CN105869909A - Preparation method of composite electrode - Google Patents
Preparation method of composite electrode Download PDFInfo
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- CN105869909A CN105869909A CN201610374113.7A CN201610374113A CN105869909A CN 105869909 A CN105869909 A CN 105869909A CN 201610374113 A CN201610374113 A CN 201610374113A CN 105869909 A CN105869909 A CN 105869909A
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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
- 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
- H01G11/46—Metal oxides
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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 provides a preparation method of a composite electrode. The preparation method includes the steps that firstly, foamed nickel is pretreated with NaOH, HCl and ethyl alcohol; then an oxidized graphene water solution is prepared through a traditional Hummers method; foam Ni of single-layer graphene is prepared through an impregnation method; a graphene/MnO2 nanosheet precursor solution is prepared, wherein the precursor solution comprises a hydrazine hydrate solution, an anhydrous manganese chloride/isopropanol solution and a potassium permanganate water solution; then (MnO2 nanosheet/oxidized graphene)n/single-layer graphene/foam Ni is prepared through a cyclic impregnation method; the obtained electrode is soaked in the hydrazine hydrate solution for a reduction reaction, and the (MnO2 nanosheet/oxidized graphene)n/single-layer graphene/foam Ni composite electrode is obtained. The composite electrode can be used as a supercapacitor electrode material, the preparation process is simple and rapid, no adhesive is needed, and cost is low.
Description
Technical field
The invention belongs to materialogy field, relate to a kind of combination electrode, specifically a kind of (MnO2Nanometer sheet/graphite
Alkene)nThe preparation method of/single-layer graphene/foam Ni combination electrode.
Background technology
Along with the further development of society, environment and energy problem become increasingly to highlight.Therefore people are in the urgent need to one
Plant environmental friendliness and continuable energy storage form.As a kind of emerging energy storage device, ultracapacitor is from once occurring
Cause the great attention of scientist.It is a kind of outstanding energy device between traditional physical capacitor and battery,
There is the advantages such as charging interval short, length in service life, operating temperature range width, it is most important that, it is a kind of environmental type
The energy.And wherein core component is the electrode material of excellent performance, it it is the key factor determining ultracapacitor chemical property
One of, therefore development has the core topic that the electrode material of excellent properties is ultracapacitor research.Ultracapacitor
Electrode material mainly have material with carbon element, transition metal oxide and conducting polymer 3 kinds.Manganese dioxide is as oxo transition metal
Compound, price is low, and electro-chemical activity is high, and environment friendly is high.The theoretical specific capacitance of pure manganese dioxide can reach 1370F/g,
It it is a kind of very promising electrode material.But nanometer MnO2It is easy to group during as electrode material for super capacitor
It is poly-, so that its cyclicity is deteriorated, it could even be possible to lose the excellent properties that nanorize is brought.A lot of researchs show, dioxy
Change manganese and can obtain more preferable capacitive property by modification.Graphene is a kind of monolayer laminated structure being made up of carbon atom
New material.Being a kind of to be formed, with sp2 hybrid orbital, the flat film that hexangle type is honeycomb lattice by carbon atom, only one of which carbon is former
The two-dimensional material of sub-thickness.Graphene is not only one the thinnest in known materials, the most very rigid；As simple substance, it
The speed at room temperature transmitting electronics is faster than known conductor.Graphene-structured is highly stable, and up to now, researcher is sent out not yet
The situation having carbon atom to lack in existing Graphene.In Graphene, the connection between each carbon atom is the most pliable and the toughest, when applying outside machine
During tool power, carbon atom face, with regard to flexural deformation, so that carbon atom need not be rearranged to adapt to external force, has also been maintained for structure steady
Fixed.This stable lattice structure makes carbon atom have outstanding electric conductivity.When electronics in Graphene moves in track, no
Can scatter because of lattice defect or introducing foreign atom.Owing to interatomic force is very strong, at normal temperatures, even if around
Carbon atom telescopes, and in Graphene, electronics experienced interference is the least.If using Graphene as carrier and nanometer MnO2Enter
Row is compound, is possible not only to preferably solve the agglomeration traits of oxide in electrochemistry circulation, and can be greatly improved charge efficiency,
And improve battery capacity, the ultracapacitor of superior performance can be developed into.One is disclosed in patent CN104599854A
Planting the preparation method of the lamellar manganese dioxide/graphene complex being applicable to super capacitor material, this method is at hydro-thermal bar
Preparing under part, condition is harsh, and when preparing electrode, complex process, complex be mixed with conductive agent and binding agent, after closing slurry
Repaste on conducting base, it addition, complex and the ratio of binding agent, close the technique of slurry and be coated with sizing process all to electrode material
Chemical property has large effect.
