CN104650817A - Heat conductive phase-change material and production method thereof - Google Patents
Heat conductive phase-change material and production method thereof Download PDFInfo
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- C09K5/02—Materials undergoing a change of physical state when used
- C09K5/06—Materials undergoing a change of physical state when used the change of state being from liquid to solid or vice versa
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Abstract
The invention relates to a heat conductive phase-change material which consists of the following components in percentage by weight: 75-90% of heat conductive filler, 2-8% of low-melting-point solid resin, 5-15% of liquid resin, 0.01-1% of an antioxidant and 0.02-2% of a coupling agent, and the phase-change material is prepared through a production method of mixing raw materials, mixing the heat conductive filler, pressing and forming, and cooling. The heat conductive phase-change material, which is prepared by mixing the heat conductive filler, the low-melting-point solid resin, the liquid resin, the antioxidant and the coupling agent, disclosed by the invention has the advantages that the phase-change material is in a shape of flaky solid at room temperature, so that the material is convenient in using and operation and can be directly attached on the surface of a heat-radiating component; when the component runs to the working temperature of the heat conductive phase-change material, phase change occurs and the material becomes soft, so as to wet the surface of the component to a great extent, and contact thermal resistance is reduced to the lowest so as to guarantee a heat conductive interstitial property better than that of heat conductive grease or a graphite flake; in addition, with excellent thixotropy, the material, when being used in a vertical direction, is protected away from circumstance of overflow or flowing.
Description
Technical field
The present invention relates to a kind of heat conduction phase change material and production method thereof.
Background technology
Now, the thermally conductive material used by hot INTERFACE DESIGN generally adopted is mainly the equal hot materials of heat conduction such as paste heat conduction lipid, heat-conducting pad or graphite flake, be placed between heating and radiating element during use, mainly through heat conducting mechanism, produced heat is delivered on radiating element and distributes.But above-mentioned thermally conductive material often exists different inferior positions, as under the effect that paste thermal grease conduction series products changes at temperature cycle, can occur progressively to overflow, be commonly called as " oil impregnate ", thus cause thermally conductive material reliability to reduce, and there is short-circuit risks between device; And heat-conducting pad fills the restriction of powder because of it, thinner gap cannot be applicable to, and because of main body base material elastic properties, make interface wet ability slightly poor, thus limit its heat conductivility, cannot be applied on high-power equipment or device.
Heat conduction phase-transition material is an analog thermoplastic material, it is solid under normal temperature, be warmed up to after more than phase change temperature and can become liquid state or cream state absorbing the heat that distributes of thermal source, thus fill device surface voids largely, get rid of " poor conductor of heat " air, realize good interface wet ability, show excellent heat conductivility; And be cooled to revert to after below phase change temperature solid, thus avoid spillover, operate simple and easy.
Summary of the invention
The technical problem to be solved in the present invention is just to provide a kind of heat conduction phase change material and production method thereof, solves the defect that existing heat conduction phase change material exists.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions: a kind of heat conduction phase change material, is made up of the component of following weight percent: heat conductive filler 75 ~ 90%, low melting point solid resin 2 ~ 8%, liquid resin 5 ~ 15%, antioxidant 0.01 ~ 1%, coupling agent 0.02 ~ 2%.
Preferably, be made up of the component of following weight percent: heat conductive filler 85%, low melting point solid resin 4%, liquid resin 10%, antioxidant 0.5%, coupling agent 0.5%.
Preferably, be made up of the component of following weight percent: heat conductive filler 77%, low melting point solid resin 7%, liquid resin 14%, antioxidant 0.75%, coupling agent 1.25%.
Preferably, be made up of the component of following weight percent: heat conductive filler 88%, low melting point solid resin 3%, liquid resin 7%, antioxidant 0.25%, coupling agent 1.75%.
Preferably, described heat conductive filler is one or both mixture in aluminum oxide, zinc oxide, boron nitride, aluminium nitride, silicon nitride, silicon carbide, aluminium powder, copper powder, silver powder, graphite or two or more mixtures, the particle diameter of described heat conductive filler is 0.2 ~ 50 μm, can select heat conductive filler according to the final performance of product, Practical Performance is good.
