CN113593929B - Electrochemical application and preparation method of aminated nano graphene - Google Patents
Electrochemical application and preparation method of aminated nano graphene Download PDFInfo
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- H—ELECTRICITY
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- 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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
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- 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
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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
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Abstract
The invention belongs to the field of material preparation, and provides electrochemical application of aminated nano-graphene and a preparation method thereof. Performing microwave digestion on acidic graphene oxide and amination agent polyaniline by using an amination mode to obtain emeraldine salt, quinoneamine (═ N-), amine (-NH-) and positively charged nitrogen cation free radical (N) with polyaniline in a semi-oxidation state under the acidic graphene oxide environment + ) And then, carrying out hydrothermal reduction to obtain the aminated nano graphene composite material with excellent electrochemical performance. The material obtained by the invention has a nano-fiber-shaped porous structure, a large specific surface area and more positively charged nitrogen cation free radicals (N) + ) Promotes better electrochemical performance, can quickly diffuse electrolyte ions after being used in a super capacitor, not only greatly improves specific capacity, but also has better stability.
Description
Technical Field
The invention belongs to the field of material preparation, and relates to electrochemical application of aminated nano-graphene and a preparation method thereof.
Background
With the continuous exhaustion of energy, the new energy storage materials are researched by various national policies. The environmental problem is also a concern of China, so that the environment-friendly energy storage material is popularized and researched. The super capacitor is used for storing electric charge through a conductor surface, so that the larger the effective surface area suitable for gathering electrons is, the larger the capacity is, and the graphene has the larger specific surface area and is an ideal super capacitor energy storage material. Experiments show that the supercapacitor taking the graphene as the electrode material can generate the capacity which is more than 6 times that of a capacitor with the same volume, and the performance of the supercapacitor is greatly improved. The market size of supercapacitors will keep growing rapidly in the future and supercapacitors have started replacing traditional batteries. The super capacitor is made of an electrode material with high specific capacity, high energy density and excellent rate performance, and the super capacitor can maintain high power output and has good reversibility to meet the charge-discharge cycle life. How to produce high-quality nano graphene in batches at low cost is crucial to future development and application.
Graphene (Graphene) is a polymer made of carbon atoms in sp 2 The hybrid tracks form a hexagonal honeycomb lattice two-dimensional carbon nanomaterial. The material has the advantages of high hardness, good toughness, large specific surface area and good energy storage performance. Due to the large specific surface area and the good conductivity of the graphene, the energy storage capacity of the graphene can be greatly enhanced, and more energy sources can be stored. Therefore, there is still much interest in developing low-cost, scalable and eco-friendly graphene preparation methods. However, the graphene is prone to have the problems of long production period, large particle size and easy agglomeration in the use process, so that the electrochemical performance of the graphene is poor. Due to the strong pi-pi interactions forming agglomerated graphene sheets, sufficient channels for electrolyte ion conduction are not provided, resulting in slowing of capacitor activity and rate capability. In order to solve the problem, the electrochemical performance of the graphene is improved by preparing the nano graphene in an amination mode.
At present, a plurality of preparation methods for graphene materials exist at home and abroad, but different preparation methods and preparation conditions have great influence on the structural performance of graphene. The main methods for preparing graphene currently include mechanical exfoliation, microwave solvothermal methods, Chemical Vapor Deposition (CVD), solid-phase microwave irradiation methods, and heat treatment methods. Although the CVD method can prepare graphene with large specific surface area, the process is complex, and the transfer difficulty of the graphene generated on the surface of the Cu substrate is large. And (3) directly carrying out microwave heating on the precursor of the graphite by a solid-phase microwave radiation method, and stripping the precursor of the graphite into single-layer or multi-layer graphene. Although the process is simple, the stripping effect is influenced by long stripping time and high oxygen content in the precursor. The nano graphene prepared by the amination method is low in cost and environment-friendly, and the product can stably exist in water or an organic solvent without subsequent substrate transfer, so that a feasible preparation method is provided for development and electrochemical application of high-quality nano graphene materials.
