CN103972465A - Preparation method of flexible thin-film electrode - Google Patents
Preparation method of flexible thin-film electrode Download PDFInfo
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- CN103972465A CN103972465A CN201410217653.5A CN201410217653A CN103972465A CN 103972465 A CN103972465 A CN 103972465A CN 201410217653 A CN201410217653 A CN 201410217653A CN 103972465 A CN103972465 A CN 103972465A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000010409 thin film Substances 0.000 title abstract 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 73
- 239000007772 electrode material Substances 0.000 claims abstract description 69
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 52
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 239000006185 dispersion Substances 0.000 claims abstract description 21
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 229910002804 graphite Inorganic materials 0.000 claims description 21
- 239000010439 graphite Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 18
- 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 17
- 239000000463 material Substances 0.000 abstract description 3
- 239000000243 solution Substances 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 abstract 1
- 238000013019 agitation Methods 0.000 description 4
- 229910052799 carbon Inorganic materials 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000008240 homogeneous mixture Substances 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 238000005253 cladding Methods 0.000 description 3
- 238000004146 energy storage Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003575 carbonaceous material 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
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002474 experimental method Methods 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
- 229920000642 polymer Polymers 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
Classifications
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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
-
- 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
-
- 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 & Material Sciences (AREA)
- Power Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- General Chemical & Material Sciences (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Carbon And Carbon Compounds (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention discloses a preparation method of a flexible thin-film electrode. The method takes thermally-treated graphene oxide as conductive support and mechanical support and obtains the flexible thin-film electrode at one step through a vacuum filtration process. The method comprises the following steps: thermally treating graphene oxide aqueous solution to obtain thermally-treated graphene oxide aqueous solution; dispersing electrode active materials in water to form an electrode active material dispersion solution; mixing the thermally-treated graphene oxide aqueous solution with the electrode active material dispersion solution to obtain a mixed solution, filtering and drying, then obtaining the flexible thin-film electrode hybridized by the thermally-treated graphene oxide and the electrode active materials. The method is simple to operate and low in cost. The flexible thin-film electrode prepared by the method and hybridized by the thermally-treated graphene oxide and the electrode active materials has uniform layer structures, is excellent in conductivity and good in flexibility and can be widely used in the fields of batteries, super capacitance materials and green and environmentally friendly vehicles.
Description
Technical field
The present invention relates to a kind of fexible film electrode, relate in particular 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, developing flexible energy storage device has become the study hotspot in energy storage field.Wherein, electrode material is as the core component of energy storage device, thereby becomes the research emphasis of researcher and be subject to paying close attention to widely.At present, the preparation method of fexible film electrode mainly contains vacuum filtration process, cladding process, in situ synthesis.Cladding process and in situ synthesis be because collector has occupied larger volume and quality in electrode, thereby reduced significantly energy density and the power density of overall electrode.And vacuum filtration process is because its prepared film is an independent film, collector is comprised in electrode interior, thereby greatly reduce the ratio of collector shared dead volume in electrode, simultaneously because its special layer structure is in electrochemical reaction, take full advantage of electrode active material, therefore improved significantly energy density and the power density of overall electrode.
Graphene is as the mono-layer graphite of sp2 hydridization Carbon Materials primitive structure, there is excellent conductivity and higher pliability, therefore be widely used as conductive supporting and the mechanical support of flexible electrode material, by vacuum filtration itself and electrode active material, obtain high performance fexible film electrode.But in actual applications, Graphene is because its hydrophobicity is usually tended to irreversible reunion or stacking, thereby loses original excellent properties.Although Graphene can be by strengthening its dispersion stabilization at other molecules of its surface graft or polymer, but can cause Graphene to there is poor conductivity, also increased the dead volume of electrode material, so its chemical property is limited by very large in the middle of practical application simultaneously.
Current research finds, heat treated graphene oxide in the situation that not adding any dispersant, can be in the aqueous solution stable existence, kept its excellent conductivity simultaneously and be similar to other performances of Graphene.In addition, not only preparation condition is gentle for heat treated graphene oxide, process is simple, and can the preparation of large scale with high yield ground.But utilize heat treated graphene oxide not to be in the news 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 a kind of method of utilizing heat treated graphene oxide to prepare high-performance flexible membrane electrode as conductive supporting and the mechanical support of flexible electrode material.
