CN109411242A - A kind of electrode material for super capacitor and preparation method thereof - Google Patents

A kind of electrode material for super capacitor and preparation method thereof Download PDF

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Publication number
CN109411242A
CN109411242A CN201710706091.4A CN201710706091A CN109411242A CN 109411242 A CN109411242 A CN 109411242A CN 201710706091 A CN201710706091 A CN 201710706091A CN 109411242 A CN109411242 A CN 109411242A
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CN
China
Prior art keywords
mno
electrode material
super capacitor
preparation
graphene
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Pending
Application number
CN201710706091.4A
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Chinese (zh)
Inventor
秦学
吕军
王宏智
周琴
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JIANGSU JINYI NEW ENERGY TECHNOLOGY Co Ltd
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JIANGSU JINYI NEW ENERGY TECHNOLOGY Co Ltd
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Priority to CN201710706091.4A priority Critical patent/CN109411242A/en
Publication of CN109411242A publication Critical patent/CN109411242A/en
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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
    • 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
    • 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
    • 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

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  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Chemical & Material Sciences (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Electric Double-Layer Capacitors Or The Like (AREA)

Abstract

The present invention relates to a kind of electrode material for super capacitor, it is Graphene gel/MnO2Composite material obtains single-layer graphene oxide using ultrasonic method and is distributed in deionized water using graphite oxide as presoma, and MnCl is added2Ultrasonic agitation is uniformly dispersed, and hydrazine hydrate is then added and is stirring uniformly to obtain mixed solution, mixed solution is poured into and carries out hydro-thermal reaction in hydrothermal reaction kettle, reaction product is filtered, washed, being dried to obtain Graphene gel/MnO2Composite material.Composite material has the characteristics that large specific surface area, good conductivity, capacitor are high, cycle performance is excellent.

