CN108461304A - A kind of preparation method of combination electrode thin-film material - Google Patents
A kind of preparation method of combination electrode thin-film material Download PDFInfo
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- CN108461304A CN108461304A CN201810287539.8A CN201810287539A CN108461304A CN 108461304 A CN108461304 A CN 108461304A CN 201810287539 A CN201810287539 A CN 201810287539A CN 108461304 A CN108461304 A CN 108461304A
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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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
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Abstract
A kind of preparation method of combination electrode thin-film material, belongs to energy storage material technical field.The present invention is by selecting different volatile organic solvents and controlling heating process, conducting polymer monomer is made to be attached to activated carbon surface using the volatilization of organic solvent molecule, saturated pressure is adjusted by controlling temperature in the process, and then the thickness that can control conducting polymer monomer reaches molecular layer rank；Be subsequently placed in oxidizing gas environment and carry out chemical polymerization, oxidizing gas molecule induces monomer molecule to polymerize by way of colliding and polymerizeing in reaction process, to realize ultra-thin conductive polymer coating activated carbon surface controllable deposition.Ultra-thin conducting polymer is little in charge and discharge process deformation, overcomes the problem of the cyclical stability difference caused by deformation is excessive in its thermal energy storage process, improves the stability of composite material entirety；And the specific capacity and electric conductivity of electrode have been obviously improved it.
Description
Technical field
The invention belongs to energy storage material technical field, more particularly to a kind of preparation method of combination electrode thin-film material.
Background technology
Ultracapacitor becomes one of the hot spot of contemporary scientific research as new green environment protection energy storage device.Electrode material
Material is the core of ultracapacitor, determines the capacitive property, production cost and application field of ultracapacitor.Therefore, electrode
Material becomes research hotspot as the bottleneck for restricting ultracapacitor development.
Abundant structural material system at present including electric double layer behavior and fake capacitance behavior is continually developed out by people.It is double
The electrode material of capacity capacitor is based on carbon material, and carbon material is due to excellent electric conductivity, cyclical stability, wider
The advantages such as potential window, cheap price and simple preparation method have become the main electricity that commercialization ultracapacitor uses
Pole material.The specific capacitance that the energy storage mechanism of carbon material electric double layer capacitance itself can generate is relatively low.In order to improve carbon material
Specific capacitance, scientific research personnel does a lot of work, for example so that carbon material is had higher specific surface area by structure regulating, with profit
In the infiltration and absorption of electrolyte, carbon material electric double layer capacitance is improved.However merely increase the specific surface area of carbon material often
Along with the reduction of electric conductivity, and specific capacitance improve it is limited, it is difficult to significantly promoted ultracapacitor energy density and
Power density.And effectively combined practical carbon material with fake capacitance material, high performance electrode material is prepared with this
Material is the hot spot of current electrode material for super capacitor research.And how to realize effective modification of the fake capacitance material to carbon material,
To which the good synergistic effect of performance between the two is particularly significant, the pass for realizing this kind of composite material functionization is also become
Key.
The electrode material of fake capacitance capacitor includes conducting polymer and metal oxide.Fake capacitance material can be in electrode table
Underpotential deposition is carried out on two-dimentional or quasi- two-dimensional space in face or body phase, the chemical reaction of high reversible occurs, is generated and electric
The related capacitance of pole charging potential.Fake capacitance can generate not only in electrode surface in entire electrode interior, thus can get
Capacitance more higher than electric double layer capacitance and energy density.In the case of identical electrodes area, fake capacitance can be electric double layer
10~100 times of capacitance.And conducting polymer is managed because of its unique electrical conduction mechanism and physical chemistry so as to become
The electrode material thought improves the utilization rate of conducting polymer by regulating and controlling dopant, and the oxidation adulterated is adulterated/go also by promoting
Original reaction improves capacitance, has carbon material and the unrivaled advantage of metal oxide in terms of as electrode.But it studies
Personage is dedicated to improving electrode material component utilization rate, and the active primitive in bulk inner is made to be filled during fast charging and discharging
The raw redox reaction of distribution, then promotes its multiplying power property, while also having in face of conducting polymer as super capacitor
Serious problems existing for device electrode material.It is by redox since conducting polymer carries out electrochemical energy storage as electrode
Cheng Shixian, and the contraction and expansion of polymer backbone structure can occur in this course, that is, in charge and discharge process
Deformation is very big, specifically refers to the article that Luan Qiong is delivered《Unipolar pulse method prepares porous composite electrode and its fake capacitance performance is ground
Study carefully》Chapter 1,1.3.3 is saved.Therefore, the bigger conducting polymer of thickness, the stereomutation occurred in its thermal energy storage process are brighter
Aobvious, the stability for eventually resulting in the material entirety being combined is poor.Therefore, realizing that conducting polymer is effective to carbon material
While modification, the be combined cyclical stability of material of conducting polymer how to be overcome to become it as super capacitor electrode
The technical barrier of pole material.
