CN101899185A - Method for making carbon nano tube/polystyrene composite conductive material - Google Patents
Method for making carbon nano tube/polystyrene composite conductive material Download PDFInfo
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Abstract
The invention discloses a method for making a carbon nano tube/polystyrene composite conductive material, which comprises the following steps of: firstly, preparing low-concentration solution of polystyrene by using a specific solvent and dispersing carbon nanotubes by using the solution of polystyrene; secondly, preparing another solution of polystyrene by using the same solvent according to the formula of the composite material, and uniformly mixing the two parts of solution; thirdly, adding a solvent, which is soluble with the solvent of the solution of polystyrene and not soluble with the polystyrene, into the mixed solution; and finally, obtaining the solid electro-conductive composite by filtering, collecting or drying. In the invention, the carbon nanotubes can be uniformly and stably dispersed by the chain winding of a polystyrene matrix material, the pi-pi interaction and the like, no auxiliary dispersing agents are added, and the post-chemical decoration dispersion is not used, so that the damages of ultrasonic treatment to the matrix are avoided, the basic structure and the performance of the matrix material are kept, and meanwhile, the purity of the composite is greatly improved. The making method of the invention has a simple operation process and obviously saves cost.
Description
Technical field
The present invention relates to field of semiconductor technology, particularly a kind of based semiconductor material is made the method for nanometer array structure solar battery, and this method can significantly be improved III group-III nitride nano array structure.
Background technology
Nano composite material is meant that disperse phase has the class matrix material of one dimension less than 100nm at least on three-dimensional dimension, is one of field, most active forward position in the materialogy in the world now.It has unique nano level and disperses microstructure, the advantage of its different components is ideally combined on nanoscale, thereby show one-component and the unapproachable excellent properties of conventional microcosmic matrix material.Yet in the polymer/inorganic matrix material, studying maximum at present is polyalcohol/clay soil and polymer/carbon nano-tube nano composite material.Nanoclay adds the compressive resistance that plastics can be improved in the plastics the inside to, carbon nanotube then can also improve conductivity of electrolyte materials and thermal conductivity, so from Ajayan in 1994 etc. CNTs is joined as mineral filler prepare polymkeric substance/CNT matrix material in the polymeric matrix since, people have just launched number of research projects, attempt CNTs fully to be separated winding and be dispersed in the polymeric matrix, with preparation novel high-performance multifunctional polymer based nano composite material.
Carbon nanotube be by Japanese Electronic Speculum expert Iijima in the Graphite Electrodes in vacuum arc evaporation in 1991 first observed to, be the another newcomer who after C60, occurs in the carbon family.Carbon nanotube be by the hexagonal mesh of similar graphite-structure reel form, coaxial hollow " microtubule ", two ends by pentagon or the sealing of heptagon carbon net.According to number of plies difference, carbon nanotube can be divided into single-walled pipe (SWCNT) and multi-walled pipes (MWCNT).Its length is several microns to several millimeters, and its diameter generally has only several nanometers to tens nanometers.Therefore, carbon nanotube is considered to typical monodimension nanometer material.Yet the CNTs of two kinds of forms demonstrates remarkable mechanical property and mechanical property.The theoretical tensile strength of CNTs is 100 times of steel, and snappiness deformation (12%) is about 60 times of steel, and density has only 1/6 of steel.According to the difference of CNTs spirality and diameter, CNTs can also show metallicity and semiconductive.On this external heat transport ability, theoretical investigation and experimental result show that all the thermal conductivity of carbon nanotube is up to 3500W/ (mK), considerably beyond the thermal conductivity 385W/ (mK) of the metallic copper with good heat-conductivity, and its proportion also is far smaller than general heat-eliminating medium metallic aluminium.These advantages make carbon nanotube become the strong rival of current material in the fields such as microelectronic device, intelligent sensing, energy conversion.
Yet because the carbocyclic ring wrapped configuration of carbon nanotube uniqueness is insoluble in common organic solvent and the water it.Although, how to obtain the uniform and stable dispersion of carbon nanotube in matrix, remain its one of bottleneck in the widespread use in matrix material of restriction so numerous theory shows that all it can significantly improve the mechanical property of body material, conductive and heat-conductive ability.Polymer materials mainly comprises rubber, plastics, fiber, sizing agent and coating etc., though the development of decades is only arranged, but because polymkeric substance has thermoplasticity, snappiness, film-forming properties, numerous performance advantage such as wear-resisting, anti-solvent, resistance to air loss are good has been widely used in the every field in the society.It is aging that yet polymerization also exists easy firing in actual applications, is easy to generate and stored charge, and electric charge such as can't effectively discharge at shortcoming.How overcoming these shortcomings, further improve the over-all properties of polymer materials, is the target that various countries' scientists is being pursued all the time.