Preferably, described low melting point solid resin is one or both mixture in paraffin, Microcrystalline Wax, silicon wax or two or more mixtures, the fusing point of described low melting point solid resin is 40 DEG C ~ 90 DEG C, in general, the production line working temperature of usual electronic components is lower than 40 DEG C, thus can in operation, heat conduction phase change material remains solid state; And the working temperature of electron device generally needs lower than 90 DEG C, and this temperature can make heat conduction phase change material be heated becomes liquid state or cream state mutually, be easy to wetting device surface.
Preferably, described liquid resin is be in a liquid state under normal temperature state, described liquid resin is polyhutadiene, polyisoprene, Polybutadiene Acrylonitrile, hydroxy-terminated polybutadienes, hydroxyl terminated polyisoprene, one or both mixture of hydroxyl terminated butadiene acrylonitrile copolymer or two or more mixtures, result of use is good, energy guarantee mixes with solid resin, good mixing effect.
Preferably, described antioxidant is 2,2-methylene-bis (4-methyl-6-tert-butylphenol), 2,6-tri-grades of butyl-4-methylphenols, four (β-(3,5-tri-grades of butyl-4-hydroxy phenyls) propionic acid) pentaerythritol ester, one or both mixture of tetraphenyl dipropyleneglycol or two or more mixtures, can effectively delay or suppress the carrying out of resinous polymer oxidising process, thus stop the aging of product and extend its work-ing life.
Preferably, described coupling agent is different tetra-n-butyl titanate, three Unimac 5680 isopropyl titanates, tetra isopropyl two (dioctyl phosphito acyloxy) titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, γ-aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, one or both mixture of γ-mercapto oxypropyl trimethyl silane or two or more mixtures, coupling agent is generally made up of two portions: a part is close inorganic group, can with inorganic heat conductive filler effect; Another part is close organic group, can with resin effect.Thus, improve the interface performance of resin and mineral filler, improve the dispersity of filling powder to improve processing characteristics, and then make product obtain good heat conductivility and mechanical property.
A production method for heat conduction phase change material, comprises the following steps:
A) low melting point solid resin, liquid resin, antioxidant and coupling agent are put into successively vessel in heating stirring and obtain uniform liquid form mixt, Heating temperature is 60 ~ 100 DEG C, and churning time is 20 ~ 40min, makes it to be melt into liquid state completely;
B) heat heat conductive filler in the liquid form mixt after step a) processes, and carry out heating mixing under vacuum, Heating temperature is 80 ~ 120 DEG C, and mixing time is 40 ~ 60min;
C) by step b) mixture that formed is pressed into sheet finished product, and press temperature is 100 ~ 120 DEG C;
D) by step c) the sheet finished product suppressed is cooled to room temperature and obtains heat conduction phase change material.
In sum, advantage of the present invention: the heat conduction phase change material be mixed by heat conductive filler, low melting point solid resin, liquid resin, antioxidant, coupling agent, at room temperature material is solid sheet material, easy to use and operation, can directly be attached at radiating element surface, when device operation reaches heat conduction phase change material working temperature, material starts to undergo phase transition deliquescing, thus soak device surface largely, its thermal contact resistance is reduced to minimum, and obtains the thermal gap characteristic being better than thermal grease conduction or graphite flake; In addition, the situation of overflowing or trickling can not be there is when its excellent thixotropy can ensure to use this material in the vertical direction.
Technique used in the present invention, simple to operate, production efficiency is high, and equipment investment cost is low; Meanwhile, because the practicality of heat conduction phase change material formula of the present invention is comparatively strong, its phase change material can be undergone phase transition repeatedly, so material is in not contaminated situation, is repeatedly can be shaped to desired size, there is not waste situation.
Embodiment
Embodiment one:
A kind of heat conduction phase change material, is made up of the component of following weight percent: heat conductive filler 84%, low melting point solid resin 5%, liquid resin 10%, antioxidant 0.5%, coupling agent 0.5%.