Invention content
It is an object of the invention to：For in the prior art since conducting polymer cyclical stability is poor so that it is modified
Carbon material is formed by the not good enough problem of composite material stability, and the present invention provides a kind of preparation side of combination electrode thin-film material
Method.
To achieve the goals above, the present invention provides the following technical solutions：
A kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：Step A：It will be through surface
The activated carbon of activating agent processing is coated on substrate surface after being mixed with binder；
Step B：The substrate obtained through processing of step A is handled using surfactant；
Step C：Conducting polymer monomer is mixed in volatile organic solvent, uniform mixed solution is made；Step D：
The substrate obtained through step B processing is placed in mixed solution made from step C, the mixed solution is heated and makes organic solvent
Volatilization, so that conducting polymer monomer deposition is in activated carbon surface；
Step E：The substrate obtained through step D processing is placed in oxidizing gas and carries out chemical polymerization, it is final to make
Obtain the combination electrode thin-film material that conducting polymer and activated carbon are formed.
Further, surfactant is silane coupling agent in the step A and B.The effect of surfactant is, increases
The adhesion of strong subsequent conductive polymer and absorbent charcoal material, to promote the electrochemical stability of composite material.
Further, bonding agent includes but not limited in the step A:Kynoar and its copolymer；Such as：It is poly- inclined
Vinyl fluoride-hexafluoropropene, Kynoar-chlorotrifluoroethylene, Kynoar-trifluoro-ethylene, poly- (vinylidene-trifluoro second
Alkene-chlorine difluoroethylene) or it is poly- (vinylidene-trifluoro-ethylene-chlorotrifluoroethylene).
Further, conducting polymer is thiophene and derivatives, pyrroles and its derivative or aniline in the step C
And its derivative.
Further, volatile organic solvent includes but not limited in the step C：Ether, diethyl ether, acetone or just
Butanol.
Further, the mixed solution is heated in the step D specifically using slow heating, and mesh is gradually increased to from room temperature
Temperature is marked, is maintained 10~30 minutes after reaching target temperature；Target temperature regarding selected organic solvent and conducting polymer monomer and
Fixed, according to embodiments of the present invention, target temperature is 40~60 DEG C, and heating rate is 1~3 DEG C/min.
Further, oxidizing gas is preferably iodine vapor in the step E.
Further, polymerization temperature is 60~100 DEG C of in the step E, and polymerization time is 10~40 minutes.
The principle of the invention is：In the deposition process of monomer, by selecting different volatile organic solvents and control
Heating process makes conducting polymer monomer be attached to activated carbon surface, in the process using the volatilization of organic solvent molecule
Saturated pressure is adjusted by controlling temperature, and then the thickness that can control conducting polymer monomer reaches molecular layer rank；So
Be placed on oxidizing gas environment and carry out chemical polymerization, in reaction process oxidizing gas molecule by way of colliding and polymerizeing come
Induction monomer molecule polymerize, to realize ultra-thin conductive polymer coating in the controllable deposition of activated carbon surface, while oxygen
The property changed gas can be used as dopant to promote the conductivity of conducting polymer, and it is easily controllable to adulterate process.
