CN112614706A - Preparation of MnO by normal temperature two-electrode electrodeposition2Method of nanoarray and products thereof - Google Patents
Preparation of MnO by normal temperature two-electrode electrodeposition2Method of nanoarray and products thereof Download PDFInfo
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- CN112614706A CN112614706A CN202011254608.9A CN202011254608A CN112614706A CN 112614706 A CN112614706 A CN 112614706A CN 202011254608 A CN202011254608 A CN 202011254608A CN 112614706 A CN112614706 A CN 112614706A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 claims abstract description 44
- 238000004070 electrodeposition Methods 0.000 claims abstract description 30
- 239000004917 carbon fiber Substances 0.000 claims abstract description 27
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 22
- 238000005868 electrolysis reaction Methods 0.000 claims abstract description 20
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims abstract description 14
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003792 electrolyte Substances 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims 1
- 238000004146 energy storage Methods 0.000 abstract description 4
- 238000003860 storage Methods 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 230000005611 electricity Effects 0.000 abstract description 2
- 239000011572 manganese Substances 0.000 description 21
- 239000000243 solution Substances 0.000 description 14
- 239000007772 electrode material Substances 0.000 description 10
- 238000000151 deposition Methods 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000003990 capacitor Substances 0.000 description 6
- 239000007787 solid Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 4
- 230000008021 deposition Effects 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011267 electrode slurry Substances 0.000 description 2
- 229910001437 manganese ion Inorganic materials 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 229910021380 Manganese Chloride Inorganic materials 0.000 description 1
- 238000003491 array Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000037427 ion transport Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000011565 manganese chloride Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000007709 nanocrystallization Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000004513 sizing Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
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Classifications
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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
-
- 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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
-
- 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
- H01G11/40—Fibres
-
- 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
- H01G11/46—Metal oxides
-
- 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 discloses a method for preparing MnO by normal temperature two-electrode electrodeposition2The preparation method of the nano array and the product thereof comprises the following steps: with Mn (NO)3)2The solution is used as electrolyte, carbon fiber is used as anode and cathode for electrolysis, and the cathode after the electrolysis is the cathode with MnO deposited on the surface2A nano-array of carbon fibers; the electrolysis is a two-electrode method, the voltage between the positive electrode and the negative electrode is 5-20V, and the electrolysis time is 10-100 min. Ultrathin lamellar MnO with embedded structure is densely distributed on surface of carbon fiber2. The preparation method disclosed by the invention is simple to operate, does not need a reference electrode, does not need complex equipment, is low in cost, and is harmless and pollution-free to the environment; product of ultra-thinStructure, carbon fiber surface densely distributed with ultrathin lamellar MnO2The battery has a large effective surface area, is beneficial to energy storage, has excellent electricity storage performance and has great application prospect.
Description
Technical Field
The invention belongs to the technical field of preparation of electrode materials of a super capacitor, and relates to preparation of MnO by normal-temperature two-electrode electrodeposition2A method of nanoarray and products thereof.
Background
The super capacitor is a novel energy storage device between a traditional capacitor and a rechargeable battery, and has the characteristics of quick charge and discharge of the capacitor and the energy storage characteristic of the battery. The super capacitor has the characteristics of high power density, long cycle life, wide working temperature limit, no maintenance and environmental protection, and is more and more widely applied in various fields.
For a supercapacitor, the electrode material thereof is one of the key factors affecting the performance and production cost of the supercapacitor. The metal oxide material becomes a common hot supercapacitor electrode material due to the characteristics of high specific heat capacity (high electrochemical capacitance behavior and excellent multiplying power and high energy density) and high stability (good cycle stability and long working life). Wherein, MnO2Is a metal oxide material which is more commonly used. Because of the defect of compact structure, the nano-treatment (MnO) is mostly carried out at present2Nanoarrays) to increase surface area, while nanocrystallization also facilitates ion transport.
The feeding process of the electrode material on the super capacitor is generally divided into two types: preparing electrode slurry and then sizing on a current collector; directly growing the electrode material on the surface of the current collector. Compared with the electrode slurry preparation process, the method has the advantages that the active area of the material can be fully utilized by directly growing the electrode material on the surface of the current collector, the generation of dead volume is reduced, and the capacitance advantage of the electrode material is fully exerted. The electrochemical deposition method is a preparation method which is simple in process and relatively universal and directly places electrode materials on a current collector, three-electrode deposition is generally adopted during deposition, a working electrode, a counter electrode and a reference electrode are required for deposition by the three-electrode deposition method, meanwhile, the electrodeposition temperature has the experimental condition that heating at a certain temperature is required to be successful, the process is relatively complex, and the cost is relatively high.
