CN107868465A - A kind of heat conductive insulating composite with anisotropic structure and preparation method thereof - Google Patents
A kind of heat conductive insulating composite with anisotropic structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of heat conductive insulating composite with anisotropic structure and preparation method thereof, and it is graphene arrangement form chain structure in matrix using silicon rubber as matrix, and composition has anisotropic passage of heat.The present invention makes full use of the excellent properties such as the high thermal conductivity factor of graphene itself and high intensity, is doped in polymeric matrix, provides new approaches to develop the polymer matrix composite of high heat conduction, improves deficiency of the traditional polymer on heat conductivility.
Description
Technical field
The invention belongs to rubber thermal conductive polymer field of compound material, and in particular to a kind of leading with anisotropic structure
Heat insulation composite material and preparation method thereof.
Background technology
With microelectronics integrated technology and the high speed development of hollow printed board high density packaging technique, packing density carries rapidly
Height, electronic component, the volume of logic circuit drastically reduce so that electronic instrument and equipment are increasingly towards light, thin, short, small side
To development.Under high-frequency work frequency, semiconductor operating thermal environment changes rapidly to high temperature direction, now, electronic component production
Raw heat is accumulated rapidly, increased, and at a temperature of use environment, the heat production of operation element makes the increase of electronic equipment heat, due to
Heat can not shed in time, cause the reduced lifetime of electronic product, reliability to reduce.When temperature often raises 2 DEG C, electronic component
Reliability will decline 10%;And temperature is when raising 50 DEG C, life-span of electronic component shortens 5 when raising 25 DEG C than temperature
Times.In order to ensure that electronic component being capable of long-time stable, reliable operation, it is necessary to efficiently control operating temperature.At present, often
Gauge material and conventional art reached bottleneck stage on the heat dissipation problem for solving electronic component, it is necessary to explore new technology and
Method.With the appearance of the superpower Heat Conduction Material such as CNT and graphene, the novel high polymer heat conduction of exploitation addition carbon material
Composite becomes new study hotspot.
The one kind of dimethyl silicone polymer (PDMS) as the macromolecule organic silicon polymer, there is high optical transmissibility, change
The characteristic such as inertia, cold resistance, nontoxic, non-flammable is learned, is widely used in bio-microelectromechanical system, microfluidic device and flexible electrical
The multiple fields such as sub- equipment.However, PDMS has high thermal expansion coefficient and low heat conductivity, prevent it from meeting dissipating for electronic system
Heat needs, so as to seriously constrain its application;It is a kind of miscellaneous with sp2 by carbon atom and graphene is as a kind of new material
Change the individual layer sheet structural plan film new material that track composition hexangle type is in honeycomb lattice, be an only carbon atom thickness
Two-dimensional material, it is that thickness is most thin in current material circle, maximum intensity, hardness are high, thermal conductivity highest and electric conductivity is best receives
Rice material.The thermal conductivity factor of graphene is up to 5300W/ (m.K), if it is compound with high molecular polymer, only needs very low
Content, thermal conductivity, mechanical property and heat endurance with regard to polymer can be greatly improved, so as to compensate for high polymer material in power
Learn, some shortcomings in hot property, thus there is huge answer in heat-transfer device, conductive devices, aerospace field etc.
Use potentiality.
In summary, the heat filling using graphene as heat conductive insulating composite, in the presence of high-intensity magnetic field, formed
Anisotropic structure so that heat conduction has directionality, will can effectively improve the heat conductivility of composite, while also have
Good mechanical property, therefore heat conductive insulating composite of the preparation containing graphene has important practical usage.
The content of the invention
It is an object of the invention to provide a kind of with the heat conductive insulating composite of anisotropic structure and its preparation side
Method, to which the heat conduction advantage of non magnetic graphene can be given full play to, make itself do not possess magnetic work(by the effect of high-intensity magnetic field
The graphene of energy has regular arrangement under high-intensity magnetic field, forms anisotropic structure, so that heat conduction has directionality, enters one
Step expands the application field of composite.
To achieve the above object, the present invention adopts the following technical scheme that:
The invention discloses a kind of heat conductive insulating composite with anisotropic structure, its feature is:It is described to lead
Heat insulation composite is graphene arrangement form chain structure in described matrix using silicon rubber as matrix, and forming has respectively
The passage of heat of anisotropy.
Wherein:The thickness of the heat conductive insulating composite is 0.5~2mm.Described silicon rubber be dimethyl silicone rubber,
Methyl vinyl silicone rubber or methyl phenyl vinyl silicone rubber.
