CN103788661A - Stress controlled high-thermal-conductivity high polymer interface material and preparation method thereof - Google Patents
Stress controlled high-thermal-conductivity high polymer interface material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a stress controlled high-thermal-conductivity high polymer interface material and a preparation method thereof, belonging to the technical field of high polymer interface materials. The interface material is composed of the following materials in parts by weight: 5-20 parts of organic silicon resins, 80-95 parts of thermal-conductive powdered filler, and 0-1 part of an interface treatment agent. The stress controlled high-thermal-conductivity high polymer interface material disclosed by the invention can control the size of a compressed product through the internal stress of the product so as to ensure that the high-thermal-conductivity high polymer interface material is closely adhered to a device; meanwhile, the high-thermal-conductivity interface material is soft, and the thermal conductivity coefficient can reach 4 W/mK.
Description
Technical field
The invention belongs to macromolecule interfacial material technology field, be specifically related to high heat-conducting polymer boundary material of a kind of stress control type and preparation method thereof.
Background technology
For a long time, find rationally effectively heat dissipation design scheme is the huge challenge that guarantees that electronic devices and components and the normal operation of associated electronic device face always.Show 2 ℃ of the every risings of electronic devices and components temperature, 1/6 when product when 10%, 50 ℃ of its reliability decrease only has 25 ℃ work-ing life according to data.Effective and reasonable heat dissipation design comprises active heat removal design and passive heat dissipation design.Nowadays,, along with the fast development of large-scale integrated circuit, under less, thinner, compacter size design requires, under operating frequency at a high speed requires, directly cause, except active heat removal design, passive Cooling Solution being had higher requirement.
Macromolecule thermal-conducting pad is used in electronic applications in a large number as the passive Cooling Solution of one, especially in communications industry, as communication equipment such as exchange board, router, RF base stations.Due to the development of communications industry, the especially drive of 3G, 4G technology, communication equipment is more and more higher to the performance requriements of macromolecule thermal-conducting boundary material, is mainly reflected in and needs high heat conductivility, interface laminating closely, reliable work-ing life etc.
At present, the thermal conductivity of perhaps of the heat-conducting pad of the stable domestic production of the comparative maturity that circulates on market is at 1-2W/mK, and individual other can reach 2.5W/mK.And for really can reach 3W/mK or more the product of high thermal conductivity coefficient almost can't see.In addition, heat-conducting pad use-pattern is to be mainly fixed between casing or casing and euthermic chip by the mode of lock screw, spacing between casing or casing and euthermic chip can be fixed like this, must cause requiring the size after the compression of heat-conducting pad to be fixed to guarantee fitting tightly of heat dissipation interface.Most of heat-conducting pads of domestic production are because much higher hard is pressed, shrinkage is low, if can be caused casing or casing to deform because product internal stress is too high after life-time service; If use the heat-conducting pad that soft rate of compression is high (many foreign), after life-time service, due to the stress relaxation of product own (cannot rationally control), can make heat-conducting pad size change, cause the contact force between casing or casing and heat-conducting pad to diminish, and then have influence on the tightness degree of fitting in interface, finally affect radiating effect.
Given this, need design and prepare a kind of have high thermal conductivity coefficient, product softness and there is the heat-conducting pad of stress control size capability, to guarantee thering is for a long time in actual applications stable high heat-sinking capability.
Summary of the invention
The present invention is directed to current macromolecule heat conduction material thermal conductivity low, the untight problem of laminating of heat-conducting interface material and device, proposes the high heat-conducting polymer boundary material of a kind of stress control type.
The present invention also aims to provide the preparation method of above-mentioned high heat-conducting polymer boundary material.
The high heat-conducting polymer boundary material of a kind of stress control type, is made up of the material of following parts by weight: silicone resin 5-20 part, conductive powder filler 80-95 part, interface treating agent 0-1 part;
Described silicone resin is siloxane-based resin;
Described conductive powder filler is by conductive powder A, conductive powder B, conductive powder C, conductive powder D, take conductive powder filler total mass mark as 100%, conductive powder A massfraction is 1-15%, and conductive powder B massfraction is 10-30%, conductive powder C massfraction is 20-50%, and conductive powder D massfraction is 30-60%;
Described conductive powder A is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 50nm-10um;
Described conductive powder B is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 2-20um;
Described conductive powder C is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 30-100um;
Described conductive powder D is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 15-80um.
