CN107170590A - 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 PDFInfo
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- CN107170590A CN107170590A CN201710350414.0A CN201710350414A CN107170590A CN 107170590 A CN107170590 A CN 107170590A CN 201710350414 A CN201710350414 A CN 201710350414A CN 107170590 A CN107170590 A CN 107170590A
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- electrode material
- super capacitor
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- formaldehyde
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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
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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
- H01G11/24—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
- H01G11/38—Carbon pastes or blends; Binders or additives therein
-
- 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 electrode material for super capacitor and preparation method thereof.The electrode material is composited by graphite oxide surface deposition thiocarbamide urea formaldehyde base carbon material.Preparation technology is mainly：Graphite oxide is prepared by Hummers methods（GO）, purify, prepare the GO solution of various concentrations；Appropriate thiocarbamide is dissolved in a water bath, and continued mechanical stirring adds appropriate dense HCl and formaldehyde, after reaction, suction filtration, washed product after freeze-drying, obtain thiocarbamide urea formaldehyde/GO composites；Carbonization treatment, obtains thiocarbamide urea formaldehyde base carbon graphite alkene composite, as electrode material for super capacitor.The electrode material for super capacitor that the present invention is prepared has the advantages that Stability Analysis of Structures, specific capacitance value be high, good cycle, the great application potential in electrode material for super capacitor, and preparation technology is simple, easily operation, cost is low, efficiency high the advantages of.
Description
Technical field
The invention belongs to new energy technical field of electronic materials, it is related to a kind of electrode material for super capacitor and its preparation side
Method.
Background technology
Twice since the industrial revolution, we recognize that the development of the mankind and energy revolution are closely bound up.Industry is removed from office for the first time
Hit, a large amount of burning coals of people drive steam engine to promote social development；In second industrial revolution, people's Devoting Major Efforts To Developing fossil
Resource, starts internal combustion engine, by various forms of energy conversions is electric energy and are used.Electric energy is using most square in the modern life
Just, most widely used form of energy.But, how efficiently to store electric energy is the problem of researcher constantly inquires into all the time.It is super
Level capacitor is that grow up in recent ten years a kind of combines traditional capacitor and the novel energy-storing of secondary cell advantage is set
Standby, high with power density, charge/discharge rates are fast, and high-low temperature resistant has extended cycle life, the advantages of non-environmental-pollution, cause a large amount of
The sight of researcher, is with a wide range of applications.
According to the energy storage mechnism of electrode material, ultracapacitor can be divided into double electric layers supercapacitor and the super electricity of fake capacitance
Two kinds of container（Lokhande V.C, Lokhande A.C, Lokhande C.D, Jin Hyeok Kim, Taeksoo Ji.
Journal of Alloys and Compounds, Supercapacitive composite metal oxide
Electrodes formed withcarbon, metal oxides and conducting polymers, 2016,682,
381-403）.Wherein, the electrode material of double electric layers supercapacitor is typically the carbon material with high-specific surface area.Common carbon
Material has graphene, CNT, activated carbon, mesoporous carbon etc..And some natural polymers, artificial-synthetic copolymer etc. is through too high
Temperature carbonization can obtain the carbon material with special construction or functional group.Wherein, graphene is with sp by carbon atom2The form of hydridization
The cellular individual layer carbon material formed.Because it has outstanding electro transfer performance, high-specific surface area, energy gap controllable and excellent
Pliability, so the application in electrode material for super capacitor is widely.But the electrode material ratio of graphene composition
Electric capacity is low, it is difficult to be used alone.Resin base carbon material is a kind of using macromolecule resin material as presoma, by high temperature cabonization
The material obtained afterwards.Compared to other carbon materials, resin base carbon material needs not move through Heteroatom doping process just can be in material
The hetero atoms such as N, S are obtained on strand, and these hetero atoms can improve the wetability and chemical property of material.And resin base
The problem of carbon material usually occurs scattered uneven in preparation process, influences its application in ultracapacitor.By inciting somebody to action
Graphene is compounded to form a kind of new composite with resin base carbon material, can improve the defect of two kinds of materials, be suitable as
Electrode material for super capacitor.Song et al. by solvent evaporation method and self assembly made a kind of mesoporous carbon of multilayer order/
Graphene composite material, obtained composite has extraordinary capacitive property and cycle performance（Song Yanjie, Li
Zhu, Guo Kunkun, Shao Ting. Nanoscale, Hierarchically ordered mesoporous
Carbon/graphene composites as supercapacitor electrode materials, 2016,8,
15671-15680）.This kind of material tests its specific capacitance value when current density is 0.5A/g in 6mol/L KOH electrolyte
329.5F/g, and in the specific capacitance retention rate still after 5000 times circulate with 96%.Song etc. is by a kind of triblock copolymer
Thing has synthesized a kind of new graphene/N doping meso-porous nano carbon material directly from being assembled on graphite oxide, it is in electric current
Specific capacitance value when density is 0.2A/g is 377F/g, and result of study confirms that this kind of composite has high-specific surface area and good
Electron conduction so that its high rate performance and cycle performance have obtained improvement by a relatively large margin（Song Yanfang,
Yang Jun, Wang Ke, Xia Yongyao. Carbon, In-situ synthesis of graphene/
nitrogen-doped ordered mesoporous carbon nanosheet for supercapacitor
Application, 2016,96,955-964）.