Polymer materials use in modern society more and more widely, but it all has a common shortcoming usually, promptly electroconductibility is bad, the polystyrene based material is all the more so.Solve the disadvantageous effect of bringing because of static in styrenic and other polymer materials uses, main method is to add conductive component or improve ambient moisture.Conductive component commonly used at present is carbon black, metal oxide etc., but the consumption of these fillers is very high, need usually to add 20%, even 40%, could in polymeric matrix, form conductive network, give the base material conductivity.Yet a large amount of carbon blacks and the adding of metal oxide particle must bring the difficult problem of a series of complete processings, and influence the mechanical property of material and optical property etc. the most at last.Yet carbon nanotube is strong because of himself conductive capability, and has high length-to-diameter ratio, for the research and development and the application of conducing composite material brought new dawn.
At present mainly contain compound three kinds of polymeric composite, solution combined and fusion about the preparation method of carbon nanotube and poly styrene composite material.Polymeric composite is exactly early stage carbon nanotube to be added in the material system in the lump with monomer, initiator etc. in polymer manufacture, finishes polymkeric substance to the parcel of carbon nanotube, compound in the polymeric process.Solution composite approach is meant under solution condition, CNTs is separated twine and be dispersed among the PS.The matrix material solution that this method obtains can directly carry out solution-cast or spin coating usually, and volatilization removes to desolvate and obtains composite material film, perhaps adds non-solvent in solution, and the matrix material precipitation is separated out.The fusion composite algorithm is studied also morely recently, mainly is more than the flow temperature of polymkeric substance, and PS resin melt and CNTs are mixed, and utilizes shearing force that CNTs is dispersed in the PS matrix.But the various effects of the physical structure of carbon nanotube uniqueness and nano material cause carbon nanotube to assemble entanglement easily, are difficult to effective dispersion.Up to the present each experiment all is to adopt to destroy carbon tube-surface Cheng Jian basically, perhaps go to realize the compound of carbon pipe and polymer materials by other components such as tensio-active agent, coupling agents, and the result greatly differs from each other with theoretical prediction still.
On July 20th, 2005, disclosed one piece of application number was that (the application people is a Chengdu Organical Chemical Co., Ltd., Chinese Academy of Sciences for 200410021654.9 Chinese patent, invention is artificially in making dragon, Chen Li, Zhang Bailan, Qu Meizhen), proposition adds carbon nanotube, polymkeric substance and tensio-active agent or coupling agent etc. in a kind of solvent simultaneously, makes its dispersing and dissolving make matrix material by mechanical stirring and ultrasonic wave effect again.This method has obtained certain innovation, but also have following two place's deficiencies with regard to its implementation process: 1) this carbon pipe dispersion process has been added tensio-active agent or coupling agent etc. and has been helped dispersion reagent, finally in matrix material, introduced impurity, must impact over-all propertieies such as the mechanical property of material, optical transparences; 2) supersound process after the polymer dissolution, ultrasonic wave effect meeting causes damage to polymer chain, even interrupts and smash, and destroys this body structure of polymer materials and character then.
Therefore, seek a kind of carbon nano-tube/polymer compound system of purified, stable dispersion, the method based on the matrix material of carbon nanotube for preparing a kind of excellent property is very necessary.
Summary of the invention
For solving prior art existing deficiency in preparation carbon nano-tube/poly benzene composite material, the invention provides that a kind of carbon nanotube is stable in polymkeric substance effectively to be disperseed, and the preparation method of the good polystyrene/carbon nano tube compound material of conductivity.
Above-mentioned purpose of the present invention, the technical scheme of realization is:
A kind of making method of carbon nano-tube/poly vinylbenzene composite conducting material, it is characterized in that comprising step: I, dispose the low concentration polystyrene solution of a solute concentration at 0.1～4wt% with specific solvent, and with this polystyrene solution dispersing Nano carbon tubes; II, according to the required proportioning of matrix material, dispose another part polystyrene solution with same solvent, and with two parts of solution uniform mixing; III, in mixing solutions, add with polystyrene solution in solvent dissolve each other but the another kind of solvent of p-poly-phenyl ethene non-solvent; IV, filtration are collected or oven dry obtains the solid composite conducting material.