Described siloxane-based resin is vinyldimethicone, apparent viscosity 100-800cp, gel hardness 20-80g.
Described interface treating agent is one or more in silane coupling agent, aluminate coupling agent, titanate coupling agent, silane crosslinker, dispersion agent, defoamer etc.
Described conductive powder A, conductive powder B, conductive powder C, the shape of conductive powder D is one or more the mixing in spherical, near-spherical, needle-like, sheet, broken shape, six side's shapes, prism-shaped etc.
The preparation method of the high heat-conducting polymer boundary material of above-mentioned stress control type, carries out in accordance with the following steps:
(1), under 0 ℃~30 ℃ conditions of temperature, silicone resin and interface treating agent are added in reactor and vacuumize and stir;
(2) add conductive powder A disposable or be divided into 2~5 equal portions or not equal portions be added to respectively in reactor, under vacuum state, stir simultaneously, wherein adding each time in the process of conductive powder A, respectively stirring velocity is adjusted to 50rpm by 10rpm, stirs 5-20 minute, stirring velocity is adjusted to 40rpm, stir 5-20 minute, repeat aforesaid operations, add and fill conductive powder B, conductive powder C and conductive powder D, make the slurry stirring;
(3) slurry stirring solidifies 10-40 minute at 110-150 ℃ of compacted under, gets final product to obtain the high heat-conducting polymer boundary material of stress control type.
Beneficial effect of the present invention: the high heat-conducting polymer boundary material of stress control type of the present invention can be by interiors of products stress control product itself size after compressed, to guarantee fitting tightly of macromolecule thermal-conducting boundary material and device, simultaneously, this heat-conducting interface material quality softness, thermal conductivity can reach 4W/mK.
Accompanying drawing explanation
Fig. 1 is the high heat-conducting polymer boundary material of stress control type practical application schematic diagram;
In figure, 1-radiator, 2-pyrotoxin, 3-heat-conducting interface material, the state before a-does not compress, b-is stressed to be compressed to 50% highly fixingly, after c-general interface material pressurized, occurs microcosmic gap, and d-material of the present invention still can guarantee that reduced size does not change.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention will be further described.
Embodiment 1
The preparation method of the high heat-conducting interface material of a kind of stress control type, comprise the following steps: the vinyldimethicone of 15g and 0.5g silane coupling agent are joined and in reactor, vacuumize mixing and stirring, add the conductive powder B (aluminum oxide of 10g, aluminium hydroxide) even to vacuum stirring in reactor, add again the conductive powder D (aluminum oxide of 37g, aluminium nitride) under vacuum state in reactor, stir, and then add the conductive powder A (zinc oxide of 8g, silver powder) stir under vacuum state, then add the conductive powder C (non-ball-aluminium oxide) of 30g.Finally, the slurry mixing is solidified 20 minutes at 110 ℃ of temperature, described in obtaining, there is the boundary material of high thermal conductivity coefficient.
Keep material compression ratio 50% condition lower 500 minutes, stress loss rate 80%, thermal conductivity 2.87W/mK, hardness 48 (Shore OO), compression schematic diagram is as shown in Figure 1.
The preparation method of the high heat-conducting interface material of a kind of stress control type, comprise the following steps: the vinyldimethicone of 10g and 0.6g aluminate coupling agent are joined and in reactor, vacuumize mixing and stirring, add the conductive powder B (aluminum oxide of 10g, aluminium hydroxide) even to vacuum stirring in reactor, add again the conductive powder D (aluminum oxide of 37g, boron nitride) under vacuum state in reactor, stir, and then add the conductive powder A (silicon oxide of 8g, silver powder) stir under vacuum state, then add the conductive powder C (ball-aluminium oxide) of 35g.Finally, the slurry mixing is solidified 30 minutes at 110 ℃ of temperature, described in obtaining, there is the boundary material of high thermal conductivity coefficient.
The above-mentioned method that adds conductive powder is: conductive powder is divided into 4 equal portions, be added to respectively in reactor, under vacuum state, stir simultaneously, wherein adding each time in the process of conductive powder, respectively stirring velocity is adjusted to 50rpm by 10rpm, stir 5-20 minute, stirring velocity is adjusted to 40rpm, stir 5-20 minute.
Keep material compression ratio 50% condition lower 500 minutes, stress loss rate 63%, thermal conductivity 3.60W/mK, hardness 51 (Shore OO), compression schematic diagram is as shown in Figure 1.
