CN101225234A - Heat conductive insulating material and preparation method thereof - Google Patents
Heat conductive insulating material and preparation method thereof Download PDFInfo
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- CN101225234A CN101225234A CNA2008100189319A CN200810018931A CN101225234A CN 101225234 A CN101225234 A CN 101225234A CN A2008100189319 A CNA2008100189319 A CN A2008100189319A CN 200810018931 A CN200810018931 A CN 200810018931A CN 101225234 A CN101225234 A CN 101225234A
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Abstract
The invention discloses a heat-conducting insulation material and a preparation method; concretely, by weight, ethylene silicone 20 to 60 portion, heat-conducting powder 40 to 80 portion, coupling agent 0.1 to 1.5 portion, antifoamer 2 to 5 portion, white carbon black 2 to 5 portion are mixed evenly, solidified and moulded to form the heat-conducting insulation material. Glass fiber or polyethylene naphthalate (PEN) or polyimide film is adopted to strengthen the penetration resistance and the tear resistance in the process of application. The insulation material is used between an electronic device and a radiator in a power supply, an automobile, a generator and other devices, can cram the unevenness surface between the electronic device and the radiator, and so reduce the thermal resistance, and accelerate the heat transfer.
Description
Technical field
The invention belongs to the organic silicon chemical field, relate to a kind of insulating interface thermally conductive material and preparation method thereof.
Background technology
The circuit layout of modern electronic equipment equipment becomes increasingly complex, and integrated level is more and more higher.The design engineer makes every effort to install more device on littler area, to realize the plant and instrument miniaturization.Guarantee that these highly integrated devices can steady running, the heat that each electronic component produced must be delivered in the surrounding environment effectively, in time and go.Usual method is the metal heat sink that high thermal conductivities such as copper, aluminium are installed at device surface, increases area of dissipation simultaneously.Fan further is installed above scatterer, is made Forced Air Convection, quicken heat passage.Yet the surface of electron device and scatterer all can not be definitely smooth, produces air gap when both contact inevitably.Because the thermal conductivity of air has only 2.3 * 10
-2W/mK, ten thousand of not enough metal heat-conducting rate/, the existence of air gap reduces the efficient of scatterer greatly.Expedited the emergence of the interface thermally conductive material in order to address this problem.
The heat-conducting silicone grease of employing surface wettability, the good property that flows is filled the air gap between device and the scatterer during beginning.But heat-conducting silicone grease uses inconvenient, pollutes circuit card easily and causes faults such as short circuit, and through repeatedly running off, become dry after the cold cycling, increases thermal resistance on the contrary.The appearance of phase-change heat conductive material and thermally conductive gel has partly solved the heat-conducting silicone grease inconvenient problem with use, but they are the same with heat-conducting silicone grease, need can not be used to the occasion of electrical isolation.Though soft docile heat conductivity gap filling material has certain electrical insulating property, but still can not be used for the very high insulating occasion of those needs, and this class material only is suitable for the lower application of pressure, his not competent big situation of vibrations such as power power-supply, gas automobile, generator that resembles.
Summary of the invention
The heat-conducting insulation material that the purpose of this invention is to provide a kind of high efficiency and heat radiation, this heat-conducting insulation material are used between heating electronic component and the scatterer, reduce thermal contact resistance, enhance heat transfer effect and and the anti-ability that penetrates, tears arranged.
Another object of the present invention provides the method for producing this heat-conducting insulation material.
Purpose of the present invention can be realized by following technology path:
A kind of heat-conducting insulation material is characterized in that this heat-conducting insulation material is mainly made by the component that contains following weight part:
Vinyl polysiloxane: 20～60 weight parts
Heat conduction powder: 40～80 weight parts
Coupling agent: 0.1～1.5 weight part
Defoamer: 2～5 weight parts
White carbon black: 2～5 weight parts.