Further, the making method of aforementioned a kind of carbon nano-tube/poly vinylbenzene composite conducting material, wherein adopting low concentration polystyrene solution dispersed carbon nano tube concentration in the step I is 0.1～3wt%, the method that adopts only uses mechanical external force that carbon nanotube is separated winding for need not to add under the condition of tensio-active agent, coupling agent.That those mechanical external forces comprise at least is ultrasonic, ball milling, decomposing force that grinding and stirring produced.
Further, the making method of aforementioned a kind of carbon nano-tube/poly vinylbenzene composite conducting material, the specific solvent that wherein is used for the proportioning polystyrene solution described in the step I comprises: N, one of dinethylformamide, N,N-dimethylacetamide, N-N-methyl-2-2-pyrrolidone N-, tetrahydrofuran (THF), benzene, vinylbenzene, toluene, ethylbenzene, dimethylbenzene, isopropyl benzene, methylene dichloride, ethylene dichloride, trichloromethane, ritalin, vinyl acetic monomer, n-butyl acetate, hexanaphthene, butanone and dithiocarbonic anhydride or its combination.
Further, the making method of aforementioned a kind of carbon nano-tube/poly vinylbenzene composite conducting material, wherein polystyrene also comprises the high molecular polymer that forms by polystyrene graft, block described in the step I, comprises high-impact polystyrene HIPS, styrene-acrylonitrile SAN, styrene-butadiene-styrene rubber SBS, styrene-butadiene rubber(SBR) SB, acrylonitrile-butadiene-styrene resin ABS and styrene-ethylene-butylene copolymer elastomerics SEBS at least.
Further, the making method of aforementioned a kind of carbon nano-tube/poly vinylbenzene composite conducting material, wherein be used for dispersed carbon nano tube described in the step I and be prepared from, and described carbon nanotube is in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes or the carbon nano fiber one or more for the method that adopts one of chemical Vapor deposition process, catalyse pyrolysis, arc-over, template or laser evaporation method.
Further, this carbon nanotube is modified with carboxyl, amido, hydroxyl, fluorine or acid amides through chemical technology.
Further, the making method of aforementioned a kind of carbon nano-tube/poly vinylbenzene composite conducting material, wherein another kind of solvent comprises water, methyl alcohol, ethanol and acetone at least described in the step III.
Further, the making method of aforementioned a kind of carbon nano-tube/poly vinylbenzene composite conducting material, wherein said solid composite conducting material comprises block, film and powder.
Implement technical scheme of the present invention, compare to its significant advantage of prior art and be:
The present invention utilizes directly that the chain of polystyrene matrix material twines, π-π interacts etc. and makes that carbon nanotube is able to evenly, stable dispersion, disperse after need not to add use auxiliary dispersants or chemically modified, avoided the destruction of supersound process to matrix, preserve the basic structure and the performance of body material, improved the purity of matrix material simultaneously greatly; In addition, operating procedure of the present invention is simple, and solvent for use can reclaim repeated use fully, has significantly reduced cost of manufacture.
For the making method that makes a kind of carbon nano-tube/poly vinylbenzene of the present invention composite conducting material is easier to understand the practicality of its substantive distinguishing features and institute's tool thereof, below constipation close accompanying drawing the some specific embodiments of the present invention be described in further detail.But following description and explanation about embodiment do not constitute any limitation protection domain of the present invention.
Description of drawings
Fig. 1 is the general flow chart of making method of the present invention;
Fig. 2 is the dispersion liquid synoptic diagram of polystyrene matrix dispersing Nano carbon tubes in DMF;
Fig. 3 is the digital photograph of the cinnamic mixed dispersion liquid of carbon nano-tube/poly in deionized water;
Fig. 4 is the powdered sample photo after the present invention makes matrix material oven dry, and wherein Fig. 4 a is that to account for the matrix material mass ratio be that 1% finished product, Fig. 4 b are that to account for the matrix material mass ratio be 0.1% finished product to carbon nanotube to carbon nanotube;
Fig. 5 a～Fig. 5 h is the film sample photo of matrix material after hot pressing that the present invention makes different carbon nanotube proportionings;
Fig. 6 is the block sample photo of matrix material after hot pressing that the present invention makes, and wherein Fig. 6 a is that sectional schematic diagram, Fig. 6 b are surface scan Electronic Speculum figure;
Fig. 7 is the conductivity graphic representation of the matrix material that makes of the present invention.
Embodiment
The invention provides a kind of preparation method of polystyrene composite conductive material of carbon nanotubes.The method includes the steps of: dispose a low concentration polystyrene solution with specific solvent, by the effect dispersing Nano carbon tubes (need not add any carbon nanotube dispersion agent) such as winding parcel of polystyrene to carbon nanotube; According to required proportioning, dispose the polystyrene solution of a higher concentration with same solvent; Two parts of dispersion liquids are mixed; Mixed solution is added in the another kind of solvent, and carbon nanotube precipitates simultaneously with the polystyrene that is wrapped on the carbon nanotube; Filter and collect the compound sample of gained solid.
