CN108461304B - Preparation method of composite electrode film material - Google Patents

Preparation method of composite electrode film material Download PDF

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Publication number
CN108461304B
CN108461304B CN201810287539.8A CN201810287539A CN108461304B CN 108461304 B CN108461304 B CN 108461304B CN 201810287539 A CN201810287539 A CN 201810287539A CN 108461304 B CN108461304 B CN 108461304B
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electrode film
film material
composite electrode
conductive polymer
steps
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CN108461304A (en
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杨亚杰
李世园
李海洲
何鑫
毛喜玲
周榆久
赵月涛
徐建华
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University of Electronic Science and Technology of China
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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
    • 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
    • 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

A preparation method of a composite electrode film material belongs to the technical field of energy storage materials. According to the invention, different volatile organic solvents are selected and the heating process is controlled, the conductive polymer monomer is attached to the surface of the active carbon by utilizing the volatilization of organic solvent molecules, and the saturated air pressure is adjusted by controlling the temperature in the process, so that the thickness of the conductive polymer monomer can be controlled to reach the molecular layer level; and then placing the carbon substrate in an oxidizing gas environment for chemical polymerization, wherein in the reaction process, oxidizing gas molecules induce monomer molecules to polymerize in a collision polymerization mode, so that the controllable deposition of the ultrathin conductive polymer layer on the surface of the activated carbon is realized. The deformation of the ultrathin conductive polymer is very slight in the charging and discharging processes, so that the problem of poor cycle stability caused by overlarge deformation in the energy storage process is solved, and the overall stability of the composite material is improved; and the specific capacity and the conductivity of the electrode are obviously improved.

Description

Preparation method of composite electrode film material
Technical Field
The invention belongs to the technical field of energy storage materials, and particularly relates to a preparation method of a composite electrode film material.
Background
The super capacitor is one of the hot spots of the current scientific research as a novel green and environment-friendly energy storage device. The electrode material is the core of the super capacitor, and determines the capacitance performance, the production cost and the application field of the super capacitor. Therefore, the electrode material becomes a research hotspot as a bottleneck restricting the development of the super capacitor.
Rich structural material systems including electric double layer behavior and pseudocapacitance behavior are being developed. The electrode material of the double-capacitance capacitor is mainly made of carbon materials, and the carbon materials have become main electrode materials used by commercial super capacitors due to the advantages of excellent conductivity, cycle stability, wider potential window, low price, simple preparation method and the like. The energy storage mechanism of the carbon material itself electric double layer capacitance makes it possible to produce a lower specific capacitance. In order to improve the specific capacitance of the carbon material, researchers do a lot of work, for example, the carbon material has a higher specific surface area through structure regulation, so that the permeation and adsorption of electrolyte are facilitated, and the electric double layer capacitance of the carbon material is improved. However, simply increasing the specific surface area of the carbon material is accompanied by a decrease in electrical conductivity and a limitation in improvement of specific capacitance, and it is difficult to greatly increase the energy density and power density of the supercapacitor. The practical carbon material is effectively combined with the pseudocapacitance material, so that the preparation of the high-performance electrode material is a hotspot of the research on the electrode material of the super capacitor at present. How to realize the effective modification of the pseudo-capacitor material on the carbon material is very important to exert good synergistic effect between the pseudo-capacitor material and the carbon material, and becomes the key for realizing the practicability of the composite material.
