CN102766304B - Three-dimensional graphene network-contained high conductivity polymer composite material and preparation method thereof - Google Patents
Three-dimensional graphene network-contained high conductivity polymer composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a three-dimensional graphene network-contained high conductivity polymer composite material and a preparation method thereof. The preparation method includes: enabling graphene oxide and cationic polymer emulsion particles to form a condensate in a solvent by means of static self-assembly and leaching for film formation; and using reductant to restore the graphene oxide in the condensate film, washing, drying and mould pressing to obtain the three-dimensional graphene network-contained high conductivity polymer composite material. The preparation method is simple, easy to operate and high in controllability and can be used for large-scale production. In addition, the three-dimensional graphene network structure enables graphene to be uniformly dispersed in polymer matrix and enables graphene sheets to be mutually connected closely, so that contact resistance among the graphene sheets is greatly reduced. Consequently, the obtained polymer composite material with low amount of the graphene added is quite high in conductivity and has important application value in fields of electromagnetic shielding, highly conductive glue, sensors, brakes and the like.
Description
Technical field
The invention belongs to Graphene/polymer composites preparation field, relate in particular to a kind of high conductivity polymer composites containing three-dimensional grapheme network and preparation method thereof.
Background technology
Graphene is a kind of carbonaceous material of closely being piled up the bi-dimensional cellular shape crystalline network forming by monolayer carbon atom.Although Graphene only has a carbon atom thickness, is one the thinnest in known materials,, it has the charming character of many uniquenesses, as high Young's modulus (1100GPa), thermal conductivity (5000W/mk) and carrier mobility (2 × 10
5cm
2v
-1s
-1).The characteristic that these are superior and two-dirnentional structure are with a wide range of applications Graphene.One of them very important application is the polymer composites that utilizes the high conduction of these character preparations of Graphene.
But, between graphene sheet layer, there is strong π-π effect and hydrophobic force effect, very easily reunite, in conventional solvent, do not dissolve and be difficult to disperse yet.In addition, Graphene not melting under hot conditions, processing difficulties, these shortcomings are had a greatly reduced quality the high-performance of Graphene, even cannot bring into play.Thereby Graphene/polymer composites specific conductivity that solvent method or scorification obtain is lower, limit its application in a lot of fields.The functionalization of Graphene can be the dispersiveness of raising Graphene in polymeric matrix an effective approach is provided.
In recent years, more existing relevant reports about the surface-functionalized modification of Graphene, as being connected to Graphene surface by covalent linkage containing phenyl ring organic molecule, improve its dispersiveness in polystyrene matrix, polymer composites conductivity value containing this functionalization graphene of 2.5vol% reaches 1S/m(S.Stankovich, et al.nature, 2006,442,04969.); Or adopt ion liquid functionalization Graphene, the specific conductivity that contains the polymer composites of 4.19vol% ion liquid functionalization Graphene reaches 13.84S/m.
But functionalization graphene/polymer composites conductivity value is still far below theoretical value.Its reason is, even if functionalization graphene is evenly dispersed in polymeric matrix, still has high contact resistance between graphene film, and in addition, functionalization group has also reduced the resistance of Graphene self.
In polymeric matrix, build three-dimensional mutual close-connected Graphene network and not only can make graphene uniform be distributed in polymeric matrix, and greatly reduced the contact resistance between graphene film.In addition, three-dimensional grapheme network, without organics function is carried out in Graphene surface, reduces the resistance of Graphene self.But how building simply and effectively three-dimensional grapheme network in polymeric matrix is a challenging job.
Summary of the invention
For the above-mentioned deficiency of prior art, the first object of the present invention is to provide a kind of high conductivity polymer composites containing three-dimensional grapheme network, and it,, under low Graphene percentage composition, can obtain high conductivity.
The second object of the present invention is to provide a kind of preparation method of the high conductivity polymer composites containing three-dimensional grapheme network.
