CN103972465B - The preparation method of a kind of fexible film electrode - Google Patents
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- CN103972465B CN103972465B CN201410217653.5A CN201410217653A CN103972465B CN 103972465 B CN103972465 B CN 103972465B CN 201410217653 A CN201410217653 A CN 201410217653A CN 103972465 B CN103972465 B CN 103972465B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 72
- 239000007772 electrode material Substances 0.000 claims abstract description 69
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- 239000007788 liquid Substances 0.000 claims abstract description 20
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract 2
- 238000001914 filtration Methods 0.000 claims description 8
- 239000012528 membrane Substances 0.000 claims description 8
- 229920002678 cellulose Polymers 0.000 claims description 6
- FFBHFFJDDLITSX-UHFFFAOYSA-N benzyl N-[2-hydroxy-4-(3-oxomorpholin-4-yl)phenyl]carbamate Chemical compound OC1=C(NC(=O)OCC2=CC=CC=C2)C=CC(=C1)N1CCOCC1=O FFBHFFJDDLITSX-UHFFFAOYSA-N 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 13
- 239000000463 material Substances 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000013019 agitation Methods 0.000 description 4
- 239000008240 homogeneous mixture Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000007669 thermal treatment Methods 0.000 description 4
- 238000000576 coating method Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000003610 charcoal Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008358 core component Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/66—Current collectors
- H01G11/68—Current collectors characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The present invention discloses the preparation method of a kind of fexible film electrode, the method is taking heat treated graphene oxide as conductive supporting and mechanical support, fexible film electrode is obtained by vacuum filtration process one step, specifically comprise the following steps: graphene oxide water solution is heat-treated, obtain heat treated graphene oxide water solution; Electrode active material is scattered in water and forms electrode active material dispersion liquid; Heat treated for gained graphene oxide water solution and electrode active material dispersion liquid are mixed to get mixing solutions, filter and after drying, obtain the fexible film electrode of heat treated graphene oxide and electrode active material hydridization. The method of the present invention is simple to operate, with low cost. The fexible film electrode of heat treated graphene oxide prepared by the inventive method and electrode active material hydridization has uniform laminate structure, and there is excellent electroconductibility and good snappiness, can extensively for fields such as battery, electrochemical capacitance material and environmental protection automobiles.
Description
Technical field
The present invention relates to a kind of fexible film electrode, particularly relate to the fexible film electrode of a kind of heat treated graphene oxide and electrode active material hydridization, can be used in new energy materials field.
Background technology
Along with the growing of flexible electronic device and development, the flexible energy storage device of exploitation has become the research focus in energy storage field. Wherein, electrode materials is as the core component of energy storage device, thus becomes the research emphasis of researcher and receive and pay close attention to widely. At present, the preparation method of fexible film electrode mainly contains vacuum filtration process, coating method, in situ synthesis. Coating method and in situ synthesis occupy bigger volume and quality in the electrodes due to collector, thus significantly reduce energy density and the power density of overall electrode. And the film of vacuum filtration process prepared by it is an independent film, collector is comprised in electrode interior, thus greatly reduce the ratio of collector shared dead volume in the electrodes, simultaneously owing to its special laminate structure is in electrochemical reaction, take full advantage of electrode active material, therefore considerably improve energy density and the power density of overall electrode.
Graphene is as the mono-layer graphite of sp2 hydridization charcoal material base meta structure, there is excellent electroconductibility and higher snappiness, therefore conductive supporting and the mechanical support being widely used as flexible electrode material, obtains high performance fexible film electrode by vacuum filtration itself and electrode active material. But, in actual applications, Graphene usually tends to irreversible reunion or stacking due to its hydrophobicity, thus loses original excellent properties. Although Graphene can by strengthening its dispersion stabilization at other molecules of its surface graft or polymkeric substance, but Graphene can be caused to have poor electroconductibility, too increasing the dead volume of electrode materials, therefore its chemical property is limited by very large in the middle of practical application simultaneously.
