CN104795248A - Electrode material of catkin super capacitor and preparation method thereof and super capacitor - Google Patents
Electrode material of catkin super capacitor and preparation method thereof and super capacitor Download PDFInfo
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- CN104795248A CN104795248A CN201510224032.4A CN201510224032A CN104795248A CN 104795248 A CN104795248 A CN 104795248A CN 201510224032 A CN201510224032 A CN 201510224032A CN 104795248 A CN104795248 A CN 104795248A
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- catkin
- electrode
- electrode material
- super capacitor
- carbonization
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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
- 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 provides an electrode material of a catkin super capacitor and a preparation method thereof and the super capacitor. The preparation method includes: firstly, blending catkin and potassium hydroxide and increasing the temperature to 400 DEG C at a heating rate of 5 DEG C per minute, and keeping 400 DEG C for one or two hours; secondly, increasing the temperature to 850 DEG C at a heating rate of 10 DEG C per minute and keeping 850 DEG C for one or 2 hours; thirdly, obtaining porous carbide catkin electrode material; adding the porous carbide catkin to thiourea solution, intensively stirring for half an hour to one hour, then heating to evaporate moisture at the temperature between 80 DEG C and 90 DEG C; heating the obtained material to 800 DEG C at a heating rate of 10 DEG C per minute under the protection of argon, continuing heating for 2 to 3 hours, and then allowing natural cooling to obtain carbide catkin electrode material with nitrogen and sulphur. A novel carbon nano-sheet material with bigger surface area, a plurality of absorption activity points, two-dimensional cellular and simplicity of preparation is prepared. The electrode prepared with the novel carbon nano-sheet material has excellent capacitance performance.
Description
Technical field
What the present invention relates to is a kind of electrode material for super capacitor.That the present invention also relates to is a kind of preparation method of electrode material for super capacitor.
Background technology
Ultracapacitor is that one can not only utilize double electric layer capacitor to carry out energy storage, and the redox reaction of electrode/solution surface can be utilized to carry out the energy accumulating device of storage power, and it is also electrochemical capacitor or fake capacitance capacitor simultaneously.Ultracapacitor has can big current fast charging and discharging, cycle-index is many, can low-temperature operation, maintenance frequency is considerably less and have the advantages such as certain memory effect.Ultracapacitor can be divided into double electric layer capacitor, Faradic pseudo-capacitor and mixed capacitor according to energy storage mechnism difference.Ultracapacitor forward high-specific-power and high-energy-density development, the hybrid super capacitor being respectively both positive and negative polarity with transition metal oxide and porous charcoal is important development direction from now on.During discharge and recharge, electrochemical reaction energy conversion process and electric double layer energy storage process are carried out at the two poles of the earth simultaneous equal respectively.Electric double layer capacitance allows big current fast charging and discharging, and pseudo capacitance by Rapid reversible faraday reaction realize macro-energy store, both combine, combine ultracapacitor and battery two kinds of energy storage mechnism, be expected to realize two kinds of energy storage mode performance complements, obtain the performances such as high-energy-density, high power density, long circulation life, high working voltage.
The key factor affecting ultracapacitor development has the technology of preparing etc. of electrode material, the electrolyte mated with electrode material and electrode, and wherein electrode material is the key of restriction ultracapacitor.People mainly concentrate on porous carbon materials, conducting polymer materials and metal oxide materials three major types to the research of electrode material.For the carbon class material of the first kind as the material of ultracapacitor, main advantage is that specific area is high, and electronic impedance is little and cycle performance is high, and current research is mainly active carbon, the material with carbon element of the zero dimension such as mesoporous carbon and carbosphere degree; Carbon nano-fiber, the material with carbon element of the one dimensions such as carbon nano-tube; Graphene, the material with carbon element of the two dimension such as graphene oxide and redox graphene.The performance improving capacitor mainly improves its specific capacity, power density and energy density.This just requires that electrode material needs the conductive ion in enough large specific area and electrolyte can transmit fast in electrode material.For zero dimension material with carbon elements such as current active carbon and mesoporous carbon, although it has larger specific area, because pore size distribution$ is unreasonable and duct is inaccessible, cause high rate performance poor.And the one dimension such as carbon nano-tube and carbon fiber material with carbon element, although have higher conductivity, specific area is less, and it is few that available ion inhales deactivation point, and therefore its specific capacitance is restricted.And for studying more fiery Graphene and derivative material with carbon element at present, owing to having larger specific area and higher conductivity, the particularly planar structure of two dimension, contributes to the delivering path shortening ion, quite favored in capacitor research field.But, the complicated process of preparation of Graphene, and required experimental facilities requires high, is unfavorable for large-scale production.
