CN110428983A - A kind of pre- sodium modification method of sodium ion capacitor MXene electrode material - Google Patents

A kind of pre- sodium modification method of sodium ion capacitor MXene electrode material Download PDF

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Publication number
CN110428983A
CN110428983A CN201910777406.3A CN201910777406A CN110428983A CN 110428983 A CN110428983 A CN 110428983A CN 201910777406 A CN201910777406 A CN 201910777406A CN 110428983 A CN110428983 A CN 110428983A
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China
Prior art keywords
sodium
ion capacitor
mxene
electrode material
sodium ion
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CN201910777406.3A
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CN110428983B (en
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牛棱渊
李军
刘卯成
张小美
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Hangzhou Realistic New Materials Technology Co Ltd
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Hangzhou Realistic New Materials Technology Co Ltd
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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]
    • 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
    • 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
    • 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
    • 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 present invention relates to a kind of pre- sodium modification methods for sodium ion capacitor MXene electrode material; main preparation step includes: under inert atmosphere protection; by multilayer MXene powder, conductive additive and binder 8:1:1 in mass ratio are uniformly mixed, and N-Methyl pyrrolidone solution are added, slurry is made；The heating of metallic sodium block is melted into metallic sodium melt；By electrode slurry and metallic sodium melt, using spray gun, successively alternating spray removes copper foil after dry on copper foil, is compacted, cut-parts, obtains the pre- sodium MXene electrode material for sodium ion capacitor after assembling button capacitor.

Description

A kind of pre- sodium modification method of sodium ion capacitor MXene electrode material
Technical field
The present invention relates to a kind of pre- sodium technologies of sodium ion capacitor MXene electrode material.
Background technique
Sodium ion capacitor is a kind of novel hybrid capacitors as made of battery-type electrode chose and capacitive electrode combination, Has many advantages, such as secondary cell high-energy density and traditional capacitor high power density and excellent cycling stability.MXene by In unique two-dimensional layered structure, the channel of fast transferring can be provided for electrolyte ion, become the sodium of great development prospect Ionistor battery-type electrode chose material.However, the pre- embedding sodium of battery-type electrode chose mainly has promotion sodium in sodium ion capacitor at present The methods of ion organic electrolyte concentration and the pre- embedding sodium of electrochemistry, there are pre- sodium degree inadequate, the pre- embedding sodium amount of electrode material The problems such as controllability is poor, pre- sodium complex steps and the consumption of sodium ion capacitor devices sodium source are too fast, becomes limitation sodium ion The bottleneck sexual factor of capacitor development.Therefore, the present invention proposes to solve this problem using the method for spraying pre- embedding sodium.This hair Bright patent direct spraying metallic sodium melt is added in sodium ion capacitor as sodium source, is connect certainly by MXene with metallic sodium The mode of embedding sodium is touched to provide enough sodium ions and carry out pre- sodium process.Compared to traditional pre- sodium mode, this method has Effect avoids the problem of pre- embedding sodium amount poor controllability and device repeated disassembled and assembled during the pre- sodium of tradition, has good controllable Property and ease for operation, be not only able to it is directly sufficient the sodium ion quantity of pre- insertion MXene electrode is provided, and can accurately control The alternately number of plies and thickness of intercalation distribution, while also reducing the use cost of sodium ion capacitor, is to having pre- sodium at present The important innovation and supplement of change technology.
Summary of the invention
The object of the present invention is to provide a kind of pre- sodium modification methods of sodium ion capacitor MXene electrode material.
The present invention is to the steps include: for the pre- sodium modification method of sodium ion capacitor MXene electrode material in inert atmosphere Under protection, by multilayer MXene powder, conductive additive and binder 8:1:1 in mass ratio are uniformly mixed, and N- methylpyrrole is added Slurry is made in alkanone solution；The heating of metallic sodium block is melted into metallic sodium molten liquid；Electrode slurry and metallic sodium melt are used Spray gun successively remove copper foil after dry on copper foil by alternating spray, is compacted, cut-parts, is used for after assembling button capacitor The pre- sodium MXene electrode material of sodium ion capacitor, concrete operation step:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) use Germany's schutze KA-2 automatic spray gun by step (1) and step (2) the electrode obtained slurry and metallic sodium melt Successively for alternating spray on copper foil, spray gun pressure 0.8-1.5Bar, jet size is 0.2 and 0.3 mm.80 DEG C of dryings 24 H removes copper foil, and the MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor stands in a manner of from the pre- embedding sodium of contact and obtains the sodium ion capacitor that pre- embedding sodium is completed afterwards for 24 hours.
Specific implementation method
Embodiment 1:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) Germany's schutze KA-2 automatic spray gun is used, nozzle diameter is 0.2 mm, and adjusting atomizing pressure is 0.8 bar, will Step (1) and step (2) the electrode obtained slurry and metallic sodium melt are successively sprayed on copper foil with spray gun, 80 DEG C of dryings 24 H removes copper foil, and the pre- sodium MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor stands in a manner of from the pre- embedding sodium of contact and obtains the sodium ion capacitor that pre- embedding sodium is completed afterwards for 24 hours.
Embodiment 2:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) Germany's schutze KA-2 automatic spray gun is used, nozzle diameter is 0.2 mm, and adjusting atomizing pressure is 1.15 bar, Step (1) and step (2) the electrode obtained slurry and metallic sodium melt will be successively sprayed on copper foil with spray gun, 80 DEG C of dryings 24 h, copper foil is removed, and the pre- sodium MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor obtains the sodium ion capacitor that pre- embedding sodium is completed after standing 24 h in a manner of from the pre- embedding sodium of contact.
Embodiment 3:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) Germany's schutze KA-2 automatic spray gun is used, nozzle diameter is 0.2 mm, and adjusting atomizing pressure is 1.5 bar, will Step (1) and step (2) the electrode obtained slurry and metallic sodium melt are successively sprayed on copper foil with spray gun, 80 DEG C of dryings 24 H removes copper foil, and the pre- sodium MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor obtains the sodium ion capacitor that pre- embedding sodium is completed after standing 24 h in a manner of from the pre- embedding sodium of contact.
Embodiment 4:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) Germany's schutze KA-2 automatic spray gun is used, nozzle diameter is 0.3 mm, and adjusting atomizing pressure is 0.8 bar, will Step (1) and step (2) the electrode obtained slurry and metallic sodium melt are successively sprayed on copper foil with spray gun, 80 DEG C of dryings 24 H removes copper foil, and the pre- sodium MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor obtains the sodium ion capacitor that pre- embedding sodium is completed after standing 24 h in a manner of from the pre- embedding sodium of contact.
Embodiment 5:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) Germany's schutze KA-2 automatic spray gun is used, nozzle diameter is 0.3 mm, and adjusting atomizing pressure is 1.15 bar, Step (1) and step (2) the electrode obtained slurry and metallic sodium melt will be successively sprayed on copper foil with spray gun, 80 DEG C of dryings 24 h, copper foil is removed, and the pre- sodium MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor obtains the sodium ion capacitor that pre- embedding sodium is completed after standing 24 h in a manner of from the pre- embedding sodium of contact.
Embodiment 6:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) Germany's schutze KA-2 automatic spray gun is used, nozzle diameter is 0.3 mm, and adjusting atomizing pressure is 1.5 bar, will Step (1) and step (2) the electrode obtained slurry and metallic sodium melt are successively sprayed on copper foil with spray gun, 80 DEG C of dryings 24 H removes copper foil, and the pre- sodium MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor obtains the sodium ion capacitor that pre- embedding sodium is completed after standing 24 h in a manner of from the pre- embedding sodium of contact.
The above is the embodiment of the present invention, is not intended to limit the scope of the invention, all to be said using the present invention Equivalent structure or equivalent flow shift made by bright book content is applied directly or indirectly in other relevant field technologies, It similarly include in the invention patent protection scope.

