggregation method to prepare, microcapsule are spherical in shape, particle diameter 40 μ m~50 μ m, 50 DEG C~60 DEG C of transformation temperatures, latent heat of phase change >=140J/g.
Preferably, the mixture that the ethenyl blocking silicone oil that the ethenyl blocking silicone oil that described ethenyl blocking silicone oil is 20000cst~30000cst by viscosity and viscosity are 3000cst~4000cst forms according to the weight ratio of 2~3 ﹕ 6.
The preparation method of electric insulation phase-change heat conductive material of the present invention is the silane coupling agent that adds described weight percent in the heat conduction powder of described weight percent, under normal temperature and pressure, stirs and obtains modification heat conduction powder; The ethenyl blocking silicone oil of described weight percent is added in the A component of described weight percent dual composition addition type liquid silastic and mix, add again paraffin-vinylformic acid phase-change microcapsule of above-mentioned modification heat conduction powder and described weight percent, and the B component of dual composition addition type liquid silastic, under 80Pa~150Pa vacuum tightness, be uniformly mixed and obtain sizing material, sulfidization molding obtains phase-change microcapsule thermally conductive material.
More specifically, electric insulation phase-change heat conductive material of the present invention can adopt following method preparation:
1). taking paraffin as core, vinylformic acid is wall material, adopts situ aggregation method to prepare paraffin-vinylformic acid phase-change microcapsule;
2). respectively the small particle size heat conduction powder of the middle particle diameter heat conduction powder of the large particle diameter heat conduction powder of particle size 70 μ m~80 μ m, particle size 30 μ m~40 μ m, particle size 0.5 μ m~1 μ m is removed after moisture in 200 DEG C of baking 30h~40h, be mixed to get heat conduction powder raw material according to the weight ratio of 6~7 ﹕ 2~3 ﹕ 1;
3). to the step 2 of described weight percent) heat conduction powder in add the silane coupling agent of described weight percent, under normal temperature and pressure, high-speed stirring obtains modification heat conduction powder;
4). the ethenyl blocking silicone oil of described weight percent is added in the A component of dual composition addition type liquid silastic of described weight percent and mix, to reduce the viscosity of liquid silastic;
5). to step 4) liquid in add step 3) modification heat conduction powder and the phase-change microcapsule of described weight percent, mix, add again the B component of the dual composition addition type liquid silastic of described weight percent, use vacuum mixer, under 80Pa~150Pa vacuum tightness, be fully uniformly mixed and obtain sizing material;
6). sizing material is poured in mould, in vulcanizing press, under 180 DEG C~240 DEG C, 10MPa~20MPa, vulcanizes 1min~3min, and moulding obtains electric insulation phase-change heat conductive material;
7). at the two sides of electric insulation phase-change heat conductive material laminating release film, not impaired with protecting materials surface.
According to using needs, the above-mentioned electric insulation phase-change heat conductive material preparing can be cut into the product of different size and shape.
Wherein, described step 3) stir speed (S.S.) that stirs of high speed is 300rpm~400rpm, churning time 60min~100min.Described step 5) in stir speed (S.S.) be 100rpm~200rpm, churning time 10min~20min.
Electric insulation phase-change heat conductive material of the present invention belongs to heat and strengthens polymkeric substance, and thermal conductivity is high, and thermal resistance is low, good insulating, can make electronic devices and components and the radiator element that is attached thereto between thermal resistance value be reduced to minimum.In the time reaching the working temperature of electronic devices and components, electric insulation phase-change heat conductive material undergoes phase transition deliquescing, but can not become liquid, two surfaces are easy to fit, in reducing thermal contact resistance, promoting heat conductivility, play the effect of electric insulation, can not cause the short circuit of electronic devices and components, and then promote the safety and reliability of electronic devices and components.
Electric insulation phase-change heat conductive material of the present invention is due to phase-change microcapsule is filled in macromolecular material, under long term high temperature state, use, after material phase transformation, can not become liquid, can not paste, damage electronic devices and components plate, electrical insulation properties is good, voltage breakdown can reach 6000Vac/mm, and life-time service also can not cause the short circuit of electronic devices and components, can meet the insulating requirements between portions of electronics components and parts and scatterer.
Electric insulation phase-change heat conductive material of the present invention uses very simple, convenient, only need remove the release film on electric insulation phase-change heat conductive material surface, directly fit on electronic devices and components plate, can play good heat conductive insulating effect, the natural binding property of material is good, without material or radiator element are carried out to preheating, greatly improve working efficiency.
Embodiment
Embodiment 1
Take respectively the aluminum oxide 14g of the aluminum oxide 42g, the median size 30 μ m that toast dewatered median size 70 μ m at 200 DEG C, the aluminium nitride 7g of median size 0.5 μ m, be mixed to get heat conduction powder raw material.
Weigh 1g silane coupling agent, add in described heat conduction powder raw material, put into homogenizer, the speed with 300rpm under normal temperature and pressure stirs 60min, obtains modification heat conduction powder.
