CN110289182B - Preparation method of manganese-doped carbon gel @ (PANI/GO) n// NGA @ PEDOT electrode material - Google Patents
Preparation method of manganese-doped carbon gel @ (PANI/GO) n// NGA @ PEDOT electrode material Download PDFInfo
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- CN110289182B CN110289182B CN201910325050.XA CN201910325050A CN110289182B CN 110289182 B CN110289182 B CN 110289182B CN 201910325050 A CN201910325050 A CN 201910325050A CN 110289182 B CN110289182 B CN 110289182B
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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
- H01G11/32—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
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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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 manganese-doped carbon gel @ (PANI/GO) n// NGA @ PEDOT electrode material, wherein melamine is dissolved in a graphene oxide solution, VC and ammonia water are added, ultrasonic dissolution is carried out, an organogel is formed by a water bath method, and the organogel is fired to obtain NGA; adding NGA into butyl acetate, adding iron p-toluenesulfonate into a mixed solution of ethanol and water, ultrasonically mixing, and standing at room temperature for polymerization to obtain an NGA @ PEDOT material; resorcinol, formaldehyde and manganese acetate are used as precursors, and sodium carbonate is used as a catalyst, so as to obtain the manganese-doped carbon gel electrode material; and (2) repeatedly dropwise adding the mixed solution of PANI n times onto the manganese-doped carbon gel material in the step (1), wherein the method has the advantages of simplicity, high efficiency, good reproducibility, large-scale preparation and the like. The material prepared by the method has the characteristics of higher specific capacitance, wider working voltage window, quick charge and discharge and the like.
Description
Technical Field
The invention belongs to the field of super-capacitor new material energy storage, and particularly relates to a preparation method of a manganese-doped carbon gel @ (PANI/GO) n// NGA @ PEDOT electrode material for an asymmetric capacitor.
Background
In order to improve the energy density of the super capacitor, the preparation of the asymmetric super capacitor is one of the safest and effective ways for improving the energy density. The asymmetric super capacitor is used for increasing the working voltage by assembling two electrodes with different potential windows. Two electrode materials with different voltage windows are needed for preparing the asymmetric super capacitor, and generally, a positive electrode material with relatively positive potential and a negative electrode material with relatively negative potential are used as the anode material.
Manganese doped carbon gel @ (PANI/GO) n// NGA @ PEDOT is a pair of electrode materials which can be used for preparing asymmetric all-solid-state supercapacitors. The manganese-doped carbon gel @ (PANI/GO) n material is used as a positive electrode, and the NGA @ PEDOT material is used as a negative electrode. The NGA @ PEDOT is a novel material formed by coating nitrogen-doped graphene gel (NGA) with poly (3, 4-ethylenedioxythiophene) (PEDOT), and the manganese-doped carbon gel @ (PANI/GO) n is a self-assembly coating manganese-doped carbon gel material formed by coating n layers of polyaniline and graphene oxide. The manganese-doped carbon gel @ (PANI/GO) n gel material has good conductivity, higher specific capacitance and simple preparation process, and the NGA @ PEDOT has the characteristics of high capacity and stability and is a good anode material of the asymmetric super capacitor.
Disclosure of Invention
Aiming at the problem of improving the energy density of the all-solid-state flexible super capacitor, the manganese-doped carbon gel @ (PANI/GO) n// NGA @ PEDOT electrode material with a wider window potential is prepared, and the method can be used for preparing the asymmetric all-solid-state flexible super capacitor
A preparation method of a manganese-doped carbon gel @ (PANI/GO) n// NGA @ PEDOT electrode material comprises the following steps:
preparation of NGA @ PEDOT
(1) Dissolving melamine in a graphene oxide solution, sequentially adding VC and ammonia water, performing ultrasonic treatment at 1-4 ℃ to completely dissolve the melamine, then forming organogel in the mixed solution at 80 ℃ by using a water bath method, and firing the organogel at 600-1200 ℃ for 2h in an inert atmosphere to obtain NGA, wherein the concentration of the graphene oxide solution is 0.5-20mg/ml, the mass ratio of graphene oxide to VC is 1:1, and the mass ratio of graphene oxide to ammonia water is 4: 1; the mass ratio of the melamine to the graphene oxide is 1:200-5: 100; NGA is nitrogen-doped graphene gel; VC is vitamin C;
(2) adding NGA into butyl acetate, wherein the content of NGA is 15 wt.%, adding EDOT according to the proportion of 50 μ l/ml, and performing ultrasonic treatment for 1 h; EDOT is 3, 4-ethylenedioxythiophene;
(3) and (3) dissolving ferric p-toluenesulfonate in a mixed solution of ethanol and water, wherein the volume ratio of ethanol to water is 3:1, the content of the ferric p-toluenesulfonate is 0.6 wt.%, dripping the solution on the material obtained in the step (2), ultrasonically mixing, and standing at room temperature for polymerization to obtain the NGA @ PEDOT material.
