CN107026027B - A kind of preparation method of the electrode material of supercapacitor - Google Patents
A kind of preparation method of the electrode material of supercapacitor Download PDFInfo
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- CN107026027B CN107026027B CN201710229104.3A CN201710229104A CN107026027B CN 107026027 B CN107026027 B CN 107026027B CN 201710229104 A CN201710229104 A CN 201710229104A CN 107026027 B CN107026027 B CN 107026027B
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- dimethyl sulfoxide
- potassium hydroxide
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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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
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Abstract
The present invention provides a kind of preparation methods of the electrode material of supercapacitor, Fanglun 1414 is stirred together in dimethyl sulfoxide with potassium hydroxide to the dimethyl sulfoxide dispersion liquid for being completely dissolved to obtain Kevlar nanofiber, add acetic acid manganese solution, it stirs evenly, obtain cotton-shaped dispersion solution, freeze drier freeze-drying is put into after being filtered by vacuum, material, which is finally put into high-temperature calcination in tube furnace, can be obtained electrode material for super capacitor.The electrochemical performance of the electrode material obtained by means of the present invention, possess higher specific capacitance, and the performance of fast charge slow play is presented during constant current charge-discharge under larger current density, great business promotion value possesses preferable development prospect in following energy storage field.
Description
Technical field
The invention belongs to electricity fields, are related to a kind of electrode material, specifically a kind of electrode material of supercapacitor
The preparation method of material.
Background technique
Supercapacitor (EDLC) is called double layer capacitor, as a kind of new between traditional capacitor and battery
Type has become the hot spot of people's concern and research without maintenance energy storage device now.Its specific power is 10 times of battery or more,
The ability for storing charge is higher than ordinary capacitor, and there is lot of advantages to enter operating temperature range is wide, can be quickly charged and discharged
And it has extended cycle life, pollution-free zero-emission etc..And electrode material the improvement of the performance of supercapacitor is played it is very important
Effect, it may be said that be the part of supercapacitor core the most, therefore developing the electrode material with excellent properties is super electricity
The most key project in container research.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation method of the electrode material of supercapacitor, described is this super
The preparation method of the electrode material of capacitor to solve supercapacitor specific capacity in the prior art is high, chemical property not
Strong technical problem.
The present invention provides a kind of preparation methods of the electrode material of supercapacitor, comprising 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) Kafra fiber and potassium hydroxide are poured into dimethylsulfoxide solvent and stirs 72 ~ 240 hours to Kafra fiber
It is completely dissolved, obtains the dimethyl sulfoxide dispersion liquid of Kevlar nanofiber, Kafra fiber, potassium hydroxide and dimethylsulfoxide solvent
Material ratio be 0.1 ~ 2 gram: 1.0 ~ 3.0 gram: 500 ~ 2000 milliliters；
4) by the dimethyl sulfoxide dispersion liquid of acetic acid manganese solution and above-mentioned Kevlar nanofiber that concentration is 1 ~ 5 mg/mL
The volume ratio of the dimethyl sulfoxide dispersion liquid of mixing, the acetic acid manganese solution and Kevlar nanofiber is 100 ~ 200 milliliters:
100 ~ 200 milliliters, stirring 1 ~ 5 hour uniformly mixed to dispersion liquid；
5) the cotton-shaped dispersing liquid for mixing step 4), vacuum filtration, and with deionized water by its potassium ion wash clean
Solid is taken later；
6) after the solid for obtaining step 5) is put into freeze drier drying 72 ~ 120 hours, under nitrogen protection, 600 ~
900 degrees Celsius of lower high-temperature calcination carbonizations, take out carbonized solid and pulverize；
7) dusty material that step 6) obtains, acetylene black, Kynoar are mixed in mass ratio for 50-99:1-49:1-49
It closes, can be used as electrode material for super capacitor after grinding uniformly.
Further, the mass ratio of the Kafra fiber and potassium hydroxide is between 1:1 ~ 1:5.
Further, the concentration for the acetic acid manganese solution matched is in 2mg/mL.
Further, the solid of step 5) vacuum filtration is needed through freeze-drying 24 hours ~ 72 hours.