Therefore, a supercapacitor electrode material (MnO) with simple process and low cost is developed2Nano array) preparation method has practical significance.
Disclosure of Invention
The invention aims to overcome the defects of complex process and high cost in the prior art, and provides a supercapacitor electrode material (MnO) with simple process and low cost2Nano array), and the preparation method is harmless and pollution-free to the environment.
In order to achieve the purpose, the invention provides the following technical scheme:
preparation of MnO by normal temperature two-electrode electrodeposition2Method of nano-array with Mn (NO)3)2The solution is used as electrolyte, carbon fiber is used as anode and cathode for electrolysis, and the cathode after the electrolysis is the cathode with MnO deposited on the surface2A nano-array of carbon fibers;
the electrolysis is a two-electrode method, the voltage between the positive electrode and the negative electrode is 5-20V, and the electrolysis time is 10-100 min.
The invention selects Mn (NO) specially3)2The solution is used as electrolyte, and bivalent manganese ions in the electrolyte lose electrodes at a negative electrode and become positive quadrivalent manganese ions to form MnO2,MnO2Deposited on the surface of carbon fiber and only selected Mn (NO) of the present invention3)2MnO with solution capable of ensuring deposition2The cathode is in a nano array state (MnO for ensuring deposition)2The appearance of the substance) of the fiber, and meanwhile, the voltage and the time length of electrolysis are set within a certain range, products cannot be obtained when the voltage of electrolysis is too high or too low, the products fall off from the surface due to too compact growth when the electrolysis time is too long, and the products are too few when the electrolysis time is too short, so that the array can not be formed and coated on the surface of the fiber.
As a preferred technical scheme:
preparation of MnO by the normal-temperature two-electrode electrodeposition2Method of nanoarray, said Mn (NO)3)2The concentration of the solution is 0.01-0.1 mol/L.The scope of the present invention is not limited thereto, and only one possible solution is provided herein, and the adjustment of Mn (NO) within a certain range can be performed by one skilled in the art3)2Concentration of solution, but not too large adjustment range, Mn (NO)3)2The product is non-arrayed, Mn (NO) when the concentration of the solution is too high3)2The concentration of the solution is too low to generate products easily.
Preparation of MnO by the normal-temperature two-electrode electrodeposition2The method of the nano array comprises the step of carrying out electrolysis in an electrolytic bath, wherein the volume of electrolyte is 40-120 ml.
Preparation of MnO by the normal-temperature two-electrode electrodeposition2In the nano-array method, the negative electrode needs to be washed and dried. The washing is performed to remove the residual solution adhering to the surface, and the drying is performed for storage.
Preparation of MnO by the normal-temperature two-electrode electrodeposition2A method of nano array, wherein the washing solution used for washing is deionized water and absolute ethyl alcohol (specifically, deionized water and absolute ethyl alcohol are used for washing alternately); the washing time is 1-60 min.
Preparation of MnO by the normal-temperature two-electrode electrodeposition2And (3) drying the nano array at the temperature of 60-120 ℃ for 1-4 h.
The invention also provides MnO preparation by adopting the normal-temperature two-electrode electrodeposition2MnO is deposited on the surface of the nano-array prepared by the method2The carbon fiber of nano-array, carbon fiber surface intensive distribution has the ultrathin slice MnO that is mosaic structure2。
As a preferred technical scheme:
MnO being deposited on the surface as described above2Nano-arrayed carbon fiber, said ultra-thin sheet MnO2The thickness of (A) is 0.1 to 1 μm.
Has the advantages that:
(1) preparation of MnO by normal temperature two-electrode electrodeposition2The method of the nano array has simple operation, no need of reference electrode and complex equipment, low cost and ring alignmentThe environment is non-toxic and pollution-free;
(2) preparation of MnO by normal temperature two-electrode electrodeposition2The product prepared by the method of the nano array has an ultrathin structure, and ultrathin lamellar MnO is densely distributed on the surface of the carbon fiber2The surface area is large, which is beneficial to energy storage;
(3) preparation of MnO by normal temperature two-electrode electrodeposition2The product prepared by the nano-array method has excellent electricity storage performance and has great application prospect.
Drawings
FIG. 1 is a scanning electron microscope image of the product obtained by the method of the present invention.
Detailed Description
The following further describes the embodiments of the present invention with reference to the attached drawings.
