CN105176086A - Oriented graphene/polymer composite system, and preparation method and application thereof - Google Patents
Oriented graphene/polymer composite system, and preparation method and application thereof Download PDFInfo
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Abstract
An oriented graphene/polymer composite system, and a preparation method and an application thereof are provided. The composite system includes an oriented network component at least including graphene and a substrate component compounded with the oriented network component, wherein at least a part of graphene is arranged according to set orientation; the composite system at least has a heat conductivity coefficient in the set direction higher than heat conductivity coefficients in other directions. The preparation method includes the steps: the oriented network component is subjected to orientation treatment, at least a part of graphene is arranged according to the set orientation, and thus an oriented network is formed; and the substrate component at least containing a polymer is taken to be compounded with the oriented network component, and thus the composite system is formed. The composite system has high heat conductivity and high electrical conductive characteristic, can efficiently transfer heat in a needed direction when in use, has the characteristics of being simple, high in efficiency and the like, is suitable for scale production, and has broad application prospects in high-efficiency heat conductivity and heat dissipation.
Description
Technical field
The present invention relates to a kind of Graphene/polymer composites, particularly relate to a kind of there is high thermal conductivity orientation Graphene/polymer composites, its preparation method and application, belong to nano material sciemtifec and technical sphere.
Background technology
Along with science and technology and industrial development, the capacity of heat transmission of people to material proposes requirements at the higher level.Especially in electric and electronic field, along with High Density Integration and the volume-diminished of electronic component, circuit, the material of more high thermal conductivity is needed.Graphene, as the thinnest Two-dimensional Carbon material, Stability Analysis of Structures, has large specific surface area and excellent electricity, calorifics and mechanical property.Especially the thermal conductance ability (5000W/mK) of its excellence, makes it have wide practical use in thermal conducting material field.
Graphene and the technique such as polymer blending, dispersion are normally realized heat conductivility by traditional Graphene/polymer bond composite material and preparation method thereof.Therefore its heat conductivility depends on content and the degree of scatter of Graphene unduly.This method needs a large amount of Graphenes, but when usually the content of Graphene reaches about 15wt.% in polymkeric substance, matrix material cannot be shaping, and this kind of preparation method's cost is high, and addition is large and cannot meet the requirement of heat conductivility.
Summary of the invention
One object of the present invention is to provide a kind of orientation Graphene/polymer composites with high thermal conductivity, thus overcomes deficiency of the prior art.
Another object of the present invention is to the method that the orientation Graphene/polymer composites described in a kind of preparation with high thermal conductivity are provided.
There is described in another object of the present invention is to provide the application of the orientation Graphene/polymer composites of high thermal conductivity.
For achieving the above object, present invention employs following technical scheme:
A kind of orientation Graphene/polymer composites, comprising:
At least comprise the oriented network component of Graphene, wherein Graphene, by setting orientations, forms oriented network at least partly,
And, with the matrix component of described oriented network component compound;
Further, the thermal conductivity of described orientation Graphene/polymer composites at least on direction initialization is higher than thermal conductivity in other directions.
Further, described matrix component comprises the compound system of polymkeric substance, polymer monomer or polymkeric substance and highly heat-conductive material, and described oriented network component comprises Graphene or Graphene-highly heat-conductive material compound system.
As one of comparatively preferred scheme, the Graphene in described compound system is all by setting orientations.
Further, described compound system comprises 0.01-90wt% matrix component and 0.01-90wt% oriented network component.
Preferably, the radial dimension of described Graphene is 10nm-1mm, and thickness is 0.34nm-1mm, and the number of plies is 1-100 layer.
Further, at least optional autoxidation Graphene of described Graphene, redox Graphene, expand and peel off any one or more that Graphene, liquid phase dissociate in Graphene, N-doped graphene, three-dimensional grapheme, and be not limited thereto.
Further, the combination of described polymkeric substance any one or more in polyaniline, polypyrrole, Polythiophene, epoxy resin, silicon rubber, polyethylene, polypropylene, polyvinyl chloride, high density polyethylene(HDPE), polyvinylidene difluoride (PVDF), tetrafluoroethylene, polyvinylpyrrolidone, polyvinyl alcohol, polyacrylic acid, resol, polymethylmethacrylate, polymeric amide, rubber resin, polyoxyethylene glycol, polycarbonate, polyimide, nylon at least optional, and be not limited thereto.
Further, described highly heat-conductive material at least can be selected from the combination of any one or more in graphite, soccerballene, carbon black, carbon nanotube, carbon nano-tube fibre, carbon fiber, boron nitride, aluminium nitride, silicon carbide, zinc, aluminium, copper, silver, nickel, cadmium, iron, carbon steel, aluminum oxide, silicon, beryllium oxide, silicon nitride, magnesium oxide, and is not limited thereto.
