CN108807006B - Preparation method of carbon-based flexible electrode - Google Patents
Preparation method of carbon-based flexible electrode Download PDFInfo
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- CN108807006B CN108807006B CN201810797128.3A CN201810797128A CN108807006B CN 108807006 B CN108807006 B CN 108807006B CN 201810797128 A CN201810797128 A CN 201810797128A CN 108807006 B CN108807006 B CN 108807006B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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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- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a preparation method of a carbon-based flexible electrode, which comprises the steps of taking a flexible carbon-based material as a working electrode, applying positive voltage in an electrolyte for electrochemical stripping, then applying negative voltage for electrochemical redeposition, and cleaning. The preparation process of the invention is carried out in the same aqueous solution system, and does not relate to the use of toxic and harmful chemicals; the preparation process is simple, safe, reliable, short in time and low in cost, and is suitable for large-scale green preparation; the initial carbon material not only provides a source for graphene preparation, but also can be used as a flexible substrate of the electrode, the prepared carbon-based electrode keeps the excellent mechanical property of the initial carbon material, and can also provide higher specific surface area and conductivity, and the three-dimensional structure of the electrode surface layer is easily regulated and controlled by adjusting the stripping-redeposition time and the electric field intensity; meanwhile, the collector material and the charge collector are integrated, so that the flexible all-solid-state energy storage device based on the carbon-based electrode material is simpler to manufacture and has excellent electrochemical performance.
Description
Technical Field
The invention belongs to the field of preparation of flexible electrodes, and particularly relates to a preparation method of a carbon-based flexible electrode.
Background
With the development of electronic products towards intellectualization, miniaturization and portability, the development of efficient flexible energy storage devices matched with the electronic products is urgently needed. The super capacitor has the characteristics of high power density, long cycle life, safety, no pollution, easy realization of flexibility and the like, and has attracted extensive attention in recent years. The graphene material has extremely high specific surface area, excellent electrochemical performance and good mechanical stability, and is widely used as an electrode material of a flexible all-solid-state supercapacitor. In the conventional planar supercapacitor, metal is generally required to be used as a charge collector, and an electrode is prepared by mixing an active material, a binder and a conductive additive and coating the mixture on the current collector. Although the powdered active material is loaded on the carbon-based material through simple hot pressing, coating, pasting and the like, the use of a non-conductive binder, the agglomeration of the active material, a relatively dense structure and the easy falling or pulverization of the electrode under the condition of folding or bending all cause the electrochemical performance of the final product to be poor, and the requirements of flexible electronic devices cannot be met.
Flexible carbon electrode materials such as carbon cloth have attracted much attention because of their relatively low cost, good electrical conductivity and high chemical stability. The storage mechanism of carbon materials is an electric double layer capacitance, and energy storage is achieved by ion adsorption and charge storage at the interface of an electrode and an electrolyte. However, the commercial carbon cloth or the commercial carbon felt which is not activated is chemically inert on the surface, and the pore channels cannot transmit electrolyte ions, so that the commercial carbon cloth or the commercial carbon felt often has a very small area specific capacitance (the commercial carbon cloth is only 1-2 millifarads per square centimeter), and cannot meet the requirements of practical application. Therefore, how to design and synthesize a carbon-based electrode material with a high active specific surface area and a through hierarchical pore structure, and effectively regulate and control functional groups on the surface of the carbon material and excellent performance is a key point of research. For example, Chinese patents [ CN 105869923A ] and [ CN 104201006B ] carry out surface treatment on carbon cloth in modes of high-temperature exercise, plasma chemical deposition and the like, but the treatment process needs inert gas protection and has high requirements on equipment; although the introduction of a large number of oxygen atoms improves the energy storage capacity of the carbon material, the final electrochemical performance of the carbon material is limited by the obviously reduced electrical conductivity of the carbon material. However, when the carbon material is made porous by etching such as acid treatment, the specific surface area is increased, but the originally excellent mechanical properties of the carbon material are deteriorated. More commonly, graphene, carbon nanotubes, activated carbon black and the like with high electrochemical activity are compounded on a two-dimensional flexible carbon-based material in a deposition, coating and other modes to form a three-dimensional structure so as to increase the specific surface area, and the two-dimensional flexible carbon-based material mainly plays a role in supporting and conducting a substrate. For example, chinese patent No. [ CN 1000358803C ] deposits carbon nanotubes on the surface of carbon cloth by vapor deposition to obtain carbon cloth electrodes coated with carbon nanotubes, which must be prepared at high temperature and in an inert gas environment, and has harsh conditions and high requirements for equipment; chinese patent No. CN 107628675A coats graphene oxide powder on the surface of carbon cloth by a coating method, and then reduces the graphene oxide powder to a conductive porous carbon cloth electrode by hydrazine hydrate, and the use of a strong reducing agent hydrazine hydrate brings new environmental hazards; according to the Chinese patent [ CN 104947134B ], graphene powder is deposited on the surface of carbon cloth by an electrochemical deposition method to obtain the carbon cloth electrode modified by porous graphene, and the graphene powder needs to be prepared independently, so that the effective electrochemical utilization area of the graphene is reduced due to the inevitable agglomeration phenomenon.
