CN103773322A - Phase change microcapsule heat conduction material and preparation method thereof - Google Patents
Phase change microcapsule heat conduction material and preparation method thereof Download PDFInfo
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- CN103773322A CN103773322A CN201410045783.5A CN201410045783A CN103773322A CN 103773322 A CN103773322 A CN 103773322A CN 201410045783 A CN201410045783 A CN 201410045783A CN 103773322 A CN103773322 A CN 103773322A
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Abstract
The invention discloses a phase change microcapsule heat conduction material and a preparation method thereof. The phase change microcapsule heat conduction material is prepared from 5%-13% of dual-component addition type liquid silicone rubber, 10%-30% of paraffin-crylic acid phase change microcapsule, 40%-70% of heat conduction powder and 6%-20% of vinyl end capping silicon oil, wherein the heat conduction powder is prepared from various oxide, nitride or carbide powders according to large, middle and small particles. The phase change microcapsule heat conduction material has high heat conduction coefficient, low heat resistance and good heat conduction property, is in a solid state at room temperature, and can be conveniently attached to the surface of a cooling fin or an electron component; when achieving the working temperature of the component, the phase change microcapsule heat conduction material becomes soft and is integrated with the matching surface, plays a good heat dissipation effect and does not pollute the electron component.
Description
Technical field
The present invention relates to a kind of hot interface thermally conductive material, particularly relate to a kind of phase-change microcapsule thermally conductive material, and the preparation method of this thermally conductive material.
Background technology
Integrated technology and package technique develop rapidly, and the volume hundreds of millions of of electronic devices and components, logical circuit doubly dwindles, and have also caused its work power consumption and thermal value sharply to increase.High temperature will produce harmful effect to the stability of electronic devices and components, reliability and life-span, 2 ℃ of the every risings of electronic devices and components temperature, 1/6 when life-span when 10%, 50 ℃ of reliability decrease only has 25 ℃.If it is bad that the heat conduction problem of electronic devices and components solves, the heat that heating element produces can not be discharged in time, will directly affect the conversion speed of electronic devices and components, increases electronic devices and components power consumption, and then affects its work-ing life.
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, hinder heat conduction, had 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 IC encapsulation and electronic radiation, and while being mainly used in filling up bi-material joint or contact, the microvoid of generation and the hole of surface irregularity, reduce heat transfer contact thermal resistance, improves device heat dispersion.Phase-change heat conductive material is wherein main one.
Traditional phase-change heat conductive material is to utilize polymer technology, is mixed with phase transformation fillers such as organic polymer material, heat conductive filler and paraffin.This material at high temperature becomes liquid, easily pollutes periphery electronic devices and components, needs in use to use silk screen printing, has increased operation sequence, uses inconvenient operation., under long term high temperature state, use, the easy aging exsiccation of phase-change heat conductive material, has dissociant to separate out and sticks on electronic devices and components plate meanwhile, pollutes and damages electronic devices and components plate.
Summary of the invention
The object of this invention is to provide a kind of phase-change microcapsule thermally conductive material, can directly fit on electronic devices and components plate, under the condition of high temperature, can not become liquid, can not paste, damage electronic devices and components plate.
Phase-change microcapsule thermally 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 5%～13%, paraffin-vinylformic acid phase-change microcapsule 10%～30%, heat conduction powder 40%～70%, ethenyl blocking silicone oil 6%～20%.
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 60 μ m～80 μ m, the particle size of middle particle diameter heat conduction powder is 35 μ m～45 μ m, and the particle size of small particle size heat conduction powder is 1 μ m～4 μ m.
Further, described heat conduction powder is one or more the arbitrary proportion mixture in aluminum oxide, boron nitride, aluminium nitride, silicon carbide.
In above-mentioned raw materials, 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 take 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 ℃～60 ℃ 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 phase-change microcapsule thermally conductive material of the present invention adds the ethenyl blocking silicone oil of described weight percent in the A component of described weight percent dual composition addition type liquid silastic and mixes, add again heat conduction powder and paraffin-vinylformic acid phase-change microcapsule of 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, phase-change microcapsule thermally conductive material of the present invention can adopt following method preparation:
1). take paraffin as core, vinylformic acid is wall material, adopts situ aggregation method to prepare 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 60 μ m～80 μ m, particle size 35 μ m～45 μ m, particle size 1 μ m～4 μ m is removed after moisture in 200 ℃ 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). 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;
4). to step 3) liquid in add the heat conduction powder raw material of described weight percent, 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, under 80Pa～150Pa vacuum tightness, be fully uniformly mixed and obtain sizing material;
5). sizing material is poured in mould, in vulcanizing press, under 180 ℃～240 ℃, 10MPa～20MPa, vulcanizes 1min～3min, and moulding obtains phase-change microcapsule thermally conductive material;
6). at the two sides of phase-change microcapsule thermally conductive material laminating release film, not impaired with protecting materials surface.
According to using needs, the above-mentioned phase-change microcapsule thermally conductive material preparing can be cut into the product of different size and shape.
Wherein, described step 4) in stir speed (S.S.) be 100rpm～200rpm, churning time 10min～20min.
Phase-change microcapsule thermally conductive material of the present invention belongs to heat and strengthens polymkeric substance, thermal conductivity is high, and thermal resistance is low, has good heat conductivility, thermal resistance value between the radiator element that can make electronic devices and components and be attached thereto is reduced to minimum, and it is best that the heat dispersion of radiator element reaches.In the time reaching the working temperature of electronic devices and components, phase-change microcapsule thermally conductive material deliquescing (but can not become liquid), be easy to just fit with two matching surfaces, and then promote the reliability of the radiating elements such as microprocessor, memory module DC/ DC transmodulator and power model.