Wherein: formerly the lower concentration polystyrene solution solute concentration that obtains of configuration is between 0.1～4wt% in the step, and institute's dispersed carbon nano tube concentration is 0.1～3wt%; The polystyrene solution fat melting concentration that configuration obtains in the step of back is usually above 5%.The solvent that is used for polystyrene in above-mentioned two steps comprises N, one of dinethylformamide, N,N-dimethylacetamide, N-N-methyl-2-2-pyrrolidone N-, tetrahydrofuran (THF), benzene, vinylbenzene, toluene, ethylbenzene, dimethylbenzene, isopropyl benzene, methylene dichloride, ethylene dichloride, trichloromethane, ritalin, vinyl acetic monomer, n-butyl acetate, hexanaphthene, butanone and dithiocarbonic anhydride or its combination.And this polystyrene also comprises the high molecular polymer that forms by polystyrene graft, block, comprises high-impact polystyrene HIPS, styrene-acrylonitrile SAN, styrene-butadiene-styrene rubber SBS, styrene-butadiene rubber(SBR) SB, acrylonitrile-butadiene-styrene resin ABS and styrene-ethylene-butylene copolymer elastomerics SEBS at least.
In addition, above-mentioned another kind of solvent for polystyrene solution in specific solvent dissolve each other, but the non-liquid that dissolves each other of p-poly-phenyl ethene matrix itself can select to comprise water, methyl alcohol, ethanol or acetone etc.
And this is used for dispersed carbon nano tube and is prepared from for the method that adopts one of chemical Vapor deposition process, catalyse pyrolysis, arc-over, template or laser evaporation method, and described carbon nanotube is in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes or the carbon nano fiber one or more.Also can further modify carboxyl, amido, hydroxyl, fluorine or acid amides etc. on the carbon nanotube.
As shown in Figure 1, be preparation method's general flow chart of carbon nano-tube/poly vinylbenzene composite conducting material of the present invention, comprise the steps:
Embodiment 2:
With polystyrene block copolymer ABS fully dissolving in DMF (N, dinethylformamide) solvent, matched proportion density is 2%, adds 0.2% carbon nanotube dust then therein, and 100W supersound process 4 hours obtains finely dispersed carbon nanotube dispersion liquid A.Add ABS again in another part DMF solvent, stirring is fully dissolved it, and matched proportion density is 5%, obtains solution B.Will A liquid and B liquid mix the back and continue to stir half an hour, mixed solution is injected the deionized water of high-speed stirring, leave standstill for some time after, the suction filtration oven dry obtains required composite conducting sample.
Embodiment 3:
Polystyrene block copolymer SBS at N, is fully dissolved in the N-dimethyl pyrrolidone, and matched proportion density is 4%, adds 0.1% carbon nanotube dust then therein, and 200W supersound process 3 hours obtains finely dispersed carbon nanotube dispersion liquid A.At another part N, add SBS in the N-dimethyl pyrrolidone again, stirring is fully dissolved it, and matched proportion density is 5%, obtains solution B.Will A liquid and B liquid mix the back and continue to stir half an hour, mixed solution is injected the deionized water of high-speed stirring, leave standstill for some time after, the suction filtration oven dry obtains required composite conducting sample.
Embodiment 4:
With polystyrene block copolymer SEBS fully dissolving in N,N-dimethylacetamide, matched proportion density is 4%, adds 3% carbon nanotube dust then therein, and 200W supersound process 3 hours obtains finely dispersed carbon nanotube dispersion liquid A.Add SEBS again in another part N,N-dimethylacetamide, stirring is fully dissolved it, and matched proportion density is 15%, obtains solution B.Will A liquid and B liquid mix the back and continue to stir half an hour, mixed solution is injected the deionized water of high-speed stirring, leave standstill for some time after, the suction filtration oven dry obtains required composite conducting sample.
In addition to the implementation, making method of the present invention:, can carry out partial purification to carbon nanotube and handle if residual in carbon nanotube have carrier and a granules of catalyst.Generally be by suitable reagent such as pickling such as nitric acid, sulfuric acid, to remove catalyzer and support of the catalyst, also further vapour phase oxidation process is removed decolorizing carbon etc.