Graphene is the thinnest material known, and has the advantages of extremely high specific surface area, super-strong conductivity, strength and the like, and because the performance of the existing equipment can be improved and the next generation equipment is more practical, the graphene-based material is regarded as a high-performance electrode material with a deep prospect, and has a good market prospect. Graphene is generally prepared by stripping graphite oxide powder by a redox method or a physical stripping method, high-temperature expansion method and the like to prepare graphene oxide, and then reducing the graphene oxide by a chemical method to obtain graphene. The chemical method is simple to operate and high in yield, but the product quality is low, strong acids such as sulfuric acid and nitric acid are often used, so that the danger is high, and a large amount of water is required to be used for cleaning, so that the environmental pollution is high. In consideration of easy agglomeration of graphene, graphene oxide is usually reduced before use, and the graphene oxide contains abundant oxygen-containing functional groups and is easy to modify; the reduction can be carried out continuously under the influence of external media such as high temperature in a carriage during sunlight irradiation and transportation, the oxygen content of the reduced graphene is difficult to control, meanwhile, the quality of the batch-by-batch graphene products produced by the oxidation-reduction method is often inconsistent, the quality is difficult to control, and the reliability and the practical application of the supercapacitor are seriously influenced. Therefore, important attention and solution are needed to continuously prepare graphene macroscopic assemblies with uniform structures and stable and controllable properties. That is to say, various three-dimensional structures can be constructed by utilizing the two-dimensional layered structure, the problem of mutual stacking between graphene sheets is overcome, the effective electrochemical utilization area of the graphene-based electrode is increased, and the problem to be solved is urgently needed to find the huge potential of graphene in the application of future energy storage devices.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a carbon-based flexible electrode, and overcomes the defects of harsh preparation conditions, high equipment requirement, low conductivity, poor mechanical property, low effective electrochemical utilization area of graphene and the like in the prior art. The method has the advantages of simple process, easy operation, safe and reliable process, short preparation time and low cost, the preparation process is carried out in the same aqueous solution system, the use of toxic and harmful chemicals is not involved, and the method is suitable for large-scale green preparation; the initial carbon material not only provides a source for graphene preparation, but also can be used as a flexible substrate of the electrode, the prepared carbon-based electrode keeps the excellent mechanical property of the initial carbon material, and can also provide higher specific surface area and conductivity, and the three-dimensional structure of the electrode surface layer is easily regulated and controlled by adjusting the stripping-redeposition time and the electric field intensity; meanwhile, the collector material and the charge collector are integrated, so that the flexible all-solid-state energy storage device based on the carbon-based electrode material is simpler to manufacture and has more excellent electrochemical performance.
The invention discloses a preparation method of a carbon-based flexible electrode, which comprises the following steps:
and (3) taking the flexible carbon-based material as a working electrode, applying positive voltage in electrolyte for electrochemical stripping, then applying negative voltage for electrochemical redeposition, and cleaning to obtain the carbon-based flexible electrode with the fluffy structure.
The preferred mode of the above preparation method is as follows:
the flexible carbon material is carbon cloth or carbon felt.
The amount of the electrolyte is 5-50 ml per square centimeter of the carbon material.
The concentration of the electrolyte is 0.05-3 mol/L.
The electrolyte is sulfate aqueous solution.
The sulfate aqueous solution is one or more of lithium sulfate, sodium bisulfate, potassium sulfate, potassium bisulfate and ammonium sulfate aqueous solution.
The electrochemical stripping comprises the following steps: the applied voltage is 2-30V; the time of electrochemical stripping is 1-60 minutes.