Described heat conductive filler is aluminum oxide, boron nitride, zinc oxide, the mixture of aluminium powder, described aluminum oxide, boron nitride, zinc oxide, the weight percent of aluminium powder is 5:1:1:3, the particle diameter of described heat conductive filler is not more than 20 μm, described low melting point solid resin is Microcrystalline Wax, the fusing point of described low melting point solid resin is 70 DEG C, described liquid resin is be in a liquid state under normal temperature state, described liquid resin is polyhutadiene, the mixture of polyisoprene, described polyhutadiene, the weight percent of polyisoprene is 2:1, antioxidant is 2, 2-methylene-bis (4-methyl-6-tert-butylphenol), coupling agent is different tetra-n-butyl titanate.
The production method that a kind of heat conduction phase change material from the above mentioned adopts, comprises the following steps:
A) liquid resin, 2 Microcrystalline Wax, polyhutadiene and polyisoprene are mixed into, vessel in heating of 2-methylene-bis (4-methyl-6-tert-butylphenol) and different tetra-n-butyl titanate putting into successively stirs and obtains uniform liquid form mixt, Heating temperature is 90 DEG C, churning time is 35min, makes it to be melt into liquid state completely;
B) add the heat conductive filler of aluminum oxide, boron nitride, zinc oxide, aluminium powder in the liquid form mixt after step a) processes successively, and carry out heating mixing under vacuum, Heating temperature is 100 DEG C, and mixing time is 55min;
C) by step b) mixture that formed is pressed into sheet finished product, and press temperature is 110 DEG C;
D) by step c) the sheet finished product suppressed is cooled to room temperature and obtains heat conduction phase change material.
Embodiment two:
A kind of heat conduction phase change material, is made up of the component of following weight percent: heat conductive filler 77%, low melting point solid resin 7%, liquid resin 14%, antioxidant 0.75%, coupling agent 1.25%.
Described heat conductive filler is zinc oxide, aluminium nitride, the mixture of silver powder, described zinc oxide, aluminium nitride, the weight percent of silver powder is 2:3:1, described low melting point solid resin is the mixture of paraffin and Microcrystalline Wax, the weight percent of described paraffin and Microcrystalline Wax is 2:1, described liquid resin is the mixture of polyisoprene and hydroxyl terminated polyisoprene, the weight percent of described polyisoprene and hydroxyl terminated polyisoprene is 3:1, described antioxidant is tetraphenyl dipropyleneglycol, described coupling agent is the mixture of three Unimac 5680 isopropyl titanates and sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, the weight percent of described three Unimac 5680 isopropyl titanates and sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester is 2:1.
The production method that a kind of heat conduction phase change material from the above mentioned adopts, comprises the following steps:
A) vessel in heating of the coupling agent that liquid resin low melting point solid resin, polyisoprene and hydroxyl terminated polyisoprene that paraffin and Microcrystalline Wax are mixed into are mixed into, tetraphenyl dipropyleneglycol and three Unimac 5680 isopropyl titanates and sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester are mixed into putting into successively stirs and obtains uniform liquid form mixt, Heating temperature is 80 DEG C, churning time is 30min, makes it to be melt into liquid state completely;
B) add zinc oxide in the liquid form mixt after step a) processes successively, heat conductive filler that aluminium nitride, silver powder are mixed into, and carry out heating mixing under vacuum, Heating temperature is 105 DEG C, and mixing time is 48min;
C) by step b) mixture that formed is pressed into sheet finished product, and press temperature is 115 DEG C;
D) by step c) the sheet finished product suppressed is cooled to room temperature and obtains heat conduction phase change material.
Embodiment three:
A kind of heat conduction phase change material, is made up of the component of following weight percent: heat conductive filler 88%, low melting point solid resin 3%, liquid resin 7%, antioxidant 0.25%, coupling agent 1.75%.