The beneficial effects of the invention are as follows：
(1) the polymer-modified activated carbon composite wood of ultra-thin conductive can be obtained with preparation method proposed by the present invention
Material, ultra-thin conducting polymer is little in charge and discharge process deformation, overcomes in its thermal energy storage process caused by deformation is excessive
The problem of cyclical stability difference, improves the stability of composite material entirety.
(2) the intrinsic structure of activated carbon is not destroyed with preparation method proposed by the present invention, is not influencing the double electricity of activated carbon
Fake capacitance is effectively introduced on the basis of layer capacity, the good synergistic effect of the two is realized, greatly improves the specific volume of electrode
Amount, while also effectively improving the electric conductivity of material entirety.
(3) preparation method operations proposed by the present invention are controllable, environmentally protective, are suitable for industrialized production,
Specific implementation mode
Specific embodiments of the present invention are described more fully below, the principle of the present invention and its practical application are explained with this,
To make others skilled in the art it will be appreciated that various embodiments of the present invention and suitable for each of specific intended application
Kind modification.
Embodiment 1：
A kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：
Step 1：
It is 10: 1 according to the mass ratio of activated carbon and Kynoar, weighs activated carbon respectively and be scattered in Kynoar
Solvent dimethylformamide (mass ratio 85%), and mechanical ball mill mixes 5 hours, obtains activated carbon/Kynoar slurry.
Step 2：
The slurry that step 1 obtains is taken and is coated on aluminium foil surface in right amount, and 80 DEG C are dried in vacuo 30 minutes；
Step 3：
The aluminium foil that step 2 is obtained with 2% methyl-monosilane solution treatment, and 80 DEG C be dried in vacuo 30 minutes；
Step 4：
Select ether as solvent, be according to the mass ratio of thiophene and ether prepare thiophene diethyl ether solutions at 20: 1, and by its
It is placed in baking oven；
Step 5：
The aluminium foil that step 3 obtains is placed in above thiophene diethyl ether solution, control heating rate is 2 DEG C/min and gradually heats up
To 50 DEG C, rises to 50 DEG C and this temperature is maintained to be kept for 10 minutes；
Step 6：
The substrate that step 5 obtains is placed in 60 DEG C of iodine steam atmosphere to react, reaction can be obtained poly- thiophene after 30 minutes
The active carbon combined electrode film of pheno modification.
Embodiment 2：
A kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：
Step 1：
It is 10: 1 according to the mass ratio of activated carbon and Kynoar, weighs activated carbon respectively and be scattered in Kynoar
Solvent dimethylformamide (mass ratio 85%), and mechanical ball mill mixes 5 hours, obtains activated carbon/Kynoar slurry.
Step 2：
The slurry that step 1 obtains is taken and is coated on aluminium foil surface in right amount, and 80 DEG C are dried in vacuo 30 minutes；
Step 3：
The aluminium foil that step 2 is obtained with 2% methyl-monosilane solution treatment, and 80 DEG C be dried in vacuo 30 minutes；
Step 4：
It selects ether as solvent, is 20: 1 preparation 3,4- ethylene according to the mass ratio of 3,4-rthylene dioxythiophene and ether
Dioxy thiophene diethyl ether solution, and place it in baking oven；
Step 5：
The aluminium foil that step 3 obtains is placed in above 3,4-rthylene dioxythiophene diethyl ether solution, control heating rate is 2 DEG C/
Minute is gradually warming up to 40 DEG C, rises to 40 DEG C and this temperature is maintained to be kept for 30 minutes；
Step 6：
The substrate that step 5 obtains is placed in 80 DEG C of iodine steam atmosphere to react, reaction can be obtained poly- 3 after twenty minutes,
The active carbon combined electrode film of 4- ethene dioxythiophenes modification.
Embodiment 3：
A kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：
Step 1：
It is 8: 1 according to the mass ratio of activated carbon and Kynoar, weighs activated carbon respectively and be scattered in Kynoar
Solvent dimethylformamide (mass ratio 82%), and mechanical ball mill mixes 5 hours, obtains activated carbon/Kynoar slurry.