Further, step 6) high-temperature calcination must under nitrogen protection, temperature at 600 ~ 900 degree, and keep the temperature 3 hours with
On, heating rate is at 2 ~ 10 degrees/min.
Further, in step 7), Kynoar is dissolved in N-Methyl pyrrolidone before the milling.
The present invention is inner with hydrogen in dimethyl sulfoxide (DMSO) by poly(p-phenylene terephthalamide) (Kafra fiber) fiber
Potassium oxide (KOH) is stirred together to the dimethyl sulfoxide dispersion liquid for being completely dissolved to obtain Kevlar nanofiber.Add manganese acetate
Solution stirs evenly, and obtains cotton-shaped dispersion solution.Freeze drier freeze-drying is put into after being filtered by vacuum.Finally material is put
Entering high-temperature calcination in tube furnace can be obtained electrode material for super capacitor.The electrode material obtained by means of the present invention
Electrochemical performance possesses higher specific capacitance, and presents during constant current charge-discharge under larger current density fast
Fill the performance of slow play.
The present invention has good chemical stabilization using the electrode material that Kafra fiber prepares nano-scale fiber reticular structure
Property, be doped with after manganese and add fake capacitance effect, its chemical property can be greatly improved.Electrode material synthesis of the invention
Simply cost is relatively low for process, and in aqueous electrolyte, and the specific discharge capacity under 1 A/g current density is in 510 ~ 820 F/g models
It encloses.
Compared with prior art, the present invention its technological progress is significant.Electrode material for super capacitor of the invention is gathered around
There are electric double layer capacitance effect and fake capacitance effect, so electrode material possesses biggish chemical property, provides specific capacity, and
And synthetic method of the invention is simple, the nano-scale fiber reticular structure prepared, possesses preferable electric double layer effect, it is great
Business promotion value possesses preferable development prospect in following energy storage field.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of the electrode material of embodiment 1.
Fig. 2 is the transmission electron microscope picture of 1 electrode material of embodiment.
Fig. 3 is constant current charge-discharge curve of 1 electrode material of embodiment under different current densities.
Fig. 4 is 1 electrode material of embodiment in the different cyclic voltammetry curves swept under speed.
Fig. 5 is the obtained electrode material XRD diagram after different carburizing temperatures of embodiment 1.
Specific 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 fiber is cut into 1cm or so length, is put into 500mLDMSO, then weigh
1.5023gKOH, grind into powder pour 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.
It prepares the acetic acid manganese solution that concentration is 2mg/mL to pour into the ANFS solution of 200mL, mechanical stirring 10h is to molten immediately
Liquid is in uniformly mixed cotton-shaped gel solution.
Cotton-shaped gel solution is filtered by vacuum using the filter paper of 22nm, and carries out filtering and washing with the deionized water of 0.5L ~ 1L.
The membranaceous solid for filtering and obtaining is collected, the heating speed being put into tube furnace according to 5 DEG C/min after freeze-drying is passed through
Rate to 700 DEG C (600,800 DEG C) keep the temperature 3 hours.Carbonized solid is taken out, grind into powder obtains 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 are dissolved in advance
In 1- methyl pyrrolidone) ratio be added together grinding, be coated in titanium net after half an hour, it is dry after 4M KOH electricity
It is tested in solution liquid.
Embodiment 2
A kind of electrode material for super capacitor ANFS/Mn2+Preparation method.
1.005g Kafra fiber is cut into 1cm or so length, is put into 500mLDMSO, then weigh 1.5072gKOH,
Grind into powder pours 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.
It prepares the acetic acid manganese solution that concentration is 2mg/mL to pour into the ANFS solution of 200mL, mechanical stirring 10h is to molten immediately
Liquid is in uniformly mixed cotton-shaped gel solution.
Cotton-shaped gel solution is filtered by vacuum using the filter paper of 22nm, and carries out filtering and washing with the deionized water of 0.5L ~ 1L.
The membranaceous solid for filtering and obtaining is collected, the heating speed being put into tube furnace according to 5 DEG C/min after freeze-drying is passed through
Rate to 800 DEG C keep the temperature 3 hours.Carbonized solid is taken out, grind into powder obtains electrode material for super capacitor.