According to the invention, the nano-graphene is prepared in an amination mode, and polyaniline is used as an amination agent to synthesize the nano-graphene so as to improve the capacitance performance of the graphene. Surface modification of acidic GO. Among many conductive polymer materials, polyaniline, as a conjugated polymer, has the advantages of large theoretical capacity, low cost, easy synthesis and the like, and is an ideal candidate material. Polyaniline has good capacitance performance, but has poor rate performance. In contrast, graphene has excellent rate performance, but due to easy stacking of graphene sheets, the specific capacity is low, and the specific surface area and ion diffusion rate of graphene are greatly reduced. Therefore, with their respective advantages, studies suggest that the combination of one-dimensional (1D) polyaniline nanofibers and two-dimensional (2D) graphene can induce the formation of hybrid structures having inherent dispersibility, high specific surface area, and extraordinary energy storage capacity. Compared with the traditional industrial method, the method has the advantages of low production cost, strong controllability and small energy production density, and has wide application prospect. At present, research work on the aspects of microstructure, performance change and the like of materials is relatively little carried out by the method, most researches on graphene modification are in an exploratory state, and researches on practical application aspects are relatively slow.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a method for preparing a nano graphene composite material with excellent electrochemical performance in an amination mode, so that the nano graphene composite material with high specific capacity is obtained and is applied to a super capacitor.
The technical scheme of the invention is as follows:
a preparation method of aminated nano-graphene comprises the following steps:
(1) preparation of aminated graphene:
2.0g of crystalline flake graphite was mixed with 220mL of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 10:1, and stirred at 45 ℃ for 30 min. And then adding potassium permanganate and graphite in a mass ratio of 6:1-8:1, continuously stirring for 40min, heating to 60 ℃, reacting for 7h, and then continuously heating to 90 ℃ for reacting for 40 min. The solution after the reaction is then cooled naturally to room temperature and is called a cooling liquid. Mixing the cooling liquid with deionized water according to the volume ratio of 1:5, reacting the cooling liquid with hydrogen peroxide according to the volume ratio of 10:1, adding excessive deionized water into the reacted solution, separating and washing the obtained acidic graphene oxide solution, and freeze-drying the acidic graphene oxide solution to obtain acidic graphene oxide powder. The acidic graphene oxide powder prepared by the modified Hummers' method was prepared as a 0.5mg/mL solution. Mixing amination agent powder (accounting for 20% -80% of the total weight of the acidic graphene oxide and the amination agent) in different weight ratios, and putting the mixture into a microwave digestion instrument for amination at 800W for about 1min to obtain an aminated graphene solution.
(2) Synthesizing a nano graphene composite material:
filling the solution in the step (1) into a high-pressure reaction kettle, heating at the temperature of 180-;
wherein the particle diameter of the graphite is 1 mu m, and the solution H 2 SO 4 The concentration is 98%, the nitric acid is 65-68%, the potassium permanganate content is more than 99.5%, the pH value of the acidic graphene oxide is approximately equal to 5-6, and the aminating agent is polyaniline.
Further, the concentrated sulfuric acid and the concentrated nitric acid used in the step (1) are mixed according to the volume ratio of 10:1, potassium permanganate and graphite are added according to the mass ratio of 6:1-8:1, the mixture is strictly mixed according to the volume ratio of 1:5 of cooling liquid and deionized water, then the cooling liquid and hydrogen peroxide are reacted according to the volume ratio of 10:1, and amination is carried out for 1-2 min.
The nano graphene with excellent electrochemical performance prepared by the method is used for manufacturing a button type super capacitor, and comprises the following steps:
(1) preparing an electrode slice: weighing the nitrogen-containing graphene serving as an active substance, acetylene black serving as a conductive agent and polyvinylidene fluoride (PVDF) serving as a binder according to the weight ratio of 80:10:10, adding a proper amount of deionized water, and mixing into slurry. The slurry was applied uniformly (weighed) to 10mm phi nickel foam. Drying at 120 deg.C for 1h under vacuum, tabletting, and weighing.
(2) Assembling the button capacitor: in a vacuum glove box, a lower shell, a current collector (foamed nickel)/positive electrode, a diaphragm and a negative electrode are arrangedThe electrode/current collector (foamed nickel), the gasket, the spring, a proper amount of 6mol/L KOH electrolyte and the upper shell are assembled into the button type super capacitor according to the sequence, and the weight of the button type super capacitor is 50kg/cm 2 And sealing the super capacitor by pressure.