Chinese patent literature CN103456520A disclose a kind of graphene/carbon nanotube composite film preparation method and
It is applied, and is comprised the steps of：（1）Expanded graphite/CNT and solvent are mixed, mixture is obtained, wherein, expanded graphite with
The mass ratio of CNT is 1:1~5:1, the mass percent of solvent in the mixture is 30~50%；（2）To the mixture
Ball milling is carried out, the compound of graphene/carbon nano-tube is obtained；（3）Added into the compound of the graphene/carbon nano-tube molten
Agent, obtains graphene/carbon nano-tube compound suspension, wherein, the concentration of the compound of graphene/carbon nano-tube for 0.25~
5mg/mL；（4）By graphene/carbon nano-tube suspension filtering, obtained filter cake heats 1~2h at 150 DEG C~200 DEG C,
Obtain the graphene/carbon nanotube composite film.But this method complex process, complex steps, raw materials used cost is high, it is difficult to
Widespread adoption.
The content of the invention
In view of the shortcomings of the prior art, it is super that the present invention provides that a kind of process is simple, efficiency high, electrochemical stability are good
Capacitor electrode material and preparation method thereof.
Technical scheme is as follows：
A kind of electrode material for super capacitor, the electrode material is combined by graphite oxide surface deposition thiocarbamide urea formaldehyde base carbon material
Form.
According to the present invention, a kind of preparation method of electrode material for super capacitor, including step are as follows：
（1）Using expanded graphite as base stock, graphite oxide is prepared using Hummers methods（GO）, be dispersed in from
In sub- water, concentration is 1.0~5.0g/L, and ultrasonically treated 2h obtains uniform GO solution；
（2）Take step（1）In GO solution 100mL, add thiocarbamide, ultrasonic dissolution, and the mechanical agitation in 40~80 DEG C of water-baths
30min, then adds the dense HCl and 6mL formaldehyde of 0.2~0.5mL, persistently 2~8h of stirring reaction, and the mol ratio of thiocarbamide and formaldehyde is
0.5:1~5:1；
（3）By step（2）Obtained reaction solution obtains frivolous powdered answer after carrying out suction filtration, washing, 12~48h of freeze-drying
Condensation material；
（4）By step（3）Obtained composite, in 600~850 DEG C of 2~5h of carbonization, obtains thiocarbamide aldehyde tree under argon gas protection
Aliphatic radical carbon graphite alkene composite.
, according to the invention it is preferred to, step（1）In take GO solution concentration be 2.0g/L.
, according to the invention it is preferred to, step（2）Middle bath temperature is 55 DEG C.
, according to the invention it is preferred to, step（2）In dense HCl consumption be 0.4mL.
, according to the invention it is preferred to, step（2）The middle reaction time is 3h.
, according to the invention it is preferred to, step（2）The mol ratio of middle thiocarbamide and formaldehyde is 3:1.
, according to the invention it is preferred to, step（3）Middle sublimation drying is 24h.
, according to the invention it is preferred to, step（4）Middle carburizing temperature is 750 DEG C.
, according to the invention it is preferred to, step（4）Middle carbonization time is 3h.
The technical advantage of the present invention is as follows：
(1) preparation technology of the present invention is simple, easily operation, cost is low, efficiency high the advantages of；
(2) the thiocarbamide urea formaldehyde base carbon graphite alkene composite that the present invention is prepared has Stability Analysis of Structures, chemical property steady
Calmly, the advantages of good wetability, electrochemical performance, good cycle, high specific capacitance, being highly suitable as electrode material should
For ultracapacitor field.
Brief description of the drawings
Fig. 1 is the transmission electron microscope picture of thiocarbamide urea formaldehyde base carbon graphite alkene composite made from the embodiment of the present invention 4.
Fig. 2 is the cycle performance curve of thiocarbamide urea formaldehyde base carbon graphite alkene composite made from the embodiment of the present invention 4
Figure.