The electrochemical redeposition: the applied voltage is-1 to-20 volts; the time for electrochemical redeposition is 1-60 minutes.
The carbon-based flexible electrode prepared by the method comprises the following steps: and meanwhile, the collector material and the charge collector are integrated.
The carbon-based flexible electrode has a fluffy porous structure.
The carbon-based flexible electrode disclosed by the invention is applied to flexible, portable and wearable electronic products, can also be applied to adsorption, capacitance deionization and other technologies, and is applied to the field of water treatment.
Advantageous effects
According to the invention, an initial carbon material is used as a source of graphene and is also used as a flexible substrate of an electrode, and a low-value carbon material is converted into an electrode material with high cost performance in an electrochemical stripping-redeposition mode; graphene oxide is directly electrically stripped from the carbon-based material, and then the carbon-based material is used as a flexible current collector to deposit and reduce the graphene oxide, so that the problem of storage denaturation or agglomeration in the conventional two-step method is solved;
the preparation process is carried out in the same aqueous solution system, toxic and harmful chemicals are not used, the problem of serious aggregation between common graphene sheets is effectively solved, and the effective usable area of the graphene electrode material is increased;
the method has the advantages of simple experimental device, simple process, easy operation, safe and reliable process, short time and low cost, and is suitable for large-scale green preparation;
the prepared carbon-based electrode keeps the excellent mechanical property of the initial carbon material, can also provide higher specific surface area and conductivity, the specific surface area is 100-600 square meters per gram, the conductivity is 200-400 Siemens per square centimeter, and the three-dimensional structure of the surface layer of the electrode is easy to regulate and control by adjusting the stripping-redeposition time and the electric field intensity;
the electrode material prepared by the invention has a fluffy porous structure, can greatly reduce excessive stacking among graphene sheets, and increases the utilization rate of the specific surface area; the flexible all-solid-state supercapacitor based on the carbon-based electrode material is simpler to manufacture and has excellent electrochemical performance, and the area capacitance value is 800-1500 millifarads/square centimeter;
the high-performance carbon-based flexible electrode prepared by the invention can be used as a carbon-based flexible electrode with simple preparation method, low cost and high performance, can be assembled into an all-solid-state energy storage device, and has great application value and potential in the fields of flexible, portable and wearable electronic products. In addition, the method can also be applied to adsorption, capacitance deionization and other technologies, and has wide application prospect in the field of water treatment.
Drawings
FIG. 1 is a schematic diagram of the electrochemical fabrication process of the high performance carbon-based flexible electrode of the present invention;
FIG. 2 is a transmission electron microscope image of the surface layer of the carbon cloth before treatment in example 1 of the present invention;
FIG. 3 is a transmission electron microscope image of the surface layer of the carbon cloth electrode after treatment in example 1 of the present invention;
FIG. 4 is a cyclic voltammogram of a carbon cloth electrode prepared in example 2 of the present invention in a 1 mol/L sulfuric acid solution;
FIG. 5 is a constant current charge and discharge curve of a carbon cloth electrode prepared in example 3 of the present invention in a 1 mol/L sulfuric acid solution;
FIG. 6 is a cyclic voltammogram of a carbon felt electrode assembled flexible solid-state supercapacitor prepared in example 4 of the present invention;
fig. 7 is a demonstration diagram of a flexible solid-state supercapacitor lighting LED lamp assembled with a carbon cloth electrode prepared in example 5 of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims. The carbon cloth is of a carbon energy W0S1002 type, and the carbon felt is of a carbon energy GF020 type, which are all from carbon energy (CeTech) science and technology, Inc.