Summary of the invention
For above-mentioned technical problem of the prior art, the invention provides the preparation method of a kind of combination electrode, utilize
Simple infusion process, prepares the sandwich structure electrode being directly loaded in foam Ni matrix.This combination electrode utilizes strong
The foam Ni of the graphene oxide laying of reduction is matrix, good conductivity；Need not utilize binding agent, internal resistance is low；MnO2 nanometer
Sheet specific surface area is big, forms ion channel with the sandwich structure of Graphene；Three aspects are effectively improved the ratio electric capacity of electrode, main
Solve the technical problem higher than electric capacity.
The invention provides the preparation method of a kind of combination electrode, comprise the steps:
1) step processing foam nickel base, is cut into small pieces by nickel foam, ultrasonic cleaning in 0.01mol/LNaOH
20min, after cleaning with deionized water, ultrasonic cleaning 20min again in the HCl solution of 0.1 ~ 1mol/L, cleans with deionized water
Ultrasonic cleaning 20min in ethanol solution again to neutrality；
2) step of a preparation graphene oxide water solution, utilizes Hummers method to prepare the oxygen that mass mark is 0.1g/L
Functionalized graphene aqueous solution；
3) one process high connductivity foam Ni matrix step, foam nickel base step 1) handled well is in step 2) oxidation
After graphene aqueous solution soaks 30min, then foam nickel base is immersed in the hydrazine hydrate solution of 50mmol/L immersion 4h, it
After again with deionized water rinsing, then be vacuum dried at 80 DEG C, obtain the foam Ni containing single-layer graphene；
4) one prepares Graphene/MnO2The step of nanometer sheet precursor solution, described precursor solution includes that hydrazine hydrate is molten
Liquid, anhydrous Manganese chloride/aqueous isopropanol and potassium permanganate solution, the concentration of hydrazine hydrate solution be respectively 20 mmol/L,
50mmol/L, the concentration of described anhydrous Manganese chloride/aqueous isopropanol is 0.054mol/L, described potassium permanganate solution
Concentration is 0.046mol/L；
5) the foam Ni utilizing the single-layer graphene that step 3) obtains by circulatory maceration is immersed in the graphene oxide of 0.1g/L
In aqueous solution 1～5min, take out after sample dries in 90 DEG C of baking ovens, be immersed in anhydrous Manganese chloride/aqueous isopropanol 1
～5min, after 90 DEG C dry, it is immersed in potassium permanganate solution, is circulated i.e. available (MnO successively2Nanometer sheet/oxidation
Graphene)n/ Graphene/foam Ni combination electrode, wherein n is cycle-index, 1 < n≤5；
6) step 5) the electrode obtained is immersed in the hydrazine hydrate solution 4h of the 20mmol/L of 90 DEG C, it is thus achieved that (MnO2Nanometer sheet/graphite
Alkene)n/ single-layer graphene/foam Ni combination electrode, wherein n is cycle-index, 1 < n≤5.
The present invention utilizes infusion method to prepare the foam Ni of single-layer graphene, strengthens its electric conductivity；Use solution dipping method
Directly by MnO2Nanometer sheet/Graphene growth in situ, on foam Ni skeleton, forms the combination electrode of sandwich, decreases biography
In system technique, the conjunction slurry step in electrode production process, reduces contact resistance, reduces inert matter ratio in the electrodes, enter
And improve specific capacity and energy electrode density of material.Combination electrode can be used for electrode material for super capacitor, its preparation technology
Simple and quick, it is not necessary to use binding agent, energy-conserving and environment-protective, low cost.