Preparation of manganese-doped carbon gel @ (PANI/GO) n
(1) Preparing the manganese-doped carbon gel material
Resorcinol, formaldehyde and manganese acetate are used as precursors, sodium carbonate is used as a catalyst, wherein the molar ratio of resorcinol to formaldehyde is 1:2, the molar ratio of resorcinol to sodium carbonate is 250:1-800:1, and the manganese content is 0.5-3 wt.%. Putting the solution into a sealed cylindrical glass tube, aging at 30 ℃ for 2 days, aging at 80 ℃ for 5 days, and extracting in acetone for 2 days to obtain a manganese-doped carbon gel electrode material;
(2) stirring PANI and DMAc in a mass ratio of 1:47 for 12 hours, adding HCl into the mixture to enable the pH value of the mixed solution to be 2.5 and the concentration of PANI to be 0.5mg/ml, and then performing ultrasonic treatment at 1-4 ℃ for 3 hours; PANI is polyaniline; DMAc is dimethylacetamide;
(3) dropwise adding the PANI mixed solution obtained in the step (2) onto the manganese-doped carbon gel material obtained in the step (1), standing for 15min, removing redundant PANI mixed solution through vacuum filtration, dropwise adding a graphene oxide solution onto the manganese-doped carbon gel, standing for 15min, and removing redundant graphene oxide solution through vacuum filtration; wherein the concentration of the graphene oxide solution is 0.5-20 mg/ml;
(4) repeating the step (3) n-1 times to obtain the manganese-doped carbon gel @ (PANI/GO) n material.
The invention has the beneficial effects that: the method has the advantages of simplicity, high efficiency, good reproducibility, large-scale preparation and the like. The material prepared by the method has the characteristics of higher specific capacitance, wider working voltage window, quick charge and discharge and the like.
Detailed Description
For a better understanding of the present invention, reference will now be made to the following examples which are set forth to illustrate, but are not to be construed to limit the present invention.
The first embodiment is as follows: dissolving melamine in a graphene oxide solution, performing ultrasonic treatment at 4 ℃ to completely dissolve the melamine, sequentially adding VC and ammonia water, sealing a membrane, performing ultrasonic treatment at low temperature for 2 hours, then forming organogel in the mixed solution at 80 ℃ by using a water bath method, and firing the organogel at 600 ℃ for 2 hours under an inert atmosphere to obtain NGA; wherein the concentration of the graphene oxide solution is 0.5mg/ml, the mass ratio of the graphene oxide to VC is 1:1, the mass ratio of the graphene oxide to ammonia water is 4:1, and the mass ratio of melamine to the graphene oxide is 1: 200; putting 1mg of NGA into butyl acetate, wherein the content of the NGA is 15 wt.%, adding EDOT according to the proportion of 50 mul/ml, and carrying out ultrasonic treatment for 1h to obtain a mixed solution; 0.25g of iron p-toluenesulfonate is dissolved in a mixed solution of 3ml of ethanol and 1ml of water, and then dropped into the mixed solution, and after ultrasonic mixing, the mixed solution is stood at room temperature for 6 hours and then polymerized. And cleaning with ethanol, and drying at room temperature for 1h to obtain the NGA @ PEDOT material.