Take the ethenyl blocking silicone oil of 5g viscosity 20000cst, after mixing with the ethenyl blocking silicone oil of 10g viscosity 3000cst, add the A component 10g in dual composition addition type liquid silastic, mix, put into vacuum mixer, add above-mentioned modification heat conduction powder, paraffin-vinylformic acid phase-change microcapsule of 10.9g median size 40 μ m, and the B component of 0.1g dual composition addition type liquid silastic, the speed with 100rpm under 100Pa vacuum tightness stirs 10min.
The sizing material obtaining is poured in mould, in vulcanizing press, under 200 DEG C, 10MPa, vulcanizes 3min, obtains electric insulation phase-change heat conductive material.
Finally, release film in the laminating of the two sides of the electric insulation phase-change heat conductive material obtaining.
Embodiment 2
Take respectively the silicon carbide 15g of the aluminum oxide 35g, the median size 35 μ m that toast dewatered median size 75 μ m at 200 DEG C, the silicon carbide 5g of median size 0.7 μ m, be mixed to get heat conduction powder raw material.
Weigh 1.5g silane coupling agent, add in described heat conduction powder raw material, put into homogenizer, the speed with 350rpm under normal temperature and pressure stirs 80min, obtains modification heat conduction powder.
Take the ethenyl blocking silicone oil of 3g viscosity 25000cst, after mixing with the ethenyl blocking silicone oil of 7.5g viscosity 3500cst, add the A component 10g in dual composition addition type liquid silastic, mix, put into vacuum mixer, add above-mentioned modification heat conduction powder, paraffin-vinylformic acid phase-change microcapsule of 22.9g median size 45 μ m, and the B component of 0.1g dual composition addition type liquid silastic, the speed with 150rpm under 120Pa vacuum tightness stirs 15min.
The sizing material obtaining is poured in mould, in vulcanizing press, under 220 DEG C, 15MPa, vulcanizes 1min, obtains electric insulation phase-change heat conductive material.
Finally, release film in the laminating of the two sides of the electric insulation phase-change heat conductive material obtaining.
Embodiment 3
Take respectively the aluminum oxide 12g of the silicon carbide 42g, the median size 40 μ m that toast dewatered median size 80 μ m at 200 DEG C, the aluminium nitride 6g of median size 1 μ m, be mixed to get heat conduction powder raw material.
Weigh 2g silane coupling agent, add in above-mentioned heat conduction powder raw material, put into homogenizer, the speed with 400rpm under normal temperature and pressure stirs 100min, obtains modification heat conduction powder.
Take the ethenyl blocking silicone oil of 3g viscosity 30000cst, after mixing with the ethenyl blocking silicone oil of 9g viscosity 4000cst, add the A component 10g in dual composition addition type liquid silastic, mix, put into vacuum mixer, add above-mentioned modification heat conduction powder, paraffin-vinylformic acid phase-change microcapsule of 15.9g median size 50 μ m, and the B component of 0.1g dual composition addition type liquid silastic, the speed with 200rpm under 110Pa vacuum tightness stirs 13min.
The sizing material obtaining is poured in mould, in vulcanizing press, under 210 DEG C, 13MPa, vulcanizes 2min, obtains electric insulation phase-change heat conductive material.
Finally, release film in the laminating of the two sides of the electric insulation phase-change heat conductive material obtaining.
Comparative example
For the performance of the electric insulation phase-change heat conductive material product prepared of checking the present invention, the phase-change heat conductive material Hi-Flow 225F producing taking Bei Gesi company, as contrast, carries out following test.
1) thermal conductivity test
The electric insulation phase-change heat conductive material that embodiment 1~3 is prepared is made the square sample that is of a size of 26mm × 26mm × 1mm, be positioned on the testing stand of LW9389 type thermal conductivity test instrument, measure its thermal conductivity, thermal resistance, the results are shown in Table 1, the thermal conductivity of all embodiment products is all apparently higher than comparative example, thermal resistance is all starkly lower than comparative example numerical value, significant difference, show that electric insulation phase-change heat conductive material of the present invention has high thermal conductivity, low thermal resistance coefficient ren, be applicable to the occasion that heat radiation is had relatively high expectations.
2) thermal storage performance test
Get the electric insulation phase-change heat conductive material that a fritter embodiment 1~3 prepares, be placed in the crucible of DZ3335 type DSC differential scanning calorimeter, test its transformation temperature, latent heat of phase change, the results are shown in Table 1, all be better than comparative example numerical value, show that electric insulation phase-change heat conductive material of the present invention has suitable transformation temperature and higher latent heat of phase change, be applicable to the requirement of gap heat radiation, there is good thermal storage performance.
