CN110136997B - Preparation method of high-flexibility composite material electrode - Google Patents
Preparation method of high-flexibility composite material electrode Download PDFInfo
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- CN110136997B CN110136997B CN201910407553.1A CN201910407553A CN110136997B CN 110136997 B CN110136997 B CN 110136997B CN 201910407553 A CN201910407553 A CN 201910407553A CN 110136997 B CN110136997 B CN 110136997B
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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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 discloses a preparation method of a high-flexibility composite material electrode, which comprises the steps of weighing mixed solution of dimethyl imidazole and pyrrole monomers dissolved in water/methanol in sequence, and mixing to obtain solution A; sequentially weighing zinc nitrate hexahydrate and anhydrous ferric chloride, dissolving in a mixed solution of water/methanol, and uniformly stirring to obtain a solution B; soaking the filter paper in the solution A for 1-4 h; taking out the filter paper, and absorbing the surface filtrate; then putting the mixture into the solution B for 20s, taking the mixture out, and then putting the mixture into the solution A for 20 s; repeating the above steps for 10 times; soaking and washing the filter paper by using deionized water to remove surface residues; drying to constant weight to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility. The obtained composite material has excellent flexibility and high mass specific capacitance, can be directly used as a working electrode without any binder, has controllable size and thickness of the electrode material, and has simple and easy preparation process, and is green and economic.
Description
Technical Field
The invention belongs to the technical field of materials, and particularly relates to a preparation method of a high-flexibility composite material electrode.
Background
As the name suggests, compared with the traditional conductive material, the flexible conductive material has excellent flexibility, when the material is deformed to a certain extent under the action of external force or used under certain severe conditions, the electrochemical performance can not be influenced at all, so that the use safety of the electrode material is improved, the controllability of the size and the thickness of the electrode material simplifies the assembly process of the capacitor, the whole device is lighter and lighter, the cost is saved, the application of the flexible conductive material is more economic and environment-friendly, and the application of the flexible conductive material in the aspects of supercapacitors, sensors, electronic skins and artificial intelligence is further widened.
ZIF-8 is a kind of zeolite imidazole ester framework structure material (ZIFs), mainly prepared by reaction of dimethyl imidazole and zinc nitrate, 2-methyl imidazole and metal atom Zn form the most basic unit, wherein each Zn atom coordinates with N atom on four 2-methyl imidazole rings to form a cage-shaped coordination compound with regular hexahedron crystal form, it has advantages of high specific surface area, adjustable aperture, functional pore canal, abundant active site, etc. and is widely favored, ZIFs material has potential application value in fields such as gas storage and separation, catalysis, sensor, super capacitor, etc.
Research and development of supercapacitor electrode materials have made remarkable progress, but the low specific surface area and porosity of the materials inhibit direct contact of the active component with the electrolyte. The electrode material with high specific surface area, rich active sites and high active component utilization rate is constructed by utilizing the high specific surface area and rich active sites of ZIF-8 and the synergistic effect of the conductive high polymer material, so that the electrochemical performance and application of the supercapacitor are improved, and the electrode material has important practical significance.
Disclosure of Invention
The invention aims to provide a preparation method of a high-flexibility composite material electrode, the obtained composite material has excellent flexibility and high mass specific capacitance, can be directly used as a working electrode without any binder, and has the advantages of controllable size and thickness of the electrode material, simple and easy preparation process, greenness and economy.
In order to achieve the purpose, the technical scheme is as follows:
a preparation method of a high-flexibility composite material electrode comprises the following steps:
1) weighing mixed solution of dimethyl imidazole and pyrrole monomers dissolved in water/methanol in sequence, and stirring and mixing uniformly to obtain solution A; sequentially weighing zinc nitrate hexahydrate and anhydrous ferric chloride, dissolving in a mixed solution of water/methanol, and uniformly stirring to obtain a solution B;
2) ultrasonically cleaning common medium-speed qualitative filter paper by acetone, ethanol and deionized water for 15 minutes respectively, washing by the deionized water for 3 times, fully removing impurities in the filter paper, and naturally drying. Weighing the pretreated filter paper, and soaking the filter paper in the solution A for 1-4h to ensure that the filter paper is fully soaked; taking out the filter paper, and absorbing the surface filtrate;
3) then putting the mixture into the solution B for 20s, taking the mixture out, and then putting the mixture into the solution A for 20 s; repeating the above steps for 10 times;
4) soaking and washing the filter paper by using deionized water to remove surface residues; drying to constant weight to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility.
