CN107026027A - A kind of preparation method of the electrode material of ultracapacitor - Google Patents

A kind of preparation method of the electrode material of ultracapacitor Download PDF

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Publication number
CN107026027A
CN107026027A CN201710229104.3A CN201710229104A CN107026027A CN 107026027 A CN107026027 A CN 107026027A CN 201710229104 A CN201710229104 A CN 201710229104A CN 107026027 A CN107026027 A CN 107026027A
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electrode material
preparation
hours
ultracapacitor
dimethyl sulfoxide
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CN107026027B (en
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范金辰
廖柯璇
章蒨
郭帅楠
朱晟
闵宇霖
徐群杰
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Shanghai University of Electric Power
University of Shanghai for Science and Technology
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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
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • 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
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • 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
    • H01G11/44—Raw materials therefor, e.g. resins or coal
    • 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 provides a kind of preparation method of the electrode material of ultracapacitor, Fanglun 1414 is stirred together to be completely dissolved in dimethyl sulfoxide (DMSO) with potassium hydroxide and obtains the dimethyl sulfoxide dispersion liquid that Kev draws nanofiber, add acetic acid manganese solution, stir, obtain cotton-shaped dispersion soln, it is put into freeze drier after being filtered by vacuum to freeze, material finally is put into high-temperature calcination in tube furnace can obtain electrode material for super capacitor.The electrochemical performance of the electrode material obtained by the method for the present invention, possess higher specific capacitance, and the performance for filling slow play soon is presented during the constant current charge-discharge under larger current density, great business promotion value possesses preferable development prospect in following energy storage field.