Description

A kind of electrode material for super capacitor and preparation method thereof
Technical field
The invention belongs to super capacitor material synthesis technical fields, and in particular to a kind of electrode material for super capacitor and Preparation method.
Background technique
Supercapacitor is that a kind of service life is long, and fills with the energy storage of the advantages such as high power density and quick charge capability It sets, causes great attention in application fields such as each class of electronic devices, energy storage, new-energy automobiles.Due to determining supercapacitor Performance is electrode material, therefore research is all concentrated mainly on this respect by most of researcher.MnO2Be it is a kind of very Potential electrode material presents very wide potential window and good capacitive property, while source in neutral electrolyte It is abundant, it is nontoxic, it is well received by the public；But MnO2Electric conductivity it is poor, effective ratio area is smaller, be restrict its as super The unfavorable factor that capacitor electrode material is promoted, and MnO2Different from general fake capacitance material, the capacitor master of manganese dioxide It to be reacted from its surface, so having a big specific surface area is to promote the most effectual way of its specific capacitance.
Graphene gel has very high power density, but its energy density is still slightly compared to other fake capacitance materials It is inadequate.
The present invention provides a kind of Graphene gel/MnO2The preparation method of composite material, the combination electrode material energy of invention Have both Graphene gel and MnO2Advantage has the characteristics that large specific surface area, good conductivity, capacitor are high, cycle performance is excellent.
Summary of the invention
The purpose of the present invention is to provide a kind of supercapacitor Graphene gel/MnO2Combination electrode material and its system Preparation Method.
The technical scheme is that a kind of electrode material for super capacitor, it is Graphene gel/MnO2Composite wood Material, using graphite oxide as presoma, ultrasound obtains single-layer graphene oxide, utilizes MnCl2Reduction-oxidation graphite flake layer obtains MnO2 The graphene film of load, these loads MnO2Lamella tired folded form multi-layer graphene and MnO2Complex three-dimensional material.
A kind of preparation method of electrode material for super capacitor of the invention, its step are as follows:
1) using graphite oxide as presoma, single-layer graphene oxide is obtained using ultrasonic method and is distributed to deionized water In, MnCl is added2Ultrasonic agitation is uniformly dispersed；
2) solution in step 1) is added hydrazine hydrate and is stirring uniformly to obtain mixed solution；
3) mixed solution in step 2) is poured into and carries out hydro-thermal reaction in hydrothermal reaction kettle；
4) reaction product in step 3) filtered, washed, being dried to obtain Graphene gel/MnO2Composite material.
Preferred steps 1) graphene oxide concentration is 2g/L in mixed solution；MnCl2Concentration is 1g/L~5g/L.
Preferred steps 2) concentration of hydrazine hydrate is 20%~30% in mixed solution.
Preferred steps 3) in hydrothermal temperature be 80 DEG C~120 DEG C, the hydro-thermal time is 16h~for 24 hours.
Preferred steps 4) in drying temperature be 55 DEG C~90 DEG C, drying time be 8h~12h.
The beneficial effects of the present invention are: according to the above method, the combination electrode material of invention can have both Graphene gel and MnO2Advantage has the characteristics that large specific surface area, good conductivity, capacitor are high, cycle performance is excellent.
Specific embodiment
Embodiment 1
1) using graphite oxide as presoma, single-layer graphene oxide is obtained using ultrasonic method and is distributed to deionized water In, MnCl is added2Ultrasonic agitation is uniformly dispersed.Wherein graphene oxide concentration is 2g/L；MnCl2Concentration is 3g/L.
2) hydrazine hydrate that volume ratio is 1/3, concentration of hydrazine hydrate 26% is added in the solution in step 1).
3) mixed solution in step 2) being poured into and carries out hydro-thermal reaction in hydrothermal reaction kettle, hydrothermal temperature is 95 DEG C, The hydro-thermal time is 20h.；
4) reaction product in step 3) filtered, washed, being dried to obtain Graphene gel/MnO2Composite material, Middle drying temperature is 70 DEG C, drying time 9h.
By above-mentioned Graphene gel/MnO2Composite material and SuperP, PVDF are equal with the ratio mixing of mass ratio 30:2:1 After even, supercapacitor, the chemical property of test material are made using carbon as reference electrode.
Test result:
Embodiment 2
1) using graphite oxide as presoma, single-layer graphene oxide is obtained using ultrasonic method and is distributed to deionized water In, MnCl is added2Ultrasonic agitation is uniformly dispersed.Wherein graphene oxide concentration is 2g/L；MnCl2Concentration is 1g/L.
2) hydrazine hydrate that volume ratio is 1/3, concentration of hydrazine hydrate 20% is added in the solution in step 1).
3) mixed solution in step 2) being poured into and carries out hydro-thermal reaction in hydrothermal reaction kettle, hydrothermal temperature is 95 DEG C, The hydro-thermal time is 20h.；
4) reaction product in step 3) filtered, washed, being dried to obtain Graphene gel/MnO2Composite material, Middle drying temperature is 70 DEG C, drying time 9h.
By above-mentioned Graphene gel/MnO2Composite material and SuperP, PVDF are equal with the ratio mixing of mass ratio 30:2:1 After even, supercapacitor, the chemical property of test material are made using carbon as reference electrode.
Test result:
Embodiment 3
1) using graphite oxide as presoma, single-layer graphene oxide is obtained using ultrasonic method and is distributed to deionized water In, MnCl is added2Ultrasonic agitation is uniformly dispersed.Wherein graphene oxide concentration is 2g/L；MnCl2Concentration is 5g/L.
2) hydrazine hydrate that volume ratio is 1/3, concentration of hydrazine hydrate 30% is added in the solution in step 1).
3) mixed solution in step 2) being poured into and carries out hydro-thermal reaction in hydrothermal reaction kettle, hydrothermal temperature is 95 DEG C, The hydro-thermal time is 20h.；
4) reaction product in step 3) filtered, washed, being dried to obtain Graphene gel/MnO2Composite material, Middle drying temperature is 70 DEG C, drying time 9h.
By above-mentioned Graphene gel/MnO2Composite material and SuperP, PVDF are equal with the ratio mixing of mass ratio 30:2:1 After even, supercapacitor, the chemical property of test material are made using carbon as reference electrode.
Test result:
The present invention is not limited to the embodiment of above-mentioned embodiment, this field inspiration according to the present invention is not departed from The improvement and modification that scope of the invention is made all should be within the scope of the present invention.

