CN101734650B - Method for preparing graphene-carbon nano tube hybrid composite - Google Patents
Method for preparing graphene-carbon nano tube hybrid composite Download PDFInfo
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- CN101734650B CN101734650B CN2009102486812A CN200910248681A CN101734650B CN 101734650 B CN101734650 B CN 101734650B CN 2009102486812 A CN2009102486812 A CN 2009102486812A CN 200910248681 A CN200910248681 A CN 200910248681A CN 101734650 B CN101734650 B CN 101734650B
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Abstract
The invention provides a method for preparing a graphene-carbon nano tube hybrid composite and relates to a method for preparing a functional high molecular material and a device thereof. The method comprises the following steps of: carrying out the stirring and sonic oscillation treatment on graphene and carbon nano tubes to preform an entangled network structure, thoroughly mixing the entangled network structure and polymer particles, and thus obtaining an uniformly-mixed system in which the graphene-carbon nano tube network is coated on the surfaces of the polymer particles after removing the solvent; and putting the uniformly-mixed system in a mould, hot-compacting, and obtaining the graphene-carbon nano tube hybrid composite after cooling and demoulding. By mingling the graphene and the carbon nano tubes in advance to form the communicated network structure, the method realizes the advantage complementation of the graphene and carbon nano tube structures and enables the hybrid composite to have favorable electric conduction and heat conduction properties. The method can be widely used in the fields such as aviation, transportation and communication, electronic industry, civil facilities, construction, chemical industry and the like, can be produced in the industrial scale, and has the advantages of low cost and environmental friendliness.
Description
Technical field
The present invention relates to the preparation method in a kind of functional high molecule material and device technology field, particularly relate to a kind of preparation method of graphene-carbon nano tube hybrid composite.
Background technology
Graphene (graphene; See for details: Novoselov K S; Et al.Electric field effects inatomically thin carbon films.Science; 2004,306:666-119) be a kind of carbonaceous novel material by the tightly packed one-tenth bi-dimensional cellular of monolayer carbon atom shape crystalline network, it is the elementary cell that makes up other dimension blacking (like zero dimension soccerballene, one dimension carbon nanotube, three-dimensional graphite).Graphene has excellent electric property and thermal property, and its room temperature electronic mobility can reach 15000cm
2V
-1S
-1, thermal conductivity can reach 3000Wm
-1K
-1In addition, Graphene is cheap, raw material is easy to get, and its unique two-dirnentional structure can carry out effective electric heating transmission, is expected to the acquisition widespread use in fields such as high-performance electronic device, field emmision material, gas sensor and energy storages.But because Graphene has the sheet structure of two dimension, it in use curls and height fold especially easily; When especially adopting melt-blending process to prepare polymer composites, Graphene takes place to curl and height fold under shear action more easily, is unfavorable in matrix, forming transporting network efficiently.Carbon nanotube (carbon nanotube is a kind of new carbon of being found by Iijima in 1991 CNT), and it can regard the seamless hollow tube that is rolled into by Graphene as, and its length is several microns to several millimeters, diameter in several nanometers between tens nanometers.Because its particular structure, carbon nanotube has significant advantage at aspects such as mechanics enhancing and the transmission of electronics long-range; But there is shortcomings such as being easy to reunion and cost height.
About the existing report of Graphene hybrid polymer thing Composite Preparation technology; For example: Chinese patent; The old Yongsheng of CN200910067708.8 etc., " Graphene and carbon-fibre composite and preparation method thereof ", its principal character comprises: it is to be raw material with Graphene and carbon fibre material; Method through applying forms in carbon fibre material surface-coated Graphene coating prepn, and the thickness of coating is 1 nanometer-5 micron.Chinese patent; The old Yongsheng of CN101474897 etc.; " Graphene-organic material layered assembling film and preparation method thereof "; Its principal character comprises: with grapheme material and organic materials is raw material, utilizes the interactions such as static, hydrogen bond, co-ordination bond or charge transfer between Graphene and the organic materials, through method for manufacturing thin film such as spin coating, spraying, dipping-the lift film forming that is layering.Chinese patent; The old Yongsheng of CN101474899 etc.; " Graphene-inorganic materials composite multi-layer film and preparation method thereof "; Its principal character comprises: with grapheme material and inorganic materials is raw material, and through typical thin films preparing methods such as spraying, spin coating, dipping, the electroless plating film forming that is layering, every tunic is thick can be controlled at 10 nanometers-2 millimeter as required.In the above method, do not mention that all utilizing Graphene and carbon nano tube hybrid technology to form twines interleaving network, and the spin coating techniques that adopt form laminated film more in the preparation.
Summary of the invention
The objective of the invention is to propose a kind of preparation method of graphene-carbon nano tube hybrid composite; Make carbon nanotube and Graphene form through stirring and sonic oscillation in solvent and mix interspersed structure; Can prevent curling or wrinkle of Graphene effectively, give full play to the excellent two-dimentional electric heating transport property of Graphene; Mixing of this graphene-carbon nano tube transports network, and it is complementary that Graphene and carbon nanotube are formed in the 26S Proteasome Structure and Function design, when satisfying heat conduction, conducting function, significantly reduces the volume of functional stuffing, the cost of reduction matrix material.In addition, because it transports network structure and can design in advance and make up according to request for utilization, has bigger design freedom.