Example 1
Preparation of MnO by normal temperature two-electrode electrodeposition2The method of the nano array comprises the following steps:
first, 12.5505 g of Mn (NO) were dissolved3)2·4H2Adding a certain amount of deionized water into the O solid, and mixing to obtain 500ml of 0.1mol/L Mn (NO)3)2An aqueous solution; then, 8ml of Mn (NO) was measured out3)2The aqueous solution was mixed with 72ml of deionized water and stirred to obtain 80ml of 0.01mol/L Mn (NO)3)2Pouring the solution into an electrolytic bath, electrolyzing by taking carbon fibers as positive and negative electrodes, and electrolyzing for 20min by applying 9V voltage (positive and negative voltage); then, washing the negative electrode for 60min by using deionized water and absolute ethyl alcohol alternately; finally drying at 100 ℃ for 4h to obtain the product with MnO deposited on the surface2A nano-array of carbon fibers.
The obtained surface is deposited with MnO2The scanning electron microscope picture of the carbon fiber of the nano array is shown in figure 1, and it can be seen from the figure that ultrathin lamellar MnO with an embedded structure is densely distributed on the surface of the carbon fiber2Ultra-thin sheet MnO2The thickness of (A) is 0.1 to 1 μm.
Comparative example 1
Electrodeposition MnO2The process of (1) is essentially the same as in example 1, except thatAfter mixing 12.5505 g of Mn (NO)3)2·4H2Replacement of O solids to 9.8950 g MnCl2·4H2And (4) O solid.
MnO is deposited on the surface of the product observed under a scanning electron microscope2The carbon fiber of (3) was found to have a flower-like morphology in which the product was independently dispersed.
Comparative example 2
Electrodeposition MnO2The procedure of (3) was substantially the same as in example 1, except that the voltage between the positive electrode and the negative electrode was 4V.
The prepared product is observed under a scanning electron microscope, and no product is formed on the surface of the fiber.
Comparative example 3
Electrodeposition MnO2The procedure of (3) was substantially the same as in example 1, except that the voltage between the positive electrode and the negative electrode was 21V.
The obtained product is observed under a scanning electron microscope, and no product is formed under high voltage.
By comprehensively analyzing example 1 and comparative examples 1 to 3, it can be found that only the specific electrolyte (Mn (NO) of the present application is selected3)2Solution) and a specific electrolytic voltage, a specific MnO can be obtained2Deposition morphology-MnO2And (4) nano arrays.
Example 2
Preparation of MnO by normal temperature two-electrode electrodeposition2The method of the nano array comprises the following steps:
first, 12.5505 g of Mn (NO) were dissolved3)2·4H2Adding a certain amount of deionized water into the O solid, and mixing to obtain 500ml of 0.1mol/L Mn (NO)3)2An aqueous solution; then 16ml Mn (NO) was measured3)2The aqueous solution was mixed with 64ml of deionized water and stirred to obtain 80ml of 0.02mol/L Mn (NO)3)2Pouring the solution into an electrolytic bath, electrolyzing by taking carbon fibers as positive and negative electrodes, and electrolyzing for 40min by applying 12V voltage (positive and negative voltage); then, washing the negative electrode for 10min by using deionized water and absolute ethyl alcohol alternately; finally drying for 2h at 80 ℃ to obtain the product with MnO deposited on the surface2A nano-array of carbon fibers.
Example 3
Preparation of MnO by normal temperature two-electrode electrodeposition2The method of the nano array comprises the following steps:
first, 12.5505 g of Mn (NO) were dissolved3)2·4H2Adding a certain amount of deionized water into the O solid, and mixing to obtain 500ml of 0.1mol/L Mn (NO)3)2An aqueous solution; then 8ml of Mn (NO) was measured3)2The aqueous solution was mixed with 64ml of deionized water in a box containing 8ml of DMSO and stirred to obtain 80ml of 0.01mol/L Mn (NO)3)2Pouring the solution into an electrolytic bath, electrolyzing by taking carbon fibers as positive and negative electrodes, and electrolyzing for 30min by applying 9V voltage (positive and negative voltage); then, washing the negative electrode for 1min by using deionized water and absolute ethyl alcohol alternately; finally drying at 100 ℃ for 4h to obtain the product with MnO deposited on the surface2A nano-array of carbon fibers.
Example 4
Preparation of MnO by normal temperature two-electrode electrodeposition2The process of the nano-array was substantially the same as in example 1 except that the voltage between the positive and negative electrodes was 5V and the electrolysis time was 100 min.
Example 5
Preparation of MnO by normal temperature two-electrode electrodeposition2The process of the nano-array was substantially the same as in example 1 except that the voltage between the positive and negative electrodes was 20V and the electrolysis time was 10 min.