Current research finds, heat treated graphene oxide is not when adding any dispersion agent, it is possible to stable existence in aqueous, maintains the electroconductibility of its excellence simultaneously and is similar to other performances of Graphene. In addition, not only preparation condition is gentle for heat treated graphene oxide, process is simple, and can high yield prepare on a large scale. But utilize heat treated graphene oxide not reported yet at present as conductive supporting and the mechanical support of flexible electrode material.
Summary of the invention
Because the above-mentioned defect of prior art, technical problem to be solved by this invention is to provide and a kind of utilizes heat treated graphene oxide as the conductive supporting of flexible electrode material and mechanical support to prepare the method for high-performance flexible membrane electrode.
For achieving the above object, the preparation method of a kind of fexible film electrode of the present invention, using heat treated graphene oxide as conductive supporting and mechanical support, obtained the hydridization fexible film electrode of heat treated graphene oxide and electrode active material by vacuum filtration process one step, specifically comprise the following steps:
(1) graphene oxide water solution is heat-treated, obtain heat treated graphene oxide water solution;
(2) electrode active material is scattered in water and forms electrode active material dispersion liquid;
(3) described heat treated graphene oxide water solution and described electrode active material dispersion liquid are mixed to get mixing solutions, after being filtered by described mixing solutions, filter paper obtains the fexible film electrode of heat treated graphene oxide and electrode active material hydridization;
(4) the fexible film electrode of the described heat treated graphene oxide obtained in step (3) and electrode active material hydridization is dried, the fexible film electrode of described heat treated graphene oxide and electrode active material hydridization is peeled off from filter paper.
Further, described in step (1), the concentration of graphene oxide water solution is 0.01��0.1mg/mL.
Further, heat treated condition described in step (1) is process 1��30 day at 50��90 DEG C.
Further, described in step (2), the concentration of electrode active material dispersion liquid is 0.01��10mg/mL.
Further, described in the described mixing solutions of step (3), the mass ratio of heat treated graphene oxide and described electrode active material is 9:1��1:9.
Further, filter paper described in step (3) is mixed cellulose ester filtering membrane, and aperture is 220nm.
Further, filtering, described in step (3), the device adopted is Vacuum filtration device.
Further, dry described in step (4) temperature is 20��70 DEG C.
Further, the fexible film electrode of described heat treated graphene oxide and electrode active material hydridization has laminate structure.
The preparation method of the fexible film electrode of the present invention has feature simple to operate, with low cost, and its useful effect is:
(1) adopting vacuum filtration process, technique is simple, and obtained heat treated graphene oxide is more even than coating method and in-situ method growth with the fexible film electrode of electrode active material hydridization;
(2) heat treated graphene oxide obtained by and the fexible film electrode of electrode active material hydridization, not only there is high electrode active material and add carrying capacity, there is excellent conductivity and high mechanical flexibility simultaneously, thus significantly increase energy density and the power density of overall electrode, and maintain the good snappiness of this membrane electrode;
(3) heat treated graphene oxide obtained by and the fexible film electrode of electrode active material hydridization, owing to having special laminate structure, effectively promote its electrochemical reaction, the lifting of its chemical property played critical effect.
The fexible film electrode of heat treated graphene oxide prepared by the preparation method of the fexible film electrode of the present invention and electrode active material hydridization can extensively for fields such as battery, electrochemical capacitance material and environmental protection automobiles.
Accompanying drawing explanation
Fig. 1 is the heat treated graphene oxide of the embodiment of the present invention 1 preparation and the scanning electron microscope (SEM) photograph of the fexible film electrode of electrode active material hydridization.
Embodiment
Doing to illustrate in detail to embodiments of the invention below in conjunction with accompanying drawing, the present embodiment is implemented under premised on technical solution of the present invention, gives detailed enforcement mode and concrete operating process, but protection domain of the present invention is not limited to following embodiment.