According to the performance need that variant production uses, this composite conducting material also can add other mineral filler in preparation process, as carbon black, titanium dioxide, magnetite, lime carbonate, silicon-dioxide, glass fibre, asbestos etc.Because some filler small molecules can improve polymkeric substance the plasticizing flowability, improve resistance of aging etc., thereby only otherwise destroy final conduction, heat conduction and the mechanical property of matrix material, other auxiliary agents can add as required in right amount.
Prepared matrix material can be applied in needs conductions or consumption electrostatic occasion according to the present invention, as is used for the travelling belt etc. of standard sheath, cable joint-box, hospital's paster, computer magnetic tape or mining site of audiovisual dish, conductive fabric, the electric wire of power consumption parts, the conduction of automobile.In addition, but the carbon nano tube compound material of this polystyrene parcel also direct heat be pressed into film or sheet material etc. and directly use, also can be used as conducting masterbatch adds in other polymeric matrixs, prepares the excellent more matrix material of over-all properties.
Below only be the representational embodiment that has much in the numerous concrete exemplary applications of the present invention, protection scope of the present invention is not constituted any limitation.All employing equivalents or equivalence are replaced and the technical scheme of formation, all drop within the rights protection scope of the present invention.
Claims (9)
1. the making method of a carbon nano-tube/poly vinylbenzene composite conducting material, it is characterized in that comprising step: I, dispose the low concentration polystyrene solution of a solute concentration at 0.1～4wt% with specific solvent, and with this polystyrene solution dispersing Nano carbon tubes;
II, according to the required proportioning of matrix material, dispose another part polystyrene solution with same solvent, and with two parts of solution uniform mixing;
III, in mixing solutions, add with polystyrene solution in solvent dissolve each other but the another kind of solvent of p-poly-phenyl ethene non-solvent;
IV, filtration are collected or oven dry obtains the solid composite conducting material.
2. the making method of a kind of carbon nano-tube/poly vinylbenzene composite conducting material according to claim 1, it is characterized in that: adopting low concentration polystyrene solution dispersed carbon nano tube concentration in the step I is 0.1～3wt%, the method that adopts only uses mechanical external force that carbon nanotube is separated winding for need not to add under the condition of tensio-active agent, coupling agent.
3. the making method of a kind of carbon nano-tube/poly vinylbenzene composite conducting material according to claim 2 is characterized in that: described mechanical external force comprises ultrasonic, ball milling, the decomposing force that grinding and stirring produced at least.
4. the making method of a kind of carbon nano-tube/poly vinylbenzene composite conducting material according to claim 1, it is characterized in that: the specific solvent that is used for the proportioning polystyrene solution described in the step I comprises: N, one of dinethylformamide, N,N-dimethylacetamide, N-N-methyl-2-2-pyrrolidone N-, tetrahydrofuran (THF), benzene, vinylbenzene, toluene, ethylbenzene, dimethylbenzene, isopropyl benzene, methylene dichloride, ethylene dichloride, trichloromethane, ritalin, vinyl acetic monomer, n-butyl acetate, hexanaphthene, butanone and dithiocarbonic anhydride or its combination.
5. according to the making method of claim 1,2 or 4 described a kind of carbon nano-tube/poly vinylbenzene composite conducting materials, it is characterized in that: described polystyrene also comprises the high molecular polymer that forms by polystyrene graft, block, comprises high-impact polystyrene HIPS, styrene-acrylonitrile SAN, styrene-butadiene-styrene rubber SBS, styrene-butadiene rubber(SBR) SB, acrylonitrile-butadiene-styrene resin ABS and styrene-ethylene-butylene copolymer elastomerics SEBS at least.
6. the making method of a kind of carbon nano-tube/poly vinylbenzene composite conducting material according to claim 1, it is characterized in that: be used for dispersed carbon nano tube in the step I and be prepared from, and described carbon nanotube is in Single Walled Carbon Nanotube, multi-walled carbon nano-tubes or the carbon nano fiber one or more for the method that adopts one of chemical Vapor deposition process, catalyse pyrolysis, arc-over, template or laser evaporation method.
7. the making method of a kind of carbon nano-tube/poly vinylbenzene composite conducting material according to claim 6 is characterized in that: described carbon nanotube is modified with carboxyl, amido, hydroxyl, fluorine or acid amides through chemical technology.
8. the making method of a kind of carbon nano-tube/poly vinylbenzene composite conducting material according to claim 1 is characterized in that: another kind of solvent comprises water, methyl alcohol, ethanol and acetone at least described in the step III.
9. the making method of a kind of carbon nano-tube/poly vinylbenzene composite conducting material according to claim 1 is characterized in that: described solid composite conducting material comprises block, film and powder.
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