Technical scheme of the present invention is as follows:
A kind of high conductivity polymer composites containing three-dimensional grapheme network, in the matrix of described polymer composites, comprise three-dimensional interconnective Graphene network, in this Graphene network, Graphene is evenly distributed, its percentage composition is within the scope of 5%-20%, and the described high conductivity polymer composites containing three-dimensional grapheme network is prepared by the method that comprises following synthesis step:
(1) by graphene oxide and cationic polymers emulsion particle, the mode by electrostatic self-assembled in solvent forms condensation product, afterwards through suction filtration film forming; Wherein, described solvent is water, the described mode by electrostatic self-assembled forms the step of condensation product and carries out under solutions of weak acidity, comprise: first graphene oxide and cationic polymers emulsion particle are dispersed in respectively in described solvent and adjust respectively pH value to 2-5, then be mixed to form condensation product and stir, wherein said cationic polymers emulsion particle is selected from one or more of cation polystyrene emulsion particle, cationic ethylene vinyl acetate emulsion particle, cation polyurethane emulsion particle or positively charged ion polymethylmethacrylate emulsion particle;
(2) graphene oxide that adopts reductive agent to reduce in above-mentioned condensation product film, temperature of reaction is 50-90 DEG C, and above-mentioned reduction process is carried out in reductant solution, and described reductive agent is selected from hydrazine hydrate, hydroiodic acid HI, sodium borohydride, xitix or vat powder; Then through washing, oven dry, mold pressing, obtain the high conductivity polymer composites containing three-dimensional grapheme network.
Preferably, the described Graphene content containing in the high conductivity polymer composites of three-dimensional grapheme network can regulate by the mass ratio of controlling graphene oxide and cationic polymers emulsion particle.
Preferably, the concentration of described graphene oxide is 0.2-2mg/ml, and the concentration of described cationic polymers emulsion particle is 1-5mg/ml.
Preferably, in the condensation product of described synthesis step (1), graphene oxide is coated on equably the surface of emulsion particle and is interconnected to constitute network.
Preferably, the oven dry in described synthesis step (2) is vacuum-drying.
Compared with prior art, beneficial effect of the present invention is as follows:
First, the present invention, taking graphene oxide and polyalcohol emulsion particle as raw material, adopts electrostatic self-assembled approach to obtain the polymer composites containing three-dimensional grapheme network, and this matrix material has high specific conductivity, compared with traditional solvent blending method, specific conductivity at least exceeds an order of magnitude.
The second, preparation process environmental protection of the present invention, the solvent of use is the aqueous solution, without a large amount of organic solvents.
The 3rd, preparation method of the present invention is simple to operation, and controllability is strong, can mass-producing amplify production.
Certainly, implement arbitrary product of the present invention and might not need to reach above-described all advantages simultaneously.
Brief description of the drawings
Fig. 1 is polystyrene and Graphene condensation product scanning electronic microscope (SEM) picture of the embodiment of the present invention 1, and Graphene content is 10%;
Fig. 2 is ethylene vinyl acetate and the Graphene condensation product SEM picture of the embodiment of the present invention 2, and Graphene content is 5%;
Fig. 3 is Graphene/poly styrene composite material and the Graphene/poly styrene composite material that adopts organic solvent blending method to prepare and the specific conductivity comparison diagram of Carbon Nanotubes/Polystyrene Nanocomposites prepared by the embodiment of the present invention 1 and embodiment 3;
Fig. 4 is the SEM picture of the three-dimensional grapheme network that retains after the polymeric matrix high temperature pyrolysis in the polystyrene/graphene matrix material prepared of the embodiment of the present invention 1.
Embodiment
High conductivity polymer composites containing three-dimensional grapheme network of the present invention is taking graphene oxide and polyalcohol emulsion particle as raw material, obtain by self-assembly approach, in the polymeric matrix of this matrix material, Graphene is evenly distributed and interconnects, its percentage composition is within the scope of 5%-20%, and the content of Graphene can regulate by the mass ratio of controlling graphene oxide and cationic polymers emulsion particle.
