CN110428983B - Pre-sodium treatment method for MXene electrode material of sodium ion capacitor - Google Patents
Pre-sodium treatment method for MXene electrode material of sodium ion capacitor Download PDFInfo
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- CN110428983B CN110428983B CN201910777406.3A CN201910777406A CN110428983B CN 110428983 B CN110428983 B CN 110428983B CN 201910777406 A CN201910777406 A CN 201910777406A CN 110428983 B CN110428983 B CN 110428983B
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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
- H01G11/04—Hybrid capacitors
- H01G11/06—Hybrid capacitors with one of the electrodes allowing ions to be reversibly doped thereinto, e.g. lithium ion capacitors [LIC]
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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
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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
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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 pre-sodium treatment method for MXene electrode material of a sodium ion capacitor, which mainly comprises the following preparation steps: under the protection of inert atmosphere, uniformly mixing multiple layers of MXene powder, a conductive additive and a binder according to the mass ratio of 8:1:1, and adding an N-methylpyrrolidone solution to prepare slurry; heating and melting a metal sodium block into a metal sodium melt; and (3) sequentially and alternately spraying the electrode slurry and the metal sodium molten liquid on the copper foil by using a spray gun, drying, peeling the copper foil, compacting, cutting the pieces, and assembling the button capacitor to obtain the pre-sodium MXene electrode material for the sodium ion capacitor.
Description
Technical Field
The invention relates to a pre-sodium treatment technology of an MXene electrode material of a sodium ion capacitor.
Background
The sodium ion capacitor is a novel hybrid capacitor formed by combining a battery type electrode and a capacitance type electrode, and has the advantages of high energy density of a secondary battery, high power density of a traditional capacitor, excellent cycle stability and the like. MXene can provide a rapid migration channel for electrolyte ions due to a unique two-dimensional layered structure, and becomes a sodium ion capacitor battery type electrode material with great development prospect. However, the method for pre-embedding sodium in a battery type electrode in a sodium ion capacitor mainly comprises the steps of increasing the concentration of a sodium ion organic electrolyte, pre-embedding sodium in electrochemistry and the like, and the problems of insufficient pre-sodium degree, poor controllability of the pre-sodium quantity of an electrode material, complicated pre-sodium step, over-quick sodium source consumption of a sodium ion capacitor device and the like exist, so that the method becomes a bottleneck factor for limiting the development of the sodium ion capacitor. Therefore, the present invention proposes to solve this problem by using a method of spraying pre-intercalated sodium. The invention provides a method for pre-sodium treatment by directly spraying metal sodium molten liquid as a sodium source to be added into a sodium ion capacitor and providing enough sodium ions by a way of self-contact sodium embedding of MXene and metal sodium. Compared with the traditional pre-sodium treatment mode, the method effectively solves the problems of poor controllability of the pre-sodium quantity in the traditional pre-sodium treatment process and repeated disassembly and assembly of devices, has good controllability and easy operability, can directly and sufficiently provide the quantity of sodium ions of the pre-embedded MXene electrode, can accurately control the number of layers and the thickness of alternate intercalation distribution, simultaneously reduces the use cost of the sodium ion capacitor, and is an important innovation and supplement for the existing pre-sodium treatment technology.
Disclosure of Invention
The invention aims to provide a pre-sodium treatment method of an MXene electrode material of a sodium ion capacitor.
The invention relates to a pre-sodium treatment method for MXene electrode material of a sodium ion capacitor, which comprises the following steps: under the protection of inert atmosphere, uniformly mixing multiple layers of MXene powder, a conductive additive and a binder according to the mass ratio of 8:1:1, and adding an N-methylpyrrolidone solution to prepare electrode slurry; heating and melting a metal sodium block to form metal sodium molten liquid; the method comprises the following steps of sequentially and alternately spraying electrode slurry and metal sodium molten liquid on a copper foil by using a spray gun, peeling the copper foil after drying, compacting, cutting into pieces, and assembling a button capacitor to obtain the pre-sodium MXene electrode material for the sodium ion capacitor, wherein the method comprises the following specific operation steps:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of a metal sodium block at 100 ℃ to form a metal sodium molten solution;
(3) and (3) sequentially and alternately spraying the electrode slurry obtained in the step (1) and the electrode slurry obtained in the step (2) and the metal sodium molten liquid on the copper foil by using a German schutze KA-2 automatic spray gun, wherein the pressure of the spray gun is 0.8-1.5Bar, and the size of a spray nozzle is 0.2mm and 0.3 mm. Drying at 80 ℃ for 24h, peeling off the copper foil, compacting and cutting into pieces to obtain the MXene electrode material for the sodium ion capacitor;