The electrode material of the pseudocapacitive capacitor comprises a conductive polymer and a metal oxide. The pseudocapacitance material can perform underpotential deposition on a two-dimensional or quasi-two-dimensional space on the surface of an electrode or in a bulk phase, and a highly reversible chemical reaction occurs to generate capacitance related to the charging potential of the electrode. The pseudocapacitance is generated not only on the electrode surface but also in the entire electrode interior, and thus higher capacitance and energy density than those of the electric double layer capacitor can be obtained. Under the condition of the same electrode area, the pseudocapacitance can be 10-100 times of the electric capacity of the electric double layer. The conductive polymer can become an ideal electrode material due to the unique conductive mechanism and the physicochemical property, the utilization rate of the conductive polymer is improved by regulating and controlling the dopant, the capacitance is improved by promoting the redox reaction of doping/dedoping, and the conductive polymer has the incomparable advantages of a carbon material and a metal oxide in the aspect of serving as an electrode. However, researchers have focused on improving the utilization rate of the electrode material components, so that the active elements in the bulk can fully undergo redox reaction during rapid charging and discharging, and then the rate characteristics of the active elements can be improved, and meanwhile, the serious problems of the conductive polymer as the electrode material of the supercapacitor also have to be faced. Since electrochemical energy storage of a conductive polymer as an electrode is realized through an oxidation-reduction process, and shrinkage and expansion of a polymer skeleton structure occur in the process, that is, deformation is large in the charging and discharging processes, reference can be made to section 1.3.3 of the first chapter of research on performance of a porous composite electrode prepared by a unipolar pulse method and pseudocapacitance thereof in article published by goldenlare. Therefore, the greater the thickness of the conductive polymer, the more significant the volume change that occurs during its energy storage, which ultimately leads to poor overall stability of the composite material. Therefore, the carbon material is effectively modified by the conductive polymer, and the technical problem that the cycling stability of the material compounded by the conductive polymer is the problem of serving as the electrode material of the supercapacitor is solved.
Disclosure of Invention
The invention aims to: aiming at the problem that the stability of a composite material formed by modifying a carbon material with a conductive polymer is poor due to poor circulation stability of the conductive polymer in the prior art, the invention provides a preparation method of a composite electrode film material.
In order to achieve the above purpose, the invention provides the following technical scheme:
the preparation method of the composite electrode film material is characterized by comprising the following steps: step A: mixing the activated carbon treated by the surfactant with a binder and coating the mixture on the surface of a substrate;
and B: treating the substrate obtained by the step A by adopting a surfactant;
and C: mixing a conductive polymer monomer in a volatile organic solvent to prepare a uniform mixed solution; step D: placing the substrate obtained by the treatment in the step B into the mixed solution prepared in the step C, and heating the mixed solution to volatilize the organic solvent so as to deposit the conductive polymer monomer on the surface of the activated carbon;
step E: and D, placing the substrate obtained by the treatment in the step D in oxidizing gas for chemical polymerization reaction, and finally preparing the composite electrode film material formed by the conductive polymer and the active carbon.
Further, the surfactant in the steps A and B is a silane coupling agent. The surfactant has the function of enhancing the adhesion of the subsequent conductive polymer and the activated carbon material, so that the electrochemical stability of the composite material is improved.
Further, the adhesive in the step A includes but is not limited to polyvinylidene fluoride and copolymers thereof; such as: polyvinylidene fluoride-hexafluoropropylene, polyvinylidene fluoride-chlorotrifluoroethylene, polyvinylidene fluoride-trifluoroethylene, poly (vinylidene fluoride-trifluoroethylene-chlorodifluoroethylene), or poly (vinylidene fluoride-trifluoroethylene-chlorotrifluoroethylene).
Further, the conductive polymer in the step C is thiophene and its derivatives, pyrrole and its derivatives, or aniline and its derivatives.
Further, the volatile organic solvent in step C includes but is not limited to: diethyl ether, acetone or n-butanol.
Further, heating the mixed solution in the step D specifically adopts slow heating, gradually increases from room temperature to a target temperature, and maintains for 10-30 minutes after the target temperature is reached; the target temperature depends on the selected organic solvent and the conductive polymer monomer, and according to the embodiment of the invention, the target temperature is 40-60 ℃, and the temperature rise rate is 1-3 ℃/min.
Further, the oxidizing gas in step E is preferably iodine vapor.
Further, in the step E, the polymerization temperature is 60-100 ℃, and the polymerization time is 10-40 minutes.
The principle of the invention is as follows: in the deposition process of the monomer, different volatile organic solvents are selected, the heating process is controlled, the conductive polymer monomer is attached to the surface of the active carbon by utilizing the volatilization of organic solvent molecules, the saturated air pressure is adjusted by controlling the temperature in the process, and the thickness of the conductive polymer monomer can be controlled to reach the molecular layer level; and then placing the carbon substrate in an oxidizing gas environment for chemical polymerization, wherein in the reaction process, oxidizing gas molecules induce monomer molecules to polymerize in a collision polymerization mode, so that the controllable deposition of the ultrathin conductive polymer layer on the surface of the activated carbon is realized, meanwhile, the oxidizing gas can be used as a dopant to improve the conductivity of the conductive polymer, and the doping process is easy to control.