In order to adapt to the application under the high pressure, also compound with glass fibre enhancing or enhanced film, described enhanced film is PEN or Kapton.The present invention adds PEN (PEN) or Kapton (Kapton) or the glass fibre that E.I.Du Pont Company produces in the vinyl polysiloxane layer.Film can be crossed and significantly improve that heat-conducting insulation material anti-penetrates, the performance of anti tear, compares with glass fibre, and reinforced effects is more obvious, and product thickness can be thinner.According to the different requirements of product to thermal conductivity and intensity, the thickness of enhanced film is 0.013～0.102mm.
The present invention, combines the powder filler of heat conduction, through being solidified into the thermally conductive material of specified shape as tackiness agent with heat-staple vinyl polysiloxane.Except playing the adherent effect, itself also has certain rigidity, flowability, stretchiness to vinyl polysiloxane in prescription, can control hardness, compliance and the viscosity of product by adding the vinyl polysiloxane of different qualities.According to the different requirements of product to thermal conductivity and kindliness, the used parts by weight of vinyl polysiloxane are also different.The present invention can use viscosity 50～5000cps, the vinyl polysiloxane of hardness 1～25 (Shore 00).
The heat conduction powder itself has higher heat conductivity, and its kind, content, size and degree of scatter are the important factors that influences the product thermal conductivity.Heat conduction powder of the present invention is one or several combinations in aluminum oxide, magnesium oxide, aluminium nitride, the boron nitride, also can be the combination of the different-grain diameter of one or several heat conduction powders.
In order to eliminate the bubble that produces in the course of processing, can add defoamer.Defoamer is a kind of in the organopolysiloxane, is phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methyl chloride phenyl silicone oil, methyl ethoxy silicone oil, methyl trifluoro propyl silicone oil, methyl ethylene silicone oil, methyl hydroxy silicon oil, ethyl containing hydrogen silicone oil or hydroxyl hydrogen silicone oil.Its surfactivity stops the generation of bubble in the colloid.
In order to improve the degree of scatter of heat conduction powder in resin, powder surface is handled (powder floods with the coupling agent ethanolic soln) with coupling agent.Coupling agent can be molecule R-Si-with following structural formula (OR ')
3, wherein, R is the above alkyl of six carbon, R ' is methyl or ethyl.As: n-hexyl Trimethoxy silane, n-octyl triethoxyl silane, positive decyl triethoxyl silane.
The preparation method of above-mentioned heat-conducting insulation material comprises:
A, take by weighing vinyl polysiloxane, stir;
B, add defoamer, white carbon black again, continue to stir evenly;
C, add the heat conduction powder of coupling agent dip treating again, under vacuum condition, stir and make raw mix;
D, with after the raw mix compression molding, under 100～180 ℃ of conditions, solidify.In addition, the preparation method of the heat-conducting insulation material of adding enhanced film is:
A, take by weighing vinyl polysiloxane, stir;
B, add defoamer, white carbon black again, continue to stir evenly;
C, add the heat conduction powder of coupling agent treatment again, under vacuum condition, stir and make raw mix;
D, raw mix is coated on surface treated enhanced film or in raw mix, adds glass fibre after, under 100～180 ℃ of conditions, solidify.
Wherein, the described raw mix of " d " step is coated on the one side or the two sides of enhanced film by roller coat, blade coating or printing.Enhanced film before coating through surface treatment to improve the bonding force of itself and silicone compound.Surface treatment comprises corona discharge, coating bonding reinforcing agent.Mixing process is carried out under the dustless condition of room temperature among the above-mentioned preparation method, and process time is decided by the amount and the stirring efficiency of raw material.
The present invention can also add silicon-dioxide powdery and regulate the preceding mixture stickiness of curing and solidify back product rebound resilience, the loss of reduction silicone oil, and its ratio is 2～5 weight parts.
The present invention regulates the rebound resilience and the oil yield of product with white carbon black.
