CN106158409A - A kind of preparation method of manganese dioxide composite graphite alkene foam electrode sheet - Google Patents
A kind of preparation method of manganese dioxide composite graphite alkene foam electrode sheet Download PDFInfo
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- CN106158409A CN106158409A CN201610671690.2A CN201610671690A CN106158409A CN 106158409 A CN106158409 A CN 106158409A CN 201610671690 A CN201610671690 A CN 201610671690A CN 106158409 A CN106158409 A CN 106158409A
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- manganese dioxide
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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
- H01G11/22—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
- H01G11/84—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 present invention provides the preparation method of a kind of nano-manganese dioxide composite graphite alkene foam electrode sheet, including following step: step (1) joins ball milling in ball mill by fine to graphite oxide and polypropylene, then the mixture after ball milling is joined ethanol and ultrasonic disperse in the mixed solution of water, forms suspension；Nickel foam is soaked in above-mentioned suspension by step (2), solvent evaporated, places into the Muffle reaction in furnace of hydrogen nitrogen mixed gas protection, natural cooling after reaction completely；Above-mentioned product be impregnated in hydrochloric acid by step (3), reaction, obtains foamy graphite alkene after reaction completely；Nano-manganese dioxide is joined in toluene by step (4), is ultrasonically formed suspension, then the toluene suspension titration containing manganese dioxide is applied on foamy graphite alkene, is dried, is then placed in Muffle furnace annealing, and after cooling, Kun pressure obtains electrode slice.Electrode slice prepared by the method need not, as adding binding agent and conductive agent in conventional electrodes sheet, reduce the cost of material.
Description
Technical field
The invention belongs to supercapacitor technologies field, particularly relate to a kind of manganese dioxide composite graphite alkene foam electrode
The preparation method of sheet.
Background technology
Graphene is a kind of Novel Carbon Nanomaterials, by monolayer sp2 carbon atom tightly packed one-tenth bi-dimensional cellular shape structure.
Graphene has electricity, calorifics, optics and the mechanical property of excellence.The theoretical specific surface area that Graphene is high simultaneously and excellent electricity
Conductance determines it as electrode material in the great potential of electrochemical energy storing device.
The two-dimensional structure of Graphene uniqueness and outstanding physical characteristic so that it is the application in ultracapacitor has greatly
Ground potentiality.Compared with tradition Dare porous carbon materials, Graphene has the highest electric conductivity, big specific surface area and substantial amounts of
Interlayer constructs, thus becomes the selection of the more promising electrode material of double layer capacitor.But Graphene is in preparation process
It is susceptible to stacking, affects grapheme material dispersibility in the electrolyte and surface wettability, reduce grapheme material
Effective ratio area and electrical conductivity.Therefore, it is to avoid Graphene stacking is to prepare high-energy-density and high power density Graphene
The technical barrier of ultracapacitor.
Summary of the invention
The technical problem to be solved in the present invention is to provide the preparation method of a kind of super capacitor electrode slice, prepared by the method
High-specific surface area, high connductivity grapheme foam compound electric pole piece both can serve as collector, active material can be served as again, negative
The capacity of electrode can be increased again after carrying activated carbon, technical process prepared by ultracapacitor can also be simplified simultaneously, reduce
Its process costs.
The present invention provides the preparation method of a kind of nano-manganese dioxide composite graphite alkene foam electrode sheet to be:
Step (1) joins ball milling 30-60min in ball mill, then by the mixing after ball milling by fine to graphite oxide and polypropylene
Thing joins ethanol and ultrasonic disperse in the mixed solution of water, forms the suspension of concentration 1-20g/L.
Nickel foam is soaked 10-60min, solvent evaporated in above-mentioned suspension by step (2), places into hydrogen nitrogen mixed gas and protects
800-1100 DEG C of reaction 1-10h, natural cooling after reaction completely in the Muffle furnace protected.
Above-mentioned product be impregnated in the hydrochloric acid of 1-3mol/L by step (3), and 60-80 DEG C of reaction 5-10h, after reaction completely
Obtain foamy graphite alkene.
Nano-manganese dioxide is joined in toluene by step (4), and ultrasonic 10-30min forms suspension, then will be containing dioxy
The toluene suspension titration changing manganese is applied on foamy graphite alkene, is dried, and is then placed in 200-300 DEG C of annealing 30-in Muffle furnace
60min, after cooling, Kun pressure obtains electrode slice.
