CN109950052A - A kind of preparation method of supercapacitor - Google Patents
A kind of preparation method of supercapacitor Download PDFInfo
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- CN109950052A CN109950052A CN201910222004.7A CN201910222004A CN109950052A CN 109950052 A CN109950052 A CN 109950052A CN 201910222004 A CN201910222004 A CN 201910222004A CN 109950052 A CN109950052 A CN 109950052A
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- electrode
- quantum dot
- black phosphorus
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
The invention discloses a kind of preparation methods of supercapacitor, and porous nitrogen-doped graphene electrode is prepared first；Cathode is made with obtained porous nitrogen-doped graphene electrode again, platinum electrode makees anode, and black phosphorus quantum dot dispersion liquid makees electrolyte assembling electrolytic cell, obtains black phosphorus quantum dot/porous nitrogen-doped graphene composite material after the reaction was completed；Using obtained black phosphorus quantum dot/porous nitrogen-doped graphene composite material as electrode, supercapacitor is assembled into conjunction with electrolyte.This method processing step is simple, by the black phosphorus quantum dot with good fake capacitance performance/porous nitrogen-doped graphene combination electrode, prepared supercapacitor is made to have excellent chemical property.
Description
Technical field
The present invention relates to new energy memory device technical field more particularly to a kind of preparation methods of supercapacitor.
Background technique
Supercapacitor is a kind of more common electrochemical energy storage device, has good service performance, as power is close
Degree is high, has extended cycle life, safety and environmental protection etc..In the field that some pairs of power densities have higher requirements, such as electric car, wind-force hair
It has a wide range of applications in electricity and large-scale pulsing unit.It is unique derived from it however compared with widely used secondary ion battery
Fake capacitance energy storage mechnism, the energy density of supercapacitor is lower, and application range is significantly restrained.To improve super electricity
The energy density of container, preparation different type, heterogeneity combination electrode material and by its with redox property
Electrolyte phase cooperation is a kind of effective method to use, this will effectively improve the chemical property of supercapacitor.
Wherein taking that efficiently easy method carrys out the preferable combination electrode of processability is one of committed step, but existing skill
The generally existing compound non-uniform phenomenon of compound prepared by solution dispersion method in art, it is difficult to obtain finely dispersed compound
Object, therefore there is important Practical significance to prepare electrode material using efficient easy, well dispersed Electrochemical adsorption method,
It is also of great significance to the use scope of broadening supercapacitor simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of supercapacitor, this method processing step is simple, passes through tool
There is black phosphorus quantum dot/porous nitrogen-doped graphene combination electrode of good fake capacitance performance, makes prepared super capacitor utensil
There is excellent chemical property.
The purpose of the present invention is what is be achieved through the following technical solutions:
A kind of preparation method of supercapacitor, which comprises
It is step 1, Aqueous Adhesives are soluble in water, it is configured to the homogeneous solution that mass fraction is 7%, then by porous nitrogen
Doped graphene is placed in the solution and forms mixed solution；
Step 2 will be coated on stainless steel base, vacuum drying after being formed by mixed solution ultrasonic disperse 10-30min
Porous nitrogen-doped graphene electrode is obtained after 24-48h；
1-100mg black phosphorus quantum dot is distributed in the organic solution of 1-100ml by step 3 again, after ultrasonic disperse 1-6h
To black phosphorus quantum dot dispersion liquid；
Step 4 makees cathode with obtained porous nitrogen-doped graphene electrode, and platinum electrode makees anode, obtained black phosphorus
Quantum dot dispersion liquid makees electrolyte assembling electrolytic cell；
Step 5 applies 0.1-3V voltage to the electrolytic cell being assembled into, and keeps 0.1-6h, after the completion by porous N doping
Graphene electrodes carry out vacuum drying 24-48h, obtain black phosphorus quantum dot/porous nitrogen-doped graphene composite material；
It is step 6, again that active electrolyte is soluble in water, electrolyte is obtained, wherein the concentration of active electrolyte is 0.1-
2mol/L, and acid compound is added into the electrolyte, make the pH value 0.001-7 of electrolyte；
Step 7, using obtained black phosphorus quantum dot/porous nitrogen-doped graphene composite material as electrode, in conjunction with the electricity
Solution liquid is assembled into supercapacitor.
