CN107603094A - A kind of preparation method of heat-conducting insulation material - Google Patents
A kind of preparation method of heat-conducting insulation material Download PDFInfo
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- CN107603094A CN107603094A CN201710929375.XA CN201710929375A CN107603094A CN 107603094 A CN107603094 A CN 107603094A CN 201710929375 A CN201710929375 A CN 201710929375A CN 107603094 A CN107603094 A CN 107603094A
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Abstract
The invention discloses a kind of preparation method of heat-conducting insulation material, belong to insulating materials field.The present invention is using silicon rubber as matrix, first dissolve silicon rubber at high temperature, mixed after dissolving with surface-active, reduce the surface tension of silicon rubber, improve group activity, utilizing vinylacetate, acetone soln, 2, the reagents such as 5 hexanes of dimethyl 2,5 pairs make polyvinyl alcohol, and polyvinyl alcohol has cohesive, the silicon rubber for reducing surface tension is merged therewith, so that material surface has viscosity；Using aluminum oxide, magnesia, carborundum as filler, improve the combination between both compatibilities of filler and silicone rubber matrix, enhancing interfaces by coupling agent so that the heat conductivility and mechanical property of silicon rubber composite material obtain a certain degree of improvement.The present invention is solved currently in order to make material surface have viscosity, and two-sided tape is attached to the surface of heat conductive isolation sheet, but the thermal conductivity of two-sided tape is low, the problem of causing the overall heat-conducting effect of heat-conducting insulation material to decline.
Description
Technical field
The invention belongs to insulating materials field, and in particular to a kind of preparation method of heat-conducting insulation material.
Background technology
Heat-conducting insulation material is a kind of conventional functional material, generally with shapes such as ceramics, plastics, rubber, adhesive, coating
Formula is widely used in the fields such as microelectronics Packaging, motor, automobile, special cable.In recent years, with semiconductor devices integrated technique
Develop rapidly, the integration degree more and more higher of semiconductor devices, design engineer makes every effort to install on smaller area
More semiconductor devices, to realize the miniaturization of instrument and equipment.To ensure that these highly integrated semiconductor devices can be steady
Fixed operation, heat caused by each electronic component effectively, timely must be delivered in surrounding environment.Usual way
It is that the metal heat sink of the high thermal conductivities such as copper, aluminium, increase radiating are installed on the electronic component surface for being integrated with semiconductor devices
Area.However, the surface of electronic component and radiator can not be definitely smooth, air is inevitably produced when both contact
Gap, the presence of air-gap cause radiating efficiency to substantially reduce.Therefore, in order to allow fin and heating device surface preferably tie
Close, make radiating effect more preferable, it is necessary to which the material of heat conduction is capable of in filling between radiator and electronic component.Common thermal conductive silicon
Fat and phase-change material have good heat-conducting effect, but electrical insulating property is poor, although soft heat conductivity gap filling material has
Certain electrical insulating property, but cannot be used for those needs the occasion of very high insulation, and this kind of material be suitable only for pressure compared with
Low application, it is impossible to competent as the field such as large power supply, automobile.Therefore the High-heat-conductiviinsulation insulation material of a kind of not only heat conduction but also insulation
It can be very good solve Heat Conduction Problems in the case where requiring high insulation conditions, heat-conducting insulation material effectively interface unit and can dissipate
Hot device, there is provided passage of heat is to reduce thermal resistance, and good electrical insulation properties can ensure the normal operation of device.At present
Heat-conducting insulation material can be generally divided into：Inorganic non-metallic heat-conducting insulation material：Usual metal (such as Au, Ag.Cu.Al, Mg
Deng) higher thermal conductivity is respectively provided with, but be conductor, so insulating materials is not used as, and part inorganic non-metallic material, such as