Step 2：
The slurry that step 1 obtains is taken and is coated on aluminium foil surface in right amount, and 80 DEG C are dried in vacuo 30 minutes；
Step 3：
The aluminium foil that step 2 is obtained with 2% methyl-monosilane solution treatment, and 80 DEG C be dried in vacuo 30 minutes；
Step 4：
It selects ether as solvent, is that 20: 1 preparation dichloro-thiophene ether are molten according to the mass ratio of dichloro-thiophene and ether
Liquid, and place it in baking oven；
Step 5：
The aluminium foil that step 3 obtains is placed in above dichloro-thiophene diethyl ether solution, control heating rate be 1 DEG C/min gradually
40 DEG C are warming up to, 40 DEG C is risen to and this temperature is maintained to be kept for 10 minutes；
Step 6：
The substrate that step 5 obtains is placed in 100 DEG C of iodine steam atmosphere to react, reaction can be obtained poly- two after ten minutes
The active carbon combined electrode film of chlorothiophene modification.
Embodiment 4：
A kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：
Step 1：
It is 10: 1 according to the mass ratio of activated carbon and Kynoar, weighs activated carbon respectively and be scattered in Kynoar
Solvent dimethylformamide (mass ratio 85%), and mechanical ball mill mixes 5 hours, obtains activated carbon/Kynoar slurry.
Step 2：
The slurry that step 1 obtains is taken and is coated on aluminium foil surface in right amount, and 80 DEG C are dried in vacuo 30 minutes；
Step 3：
The aluminium foil that step 2 is obtained with 2% methyl-monosilane solution treatment, and 80 DEG C be dried in vacuo 30 minutes；
Step 4：
It selects ether as solvent, is that 15: 1 preparation dibromo thiophene ether are molten according to the mass ratio of dibromo thiophene and ether
Liquid, and place it in baking oven；
Step 5：
The aluminium foil that step 3 obtains is placed in above dibromo thiophene diethyl ether solution, control heating rate be 3 DEG C/min gradually
60 DEG C are warming up to, 60 DEG C is risen to and this temperature is maintained to be kept for 15 minutes；
Step 6：
The substrate that step 5 obtains is placed in 50 DEG C of iodine steam atmosphere to react, reaction can be obtained poly- two after 25 minutes
The active carbon combined electrode film of bromothiophene modification.
Embodiment 5：
A kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：
Step 1：
It is 10: 1 according to activated carbon and the mass ratio of Kynoar-chlorotrifluoroethylene, weighs activated carbon respectively and gather partially
Vinyl fluoride-chlorotrifluoroethylene is scattered in solvent dimethylformamide (mass ratio 85%), and mechanical ball mill mixes 5 hours, obtains
Activated carbon/Kynoar-chlorotrifluoroethylene slurry.
Step 2：
The slurry that step 1 obtains is taken and is coated on aluminium foil surface in right amount, and 80 DEG C are dried in vacuo 30 minutes；
Step 3：
The aluminium foil that step 2 is obtained with 2% methyl-monosilane solution treatment, and 80 DEG C be dried in vacuo 30 minutes；
Step 4：
It selects n-butanol as solvent, is 18: 1 preparation pyrroles's butanol solutions according to the mass ratio of pyrroles and n-butanol,
And it places it in baking oven；
Step 5：
The aluminium foil that step 3 obtains is placed in above pyrroles's butanol solution, control heating rate is 2 DEG C/min and gradually rises
Temperature rises to 50 DEG C and this temperature is maintained to be kept for 20 minutes to 50 DEG C；
Step 6：
The substrate that step 5 obtains is placed in 60 DEG C of iodine steam atmosphere to react, reaction can be obtained poly- pyrrole after twenty minutes
Cough up the active carbon combined electrode film of modification.