The present invention compares with prior art, and its technological progress is significant.(the MnO of the present invention2Nanometer sheet/Graphene)n/
Single-layer graphene/foam Ni composite, its preparation technology is the most controlled, low temperature, quickly, mild condition, low production cost,
After assembling, it is more maximum up to 410Fg than electric capacity-1.And the conjunction slurry step decreased in traditional handicraft in electrode production process
Suddenly, reducing production cost further, newly synthesized complex nano material has good chemical property.
Accompanying drawing explanation
Fig. 1 is embodiment 1 gained (MnO2Nanometer sheet/Graphene)nThe GCD figure of/single-layer graphene/foam Ni composite.
Detailed description of the invention
Embodiment 1
(1) process of foam nickel base
Nickel foam is cut into small pieces, and ultrasonic cleaning 20min in 0.01mol/LNaOH, after cleaning with deionized water, at dilute HCl
Ultrasonic cleaning 20min again in solution, cleans to neutrality ultrasonic cleaning 20min in ethanol solution again with deionized water.
(2) preparation of graphene oxide water solution:
Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L.
(3) high connductivity foam Ni matrix processes
(1) will be handled well in (2) after immersion 30min, after immersion by foam Ni again in the hydrazine hydrate solution of 50mmol/L
Soak 4h, use deionized water rinsing 3 times the most again, then be vacuum dried at 80 DEG C, obtain the foam Ni containing single-layer graphene.
(4) Graphene/MnO2Nanometer sheet precursor solution prepares,
I#Solution: 20mmol/L hydrazine hydrate solution,
II#Solution: 0.054mol/L anhydrous Manganese chloride/aqueous isopropanol,
III#Solution: 0.046mol/L potassium permanganate solution
(5) (MnO2Nanometer sheet/graphene oxide)nPrepared by/single-layer graphene/foam Ni combination electrode,
Utilize circulatory maceration that (3) are immersed in the graphene oxide water solution of 0.1g/L 1～5min, take out sample at 90 DEG C
After baking oven is dried, it is immersed in II#Solution 1～5min, after 90 DEG C dry, is immersed in III#In solution 1～5min,
Circulate i.e. available (MnO successively2Nanometer sheet/graphene oxide)n/ Graphene/foam Ni(n is cycle-index, n=3) compound electric
Pole.
(6) (MnO2Nanometer sheet/Graphene)n/ single-layer graphene/foam Ni
(5) the electrode obtained is immersed in the hydrazine hydrate solution 2h of the 20mmol/L of 90 DEG C, it is thus achieved that (MnO2Nanometer sheet/Graphene)n/
Single-layer graphene/foam Ni(n is cycle-index, n=3).
Utilize the chemical property of CHI660E model electrochemical workstation test sample.With constant current charge charging method
At 0.5Ag-1Under electric current density, recording than electric capacity is 245Fg-1。
Embodiment 2
(1) process of foam nickel base
Nickel foam is cut into small pieces, and ultrasonic cleaning 20min in 0.01mol/LNaOH, after cleaning with deionized water, at dilute HCl
In ultrasonic cleaning 20min again, clean to neutrality ultrasonic cleaning 20min in ethanol solution again with deionized water.
(2) preparation of graphene oxide water solution:
Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L.
(3) high connductivity foam Ni matrix processes
(1) will be handled well in (2) after immersion 30min, after being soaked again by foam Ni in the hydrazine hydrate solution of 50mmol/L
Soak 4h, use deionized water rinsing 3 times the most again, then be vacuum dried at 80 DEG C, obtain the foam Ni containing single-layer graphene.