The preparation method of above-mentioned heat conductive insulating composite, comprises the following steps:
(1) 100mg graphene oxides are added in 60mL absolute ethyl alcohols, ultrasonic disperse is uniform, then adds HCl regulations pH=
3~4, obtain the dispersion liquid of graphene oxide;
The 10mL ethanol solutions for containing 0.3g silane couplers are added slowly with stirring in the dispersion liquid, added
60 DEG C of water-bath 24h afterwards, it is then centrifuged for separating, gained solid product is washed into repeatedly with absolute ethyl alcohol and deionized water
Property, to remove unreacted silane coupler, 10~24h is finally dried under the conditions of 60~80 DEG C in vacuum drying oven, is obtained
The graphene of surface modification;
(2) graphene for the surface modification for being obtained step (1) is added in dispersant, 20~30min of ultrasound, then
Silicone rubber matrix is added, is stirred, then ultrasound is volatilized completely to dispersant, obtains mixture;Wherein, the graphene accounts for institute
The 0.1~2% of silicone rubber matrix quality is stated, the volume mass ratio of the dispersant and the silicone rubber matrix is 1mL:1.5~
3g;
The bubble removed in the mixture is vacuumized, is subsequently poured into mould, 80~100 DEG C of solidifications under high-intensity magnetic field
2h, make graphene arrangement form chain structure in matrix, so as to form with anisotropic passage of heat, that is, obtain target
Product heat conductive insulating composite.
Preferably, the silane coupler described in step (1) is octadecyl trimethoxysilane, the second of γ-aminopropyl three
TMOS or γ-methacryloxypropyl trimethoxy silane.
Preferably, the dispersant described in step (2) is Isosorbide-5-Nitrae-dioxane, dimethylformamide or tetrahydrofuran.
The average diameter of the graphene for the surface modification that step (1) is obtained be less than 10 μm, the number of plies be 5~10 layers, thickness
It is more than 120m for 3~8nm, specific surface area2/g。
Preferably, the size of high-intensity magnetic field described in step (2) is 10T.
Compared with the prior art, beneficial effects of the present invention are embodied in:
1st, graphene is non-magnetic flake material, it is difficult to be polarized under general magnetic field;But in the presence of high-intensity magnetic field, it is managed
Shape structure can arrange in polymeric matrix along field orientation, so as to form the polymer composite of orderly heat conduction chain.With
Isotropism heat-conductive composite material is compared, and under identical material and filling proportion, heat filling aligns easy formation
The passage of heat of directionality, the heat conductivility of polymer composites can be effectively improved.
2nd, the present invention makes full use of the excellent performances such as the high thermal conductivity factor of graphene itself and high intensity, adulterates
Into polymeric matrix, new approaches are provided to develop the polymer matrix composite of high heat conduction, traditional polymer is improved and exists
Deficiency on heat conductivility.
3rd, the present invention carries out surface modification to graphene, and it can be made more uniformly to disperse in the base, so as to more have
Reason forms heat conduction network, by controlling the content of graphene composite can be made to reach insulation effect.
4th, the inventive method is simple to operate, safe, short preparation period.
Brief description of the drawings
Fig. 1 is change schematic diagram of the heat conductive insulating composite microstructure under external magnetic field.
Fig. 2 is the profile scanning electron microscope of graphene filling PDMS composites behind application magnetic field.
Fig. 3 is the increase with graphene mass fraction, isotropic structure and anisotropic structure heat conductivity
Change.
Embodiment
Technical scheme is elaborated with reference to embodiment, following embodiments are with the technology of the present invention side
Implemented under premised on case, give detailed embodiment and specific operating process, but protection scope of the present invention is not
It is limited to following embodiments.
The graphene of surface modification used in following embodiments is prepared as follows:
100mg graphene oxides are added in 60mL absolute ethyl alcohols, ultrasonic disperse 1h, then add HCl regulations pH=3~4,
Obtain the dispersion liquid of graphene oxide;
10mL 95% ethanol solutions for containing 0.3g KH-570 are added slowly with stirring in dispersion liquid, after adding
60 DEG C of water-bath 24h, then 3000r/min centrifuge 5min, gained solid product absolute ethyl alcohol and deionized water are anti-
After backwashing is washed to neutrality, to remove unreacted silane coupler, is finally dried 10h under the conditions of 80 DEG C in vacuum drying oven, is obtained
Obtain the graphene of surface modification.