Fig. 3 is thiocarbamide urea formaldehyde base carbon graphite alkene composite made from the embodiment of the present invention 4 under different current densities
Charge and discharge electrograph.
Embodiment
With reference to specific embodiments and the drawings, the present invention is described further, but not limited to this.
Experimental method described in following embodiments, is conventional method unless otherwise specified simultaneously；The reagent and material
Material, unless otherwise specified, is commercially obtained.
Embodiment 1：
Using expanded graphite as base stock, graphite oxide is prepared using Hummers methods（GO）, it is dispersed in deionized water
In, concentration is 1.0g/L, and ultrasonically treated 2h obtains uniform GO solution；The GO solution 100mL obtained, add thiocarbamide, ultrasound
Dissolving, and the mechanical agitation 30min in 40 DEG C of water-baths, then add the dense HCl and 6mL formaldehyde of 0.3mL, continue stirring reaction 2h,
The mol ratio of thiocarbamide and formaldehyde is 1:1；After reaction terminates, obtained reaction solution is obtained after carrying out suction filtration, washing, freeze-drying 24h
To frivolous powdered composite；By obtained composite argon gas protection under in 800 DEG C be carbonized 2h, obtain thiocarbamide aldehyde tree
Aliphatic radical carbon graphite alkene composite；
Using three-electrode system, using the 6mol/L KOH aqueous solution as electrolyte, specific capacitance is measured for 167.5F/g, thiocarbamide urea formaldehyde
The stability of base carbon graphite alkene composite is preferable.
Embodiment 2：
Using expanded graphite as base stock, graphite oxide is prepared using Hummers methods（GO）, it is dispersed in deionized water
In, concentration is 3.0g/L, and ultrasonically treated 2h obtains uniform GO solution；The GO solution 100mL obtained, add thiocarbamide, ultrasound
Dissolving, and the mechanical agitation 30min in 60 DEG C of water-baths, then add the dense HCl and 6mL formaldehyde of 0.2mL, continue stirring reaction 4h,
The mol ratio of thiocarbamide and formaldehyde is 0.5:1；After reaction terminates, obtained reaction solution is carried out after suction filtration, washing, freeze-drying 12h
Obtain frivolous powdered composite；By obtained composite argon gas protection under in 850 DEG C be carbonized 3h, obtain thiocarbamide aldehyde
Resin base carbon graphite alkene composite；
Using three-electrode system, using the 6mol/L KOH aqueous solution as electrolyte, specific capacitance is measured for 214.2F/g, thiocarbamide urea formaldehyde
The stability of base carbon graphite alkene composite is preferable.
Embodiment 3：
Using expanded graphite as base stock, graphite oxide is prepared using Hummers methods（GO）, it is dispersed in deionized water
In, concentration is 5.0g/L, and ultrasonically treated 2h obtains uniform GO solution；The GO solution 100mL obtained, add thiocarbamide, ultrasound
Dissolving, and the mechanical agitation 30min in 80 DEG C of water-baths, then add the dense HCl and 6mL formaldehyde of 0.5mL, continue stirring reaction 8h,
The mol ratio of thiocarbamide and formaldehyde is 2:1；After reaction terminates, obtained reaction solution is obtained after carrying out suction filtration, washing, freeze-drying 48h
To frivolous powdered composite；By obtained composite argon gas protection under in 600 DEG C be carbonized 5h, obtain thiocarbamide aldehyde tree
Aliphatic radical carbon graphite alkene composite；
Using three-electrode system, using the 6mol/L KOH aqueous solution as electrolyte, specific capacitance is measured for 298F/g, thiocarbamide urea formaldehyde base
The stability of carbon graphite alkene composite is preferable.