Description

A kind of preparation method of the electrode material of ultracapacitor
Technical field
The invention belongs to electricity field, it is related to a kind of electrode material, specifically a kind of electrode material of ultracapacitor The preparation method of material.
Background technology
Ultracapacitor (EDLC) is called double layer capacitor, as a kind of new between traditional capacitor and battery Type has become the focus of people's concern and research now without energy storage device is safeguarded.Its specific power is more than 10 times of battery, The ability for storing electric charge is higher than ordinary capacitor, and with lot of advantages enter operating temperature range it is wide, can fast charging and discharging And have extended cycle life, pollution-free zero-emission etc..And improvement of the electrode material to the performance of ultracapacitor plays very important Effect, it may be said that be the part of ultracapacitor core the most, therefore electrode material of the exploitation with excellent properties is super electricity The most key problem in container research.
The content of the invention
It is an object of the invention to provide a kind of preparation method of the electrode material of ultracapacitor, described is this super The preparation method of the electrode material of capacitor will solve that supercapacitor specific capacity of the prior art is high, chemical property not Strong technical problem.
The invention provides a kind of preparation method of the electrode material of ultracapacitor, comprise the following steps：
1) Kafra fiber is cut into the short-term of 0.1 ~ 20 centimeter length；
2) potassium hydroxide is weighed, is pulverized；
3) by Kafra fiber and potassium hydroxide pour into dimethylsulfoxide solvent stir 72 ~ 240 hours it is complete to Kafra fiber Dissolving, obtains the dimethyl sulfoxide dispersion liquid that Kev draws nanofiber, the thing of Kafra fiber, potassium hydroxide and dimethylsulfoxide solvent Material is than being 0.1 ~ 2 gram：1.0 ~ 3.0 grams：500 ~ 2000 milliliters；
4) the dimethyl sulfoxide dispersion liquid of nanofiber is drawn to mix for 1 ~ 5 mg/mL acetic acid manganese solution and above-mentioned Kev concentration Close, described acetic acid manganese solution and Kev draw the volume ratio of the dimethyl sulfoxide dispersion liquid of nanofiber to be 100 ~ 200 milliliters：100 ~ 200 milliliters, stirring 1 ~ 5 hour is well mixed to dispersion liquid；
5) by step 4）The cotton-shaped dispersing liquid mixed, vacuum filtration, and with deionized water by after its potassium ion wash clean Take solid；
6) by step 5）After obtained solid is put into freeze drier drying 72 ~ 120 hours, under nitrogen protection, 600 ~ 900 take the photograph High-temperature calcination is carbonized under family name's degree, takes out carbonized solid and pulverizes；
7) by step 6）Obtained dusty material, acetylene black, Kynoar is 50-99 in mass ratio:1-49:1-49 is mixed, Electrode material for super capacitor is can be used as after grinding is uniform.
Further, the mass ratio of described Kafra fiber and potassium hydroxide is 1:1~1:Between 5.
Further, the concentration for the acetic acid manganese solution matched somebody with somebody is in 2mg/mL.
Further, step 5）The solid of vacuum filtration is needed by being freeze-dried 24 hours ~ 72 hours.
Further, step 6）High-temperature calcination must under nitrogen protection, temperature at 600 ~ 900 degree, and be incubated 3 hours with On, heating rate is at 2 ~ 10 degrees/min.
Further, in step 7）In, Kynoar is dissolved in 1-METHYLPYRROLIDONE before the milling.
The present invention is by PPTA (Kafra fiber) fiber in dimethyl sulfoxide (DMSO)（DMSO）In with hydrogen Potassium oxide（KOH）It is stirred together to be completely dissolved and obtains the dimethyl sulfoxide dispersion liquid that Kev draws nanofiber.Add manganese acetate Solution, stirs, and obtains cotton-shaped dispersion soln.Freeze drier is put into after being filtered by vacuum to freeze.Finally material is put Enter high-temperature calcination in tube furnace and can obtain electrode material for super capacitor.The electrode material obtained by the method for the present invention Electrochemical performance, possesses higher specific capacitance, and is presented during the constant current charge-discharge under larger current density fast Fill the performance of slow play.
The electrode material that the present invention prepares nano-scale fiber network structure using Kafra fiber has good chemically stable Property, be doped with after manganese and add fake capacitance effect, its chemical property can be greatly improved.The electrode material synthesis of the present invention The simple cost of process is relatively low, and in aqueous electrolyte, the specific discharge capacity under 1 A/g current densities is in 510 ~ 820 F/g models Enclose.
Compared with prior art, its technological progress is significant to the present invention.The electrode material for super capacitor of the present invention is gathered around There are electric double layer capacitance effect and fake capacitance effect, so electrode material possesses larger chemical property there is provided specific capacity, and And the synthetic method of the present invention is simple, the nano-scale fiber network structure prepared possesses preferable electric double layer effect, great Business promotion is worth, and possesses preferable development prospect in following energy storage field.