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, the hydridization fexible film electrode that obtains heat treated graphene oxide and electrode active material by vacuum filtration process one step, specifically comprises the following steps:
(1) graphite oxide aqueous solution is heat-treated, obtain heat treated graphite oxide aqueous solution;
(2) electrode active material is scattered in and in water, forms electrode active material dispersion liquid;
(3) described heat treated graphite oxide aqueous solution and described electrode active material dispersion liquid are mixed to get to mixed solution, after described mixed solution is filtered, on filter paper, obtain 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 obtaining 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 graphite oxide aqueous solution is 0.01～0.1mg/mL.
Further, heat treated condition described in step (1) is at 50～90 ℃, to process 1～30 day.
Further, described in step (2), the concentration of electrode active material dispersion liquid is 0.01～10mg/mL.
Further, described in the described mixed solution of step (3), the mass ratio of heat treated graphene oxide and described electrode active material is 9:1～1:9.
Further, described in step (3), filter paper is mixed cellulose ester filter membrane, and aperture is 220nm.
Further, described in step (3), filtering the device adopting is vacuum filtration device.
Further, described in step (4), dry temperature is 20～70 ℃.
Further, the fexible film electrode of described heat treated graphene oxide and electrode active material hydridization has layer structure.
The preparation method of fexible film electrode of the present invention has feature simple to operate, with low cost, and its beneficial effect is:
(1) adopt vacuum filtration process, technique is simple, and prepared heat treated graphene oxide is more even than cladding process and in-situ method growth with the fexible film electrode of electrode active material hydridization;
(2) the fexible film electrode of prepared heat treated graphene oxide and electrode active material hydridization, not only there is high electrode active material heap(ed) capacity, there is excellent electric conductivity and high mechanical flexibility simultaneously, thereby increased significantly energy density and the power density of overall electrode, and kept the good pliability of this membrane electrode;
(3) the fexible film electrode of prepared heat treated graphene oxide and electrode active material hydridization, owing to having special layer structure, promotes its electrochemical reaction effectively, and the lifting of its chemical property is played to critical effect.
Heat treated graphene oxide prepared by the preparation method of fexible film electrode of the present invention and the fexible film electrode of electrode active material hydridization can be widely used in the fields such as battery, electrochemical capacitance material and environmental protection automobile.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph of the embodiment of the present invention 1 heat treated graphene oxide of preparation and the fexible film electrode of electrode active material hydridization.
Embodiment
Below in conjunction with accompanying drawing, embodiments of the invention are elaborated, the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed execution mode and concrete operating process, but protection range of the present invention is not limited to following embodiment.
Embodiment 1:
The graphite oxide aqueous solution that is 0.05mg/mL by 100mL concentration heat treatment 30 days at 50 ℃, obtains heat treated graphite oxide aqueous solution; Electrode active material is dispersed in simultaneously and in water, forms the electrode active material dispersion liquid that concentration is 0.1mg/mL.By the heat treated graphite oxide aqueous solution of gained, according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio, be that 9:1 mixes with electrode active material dispersion liquid, through ultrasonic and magnetic agitation, make it form homogeneous mixture solotion, after utilizing cellulose esters filter membrane to this mixed solution vacuum filtration, on filter paper, obtain the fexible film electrode of heat treated graphene oxide and electrode active material hydridization.The heat treated graphene oxide of gained is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, at 40 ℃, be dried, 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 heat treated graphene oxide that the present embodiment obtains and the fexible film electrode of electrode active material hydridization have uniform layer structure.In addition, the heat treated graphene oxide that the present embodiment obtains and the fexible film electrode of electrode active material hydridization also have excellent conductivity and good pliability.