(4) Graphene/MnO2Nanometer sheet precursor solution prepares,
I#The hydrazine hydrate solution of solution: 20mmol/L,
II#Solution: 0.054mol/L anhydrous Manganese chloride/aqueous isopropanol,
III#Solution: 0.046mol/L potassium permanganate solution
(5) (MnO2Nanometer sheet/graphene oxide)nPrepared by/single-layer graphene/foam Ni combination electrode,
Utilize circulatory maceration that (3) are immersed in the graphene oxide water solution of 0.1g/L 1～5min, take out sample at 90 DEG C
After baking oven is dried, it is immersed in II#Solution 1～5min, after 90 DEG C dry, is immersed in III#In solution 1～5min,
Circulate i.e. available (MnO successively2Nanometer sheet/graphene oxide)n/ single-layer graphene/foam Ni(n is cycle-index, n=4) multiple
Composite electrode.
(6) (MnO2Nanometer sheet/Graphene)n/ single-layer graphene/foam Ni
(5) the electrode obtained is immersed in the hydrazine hydrate solution 2h of the 20mmol/L of 90 DEG C, it is thus achieved that (MnO2Nanometer sheet/Graphene)n/
Single-layer graphene/foam Ni(n is cycle-index, n=4).
Utilize the chemical property of CHI660E model electrochemical workstation test sample.With constant current charge charging method
At 0.5Ag-1Under electric current density, recording than electric capacity is 310Fg-1。
Embodiment 3
(1) process of foam nickel base
Nickel foam is cut into small pieces, and ultrasonic cleaning 20min in 0.01mol/LNaOH, after cleaning with deionized water, at dilute HCl
In ultrasonic cleaning 20min again, clean to neutrality ultrasonic cleaning 20min in ethanol solution again with deionized water.
(2) preparation of graphene oxide water solution:
Hummers method is utilized to prepare the graphene oxide water solution that mass mark is 0.1g/L.
(3) high connductivity foam Ni matrix processes
(1) will be handled well in (2) after immersion 30min, after being soaked again by foam Ni in the hydrazine hydrate solution of 50mmol/L
Soak 4h, use deionized water rinsing 3 times the most again, then be vacuum dried at 80 DEG C, obtain the foam Ni containing single-layer graphene.
(4) Graphene/MnO2Nanometer sheet precursor solution prepares,
I#The hydrazine hydrate solution of solution: 20mmol/L,
II#Solution: 0.054mol/L anhydrous Manganese chloride/aqueous isopropanol,
III#Solution: 0.046mol/L potassium permanganate solution
(5) (MnO2Nanometer sheet/graphene oxide)nPrepared by/single-layer graphene/foam Ni combination electrode,
Utilize circulatory maceration that (3) are immersed in the graphene oxide water solution of 0.1g/L 1～5min, take out sample at 90 DEG C
After baking oven is dried, it is immersed in II#Solution 1～5min, after 90 DEG C dry, is immersed in III#In solution 1～5min,
Circulate i.e. available (MnO successively2Nanometer sheet/graphene oxide)n/ single-layer graphene/foam Ni(n is cycle-index, n=5) multiple
Composite electrode.
(6) (MnO2Nanometer sheet/Graphene)n/ single-layer graphene/foam Ni
(5) the electrode obtained is immersed in the hydrazine hydrate solution 2h of the 20mmol/L of 90 DEG C, it is thus achieved that (MnO2Nanometer sheet/Graphene)n/
Single-layer graphene/foam Ni(n is cycle-index, n=5).