Beneficial effect of the present invention:
Heat-conducting insulation material of the present invention can be used for the occasion of insulating requirements high (up to 10000kV).Heat-conducting insulation material voltage breakdown of the present invention improves 35% with respect to other glass fibre enhanced insulating material.In addition, film of the present invention strengthens tensile strength and reaches more than the 50MPa, is 10 times of other glass fibre enhanced insulating material; Elongation at break reaches 85%, is 4 times of other glass fibre enhanced insulating material.Insulating material of the present invention can be used for can filling up irregular surface between the two between electron device such as power power-supply, automobile, generator and the scatterer, thereby reduces thermal resistance, accelerated heat transmission.
Embodiment
The following examples just are used for describing in detail superiority of the present invention, and the manufacturing and the application of heat-conducting insulation material of the present invention are not limited to this.
The performance test methods of heat-conducting insulation material is as follows among the embodiment:
Heat-conducting insulation material is clipped in the middle of hot plate and the scatterer, with thermosensitive resistance measurement hot-plate, heat-conducting insulation material and radiator temperature changing conditions.
Embodiment 1:
(1) with 20g viscosity 500cps, the vinyl polysiloxane of hardness 5 (shore 00) is put into agitator and is stirred, and with its mixing, temperature is a room temperature.
(2) take by weighing the agitator that defoamer phenyl silicone oil 5g, white carbon black 5g put into step (1) and stir 20min.
(3) take by weighing mean diameter be 40 microns aluminum oxide 40g through containing the ethanolic soln dip treating of n-hexyl Trimethoxy silane 1g, after the oven dry, the agitator of putting into step (2) vacuumizes to stir made raw mix in 1 hour.
(4) solidify down at 150 ℃ behind the raw mix compressing tablet, be heat-conducting insulation material after 30min comes out.
(5) heat-conducting insulation material of step (4) being put into the hardness proofing unit tests.
(6) device of the heat-conducting insulation material of step (4) being put into the heat conduction detection detects thermal conductivity.
(7) device of the heat-conducting insulation material of step (4) being put into the voltage breakdown detection detects voltage breakdown.
The data presentation of test, thickness is 0.5mm, and the thermal conductivity of this heat-conducting insulation material is 2.5W/mK, and hardness is 60 (shore 00); When pressure was 0psi, during electronic component power 14w, the temperature of chip was 60 ℃, and the temperature of heat-conducting insulation material is 53 ℃; Voltage breakdown is 6000kV.
Embodiment 2:
(1) with 60g viscosity 5000cps, the vinyl polysiloxane of hardness 25 (shore 00) is put into agitator and is stirred, and with its mixing, temperature is a room temperature.
(2) take by weighing the agitator that defoamer Methyl Hydrogen Polysiloxane Fluid 2g, white carbon black 2g, silicon-dioxide powdery 4g put into step (1) and stir 20min.
(3) taking by weighing diameter is that the agitator of putting into step (2) after ethanolic soln dip treating through containing positive decyl triethoxyl silane 0.5g of 40 microns boron nitride 80g, the oven dry vacuumizes to stir and made raw mix in 1 hour.
(4) solidify down at 100 ℃ behind PEN (PEN) film that the 0.1mm that 80 ℃ of lower rolls of raw mix are applied to coated bonding reinforcing agent is thick, be heat-conducting insulation material after 30min comes out.
(5) heat-conducting insulation material of step (4) being put into the hardness proofing unit tests.
(6) device of the heat-conducting insulation material of step (4) being put into the heat conduction detection detects thermal conductivity.
(7) device of the heat-conducting insulation material of step (4) being put into the voltage breakdown detection detects voltage breakdown.
The data presentation of test, thickness is 0.5mm, and the thermal conductivity of this heat-conducting insulation material is 3W/mK, and hardness is 70 (shore00).When pressure was 0psi, during electronic component power 14w, the temperature of chip was 60 ℃, and the temperature of heat-conducting insulation material is 51 ℃.Voltage breakdown is 6500kV.
Embodiment 3:
(1) with 40g viscosity 50cps, the vinyl polysiloxane of hardness 15 (shore 00) is put into agitator and is stirred, and with its mixing, temperature is a room temperature.