Embodiment 1:
It is graphene oxide water solution thermal treatment 30 days at 50 DEG C of 0.05mg/mL by 100mL concentration, obtains heat treated graphene oxide water solution; Electrode active material is dispersed in water simultaneously and forms the electrode active material dispersion liquid that concentration is 0.1mg/mL. It is that 9:1 mix with electrode active material dispersion liquid according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio by heat treated for gained graphene oxide water solution, it is made to form homogeneous mixture solotion through ultrasonic and magnetic agitation, utilize cellulose ester filtering membrane to, after this mixing solutions vacuum filtration, filter paper obtaining the fexible film electrode of heat treated graphene oxide and electrode active material hydridization. Heat treated for gained graphene oxide is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, it is dried at 40 DEG C, the fexible film electrode of the heat treated graphene oxide of gained and electrode active material hydridization is peeled off from filter paper.
As shown in Figure 1, the present embodiment obtains heat treated graphene oxide and the fexible film electrode of electrode active material hydridization have uniform laminate structure. In addition, the present embodiment obtains heat treated graphene oxide and the fexible film electrode of electrode active material hydridization also have excellent electroconductibility and good snappiness.
Embodiment 2:
It is graphene oxide water solution thermal treatment 15 days at 70 DEG C of 0.01mg/mL by 200mL concentration, obtains heat treated graphene oxide water solution; Electrode active material is dispersed in water simultaneously and forms the electrode active material dispersion liquid that concentration is 0.01mg/mL. It is that 5:5 mix with electrode active material dispersion liquid according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio by heat treated for gained graphene oxide water solution, it is made to form homogeneous mixture solotion through ultrasonic and magnetic agitation, utilize cellulose ester filtering membrane to, after this mixing solutions vacuum filtration, filter paper obtaining the fexible film electrode of heat treated graphene oxide and electrode active material hydridization. Heat treated for gained graphene oxide is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, it is dried at 20 DEG C, the fexible film electrode of the heat treated graphene oxide of gained and electrode active material hydridization is peeled off from filter paper.
Embodiment 3:
It is graphene oxide water solution thermal treatment 1 day at 90 DEG C of 0.1mg/mL by 50mL concentration, obtains heat treated graphene oxide water solution; Electrode active material is dispersed in water simultaneously and forms the electrode active material dispersion liquid that concentration is 1mg/mL. It is that 1:9 mix with electrode active material dispersion liquid according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio by heat treated for gained graphene oxide water solution, it is made to form homogeneous mixture solotion through ultrasonic and magnetic agitation, utilize cellulose ester filtering membrane to, after this mixing solutions vacuum filtration, filter paper obtaining the fexible film electrode of heat treated graphene oxide and electrode active material hydridization. Heat treated for gained graphene oxide is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, it is dried at 70 DEG C, the fexible film electrode of the heat treated graphene oxide of gained and electrode active material hydridization is peeled off from filter paper.
Embodiment 4:
Will: 100mL concentration is graphene oxide water solution thermal treatment 1 day at 90 DEG C of 0.05mg/mL, obtains heat treated graphene oxide water solution; Electrode active material is dispersed in water simultaneously and forms the electrode active material dispersion liquid that concentration is 10mg/mL. It is that 9:1 mix with electrode active material dispersion liquid according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio by heat treated for gained graphene oxide water solution, it is made to form homogeneous mixture solotion through ultrasonic and magnetic agitation, utilize cellulose ester filtering membrane to, after this mixing solutions vacuum filtration, filter paper obtaining the fexible film electrode of heat treated graphene oxide and electrode active material hydridization. Heat treated for gained graphene oxide is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, it is dried at 40 DEG C, the fexible film electrode of the heat treated graphene oxide of gained and electrode active material hydridization is peeled off from filter paper.
Below the preferred embodiment of the present invention is described in detail. It is to be understood that the ordinary skill of this area just can make many modifications and variations according to the design of the present invention without the need to creative work. Therefore, the technical scheme that all technician in the art can be obtained by logical analysis, reasoning, or a limited experiment under this invention's idea on the basis of existing technology, all should by the determined protection domain of claim book.