The technical scheme that the present invention adopted is:
A kind of preparation method of graphene-carbon nano tube hybrid composite, this preparing method's process step is following:
(1) preparation comprises the suspension system of Graphene, carbon nanotube, dispersion solvent, makes that through stirring, sonic oscillation Graphene and carbon nanotube intert each other, winding forms the network structure that is communicated with;
(2) add polymer beads,, make the polymer beads surface wrapped up by the graphene-carbon nano tube interleaving network through stirring and sonic oscillation;
(3) behind the removal solvent, form the uniform mixing system that graphene-carbon nano tube is wrapped in the polymer beads surface;
(4) said mixed system is put into mould, make graphene-carbon nano tube hybrid composite after, the cooling and demolding hot-forming through heating up.
The preparation method of described a kind of graphene-carbon nano tube hybrid composite, used Graphene is meant mono-layer graphite sheet, multilayer graphite flake or their mixture; Used carbon nanotube is meant that diameter is that 5-200 nanometer, length are the hollow tubular carbon material of 0.1-100 micron.
The preparation method of described a kind of graphene-carbon nano tube hybrid composite, used dispersion solvent is absolute ethyl alcohol, acetone, toluene and vinylbenzene.
The preparation method of described a kind of graphene-carbon nano tube hybrid composite makes Graphene and carbon nanotube be pre-formed a kind of network structure that interweaves, twines behind sonic oscillation.。
The preparation method of described a kind of graphene-carbon nano tube hybrid composite, polymer beads is Vilaterm, SE, Vestolen PP 7052, polymeric amide, PS, PS, polyoxymethylene, tetrafluoroethylene, polycarbonate, ppe, polysulfones.
The preparation method of described a kind of graphene-carbon nano tube hybrid composite removes solvent and realizes through heating or vacuum filtration method.
The preparation method of described a kind of graphene-carbon nano tube hybrid composite, the graphene-carbon nano tube network packet is rolled in the polymer beads surface, forms the connected network along the polymer beads surface arrangement.
The preparation method of described a kind of graphene-carbon nano tube hybrid composite, hot pressing temperature are higher than melting point polymer or softening temperature more than 20 ℃, and forming pressure is greater than 10MPa, and the cooling and demolding temperature is lower than 60 ℃.
The preparation method of described a kind of graphene-carbon nano tube hybrid composite, the initial content proportioning (mass percent) of raw material is:
Graphene 0.1-10 part;
Carbon nanotube 0.1-10 part;
Polymkeric substance: 100 parts;
Dispersion solvent: 100-500 part.
The invention has the beneficial effects as follows:
1. the present invention adopts the graphene-carbon nano tube hybrid technology; Make that through sonic oscillation carbon nanotube and Graphene carry out interting each other and twining; Utilize the advantage that the Graphene cost is low, electric property is excellent, the characteristics big by carbon nanotube rigidity, that length-to-diameter ratio is high prevent curling of two-dimentional graphene film; Give full play to constructional feature, the formation of Graphene and carbon nanotube and have complementary advantages, help to form three-dimensional efficiently electric heating and transport network.
2. through designing in advance and structure transports network, the polymkeric substance that can avoid traditional melt blending to prepare effectively occurring in the process is to contact electricity (heat) resistance increases, conduction (heat) performance reduces between the parcel of functional stuffing, filler limitation.Transporting being built with in advance of network among the present invention helps form and effectively has a common boundary, improves the electricity, the heat conduction transmission efficiency that transport network between functional stuffing.
3. the immingling technology that combines graphene-carbon nano tube network and polymer beads; Make the graphene-carbon nano tube network packet be rolled in the polymer beads surface; Form the three-dimensional network that transports, significantly improve the effective rate of utilization of filler aspect electric heating transmission enhancing, only need very low volume; Hybrid composite just can have conduction (heat) performance preferably, significantly reduces the cost of matrix material.In addition, if adopt the matrix of high crystalline polymkeric substance, hybrid composite can have certain positive temperature coefficient effect, can be widely used at thermistor and devices field.。
4. the present invention prepares hybrid composite with graphene-carbon nano tube conductive network and polymeric matrix through solvent blend, hot-forming mode; Equipment is simple; Operating process is simple and easy, can be used for the preparation of multiple thermoplastic polymer and graphene-carbon nano tube hybrid composite.Select different matrix material, size distribution and amount of filler, can be according to actual user demand, design in advance and make functional composite material with particular network structure, have great design freedom.