Summary of the invention
An object of the present invention is to provide a kind of cheap, the catkin electrode material for super capacitor that energy density is high.Two of object of the present invention is to provide three of a kind of preparation method's object of the present invention of catkin electrode material for super capacitor to be to provide a kind of ultracapacitor containing catkin electrode.
Catkin electrode material for super capacitor of the present invention is 1:1 ~ 2 in mass ratio; catkin and potassium hydroxide are mixed; grind into powder; under argon shield; first be raised to 400 DEG C of lasting 1-2h with the heating rate of 5 DEG C/min; be raised to 850 DEG C of lasting 1-2h with the heating rate of 10 DEG C/min again, then naturally cool, the porous silicon carbide catkin electrode material obtained.
Catkin electrode material for super capacitor of the present invention can also be the ratio of 1:3 ~ 4 according to porous in the mass ratio of carbonization catkin and thiocarbamide, adds in thiourea solution, after strong agitation 0.5-1h, heat porous silicon carbide catkin moisture evaporate to dryness at 80-90 DEG C; By the material that obtains under argon shield, be raised to 800 DEG C with the programming rate of 10 DEG C/min, naturally cool after continuous heating 2-3h, the nitrogen sulfur doping carbonization catkin electrode material obtained.
The preparation method of catkin electrode material for super capacitor of the present invention is: be 1:1 ~ 2 in mass ratio; catkin and potassium hydroxide are mixed; grind into powder; under argon shield; first be raised to 400 DEG C of lasting 1-2h with the heating rate of 5 DEG C/min; be raised to 850 DEG C of lasting 1-2h with the heating rate of 10 DEG C/min again, then naturally cool, obtain porous silicon carbide catkin electrode material.
Catkin electrode material for super capacitor of the present invention obtains preparation method and can also comprise: be the ratio of 1:3 ~ 4 according to porous in the mass ratio of carbonization catkin and thiocarbamide, porous silicon carbide catkin is added in thiourea solution, after strong agitation 0.5-1h, heat moisture evaporate to dryness at 80-90 DEG C; By the material that obtains under argon shield, be raised to 800 DEG C with the programming rate of 10 DEG C/min, naturally cool after continuous heating 2-3h, obtain nitrogen sulfur doping carbonization catkin electrode material.
Ultracapacitor containing catkin electrode of the present invention is: using carbonization catkin be work electrode, platinum electrode for electrode, saturated calomel electrode as reference electrode, with 6mol L
-1kOH, 1molL
-1na
2sO
4or their mixture is electrolyte, form ultracapacitor.
Ultracapacitor containing catkin electrode of the present invention is: using nitrogen sulfur doping carbonization catkin be work electrode, platinum electrode for electrode, saturated calomel electrode as reference electrode, with 6mol L
-1kOH, 1molL
-1na
2sO
4or their mixture is electrolyte, form ultracapacitor.
The present invention is by carrying out simple carbonization to biomass catkin and carrying out nitrogen sulfur doping effectively, and having prepared one, to have specific area large simultaneously, and adsorption activity point is many, has two-dimentional porous, and the New Type of Carbon nanometer sheet material of the feature such as preparation technology is simple.The electrode prepared by this carbon nanosheet material shows splendid capacitive property.
Essence of the present invention is the electrode structure adopting ultracapacitor, replaces charcoal and RuO with nitrogen sulfur doping carbonization catkin
2deng the electrode material as ultracapacitor, in neutral electrolyte, carry out discharge and recharge, form the electrode of ultracapacitor, obtain super electrochemical capacitance.
The invention has the advantages that natural catkin is the tube of hollow, after KOH activation, carbonization and nitrogen sulfur doping, become that specific surface is large, pore size distribution$ rationally, activation point is many, has the nitrogen sulfur doping carbonization catkin electrode material of two-dimentional loose structure.Overcome the shortcoming that other material conductivity is poor, capacity is low.Nitrogen sulfur doping carbonization catkin electrode material, had both maintained the cyclical stability of carbon, had had again the height ratio capacity characteristic of fake capacitance concurrently.Utilize nitrogen sulfur doping carbonization catkin electrode as the electrode material of ultracapacitor, not only raw material rich reserves is easy to get, cheap, and super capacitor performance is high, large high rate performance number, stable cycle performance.
Embodiment
Illustrate below and the present invention is described in more detail.
Be 1:1 ~ 2 in mass ratio, 5g catkin and potassium hydroxide are mixed, grind into powder puts into tube furnace; under argon shield, first under 5 DEG C/min heating rate, be raised to 400 DEG C of lasting 1-2h, 10 DEG C/min is warmed up to 850 DEG C afterwards; continue 1-2h, then naturally cool, obtain porous silicon carbide catkin.