Embodiment 6：
A kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：
Step 1：
It is 10: 1 according to the mass ratio of activated carbon and poly- (vinylidene-trifluoro-ethylene-chlorine difluoroethylene), weighs work respectively
Property charcoal and poly- (vinylidene-trifluoro-ethylene-chlorine difluoroethylene) be scattered in solvent dimethylformamide (mass ratio 85%), and machine
Tool ball milling mixing 5 hours obtains activated carbon/poly- (vinylidene-trifluoro-ethylene-chlorine difluoroethylene) slurry.
Step 2：
The slurry that step 1 obtains is taken and is coated on aluminium foil surface in right amount, and 80 DEG C are dried in vacuo 30 minutes；
Step 3：
The aluminium foil that step 2 is obtained with 2% methyl-monosilane solution treatment, and 80 DEG C be dried in vacuo 30 minutes；
Step 4：
Select acetone as solvent, be according to the mass ratio of aniline and acetone prepare aniline acetone solns at 15: 1, and by its
It is placed in baking oven；
Step 5：
The aluminium foil that step 3 obtains is placed in above aniline acetone soln, control heating rate is 2 DEG C/min and gradually heats up
To 50 DEG C, rises to 50 DEG C and this temperature is maintained to be kept for 20 minutes；
Step 6：
The substrate that step 5 obtains is placed in 70 DEG C of iodine steam atmosphere to react, reaction can be obtained polyphenyl after 15 minutes
Amine-modified active carbon combined electrode film.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.
Claims (9)
1. a kind of preparation method of combination electrode thin-film material, which is characterized in that include the following steps：
Step A：Substrate surface is coated on after the activated carbon handled through surfactant is mixed with binder；
Step B：The substrate obtained through processing of step A is handled using surfactant；
Step C：Conducting polymer monomer is mixed in volatile organic solvent, uniform mixed solution is made；Step D：It will be through
The substrate that step B processing obtains is placed in mixed solution made from step C, heats the mixed solution and organic solvent is waved
Hair, so that conducting polymer monomer deposition is in activated carbon surface；
Step E：The substrate obtained through step D processing is placed in oxidizing gas and carries out chemical polymerization, final be made is led
The combination electrode thin-film material that electric polymer and activated carbon are formed.
2. a kind of preparation method of combination electrode thin-film material according to claim 1, it is characterised in that：The step A
It is silane coupling agent with surfactant in B.
3. a kind of preparation method of combination electrode thin-film material according to claim 1, it is characterised in that：The step A
Middle bonding agent includes but not limited to:Kynoar and its copolymer.
4. a kind of preparation method of combination electrode thin-film material according to claim 1, it is characterised in that：The step C
Middle conducting polymer is thiophene and derivatives, pyrroles and its derivative or aniline and its derivatives.
5. a kind of preparation method of combination electrode thin-film material according to claim 1, it is characterised in that：The step C
Middle volatile organic solvent includes but not limited to：Ether, diethyl ether, acetone or n-butanol.
6. a kind of preparation method of combination electrode thin-film material according to claim 1, it is characterised in that：The step D
The middle heating mixed solution is gradually increased to target temperature from room temperature, is maintained 10~30 minutes after reaching target temperature.
7. a kind of preparation method of combination electrode thin-film material according to claim 6, it is characterised in that：The target temperature
Degree is 40~60 DEG C, and heating rate is 1~3 DEG C/min.
8. a kind of preparation method of combination electrode thin-film material according to claim 1, it is characterised in that：The step E
Middle oxidizing gas is preferably iodine vapor.
9. a kind of preparation method of combination electrode thin-film material according to claim 1, it is characterised in that：The step E
Middle polymerization temperature is 60~100 DEG C of, and polymerization time is 10~40 minutes.
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| CN111029158A (en) * | 2019-12-22 | 2020-04-17 | 北京蒙京石墨新材料科技研究院有限公司 | Lithium ion supercapacitor lithium pre-embedding method |
| CN111463027A (en) * | 2020-04-09 | 2020-07-28 | 西安合容新能源科技有限公司 | Method for improving performance of super capacitor |
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| CN111463027B (en) * | 2020-04-09 | 2021-11-23 | 西安合容新能源科技有限公司 | Method for improving performance of super capacitor |
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| CN108461304B (en) | 2020-04-14 |
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