Utilize the chemical property of CHI660E model electrochemical workstation test sample.With constant current charge charging method
At 0.5Ag-1Under electric current density, recording than electric capacity is 410Fg-1。
Claims (1)
1. the preparation method of a combination electrode, it is characterised in that comprise the steps:
1) step processing foam nickel base, is cut into small pieces by nickel foam, ultrasonic cleaning in 0.01mol/LNaOH
20min, after cleaning with deionized water, ultrasonic cleaning 20min again in the HCl solution of 0.1 ~ 1mol/L, cleans with deionized water
Ultrasonic cleaning 20min in ethanol solution again to neutrality；
2) step of a preparation graphene oxide water solution, utilizes Hummers method to prepare the oxygen that mass mark is 0.1g/L
Functionalized graphene aqueous solution；
3) step preparing high connductivity foam Ni matrix, foam nickel base step 1) handled well is in step 2) oxidation
After graphene aqueous solution soaks 30min, then foam nickel base is immersed in the hydrazine hydrate solution of 50mmol/L immersion 4h, it
After again with deionized water rinsing, then be vacuum dried at 80 DEG C, obtain the foam Ni containing single-layer graphene；
4) one prepares Graphene/MnO2The step of nanometer sheet precursor solution, described precursor solution includes that hydrazine hydrate is molten
Liquid, anhydrous Manganese chloride/aqueous isopropanol and potassium permanganate solution, the concentration of hydrazine hydrate solution be respectively 20 mmol/L,
50mmol/L, the concentration of described anhydrous Manganese chloride/aqueous isopropanol is 0.054mol/L, described potassium permanganate solution
Concentration is 0.046mol/L；
5) the foam Ni utilizing the single-layer graphene that step 3) obtains by circulatory maceration is immersed in the graphene oxide of 0.1g/L
In aqueous solution 1～5min, take out after sample dries in 90 DEG C of baking ovens, be immersed in anhydrous Manganese chloride/aqueous isopropanol 1
～5min, after 90 DEG C dry, it is immersed in potassium permanganate solution, is circulated i.e. available (MnO successively2Nanometer sheet/oxidation
Graphene)n/ single-layer graphene/foam Ni combination electrode, wherein n is cycle-index, 1 < n≤5；
6) step 5) the electrode obtained is immersed in the hydrazine hydrate solution 4h of the 20mmol/L of 90 DEG C, it is thus achieved that (MnO2Nanometer sheet/graphite
Alkene)n/ single-layer graphene/foam Ni combination electrode, wherein n is cycle-index, 1 < n≤5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111454482A (en) * | 2020-04-22 | 2020-07-28 | 江苏海洋大学 | Application of water-soluble high molecular polymer in preparation of plastic conductive composite foam |
| CN113979514A (en) * | 2021-10-22 | 2022-01-28 | 周口师范学院 | Ni-based CuFe2O4Preparation method of spinel coating electrode material |
| CN114044912A (en) * | 2021-10-19 | 2022-02-15 | 上海应用技术大学 | Ni-Co-ZIF composite material and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103065813A (en) * | 2012-12-20 | 2013-04-24 | 中国科学技术大学 | Preparing method and application of super capacitor electrode |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103065813A (en) * | 2012-12-20 | 2013-04-24 | 中国科学技术大学 | Preparing method and application of super capacitor electrode |
Non-Patent Citations (3)
| Title |
|---|
| YOUYI SUN等: "Facile synthesis of MnO2/rGO/Ni composite foam with excellent pseudocapacitive behavior for supercapacitors", 《JOURNAL OF ALLOY AND COMPOUNDS》 * |
| ZHANGPENG LI等: "Electrostatic layer-by-layer self-assembly multilayer films based on graphene and manganese dioxide sheets as novel electrode materials for supercapacitors", 《JOURNAL OF MATERIALS CHEMISTRY》 * |
| 刘双宇: "石墨烯基材料的合成及其在储能方面的应用研究", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111454482A (en) * | 2020-04-22 | 2020-07-28 | 江苏海洋大学 | Application of water-soluble high molecular polymer in preparation of plastic conductive composite foam |
| CN111454482B (en) * | 2020-04-22 | 2022-03-22 | 江苏海洋大学 | Application of water-soluble high molecular polymer in preparation of plastic conductive composite foam |
| CN114044912A (en) * | 2021-10-19 | 2022-02-15 | 上海应用技术大学 | Ni-Co-ZIF composite material and preparation method and application thereof |
| CN113979514A (en) * | 2021-10-22 | 2022-01-28 | 周口师范学院 | Ni-based CuFe2O4Preparation method of spinel coating electrode material |
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