Embodiment 4：
Using expanded graphite as base stock, graphite oxide is prepared using Hummers methods（GO）, it is dispersed in deionized water
In, concentration is 2.0g/L, and ultrasonically treated 2h obtains uniform GO solution；The GO solution 100mL obtained, add thiocarbamide, ultrasound
Dissolving, and the mechanical agitation 30min in 55 DEG C of water-baths, then add the dense HCl and 6mL formaldehyde of 0.4mL, continue stirring reaction 3h,
The mol ratio of thiocarbamide and formaldehyde is 3:1；After reaction terminates, obtained reaction solution is obtained after carrying out suction filtration, washing, freeze-drying 24h
To frivolous powdered composite；By obtained composite argon gas protection under in 750 DEG C be carbonized 3h, obtain thiocarbamide aldehyde tree
Aliphatic radical carbon graphite alkene composite；
Using three-electrode system, using the 6mol/L KOH aqueous solution as electrolyte, specific capacitance is measured for 355F/g, thiocarbamide urea formaldehyde base
The stability of carbon graphite alkene composite is preferable；
The transmission electron microscope picture of thiocarbamide urea formaldehyde base carbon graphite alkene composite is as shown in figure 1, can by Fig. 1 made from the present embodiment
Know, the thiocarbamide urea formaldehyde base carbon material deposition of preparation shows stable 3-D solid structure in the graphenic surface of fold.Should
Structure provides larger specific surface area, is conducive to being completely immersed in for electrolyte, promotes the quick biography of electrolyte intermediate ion and electric charge
It is defeated；
The cycle performance curve map of thiocarbamide urea formaldehyde base carbon graphite alkene composite is as shown in Fig. 2 by scheming made from the present embodiment
2 understand, stable circulation of the thiocarbamide urea formaldehyde base carbon graphite alkene composite in 10A/g after 5000 cycles of cycle charge-discharge
Property preferably, its specific capacitance circulate 5000 cycles after still be its initial specific capacitance 90.97%；
The constant current charge-discharge curve of the thiocarbamide urea formaldehyde base carbon graphite alkene composite of preparation as shown in figure 3, from the figure 3, it may be seen that
Thiocarbamide urea formaldehyde base carbon graphite alkene composite has good charge-discharge characteristic, the specific capacitance under 1A/g current density
It is worth for 355 F/g, specific capacitance is higher.
Embodiment 5：
Using expanded graphite as base stock, graphite oxide is prepared using Hummers methods（GO）, it is dispersed in deionized water
In, concentration is 4.0g/L, and ultrasonically treated 2h obtains uniform GO solution；The GO solution 100mL obtained, add thiocarbamide, ultrasound
Dissolving, and the mechanical agitation 30min in 75 DEG C of water-baths, then add the dense HCl and 6mL formaldehyde of 0.3mL, continue stirring reaction 6h,
The mol ratio of thiocarbamide and formaldehyde is 5:1；After reaction terminates, obtained reaction solution is obtained after carrying out suction filtration, washing, freeze-drying 48h
To frivolous powdered composite；By obtained composite argon gas protection under in 650 DEG C be carbonized 4h, obtain thiocarbamide aldehyde tree
Aliphatic radical carbon graphite alkene composite；
Using three-electrode system, using the 6mol/L KOH aqueous solution as electrolyte, specific capacitance is measured for 265F/g, thiocarbamide urea formaldehyde base
The stability of carbon graphite alkene composite is preferable.
Claims (11)
1. a kind of electrode material for super capacitor, it is characterised in that the electrode material deposits thiocarbamide urea formaldehyde by graphenic surface
Base carbon material is composited.
2. a kind of preparation method of the electrode material for super capacitor described in claim 1, including step are as follows：
（1）Using expanded graphite as base stock, graphite oxide is prepared using Hummers methods（GO）, be dispersed in from
In sub- water, concentration is 1.0~5.0g/L, and ultrasonically treated 2h obtains uniform GO solution；
（2）Take step（1）In GO solution 100mL, add thiocarbamide, ultrasonic dissolution, and the mechanical agitation in 40~80 DEG C of water-baths
30min, then adds the dense HCl and 6mL formaldehyde of 0.2~0.5mL, persistently 2~8h of stirring reaction, and the mol ratio of thiocarbamide and formaldehyde is
0.5:1~5:1；
（3）By step（2）Obtained reaction solution obtains frivolous powdered answer after carrying out suction filtration, washing, 12~48h of freeze-drying
Condensation material；
（4）By step（3）Obtained composite, in 600~850 DEG C of 2~5h of carbonization, obtains thiocarbamide aldehyde tree under argon gas protection
Aliphatic radical carbon graphite alkene composite.
3. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（1）In take
The concentration of GO solution is 2.0g/L.
4. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（2）Reclaimed water
Bath temperature is 55 DEG C.
5. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（2）In it is dense
HCl consumption is 0.4mL.
6. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（2）In it is anti-
It is 3h between seasonable.
7. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（2）Middle sulphur
The mol ratio of urea and formaldehyde is 3:1.
8. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（3）In it is cold
Jelly drying time is 24h.
9. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（4）Middle carbon
It is 750 DEG C to change temperature.
10. the preparation method of electrode material for super capacitor according to claim 2, it is characterised in that step（4）Middle carbon
The change time is 3h.
11. a kind of application of thiocarbamide urea formaldehyde base carbon graphite alkene composite, the electrode material for ultracapacitor.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110415992A (en) * | 2019-07-31 | 2019-11-05 | 上海应用技术大学 | A kind of nitrogen of porous structure, sulfur doping carbon material preparation method and applications |
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Application publication date: 20170915 |