Brief description of the drawings
Fig. 1 is the scanning electron microscopic picture of the electrode material of embodiment 1.
Fig. 2 is the transmission electron microscope picture of the electrode material of embodiment 1.
Fig. 3 is constant current charge-discharge curve of the electrode material of embodiment 1 under different current densities.
Fig. 4 is the electrode material of embodiment 1 in the different cyclic voltammetry curves swept under speed.
Fig. 5 is the electrode material XRD that embodiment 1 is obtained after different carburizing temperatures.
Embodiment
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of electrode material for super capacitor ANFS/Mn2+Preparation method.
1.0341g Kafra fibers are cut into 1cm or so length, are put into 500mLDMSO, then weigh 1.5023gKOH, grind into powder is poured into DMSO solution, and magnetic agitation obtains brown liquid after 168 hours, and Kev is towed Dimension is dissolved completely in DMSO solution, obtains ANFS solution.
Prepare the acetic acid manganese solution that concentration is 2mg/mL to pour into 200mL ANFS solution, mechanical agitation 10h is to molten immediately Liquid is in well mixed cotton-shaped gel solution.
Cotton-shaped gel solution is filtered by vacuum using 22nm filter paper, and filtering and washing is carried out with 0.5L ~ 1L deionized water.
The membranaceous solid that suction filtration is obtained is collected, passes through the heating speed being put into after freeze-drying in tube furnace according to 5 DEG C/min Rate is to 700 DEG C（600、800℃）Insulation 3 hours.Carbonized solid is taken out, grind into powder is to obtain electrode of super capacitor material Material.
By the electrode material of preparation according to electrode material：Acetylene black：PVDF=8:1:1（Mass ratio, PVDF is dissolved in advance In 1- methyl pyrrolidones）Ratio be added together grinding, half an hour after be coated in titanium net, dry after 4M KOH electricity Solve in liquid and test.
Embodiment 2
A kind of electrode material for super capacitor ANFS/Mn2+Preparation method.
1.005g Kafra fibers are cut into 1cm or so length, are put into 500mLDMSO, then weigh 1.5072gKOH, Grind into powder is poured into DMSO solution, and magnetic agitation obtains brown liquid after 168 hours, and Kafra fiber is dissolved completely in In DMSO solution, ANFS solution is obtained.
Prepare the acetic acid manganese solution that concentration is 2mg/mL to pour into 200mL ANFS solution, mechanical agitation 10h is to molten immediately Liquid is in well mixed cotton-shaped gel solution.
Cotton-shaped gel solution is filtered by vacuum using 22nm filter paper, and filtering and washing is carried out with 0.5L ~ 1L deionized water.
The membranaceous solid that suction filtration is obtained is collected, passes through the heating speed being put into after freeze-drying in tube furnace according to 5 DEG C/min Rate to 800 DEG C be incubated 3 hours.Carbonized solid is taken out, grind into powder is to obtain electrode material for super capacitor.
By the electrode material of preparation according to electrode material：Acetylene black：PVDF=8:1:1（Mass ratio, PVDF is dissolved in advance In 1- methyl pyrrolidones）Ratio be added together grinding, half an hour after be coated in titanium net, dry after 4M KOH electricity Solve in liquid and test.
Embodiment 3
A kind of electrode material for super capacitor ANFS/Mn2+Preparation method.
2.0137g Kafra fibers are cut into 1cm or so length, are put into 500mLDMSO, then weigh 1.5001gKOH, grind into powder is poured into DMSO solution, and magnetic agitation obtains brown liquid after 200 hours, and Kev is towed Dimension is dissolved completely in DMSO solution, obtains ANFS solution.
Prepare the acetic acid manganese solution that concentration is 4mg/mL to pour into 200mL ANFS solution, mechanical agitation 10h is to molten immediately Liquid is in well mixed cotton-shaped gel solution.
Cotton-shaped gel solution is filtered by vacuum using 22nm filter paper, and filtering and washing is carried out with 0.5L ~ 1L deionized water.
The membranaceous solid that suction filtration is obtained is collected, passes through the heating speed being put into after freeze-drying in tube furnace according to 5 DEG C/min Rate to 900 DEG C be incubated 3 hours.Carbonized solid is taken out, grind into powder is to obtain electrode material for super capacitor
The electrode material that the example of the above three is finally obtained is as ultracapacitor active material, according to active material:Acetylene black: PVDF= 8:1:1（Mass ratio, PVDF is dissolved in 1- methyl pyrrolidones in advance）Ratio be added together grinding, half an hour After be coated in nickel foam, dry after in 4M KOH electrolyte test.Its constant current charge-discharge under different current densities Curve is as shown in figure 3, utilize calculation formulaWithFormula can calculate the ratio for obtaining the composite Capacity is 510 ~ 820F/g.
While specific embodiments of the present invention have been shown and described, but for a person skilled in the art, Be appreciated that without departing from the principles and spirit of the present invention can to these embodiments carry out it is a variety of change, replace, Modification and modification, the scope invented are defined by the appended claims and the equivalents thereof.