Example 1
The high-performance carbon electrode is prepared by adopting electrochemical stripping-redeposition, and the flow diagram is shown in figure 1. The clean carbon cloth is used as a working electrode (the transmission electron microscope image of the clean carbon cloth is shown in figure 2, the surface layer structure is compact), and the platinum wire electrode is used as a counter electrode; selecting 0.5 mol/L sodium bisulfate solution as electrolyte, wherein the dosage of the electrolyte is 5 ml per square centimeter of carbon material; applying a voltage of 5V to carry out electrochemical stripping for 20 minutes, and then applying a voltage of-2V to carry out redeposition for 20 minutes; after the reaction is finished, the carbon cloth is washed by water to obtain an electrode material, the fluffy structure of the surface layer of the electrode material is shown in a transmission electron microscope picture in figure 3, the modulus of the original commercial carbon cloth is 0.15 MPa, the modulus of the treated carbon cloth is 0.15 MPa, and the excellent mechanical property of the initial carbon material is kept; the specific surface area of the commercial carbon cloth is 8 square meters per gram, the specific surface area of the treated carbon cloth is 247 square meters per gram, the thickness of the porous layer is 300 nanometers, and the specific surface area of the carbon cloth is greatly improved by the fluffy structure; the conductivity of the original carbon cloth is 208 Siemens/square centimeter, the conductivity of the treated carbon cloth is 278 Siemens/square centimeter, and the surface conductivity is higher; when the current density is 2 milliampere/square centimeter, the specific capacitance value is 1088 millifarads/square centimeter, and the area capacitance value is higher than that of the existing carbon cloth surface treatment technology (after the carbon cloth is treated by the existing technology, the area capacitance value is 400-750 millifarads/square centimeter).
Example 2
Using clean carbon cloth as a working electrode and a platinum sheet electrode as a counter electrode; selecting 1 mol/L ammonium sulfate solution as electrolyte, wherein the dosage of the electrolyte is 10 ml per square centimeter of carbon material; applying a voltage of 30V for electrochemical stripping for 1 minute, and then applying a voltage of-5V for redeposition for 15 minutes; after the reaction is finished, cleaning the carbon cloth with water to obtain a carbon cloth electrode material;
connecting the carbon cloth electrode serving as a working electrode to an electrochemical workstation, and performing cyclic voltammetry in a sulfuric acid solution of 1 mol/L by adopting a three-electrode system to obtain a cyclic voltammetry test curve of the carbon cloth electrode as shown in FIG. 4, wherein the modulus of the original commercial carbon cloth is 0.15 MPa, the modulus of the treated carbon cloth is 0.14 MPa, and the excellent mechanical properties of the initial carbon material are retained; the specific surface area of the commercial carbon cloth is 8 square meters per gram, the specific surface area of the treated carbon cloth is 225 square meters per gram, the thickness of the porous layer is 220 nanometers, and the specific surface area of the carbon cloth is greatly improved by the fluffy structure; the conductivity of the original carbon cloth is 208 siemens/square centimeter, the conductivity of the treated carbon cloth is 266 siemens/square centimeter, and the surface has higher conductivity; when the current density is 2 milliampere/square centimeter, the specific capacitance value is 1254 millifarads/square centimeter, and the area capacitance value is higher than that of the existing carbon cloth surface treatment technology.
Example 3
Using clean carbon cloth as a working electrode and a platinum wire electrode as a counter electrode; selecting 2 mol/L sodium sulfate solution as electrolyte, wherein the dosage of the electrolyte is 20 ml per square centimeter of carbon material; applying a voltage of 10V to carry out electrochemical stripping for 10 minutes, and then applying a voltage of-20V to carry out redeposition for 5 minutes; after the reaction is finished, cleaning the carbon cloth with water to obtain a carbon cloth electrode material;
connecting the electrode serving as a working electrode to an electrochemical workstation, and performing constant current charge and discharge test in a 1 mol/L sulfuric acid solution by adopting a three-electrode system to obtain a curve of the constant current charge and discharge test shown in figure 5, wherein when the current density is 2 milliampere/square centimeter, the specific capacitance value is 1134 millifarads/square centimeter, and the area capacitance value is higher than that of the existing carbon cloth surface treatment technology; the modulus of the original commercial carbon cloth is 0.15 MPa, the modulus of the treated carbon cloth is 0.15 MPa, and the excellent mechanical property of the initial carbon material is kept; the specific surface area of the commercial carbon cloth is 8 square meters per gram, the specific surface area of the treated carbon cloth is 238 square meters per gram, the thickness of the porous layer is 260 nanometers, and the specific surface area of the carbon cloth is greatly improved by the fluffy structure; the conductivity of the original carbon cloth is 208 Siemens/square centimeter, the conductivity of the treated carbon cloth is 293 Siemens/square centimeter, and the surface conductivity is higher.