The invention has the beneficial effects that:
(1) the preparation method provided by the invention can be used for obtaining the ultrathin conductive polymer modified activated carbon composite material, the ultrathin conductive polymer has little deformation in the charging and discharging process, the problem of poor cycle stability caused by overlarge deformation in the energy storage process is solved, and the overall stability of the composite material is improved.
(2) The preparation method provided by the invention does not damage the intrinsic structure of the activated carbon, effectively introduces pseudo-capacitance on the basis of not influencing the capacity of the double electric layers of the activated carbon, realizes good synergistic effect of the activated carbon and the pseudo-capacitance, greatly improves the specific capacity of the electrode, and simultaneously effectively improves the overall conductivity of the material.
(3) The preparation method provided by the invention has controllable operation, is green and environment-friendly, is suitable for industrial production,
Detailed Description
Reference will now be made in detail to the present embodiments of the invention, examples of which are illustrated in the accompanying drawings, wherein like reference numerals refer to like elements throughout.
Example 1:
the preparation method of the composite electrode film material is characterized by comprising the following steps:
step 1:
respectively weighing the activated carbon and the polyvinylidene fluoride according to the mass ratio of 10: 1, dispersing the activated carbon and the polyvinylidene fluoride in a solvent dimethylformamide (the mass ratio is 85%), and mechanically ball-milling and mixing for 5 hours to obtain activated carbon/polyvinylidene fluoride slurry.
Step 2:
coating a proper amount of the slurry obtained in the step 1 on the surface of an aluminum foil, and carrying out vacuum drying for 30 minutes at 80 ℃;
and step 3:
treating the aluminum foil obtained in the step 2 with 2% methyl silane solution, and vacuum-drying for 30 minutes at 80 ℃;
and 4, step 4:
selecting diethyl ether as a solvent, preparing a thiophene diethyl ether solution according to the mass ratio of thiophene to diethyl ether of 20: 1, and placing the thiophene diethyl ether solution in an oven;
and 5:
placing the aluminum foil obtained in the step 3 above a thiophene ether solution, gradually heating to 50 ℃ at a heating rate of 2 ℃/min, and maintaining the temperature for 10 minutes after heating to 50 ℃;
step 6:
and (3) placing the substrate obtained in the step (5) in an iodine steam atmosphere at 60 ℃ for reaction, and reacting for 30 minutes to obtain the polythiophene modified active carbon composite electrode film.
Example 2:
the preparation method of the composite electrode film material is characterized by comprising the following steps:
step 1:
respectively weighing the activated carbon and the polyvinylidene fluoride according to the mass ratio of 10: 1, dispersing the activated carbon and the polyvinylidene fluoride in a solvent dimethylformamide (the mass ratio is 85%), and mechanically ball-milling and mixing for 5 hours to obtain activated carbon/polyvinylidene fluoride slurry.
Step 2:
coating a proper amount of the slurry obtained in the step 1 on the surface of an aluminum foil, and carrying out vacuum drying for 30 minutes at 80 ℃;
and step 3:
treating the aluminum foil obtained in the step 2 with 2% methyl silane solution, and vacuum-drying for 30 minutes at 80 ℃;
and 4, step 4:
selecting diethyl ether as a solvent, preparing a 3, 4-ethylenedioxythiophene diethyl ether solution according to the mass ratio of 3, 4-ethylenedioxythiophene to diethyl ether of 20: 1, and placing the 3, 4-ethylenedioxythiophene diethyl ether solution in an oven;
and 5:
placing the aluminum foil obtained in the step 3 above a 3, 4-ethylenedioxythiophene ether solution, gradually heating to 40 ℃ at the heating rate of 2 ℃/min, and maintaining the temperature for 30 min after heating to 40 ℃;
step 6:
and (3) placing the substrate obtained in the step (5) in an iodine steam atmosphere at the temperature of 80 ℃ for reaction, and reacting for 20 minutes to obtain the activated carbon composite electrode film modified by the poly (3, 4-ethylenedioxythiophene).