Claims (6)

1. a kind of preparation method of the electrode material of ultracapacitor, it is characterised in that comprise the following steps：
1）Kafra fiber is cut into the short-term of 0.1 ~ 20 centimeter length；
2）Potassium hydroxide is weighed, is pulverized；
3）By Kafra fiber and potassium hydroxide pour into dimethylsulfoxide solvent stir 72 ~ 240 hours it is complete to Kafra fiber Dissolving, obtains the dimethyl sulfoxide dispersion liquid that Kev draws nanofiber, the thing of Kafra fiber, potassium hydroxide and dimethylsulfoxide solvent Material is than being 0.1 ~ 2 gram：1.0 ~ 3.0 grams：500 ~ 2000 milliliters；
4）The dimethyl sulfoxide dispersion liquid of nanofiber is drawn to mix for 1 ~ 5 mg/mL acetic acid manganese solution and above-mentioned Kev concentration Close, described acetic acid manganese solution and Kev draw the volume ratio of the dimethyl sulfoxide dispersion liquid of nanofiber to be 100 ~ 200 milliliters：100 ~ 200 milliliters, stirring 1 ~ 5 hour is well mixed to dispersion liquid；
5）By step 4）The cotton-shaped dispersing liquid mixed, vacuum filtration, and with deionized water by after its potassium ion wash clean Take out solid；
6）By step 5）After obtained solid is put into freeze drier drying 72 ~ 120 hours, under nitrogen protection, 600 ~ 900 Degree Celsius lower high-temperature calcination carbonization, takes out carbonized solid and pulverizes；
7）By step 6）Obtained dusty material, acetylene black, Kynoar is 50-99 in mass ratio:1-49:1-49 is mixed, Electrode material for super capacitor is can be used as after grinding is uniform.
2. a kind of preparation method of the electrode material of ultracapacitor according to claim 1, it is characterised in that：Kev is drawn The mass ratio of fiber and potassium hydroxide is 1:1~1:Between 5.
3. a kind of preparation method of the electrode material of ultracapacitor according to claim 1, it is characterised in that：Matched somebody with somebody The concentration of acetic acid manganese solution is in 2mg/mL.
4. a kind of preparation method of the electrode material of ultracapacitor according to claim 1, it is characterised in that：Step 5） The solid of vacuum filtration is needed by being freeze-dried 24 hours ~ 72 hours.
5. a kind of preparation method of the electrode material of ultracapacitor according to claim 1, it is characterised in that：Step 6） High-temperature calcination must under nitrogen protection, and temperature is incubated more than 3 hours at 600 ~ 900 degree, and heating rate is in 2 ~ 10 degree mins Clock.
6. a kind of preparation method of the electrode material of ultracapacitor according to claim 1, it is characterised in that：In step 7）In, Kynoar is dissolved in 1-METHYLPYRROLIDONE before the milling.
CN201710229104.3A 2017-04-10 2017-04-10 A kind of preparation method of the electrode material of supercapacitor Active CN107026027B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110838412A (en) * 2018-06-20 2020-02-25 苏州大学 Aramid fiber electrochemical capacitor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030030963A1 (en) * 1996-05-15 2003-02-13 Howard Tennent Graphitic nanofibers in electrochemical capacitors
CN102823038A (en) * 2010-12-22 2012-12-12 韩华石油化学株式会社 A composite comprising an electrode-active transition metal compound and a fibrous carbon material, and a method for preparing the same
CN105826088A (en) * 2016-05-10 2016-08-03 复旦大学 Carbon aerogel/manganese dioxide combined electrode material with multi-level structure, and preparation method thereof
CN105845455A (en) * 2016-05-10 2016-08-10 复旦大学 Polyacrylonitrile nanometer fiber/polyimide-based composite carbon aerogel electrode material and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030030963A1 (en) * 1996-05-15 2003-02-13 Howard Tennent Graphitic nanofibers in electrochemical capacitors
CN102823038A (en) * 2010-12-22 2012-12-12 韩华石油化学株式会社 A composite comprising an electrode-active transition metal compound and a fibrous carbon material, and a method for preparing the same
CN105826088A (en) * 2016-05-10 2016-08-03 复旦大学 Carbon aerogel/manganese dioxide combined electrode material with multi-level structure, and preparation method thereof
CN105845455A (en) * 2016-05-10 2016-08-10 复旦大学 Polyacrylonitrile nanometer fiber/polyimide-based composite carbon aerogel electrode material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110838412A (en) * 2018-06-20 2020-02-25 苏州大学 Aramid fiber electrochemical capacitor
CN110838412B (en) * 2018-06-20 2021-06-18 苏州大学 Aramid fiber electrochemical capacitor

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