Preferably, described highly heat-conductive material is of a size of 1nm-1mm, such as, if select graphite, then its particle diameter is 10nm-1mm, if select single wall or multi-walled carbon nano-tubes, then its length is 10nm-1cm, if select other carbon materials, metal or non-metallic particle, then its particle diameter is 1nm-1mm.
A preparation method for orientation Graphene/polymer composites, comprising:
The oriented network component at least comprising Graphene is provided, and makes at least part of Graphene wherein by setting orientations, form oriented network,
And, be taken to the matrix component less containing polymkeric substance and described oriented network component compound, form described orientation Graphene/polymer composites, the thermal conductivity of described orientation Graphene/polymer composites at least on direction initialization is higher than thermal conductivity in other directions.
Further, the mode of described orientation process or the combination of any one or more that the mode of described basic components and oriented network component compound at least can be selected from ball milling, spin coating, solution blending, self-assembly, electrostatic spinning, solvent spinning, melt-spinning, twin-screw extrusion, vacuum assisted resin infusion, vacuum filtration, filter type, and be not limited thereto.
Among an embodiment, described preparation method can also comprise: by described oriented network component disperses in solvent, then carry out orientation process, makes at least part of Graphene wherein by setting orientations, forms described oriented network.
Further, described solvent at least can be selected from hexanaphthene, acetone, acetonitrile, ethanol, water, N, N,-dimethyl formamide, N-Methyl pyrrolidone, 1, any one or more in 2-ethylene dichloride, ether, tetrahydrofuran (THF), trichloromethane, methylene dichloride, toluene, dimethylbenzene, and be not limited thereto.
Any one orientation Graphene/polymer composites aforementioned are preparing the application in thermally conductive material.
Compared with prior art, advantage of the present invention comprises:
(1) the present invention is by forming oriented network structure by Graphene by after all or part of orientation in same direction, and by polymkeric substance or polymkeric substance and highly heat-conductive material mode and the oriented network structure composite such as to fill, formation has high heat conduction, the Novel heat-conducting compound system of high connductivity characteristic, and described compound system thermal conductivity at least is in one direction higher than the thermal conductivity on other directions, thus in use, can transferring heat efficiently in a desired direction, at high-efficiency heat conduction, heat radiation aspect has broad application prospects.
(2) orientation Graphene/polymer composites preparation technology of the present invention has the features such as simple, efficient, is suitable for large-scale production.
Accompanying drawing explanation
Fig. 1 is preparation technology's schema of a kind of orientation Graphene/polymer composites among the present invention one typical embodiments.
Fig. 2 is the SEM figure of a kind of orientation Graphene/polymer composites obtained in embodiment of the present invention 2-1.
Fig. 3 is shown in embodiment of the present invention 1-1(S1-1), shown in embodiment 1-2(S1-2), shown in embodiment 2-1(S2-1), shown in embodiment 2-2(S2-2), shown in embodiment 3-1((S3-1), shown in embodiment 3-2((S3-2)) the thermal conductivity figure of orientation graphene composite material in differently-oriented directivity and non-oriented direction.
Embodiment
For many deficiencies of existing heat conduction product, such as heat conductive filler addition is large, heat conductivility but can not satisfy the demands growing situation, inventor is through studying for a long period of time and putting into practice in a large number, provide a kind of orientation Graphene/polymer composites with high thermal conductivity and preparation method thereof, this compound system has the characteristic of high heat conduction, high connductivity, and thermal conductivity at least is in one direction higher than the thermal conductivity on other directions, and this preparation method has simply, efficient feature.
Further, orientation Graphene/polymer composites of the present invention mainly comprise matrix and oriented network, wherein matrix forms primarily of polymeric constituent, and oriented network is formed primarily of Graphene, and Graphene system contained in a network all or part of orientations in a direction.
As one of comparatively preferred embodiment, described orientation Graphene/polymer composites comprise 0.01-90wt% matrix component and 0.01-90wt% oriented network component.
Further, described oriented network component comprises the compound system of Graphene or Graphene and highly heat-conductive material.
Further, described matrix component comprises the compound system of polymkeric substance or polymer monomer or polymkeric substance and highly heat-conductive material.
Such as, in some embodiments:
Matrix component is polymkeric substance or polymer monomer, and oriented network component (also can think heat conduction component, lower same) is Graphene;
Matrix component is polymkeric substance or polymer monomer, and oriented network component is the compound system of Graphene and highly heat-conductive material;
Matrix component is the compound system of polymkeric substance and highly heat-conductive material, and oriented network component is Graphene;
Matrix component is the compound system of polymkeric substance and highly heat-conductive material, and oriented network component is the compound system of Graphene and highly heat-conductive material.
Described polymkeric substance, highly heat-conductive material, Graphene etc. can be selected but be not limited to previously described various types of materials, repeat no more herein.