Described heat conductive filler is zinc oxide, aluminium powder, the mixture of graphite, described zinc oxide, aluminium powder, the weight percent of graphite is 2:3:1, described low melting point solid resin is the mixture of Microcrystalline Wax and silicon wax, the weight percent of described Microcrystalline Wax and silicon wax is 1:2, described liquid resin is the mixture of hydroxy-terminated polybutadienes and hydroxyl terminated butadiene acrylonitrile copolymer, the weight percent of described hydroxy-terminated polybutadienes and hydroxyl terminated butadiene acrylonitrile copolymer is 1:1, described antioxidant is four (β-(3, 5-tri-grades of butyl-4-hydroxy phenyls) propionic acid) mixture of pentaerythritol ester and tetraphenyl dipropyleneglycol, described four (β-(3, 5-tri-grades of butyl-4-hydroxy phenyls) propionic acid) weight percent of pentaerythritol ester and tetraphenyl dipropyleneglycol is 2:1, described coupling agent is γ-aminopropyl triethoxysilane.
The production method that a kind of heat conduction phase change material from the above mentioned adopts, comprises the following steps:
A) liquid resin low melting point solid resin, hydroxy-terminated polybutadienes and hydroxyl terminated butadiene acrylonitrile copolymer that Microcrystalline Wax and silicon wax are mixed into are mixed into, four (β-(3,5-tri-grades of butyl-4-hydroxy phenyls) propionic acid) antioxidant that is mixed into of pentaerythritol ester and tetraphenyl dipropyleneglycol and γ-aminopropyl triethoxysilane put into vessel in heating successively and stir and obtain uniform liquid form mixt, Heating temperature is 80 DEG C, churning time is 22min, makes it to be melt into liquid state completely;
B) add zinc oxide in the liquid form mixt after step a) processes successively, heat conductive filler that aluminium powder, graphite are mixed into, and carry out heating mixing under vacuum, Heating temperature is 90 DEG C, and mixing time is 60min;
C) by step b) mixture that formed is pressed into sheet finished product, and press temperature is 105 DEG C;
D) by step c) the sheet finished product suppressed is cooled to room temperature and obtains heat conduction phase change material.
By the heat conduction phase change material that heat conductive filler, low melting point solid resin, liquid resin, antioxidant, coupling agent are mixed, at room temperature material is solid sheet material, easy to use and operation, can directly be attached at radiating element surface, when device operation reaches heat conduction phase change material working temperature, material starts to undergo phase transition deliquescing, thus soaks device surface largely, its thermal contact resistance is reduced to minimum, and obtains the thermal gap characteristic being better than thermal grease conduction or graphite flake; In addition, the situation of overflowing or trickling can not be there is when its excellent thixotropy can ensure to use this material in the vertical direction.
Technique used in the present invention, simple to operate, production efficiency is high, and equipment investment cost is low; Meanwhile, because the practicality of heat conduction phase change material formula of the present invention is comparatively strong, its phase change material can be undergone phase transition repeatedly, so material is in not contaminated situation, is repeatedly can be shaped to desired size, there is not waste situation.
Claims (10)
1. a heat conduction phase change material, is characterized in that: be made up of the component of following weight percent: heat conductive filler 75 ~ 90%, low melting point solid resin 2 ~ 8%, liquid resin 5 ~ 15%, antioxidant 0.01 ~ 1%, coupling agent 0.02 ~ 2%.
2. a kind of heat conduction phase change material according to claim 1, is characterized in that: be made up of the component of following weight percent: heat conductive filler 85%, low melting point solid resin 4%, liquid resin 10%, antioxidant 0.5%, coupling agent 0.5%.
3. a kind of heat conduction phase change material according to claim 1, is characterized in that: be made up of the component of following weight percent: heat conductive filler 77%, low melting point solid resin 7%, liquid resin 14%, antioxidant 0.75%, coupling agent 1.25%.
4. a kind of heat conduction phase change material according to claim 1, is characterized in that: be made up of the component of following weight percent: heat conductive filler 88%, low melting point solid resin 3%, liquid resin 7%, antioxidant 0.25%, coupling agent 1.75%.
5. a kind of heat conduction phase change material according to any one of Claims 1-4, it is characterized in that: described heat conductive filler is one or both mixture in aluminum oxide, zinc oxide, boron nitride, aluminium nitride, silicon nitride, silicon carbide, aluminium powder, copper powder, silver powder, graphite or two or more mixtures, and the particle diameter of described heat conductive filler is 0.2 ~ 50 μm.