Embodiment 3
The preparation method of the high heat-conducting interface material of a kind of stress control type, comprise the following steps: the vinyldimethicone of 5g and 0.1g titanate coupling agent are joined and in reactor, vacuumize mixing and stirring, add 10g conductive powder B (silver powder, aluminium hydroxide) even to vacuum stirring in reactor, add again the conductive powder D (aluminium nitride of 47g, boron nitride) under vacuum state in reactor, stir, and then add 8g conductive powder A (silicon oxide, zinc oxide) stir under vacuum state, then add 30g conductive powder C (ball-aluminium oxide, aluminium nitride).Finally, the slurry mixing is solidified 30 minutes at 120 ℃ of temperature, described in obtaining, there is the boundary material of high thermal conductivity coefficient.
The above-mentioned method that adds conductive powder is: conductive powder is divided into 2 equal portions, be added to respectively in reactor, under vacuum state, stir simultaneously, wherein adding each time in the process of conductive powder, respectively stirring velocity is adjusted to 50rpm by 10rpm, stir 5-20 minute, stirring velocity is adjusted to 40rpm, stir 5-20 minute.
Keep material compression ratio 50% condition lower 500 minutes, stress loss rate 24%, thermal conductivity 4.52W/mK, hardness 75 (Shore OO), compression schematic diagram is as shown in Figure 1.
Embodiment 4
The preparation method of the high heat-conducting interface material of a kind of stress control type, comprise the following steps: 8g vinyldimethicone and 1g silane crosslinker are joined and in reactor, vacuumize mixing and stirring, add 10g conductive powder B (aluminum oxide) even to vacuum stirring in reactor, add again 44g conductive powder D (aluminum oxide, boron nitride) to stir under vacuum state in reactor, and then add under 8g conductive powder A (zinc oxide) vacuum state and stir, then add 30g conductive powder C (ball-aluminium oxide).Finally, the slurry mixing is solidified 30 minutes at 125 ℃ of temperature, described in obtaining, there is the boundary material of high thermal conductivity coefficient.
The above-mentioned method that adds conductive powder is: conductive powder is divided into 5 parts (not deciles), be added to respectively in reactor, under vacuum state, stir simultaneously, wherein adding each time in the process of conductive powder, respectively stirring velocity is adjusted to 50rpm by 10rpm, stir 5-20 minute, stirring velocity is adjusted to 40rpm, stir 5-20 minute.
Keep material compression ratio 50% condition lower 500 minutes, stress loss rate 33%, thermal conductivity 4.28W/mK, hardness 60 (Shore OO), compression schematic diagram is as shown in Figure 1.
Embodiment 5
The preparation method of the high heat-conducting interface material of a kind of stress control type, comprise the following steps: by 8g vinyldimethicone and 0.3g hexenyl bis-stearamides (dispersion agent), 0.2g silicone oil (defoamer) joins and in reactor, vacuumizes mixing and stirring, add 10g conductive powder B (aluminum oxide) even to vacuum stirring in reactor, add again the conductive powder D (aluminum oxide of 40g, boron nitride) under vacuum state in reactor, stir, and then add under conductive powder A (zinc oxide) vacuum state of 8g and stir, then add the conductive powder C (ball-aluminium oxide) of 34g.Finally, the slurry mixing is solidified 30 minutes at 125 ℃ of temperature, described in obtaining, there is the boundary material of high thermal conductivity coefficient.
The above-mentioned method that adds conductive powder is: by the conductive powder part that classifies in three categories, be added to respectively in reactor, under vacuum state, stir simultaneously, wherein adding each time in the process of conductive powder, respectively stirring velocity is adjusted to 50rpm by 10rpm, stir 5-20 minute, stirring velocity is adjusted to 40rpm, stir 5-20 minute.
Keep material compression ratio 50% condition lower 500 minutes, stress loss rate 38%, thermal conductivity 4.10W/mK, hardness 49 (Shore OO).
The foregoing is only preferred embodiment of the present invention, in order to limit the present invention, within the spirit and principles in the present invention not all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (5)
1. the high heat-conducting polymer boundary material of stress control type, is characterized in that, is made up of the material of following parts by weight: silicone resin 5-20 part, conductive powder filler 80-95 part, interface treating agent 0-1 part;
Described silicone resin is siloxane-based resin;
Described conductive powder filler is by conductive powder A, conductive powder B, conductive powder C, conductive powder D, take conductive powder filler total mass mark as 100%, conductive powder A massfraction is 1-15%, and conductive powder B massfraction is 10-30%, conductive powder C massfraction is 20-50%, and conductive powder D massfraction is 30-60%;
Described conductive powder A is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 50nm-10um;
Described conductive powder B is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 2-20um;
Described conductive powder C is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 30-100um;
Described conductive powder D is one or more the mixing in aluminum oxide, zinc oxide, aluminium powder, silver powder, boron nitride, aluminium nitride, copper powder, titanium oxide, aluminium hydroxide, graphite etc., and particle diameter is 15-80um.