Further, the preparation method of a kind of orientation Graphene/polymer composites of the present invention can comprise:
The oriented network component be taken to less containing Graphene carries out orientation process, making at least part of Graphene wherein by setting orientations, forming oriented network,
And, be taken to the matrix component less containing polymkeric substance and described oriented network component compound, form described orientation Graphene/polymer composites.
Consult the preparation technology being a kind of typical orientation Graphene/polymer composites shown in Fig. 1.
Wherein, the mode of described orientation process at least can be selected from but be not limited to one or more modes such as ball milling, spin coating, solution blending, LBL self-assembly, electrostatic spinning, solvent spinning, melt-spinning, twin-screw extrusion, vacuum assisted resin infusion, vacuum filtration, filtration.
Wherein, by the mode of described matrix component and oriented network component compound, such as, fill in oriented network and can be selected from the method for matrix component but to be not limited to one or more modes such as melt-processed, ball milling, solution blending, electrostatic spinning, solvent spinning, melt-spinning, immersion, twin-screw extrusion, vacuum assisted resin infusion, mill mixing, vacuum filtration, filtration.
The mode that orientation Graphene/polymer composites of the present invention can adopt industry known, such as can use such as electricity, the multiple methods such as chemistry or physics, make heat conducting film, heat conductive pad, heat-conducting cream, heat-conducting glue, heat-conducting resin etc., shape can be membranous type, plate, camber, tubular type or other abnormal shapes etc., with various particular requirement under satisfied different working conditions, such as, can be applicable to the heat conduction of the devices such as computer chip, photodiode, device package, mobile phone, heat exchanger, heat radiation.
embodiment 1the preparation of orientation Graphene/copper/silicon rubber high-heat-conductive composite material
1-1)get 1g Graphene, 0.5g copper powder joins in 250mlDMF, at room temperature Homogeneous phase mixing, at room temperature leave standstill after 48 hours, again 80 DEG C leave standstill 24 hours, then drip silicon rubber, to time saturated 80 DEG C solidification 12 hours, namely obtain heat-conductive composite material, this matrix material can be processed into heat conductive pad.
)getting 1g Graphene joins in 250mlDMF, at room temperature Homogeneous phase mixing, at room temperature leave standstill after 48 hours, 24 hours are left standstill at 80 DEG C, add 20g silicon rubber and 2g aluminium powder at room temperature Homogeneous phase mixing again, mechanical stirring 15 minutes, then drips silicon rubber, to time saturated 80 DEG C solidification 12 hours, namely obtain heat-conductive composite material.Mixture is processed into heat conductive pad.
reference examples 1-1get 1g Graphene, 0.5g copper powder and 10g silicon rubber to be uniformly mixed in 250mlDMF, 80 DEG C solidify 12 hours, and obtain heat-conductive composite material, thermal conductivity is 1.1W/mK.
reference examples 2-1get 1g Graphene, 2g aluminium powder and 10g silicon rubber to be uniformly mixed in 250mlDMF, 80 DEG C solidify 12 hours, and obtain heat-conductive composite material, thermal conductivity is 1.6W/mK.
embodiment 2the preparation of orientation Graphene/epoxy resin heat conduction matrix material
2-1)getting 1g Graphene joins in 250mlNMP, and at room temperature Homogeneous phase mixing, at room temperature filters, then leaves standstill 24 hours at 80 DEG C, forms orientation Graphene network.In 20g epoxy resin, add 25g solidifying agent mechanical stirring after 15 minutes, vacuum leave standstill 1 hour, be then added drop-wise in orientation Graphene network, to time saturated 80 DEG C solidification 24 hours, namely obtain heat-conductive composite material, this matrix material can be processed into heat-conducting resin.
)getting 1g Graphene joins in 250mlNMP, and at room temperature Homogeneous phase mixing, at room temperature filters, then leaves standstill 24 hours at 80 DEG C, forms orientation Graphene network.Separately getting 1g graphite joins in 20g epoxy resin, after mechanical stirring added 25g solidifying agent after 15 minutes, continue stirring 45 minutes, vacuum leaves standstill 1 hour, then be added drop-wise in orientation Graphene network, to time saturated 80 DEG C solidification 24 hours, namely obtain heat-conductive composite material, this matrix material can be processed into heat-conducting resin.
reference examples 2-1get the mechanical stirring mixing in 250mlNMP of 1g Graphene, 20g epoxy resin and 25g solidifying agent, 80 DEG C solidify 24 hours, and obtain heat-conductive composite material, thermal conductivity is 0.5W/mK.
reference examples 2-2get 1g Graphene, 1g graphite and 20g epoxy resin and the mechanical stirring mixing in 250mlDMF of 25g solidifying agent, 80 DEG C solidify 24 hours, and obtain heat-conductive composite material, thermal conductivity is 0.8W/mK.
embodiment 3the preparation of orientation Graphene/magnesium oxide/acrylic resin heat-conductive composite material
3-1)getting 1g Graphene joins in 100ml vinylformic acid, and mechanical stirring is after 30 minutes, and spin coating under the speed of 2000rpm, namely spin coating obtained heat-conductive composite material after 10 minutes.Mixture is processed into heat-conducting glue.