Be the mass ratio of 1:3 ~ 4 by carbonization catkin and thiocarbamide, 0.1g porous silicon carbide catkin added in thiourea solution, after strong agitation 0.5-1h, then heats moisture evaporate to dryness at 80-90 DEG C; The material obtained is sent in tube furnace, under argon shield, is raised to 800 DEG C with the programming rate of 10 DEG C/min, naturally cool after continuous heating 2-3h, obtain nitrogen sulfur doping carbonization catkin electrode material.
With nitrogen sulfur doping carbonization catkin for work electrode, be platinum electrode to electrode, adopt saturated calomel electrode (SCE) as reference electrode, respectively with 6mol L
-1kOH and 1molL
-1na
2sO
4deng being electrolyte, test its chemical property.In addition, by carbonization catkin composite metal oxide, as MnO
2deng and composite conductive polymer, as PANI etc., in different voltage ranges, carry out cyclic voltammetric respectively, discharge and recharge, the test such as AC impedance and cycle life, obtain its chemical property.
1, with nitrogen sulfur doping carbonization catkin electrode material for work electrode, be platinum electrode to electrode, adopt saturated calomel electrode (SCE) as reference electrode, with 6molL
-1kOH be electrolyte, in-1 ~ 0V voltage range, with 1Ag
-1current density obtain 357Fg
-1capacity, 10000 capacity of circulating keep 98%.
2, directly with nitrogen sulfur doping carbonization catkin electrode material for work electrode, with 1molL
-1na
2sO
4for electrolyte, be assembled into symmetry capacitor, in 0 ~ 1.6V voltage range, with 5Ag
-1current density obtain 62Fg
-1capacity, 10000 capacity of circulating keep 97%.
3, directly with nitrogen sulfur doping carbonization catkin compound MnO
2electrode material is work electrode, with 1molL
-1na
2sO
4for electrolyte, in 0 ~ 1.0V voltage range, with 1Ag
-1current density obtain 268Fg
-1capacity, 5000 capacity of circulating keep 93%.
4, directly with nitrogen sulfur doping carbonization catkin compound PANI electrode material for work electrode, with 1molL
-1h
2sO
4for electrolyte, in 0 ~ 1.0V voltage range, with 0.5Ag
-1current density obtain 357Fg
-1capacity, 2000 capacity of circulating keep 94%.
Claims (6)
1. a catkin electrode material for super capacitor; it is characterized in that being 1:1 ~ 2 in mass ratio; catkin and potassium hydroxide are mixed; grind into powder; under argon shield, be first raised to 400 DEG C of lasting 1-2h with the heating rate of 5 DEG C/min, then be raised to 850 DEG C of lasting 1-2h with the heating rate of 10 DEG C/min; then naturally cool, the porous silicon carbide catkin electrode material obtained.
2. catkin electrode material for super capacitor according to claim 1, to it is characterized in that according to porous in the mass ratio of carbonization catkin and thiocarbamide being the ratio of 1:3 ~ 4, porous silicon carbide catkin is added in thiourea solution, after strong agitation 0.5-1h, heats moisture evaporate to dryness at 80-90 DEG C; By the material that obtains under argon shield, be raised to 800 DEG C with the programming rate of 10 DEG C/min, naturally cool after continuous heating 2-3h, the nitrogen sulfur doping carbonization catkin electrode material obtained.
3. the preparation method of a catkin electrode material for super capacitor; it is characterized in that: be 1:1 ~ 2 in mass ratio; catkin and potassium hydroxide are mixed; grind into powder; under argon shield, be first raised to 400 DEG C of lasting 1-2h with the heating rate of 5 DEG C/min, then be raised to 850 DEG C of lasting 1-2h with the heating rate of 10 DEG C/min; then naturally cool, obtain porous silicon carbide catkin electrode material.
4. catkin electrode material for super capacitor according to claim 3 obtains preparation method, it is characterized in that: be the ratio of 1:3 ~ 4 according to porous in the mass ratio of carbonization catkin and thiocarbamide, porous silicon carbide catkin is added in thiourea solution, after strong agitation 0.5-1h, heat moisture evaporate to dryness at 80-90 DEG C; By the material that obtains under argon shield, be raised to 800 DEG C with the programming rate of 10 DEG C/min, naturally cool after continuous heating 2-3h, obtain nitrogen sulfur doping carbonization catkin electrode material.
5. a ultracapacitor for the catkin electrode containing catkin electrode material for super capacitor described in claim 1, is characterized in that: using carbonization catkin be work electrode, platinum electrode for electrode, saturated calomel electrode as reference electrode, with 6mol L
-1kOH, 1molL
-1na
2sO
4or their mixture is electrolyte, form ultracapacitor.