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network of the present invention mainly comprises following two steps:
(1) graphene oxide and the cationic polymers emulsion particle mode by electrostatic self-assembled in solvent forms condensation product, and through suction filtration film forming, preferably, this process can be carried out under solutions of weak acidity, but is not limited to solutions of weak acidity;
(2) graphene oxide that adopts reductive agent to reduce in above-mentioned condensation product film, temperature of reaction is 50-90 DEG C, through washing, oven dry, mold pressing, obtains the high electricity conductive polymer composite material that contains three-dimensional grapheme network.
Below in conjunction with specific embodiment, further set forth the present invention.Should be appreciated that, these embodiment are only for the present invention is described, and are not intended to limit the scope of the invention.Technician makes according to the present invention in actual applications improvement and adjustment, still belong to protection scope of the present invention.
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network in the present embodiment is as follows:
(1) 0.1g graphene oxide and 0.95g cation polystyrene emulsion particle are dispersed in respectively in the 200ml aqueous solution, and the pH value of the aqueous solution is adjusted to respectively to 4-5, then, under stirring and adjusting, above-mentioned two kinds of solution are slowly joined in an empty receptacle simultaneously, graphene oxide forms condensation product immediately after contacting with emulsion particle, stir after 10min, by the condensation product suction filtration film forming obtaining;
(2) obtain graphene oxide-latex granulosa to be immersed in 200ml concentration be redox graphene in 50% hydroiodic acid HI solution above-mentioned, after 90 DEG C of reaction 4h, with deionized water repeated washing Graphene-latex granulosa, then 60 DEG C of vacuum-dryings and 120 DEG C of mold pressings, obtain the high conductivity polymer composites containing three-dimensional grapheme network.Characterize as follows to this matrix material:
Morphology characterization: Fig. 1 is the polystyrene latex grain of the present embodiment and the SEM picture of Graphene condensation product, visible in Fig. 1, is coated on the surface of emulsion particle graphene uniform and is interconnected to form three-dimensional grapheme network; The polymeric matrix of the high conductivity polymer composites containing three-dimensional grapheme network that the present embodiment is obtained carries out high temperature pyrolysis, and the three-dimensional grapheme network retaining is carried out to SEM sign, referring to Fig. 4, visible in Fig. 4, Graphene has formed three-dimensional net structure.
Specific conductivity characterizes: the high conductivity polymer composites containing three-dimensional grapheme network that the present embodiment is obtained carries out conductivity measurement, as shown in Figure 3, and Graphene/poly styrene composite material that it is prepared with organic solvent blending method is compared with Carbon Nanotubes/Polystyrene Nanocomposites, in Fig. 3, can find out, the specific conductivity of the matrix material that the present embodiment obtains at least exceeds an order of magnitude, high specific conductivity mainly gives the credit to this matrix material and contains three-dimensional close-connected Graphene network, as shown in Figure 4.
In the present embodiment, be 5% (volume fraction percentage composition 2.4%) containing the percentage composition of Graphene in the high conductivity polymer composites of three-dimensional grapheme network.
Embodiment 2
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network in the present embodiment is as follows:
(1) 0.1g graphene oxide and 0.95g cationic ethylene vinyl acetate emulsion particle are dispersed in respectively in the 200ml aqueous solution, and the pH value of the aqueous solution is adjusted to respectively to 2-4, then, under stirring and adjusting, above-mentioned two kinds of solution are slowly joined in an empty receptacle simultaneously, graphene oxide forms condensation product immediately after contacting with emulsion particle, stir after 10min, by the condensation product suction filtration film forming obtaining;
(2) obtain graphene oxide-latex granulosa to be immersed in 200ml concentration be redox graphene in 50% hydroiodic acid HI solution above-mentioned, after 90 DEG C of reaction 4h, with deionized water repeated washing Graphene-latex granulosa, then 50 DEG C of vacuum-dryings and 75 DEG C of mold pressings, obtain the high conductivity polymer composites containing three-dimensional grapheme network.Fig. 2 is plastic of poly vinyl acetate emulsion particle and the Graphene condensation product SEM picture of the present embodiment, visible in Fig. 2, is coated on the surface of emulsion particle graphene uniform and is interconnected to form three-dimensional grapheme network.