The problems of poor conductivity and low specific capacity caused by high cost, long production period, graphene stacking and large particle size exist in the prior art. The method utilizes the defects of long production period, easy stacking of graphene and large particle size, and utilizes an amination mode to make polyaniline have emeraldine salt in a semi-oxidation state, quinone amine (═ N-), amine (-NH-) and positively charged nitrogen cation free radical (N-), under the environment of acidic graphene oxide by using a microwave digestion instrument through the acidic graphene oxide and an aminating agent polyaniline + ) The nano graphene composite material is formed through electrostatic self-assembly reaction, and the aminated nano graphene composite material with excellent electrochemical performance is obtained through hydrothermal reduction. The obtained aminated nano graphene composite material has the advantages of simple process flow, low cost, easy operation, nano fibrous and porous structure, large specific surface area and more positively charged nitrogen cation free radicals (N) + ) Promotes better electrochemical performance, can quickly diffuse electrolyte ions after being used in a super capacitor, not only greatly improves specific capacity, but also has better stability.
Drawings
FIG. 1 is a SEM (scanning electron microscope) morphology image of a material.
Detailed Description
Example 1
The preparation method of the nano-graphene with excellent electrochemical properties of the embodiment is carried out according to the following steps:
(1) preparation of aminated graphene:
2.0g of flake graphite was mixed with 220mL of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 10:1, and stirred at 45 ℃ for 30 min. And then adding 14.0g of potassium permanganate, continuously stirring for 40min, heating to 60 ℃, reacting for 7h, and then continuously heating to 90 ℃ to react for 40 min. The solution after the reaction is then cooled naturally to room temperature and is called a cooling liquid. Mixing the cooling liquid with deionized water according to the volume ratio of 1:5, reacting the cooling liquid with hydrogen peroxide according to the volume ratio of 10:1, adding excessive deionized water into the reacted solution, separating and washing the obtained acidic graphene oxide solution, and freeze-drying the acidic graphene oxide solution to obtain acidic graphene oxide powder. The acidic graphene oxide powder prepared by the modified Hummers' method was prepared as a 0.5mg/mL solution. Mixing amination agent powder (accounting for 20% of the total weight of the acidic graphene oxide and the amination agent) in different weight ratios, and putting the mixture into a microwave digestion instrument for amination at 800W for 1min to obtain an aminated graphene solution.
(2) Synthesizing a nano graphene composite material:
putting the solution obtained in the step (1) into a high-pressure reaction kettle, heating at 180 ℃ for 3h, adding deionized water for suspension, pouring out the upper layer liquid, and freeze-drying to obtain nano graphene composite material powder;
wherein the particle diameter of the graphite is 1 mu m, and the solution H 2 SO 4 The concentration is 98%, the nitric acid is 65-68%, the potassium permanganate content is more than 99.5%, the pH value of the acidic graphene oxide is approximately equal to 5, and the aminating agent is polyaniline.
Further, mixing concentrated sulfuric acid and concentrated nitric acid used in the step (1) according to a volume ratio of 10:1, adding potassium permanganate and graphite according to a mass ratio of 7:1, mixing the cooling liquid and deionized water according to a strict volume ratio of 1:5, reacting the cooling liquid and hydrogen peroxide according to a volume ratio of 10:1, and aminating for 1 min.
The heating temperature in the reaction kettle is 180 ℃, and the reaction time is 3 hours.
The application of the nanographene with excellent electrochemical performance in the embodiment is to use the nanographene for manufacturing a button type supercapacitor, and the method specifically comprises the following steps:
(1) preparing an electrode slice: weighing the nitrogen-containing graphene serving as an active substance, acetylene black serving as a conductive agent and polytetrafluoroethylene serving as a binder according to the weight ratio of 80:10:10 (wt%), adding a proper amount of deionized water, and mixing into a slurry. The slurry was applied uniformly (weighed) to 10mm phi nickel foam. Drying at 120 deg.C for 1h under vacuum, tabletting, and weighing.