By the electrode material of preparation according to electrode material: acetylene black: PVDF=8:1:1(mass ratio, PVDF are dissolved in advance
In 1- methyl pyrrolidone) ratio be added together grinding, be coated in titanium net after half an hour, it is dry after 4M KOH electricity
It is tested in solution liquid.
Embodiment 3
A kind of electrode material for super capacitor ANFS/Mn2+Preparation method.
2.0137g Kafra fiber is cut into 1cm or so length, is put into 500mLDMSO, then weigh
1.5001gKOH, grind into powder pour 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.
It prepares the acetic acid manganese solution that concentration is 4mg/mL to pour into the ANFS solution of 200mL, mechanical stirring 10h is to molten immediately
Liquid is in uniformly mixed cotton-shaped gel solution.
Cotton-shaped gel solution is filtered by vacuum using the filter paper of 22nm, and carries out filtering and washing with the deionized water of 0.5L ~ 1L.
The membranaceous solid for filtering and obtaining is collected, the heating speed being put into tube furnace according to 5 DEG C/min after freeze-drying is passed through
Rate to 900 DEG C keep the temperature 3 hours.Carbonized solid is taken out, grind into powder obtains electrode material for super capacitor
The electrode material that above three example finally obtains is as supercapacitor active material, according to active material: acetylene
Black: PVDF=8:1:1(mass ratio, PVDF are dissolved in advance in 1- methyl pyrrolidone) ratio be added together grinding, half
It is coated in nickel foam after hour, is tested in the electrolyte of 4M KOH after dry.Its constant current under different current densities is filled
Discharge curve is as shown in figure 3, utilize calculation formulaWithThe composite material can be calculated in formula
Specific capacity be 510 ~ 820F/g.
While specific embodiments of the present invention have been shown and described, however for a person skilled in the art,
It is understood that a variety of to the progress of these embodiments can change without departing from the principles and spirit of the present invention, replace,
Modification and modification, the range invented are defined by the appended claims and the equivalents thereof.
Claims (3)
1. a kind of preparation method of the electrode material of supercapacitor, it is characterised in that the following steps are included:
1) Kafra fiber is cut into the short-term of 0.1~20 centimeter length；
2) potassium hydroxide is weighed, is pulverized；
3) Kafra fiber and potassium hydroxide are poured into dimethylsulfoxide solvent stir 72~240 hours it is complete to Kafra fiber
Dissolution, obtains the dimethyl sulfoxide dispersion liquid of Kevlar nanofiber, the object of Kafra fiber, potassium hydroxide and dimethylsulfoxide solvent
Material is than being 0.1~2 gram: 1.0~3.0 gram: 500~2000 milliliters；
4) the dimethyl sulfoxide dispersion liquid of acetic acid manganese solution and above-mentioned Kevlar nanofiber that concentration is 1~5mg/mL is mixed
It closes, the volume ratio of the dimethyl sulfoxide dispersion liquid of the acetic acid manganese solution and Kevlar nanofiber is 100~200 milliliters: 100
~200 milliliters, stirring 1~5 hour uniformly mixed to dispersion liquid；
5) the cotton-shaped dispersing liquid for mixing step 4), vacuum filtration, and will be after its potassium ion wash clean with deionized water
Take out solid；
6) after the solid for obtaining step 5) is put into freeze drier drying 72~120 hours, under nitrogen protection, 600~900
Degree Celsius lower high-temperature calcination is carbonized and keeps the temperature 3 hours or more, and heating rate is taken out carbonized solid and be ground at 2~10 degrees/min
Powder；
It 7) is in mass ratio that 50-99:1-49:1-49 is mixed by dusty material that step 6) obtains, acetylene black, Kynoar,
Kynoar is dissolved in N-Methyl pyrrolidone before the milling, can be used as electrode of super capacitor material after grinding uniformly
Material.
2. a kind of preparation method of the electrode material of supercapacitor according to claim 1, it is characterised in that: Kevlar
The mass ratio of fiber and potassium hydroxide is between 1:1~1:5.
3. a kind of preparation method of the electrode material of supercapacitor according to claim 1, it is characterised in that: matched
The concentration of acetic acid manganese solution is in 2mg/mL.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0972292B1 (en) * | 1996-05-15 | 2008-12-31 | Hyperion Catalysis International, Inc. | Graphitic nanofibers in electrochemical capacitors |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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