(2) take by weighing the agitator that defoamer methyl ethoxy silicone oil 3g, white carbon black 3g put into step (1) and stir 20min.
(3) taking by weighing diameter is that agitator that the aluminium nitride of 40 microns magnesium oxide and 50 microns is put into step (2) altogether after the ethanolic soln dip treating of 60g through containing positive decyl triethoxyl silane 1g, the oven dry vacuumizes to stir and makes raw mix after being 1 hour.
(4) 80 ℃ of raw mixs are printed in curing under 120 ℃ behind the 0.015mm of corona discharge thick polyimide film, are heat-conducting insulation material after 30min comes out.
(5) heat-conducting insulation material of step (4) being put into the hardness proofing unit tests.
(6) device of the heat-conducting insulation material of step (4) being put into the heat conduction detection detects thermal conductivity.
(7) device of the heat-conducting insulation material of step (4) being put into the voltage breakdown detection detects voltage breakdown.
The data presentation of test, thickness is 1mm, and the thermal conductivity of this heat-conducting insulation material is 2.8W/mK, and hardness is 65 (shore00).When pressure was 0psi, during electronic component power 14w, the temperature of chip was 60 ℃, and the temperature of heat-conducting insulation material is 52 ℃.Voltage breakdown is 10000kV.
Embodiment 4:
(1) with 40g viscosity 500cps, the vinyl polysiloxane of hardness 10 (shore 00) is put into agitation vat and is stirred, and with its mixing, temperature is a room temperature.
(2) take by weighing the agitation vat that defoamer ethyl containing hydrogen silicone oil 2g, white carbon black 2g, silicon-dioxide powdery 2g put into step (1) and stir 20min.
(3) taking by weighing mean diameter is that the agitation vat of putting into step (2) after ethanolic soln dip treating through containing n-octyl triethoxyl silane 1g of 80 microns boron nitride 50g, the oven dry stirs, and this process vacuumizes and stirs is 1 hour.
(4) 80 ℃ of raw mixs are printed in behind the thick Kapton of the 0.025mm of corona discharge and solidify down at 180 ℃, the 30min back of coming out is heat-conducting insulation material.
(5) heat-conducting insulation material of step (4) being put into the hardness proofing unit tests.
(6) device of the heat-conducting insulation material of step (4) being put into the heat conduction detection detects thermal conductivity.
(7) device of the heat-conducting insulation material of step (4) being put into the voltage breakdown detection detects voltage breakdown.
The data presentation of test, thickness is 0.5mm, and the thermal conductivity of this heat-conducting insulation material is 5W/mK, and hardness is 50 (shore00).When pressure was 0psi, during electronic component power 14w, the temperature of chip was 60 ℃, and the temperature of heat-conducting insulation material is 49 ℃.Voltage breakdown is 5000kV.
Embodiment 5:
(1) with 20g viscosity 2500cps, the vinyl polysiloxane of hardness 5 (shore 00) is put into agitation vat and is stirred, and with its mixing, temperature is a room temperature.
(2) take by weighing the agitation vat that defoamer hydroxyl hydrogen silicone oil 5g, white carbon black 5g put into step (1) and stir 20min.
(3) take by weighing diameter be 80 microns aluminium nitride 40g after containing n-octyl triethoxyl silane 0.1g ethanolic soln dip treating, oven dry, the agitation vat of putting into step (2) vacuumizes to stir made raw mix in 1 hour.
(4) in raw mix, solidify down at 130 ℃ behind the adding glass fibre, be heat-conducting insulation material after 30min comes out.
(5) heat-conducting insulation material of step (4) being put into the hardness proofing unit tests.
(6) device of the heat-conducting insulation material of step (4) being put into the heat conduction detection detects thermal conductivity.
(7) device of the heat-conducting insulation material of step (4) being put into the voltage breakdown detection detects voltage breakdown.