(2) Assembling the button capacitor: in a vacuum glove box, a lower shell, a current collector (foamed nickel)/positive electrode, a diaphragm, a negative electrode/current collector (foamed nickel), a gasket, a spring and a proper amount of 6mol/L KOHThe electrolyte and the upper shell are assembled into a button type super capacitor according to the sequence, and the volume of the electrolyte and the upper shell is 50kg/cm 2 The pressure of the sealing cap seals the supercapacitor.
The aminated graphene composite material finally obtained after the steps (1) and (2) has good electron and ion mobility, is applied to preparation of capacitor electrode materials, and has specific capacity of 369F/g under the current density of 0.5A/g.
Example 2
(1) Preparing aminated graphene:
2.0g of crystalline flake graphite was mixed with 220mL of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 10:1, and stirred at 45 ℃ for 30 min. And then adding 16.0g of potassium permanganate, continuously stirring for 40min, heating to 60 ℃, reacting for 7h, and then continuously heating to 90 ℃ to react for 40 min. The solution after the reaction is then cooled naturally to room temperature and is called a cooling liquid. Mixing the cooling liquid with deionized water according to the volume ratio of 1:5, reacting the cooling liquid with hydrogen peroxide according to the volume ratio of 10:1, adding excessive deionized water into the reacted solution, separating and washing the obtained acidic graphene oxide solution, and freeze-drying the acidic graphene oxide solution to obtain acidic graphene oxide powder. The acidic graphene oxide powder prepared by the modified Hummers' method was prepared as a 0.5mg/mL solution. Mixing amination agent powder (accounting for 50% of the total weight of the acidic graphene oxide and the amination agent) in different weight ratios, and putting the mixture into a microwave digestion instrument for amination at 800W for 2min to obtain an aminated graphene solution.
(2) Synthesizing a nano graphene composite material:
putting the solution obtained in the step (1) into a high-pressure reaction kettle, heating at 220 ℃ for 5 hours, adding deionized water for suspension, pouring out the upper layer liquid, and freeze-drying to obtain nano graphene composite material powder;
wherein the particle diameter of the graphite is 1 mu m, and the solution H 2 SO 4 The concentration is 98%, the nitric acid is 68%, the potassium permanganate content is more than 99.5%, the pH value of the acidic graphene oxide is approximately equal to 6, and the aminating agent is polyaniline.
Further, the concentrated sulfuric acid and the concentrated nitric acid used in the step (1) are mixed according to the volume ratio of 10:1, potassium permanganate and graphite are added according to the mass ratio of 8:1, the mixture is strictly mixed according to the volume ratio of 1:5 of cooling liquid and deionized water, then the cooling liquid and hydrogen peroxide are reacted according to the volume ratio of 10:1, and amination is carried out for 2 min.
The heating temperature in the reaction kettle is 220 ℃, and the reaction time is 5 hours.
The application of the nanographene with excellent electrochemical performance in the embodiment is to use the nanographene for manufacturing a button type supercapacitor, and the method specifically comprises the following steps:
(1) preparing an electrode slice: weighing the nitrogen-containing graphene serving as an active substance, acetylene black serving as a conductive agent and polytetrafluoroethylene serving as a binder according to the weight ratio of 80:10:10 (wt%), adding a proper amount of deionized water, and mixing into a slurry. The slurry was uniformly applied to 10mm phi foamed nickel (weighed). Drying at 120 deg.C for 1h under vacuum, tabletting, and weighing.
(2) Assembling the button capacitor: in a vacuum glove box, a lower shell, a current collector (foamed nickel)/positive electrode, a diaphragm, a negative electrode/current collector (foamed nickel), a gasket, a spring, a proper amount of 6mol/L KOH electrolyte and an upper shell are assembled into a button type super capacitor according to the sequence, and 50kg/cm of the current collector/positive electrode, the diaphragm, the negative electrode/current collector (foamed nickel), the gasket, the spring, the proper amount of 6mol/L KOH electrolyte and the upper shell are assembled into the button type super capacitor 2 The pressure of the sealing cap seals the supercapacitor.
The aminated graphene composite material finally obtained after the steps (1) and (2) has good electron and ion mobility, is applied to preparation of capacitor electrode materials, and has specific capacity of 456F/g under the current density of 0.5A/g.