Example 3:
the preparation method of the composite electrode film material is characterized by comprising the following steps:
step 1:
respectively weighing the activated carbon and the polyvinylidene fluoride according to the mass ratio of 8: 1, dispersing the activated carbon and the polyvinylidene fluoride in a solvent dimethylformamide (the mass ratio is 82%), and mechanically ball-milling and mixing for 5 hours to obtain activated carbon/polyvinylidene fluoride slurry.
Step 2:
coating a proper amount of the slurry obtained in the step 1 on the surface of an aluminum foil, and carrying out vacuum drying for 30 minutes at 80 ℃;
and step 3:
treating the aluminum foil obtained in the step 2 with 2% methyl silane solution, and vacuum-drying for 30 minutes at 80 ℃;
and 4, step 4:
selecting diethyl ether as a solvent, preparing a dichlorothiophene diethyl ether solution according to the mass ratio of dichlorothiophene to diethyl ether of 20: 1, and placing the solution in an oven;
and 5:
placing the aluminum foil obtained in the step 3 above a dichlorothiophene ether solution, gradually heating to 40 ℃ at the heating rate of 1 ℃/minute, and maintaining the temperature for 10 minutes after heating to 40 ℃;
step 6:
and (3) placing the substrate obtained in the step (5) in an iodine steam atmosphere at 100 ℃ for reaction, and reacting for 10 minutes to obtain the activated carbon composite electrode film modified by the polydichlorothiophene.
Example 4:
the preparation method of the composite electrode film material is characterized by comprising the following steps:
step 1:
respectively weighing the activated carbon and the polyvinylidene fluoride according to the mass ratio of 10: 1, dispersing the activated carbon and the polyvinylidene fluoride in a solvent dimethylformamide (the mass ratio is 85%), and mechanically ball-milling and mixing for 5 hours to obtain activated carbon/polyvinylidene fluoride slurry.
Step 2:
coating a proper amount of the slurry obtained in the step 1 on the surface of an aluminum foil, and carrying out vacuum drying for 30 minutes at 80 ℃;
and step 3:
treating the aluminum foil obtained in the step 2 with 2% methyl silane solution, and vacuum-drying for 30 minutes at 80 ℃;
and 4, step 4:
selecting diethyl ether as a solvent, preparing a dibromothiophene diethyl ether solution according to the mass ratio of dibromothiophene to diethyl ether of 15: 1, and placing the dibromothiophene diethyl ether solution in an oven;
and 5:
placing the aluminum foil obtained in the step 3 above a dibromothiophene ether solution, gradually heating to 60 ℃ at a heating rate of 3 ℃/min, and maintaining the temperature for 15 minutes after heating to 60 ℃;
step 6:
and (3) placing the substrate obtained in the step (5) in an iodine steam atmosphere at 50 ℃ for reaction, and reacting for 25 minutes to obtain the polydibromothiophene modified active carbon composite electrode film.
Example 5:
the preparation method of the composite electrode film material is characterized by comprising the following steps:
step 1:
respectively weighing the activated carbon and the polyvinylidene fluoride-chlorotrifluoroethylene according to the mass ratio of 10: 1, dispersing the activated carbon and the polyvinylidene fluoride-chlorotrifluoroethylene in a solvent dimethylformamide (the mass ratio is 85%), and mechanically ball-milling and mixing for 5 hours to obtain the activated carbon/polyvinylidene fluoride-chlorotrifluoroethylene slurry.
Step 2:
coating a proper amount of the slurry obtained in the step 1 on the surface of an aluminum foil, and carrying out vacuum drying for 30 minutes at 80 ℃;
and step 3:
treating the aluminum foil obtained in the step 2 with 2% methyl silane solution, and vacuum-drying for 30 minutes at 80 ℃;
and 4, step 4:
selecting n-butanol as a solvent, preparing a pyrrole n-butanol solution according to the mass ratio of pyrrole to n-butanol of 18: 1, and placing the pyrrole n-butanol solution in an oven;
and 5:
placing the aluminum foil obtained in the step 3 above a pyrrole n-butanol solution, gradually heating to 50 ℃ at a heating rate of 2 ℃/min, and maintaining the temperature for 20 minutes after heating to 50 ℃;
step 6:
and (3) placing the substrate obtained in the step (5) in an iodine steam atmosphere at 60 ℃ for reaction, and reacting for 20 minutes to obtain the polypyrrole-modified activated carbon composite electrode film.