The data presentation of test, thickness is 0.5mm, and the thermal conductivity of this heat-conducting insulation material is 4W/mK, and hardness is 65 (shore00).When pressure was 0psi, during electronic component power 14w, the temperature of chip was 60 ℃, and the temperature of heat-conducting insulation material is 51 ℃.Voltage breakdown is 5000kV.
Claims (11)
1. heat-conducting insulation material is characterized in that this heat-conducting insulation material is mainly made by the component of following weight part:
Vinyl polysiloxane 20～60 weight parts
Heat conduction powder 40～80 weight parts
Coupling agent 0.1～1.5 weight part
Defoamer 2～5 weight parts
White carbon black 2～5 weight parts.
2. heat-conducting insulation material according to claim 1, it is characterized in that also strengthening with glass fibre or enhanced film compound, described enhanced film is PEN or Kapton, thickness is 0.013～0.102mm.
3. heat-conducting insulation material according to claim 1, the viscosity that it is characterized in that described vinyl polysiloxane is 50～5000cps, hardness 1～25 (Shore 00).
4. heat-conducting insulation material according to claim 1 is characterized in that described heat conduction powder is one or several combinations in aluminum oxide, magnesium oxide, aluminium nitride, the boron nitride, or the combination of the different-grain diameter of one or more heat conduction powders.
5. heat-conducting insulation material according to claim 1 is characterized in that described defoamer is a kind of in the organopolysiloxane.
6. the heat-conducting insulation material of stating according to claim 5 is characterized in that described organopolysiloxane is phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methyl chloride phenyl silicone oil, methyl ethoxy silicone oil, methyl trifluoro propyl silicone oil, methyl ethylene silicone oil, methyl hydroxy silicon oil, ethyl containing hydrogen silicone oil or hydroxyl hydrogen silicone oil.
7. heat-conducting insulation material according to claim 1 is characterized in that described coupling agent is to have formula R-Si-(OR ')
3Molecule; Wherein, R is the above alkyl of six carbon, and R ' is methyl or ethyl.
8. the preparation method of the described heat-conducting insulation material of claim 1 comprises:
A, take by weighing vinyl polysiloxane, stir;
B, add defoamer, white carbon black again, continue to stir evenly;
C, add heat conduction powder again, under vacuum condition, stir and make raw mix through the coupling agent dip treating;
D, with after the raw mix compression molding, under 100～180 ℃ of conditions, solidify.
9. the preparation method of heat-conducting insulation material according to claim 2 comprises:
A, take by weighing vinyl polysiloxane, stir;
B, add defoamer, white carbon black, continue to stir evenly;
C, add heat conduction powder again, under vacuum condition, stir and make raw mix through the coupling agent dip treating;
D, raw mix is coated on surface treated enhanced film or in raw mix, adds glass fibre after, under 100～180 ℃ of conditions, solidify.
10. according to the preparation method of claim 9, it is characterized in that the described raw mix of " d " step is coated on the one side or the two sides of enhanced film by roller coat, blade coating or printing.
11., it is characterized in that described surface treatment is corona discharge or coating bonding reinforcing agent according to the preparation method of claim 9.
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| CN2008100189319A CN101225234B (en) | 2008-02-01 | 2008-02-01 | Heat conductive insulating material and preparation method thereof |
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| CN2008100189319A CN101225234B (en) | 2008-02-01 | 2008-02-01 | Heat conductive insulating material and preparation method thereof |
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| CN101225234B CN101225234B (en) | 2010-08-11 |
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| CN113444497B (en) * | 2021-06-15 | 2022-04-08 | 苏州柯仕达电子材料有限公司 | Low-oil-yield heat-conducting gel and preparation method thereof |
| CN114589906A (en) * | 2022-03-12 | 2022-06-07 | 泉州爱丽卡新材料科技有限公司 | Novel concave-convex plastic suction product and plastic suction process |
| CN114854208A (en) * | 2022-04-26 | 2022-08-05 | 苏州阳池科技有限公司 | Heat-conducting silica gel gasket composite material and preparation method thereof |
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