6. a ultracapacitor for the catkin electrode containing catkin electrode material for super capacitor described in claim 2, is characterized in that: using nitrogen sulfur doping carbonization catkin be work electrode, platinum electrode for electrode, saturated calomel electrode as reference electrode, with 6molL
-1kOH, 1molL
-1na
2sO
4or their mixture is electrolyte, form ultracapacitor.
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| CN201510224032.4A CN104795248B (en) | 2015-05-05 | 2015-05-05 | A kind of catkin electrode material for super capacitor and preparation method and ultracapacitor |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105140050A (en) * | 2015-08-20 | 2015-12-09 | 西安岳达植物科技有限公司 | Preparation method for nitrogen sulfur doped wormlike graphite supercapacitor electrode material |
| CN105788885A (en) * | 2016-03-09 | 2016-07-20 | 湘潭大学 | Process for preparing camellia petal based sulfur and nitrogen co-doping draped nanosheet by explosion method and fabrication method of supercapacitor electrode |
| CN106744947A (en) * | 2017-01-16 | 2017-05-31 | 东华大学 | A kind of preparation method of bio-based nitrogen sulfur doping carbon material |
| CN106904606A (en) * | 2017-03-20 | 2017-06-30 | 中国石油大学(北京) | A kind of preparation method and its obtained doping carbon material of the carbon material that adulterates |
| CN107298441A (en) * | 2016-12-21 | 2017-10-27 | 北京化工大学 | A kind of method that use waste biomass material prepares super capacitor material |
| CN109607508A (en) * | 2018-12-29 | 2019-04-12 | 南京工程学院 | A kind of preparation method of electrode material for super capacitor |
| CN109994319A (en) * | 2019-04-11 | 2019-07-09 | 合肥工业大学 | The biomass derived carbon material and its synthetic method of a kind of nitrogen sulphur codope and application |
| CN111115629A (en) * | 2019-12-27 | 2020-05-08 | 暨南大学 | High-specific-surface-area carbon material based on waste tobacco stems and preparation method and application thereof |
| CN111186838A (en) * | 2020-01-07 | 2020-05-22 | 西安理工大学 | Preparation method and application of biomass-based electrode material |
| CN111341567A (en) * | 2020-03-02 | 2020-06-26 | 齐鲁工业大学 | 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and preparation method thereof |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105140050A (en) * | 2015-08-20 | 2015-12-09 | 西安岳达植物科技有限公司 | Preparation method for nitrogen sulfur doped wormlike graphite supercapacitor electrode material |
| CN105788885A (en) * | 2016-03-09 | 2016-07-20 | 湘潭大学 | Process for preparing camellia petal based sulfur and nitrogen co-doping draped nanosheet by explosion method and fabrication method of supercapacitor electrode |
| CN107298441A (en) * | 2016-12-21 | 2017-10-27 | 北京化工大学 | A kind of method that use waste biomass material prepares super capacitor material |
| CN106744947A (en) * | 2017-01-16 | 2017-05-31 | 东华大学 | A kind of preparation method of bio-based nitrogen sulfur doping carbon material |
| CN106904606A (en) * | 2017-03-20 | 2017-06-30 | 中国石油大学(北京) | A kind of preparation method and its obtained doping carbon material of the carbon material that adulterates |
| CN109607508A (en) * | 2018-12-29 | 2019-04-12 | 南京工程学院 | A kind of preparation method of electrode material for super capacitor |
| CN109994319A (en) * | 2019-04-11 | 2019-07-09 | 合肥工业大学 | The biomass derived carbon material and its synthetic method of a kind of nitrogen sulphur codope and application |
| CN111115629A (en) * | 2019-12-27 | 2020-05-08 | 暨南大学 | High-specific-surface-area carbon material based on waste tobacco stems and preparation method and application thereof |
| CN111186838A (en) * | 2020-01-07 | 2020-05-22 | 西安理工大学 | Preparation method and application of biomass-based electrode material |
| CN111341567A (en) * | 2020-03-02 | 2020-06-26 | 齐鲁工业大学 | 3D poplar catkin derived carbon-supported NiCo-LDH nanosheet supercapacitor and preparation method thereof |
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| Publication number | Publication date |
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| CN104795248B (en) | 2018-04-24 |
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Effective date of registration: 20220617 Address after: 158200 floor 5, national graphite product quality supervision and inspection center, No. 88, Kangxin Road, Jiguan District, Jixi City, Heilongjiang Province Patentee after: Heilongjiang hachang carbon material technology Co.,Ltd. Address before: 150001 Intellectual Property Office, Harbin Engineering University science and technology office, 145 Nantong Avenue, Nangang District, Harbin, Heilongjiang Patentee before: HARBIN ENGINEERING University |