Example 3
(1) Preparation of aminated graphene:
2.0g of flake graphite was mixed with 220mL of concentrated sulfuric acid and concentrated nitric acid at a volume ratio of 10:1, and stirred at 45 ℃ for 30 min. And then adding 12.0g of potassium permanganate, continuously stirring for 40min, heating to 60 ℃, reacting for 7h, and then continuously heating to 90 ℃ to react for 40 min. The solution after the reaction is then cooled naturally to room temperature and is called a cooling liquid. Mixing the cooling liquid with deionized water according to the volume ratio of 1:5, reacting the cooling liquid with hydrogen peroxide according to the volume ratio of 10:1, adding excessive deionized water into the reacted solution, separating and washing the obtained acidic graphene oxide solution, and freeze-drying the acidic graphene oxide solution to obtain acidic graphene oxide powder. The acidic graphene oxide powder prepared by the modified Hummers' method was prepared as a 0.5mg/mL solution. Mixing amination agent powder (accounting for 80% of the total weight of the acidic graphene oxide and the amination agent) in different weight ratios, and putting the mixture into a microwave digestion instrument for amination at 800W for 1min to obtain an aminated graphene solution.
(2) Synthesizing a nano graphene composite material:
putting the solution obtained in the step (1) into a high-pressure reaction kettle, heating at 200 ℃ for 5 hours, adding deionized water for suspension, pouring out the upper layer liquid, and freeze-drying to obtain nano graphene composite material powder;
wherein the particle diameter of the graphite is 1 mu m, and the solution H 2 SO 4 The concentration is 98%, the nitric acid is 65%, the potassium permanganate content is more than 99.5%, the pH value of the acidic graphene oxide is approximately equal to 5, and the aminating agent is polyaniline.
Further, mixing concentrated sulfuric acid and concentrated nitric acid used in the step (1) according to a volume ratio of 10:1, adding potassium permanganate and graphite according to a mass ratio of 6:1, mixing the cooling liquid and deionized water according to a strict volume ratio of 1:5, reacting the cooling liquid and hydrogen peroxide according to a volume ratio of 10:1, and aminating for 1 min.
The heating temperature in the reaction kettle is 200 ℃, and the reaction time is 5 hours.
The nano graphene with excellent electrochemical performance of the embodiment is used for manufacturing a button type supercapacitor, and the method specifically comprises the following steps:
(1) preparing an electrode slice: weighing the nitrogen-containing graphene serving as an active substance, acetylene black serving as a conductive agent and polytetrafluoroethylene serving as a binder according to the weight ratio of 80:10:10 (wt%), adding a proper amount of deionized water, and mixing into a slurry. The slurry was applied uniformly (weighed) to 10mm phi nickel foam. Drying at 120 deg.C for 1h under vacuum, tabletting, and weighing.
(2) Assembling the button capacitor: in a vacuum glove box, a lower shell, a current collector (foamed nickel)/positive electrode, a diaphragm, a negative electrode/current collector (foamed nickel), a gasket, a spring, a proper amount of 6mol/L KOH electrolyte and an upper shell are assembled into a button type super capacitor according to the sequence, and 50kg/cm of the current collector/positive electrode, the diaphragm, the negative electrode/current collector (foamed nickel), the gasket, the spring, the proper amount of 6mol/L KOH electrolyte and the upper shell are assembled into the button type super capacitor 2 The pressure of the sealing cap seals the supercapacitor.
The aminated graphene composite material finally obtained after the steps (1) and (2) has good electron and ion mobility, is applied to preparation of capacitor electrode materials, and has specific capacity of 584F/g under the current density of 0.5A/g.
As shown in fig. 1, the micro-morphology of the nanographene composite was analyzed. Polyaniline fibers are embedded in the honeycomb porous structures and have high content. Polyaniline with uniform particle size can be uniformly dispersed in the cellular graphene, and the material is a nano-structure composite material.