Example 6:
the preparation method of the composite electrode film material is characterized by comprising the following steps:
step 1:
respectively weighing the activated carbon and the poly (vinylidene fluoride-trifluoroethylene-chlorodifluoroethylene) according to the mass ratio of 10: 1, dispersing the activated carbon and the poly (vinylidene fluoride-trifluoroethylene-chlorodifluoroethylene) in a solvent dimethylformamide (mass ratio of 85%), and mechanically ball-milling and mixing for 5 hours to obtain activated carbon/poly (vinylidene fluoride-trifluoroethylene-chlorodifluoroethylene) slurry.
Step 2:
coating a proper amount of the slurry obtained in the step 1 on the surface of an aluminum foil, and carrying out vacuum drying for 30 minutes at 80 ℃;
and step 3:
treating the aluminum foil obtained in the step 2 with 2% methyl silane solution, and vacuum-drying for 30 minutes at 80 ℃;
and 4, step 4:
selecting acetone as a solvent, preparing an aniline acetone solution according to the mass ratio of aniline to acetone of 15: 1, and placing the aniline acetone solution in an oven;
and 5:
placing the aluminum foil obtained in the step 3 above an aniline acetone solution, gradually heating to 50 ℃ at the heating rate of 2 ℃/min, and maintaining the temperature for 20 minutes after heating to 50 ℃;
step 6:
and (3) placing the substrate obtained in the step (5) in an iodine steam atmosphere at 70 ℃ for reaction, and reacting for 15 minutes to obtain the polyaniline-modified activated carbon composite electrode film.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (9)

1. The preparation method of the composite electrode film material is characterized by comprising the following steps:
step A: mixing the activated carbon treated by the surfactant with a binder and coating the mixture on the surface of a substrate;
and B: treating the substrate obtained by the step A by adopting a surfactant;
and C: mixing a conductive polymer monomer in a volatile organic solvent to prepare a uniform mixed solution; step D: placing the substrate obtained by the treatment in the step B into the mixed solution prepared in the step C, and heating the mixed solution to volatilize the organic solvent so as to deposit the conductive polymer monomer on the surface of the activated carbon;
step E: and D, placing the substrate obtained by the treatment in the step D in oxidizing gas for chemical polymerization reaction, and finally preparing the composite electrode film material formed by the conductive polymer and the active carbon.
2. The method for preparing the composite electrode film material according to claim 1, wherein the method comprises the following steps: and the surfactant in the steps A and B is a silane coupling agent.
3. The method for preparing the composite electrode film material according to claim 1, wherein the method comprises the following steps: and the adhesive in the step A is polyvinylidene fluoride and a copolymer thereof.
4. The method for preparing the composite electrode film material according to claim 1, wherein the method comprises the following steps: and the conductive polymer in the step C is thiophene and derivatives thereof, pyrrole and derivatives thereof or aniline and derivatives thereof.
5. The method for preparing the composite electrode film material according to claim 1, wherein the method comprises the following steps: and the volatile organic solvent in the step C is diethyl ether, acetone or n-butanol.
6. The method for preparing the composite electrode film material according to claim 1, wherein the method comprises the following steps: and D, heating the mixed solution from room temperature to the target temperature gradually, and maintaining for 10-30 minutes after the target temperature is reached.
7. The method for preparing the composite electrode film material according to claim 6, wherein the method comprises the following steps: the target temperature is 40-60 ℃, and the heating rate is 1-3 ℃/min.
8. The method for preparing the composite electrode film material according to claim 1, wherein the method comprises the following steps: the oxidizing gas in the step E is iodine vapor.
9. The method for preparing the composite electrode film material according to claim 1, wherein the method comprises the following steps: and in the step E, the polymerization temperature is 60-100 ℃, and the polymerization time is 10-40 minutes.
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