Claims (7)
1. the preparation method of a fexible film electrode, it is characterised in that, comprise the following steps:
(1) graphene oxide water solution is heat-treated, obtain heat treated graphene oxide water solution; Wherein, described heat treated condition is process 1��30 day at 50��90 DEG C;
(2) electrode active material is scattered in water and forms electrode active material dispersion liquid;
(3) described heat treated graphene oxide water solution and described electrode active material dispersion liquid are mixed to get mixing solutions, after being filtered by described mixing solutions, filter paper obtains the fexible film electrode of heat treated graphene oxide and electrode active material hydridization;
(4) the fexible film electrode of the described heat treated graphene oxide obtained in step (3) and electrode active material hydridization is dried, the temperature of described drying is 20��70 DEG C, and the fexible film electrode of described heat treated graphene oxide and electrode active material hydridization is peeled off from filter paper.
2. the preparation method of fexible film electrode as claimed in claim 1, it is characterised in that, described in step (1), the concentration of graphene oxide water solution is 0.01��0.1mg/mL.
3. the preparation method of fexible film electrode as claimed in claim 1, it is characterised in that, described in step (2), the concentration of electrode active material dispersion liquid is 0.01��10mg/mL.
4. the preparation method of fexible film electrode as claimed in claim 1, it is characterised in that, described in the described mixing solutions of step (3), the mass ratio of heat treated graphene oxide and described electrode active material is 9:1��1:9.
5. the preparation method of fexible film electrode as claimed in claim 1, it is characterised in that, filter paper described in step (3) is mixed cellulose ester filtering membrane, and aperture is 220nm.
6. the preparation method of fexible film electrode as claimed in claim 1, it is characterised in that, filtering, described in step (3), the device adopted is Vacuum filtration device.
7. the fexible film electrode of the heat treated graphene oxide prepared such as the preparation method of fexible film electrode as described in any one in claim 1��6 and electrode active material hydridization, it is characterized in that, the fexible film electrode of described heat treated graphene oxide and electrode active material hydridization has laminate structure.
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| CN106602012B (en) * | 2016-12-13 | 2020-05-26 | 上海交通大学 | Flexible thin film electrode and preparation method and application thereof |
| CN106847555A (en) * | 2017-02-24 | 2017-06-13 | 安徽桑瑞斯环保新材料有限公司 | A kind of method for preparing graphene-based superconduction electrode for capacitors |
| CN109870174A (en) * | 2019-03-08 | 2019-06-11 | 华南协同创新研究院 | A kind of flexible electrode and preparation method thereof |
| CN111613775A (en) * | 2020-05-20 | 2020-09-01 | 东莞东阳光科研发有限公司 | Electrode plate and preparation method and application thereof |
| CN112017869A (en) * | 2020-08-19 | 2020-12-01 | 五邑大学 | Self-supporting flexible composite film and preparation method thereof |
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| CN102683657A (en) * | 2012-05-11 | 2012-09-19 | 常州第六元素材料科技股份有限公司 | Graphene composite material for cathode of lithium ion battery and preparation method of graphene composite material |
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| CN103021663B (en) * | 2012-12-20 | 2016-08-03 | 同济大学 | The carbon nano-tube film solaode preparation method to electrode material |
| CN103265017B (en) * | 2013-05-17 | 2015-09-30 | 山西大学 | The preparation method of a kind of flexible self-supporting paper-like graphene film and composite membrane thereof |
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| CN102683657A (en) * | 2012-05-11 | 2012-09-19 | 常州第六元素材料科技股份有限公司 | Graphene composite material for cathode of lithium ion battery and preparation method of graphene composite material |
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| Strong and ductile poly(vinyl alcohol)/graphene oxide composite films with a layered structure;Yuxi Xu, et al;《CARBON》;20090815;第47卷;3538-3543 * |
| The effect of heat treatment on formation of graphene thin films from graphene oxide nanosheets;O.Akhavan;《CARBON》;20090929;第48卷;509-519 * |
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