Metal oxide Al2O3, MgO, ZnO, NiO, metal nitride AIN, Si3N4, BN etc., and the ceramics such as SiC can then be used as it is exhausted
Edge material；Polymer matrix heat-conducting insulation material：Due to polymeric material have excellent electrical insulation properties, decay resistance,
Mechanical property, workability etc., therefore people progressively replace conventional electrical insulating materials, but most of polymerizations with polymeric material
The thermal conductivity of thing material is very low, can not be directly used as Heat Conduction Material, it is therefore desirable to by adding thermal conductivity material, becomes and leads
Heat insulator.Nowadays the heat-conducting insulation material routinely applied is the silicone resin composite material being fully cured, and it is usually to use
Silicones is base material, using the ceramic particle of the heat conductive insulatings such as aluminum oxide, aluminium nitride, zinc oxide as filler, although having certain
Effect, still, in actual use or there is some problems.Because the silicone surface of completion of cure is without viscous
Property, in use, displacement is easily slid during insulating materials is installed into radiator or device, especially hung down
When being operated in straight plane.In order that obtaining material surface has viscosity, currently used method is to be attached to two-sided tape
The surface of heat conductive isolation sheet so that heat-conducting insulation material surface has certain viscosity.But this method brings many drawbacks, one
Aspect, heat-conducting insulation material surface energy is very low, and adhesive tape can not be affixed directly to surface, it is necessary to expensive silicone band or by volume
Outer corona etc. is handled heat-conducting insulation material to improve material surface energy, then again with tape-stripping on surface.Using
Silicone band undoubtedly adds cost, and corona process is easy to produce destruction to material property especially insulating properties.It is another
Aspect, the thermal conductivity of two-sided tape are very low so that the overall heat-conducting effect of heat-conducting insulation material declines.Therefore a kind of height is prepared
Heat-conducting insulation material is very urgent.
The content of the invention
The technical problems to be solved by the invention：For currently in order to so that material surface has viscosity, conventional method
It is the surface that two-sided tape is attached to heat conductive isolation sheet, but the thermal conductivity of two-sided tape is very low, causes heat-conducting insulation material overall
Heat-conducting effect decline the problem of, there is provided a kind of preparation method of heat-conducting insulation material.
In order to solve the above technical problems, the present invention is using technical scheme as described below：
A kind of preparation method of heat-conducting insulation material, it is characterised in that the preparation method comprises the following steps：
（1）Silicon rubber is put into container, heated, when temperature is warming up to 110 ~ 120 DEG C, silicon rubber quality is added into container
10 ~ 15% surfactant, 20 ~ 30min is stirred, be incubated 3 ~ 4h, obtain stirring thing；
（2）Count in parts by weight, take 50 ~ 80 parts of vinylacetates, 40 ~ 60 parts of acetone solns, 3 ~ 4 parts of 2,5- dimethyl -2,5-
Double hexanes, 1 ~ 2 part of double thiobenzoate are estimated base ester and reacted, and reaction temperature is 30 ~ 60 DEG C, 1 ~ 2h of time, obtains reactant, presses
Mass ratio 10 ~ 15：8~10：5~6：1 ~ 2, reactant, stirring thing, methanol, sodium hydroxide are mixed, are heated to 35 ~ 45 DEG C,
Cooled down after 30 ~ 45min, obtain cooling thing；
（3）Count in parts by weight, take 12 ~ 15 parts of aluminum oxide, 5 ~ 10 parts of magnesia, 3 ~ 4 parts of coupling agents, 2 ~ 4
Part carborundum, 1 ~ 2 part of fatty acid amide carry out heating stirring, obtain heating stirring thing；
（4）In mass ratio 7 ~ 8：3 ~ 4, cooling thing, heating stirring thing are mixed, heated under vacuum
Stirring, is cooled to room temperature, solidifies, and collects solidfied material, produces heat-conducting insulation material.
The step（1）Middle surfactant be lauryl sodium sulfate, polyethylene glycol it is therein any one.
The step（3）Middle coupling agent is aminopropyl triethoxysilane, VTES, vinyl front three
TMOS it is therein any one.
The step（3）Middle heating-up temperature is 40 ~ 60 DEG C, and mixing speed is 250 ~ 300rpm.