In step 1, the mass ratio of porous nitrogen-doped graphene and Aqueous Adhesives is 7:3 to 9:1 in mixed solution.
In step 1, the specific surface area of the porous nitrogen-doped graphene is 300-2000m2/ g, pore-size distribution are
0.001-20nm, nitrogen percent 1-5%.
In step 1, the Aqueous Adhesives include brown seaweed glue, gelatin, sodium carboxymethylcellulose, polyvinyl alcohol,
One of polyacrylamide, polyacrylic acid, polyethylene glycol oxide, polyethylene glycol, polymaleic anhydride are a variety of；And the water-base cement
The purity of glutinous agent is 99.9% or more.
In step 3: the size of the black phosphorus quantum dot is 1-20nm；
The organic solution include tetrahydrofuran, ethylene carbonate, propene carbonate, chloroform, in N methyl pyrrolidone
It is one or more.
In step 6: the active electrolyte include the ionizable compound of iodide ion or bromide ion, hydroquinone and its
One of derivative, p-phenylenediamine and its derivative are a variety of；
The acid compound being added includes one of hydrochloric acid, sulfuric acid, nitric acid, acetic acid, formic acid or a variety of.
The electrode spacing of the supercapacitor is 10-100 microns.
As seen from the above technical solution provided by the invention, above method processing step is simple, good by having
The black phosphorus quantum dot of fake capacitance performance/porous nitrogen-doped graphene combination electrode has prepared supercapacitor excellent
Chemical property.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, required use in being described below to embodiment
Attached drawing be briefly described, it should be apparent that, drawings in the following description are only some embodiments of the invention, for this
For the those of ordinary skill in field, without creative efforts, it can also be obtained according to these attached drawings other
Attached drawing.
Fig. 1 is the preparation method flow diagram of supercapacitor provided in an embodiment of the present invention；
Fig. 2 is the assembly structure diagram of the supercapacitor of the method for embodiment of the present invention preparation；
Fig. 3 is the cyclic voltammetry curve schematic diagram of supercapacitor in example of the present invention.
Specific embodiment
With reference to the attached drawing in the embodiment of the present invention, technical solution in the embodiment of the present invention carries out clear, complete
Ground description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based on this
The embodiment of invention, every other implementation obtained by those of ordinary skill in the art without making creative efforts
Example, belongs to protection scope of the present invention.
The embodiment of the present invention is described in further detail below in conjunction with attached drawing, is implemented as shown in Figure 1 for the present invention
The preparation method flow diagram for the supercapacitor that example provides, which comprises
It is step 1, Aqueous Adhesives are soluble in water, it is configured to the homogeneous solution that mass fraction is 7%, then by porous nitrogen
Doped graphene is placed in the solution and forms mixed solution；
In this step, the mass ratio of porous nitrogen-doped graphene and Aqueous Adhesives is 7:3 to 9:1 in mixed solution.
In the specific implementation, the specific surface area of above-mentioned porous nitrogen-doped graphene is 300-2000m2/ g, pore-size distribution are
0.001-20nm, nitrogen percent 1-5%.
Above-mentioned Aqueous Adhesives include brown seaweed glue, gelatin, sodium carboxymethylcellulose, polyvinyl alcohol, polyacrylamide,
One of polyacrylic acid, polyethylene glycol oxide, polyethylene glycol, polymaleic anhydride are a variety of；And the purity of the Aqueous Adhesives
It is 99.9% or more.
Step 2 will be coated on stainless steel base, vacuum drying after being formed by mixed solution ultrasonic disperse 10-30min
Porous nitrogen-doped graphene electrode is obtained after 24-48h；
1-100mg black phosphorus quantum dot is distributed in the organic solution of 1-100ml by step 3 again, after ultrasonic disperse 1-6h
To black phosphorus quantum dot dispersion liquid；
In this step, the size of the black phosphorus quantum dot is 1-20nm；
The organic solution include tetrahydrofuran, ethylene carbonate, propene carbonate, chloroform, in N methyl pyrrolidone
It is one or more.