Embodiment 1
The present embodiment is prepared as follows heat conductive insulating composite, and (graphene accounts for silicone rubber matrix quality
0.2%):
The graphene of precise 0.044g surface modifications first, it is added in 10mL dispersants Isosorbide-5-Nitrae-dioxane, surpasses
Sound disperses 30min, then adds 20g PDMS component As, uniform stirring 10min, ultrasonic disperse 30min, adds 2g's
PDMS B components, ultrasound are volatilized completely to dispersant, obtain mixture;
The bubble removed in mixture is vacuumized, is subsequently poured into mould, 80 DEG C of solidification 2h, make stone under 10T high-intensity magnetic fields
Black alkene arrangement form chain structure in matrix, so as to form with anisotropic passage of heat, that is, obtain target product and lead
Heat insulation composite.
Fig. 1 is heat conductive insulating composite microstructure change schematic diagram under external magnetic field.
Fig. 2 is the profile scanning electron microscope of graphene filling PDMS composites behind application magnetic field, it can be seen that
Graphene is dispersed in PDMS in the form of sheets, by foring anisotropic structure in the presence of magnetic field, has obvious heat conduction
Path.
For influence of the contrast anisotropic structure to composite property, obtained by the present embodiment identical method each to same
Property structure composite, differ only in high-intensity magnetic field it is lower 80 DEG C solidification when do not apply high-intensity magnetic field.
Fig. 3 is the change of heat conductivity, it can be seen that being continuously increased with graphene content, multiple
The thermal conductivity of condensation material is consequently increased, when graphene content is 0.2wt%, isotropism and anisotropic composite material
Thermal conductivity is respectively:(when graphene content is 0wt%, isotropism and anisotropy are answered by 0.22W/m.K and 0.26W/m.K
The thermal conductivity of condensation material is respectively:0.178W/m.K and 0.179W/m.K), and can be clearly seen that, after application magnetic field
Anisotropic structure is formed, there is passage of heat, composite of the heat conductivity apparently higher than isotropic structure.
Embodiment 2
The present embodiment is prepared as follows heat conductive insulating composite, and (graphene accounts for silicone rubber matrix quality
0.5%):
The graphene of precise 0.11g surface modifications first, it is added in 10mL dispersants Isosorbide-5-Nitrae-dioxane, ultrasound
Disperse 30min, then addition 20g PDMS component As, uniform stirring 10min, ultrasonic disperse 30min, add 2g PDMS
B component, ultrasound are volatilized completely to dispersant, obtain mixture;
The bubble removed in mixture is vacuumized, is subsequently poured into mould, 80 DEG C of solidification 2h, make stone under 10T high-intensity magnetic fields
Black alkene arrangement form chain structure in matrix, so as to form with anisotropic passage of heat, that is, obtain target product and lead
Heat insulation composite.
For influence of the contrast anisotropic structure to composite property, obtained by the present embodiment identical method each to same
Property structure composite, differ only in high-intensity magnetic field it is lower 80 DEG C solidification when do not apply high-intensity magnetic field.
From figure 3, it can be seen that when graphene content is 0.5wt%, isotropism and anisotropic composite material
Thermal conductivity is respectively:0.26W/m.K and 0.29W/m.K, it is apparent that forming anisotropy knot after applying magnetic field
Structure, there is passage of heat, composite of the heat conductivity apparently higher than isotropic structure.
Embodiment 3
The present embodiment is prepared as follows heat conductive insulating composite, and (graphene accounts for silicone rubber matrix quality
1.0%):
The graphene of precise 0.22g surface modifications first, it is added in 10mL dispersants Isosorbide-5-Nitrae-dioxane, ultrasound
Disperse 30min, then addition 20g PDMS component As, uniform stirring 10min, ultrasonic disperse 30min, add 2g PDMS
B component, ultrasound are volatilized completely to dispersant, obtain mixture;
The bubble removed in mixture is vacuumized, is subsequently poured into mould, 80 DEG C of solidification 2h, make stone under 10T high-intensity magnetic fields
Black alkene arrangement form chain structure in matrix, so as to form with anisotropic passage of heat, that is, obtain target product and lead
Heat insulation composite.
For influence of the contrast anisotropic structure to composite property, obtained by the present embodiment identical method each to same
Property structure composite, differ only in high-intensity magnetic field it is lower 80 DEG C solidification when do not apply high-intensity magnetic field.
From figure 3, it can be seen that when graphene content is 1.0wt%, isotropism and anisotropic composite material
Thermal conductivity is respectively:0.29W/m.K and 0.37W/m.K, it is apparent that forming anisotropy knot after applying magnetic field
Structure, there is passage of heat, composite of the heat conductivity apparently higher than isotropic structure.