Claims (6)

1. a kind of electrode material for super capacitor, it is Graphene gel/MnO2Composite material, which is characterized in that with graphite oxide For presoma, ultrasound obtains single-layer graphene oxide, utilizes MnCl2Reduction-oxidation graphite flake layer obtains MnO2The graphene of load Piece, these loads MnO2Lamella tired folded form multi-layer graphene and MnO2Complex three-dimensional material.
2. a kind of preparation method of electrode material for super capacitor according to claim 1, it is characterized in that steps are as follows:
1) using graphite oxide as presoma, single-layer graphene oxide is obtained using ultrasonic method and is distributed in deionized water, is added Enter MnCl2Ultrasonic agitation is uniformly dispersed；
2) solution in step 1) is added hydrazine hydrate and is stirring uniformly to obtain mixed solution；
3) mixed solution in step 2) is poured into and carries out hydro-thermal reaction in hydrothermal reaction kettle；
4) reaction product in step 3) filtered, washed, being dried to obtain Graphene gel/MnO2Composite material.
3. a kind of preparation method of electrode material for super capacitor according to claim 2, it is characterised in that: step 1) is mixed Closing graphene oxide concentration in solution is 2g/L；MnCl2Concentration is 1g/L~5g/L.
4. a kind of preparation method of electrode material for super capacitor according to claim 2, it is characterised in that: step 2) is mixed Closing concentration of hydrazine hydrate in solution is 20%~30%.
5. a kind of preparation method of electrode material for super capacitor according to claim 2, it is characterised in that: in step 3) Hydrothermal temperature is 80 DEG C~120 DEG C, and the hydro-thermal time is 16h~for 24 hours.
6. a kind of preparation method of electrode material for super capacitor according to claim 2, it is characterised in that: in step 4) Drying temperature is 55 DEG C~90 DEG C, and drying time is 8h~12h.
CN201710706091.4A 2017-08-17 2017-08-17 A kind of electrode material for super capacitor and preparation method thereof Pending CN109411242A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210319960A1 (en) * 2020-04-14 2021-10-14 National Chin-Yi University Of Technology Supercapacitor electrode including silicon dioxide microsphere and fabrication method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110165321A1 (en) * 2010-01-07 2011-07-07 Aruna Zhamu Continuous process for producing spacer-modified nano Graphene electrodes for supercapacitors
CN105271211A (en) * 2015-11-26 2016-01-27 清华大学深圳研究生院 Graphene-based three-dimensional macro body as well as preparation method and application thereof
CN107039622A (en) * 2017-02-22 2017-08-11 东莞市佳乾新材料科技有限公司 A kind of preparation method of the sodium-ion battery based on graphite/Prussian blue positive electrode

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20110165321A1 (en) * 2010-01-07 2011-07-07 Aruna Zhamu Continuous process for producing spacer-modified nano Graphene electrodes for supercapacitors
CN105271211A (en) * 2015-11-26 2016-01-27 清华大学深圳研究生院 Graphene-based three-dimensional macro body as well as preparation method and application thereof
CN107039622A (en) * 2017-02-22 2017-08-11 东莞市佳乾新材料科技有限公司 A kind of preparation method of the sodium-ion battery based on graphite/Prussian blue positive electrode

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20210319960A1 (en) * 2020-04-14 2021-10-14 National Chin-Yi University Of Technology Supercapacitor electrode including silicon dioxide microsphere and fabrication method thereof
US11776767B2 (en) * 2020-04-14 2023-10-03 National Chin-Yi University Of Technology Fabrication methods for supercapacitor electrode including silicon dioxide microsphere

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Application publication date: 20190301