MnO was deposited on the surfaces of the films prepared in examples 2 to 5 by observation under a scanning electron microscope2The nano-array carbon fiber was found to be substantially the same as that of FIG. 1, i.e., ultra-thin lamellar MnO of mosaic structure is densely distributed on the surface of the carbon fiber2Ultra-thin sheet MnO2The thickness of (A) is 0.1 to 1 μm.
Proved by verification, the invention prepares MnO by the normal temperature two-electrode electrodeposition2The method of the nano array has the advantages of simple operation, no need of a reference electrode, no need of complex equipment, low cost, no toxicity and no pollution to the environment and great application prospect.
Although specific embodiments of the present invention have been described above, it will be appreciated by those skilled in the art that these embodiments are merely illustrative and various changes or modifications may be made without departing from the principles and spirit of the invention.
Claims (8)
1. Preparation of MnO by normal temperature two-electrode electrodeposition2Method for nanoarray, characterized in that Mn (NO) is used3)2The solution is used as electrolyte, carbon fiber is used as anode and cathode for electrolysis, and the cathode after the electrolysis is the cathode with MnO deposited on the surface2A nano-array of carbon fibers;
the electrolysis is a two-electrode method, the voltage between the positive electrode and the negative electrode is 5-20V, and the electrolysis time is 10-100 min.
2. The method of claim 1 for preparing MnO by normal temperature two-electrode electrodeposition2Method of nanoarray, characterized in that said Mn (NO)3)2The concentration of the solution is 0.01-0.1 mol/L.
3. The method of claim 1 for preparing MnO by normal temperature two-electrode electrodeposition2The method for preparing the nano array is characterized in that the electrolysis is carried out in an electrolytic cell, and the volume of electrolyte is 40-120 ml.
4. The method of claim 1 for preparing MnO by normal temperature two-electrode electrodeposition2The method of nano-array is characterized in that the negative electrode is washed and dried.
5. The method of claim 4 for preparing MnO by normal temperature two-electrode electrodeposition2The method for nano array is characterized in that the washing liquid used for washing is deionized water and absolute ethyl alcohol; the washing time is 1-60 min.
6. The method of claim 4 for preparing MnO by normal temperature two-electrode electrodeposition2The method for preparing the nano array is characterized in that the drying is drying for 1-4 hours at the temperature of 60-120 ℃.
7. Preparation of MnO by the normal temperature two-electrode electrodeposition according to any one of claims 1 to 62MnO is deposited on the surface of the nano-array prepared by the method2The carbon fiber of the nano array is characterized in that ultrathin lamellar MnO with an embedded structure is densely distributed on the surface of the carbon fiber2。
8. The surface of claim 7 deposited with MnO2Nanoarrayed carbon fibers characterized in that said ultrathin lamellar MnO is2The thickness of (A) is 0.1 to 1 μm.
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Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101916667A (en) * | 2010-09-19 | 2010-12-15 | 西安交通大学 | Asymmetrical super capacitor based on composite material of MnO2 and PPy/F-CNTs |
US20120236467A1 (en) * | 2011-03-16 | 2012-09-20 | Vanderbilt University, Center For Technology Transfer And Commercialization | Ultracapacitor, methods of manufacturing and applications of the same |
CN103361698A (en) * | 2013-07-15 | 2013-10-23 | 清华大学深圳研究生院 | Method for preparing supercapacitor electrode material by means of coelectrodeposition |
CN108987123A (en) * | 2018-06-07 | 2018-12-11 | 武汉科技大学 | A kind of manganese dioxide-expanded graphite-cotton fiber tri compound electrochemical capacitance electrode material and preparation method thereof |
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2020
- 2020-11-11 CN CN202011254608.9A patent/CN112614706A/en active Pending
Patent Citations (4)
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CN101916667A (en) * | 2010-09-19 | 2010-12-15 | 西安交通大学 | Asymmetrical super capacitor based on composite material of MnO2 and PPy/F-CNTs |
US20120236467A1 (en) * | 2011-03-16 | 2012-09-20 | Vanderbilt University, Center For Technology Transfer And Commercialization | Ultracapacitor, methods of manufacturing and applications of the same |
CN103361698A (en) * | 2013-07-15 | 2013-10-23 | 清华大学深圳研究生院 | Method for preparing supercapacitor electrode material by means of coelectrodeposition |
CN108987123A (en) * | 2018-06-07 | 2018-12-11 | 武汉科技大学 | A kind of manganese dioxide-expanded graphite-cotton fiber tri compound electrochemical capacitance electrode material and preparation method thereof |
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MANAB KUNDU: "Direct growth of mesoporous MnO2 nanosheet arrays on nickel foam current collectors for high-performance pseudocapacitors", 《JOURNAL OF POWER SOURCES》 * |
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