In the present embodiment, be 5% containing the percentage composition of Graphene in the high conductivity polymer composites of three-dimensional grapheme network.
Embodiment 3
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network in the present embodiment is as follows:
(1) 0.2g graphene oxide and 0.9g polystyrene latex grain are dispersed in respectively in the 200ml aqueous solution, and the pH value of the aqueous solution is adjusted to respectively to 2-4, then, under stirring and adjusting, above-mentioned two kinds of solution are slowly joined in an empty receptacle simultaneously, graphene oxide forms condensation product immediately after contacting with emulsion particle, stir after 10min, by the condensation product suction filtration film forming obtaining;
(2) obtain graphene oxide-latex granulosa to be immersed in 200ml concentration be redox graphene in 10% hydrazine hydrate solution above-mentioned, after 80 DEG C of reaction 4h, with deionized water repeated washing Graphene-latex granulosa, then 50o vacuum-drying and 120 DEG C of mold pressings, obtain the high conductivity polymer composites containing three-dimensional grapheme network.
The high conductivity polymer composites containing three-dimensional grapheme network that the present embodiment is obtained carries out conductivity measurement, as shown in Figure 3, and Graphene/poly styrene composite material that it is prepared with organic solvent blending method is compared with Carbon Nanotubes/Polystyrene Nanocomposites, in Fig. 3, can find out, the specific conductivity of the matrix material that the present embodiment obtains at least exceeds an order of magnitude, and high specific conductivity mainly gives the credit to this matrix material and contains three-dimensional close-connected Graphene network.
In the present embodiment, be 10% (volume fraction percentage composition 4.8%) containing the percentage composition of Graphene in the high conductivity polymer composites of three-dimensional grapheme network.
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network in the present embodiment is as follows:
(1) 0.2g graphene oxide and 0.6g polyurethane latex grain are dispersed in respectively in the 200ml aqueous solution, and the pH value of the aqueous solution is adjusted to respectively to 2-3, then, under stirring and adjusting, above-mentioned two kinds of solution are slowly joined in an empty receptacle simultaneously, graphene oxide forms condensation product immediately after contacting with emulsion particle, stir after 10min, by the condensation product suction filtration film forming obtaining;
(2) obtain graphene oxide-latex granulosa to be immersed in 200ml concentration be redox graphene in 30% ascorbic acid solution above-mentioned, after 80 DEG C of reaction 4h, with deionized water repeated washing Graphene-latex granulosa, then 50 DEG C of vacuum-dryings and 100 DEG C of mold pressings, obtain the high conductivity polymer composites containing three-dimensional grapheme network.
In the present embodiment, be 15% containing the percentage composition of Graphene in the high conductivity polymer composites of three-dimensional grapheme network.
Embodiment 5
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network in the present embodiment is as follows:
(1) 0.3g graphene oxide and 0.6g polymethyl acrylic acid emulsion particle are dispersed in respectively in the 200ml aqueous solution, and the pH value of the aqueous solution is adjusted to respectively to 2-4, then, under stirring and adjusting, above-mentioned two kinds of solution are slowly joined in an empty receptacle simultaneously, graphene oxide forms condensation product immediately after contacting with emulsion particle, stir after 10min, will obtain condensation product suction filtration film forming;
(2) obtain graphene oxide-latex granulosa to be immersed in 200ml concentration be redox graphene in 20% safety powder solution above-mentioned, after 80 DEG C of reaction 10h, with deionized water repeated washing Graphene-latex granulosa, then 50 DEG C of vacuum-dryings and 120 DEG C of mold pressings, obtain the high conductivity polymer composites containing three-dimensional grapheme network.