2. the high heat-conducting polymer boundary material of a kind of stress control type according to claim 1, is characterized in that, described siloxane-based resin is vinyldimethicone, apparent viscosity 100-800cp, gel hardness 20-80g.
3. the high heat-conducting polymer boundary material of a kind of stress control type according to claim 1, it is characterized in that, described interface treating agent is one or more in silane coupling agent, aluminate coupling agent, titanate coupling agent, silane crosslinker, dispersion agent, defoamer etc.
4. the high heat-conducting polymer boundary material of a kind of stress control type according to claim 1, it is characterized in that, described conductive powder A, conductive powder B, conductive powder C, the shape of conductive powder D is one or more the mixing in spherical, near-spherical, needle-like, sheet, broken shape, six side's shapes, prism-shaped etc.
5. the preparation method of the high heat-conducting polymer boundary material of stress control type described in claim 1, is characterized in that, carries out in accordance with the following steps:
(1), under 0 ℃~30 ℃ conditions of temperature, silicone resin and interface treating agent are added in reactor and vacuumize and stir;
(2) add conductive powder A disposable or be divided into 2~5 equal portions or not equal portions be added to respectively in reactor, under vacuum state, stir simultaneously, wherein adding each time in the process of conductive powder A, respectively stirring velocity is adjusted to 30rpm by 10rpm, stirs 5-20 minute, stirring velocity is adjusted to 40rpm, stir 5-20 minute, repeat aforesaid operations, add and fill conductive powder B, conductive powder C and conductive powder D, make the slurry stirring;
(3) slurry stirring solidifies 10-40 minute at 110-150 ℃ of compacted under, gets final product to obtain the high heat-conducting polymer boundary material of stress control type.
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WO2017041454A1 (en) * | 2015-09-09 | 2017-03-16 | 中兴通讯股份有限公司 | High thermal conductivity composite interface material and preparation method therefor |
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CN112080258A (en) * | 2014-12-05 | 2020-12-15 | 霍尼韦尔国际公司 | High performance thermal interface material with low thermal resistance |
WO2017041454A1 (en) * | 2015-09-09 | 2017-03-16 | 中兴通讯股份有限公司 | High thermal conductivity composite interface material and preparation method therefor |
CN107057558A (en) * | 2016-09-13 | 2017-08-18 | 华北电力大学 | A kind of environment-friendly type heat conductive silicone grease composition and its preparation method and application |
CN107189767A (en) * | 2017-05-27 | 2017-09-22 | 广州中科检测技术服务有限公司 | A kind of high interface heat transfer effect, interface heat transfer material plastic, without pickup and preparation method thereof |
CN107189767B (en) * | 2017-05-27 | 2020-11-27 | 广州中科检测技术服务有限公司 | Plastic and non-fouling interface heat transfer material with high interface heat transfer effect and preparation method thereof |
CN111363358A (en) * | 2020-03-16 | 2020-07-03 | 平湖阿莱德实业有限公司 | Oriented high-thermal-conductivity interface material and preparation method thereof |
WO2022042176A1 (en) * | 2020-08-27 | 2022-03-03 | 深圳先进电子材料国际创新研究院 | Heat-conducting gel and preparation method therefor |
CN112608720A (en) * | 2020-11-25 | 2021-04-06 | 上海普力通新材料科技有限公司 | High-thermal-conductivity interface material and preparation method thereof |
CN112608720B (en) * | 2020-11-25 | 2021-12-14 | 上海普力通新材料科技有限公司 | High-thermal-conductivity interface material and preparation method thereof |
CN115386227A (en) * | 2021-12-09 | 2022-11-25 | 上海阿莱德实业股份有限公司 | Oriented high-thermal-conductivity interface material and preparation method thereof |
CN115612300A (en) * | 2022-11-03 | 2023-01-17 | 苏州泰吉诺新材料科技有限公司 | Heat-conducting gasket and preparation method thereof |
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