6. a kind of heat conduction phase change material according to any one of Claims 1-4, it is characterized in that: described low melting point solid resin is one or both mixture in paraffin, Microcrystalline Wax, silicon wax or two or more mixtures, and the fusing point of described low melting point solid resin is 40 DEG C ~ 90 DEG C.
7. a kind of heat conduction phase change material according to any one of Claims 1-4, it is characterized in that: described liquid resin is be in a liquid state under normal temperature state, described liquid resin is polyhutadiene, polyisoprene, Polybutadiene Acrylonitrile, hydroxy-terminated polybutadienes, hydroxyl terminated polyisoprene, one or both mixture of hydroxyl terminated butadiene acrylonitrile copolymer or two or more mixtures.
8. a kind of heat conduction phase change material according to any one of Claims 1-4, it is characterized in that: described antioxidant is 2,2-methylene-bis (4-methyl-6-tert-butylphenol), 2, one or both mixture of 6-tri-grades of butyl-4-methylphenols, four (β-(3,5-, tri-grades of butyl-4-hydroxy phenyls) propionic acid) pentaerythritol ester, tetraphenyl dipropyleneglycol or two or more mixtures.
9. a kind of heat conduction phase change material according to any one of Claims 1-4, it is characterized in that: described coupling agent is different tetra-n-butyl titanate, three Unimac 5680 isopropyl titanates, tetra isopropyl two (dioctyl phosphito acyloxy) titanic acid ester, sec.-propyl three (dioctylphyrophosphoric acid acyloxy) titanic acid ester, γ-aminopropyl triethoxysilane, γ-(2,3-epoxy third oxygen) propyl trimethoxy silicane, one or both mixture of γ-mercapto oxypropyl trimethyl silane or two or more mixtures.
10. the production method that adopts of a kind of heat conduction phase change material as claimed in claim 1, is characterized in that: comprise the following steps:
A) low melting point solid resin, liquid resin, antioxidant and coupling agent are put into successively vessel in heating stirring and obtain uniform liquid form mixt, Heating temperature is 60 ~ 100 DEG C, and churning time is 20 ~ 40min, makes it to be melt into liquid state completely;
B) add heat conductive filler in the liquid form mixt after step a) processes, and carry out heating mixing under vacuum, Heating temperature is 80 ~ 120 DEG C, and mixing time is 40 ~ 60min;
C) by step b) mixture that formed is pressed into sheet finished product, and press temperature is 100 ~ 120 DEG C;
D) by step c) the sheet finished product suppressed is cooled to room temperature and obtains heat conduction phase change material.
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| CN105348821A (en) * | 2015-11-06 | 2016-02-24 | 深圳德邦界面材料有限公司 | Phase change graphite heat conduction material with high thermal conductivity and preparation method |
| CN106188903A (en) * | 2016-08-29 | 2016-12-07 | 昆山裕凌电子科技有限公司 | Phase-change heat conductive material and preparation method thereof |
| CN106224547A (en) * | 2016-07-15 | 2016-12-14 | 上海阿莱德实业有限公司 | Sealing gasket is filled in a kind of phase transformation |
| CN106240037A (en) * | 2016-07-15 | 2016-12-21 | 上海阿莱德实业有限公司 | A kind of phase transformation packing matcrial of built-in graphite fibre |
| CN106752117A (en) * | 2016-12-12 | 2017-05-31 | 深圳德邦界面材料有限公司 | Modified graphite and preparation method thereof, organic siliconresin |
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| JP2018538690A (en) * | 2015-12-03 | 2018-12-27 | 深▲セン▼▲徳▼邦界面材料有限公司Ｓｈｅｎｚｈｅｎ Ｄａｒｂｏｎｄ Ｉｎｔｅｒｆａｃｅ Ｍａｔｅｒｉａｌｓ Ｃｏ．，Ｌｔｄ． | Rubber-modified phase change heat conductive material and method for producing the same |
| CN106240037B (en) * | 2016-07-15 | 2018-06-01 | 上海阿莱德实业股份有限公司 | A kind of phase transformation filling sealing material of built-in graphite fibre |
| CN106224547A (en) * | 2016-07-15 | 2016-12-14 | 上海阿莱德实业有限公司 | Sealing gasket is filled in a kind of phase transformation |
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Application publication date: 20150527 |