According to the scheme, the volume ratio of the water/methanol mixed solution is 1:3-3: 1.
According to the scheme, the molar concentration of the dimethyl imidazole in the solution A is 0.2-0.5mol/L, and the molar concentration of the pyrrole monomer is 0.1-0.4 mol/L.
According to the scheme, the molar concentration of the zinc nitrate hexahydrate in the solution B is 0.08-0.1mol/L, and the molar concentration of the anhydrous ferric trichloride is 0.5-0.8 mol/L.
Compared with the prior art, the invention has the following outstanding effects:
the electrode material has the mechanical properties of fibers, high flexibility, good electrochemical properties of conductive polymers and high mass specific capacitance;
the preparation method comprises the steps of mixing dimethylimidazole and pyrrole, mixing zinc nitrate and ferric trichloride, enabling the synthesis reaction of ZIF-8 and the polymerization reaction of pyrrole to occur simultaneously, enabling the synthesis reaction and the polymerization reaction of the pyrrole to act in a synergistic manner, being beneficial to preparing an ideal supercapacitor material, controlling the content of ZIF-8 by adjusting the mass molar ratio of dimethylimidazole to zinc nitrate, and controlling the amount of polypyrrole by adjusting the mass molar ratio of pyrrole monomers to ferric trichloride;
ZIF-8 enables the composite material to have rich active sites, and polypyrrole enables the composite material to have good electrochemical performance; the preparation is convenient, and the process is simple and easy.
Detailed Description
The following examples further illustrate the technical solutions of the present invention, but should not be construed as limiting the scope of the present invention.
Example 1:
1) preparing a solution A, weighing 0.526g of dimethylimidazole, weighing 0.278mL of pyrrole monomer, dissolving in a mixed solution of 5mL of water and 15mL of methanol, and stirring by magnetic force to fully dissolve;
2) weighing the pretreated filter paper, and soaking the filter paper in the solution A1 for ensuring that the filter paper is fully soaked;
3) preparing a solution B, sequentially weighing 0.516g of zinc nitrate hexahydrate and 1.94g of anhydrous ferric chloride, dissolving the zinc nitrate hexahydrate and the anhydrous ferric chloride in a mixed solution of 5mL of water and 15mL of methanol, and stirring by magnetic force to fully dissolve;
4) taking out the soaking solution A filter paper, removing the surface filtrate by suction, putting into the solution B20s, taking out, putting into another prepared solution A20s, and repeating the steps for 10 times;
5) and soaking and washing the filter paper by using deionized water, removing monomers or initiator residues on the surface, placing the sample in a vacuum drier to constant weight, and weighing to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility.
6) Making the filter paper/ZIF-8/polypyrrole functional composite material into a working electrode, measuring the electrochemistry of the three electrodes, and measuring the electrochemistry of the three electrodes at 10Ag-1Has a mass specific capacitance of up to 78Fg at a current density of-1And after 2000 cycles, the mass-to-capacitance retention rate is 99%, the solid-state capacitor is assembled and bent into different angles, the mass-to-capacitance of the electrode material is basically kept unchanged, and the stacking performance of the capacitor is excellent.