Step 4 makees cathode with obtained porous nitrogen-doped graphene electrode, and platinum electrode makees anode, obtained black phosphorus
Quantum dot dispersion liquid makees electrolyte assembling electrolytic cell；
Step 5 applies 0.1-3V voltage to the electrolytic cell being assembled into, and keeps 0.1-6h, after the completion by porous N doping
Graphene electrodes carry out vacuum drying 24-48h, obtain black phosphorus quantum dot/porous nitrogen-doped graphene composite material；
It is step 6, again that active electrolyte is soluble in water, electrolyte is obtained, wherein the concentration of active electrolyte is 0.1-
2mol/L, and acid compound is added into the electrolyte, make the pH value 0.001-7 of electrolyte；
In this step, the active electrolyte include the ionizable compound of iodide ion or bromide ion, hydroquinone and
One of its derivative, p-phenylenediamine and its derivative are a variety of；
The acid compound being added includes one of hydrochloric acid, sulfuric acid, nitric acid, acetic acid, formic acid or a variety of.
Step 7, using obtained black phosphorus quantum dot/porous nitrogen-doped graphene composite material as electrode, in conjunction with the electricity
Solution liquid is assembled into supercapacitor.
It is illustrated in figure 2 the assembly structure diagram of the supercapacitor of the method for embodiment of the present invention preparation, in figure
The electrode spacing of supercapacitor is 10-100 microns.
Above-mentioned preparation method is described in detail with specific example below:
It is example 1, brown seaweed glue is soluble in water, it is configured to the homogeneous solution that mass fraction is 7%, then by porous nitrogen
Doped graphene is placed in the solution and forms mixed solution, porous nitrogen-doped graphene and brown seaweed glue in the mixed solution
Mass ratio is 7:3.
By coating after this mixed solution ultrasonic disperse 10min on stainless steel base, vacuum drying for 24 hours, obtains electrode 1.
1mg black phosphorus quantum dot is distributed in 20ml tetrahydrofuran, ultrasonic disperse 2h, obtains black phosphorus quantum dot dispersion liquid.
Make cathode with electrode 1, platinum electrode makees anode, and black phosphorus quantum dot dispersion liquid makees electrolyte assembling electrolytic cell.To electrolysis
Pond applies 0.5V voltage, and keeps 0.5h, is after the completion dried in vacuo for 24 hours electrode 1, obtains black phosphorus quantum dot/porous nitrogen
Doped graphene composite material.
Potassium iodide is soluble in water, solution 1 is obtained, wherein the concentration of potassium iodide is 0.1mol/L, and salt is added into solution
Acid makes ph value 0.001.
Electrode is done with black phosphorus quantum dot/porous nitrogen-doped graphene composite material, solution 1 is that electrolyte assembles super capacitor
Device is illustrated in figure 3 the cyclic voltammetry curve schematic diagram of supercapacitor in example of the present invention, as shown in Figure 3: due to this
Using black phosphorus quantum dot/porous nitrogen-doped graphene composite material as electrode material in example, the porosity of electrode material is utilized
With fake capacitance characteristic, and combine redox active electrolyte fake capacitance characteristic, so that supercapacitor greatly improved
Energy density.
It is example 2, gelatin is soluble in water, it is configured to the homogeneous solution that mass fraction is 7%, then by porous N doping stone
Black alkene is placed in the solution and forms mixed solution, and the mass ratio of porous nitrogen-doped graphene and gelatin is 8:2 in the mixed solution.
By coating after this mixed solution ultrasonic disperse 30min on stainless steel base, it is dried in vacuo 36h, obtains electrode 1.
5mg black phosphorus quantum dot is distributed in 50ml propene carbonate, ultrasonic disperse 3h, obtains the dispersion of black phosphorus quantum dot
Liquid.
Make cathode with electrode 1, platinum electrode makees anode, and black phosphorus quantum dot dispersion liquid makees electrolyte assembling electrolytic cell.To electrolysis
Pond applies 1V voltage, and keeps 1h, and electrode 1 is carried out vacuum drying 36h after the completion, obtains black phosphorus quantum dot/porous N doping
Graphene composite material.
Potassium bromide is soluble in water, solution 1 is obtained, wherein the concentration of potassium bromide is 0.3mol/L, and sulphur is added into solution
Acid makes ph value 0.01.Electrode is done with black phosphorus quantum dot/porous nitrogen-doped graphene composite material, solution 1 is electrolyte assembling
Supercapacitor.