)get 1g Graphene, 0.5g magnesium oxide joins in 100ml vinylformic acid, mechanical stirring is after 30 minutes, and spin coating under the rotating speed of 2000rpm, namely spin coating obtained heat-conductive composite material after 10 minutes.Mixture is processed into heat-conducting glue.
Should be appreciated that above explanation, drawing and embodiment can not resolve to restriction design philosophy of the present invention.Hold in ken of the present invention and identically know that the knowledgeable can to technological thought of the present invention with the improvement of various form, such improvement and change and also should belong to protection scope of the present invention.
Claims (10)
1. orientation Graphene/polymer composites, is characterized in that comprising:
At least comprise the oriented network component of Graphene, wherein Graphene, by setting orientations, forms oriented network at least partly,
And, with the matrix component of described oriented network component compound;
Further, the thermal conductivity of described orientation Graphene/polymer composites at least on direction initialization is higher than thermal conductivity in other directions.
2. orientation Graphene/polymer composites according to claim 1, it is characterized in that described matrix component comprises the compound system of polymkeric substance, polymer monomer or polymkeric substance and highly heat-conductive material, described oriented network component comprises Graphene or Graphene-highly heat-conductive material compound system.
3. the orientation Graphene/polymer composites according to any one of claim 1-2, is characterized in that Graphene in described compound system all by setting orientations.
4. the orientation Graphene/polymer composites according to any one of claim 1-3, is characterized in that described compound system comprises 0.01-90wt% matrix component and 0.01-90wt% oriented network component.
5. the orientation Graphene/polymer composites according to any one of claim 1-3, it is characterized in that the radial dimension of described Graphene is 10nm-1mm, thickness is 0.34nm-1mm, and described Graphene is at least selected from graphene oxide, redox Graphene, expands and peel off any one that Graphene, liquid phase dissociate in Graphene, N-doped graphene, three-dimensional grapheme.
6. orientation Graphene/polymer composites according to claim 2, is characterized in that described polymkeric substance is at least selected from the combination of any one or more in polyaniline, polypyrrole, Polythiophene, epoxy resin, silicon rubber, polyethylene, polypropylene, polyvinyl chloride, high density polyethylene(HDPE), polyvinylidene difluoride (PVDF), tetrafluoroethylene, polyvinylpyrrolidone, polyvinyl alcohol, polyacrylic acid, resol, polymethylmethacrylate, polymeric amide, rubber resin, polyoxyethylene glycol, polycarbonate, polyimide, nylon.
7. orientation Graphene/polymer composites according to claim 2, it is characterized in that described highly heat-conductive material is at least selected from the combination of any one or more in graphite, soccerballene, carbon black, carbon nanotube, carbon nano-tube fibre, carbon fiber, boron nitride, aluminium nitride, silicon carbide, zinc, aluminium, copper, silver, nickel, cadmium, iron, carbon steel, aluminum oxide, silicon, beryllium oxide, silicon nitride, magnesium oxide, and described highly heat-conductive material is of a size of 1nm-1mm.
8. a preparation method for orientation Graphene/polymer composites, is characterized in that comprising:
The oriented network component at least comprising Graphene is provided, and makes at least part of Graphene wherein by setting orientations, form oriented network,
And, be taken to the matrix component less containing polymkeric substance and described oriented network component compound, form described orientation Graphene/polymer composites, the thermal conductivity of described orientation Graphene/polymer composites at least on direction initialization is higher than thermal conductivity in other directions;
Wherein, described orientation process mode or the mode of described matrix component and oriented network component compound is at least selected from any one in ball milling, spin coating, solution blending, self-assembly, electrostatic spinning, solvent spinning, melt-spinning, twin-screw extrusion, vacuum assisted resin infusion, vacuum filtration, filter type.
9. the preparation method of orientation Graphene/polymer composites according to claim 8, it is characterized in that comprising: by described oriented network component disperses in solvent, carry out orientation process again, make at least part of Graphene wherein by setting orientations, form described oriented network;
Wherein, described solvent is at least selected from hexanaphthene, acetone, acetonitrile, ethanol, water, N, N, any one in-dimethyl formamide, N-Methyl pyrrolidone, 1,2-ethylene dichloride, ether, tetrahydrofuran (THF), trichloromethane, methylene dichloride, toluene, dimethylbenzene.
10. according to any one of claim 1-9, orientation Graphene/polymer composites are preparing the application in thermally conductive material.
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