Example 4
The clean carbon felt is used as a working electrode, and a platinum sheet electrode is used as a counter electrode; selecting 3 mol/L potassium sulfate solution as electrolyte, wherein the using amount of the electrolyte is 30 ml per square centimeter of carbon material; applying 2V voltage to carry out electrochemical stripping for 60 minutes, and then applying-10V voltage to carry out redeposition for 15 minutes; after the reaction is finished, cleaning the carbon felt with water to obtain a carbon felt electrode material, wherein the modulus of the original commercial carbon felt is 0.18 MPa, the modulus of the treated carbon felt is 0.18 MPa, and the excellent mechanical property of the initial carbon material is kept; the specific surface area of the commercial carbon felt is 18 square meters per gram, the specific surface area of the treated carbon felt is 571 square meters per gram, the thickness of the porous layer is 250 nanometers, and the specific surface area of the carbon felt is greatly improved by the fluffy structure; the conductivity of the original carbon felt is 224 siemens per square centimeter, the conductivity of the treated carbon felt is 325 siemens per square centimeter, and the surface conductivity is higher; when the current density is 2 milliampere/square centimeter, the specific capacitance value is 1458 millifaradays/square centimeter, and the area capacitance value is higher than that of the existing carbon cloth surface treatment technology;
preparing a solid electrolyte solution by using water/sulfuric acid/polyvinyl alcohol in a mass ratio of 10:1:1, assembling carbon felt electrodes into a symmetrical solid super capacitor, connecting the solid super capacitor to an electrochemical workstation to perform cyclic voltammetry to obtain cyclic voltammetry curves under different bending angles shown in figure 6, wherein the cyclic voltammetry curves show excellent mechanical properties.
Example 5
Using clean carbon cloth as a working electrode of an electrolytic system, and using a platinum sheet electrode as a counter electrode; selecting 0.1 mol/L lithium sulfate solution as electrolyte, wherein the dosage of the electrolyte is 50 ml per square centimeter of carbon material; applying a voltage of 5V for electrochemical stripping for 10 minutes, and then applying a voltage of-1V for redeposition for 60 minutes; after the reaction is finished, the carbon cloth is cleaned by water to obtain the carbon cloth electrode material, the modulus of the original commercial carbon cloth is 0.15 MPa, the modulus of the treated carbon cloth is 0.15 MPa, and the excellent mechanical property of the initial carbon material is kept; the specific surface area of the commercial carbon cloth is 8 square meters per gram, the specific surface area of the treated carbon cloth is 305 square meters per gram, the thickness of the porous layer is 380 nanometers, and the specific surface area of the carbon cloth is greatly improved by the fluffy structure; the conductivity of the original carbon cloth is 208 Siemens/square centimeter, the conductivity of the treated carbon cloth is 287 Siemens/square centimeter, and the surface has higher conductivity; when the current density is 2 milliampere/square centimeter, the specific capacitance value is 1333 millifarads/square centimeter, and the area capacitance value is higher than that of the existing carbon cloth surface treatment technology.
Preparing a solid electrolyte solution by using water/sulfuric acid/polyvinyl alcohol in a mass ratio of 10:1:1, and assembling the carbon cloth electrodes into a symmetrical solid super capacitor. Fig. 7 is a demonstration diagram of lighting the LED lamp after the flexible solid-state supercapacitor is charged, and the flexible solid-state supercapacitor can continuously light the LED lamp for 5 minutes, and shows excellent energy storage capacity.
Claims (7)
1. A preparation method of a carbon-based flexible electrode comprises the following steps:
the method comprises the following steps of (1) taking a flexible carbon-based material as a working electrode, applying positive voltage in electrolyte for electrochemical stripping, then applying negative voltage for electrochemical redeposition, and cleaning to obtain a carbon-based flexible electrode; wherein the electrolyte is sulfate aqueous solution; electrochemical stripping: the applied voltage is 2-30V, and the electrochemical stripping time is 1-60 minutes; electrochemical redeposition: the applied voltage is-1 to-20 volts, and the time of electrochemical redeposition is 1 to 60 minutes; wherein the applied voltages are all constant voltages.
2. The production method according to claim 1, wherein the flexible carbon material is a carbon cloth or a carbon felt.
3. The method according to claim 1, wherein the amount of the electrolyte is 5 to 50 ml per square centimeter of the carbon material.
4. The method according to claim 1, wherein the electrolyte concentration is 0.05 to 3 mol/l.
5. The preparation method according to claim 1, wherein the sulfate aqueous solution is one or more of lithium sulfate, sodium bisulfate, potassium sulfate, potassium bisulfate and ammonium sulfate aqueous solution.
6. A carbon-based flexible electrode prepared by the method of claim 1.
7. Use of a carbon-based flexible electrode prepared by the method of claim 1.
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