Resorcinol, formaldehyde and manganese acetate are used as precursors, sodium carbonate is used as a catalyst, wherein the molar ratio of resorcinol to formaldehyde is 1:2, the molar ratio of resorcinol to sodium carbonate is 250:1, and the manganese content is 1 wt.%. And (3) putting the solution into a sealed cylindrical glass tube with the outer diameter of 1cm, aging at 30 ℃ for 2 days, aging at 80 ℃ for 5 days, and extracting in acetone for 2 days to obtain the manganese-doped carbon gel electrode material. 1g of PANI and 50ml of DMAc were mixed, stirred for 12h, and HCl was added to the mixture to make the pH of the mixture 2.5 and the concentration of PANI 0.5mg/ml, followed by sonication at 4 ℃ for 3h to obtain a mixture of PANI. Dropwise adding the PANI mixed solution onto a manganese-doped carbon gel material, standing for 15min, carrying out vacuum filtration to remove redundant PANI, dropwise adding 0.5mg/ml graphene oxide solution onto the material, standing for 15min, and carrying out vacuum filtration to remove redundant graphene oxide solution. Repeating the operation for 4 times to obtain manganese-doped carbon gel @ (PANI/GO)5A material.
The second embodiment is as follows: dissolving melamine in a graphene oxide solution, performing ultrasonic treatment at 4 ℃ to completely dissolve the melamine, adding VC and ammonia water, sealing a membrane, performing ultrasonic treatment at low temperature for 2 hours, then forming organogel in the mixed solution at 80 ℃ by using a water bath method, and firing the organogel at 900 ℃ for 2 hours under an inert atmosphere to obtain NGA; the graphene oxide solution is 10mg/ml in concentration, the mass ratio of graphene oxide to VC is 1:1, the mass ratio of graphene oxide to ammonia water is 4:1, and the mass ratio of melamine to graphene oxide is 1: 50; putting 1mg of NGA into butyl acetate, wherein the content of the NGA is 15 wt.%, adding EDOT according to the proportion of 50 mul/ml, and carrying out ultrasonic treatment for 1h to obtain a mixed solution; 0.25g of iron p-toluenesulfonate is dissolved in a mixed solution of 3ml of ethanol and 1ml of water, and then dropped into the mixed solution, and after ultrasonic mixing, the mixed solution is stood at room temperature for 6 hours and then polymerized. And cleaning with ethanol, and drying at room temperature for 1h to obtain the NGA @ PEDOT material.
Resorcinol, formaldehyde and manganese acetate are used as precursors, sodium carbonate is used as a catalyst, wherein the molar ratio of resorcinol to formaldehyde is 1:2, the molar ratio of resorcinol to sodium carbonate is 500:1, and the manganese content is 2 wt.%. And (3) putting the solution into a sealed cylindrical glass tube with the outer diameter of 1cm, aging at 30 ℃ for 2 days, aging at 80 ℃ for 5 days, and extracting in acetone for 2 days to obtain the manganese-doped carbon gel electrode material. 1g of PANI and 50ml of DMAc were mixed and stirred for 12h, HCl was added to the mixture to make the pH of the mixture 2.5 and the concentration of PANI 0.5mg/ml, followed by sonication at 4 ℃ for 3h to obtain a mixture of PANI. Dropwise adding the PANI mixed solution onto a manganese-doped carbon gel material, standing for 15min, carrying out vacuum filtration to remove redundant PANI, dropwise adding a 10mg/ml graphene oxide solution onto the material, standing for 15min, and carrying out vacuum filtration to remove redundant graphene oxide solution. Repeating the operation for 19 times to obtain manganese-doped carbon gel @ (PANI/GO)20A material.
The third concrete implementation mode: dissolving melamine in a graphene oxide solution, performing ultrasonic treatment at 4 ℃ to completely dissolve the melamine, adding VC and ammonia water, performing low-temperature ultrasonic treatment for 2 hours while sealing a membrane, then forming organogel in the mixed solution at 80 ℃ by using a water bath method, and firing the organogel for 2 hours at 1000 ℃ in an inert atmosphere to obtain NGA; wherein the concentration of the graphene oxide solution is 20mg/ml, the mass ratio of the graphene oxide to VC is 1:1, the mass ratio of the graphene oxide to ammonia water is 4:1, and the mass ratio of melamine to the graphene oxide is 3: 100; putting 1mg of NGA into butyl acetate, wherein the content of the NGA is 15 wt.%, adding EDOT according to the proportion of 50 mul/ml, and carrying out ultrasonic treatment for 1h to obtain a mixed solution; 0.25g of iron p-toluenesulfonate is dissolved in a mixed solution of 3ml of ethanol and 1ml of water, and then dropped again into the mixed solution, and after ultrasonic mixing, the mixed solution is stood at room temperature for 6 hours and then polymerized. And cleaning with ethanol, and drying at room temperature for 1h to obtain the NGA @ PEDOT material.