Embodiment 2:
The graphite oxide aqueous solution that is 0.01mg/mL by 200mL concentration heat treatment 15 days at 70 ℃, obtains heat treated graphite oxide aqueous solution; Electrode active material is dispersed in simultaneously and in water, forms the electrode active material dispersion liquid that concentration is 0.01mg/mL.By the heat treated graphite oxide aqueous solution of gained, according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio, be that 5:5 mixes with electrode active material dispersion liquid, through ultrasonic and magnetic agitation, make it form homogeneous mixture solotion, after utilizing cellulose esters filter membrane to this mixed solution vacuum filtration, on filter paper, obtain the fexible film electrode of heat treated graphene oxide and electrode active material hydridization.The heat treated graphene oxide of gained is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, at 20 ℃, be dried, 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:
The graphite oxide aqueous solution that is 0.1mg/mL by 50mL concentration heat treatment 1 day at 90 ℃, obtains heat treated graphite oxide aqueous solution; Electrode active material is dispersed in simultaneously and in water, forms the electrode active material dispersion liquid that concentration is 1mg/mL.By the heat treated graphite oxide aqueous solution of gained, according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio, be that 1:9 mixes with electrode active material dispersion liquid, through ultrasonic and magnetic agitation, make it form homogeneous mixture solotion, after utilizing cellulose esters filter membrane to this mixed solution vacuum filtration, on filter paper, obtain the fexible film electrode of heat treated graphene oxide and electrode active material hydridization.The heat treated graphene oxide of gained is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, at 70 ℃, be dried, 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: the graphite oxide aqueous solution that 100mL concentration is 0.05mg/mL heat treatment 1 day at 90 ℃, obtains heat treated graphite oxide aqueous solution; Electrode active material is dispersed in simultaneously and in water, forms the electrode active material dispersion liquid that concentration is 10mg/mL.By the heat treated graphite oxide aqueous solution of gained, according to heat treated graphene oxide and electrode active material dispersion liquid mass ratio, be that 9:1 mixes with electrode active material dispersion liquid, through ultrasonic and magnetic agitation, make it form homogeneous mixture solotion, after utilizing cellulose esters filter membrane to this mixed solution vacuum filtration, on filter paper, obtain the fexible film electrode of heat treated graphene oxide and electrode active material hydridization.The heat treated graphene oxide of gained is inserted in baking oven with the fexible film electrode of electrode active material hydridization together with filter paper, at 40 ℃, be dried, the fexible film electrode of the heat treated graphene oxide of gained and electrode active material hydridization is peeled off from filter paper.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area just can design according to the present invention be made many modifications and variations without creative work.Therefore, all technical staff in the art, all should be in the determined protection range by claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (9)
1. a preparation method for fexible film electrode, is characterized in that, comprises the following steps:
(1) graphite oxide aqueous solution is heat-treated, obtain heat treated graphite oxide aqueous solution;
(2) electrode active material is scattered in and in water, forms electrode active material dispersion liquid;
(3) described heat treated graphite oxide aqueous solution and described electrode active material dispersion liquid are mixed to get to mixed solution, after described mixed solution is filtered, on filter paper, obtain 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 obtaining 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.
2. the preparation method of fexible film electrode as claimed in claim 1, is characterized in that, described in step (1), the concentration of graphite oxide aqueous solution is 0.01～0.1mg/mL.
3. the preparation method of fexible film electrode as claimed in claim 1, is characterized in that, heat treated condition described in step (1) is at 50～90 ℃, to process 1～30 day.
4. the preparation method of fexible film electrode as claimed in claim 1, is characterized in that, described in step (2), the concentration of electrode active material dispersion liquid is 0.01～10mg/mL.
5. the preparation method of fexible film electrode as claimed in claim 1, is characterized in that, described in the described mixed solution of step (3), the mass ratio of heat treated graphene oxide and described electrode active material is 9:1～1:9.
6. the preparation method of fexible film electrode as claimed in claim 1, is characterized in that, described in step (3), filter paper is mixed cellulose ester filter membrane, and aperture is 220nm.
7. the preparation method of fexible film electrode as claimed in claim 1, is characterized in that, described in step (3), filtering the device adopting is vacuum filtration device.
8. the preparation method of fexible film electrode as claimed in claim 1, is characterized in that, described in step (4), dry temperature is 20～70 ℃.
9. the heat treated graphene oxide that prepared by the preparation method of the fexible film electrode as described in any one in claim 1～8 and the fexible film electrode of 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 layer structure.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106602012A (en) * | 2016-12-13 | 2017-04-26 | 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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| CN103021663A (en) * | 2012-12-20 | 2013-04-03 | 同济大学 | Novel method for preparing counter electrode material of carbon nanotube thin-film solar cell |
| CN103265017A (en) * | 2013-05-17 | 2013-08-28 | 山西大学 | Preparation method of flexible self-supported paper graphene membrane and composite membrane thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102683657B (en) * | 2012-05-11 | 2015-10-07 | 常州第六元素材料科技股份有限公司 | A kind of used as negative electrode of Li-ion battery graphene composite material and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103021663A (en) * | 2012-12-20 | 2013-04-03 | 同济大学 | Novel method for preparing counter electrode material of carbon nanotube thin-film solar cell |
| CN103265017A (en) * | 2013-05-17 | 2013-08-28 | 山西大学 | Preparation method of flexible self-supported paper graphene membrane and composite membrane thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106602012A (en) * | 2016-12-13 | 2017-04-26 | 上海交通大学 | Flexible thin-film electrode and preparation method and application thereof |
| 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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