Phase-change microcapsule thermally conductive material of the present invention uses very simple, convenient, only need remove the release film on phase-change microcapsule thermally conductive material surface, directly fit on radiator element or electronic devices and components plate, can play good radiating effect, the natural binding property of material is good, without material or radiator element are carried out to preheating, do not need the silkscreen process of traditional phase-change heat conductive material simultaneously yet, greatly improve working efficiency.
Phase-change microcapsule thermally conductive material of the present invention, due to phase change material is encapsulated in microcapsule, uses under long term high temperature state, and material can not become liquid yet, can not paste, damage electronic devices and components plate, and life-time service also can not pollute electronic devices and components.
Embodiment
Embodiment 1
Take respectively the aluminum oxide 14g of the aluminum oxide 42g, the median size 40 μ m that toast dewatered median size 70 μ m at 200 ℃, the aluminium nitride 7g of median size 1 μ m, be mixed to get heat conduction powder raw material.
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 heat conduction powder raw material, paraffin-vinylformic acid phase-change microcapsule of 15g 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 ℃, 10MPa, vulcanizes 3min, obtains phase-change microcapsule thermally conductive material.
Finally, release film in the laminating of the two sides of the phase-change microcapsule thermally conductive material obtaining.
Embodiment 2
The aluminum oxide 15g, the boron nitride 5g of median size 2 μ m that take respectively the aluminum oxide 35g, the median size 45 μ m that at 200 ℃, toast dewatered median size 75 μ m, be mixed to get heat conduction powder raw material.
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 heat conduction powder raw material, paraffin-vinylformic acid phase-change microcapsule of 23g 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 ℃, 15MPa, vulcanizes 1min, obtains phase-change microcapsule thermally conductive material.
Finally, release film in the laminating of the two sides of the phase-change microcapsule thermally conductive material obtaining.
Embodiment 3
Take respectively the silicon carbide 12g of the silicon carbide 42g, the median size 35 μ m that toast dewatered median size 60 μ m at 200 ℃, the aluminium nitride 6g of median size 1 μ m, be mixed to get heat conduction powder raw material.
Take the ethenyl blocking silicone oil of 2g viscosity 30000cst, after mixing with the ethenyl blocking silicone oil of 6g viscosity 4000cst, add the A component 10g in dual composition addition type liquid silastic, mix, put into vacuum mixer, add above-mentioned heat conduction powder raw material, paraffin-vinylformic acid phase-change microcapsule of 24g 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 ℃, 13MPa, vulcanizes 2min, obtains phase-change microcapsule thermally conductive material.
Finally, release film in the laminating of the two sides of the phase-change microcapsule thermally conductive material obtaining.
Comparative example
For the performance of the phase-change microcapsule thermally conductive material product prepared of checking the present invention, the phase-change heat conductive material T-PCM 910 producing take laird company, for contrasting, carries out following test.
1) thermal conductivity test
The phase-change microcapsule thermally 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 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 phase-change microcapsule thermally 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 phase-change microcapsule thermally conductive material that a fritter embodiment 1～3 prepares, be placed in the crucible of DZ3335 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 phase-change microcapsule thermally 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.
Claims (8)
1. a phase-change microcapsule thermally conductive material, is prepared by the raw material of following weight per-cent: dual composition addition type liquid silastic 5%～13%, paraffin-vinylformic acid phase-change microcapsule 10%～30%, heat conduction powder 40%～70%, ethenyl blocking silicone oil 6%～20%.
2. phase-change microcapsule thermally 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 60 μ m～80 μ m, the particle size of middle particle diameter heat conduction powder is 35 μ m～45 μ m, and the particle size of small particle size heat conduction powder is 1 μ m～4 μ m.
3. phase-change microcapsule thermally 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, boron nitride, aluminium nitride, silicon carbide.
4. phase-change microcapsule thermally 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 ℃～60 ℃ of transformation temperatures, latent heat of phase change >=140J/g.
5. phase-change microcapsule thermally 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.
6. the preparation method of claim 1 phase-change microcapsule thermally conductive material, that 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 mixed, add again heat conduction powder and paraffin-vinylformic acid phase-change microcapsule of 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.
7. the preparation method of claim 2 phase-change microcapsule thermally conductive material, comprises the following steps:
1). take paraffin as core, vinylformic acid is wall material, adopts situ aggregation method to prepare 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 60 μ m～80 μ m, particle size 35 μ m～45 μ m, particle size 1 μ m～4 μ m is removed after moisture in 200 ℃ 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). 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;
4). to step 3) liquid in add the heat conduction powder raw material of described weight percent, 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, under 80Pa～150Pa vacuum tightness, be fully uniformly mixed and obtain sizing material;
5). sizing material is poured in mould, in vulcanizing press, under 180 ℃～240 ℃, 10MPa～20MPa, vulcanizes 1min～3min, and moulding obtains phase-change microcapsule thermally conductive material;
6). at the two sides of phase-change microcapsule thermally conductive material laminating release film, not impaired with protecting materials surface.
8. the preparation method of phase-change microcapsule thermally conductive material according to claim 7, is characterized in that described step 4) in stir speed (S.S.) be 100rpm～200rpm, churning time 10min～20min.
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