(4) and (4) assembling the button sodium ion capacitor by taking the activated carbon and the MXene electrode slice obtained in the step (3) as the anode and the cathode of the sodium ion capacitor respectively, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
Detailed description of the invention
Example 1:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of metal sodium block at 100 ℃ to form metal sodium molten liquid;
(3) using a German schutze KA-2 automatic spray gun, wherein the caliber of the spray nozzle is 0.2mm, adjusting the atomization pressure to be 0.8bar, sequentially spraying the electrode slurry obtained in the step (1) and the step (2) and the metal sodium molten liquid on a copper foil by using the spray gun, drying for 24 hours at the temperature of 80 ℃, stripping and compacting the copper foil, and cutting pieces to obtain the pre-sodiumized MXene electrode material for the sodium ion capacitor;
(4) and (4) assembling the button sodium ion capacitor by taking the activated carbon and the MXene electrode slice obtained in the step (3) as the anode and the cathode of the sodium ion capacitor respectively, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
Example 2:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of metal sodium block at 100 ℃ to form metal sodium molten liquid;
(3) using a German schutze KA-2 automatic spray gun, wherein the caliber of the spray nozzle is 0.2mm, adjusting the atomization pressure to 1.15bar, sequentially spraying the electrode slurry obtained in the step (1) and the step (2) and the metal sodium molten liquid on a copper foil by using the spray gun, drying for 24 hours at the temperature of 80 ℃, stripping and compacting the copper foil, and cutting pieces to obtain the pre-sodiumized MXene electrode material for the sodium ion capacitor;
(4) and (4) assembling the button sodium ion capacitor by taking the activated carbon and the MXene electrode slice obtained in the step (3) as the anode and the cathode of the sodium ion capacitor respectively, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
Example 3:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of metal sodium block at 100 ℃ to form metal sodium molten liquid;
(3) using a German schutze KA-2 automatic spray gun, wherein the caliber of the spray nozzle is 0.2mm, adjusting the atomization pressure to 1.5bar, sequentially spraying the electrode slurry obtained in the step (1) and the step (2) and the metal sodium molten liquid on a copper foil by using the spray gun, drying for 24 hours at the temperature of 80 ℃, stripping and compacting the copper foil, and cutting pieces to obtain the pre-sodiumized MXene electrode material for the sodium ion capacitor;
(4) and (4) assembling the button sodium ion capacitor by taking the activated carbon and the MXene electrode slice obtained in the step (3) as the anode and the cathode of the sodium ion capacitor respectively, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
Example 4:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of metal sodium block at 100 ℃ to form metal sodium molten liquid;
(3) using a German schutze KA-2 automatic spray gun, wherein the caliber of the spray nozzle is 0.3mm, adjusting the atomization pressure to be 0.8bar, sequentially spraying the electrode slurry obtained in the step (1) and the step (2) and the metal sodium molten liquid on a copper foil by using the spray gun, drying for 24 hours at the temperature of 80 ℃, stripping and compacting the copper foil, and cutting pieces to obtain the pre-sodiumized MXene electrode material for the sodium ion capacitor;
(4) and (4) assembling the button sodium ion capacitor by taking the activated carbon and the MXene electrode slice obtained in the step (3) as the anode and the cathode of the sodium ion capacitor respectively, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
Example 5:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of metal sodium block at 100 ℃ to form metal sodium molten liquid;
(3) using a German schutze KA-2 automatic spray gun, wherein the caliber of the spray nozzle is 0.3mm, adjusting the atomization pressure to be 1.15bar, sequentially spraying the electrode slurry obtained in the step (1) and the step (2) and the metal sodium molten liquid on a copper foil by using the spray gun, drying for 24 hours at the temperature of 80 ℃, stripping and compacting the copper foil, and cutting pieces to obtain the pre-sodiumized MXene electrode material for the sodium ion capacitor;
(4) and (4) assembling the button sodium ion capacitor by taking the activated carbon and the MXene electrode slice obtained in the step (3) as the anode and the cathode of the sodium ion capacitor respectively, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
Example 6:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of metal sodium block at 100 ℃ to form metal sodium molten liquid;
(3) using a German schutze KA-2 automatic spray gun, wherein the caliber of the spray nozzle is 0.3mm, adjusting the atomization pressure to be 1.5bar, sequentially spraying the electrode slurry obtained in the step (1) and the step (2) and the metal sodium molten liquid on a copper foil by using the spray gun, drying for 24 hours at the temperature of 80 ℃, stripping and compacting the copper foil, and cutting pieces to obtain the pre-sodiumized MXene electrode material for the sodium ion capacitor;
(4) and (4) assembling the button sodium ion capacitor by taking the activated carbon and the MXene electrode slice obtained in the step (3) as the anode and the cathode of the sodium ion capacitor respectively, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
The above description is an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications that can be made by using the equivalent structures or equivalent processes of the present invention as described in the specification of the present invention or applied to other related fields directly or indirectly are intended to be encompassed by the present invention.