Resorcinol, formaldehyde and manganese acetate are used as precursors, sodium carbonate is used as a catalyst, wherein the molar ratio of resorcinol to formaldehyde is 1:2, the molar ratio of resorcinol to sodium carbonate is 800:1, and the manganese content is 3 wt.%. And (3) putting the solution into a sealed cylindrical glass tube with the outer diameter of 1cm, aging at 30 ℃ for 2 days, aging at 80 ℃ for 5 days, and extracting in acetone for 2 days to obtain the manganese-doped carbon gel electrode material. 1g of PANI and 50ml of DMAc were mixed and stirred for 12h, HCl was added to the mixture to make the pH of the mixture 2.5 and the concentration of PANI 0.5mg/ml, followed by sonication at 4 ℃ for 3h to obtain a mixture of PANI. Dropwise adding the PANI mixed solution onto a manganese-doped carbon gel material, standing for 15min, carrying out vacuum filtration to remove redundant PANI, dropwise adding a 20mg/ml graphene oxide solution onto the material, standing for 15min, and carrying out vacuum filtration to remove redundant graphene oxide solution. Repeating the operation 29 times to obtain manganese-doped carbon gel @ (PANI/GO)30A material.
Claims (1)
1. The preparation method of the manganese-doped carbon gel @ (PANI/GO) n// NGA @ PEDOT electrode material comprises the following steps:
preparation of NGA @ PEDOT
(1) Dissolving melamine in a graphene oxide solution, sequentially adding VC and ammonia water, performing ultrasonic treatment at 1-4 ℃ to completely dissolve the melamine, then forming organogel in the mixed solution at 80 ℃ by using a water bath method, and firing the organogel at 600-1200 ℃ for 2h in an inert atmosphere to obtain NGA, wherein the concentration of the graphene oxide solution is 0.5-20mg/ml, the mass ratio of graphene oxide to VC is 1:1, and the mass ratio of graphene oxide to ammonia water is 4: 1; the mass ratio of the melamine to the graphene oxide is 1:200-5: 100; NGA is nitrogen-doped graphene gel; VC is vitamin C;
(2) adding NGA into butyl acetate, wherein the content of NGA is 15 wt.%, adding EDOT according to the proportion of 50 μ l/ml, and performing ultrasonic treatment for 1 h; EDOT is 3, 4-ethylenedioxythiophene;
(3) dissolving ferric p-toluenesulfonate in a mixed solution of ethanol and water, wherein the volume ratio of ethanol to water is 3:1, the content of the ferric p-toluenesulfonate is 0.6 wt.%, dripping the solution on the material obtained in the step (2), ultrasonically mixing, and standing at room temperature for polymerization to obtain the NGA @ PEDOT material;
preparation of manganese-doped carbon gel @ (PANI/GO) n
(1) Preparing the manganese-doped carbon gel material
Resorcinol, formaldehyde and manganese acetate are used as precursors, sodium carbonate is used as a catalyst, wherein the molar ratio of resorcinol to formaldehyde is 1:2, the molar ratio of resorcinol to sodium carbonate is 250:1-800:1, and the manganese content is 0.5-3 wt.%; then putting the mixture into a sealed cylindrical glass tube, aging the mixture for 2 days at 30 ℃, aging the mixture for 5 days at 80 ℃, and putting the mixture into acetone for extraction for 2 days to obtain a manganese-doped carbon gel electrode material;
(2) stirring PANI and DMAc in a mass ratio of 1:47 for 12 hours to obtain a mixture, adding HCl into the mixture to enable the pH value of the mixed solution to be 2.5 and the concentration of the PANI to be 0.5mg/ml, and then performing ultrasonic treatment at 1-4 ℃ for 3 hours; PANI is polyaniline; DMAc is dimethylacetamide;
(3) dropwise adding the PANI mixed solution obtained in the step (2) onto the manganese-doped carbon gel material obtained in the step (1), standing for 15min, removing redundant PANI mixed solution through vacuum filtration, dropwise adding a graphene oxide solution onto the manganese-doped carbon gel, standing for 15min, and removing redundant graphene oxide solution through vacuum filtration; wherein the concentration of the graphene oxide solution is 0.5-20 mg/ml;
(4) repeating the step (3) n-1 times to obtain the manganese-doped carbon gel @ (PANI/GO) n material.
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