In the present embodiment, be 20% containing the percentage composition of Graphene in the high conductivity polymer composites of three-dimensional grapheme network.
Embodiment 6
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network in the present embodiment is as follows:
(1) 0.04g graphene oxide and 0.2g polymethyl acrylic acid emulsion particle are dispersed in respectively in the 200ml aqueous solution, and the pH value of the aqueous solution is adjusted to respectively to 2-4, then, under stirring and adjusting, above-mentioned two kinds of solution are slowly joined in an empty receptacle simultaneously, graphene oxide forms condensation product immediately after contacting with emulsion particle, stir after 10min, will obtain condensation product suction filtration film forming;
(2) obtain graphene oxide-latex granulosa to be immersed in 200ml concentration be redox graphene in 10% sodium borohydride solution above-mentioned, after 80o DEG C of reaction 10h, with deionized water repeated washing Graphene-latex granulosa, then 50 DEG C of vacuum-dryings and 120 DEG C of mold pressings, obtain the high conductivity polymer composites containing three-dimensional grapheme network.
In the present embodiment, be 9% containing the percentage composition of Graphene in the high conductivity polymer composites of three-dimensional grapheme network.
Embodiment 7
The preparation method of the high conductivity polymer composites containing three-dimensional grapheme network in the present embodiment is as follows:
(1) 0.4g graphene oxide and 1.0g polymethyl acrylic acid emulsion particle are dispersed in respectively in the 200ml aqueous solution, and the pH value of the aqueous solution is adjusted to respectively to 2-4, then, under stirring and adjusting, above-mentioned two kinds of solution are slowly joined in an empty receptacle simultaneously, graphene oxide forms condensation product immediately after contacting with emulsion particle, stir after 10min, will obtain condensation product suction filtration film forming;
(2) obtain graphene oxide-latex granulosa to be immersed in 200ml concentration be redox graphene in 10% sodium borohydride solution above-mentioned, after 80 DEG C of reaction 10h, with deionized water repeated washing Graphene-latex granulosa, then 50 DEG C of vacuum-dryings and 120 DEG C of mold pressings, obtain the high conductivity polymer composites containing three-dimensional grapheme network.
In the present embodiment, be 17% containing the percentage composition of Graphene in the high conductivity polymer composites of three-dimensional grapheme network.
The disclosed preferred embodiment of the present invention is just for helping to set forth the present invention above.Preferred embodiment does not have all details of detailed descriptionthe, and also not limiting this invention is only described embodiment.Obviously,, according to the content of this specification sheets, can make many modifications and variations.These embodiment are chosen and specifically described to this specification sheets, is in order to explain better principle of the present invention and practical application, thereby under making, technical field technician can understand and utilize the present invention well.The present invention is only subject to the restriction of claims and four corner and equivalent.
Claims (5)
1. the high conductivity polymer composites containing three-dimensional grapheme network, it is characterized in that, in the matrix of described polymer composites, comprise three-dimensional interconnective Graphene network, in this Graphene network, Graphene is evenly distributed, its percentage composition is within the scope of 5%-20%, and the described high conductivity polymer composites containing three-dimensional grapheme network is prepared by the method that comprises following synthesis step:
(1) by graphene oxide and cationic polymers emulsion particle, the mode by electrostatic self-assembled in solvent forms condensation product, afterwards through suction filtration film forming, wherein, described solvent is water, the described mode by electrostatic self-assembled forms the step of condensation product and carries out under solutions of weak acidity, comprise: first graphene oxide and cationic polymers emulsion particle are dispersed in respectively in described solvent and distinguish adjust pH to 2-5, then be mixed to form condensation product and stir, wherein said cationic polymers emulsion particle is selected from cation polystyrene emulsion particle, cationic ethylene vinyl acetate emulsion particle, one or more of cation polyurethane emulsion particle or positively charged ion polymethylmethacrylate emulsion particle,
(2) graphene oxide that adopts reductive agent to reduce in above-mentioned condensation product film, temperature of reaction is 50-90 DEG C, and above-mentioned reduction process is carried out in reductant solution, and described reductive agent is selected from hydrazine hydrate, hydroiodic acid HI, sodium borohydride, xitix or vat powder; Then through washing, oven dry, mold pressing, obtain the high conductivity polymer composites containing three-dimensional grapheme network.