It is example 3, sodium carboxymethylcellulose is soluble in water, it is configured to the homogeneous solution that mass fraction is 7%, it then will be more
Hole nitrogen-doped graphene is placed in the solution and forms mixed solution, and porous nitrogen-doped graphene and carboxymethyl are fine in the mixed solution
The mass ratio for tieing up plain sodium is 9:1.
By coating after this mixed solution ultrasonic disperse 20min on stainless steel base, it is dried in vacuo 48h, obtains electrode 1.
10mg black phosphorus quantum dot is distributed in the mixed solution of 50ml propene carbonate and 10ml ethylene carbonate, ultrasound
Disperse 4h, obtains black phosphorus quantum dot dispersion liquid.
Make cathode with electrode 1, platinum electrode makees anode, and black phosphorus quantum dot dispersion liquid makees electrolyte assembling electrolytic cell.To electrolysis
Pond applies 2V voltage, and keeps 2h, and electrode 1 is carried out vacuum drying 48h after the completion, obtains black phosphorus quantum dot/porous N doping
Graphene composite material.
Potassium bromide is soluble in water, solution 1 is obtained, wherein the concentration of p-phenylenediamine is 2mol/L, and second is added into solution
Acid makes ph value 3.Electrode is done with black phosphorus quantum dot/porous nitrogen-doped graphene composite material, solution 1 is that electrolyte assembling is super
Grade capacitor.
It is example 4, polyacrylamide is soluble in water, it is configured to the homogeneous solution that mass fraction is 7%, then by porous nitrogen
Doped graphene is placed in the solution and forms mixed solution, porous nitrogen-doped graphene and polyacrylamide in the mixed solution
Mass ratio is 9:1.
By coating after this mixed solution ultrasonic disperse 30min on stainless steel base, vacuum drying for 24 hours, obtains electrode 1.
70mg black phosphorus quantum dot is distributed in the mixed solution of 100ml chloroform and 50ml tetrahydrofuran, ultrasonic disperse 6h,
Obtain black phosphorus quantum dot dispersion liquid.
Make cathode with electrode 1, platinum electrode makees anode, and black phosphorus quantum dot dispersion liquid makees electrolyte assembling electrolytic cell.To electrolysis
Pond applies 3V voltage, and keeps 5h, and electrode 1 is carried out vacuum drying 48h after the completion, obtains black phosphorus quantum dot/porous N doping
Graphene composite material.
Potassium bromide and hydroquinone is soluble in water, solution 1 is obtained, wherein the concentration of potassium bromide is 1mol/L, to benzene two
The concentration of phenol is 3mol/L, and potassium acid is added into solution, makes ph value 2.It is compound with black phosphorus quantum dot/porous nitrogen-doped graphene
Material does electrode, and solution 1 is that electrolyte assembles supercapacitor.
It is worth noting that, the content being not described in detail in the embodiment of the present invention belongs to professional and technical personnel in the field's public affairs
The prior art known.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Within the technical scope of the present disclosure, any changes or substitutions that can be easily thought of by anyone skilled in the art,
It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of claims
Subject to enclosing.
Claims (7)
1. a kind of preparation method of supercapacitor, which is characterized in that the described method includes:
It is step 1, Aqueous Adhesives are soluble in water, it is configured to the homogeneous solution that mass fraction is 7%, then by porous N doping
Graphene is placed in the solution and forms mixed solution；
Step 2 will be coated on stainless steel base after being formed by mixed solution ultrasonic disperse 10-30min, be dried in vacuo 24-
Porous nitrogen-doped graphene electrode is obtained after 48h；
1-100mg black phosphorus quantum dot is distributed in the organic solution of 1-100ml by step 3 again, is obtained after ultrasonic disperse 1-6h black
Phosphorus quantum dot dispersion liquid；
Step 4 makees cathode with obtained porous nitrogen-doped graphene electrode, and platinum electrode makees anode, obtained black phosphorus quantum
Point dispersion liquid makees electrolyte assembling electrolytic cell；
Step 5 applies 0.1-3V voltage to the electrolytic cell being assembled into, and keeps 0.1-6h, after the completion by porous N doping graphite
Alkene electrode carries out vacuum drying 24-48h, obtains black phosphorus quantum dot/porous nitrogen-doped graphene composite material；
It is step 6, again that active electrolyte is soluble in water, electrolyte is obtained, wherein the concentration of active electrolyte is 0.1-2mol/L,
And acid compound is added into the electrolyte, make the pH value 0.001-7 of electrolyte；
Step 7, using obtained black phosphorus quantum dot/porous nitrogen-doped graphene composite material as electrode, in conjunction with the electrolyte
It is assembled into supercapacitor.