Claims (7)
1. A pre-sodium treatment method for MXene electrode material of sodium ion capacitor comprises the following steps: under the protection of inert atmosphere, uniformly mixing multiple layers of MXene powder, a conductive additive and a binder according to the mass ratio of 8:1:1, and adding an N-methylpyrrolidone solution to prepare electrode slurry; heating and melting a metal sodium block to form metal sodium molten liquid; the method comprises the following steps of sequentially and alternately spraying electrode slurry and metal sodium molten liquid on a copper foil by using a spray gun, peeling the copper foil after drying, compacting, cutting into pieces, and assembling a button capacitor to obtain a pre-sodium MXene electrode material for a sodium ion capacitor, wherein the method comprises the following specific operation steps:
(1) mixing 80mg of MXene powder, 10mg of conductive additive and 10mg of binder in an inert atmosphere operation box, and adding N-methylpyrrolidone solution to prepare electrode slurry;
(2) heating 1g of metal sodium block at 100 ℃ to form metal sodium molten liquid;
(3) sequentially and alternately spraying the electrode slurry obtained in the step (1) and the electrode slurry obtained in the step (2) and a metal sodium molten liquid on a copper foil by using a German schutze KA-2 automatic spray gun, wherein the pressure of the spray gun is 0.8-1.5Bar, the size of a spray nozzle is 0.2mm and 0.3mm, drying for 24 hours at the temperature of 80 ℃, stripping the copper foil, compacting and cutting pieces to obtain the MXene electrode material for the sodium ion capacitor;
(4) and (4) respectively taking the activated carbon and the MXene electrode material obtained in the step (3) as the anode and the cathode of the sodium ion capacitor, assembling the button sodium ion capacitor, and standing for 24 hours in a self-contact sodium pre-intercalation mode to obtain the sodium ion capacitor completed by sodium pre-intercalation.
2. The pre-sodium treatment method for the MXene electrode material of the sodium ion capacitor as claimed in claim 1, wherein: the MXene is Ti3C2Tx，Ti2CTx，V2CTx，Mo3C2TxOr one or more of them.
3. The pre-sodium treatment method for the MXene electrode material of the sodium ion capacitor as claimed in claim 1, wherein: the conductive additive is one or more of acetylene black, Ketjen black, Super P or the like.
4. The pre-sodium treatment method for the MXene electrode material of the sodium ion capacitor as claimed in claim 1, wherein: the binder is one or two of polytetrafluoroethylene and sodium carboxymethylcellulose.
5. The pre-sodium treatment method for the MXene electrode material of the sodium ion capacitor as claimed in claim 1, wherein: the compaction process uses a powder tablet press with a pressure of 10 MPa.
6. The pre-sodium treatment method for the MXene electrode material of the sodium ion capacitor as claimed in claim 1, wherein: a button cell punching machine is used in the cutting process, and the diameter of the MXene electrode material is 16 mm.
7. The pre-sodium treatment method for the MXene electrode material of the sodium ion capacitor as claimed in claim 1, wherein: the thickness of the copper foil used in the spraying is 0.02 mm.
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| CN110061228A (en) * | 2019-05-07 | 2019-07-26 | 大连理工大学 | Anode material of lithium-ion battery and synthetic method based on MXene Yu fake capacitance type transition metal oxide nano composite construction |
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| JP2013235949A (en) * | 2012-05-09 | 2013-11-21 | Aisin Seiki Co Ltd | Process of manufacturing lithium-ion capacitor |
| CN105374571B (en) * | 2014-08-26 | 2018-01-23 | 万星光电子(东莞)有限公司 | Lithium-ion capacitor negative plate and preparation method thereof, winding type lithium ion capacitor |
| DE102015217809A1 (en) * | 2015-09-17 | 2017-03-23 | Robert Bosch Gmbh | Prelithiated, carbon-coated anode active material |
| CN105590760A (en) * | 2015-12-29 | 2016-05-18 | 上海奥威科技开发有限公司 | Lithium ion capacitor cathode novel lithium pre-insertion method |
| CN105845894B (en) * | 2016-05-04 | 2018-11-02 | 合肥国轩高科动力能源有限公司 | A kind of lithium ion battery negative electrode carries out the method and device of prelithiation |
| CN106876781A (en) * | 2017-03-10 | 2017-06-20 | 欣旺达电子股份有限公司 | Sodium-ion battery and preparation method thereof |
| CN108134055B (en) * | 2017-11-22 | 2020-10-02 | 同济大学 | Method for synthesizing sodium titanate nanoribbon/titanium carbide nanosheet compound |
| CN108336301A (en) * | 2018-02-06 | 2018-07-27 | 哈尔滨工业大学 | A kind of high-performance sodium-ion battery cathode and preparation method thereof |
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