The step（4）Middle vacuum is 0.08 ~ 0.1MPa, and heating-up temperature is 50 ~ 70 DEG C.
Compared with other method, advantageous effects are the present invention：
（1）The present invention is first dissolved silicon rubber at high temperature, mixed after dissolving with surface-active using silicon rubber as matrix,
The surface tension of silicon rubber is reduced, improves group activity, double using vinylacetate, acetone soln, 2,5- dimethyl -2,5-
During the reagents such as hexane make polyvinyl alcohol, in the presence of double thiobenzoates estimate base ester, by polyvinyl alcohol and activation
Silicon rubber carry out it is partially grafted, so as to add the cohesive of material, while by the silicon rubber for reducing surface tension and poly- second
Enol is merged, so as to further such that material surface has viscosity.
（2）Using aluminum oxide, magnesia, carborundum as filler in the present invention, filler and silicon rubber can be improved by coupling agent
Combination between both compatibilities of matrix body, enhancing interfaces so that the heat conductivility and mechanical property of silicon rubber composite material
A certain degree of improvement can be obtained.
Embodiment
Surfactant be lauryl sodium sulfate, polyethylene glycol it is therein any one.
Coupling agent be aminopropyl triethoxysilane, VTES, vinyltrimethoxy silane wherein
Any one.
A kind of preparation method of heat-conducting insulation material, the preparation method comprise the following steps：
（1）Silicon rubber is put into container, heated, when temperature is warming up to 110 ~ 120 DEG C, silicon rubber quality is added into container
10 ~ 15% surfactant, 20 ~ 30min is stirred, be incubated 3 ~ 4h, obtain stirring thing；
（2）Count in parts by weight, take 50 ~ 80 parts of vinylacetates, 40 ~ 60 parts of acetone solns, 3 ~ 4 parts of 2,5- dimethyl -2,5-
Double hexanes, 1 ~ 2 part of double thiobenzoate are estimated base ester and reacted, and reaction temperature is 30 ~ 60 DEG C, 1 ~ 2h of time, obtains reactant, presses
Mass ratio 10 ~ 15：8~10：5~6：1 ~ 2, reactant, stirring thing, methanol, sodium hydroxide are mixed, are heated to 35 ~ 45 DEG C,
Cooled down after 30 ~ 45min, obtain cooling thing；
（3）Count in parts by weight, take 12 ~ 15 parts of aluminum oxide, 5 ~ 10 parts of magnesia, 3 ~ 4 parts of coupling agents, 2 ~ 4
Part carborundum, 1 ~ 2 part of fatty acid amide carry out heating stirring, and heating-up temperature is 40 ~ 60 DEG C, and mixing speed is 250 ~
300rpm, obtain heating stirring thing；
（4）In mass ratio 7 ~ 8：3 ~ 4, cooling thing, heating stirring thing are mixed, heated under vacuum
Stirring, vacuum are 0.08 ~ 0.1MPa, and heating-up temperature is 50 ~ 70 DEG C, is cooled to room temperature, is solidified, and collects solidfied material, i.e.,
Obtain heat-conducting insulation material.
Example 1
Surfactant is lauryl sodium sulfate.
Coupling agent is aminopropyl triethoxysilane.
A kind of preparation method of heat-conducting insulation material, the preparation method comprise the following steps：
（1）Silicon rubber is put into container, heated, when temperature is warming up to 110 DEG C, silicon rubber quality 10% is added into container
Surfactant, stir 20min, be incubated 3h, obtain stirring thing；
（2）Count in parts by weight, take 50 parts of vinylacetates, 40 parts of acetone solns, 3 parts of 2,5- dimethyl -2,5- double hexane, 1
The double thiobenzoates of part are estimated base ester and reacted, and reaction temperature is 30 DEG C, time 1h, obtains reactant, in mass ratio 10：8：5：1,
Reactant, stirring thing, methanol, sodium hydroxide are mixed, 35 DEG C is heated to, is cooled down after 30min, obtain cooling thing；
（3）Count in parts by weight, take 12 parts of aluminum oxide, 5 parts of magnesia, 3 parts of coupling agents, 2 parts of carborundum, 1 part of fatty acid amide
Heating stirring is carried out, heating-up temperature is 40 DEG C, mixing speed 250rpm, obtains heating stirring thing；
（4）In mass ratio 7：3, cooling thing, heating stirring thing are mixed, heating stirring, vacuum are under vacuum
0.08MPa, heating-up temperature are 50 DEG C, are cooled to room temperature, are solidified, and collect solidfied material, produce heat-conducting insulation material.