2. the high conductivity polymer composites containing three-dimensional grapheme network as claimed in claim 1, it is characterized in that, the described Graphene content containing in the high conductivity polymer composites of three-dimensional grapheme network can regulate by the mass ratio of controlling graphene oxide and cationic polymers emulsion particle.
3. the high conductivity polymer composites containing three-dimensional grapheme network as claimed in claim 1, is characterized in that, the concentration of described graphene oxide is 0.2-2mg/ml, and the concentration of described cationic polymers emulsion particle is 1-5mg/ml.
4. the high conductivity polymer composites containing three-dimensional grapheme network as claimed in claim 1, is characterized in that, in the condensation product of described synthesis step (1), graphene oxide is coated on equably the surface of emulsion particle and is interconnected to constitute network.
5. the high conductivity polymer composites containing three-dimensional grapheme network as claimed in claim 1, is characterized in that, the oven dry in described synthesis step (2) is vacuum-drying.
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| CN103074619A (en) * | 2013-02-06 | 2013-05-01 | 上海应用技术学院 | Graphene oxide-silver compound particle and preparation method thereof |
| CN104650498B (en) * | 2013-11-22 | 2017-06-09 | 中国科学院金属研究所 | A kind of Graphene/polymer composite conductive thin film material and preparation method thereof |
| CN103937234B (en) * | 2014-04-19 | 2016-03-23 | 中山市永威新材料有限公司 | Heat-conducting plastic of a kind of applying modified carbon material and preparation method thereof |
| CN106349658B (en) * | 2016-08-22 | 2018-04-06 | 广东纳路纳米科技有限公司 | The plastic composite being modified based on three-dimensional grapheme and its preparation |
| CN107841123B (en) * | 2016-09-18 | 2022-03-04 | 洛阳尖端技术研究院 | Three-dimensional graphene-based wave-absorbing metamaterial base material and preparation method thereof |
| CN106556677B (en) * | 2016-10-27 | 2018-07-06 | 苏州大学 | A kind of three-dimensional porous graphene extra-thin film gas sensor and preparation method thereof |
| CN108530073B (en) * | 2017-10-08 | 2020-06-19 | 北京化工大学 | Preparation method of flexible self-supporting three-dimensional porous graphene membrane |
| CN108752722B (en) * | 2018-05-21 | 2020-11-24 | 福州大学 | Antistatic EVA foam composite material and preparation method thereof |
| CN109233124B (en) * | 2018-06-27 | 2020-02-11 | 天津大学 | Polystyrene-graphene oxide composite block material, graphene-based porous block material and preparation method thereof |
| CN109280260B (en) * | 2018-09-17 | 2021-05-18 | 辽宁通用电缆有限公司 | Graphene-added ethylene-vinyl acetate copolymer conductive granules and preparation method thereof |
| CN109912960B (en) * | 2019-03-06 | 2021-06-22 | 常州大学 | Preparation method of high-conductivity tensile strain response material |
| CN110343347B (en) * | 2019-07-19 | 2021-09-14 | 广州特种承压设备检测研究院 | Polyvinylidene fluoride SiO2Modified graphene composite material and preparation method thereof |
| CN113604133A (en) * | 2021-08-30 | 2021-11-05 | 航天科工武汉磁电有限责任公司 | Light carbon-based electromagnetic shielding coating and preparation method thereof |
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