Claims (7)

1. the steps include: provided by the present invention for the pre- sodium modification method of sodium ion capacitor MXene electrode material in indifferent gas Under atmosphere protection, by multilayer MXene powder, conductive additive and binder 8:1:1 in mass ratio are uniformly mixed, and N- methyl pyrrole is added Slurry is made in pyrrolidone solution；The heating of metallic sodium block is melted into metallic sodium molten liquid；Electrode slurry and metallic sodium melt are made With spray gun, successively alternating spray removes copper foil after dry on copper foil, is compacted, cut-parts, is used after assembling button capacitor In the pre- sodium MXene electrode material of sodium ion capacitor, concrete operation step:
(1) in inert atmosphere control box, by 80 mg MXene powder, 10 mg conductive additives and the mixing of 10 mg binders, N-Methyl pyrrolidone solution is added, slurry is made；
(2) 1 g metallic sodium block is heated into metallic sodium melt at 100 DEG C；
(3) use Germany's schutze KA-2 automatic spray gun by step (1) and step (2) the electrode obtained slurry and metallic sodium melt Successively for alternating spray on copper foil, spray gun pressure is 0.8-1.5 Bar, and jet size is 0.2 and 0.3 mm；80 DEG C of dryings 24 H removes copper foil, and the MXene electrode material for sodium ion capacitor can be obtained in compacting, cut-parts；
(4) button is assembled as the positive and negative anodes of sodium ion capacitor using MXene electrode slice obtained by active carbon and step (3) Sodium ion capacitor obtains the sodium ion capacitor that pre- embedding sodium is completed after standing 24 h in a manner of from the pre- embedding sodium of contact.
2. the pre- sodium modification method according to claim 1 for the MXene electrode material for sodium ion capacitor, special Be: described MXene is Ti3C2TX,, Ti2CTx, V2CTx, Mo3C2TxOr in which one or more.
3. the pre- sodium modification method of the MXene electrode material according to claim 1 for sodium ion capacitor, spy exists In: described conductive agent be acetylene black, Ketjen black, Super P or in which one or more.
4. the pre- sodium modification method of the MXene electrode material according to claim 1 for sodium ion capacitor, spy exists In: described binder is polytetrafluoroethylene (PTFE), one or both of sodium carboxymethylcellulose.
5. the pre- sodium modification method of the MXene electrode material according to claim 1 for sodium ion capacitor, spy exists In: described compacting process uses powder compressing machine, and pressure is 10 MPa.
6. the pre- sodium modification method of the MXene electrode material according to claim 1 for sodium ion capacitor, spy exists In: described cut-parts process uses button cell sheet-punching machine, and MXene electrode slice diameter is 16 mm.
7. the pre- sodium modification method of the MXene electrode material according to claim 1 for sodium ion capacitor, spy exists In: used copper foil with a thickness of 0.02 mm when described spraying.
CN201910777406.3A 2019-08-22 2019-08-22 Pre-sodium treatment method for MXene electrode material of sodium ion capacitor Active CN110428983B (en)

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Publication number Priority date Publication date Assignee Title
CN110911175A (en) * 2019-11-12 2020-03-24 武汉工程大学 Carbonized eggshell membrane, MXene and polypyrrole composite gel and preparation method and application thereof
US11682531B1 (en) * 2022-01-20 2023-06-20 Imam Abdulrahman Bin Faisal University Nanocomposite electrodes and method of preparation thereof
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