Example 2
Surfactant is polyethylene glycol.
Coupling agent is VTES.
A kind of preparation method of heat-conducting insulation material, the preparation method comprise the following steps：
（1）Silicon rubber is put into container, heated, when temperature is warming up to 120 DEG C, silicon rubber quality 15% is added into container
Surfactant, stir 30min, be incubated 4h, obtain stirring thing；
（2）Count in parts by weight, take 80 parts of vinylacetates, 60 parts of acetone solns, 4 parts of 2,5- dimethyl -2,5- double hexane, 2
The double thiobenzoates of part are estimated base ester and reacted, and reaction temperature is 60 DEG C, time 2h, obtains reactant, in mass ratio 15：10：6：
2, reactant, stirring thing, methanol, sodium hydroxide are mixed, 45 DEG C is heated to, is cooled down after 45min, obtain cooling thing；
（3）Count in parts by weight, take 15 parts of aluminum oxide, 10 parts of magnesia, 4 parts of coupling agents, 4 parts of carborundum, 2 parts of fatty acid amides
Heating stirring is carried out, heating-up temperature is 60 DEG C, mixing speed 300rpm, obtains heating stirring thing；
（4）In mass ratio 2：1, cooling thing, heating stirring thing are mixed, heated under vacuum
Stirring, vacuum 0.1MPa, heating-up temperature are 70 DEG C, are cooled to room temperature, are solidified, and collect solidfied material, it is exhausted to produce heat conduction
Edge material.
Example 3
Surfactant is lauryl sodium sulfate.
Coupling agent is vinyltrimethoxy silane.
A kind of preparation method of heat-conducting insulation material, the preparation method comprise the following steps：
（1）Silicon rubber is put into container, heated, when temperature is warming up to 115 DEG C, silicon rubber quality 13% is added into container
Surfactant, stir 25min, be incubated 3.5h, obtain stirring thing；
（2）Count in parts by weight, take 65 parts of vinylacetates, 50 parts of acetone solns, the double hexanes of 3.5 parts of 2,5- dimethyl -2,5-,
1.5 parts of double thiobenzoates are estimated base ester and reacted, and reaction temperature is 45 DEG C, time 1.5h, obtains reactant, in mass ratio 13：
9：7：1.5, reactant, stirring thing, methanol, sodium hydroxide are mixed, 40 DEG C is heated to, is cooled down after 37min, must be cooled down
Thing；
（3）Count in parts by weight, take 13 parts of aluminum oxide, 7 parts of magnesia, 3.5 parts of coupling agents, 3 parts of carborundum, 1.5 parts of aliphatic acid
Acid amides carries out heating stirring, and heating-up temperature is 50 DEG C, mixing speed 275rpm, obtains heating stirring thing；
（4）In mass ratio 7.5：3.5, cooling thing, heating stirring thing are mixed, heated under vacuum
Stirring, vacuum 0.09MPa, heating-up temperature are 60 DEG C, are cooled to room temperature, are solidified, and collect solidfied material, it is exhausted to produce heat conduction
Edge material.
Reference examples：The heat-conducting insulation material of company of Nantong City production.
The heat-conducting insulation material of gained in examples detailed above and the heat-conducting insulation material of reference examples are detected, specific detection
It is as follows：
Universal testing machine test product is respectively adopted, tests its impact strength, tests thermal conductivity factor using heat transfer analysis instrument, utilizes
Its viscosity of viscosity meter and record data, test result are shown in Table 1.