Example 2:
1) preparing a solution A, weighing 0.789g of dimethylimidazole, weighing 0.278mL of pyrrole monomer, dissolving in a mixed solution of 10mL of water and 10mL of methanol, and stirring by magnetic force to fully dissolve;
2) weighing the pretreated filter paper, and soaking the filter paper in the solution A2 for ensuring that the filter paper is fully soaked;
3) preparing a solution B, sequentially weighing 0.516g of zinc nitrate hexahydrate and 1.94g of anhydrous ferric chloride, dissolving the zinc nitrate hexahydrate and the anhydrous ferric chloride in a mixed solution of 10mL of water and 10mL of methanol, and stirring by magnetic force to fully dissolve;
4) taking out the soaking solution A filter paper, removing the surface filtrate by suction, putting into the solution B20s, taking out, putting into another prepared solution A20s, and repeating the steps for 10 times;
5) and soaking and washing the filter paper by using deionized water, removing monomers or initiator residues on the surface, placing the sample in a vacuum drier to constant weight, and weighing to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility.
6) Making the filter paper/ZIF-8/polypyrrole functional composite material into a working electrode, measuring the electrochemistry of the three electrodes, and measuring the electrochemistry of the three electrodes at 10Ag-1Has a mass specific capacitance of 55Fg at a current density of-1And after 2000 cycles, the mass-to-capacitance retention rate is 99%, the solid-state capacitor is assembled and bent into different angles, the mass-to-capacitance of the electrode material is basically kept unchanged, and the stacking performance of the capacitor is excellent.
Example 3:
1) preparing a solution A, weighing 1.052g of dimethylimidazole, weighing 0.278mL of pyrrole monomer, dissolving in a mixed solution of 10mL of water and 10mL of methanol, and stirring by magnetic force to dissolve fully;
2) weighing the pretreated filter paper, and soaking the filter paper in the solution A3 for ensuring that the filter paper is fully soaked;
3) preparing a solution B, sequentially weighing 0.516g of zinc nitrate hexahydrate and 1.94g of anhydrous ferric chloride, dissolving the zinc nitrate hexahydrate and the anhydrous ferric chloride in a mixed solution of 10mL of water and 10mL of methanol, and stirring by magnetic force to fully dissolve;
4) taking out the soaking solution A filter paper, removing the surface filtrate by suction, putting into the solution B20s, taking out, putting into another prepared solution A20s, and repeating the steps for 10 times;
5) and soaking and washing the filter paper by using deionized water, removing monomers or initiator residues on the surface, placing the sample in a vacuum drier to constant weight, and weighing to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility.
6) Making the filter paper/ZIF-8/polypyrrole functional composite material into a working electrode, measuring the electrochemistry of the three electrodes, and measuring the electrochemistry of the three electrodes at 10Ag-1Has a mass specific capacitance of 50Fg at a current density of-1The solid capacitor is assembled and bent into different angles, the mass specific capacitance of the electrode material is basically kept unchanged, and the stacking performance of the capacitor is excellent.
Example 4:
1) preparing a solution A, weighing 0.789g of dimethylimidazole, weighing 0.278mL of pyrrole monomer, dissolving in a mixed solution of 15mL of water and 5mL of methanol, and stirring by magnetic force to fully dissolve;
2) weighing the pretreated filter paper, and soaking the filter paper in the solution A4 for ensuring that the filter paper is fully soaked;
3) preparing a solution B, sequentially weighing 0.516g of zinc nitrate hexahydrate and 1.94g of anhydrous ferric chloride, dissolving the zinc nitrate hexahydrate and the anhydrous ferric chloride in a mixed solution of 15mL of water and 5mL of methanol, and stirring by magnetic force to fully dissolve;
4) taking out the soaking solution A filter paper, removing the surface filtrate by suction, adding the solution B20s, taking out, adding the prepared solution A20s, and repeating the above steps for 10 times.
5) And soaking and washing the filter paper by using deionized water, removing monomers or initiator residues on the surface, placing the sample in a vacuum drier to constant weight, and weighing to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility.
6) Making filter paper/ZIF-8/polypyrrole functional composite material into working electrode, measuring electrochemical performance of the three electrodes at 10Ag-1The mass specific capacitance of the capacitor reaches 58Fg under the current density-1The solid capacitor is assembled and bent into different angles, the mass specific capacitance of the electrode material is basically kept unchanged, and the stacking performance of the capacitor is excellent.