Embodiment
Embodiment 1:
0.01 gram Graphene and 0.01 gram carbon nanotube are scattered in the 10 gram absolute ethyl alcohols, form steady suspension after ultrasonic 2 hours; 10 gram high density polyethylene(HDPE) ultrafine powder are joined in this suspension-s, ultrasonic 30 minutes, when treating that graphene-carbon nano tube is wrapped in the high-density polyethylene powder surface and forms the uniform mixing system, be warming up to 60 ℃ and carry out drying with except that desolvating.It is transferred in the mould, is warming up to 170 ℃, and under the 10MPa condition hot-forming 5 minutes, be cooled to room temperature, the demoulding obtains graphene-carbon nano tube hybrid composite.Measure matrix material volume resistance, calculating its resistivity is 7.09 * 10
6Ohmcm.
Embodiment 2:
0.1 gram Graphene and 0.1 gram carbon nanotube are scattered in the 10 gram acetone, form steady suspension after ultrasonic 2 hours; 10 gram PP GRANULESs are joined in this suspension-s, ultrasonic 30 minutes, when treating that graphene-carbon nano tube is wrapped in the high density poly propylene particle surface and forms the uniform mixing system, under normal temperature, carry out vacuum filtration except that desolvating.It is transferred in the mould, is warming up to 200 ℃, and under the 10MPa condition hot-forming 5 minutes, be cooled to the room temperature demoulding, obtain graphene-carbon nano tube hybrid composite.Measure matrix material volume resistance, calculating its resistivity is 2.00 * 10
4Ohmcm.
Embodiment 3:
0.5 gram Graphene and 0.5 gram carbon nanotube are scattered in the 25 gram absolute ethyl alcohols, form steady suspension after ultrasonic 2 hours; 10 gram poly methyl methacrylate particles are joined in this suspension-s, ultrasonic 30 minutes, when treating that graphene-carbon nano tube is wrapped in the poly methyl methacrylate particle surface and forms the uniform mixing system, under normal temperature, carry out vacuum filtration and desolvate to remove.It is transferred in the mould, is warming up to 180 ℃, and under the 10MPa condition hot-forming 5 minutes, be cooled to the room temperature demoulding, obtain graphene-carbon nano tube hybrid composite.Measure matrix material volume resistance, calculating its resistivity is 8.84 * 10
2Ohmcm.
Embodiment 4:
1 gram Graphene and 1 gram carbon nanotube are scattered in the 50 gram absolute ethyl alcohols, form steady suspension after ultrasonic 2 hours; 10 gram granules of polystyrene are joined in this suspension-s, ultrasonic 30 minutes, when treating that graphene-carbon nano tube is wrapped in granules of polystyrene surface and forms the uniform mixing system, be warming up to 60 ℃ and carry out heat drying and desolvate to remove.Further be transferred in the mould, be warming up to 160 ℃, and under the 10MPa condition hot-forming 5 minutes, be cooled to the room temperature demoulding, obtain graphene-carbon nano tube hybrid composite.Measure matrix material volume resistance, calculating its resistivity is 4.55 * 10
1Ohmcm.
Claims (9)
1. the preparation method of a graphene-carbon nano tube hybrid composite is characterized in that said preparing method's process step is following:
(1) preparation comprises the suspension system of Graphene, carbon nanotube, dispersion solvent, and through stirring, sonic oscillation makes that Graphene and carbon nanotube intert each other, winding forms the network structure that is communicated with;
(2) add polymer beads,, make the polymer beads surface wrapped up by the graphene-carbon nano tube interleaving network through stirring and sonic oscillation;
(3) behind the removal solvent, form the uniform mixing system that graphene-carbon nano tube is wrapped in the polymer beads surface;
(4) said mixed system is put into mould, make graphene-carbon nano tube hybrid composite after, the cooling and demolding hot-forming through heating up.
2. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that used Graphene is meant mono-layer graphite sheet, multilayer graphite flake or their mixture; Used carbon nanotube is meant that diameter is that 5-200 nanometer, length are the hollow tubular carbon material of 0.1-100 micron.
3. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that used dispersion solvent is absolute ethyl alcohol, acetone, toluene and vinylbenzene.
4. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that behind sonic oscillation, making Graphene and carbon nanotube to be pre-formed a kind of network structure that interweaves, twines.
5. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that polymer beads is Vilaterm, SE, Vestolen PP 7052, polymeric amide, PS, polyoxymethylene, tetrafluoroethylene, polycarbonate, ppe, polysulfones.
6. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that removing solvent and realizes through heating or vacuum filtration method.
7. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that the graphene-carbon nano tube network packet is rolled in the polymer beads surface, forms the connected network along the polymer beads surface arrangement.
8. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that hot pressing temperature is higher than melting point polymer or softening temperature more than 20 ℃, and forming pressure is greater than 10MPa, and the cooling and demolding temperature is lower than 60 ℃.
9. the preparation method of a kind of graphene-carbon nano tube hybrid composite according to claim 1 is characterized in that the initial content weight proportion of raw material is:
Graphene: 0.1-10 part;
Carbon nanotube: 0.1-10 part;
Polymkeric substance: 100 parts;
Dispersion solvent: 100-500 part.
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