Table 1：
Inherent viscosity η=1/c √ 2（ηsp-lnηr）, wherein η r are relative viscosity, and η sp are that specific viscosity η sp=η r-1, c are molten
Liquid concentration.
In summary, heat-conducting insulation material of the invention in actual use heat-conducting effect it is more preferable also more can shock resistance, value
It must promote.
Claims (5)
1. a kind of preparation method of heat-conducting insulation material, it is characterised in that the preparation method comprises the following steps：
（1）Silicon rubber is put into container, heated, when temperature is warming up to 110 ~ 120 DEG C, silicon rubber quality is added into container
10 ~ 15% surfactant, 20 ~ 30min is stirred, be incubated 3 ~ 4h, obtain stirring thing；
（2）Count in parts by weight, take 50 ~ 80 parts of vinylacetates, 40 ~ 60 parts of acetone solns, 3 ~ 4 parts of 2,5- dimethyl -2,5-
Double hexanes, 1 ~ 2 part of double thiobenzoate are estimated base ester and reacted, and reaction temperature is 30 ~ 60 DEG C, 1 ~ 2h of time, obtains reactant, presses
Mass ratio 10 ~ 15：8~10：5~6：1 ~ 2, reactant, stirring thing, methanol, sodium hydroxide are mixed, are heated to 35 ~ 45 DEG C,
Cooled down after 30 ~ 45min, obtain cooling thing；
（3）Count in parts by weight, take 12 ~ 15 parts of aluminum oxide, 5 ~ 10 parts of magnesia, 3 ~ 4 parts of coupling agents, 2 ~ 4
Part carborundum, 1 ~ 2 part of fatty acid amide carry out heating stirring, obtain heating stirring thing；
（4）In mass ratio 7 ~ 8：3 ~ 4, cooling thing, heating stirring thing are mixed, heated under vacuum
Stirring, is cooled to room temperature, solidifies, and collects solidfied material, produces heat-conducting insulation material.
2. heat-conducting insulation material preparation method according to claim 1, it is characterised in that the step（1）
Middle surfactant be lauryl sodium sulfate, polyethylene glycol it is therein any one.
3. heat-conducting insulation material preparation method according to claim 1, it is characterised in that the step（3）
Middle coupling agent is that aminopropyl triethoxysilane, VTES, vinyltrimethoxy silane are therein
Any one.
4. heat-conducting insulation material preparation method according to claim 1, it is characterised in that the step（3）
Middle heating-up temperature is 40 ~ 60 DEG C, and mixing speed is 250 ~ 300rpm.
5. heat-conducting insulation material preparation method according to claim 1, it is characterised in that the step（4）
Middle vacuum is 0.08 ~ 0.1MPa, and heating-up temperature is 50 ~ 70 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113416502A (en) * | 2021-05-14 | 2021-09-21 | 杨智童 | Insulating and heat-conducting double-sided adhesive tape and preparation method thereof |
| CN115521727B (en) * | 2022-09-15 | 2023-03-31 | 北京中能航科科技有限公司 | Color-changing adhesive tape for ammonia gas leakage detection and preparation method thereof |
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| CN105368059A (en) * | 2015-12-15 | 2016-03-02 | 苏州鑫德杰电子有限公司 | Anti-abrasion heat-conducting silicon rubber material and preparation method thereof |
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Patent Citations (3)
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| CN101225234A (en) * | 2008-02-01 | 2008-07-23 | 南京凯汇工业科技有限公司 | Heat conductive insulating material and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113416502A (en) * | 2021-05-14 | 2021-09-21 | 杨智童 | Insulating and heat-conducting double-sided adhesive tape and preparation method thereof |
| CN113416502B (en) * | 2021-05-14 | 2023-08-29 | 安徽富印新材料股份有限公司 | Insulating heat-conducting double-sided adhesive tape and preparation method thereof |
| CN115521727B (en) * | 2022-09-15 | 2023-03-31 | 北京中能航科科技有限公司 | Color-changing adhesive tape for ammonia gas leakage detection and preparation method thereof |
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