Embodiment 4
The present embodiment is prepared as follows heat conductive insulating composite, and (graphene accounts for silicone rubber matrix quality
1.5%):
The graphene of precise 0.33g surface modifications first, it is added in 10mL dispersants Isosorbide-5-Nitrae-dioxane, ultrasound
Disperse 30min, then addition 20g PDMS component As, uniform stirring 10min, ultrasonic disperse 30min, add 2g PDMS
B component, ultrasound are volatilized completely to dispersant, obtain mixture;
The bubble removed in mixture is vacuumized, is subsequently poured into mould, 80 DEG C of solidification 2h, make stone under 10T high-intensity magnetic fields
Black alkene arrangement form chain structure in matrix, so as to form with anisotropic passage of heat, that is, obtain target product and lead
Heat insulation composite.
For influence of the contrast anisotropic structure to composite property, obtained by the present embodiment identical method each to same
Property structure composite, differ only in high-intensity magnetic field it is lower 80 DEG C solidification when do not apply high-intensity magnetic field.
From figure 3, it can be seen that when graphene content is 1.5wt%, isotropism and anisotropic composite material
Thermal conductivity is respectively:0.298W/m.K and 0.387W/m.K, it is apparent that forming anisotropy knot after applying magnetic field
Structure, there is passage of heat, composite of the heat conductivity apparently higher than isotropic structure.
Embodiment 5
The present embodiment is prepared as follows heat conductive insulating composite, and (graphene accounts for silicone rubber matrix quality
2.0%):
The graphene of precise 0.44g surface modifications first, it is added in 10mL dispersants Isosorbide-5-Nitrae-dioxane, ultrasound
Disperse 30min, then addition 20g PDMS component As, uniform stirring 10min, ultrasonic disperse 30min, add 2g PDMS
B component, ultrasound are volatilized completely to dispersant, obtain mixture;
The bubble removed in mixture is vacuumized, is subsequently poured into mould, 80 DEG C of solidification 2h, make stone under 10T high-intensity magnetic fields
Black alkene arrangement form chain structure in matrix, so as to form with anisotropic passage of heat, that is, obtain target product and lead
Heat insulation composite.
For influence of the contrast anisotropic structure to composite property, obtained by the present embodiment identical method each to same
Property structure composite, differ only in high-intensity magnetic field it is lower 80 DEG C solidification when do not apply 10T high-intensity magnetic fields.
From figure 3, it can be seen that when graphene content is 2.0wt%, isotropism and anisotropic composite material
Thermal conductivity is respectively:0.31W/m.K and 0.41W/m.K, it is apparent that forming anisotropy knot after applying magnetic field
Structure, there is passage of heat, composite of the heat conductivity apparently higher than isotropic structure.
The exemplary embodiment of the present invention is these are only, is not intended to limit the invention, all spirit in the present invention
With all any modification, equivalent and improvement made within principle etc., it should be included in the scope of the protection.
Claims (8)
- A kind of 1. heat conductive insulating composite with anisotropic structure, it is characterised in that:The heat conductive insulating composite It is graphene arrangement form chain structure in described matrix using silicon rubber as matrix, forming, there is anisotropic heat conduction to lead to Road.
- 2. heat conductive insulating composite according to claim 1, it is characterised in that:The thickness of the heat conductive insulating composite Spend for 0.5~2mm.
- 3. heat conductive insulating composite according to claim 1, it is characterised in that:Described silicon rubber is dimethyl-silicon rubber Glue, methyl vinyl silicone rubber or methyl phenyl vinyl silicone rubber.
- A kind of 4. preparation method of heat conductive insulating composite described in any one in claims 1 to 3, it is characterised in that bag Include following steps:(1) 100mg graphene oxides are added in 60mL absolute ethyl alcohols, ultrasonic disperse is uniform, then add HCl regulation pH=3~ 4, obtain the dispersion liquid of graphene oxide;The 10mL ethanol solutions for containing 0.3g silane couplers are added slowly with stirring in the dispersion liquid, 60 after adding DEG C water-bath 24h, is then centrifuged for separating, and gained solid product is washed to neutrality repeatedly with absolute ethyl alcohol and deionized water, with Unreacted silane coupler is removed, finally dries 10~24h under the conditions of 60~80 DEG C in vacuum drying oven, surface is obtained and repaiies The graphene of decorations;(2) graphene for the surface modification for being obtained step (1) is added in dispersant, 20~30min of ultrasound, is then added Silicone rubber matrix, stir, then ultrasound is volatilized completely to dispersant, obtains mixture;Wherein, the graphene accounts for the silicon The 0.1~2% of rubber matrix quality, the volume mass ratio of the dispersant and the silicone rubber matrix is 1mL:1.5~3g;The bubble removed in the mixture is vacuumized, is subsequently poured into mould, 80~100 DEG C of solidification 2h, make under high-intensity magnetic field Graphene arrangement form chain structure in matrix, so as to form with anisotropic passage of heat, that is, obtain target product Heat conductive insulating composite.