Example 5:
1) preparing a solution A, weighing 0.789g of dimethylimidazole, weighing 0.278mL of pyrrole monomer, dissolving in a mixed solution of 10mL of water and 10mL of methanol, and stirring by magnetic force to fully dissolve;
2) weighing the pretreated filter paper, and soaking the filter paper in the solution A4 for ensuring that the filter paper is fully soaked;
3) preparing a solution B, sequentially weighing 0.516g of zinc nitrate hexahydrate and 2.92g of anhydrous ferric chloride, dissolving the zinc nitrate hexahydrate and the anhydrous ferric chloride in a mixed solution of 10mL of water and 10mL of methanol, and stirring by magnetic force to fully dissolve;
4) taking out the soaking solution A filter paper, removing the surface filtrate by suction, adding the solution B20s, taking out, adding the prepared solution A20s, and repeating the above steps for 10 times.
5) And soaking and washing the filter paper by using deionized water, removing monomers or initiator residues on the surface, placing the sample in a vacuum drier to constant weight, and weighing to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility.
6) Making filter paper/ZIF-8/polypyrrole functional composite material into working electrode, measuring electrochemical performance of the three electrodes at 10Ag-1Has a mass specific capacitance of 45Fg at a current density of-1。
The invention can be realized by all the listed raw materials, and the invention can be realized by the upper and lower limit values and interval values of all the raw materials; the examples are not to be construed as limiting the scope of the invention. The upper and lower limit values and interval values of the process parameters (such as temperature, time and the like) of the invention can realize the invention, and the embodiments are not listed.
Claims (4)
1. A preparation method of a high-flexibility composite material electrode is characterized by comprising the following steps:
1) weighing mixed solution of dimethyl imidazole and pyrrole monomers dissolved in water/methanol in sequence, and stirring and mixing uniformly to obtain solution A; sequentially weighing zinc nitrate hexahydrate and anhydrous ferric chloride, dissolving in a mixed solution of water/methanol, and uniformly stirring to obtain a solution B;
2) ultrasonically cleaning common medium-speed qualitative filter paper for 15 minutes by acetone, ethanol and deionized water respectively, washing for 3 times by the deionized water, fully removing impurities in the filter paper, and naturally drying; weighing the pretreated filter paper, and soaking the filter paper in the solution A for 1-4h to ensure that the filter paper is fully soaked; taking out the filter paper, and absorbing the surface filtrate;
3) then putting the mixture into the solution B for 20s, taking the mixture out, and then putting the mixture into the solution A for 20 s; repeating the above steps for 10 times;
4) soaking and washing the filter paper by using deionized water to remove surface residues; drying to constant weight to obtain the filter paper/ZIF-8/polypyrrole functional composite material with excellent flexibility.
2. The method for preparing the high-flexibility composite material electrode as claimed in claim 1, wherein the volume ratio of the water/methanol mixed solution is 1:3-3: 1.
3. The method for preparing a highly flexible composite electrode according to claim 1, wherein the molar concentration of the dimethylimidazole in the solution A is 0.2 to 0.5mol/L, and the molar concentration of the pyrrole monomer is 0.1 to 0.4 mol/L.
4. The method for preparing the high-flexibility composite material electrode as claimed in claim 1, wherein the molar concentration of the zinc nitrate hexahydrate in the solution B is 0.08-0.1mol/L, and the molar concentration of the anhydrous ferric chloride is 0.5-0.8 mol/L.
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| CN110634684B (en) * | 2019-09-27 | 2021-04-27 | 济南大学 | Preparation of flexible paper-based cerium dioxide nanowire-metal organic framework heterojunction |
| CN110634685A (en) * | 2019-09-29 | 2019-12-31 | 华东师范大学 | Ppy @ ZIF-67 composite material, and preparation method and application thereof |
| CN110993374B (en) * | 2019-11-26 | 2021-08-24 | 武汉工程大学 | Preparation method of flexible conductive composite material, product prepared by preparation method and application of product |
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