3) voltage breakdown test
The electric insulation phase-change heat conductive material that embodiment 1~3 is prepared is made the square sample that is of a size of 100mm × 100mm × 1mm, be placed on the testing stand of KZT type power frequency withstand test instrument, test its voltage breakdown, the results are shown in Table 1, be all better than comparative example numerical value, show that electric insulation phase-change heat conductive material of the present invention has higher voltage breakdown, be applicable to the requirement of gap electric insulation, there is good withstand voltage properties.

Claims (10)

1. an electric insulation phase-change heat conductive material, raw material by following weight per-cent prepares: dual composition addition type liquid silastic 4%~12%, paraffin-vinylformic acid phase-change microcapsule 10%~30%, heat conduction powder 50%~70%, silane coupling agent 1%~2%, ethenyl blocking silicone oil 10%~25%.
2. electric insulation phase-change heat conductive material according to claim 1, it is characterized in that described heat conduction powder is made up of according to the weight ratio of 6~7 ﹕ 2~3 ﹕ 1 the heat conduction powder of large, medium and small three kinds of particle diameters, the particle size of described large particle diameter heat conduction powder is 70 μ m~80 μ m, the particle size of middle particle diameter heat conduction powder is 30 μ m~40 μ m, and the particle size of small particle size heat conduction powder is 0.5 μ m~1 μ m.
3. electric insulation phase-change heat conductive material according to claim 1 and 2, is characterized in that described heat conduction powder is one or more the arbitrary proportion mixture in aluminum oxide, aluminium nitride, silicon carbide.
4. electric insulation phase-change heat conductive material according to claim 1 and 2, is characterized in that described silane coupling agent is KH-570.
5. electric insulation phase-change heat conductive material according to claim 1 and 2, is characterized in that described paraffin-vinylformic acid phase-change microcapsule particle diameter 40 μ m~50 μ m, 50 DEG C~60 DEG C of transformation temperatures, latent heat of phase change >=140J/g.
6. electric insulation phase-change heat conductive material according to claim 1 and 2, the mixture that the ethenyl blocking silicone oil that the ethenyl blocking silicone oil that the ethenyl blocking silicone oil described in it is characterized in that is 20000cst~30000cst by viscosity and viscosity are 3000cst~4000cst forms according to the weight ratio of 2~3 ﹕ 6.
7. the preparation method of claim 1 electric insulation phase-change heat conductive material, is the silane coupling agent that adds described weight percent in the heat conduction powder of described weight percent, under normal temperature and pressure, stirs and obtains modification heat conduction powder; The ethenyl blocking silicone oil of described weight percent is added in the A component of described weight percent dual composition addition type liquid silastic and mix, add again paraffin-vinylformic acid phase-change microcapsule of described modification heat conduction powder and described weight percent, and the B component of dual composition addition type liquid silastic, under 80Pa~150Pa vacuum tightness, be uniformly mixed and obtain sizing material, sulfidization molding obtains electric insulation phase-change heat conductive material.
8. the preparation method of claim 2 electric insulation phase-change heat conductive material, comprises the following steps:
1). taking paraffin as core, vinylformic acid is wall material, adopts situ aggregation method to prepare paraffin-vinylformic acid phase-change microcapsule;
2). respectively the small particle size heat conduction powder of the middle particle diameter heat conduction powder of the large particle diameter heat conduction powder of particle size 70 μ m~80 μ m, particle size 30 μ m~40 μ m, particle size 0.5 μ m~1 μ m is removed after moisture in 200 DEG C of baking 30h~40h, be mixed to get heat conduction powder raw material according to the weight ratio of 6~7 ﹕ 2~3 ﹕ 1;
3). to the step 2 of described weight percent) heat conduction powder in add the silane coupling agent of described weight percent, under normal temperature and pressure, high-speed stirring obtains modification heat conduction powder;
4). the ethenyl blocking silicone oil of described weight percent is added in the A component of dual composition addition type liquid silastic of described weight percent and mix;
5). to step 4) liquid in add step 3) modification heat conduction powder and the phase-change microcapsule of described weight percent, mix, add again the B component of the dual composition addition type liquid silastic of described weight percent, use vacuum mixer, under 80Pa~150Pa vacuum tightness, be fully uniformly mixed and obtain sizing material;
6). sizing material is poured in mould, in vulcanizing press, under 180 DEG C~240 DEG C, 10MPa~20MPa, vulcanizes 1min~3min, and moulding obtains electric insulation phase-change heat conductive material;
7). at the two sides of electric insulation phase-change heat conductive material laminating release film.
9. the preparation method of electric insulation phase-change heat conductive material according to claim 8, is characterized in that described step 3) high speed stir stir speed (S.S.) be 300rpm~400rpm, churning time 60min~100min.
10. the preparation method of electric insulation phase-change heat conductive material according to claim 8, is characterized in that described step 5) in stir speed (S.S.) be 100rpm~200rpm, churning time 10min~20min.
CN201410102937.XA 2014-03-20 2014-03-20 Electrical insulating phase-change heat conducting material and preparation method thereof Pending CN103849356A (en)

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