Claims (4)
1. The preparation method of aminated nano graphene is characterized by comprising the following steps:
(1) preparation of aminated graphene
Mixing 2.0g of flake graphite with 220mL of concentrated sulfuric acid and concentrated nitric acid according to a volume ratio of 10:1, and stirring for 30min at 45 ℃; then adding 12.0g of potassium permanganate, continuously stirring for 40min, heating to 60 ℃, reacting for 7h, and then continuously heating to 90 ℃ to react for 40 min; then the solution after reaction is naturally cooled to room temperature and is called as cooling liquid; mixing the cooling liquid with deionized water according to the volume ratio of 1:5, reacting the cooling liquid with hydrogen peroxide according to the volume ratio of 10:1, adding excessive deionized water into the reacted solution, separating and washing the obtained acidic graphene oxide solution, and freeze-drying the acidic graphene oxide solution to obtain acidic graphene oxide powder; preparing acidic graphene oxide powder into a 0.5mg/mL solution; mixing amination agent powder which accounts for 20% -80% of the total weight of the acidic graphene oxide and the amination agent, and putting the mixture into a microwave digestion instrument for amination at 800W for 1min to obtain an aminated graphene solution;
(2) synthesizing a nano graphene composite material:
and (3) filling the solution in the step (1) into a high-pressure reaction kettle, heating at the temperature of 180 ℃ for 220 ℃, heating for 3-5h, adding deionized water for suspension, pouring out the upper layer liquid, and freeze-drying to obtain nano graphene composite material powder.
2. The method for preparing aminated nanographene according to claim 1, wherein the acidic graphene oxide has a pH =5-6, and the aminating agent is polyaniline.
3. The method for preparing aminated nano graphene according to claim 1 or 2, wherein said graphite particle size is 1 μm, and said H is 2 SO 4 The concentration is 98%, the nitric acid is 65-68%, and the potassium permanganate content is more than 99.5%.
4. The application of the nano graphene composite material prepared by the preparation method of any one of claims 1 to 3 in manufacturing a button type supercapacitor comprises the following steps:
(1) preparing an electrode slice: weighing the nano graphene composite material, acetylene black serving as a conductive agent and polyvinylidene fluoride (PVDF) serving as a binder according to the weight ratio of 80:10:10, adding a proper amount of deionized water, and mixing into slurry; uniformly coating the slurry on foam nickel with phi =10 mm; drying at 120 deg.C for 1h under vacuum, tabletting, and weighing;
(2) assembling the button capacitor: in a vacuum glove box, a lower shell, a foamed nickel/positive electrode, a diaphragm, a negative electrode/foamed nickel, a gasket, a spring, 6mol/L KOH electrolyte and an upper shell are assembled into a button type super capacitor in this order, and 50kg/cm is used 2 The pressure of the sealing cap seals the supercapacitor.
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| CN102115598A (en) * | 2010-01-06 | 2011-07-06 | 海洋王照明科技股份有限公司 | Graphene-polyaniline composite material and preparation method thereof |
| CN104229781A (en) * | 2014-09-09 | 2014-12-24 | 东莞市翔丰华电池材料有限公司 | Method for preparing nitrogen-doped graphene with high nitrogen doping amount |
| CN106946246A (en) * | 2017-04-27 | 2017-07-14 | 山东金城石墨烯科技有限公司 | A kind of preparation method of amination graphene |
| CN111591981A (en) * | 2020-04-21 | 2020-08-28 | 东北大学 | Preparation method of low-layer gauze-shaped nitrogen-doped graphene |
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| JP2014093412A (en) * | 2012-11-02 | 2014-05-19 | Yokohama Rubber Co Ltd:The | Polyaniline/graphene complex, and electrode material using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102115598A (en) * | 2010-01-06 | 2011-07-06 | 海洋王照明科技股份有限公司 | Graphene-polyaniline composite material and preparation method thereof |
| CN104229781A (en) * | 2014-09-09 | 2014-12-24 | 东莞市翔丰华电池材料有限公司 | Method for preparing nitrogen-doped graphene with high nitrogen doping amount |
| CN106946246A (en) * | 2017-04-27 | 2017-07-14 | 山东金城石墨烯科技有限公司 | A kind of preparation method of amination graphene |
| CN111591981A (en) * | 2020-04-21 | 2020-08-28 | 东北大学 | Preparation method of low-layer gauze-shaped nitrogen-doped graphene |
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