- 5. preparation method according to claim 4, it is characterised in that:Silane coupler described in step (1) is 18 Alkyl trimethoxysilane, gamma-aminopropyl-triethoxy-silane or γ-methacryloxypropyl trimethoxy silane.
- 6. preparation method according to claim 4, it is characterised in that:Dispersant described in step (2) is 1,4- dioxies Six rings, dimethylformamide or tetrahydrofuran.
- 7. preparation method according to claim 4, it is characterised in that:The graphene for the surface modification that step (1) is obtained Average diameter be less than 10 μm, the number of plies be 5~10 layers, thickness is 3~8nm, specific surface area is more than 120m2/g。
- 8. preparation method according to claim 4, it is characterised in that:The size of high-intensity magnetic field described in step (2) is 10T.
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108976799A (en) * | 2018-06-29 | 2018-12-11 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of heat-conducting silicon rubber |
CN109943075A (en) * | 2019-03-27 | 2019-06-28 | 华南理工大学 | A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning |
CN110591381A (en) * | 2019-10-10 | 2019-12-20 | 广州赫尔普化工有限公司 | Heat-conducting silicone rubber composite material and preparation method thereof |
CN110862689A (en) * | 2019-11-29 | 2020-03-06 | 中国科学院合肥物质科学研究院 | Preparation method of magnetic control flexible surface material with orthotropic wettability |
CN111607365A (en) * | 2020-06-03 | 2020-09-01 | 彗晶新材料科技(深圳)有限公司 | Flake graphite heat conduction material, preparation method thereof and electronic equipment |
CN112679841A (en) * | 2019-10-17 | 2021-04-20 | 中国石油天然气股份有限公司 | Anisotropic heat-conducting polypropylene/graphene composite film and preparation method thereof |
CN113416420A (en) * | 2021-06-25 | 2021-09-21 | 厦门大学 | Preparation method of high-orientation-arrangement graphene sheet thermal interface material |
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CN105778510A (en) * | 2016-05-09 | 2016-07-20 | 中国科学院合肥物质科学研究院 | Method for preparing thermally conductive composite material with directivity |
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CN105694461A (en) * | 2015-12-14 | 2016-06-22 | 上海应用技术学院 | Graphene oxide-modified silicone rubber composite and preparation method thereof |
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Cited By (10)
Publication number | Priority date | Publication date | Assignee | Title |
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CN108976799A (en) * | 2018-06-29 | 2018-12-11 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of heat-conducting silicon rubber |
CN109943075A (en) * | 2019-03-27 | 2019-06-28 | 华南理工大学 | A kind of preparation method of the graphene thermally conductive silicone rubber composite material of magnetic aligning |
CN110591381A (en) * | 2019-10-10 | 2019-12-20 | 广州赫尔普化工有限公司 | Heat-conducting silicone rubber composite material and preparation method thereof |
CN112679841A (en) * | 2019-10-17 | 2021-04-20 | 中国石油天然气股份有限公司 | Anisotropic heat-conducting polypropylene/graphene composite film and preparation method thereof |
CN112679841B (en) * | 2019-10-17 | 2022-07-05 | 中国石油天然气股份有限公司 | Anisotropic heat-conducting polypropylene/graphene composite film and preparation method thereof |
CN110862689A (en) * | 2019-11-29 | 2020-03-06 | 中国科学院合肥物质科学研究院 | Preparation method of magnetic control flexible surface material with orthotropic wettability |
CN110862689B (en) * | 2019-11-29 | 2022-04-26 | 中国科学院合肥物质科学研究院 | Preparation method of magnetic control flexible surface material with orthotropic wettability |
CN111607365A (en) * | 2020-06-03 | 2020-09-01 | 彗晶新材料科技(深圳)有限公司 | Flake graphite heat conduction material, preparation method thereof and electronic equipment |
CN111607365B (en) * | 2020-06-03 | 2021-04-27 | 彗晶新材料科技(深圳)有限公司 | Flake graphite heat conduction material, preparation method thereof and electronic equipment |
CN113416420A (en) * | 2021-06-25 | 2021-09-21 | 厦门大学 | Preparation method of high-orientation-arrangement graphene sheet thermal interface material |
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Application publication date: 20180403 |