2. the preparation method of supercapacitor according to claim 1, which is characterized in that in step 1, more in mixed solution
The mass ratio of hole nitrogen-doped graphene and Aqueous Adhesives is 7:3 to 9:1.
3. the preparation method of supercapacitor according to claim 1, which is characterized in that in step 1, the porous nitrogen is mixed
The specific surface area of miscellaneous graphene is 300-2000m2/ g, pore-size distribution 0.001-20nm, nitrogen percent 1-5%.
4. the preparation method of supercapacitor according to claim 1, which is characterized in that in step 1, the aqueous gluing
Agent include brown seaweed glue, gelatin, sodium carboxymethylcellulose, polyvinyl alcohol, polyacrylamide, polyacrylic acid, polyethylene glycol oxide,
One of polyethylene glycol, polymaleic anhydride are a variety of；And the purity of the Aqueous Adhesives is 99.9% or more.
5. the preparation method of supercapacitor according to claim 1, which is characterized in that in step 3:
The size of the black phosphorus quantum dot is 1-20nm；
The organic solution includes one of tetrahydrofuran, ethylene carbonate, propene carbonate, chloroform, N methyl pyrrolidone
Or it is a variety of.
6. the preparation method of supercapacitor according to claim 1, which is characterized in that in step 6:
The active electrolyte includes ionizable compound, hydroquinone and its derivative of iodide ion or bromide ion, to benzene two
One of amine and its derivative are a variety of；
The acid compound being added includes one of hydrochloric acid, sulfuric acid, nitric acid, acetic acid, formic acid or a variety of.
7. the preparation method of supercapacitor according to claim 1, which is characterized in that
The electrode spacing of the supercapacitor is 10-100 microns.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015016700A1 (en) * | 2013-07-30 | 2015-02-05 | Universiti Putra Malaysia | Method for preparing catalysst-assisted polypyrrole nanoparticles decorated graphene film for high-performance supercapacitor |
| CN104701019A (en) * | 2015-03-27 | 2015-06-10 | 湖北科技学院 | Preparation method of composite counter electrode for quantum dot-sensitized solar cell |
| CN106892426A (en) * | 2017-03-24 | 2017-06-27 | 福州大学 | The preparation method of Graphene and black phosphorus quantum dot composite material |
| CN107176595A (en) * | 2017-05-24 | 2017-09-19 | 北京石油化工学院 | A kind of phosphorus alkene graphene composite material and preparation method thereof |
| CN107275109A (en) * | 2017-06-21 | 2017-10-20 | 太原理工大学 | Preparation method for the manganese dioxide composite material electrode of ultracapacitor |
-
2019
- 2019-03-22 CN CN201910222004.7A patent/CN109950052A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015016700A1 (en) * | 2013-07-30 | 2015-02-05 | Universiti Putra Malaysia | Method for preparing catalysst-assisted polypyrrole nanoparticles decorated graphene film for high-performance supercapacitor |
| CN104701019A (en) * | 2015-03-27 | 2015-06-10 | 湖北科技学院 | Preparation method of composite counter electrode for quantum dot-sensitized solar cell |
| CN106892426A (en) * | 2017-03-24 | 2017-06-27 | 福州大学 | The preparation method of Graphene and black phosphorus quantum dot composite material |
| CN107176595A (en) * | 2017-05-24 | 2017-09-19 | 北京石油化工学院 | A kind of phosphorus alkene graphene composite material and preparation method thereof |
| CN107275109A (en) * | 2017-06-21 | 2017-10-20 | 太原理工大学 | Preparation method for the manganese dioxide composite material electrode of ultracapacitor |
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| Title |
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| LONG PAN: ""Molecular level distribution of black phosphorus quantum dots on nitrogendoped graphene nanosheets for superior lithium storage"", 《NANO ENERGY》 * |
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