Further, in described step (1), Ball-milling Time is 30-60min；
Further, the 0.01-5% that quality is graphite oxide quality that in described step (1), polypropylene is fine；
Further, in described step (1), in the mixed solution of ethanol and water, the volume ratio of ethanol and water is 0.25-4；
Further, described step (1) is at the suspension that concentration is 1-20g/L of graphite oxide suspension；
Further, in described step (2), nickel foam is immersed in the time in graphite oxide suspension is 10-60min；
Further, in described step (2), the atmosphere in Muffle furnace is the hydrogen nitrogen mixed gas containing 5% hydrogen；
Further, the described step (2) reaction temperature in Muffle furnace is 800-1100 DEG C, and the response time is 1-10h；
Further, in described step (3), concentration of hydrochloric acid is 1-3mol/L；
Further, the described step (3) reaction temperature in hydrochloric acid is 60-80 DEG C, and the response time is 5-10h；
Further, in described step (4), the mass concentration of manganese dioxide toluene suspension is 30-70%；
Further, in described step (4), ultrasonic time is 10-30min；
Further, in described step (4), annealing temperature is 200-300 DEG C, and annealing time is 30-60min；
Further, the thickness of the electrode slice obtained in described step (4) is 100-500um.
There is advantages that (1) high-specific surface area, high conductivity grapheme foam both as collector
Again as active material, simplify preparation technology, reduce cost；(2) after manganese dioxide load, Graphene and manganese dioxide is all
Capacity can be played, the capacity of electrode can be effectively increased；(3) loose structure of grapheme foam can provide effective electronics
And ion conduction channel, it is achieved high-energy-density and high power density；(4) electrode slice prepared by the method need not as conventional electricity
Pole piece adds binding agent and conductive agent, reduces the cost of material.
Accompanying drawing explanation
Fig. 1 is preparation technology flow chart of the present invention.
Detailed description of the invention
Below in conjunction with the accompanying drawings, the preferably embodiment of the present invention is described in further detail:
Embodiment 1
(1) ball milling 30min in ball mill is joined, then by mixing after ball milling by fine to 10g graphite oxide and 0.001g polypropylene
Compound joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 0.25, forms the suspension of concentration 1g/L.
(2) nickel foam is soaked in above-mentioned suspension 10min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
800 DEG C of reaction 10h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 1mol/L, 60 DEG C of reaction 10h, obtain foam stone after reaction completely
Ink alkene.
(4) joining in toluene by nano-manganese dioxide, it is 30% suspension that ultrasonic 10min forms mass concentration, then will contain
The toluene suspension titration having manganese dioxide is applied on foamy graphite alkene, is dried, is then placed in 200 DEG C of annealing in Muffle furnace
60min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination
Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor
Device.
Embodiment 2
(1) ball milling 60min in ball mill is joined, then by the mixing after ball milling by fine to 10g graphite oxide and 0.5g polypropylene
Thing joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 4, forms the suspension of concentration 20g/L.
(2) nickel foam is soaked in above-mentioned suspension 60min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
1100 DEG C of reaction 1h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 3mol/L, 80 DEG C of reaction 5h, obtain foam stone after reaction completely
Ink alkene.
(4) joining in toluene by nano-manganese dioxide, it is 70% suspension that ultrasonic 10-30min forms mass concentration, then
Toluene suspension containing manganese dioxide is titrated and is applied on foamy graphite alkene, be dried, be then placed in Muffle furnace 300 DEG C and move back
Fire 30min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination
Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor
Device.
Embodiment 3
(1) ball milling 45min in ball mill is joined, then by the mixing after ball milling by fine to 10g graphite oxide and 0.1g polypropylene
Thing joins ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 0.5, forms the suspension of concentration 3g/L.
(2) nickel foam is soaked in above-mentioned suspension 30min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
900 DEG C of reaction 5h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 2mol/L, 75 DEG C of reaction 7h, obtain foamy graphite after reaction completely
Alkene.
(4) joining in toluene by nano-manganese dioxide, it is 50% suspension that ultrasonic 20min forms mass concentration, then will contain
The toluene suspension titration having manganese dioxide is applied on foamy graphite alkene, is dried, is then placed in 250 DEG C of annealing in Muffle furnace
450min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination
Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor
Device.
Embodiment 4
(1) ball milling 40min in ball mill is joined, then by the mixture after ball milling by fine to 10g graphite oxide and 3g polypropylene
Join ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 2, form the suspension of concentration 10g/L.
(2) nickel foam is soaked in above-mentioned suspension 50min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
1000 DEG C of reaction 3h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 1.5mol/L, 65 DEG C of reaction 9h, obtain foam stone after reaction completely
Ink alkene.
(4) joining in toluene by nano-manganese dioxide, it is 50% suspension that ultrasonic 15min forms mass concentration, then will contain
The toluene suspension titration having manganese dioxide is applied on foamy graphite alkene, is dried, is then placed in 220 DEG C of annealing in Muffle furnace
40min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination
Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor
Device.
Embodiment 5
(1) ball milling 40min in ball mill is joined, then by the mixture after ball milling by fine to 10g graphite oxide and 1g polypropylene
Join ultrasonic disperse in the mixed solution that ethanol and water volume ratio are 1, form the suspension of concentration 5g/L.
(2) nickel foam is soaked in above-mentioned suspension 20min, solvent evaporated, place into the hydrogen nitrogen mixing containing 5% hydrogen
950 DEG C of reaction 80h, natural cooling after reaction completely in the Muffle furnace of gas shielded.
(3) above-mentioned product be impregnated in the hydrochloric acid of 2.5mol/L, 75 DEG C of reaction 4h, obtain foam stone after reaction completely
Ink alkene.
(4) joining in toluene by nano-manganese dioxide, it is 60% suspension that ultrasonic 25min forms mass concentration, then will contain
The toluene suspension titration having manganese dioxide is applied on foamy graphite alkene, is dried, is then placed in 280 DEG C of annealing in Muffle furnace
35min, after cooling, Kun pressure obtains electrode slice.
(5) according to the preparation technology of usual ultracapacitor by electrode slice, barrier film and electrode slice group by the way of lamination
Becoming battery core, be then injected into electrolyte, the electrolyte of injection is 1mol/L Et4NBF4AN solution, sealing, obtain super capacitor
Device.
Its method is as it is shown in figure 1, its effect is as shown in table 1, as shown in Table 1: the present invention prepares super capacitor energy density and reaches
Arrive 45.3-56.2 Wh/Kg.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Energy density (Wh/Kg) | 45.3 | 55.8 | 47.8 | 56.2 | 54.1 |
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert this
Bright being embodied as is confined to these explanations.For general technical staff of the technical field of the invention, do not taking off
On the premise of present inventive concept, it is also possible to make some simple deduction or replace, all should be considered as belonging to the protection of the present invention
Scope.
Claims (10)
1. the preparation method of a nano-manganese dioxide composite graphite alkene foam electrode sheet, it is characterised in that include following
Step:
Step (1) joins ball milling in ball mill by fine to graphite oxide and polypropylene, is then joined by the mixture after ball milling
Ethanol and ultrasonic disperse in the mixed solution of water, form suspension；
Nickel foam is soaked in above-mentioned suspension by step (2), solvent evaporated, places in the Muffle furnace of hydrogen nitrogen mixed gas protection
Reaction, natural cooling after reaction completely；
Above-mentioned product be impregnated in hydrochloric acid by step (3), reaction, obtains foamy graphite alkene after reaction completely；
Nano-manganese dioxide is joined in toluene by step (4), is ultrasonically formed suspension, then is hanged by the toluene containing manganese dioxide
Supernatant liquid titration is applied on foamy graphite alkene, is dried, is then placed in Muffle furnace annealing, and after cooling, Kun pressure obtains electrode slice.
2. the method for claim 1, it is characterised in that in described step (1), Ball-milling Time is 30-60min；Described step
Suddenly the 0.01-5% that quality is graphite oxide quality that in (1), polypropylene is fine.
3. the method for claim 1, it is characterised in that ethanol and ethanol in the mixed solution of water in described step (1)
It is 0.25-4 with the volume ratio of water；Described step (1) is at the suspension that concentration is 1-20g/L of graphite oxide suspension.
4. the method for claim 1, it is characterised in that in described step (2), nickel foam is immersed in graphite oxide suspension
Time in liquid is 10-60min.
5. the method for claim 1, it is characterised in that in described step (2), the atmosphere in Muffle furnace is containing 5% hydrogen
Hydrogen nitrogen mixed gas.
6. the method for claim 1, it is characterised in that the described step (2) reaction temperature in Muffle furnace is 800-
1100 DEG C, the response time is 1-10h.
7. the method for claim 1, it is characterised in that in described step (3), concentration of hydrochloric acid is 1-3mol/L；At hydrochloric acid
In reaction temperature be 60-80 DEG C, the response time is 5-10h.
8. the method for claim 1, it is characterised in that the quality of manganese dioxide toluene suspension in described step (4)
Concentration is 30-70%；Ultrasonic time is 10-30min.
9. the method for claim 1, it is characterised in that in described step (4), annealing temperature is 200-300 DEG C, annealing
Time is 30-60min.
10. the method for claim 1, it is characterised in that the thickness of the electrode slice obtained in described step (4) is 100-
500um。
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106082179A (en) * | 2016-06-03 | 2016-11-09 | 济南大学 | A kind of preparation method of manganese dioxide composite material |
| WO2018032324A1 (en) * | 2016-08-16 | 2018-02-22 | 肖丽芳 | Method for manufacturing manganese dioxide-graphene foam composite electrode |
| CN109037678A (en) * | 2018-06-15 | 2018-12-18 | 陕西科技大学 | A kind of preparation method of nitrogen sulphur codope three-dimensional graphene foam electrode active material |
| CN110256721A (en) * | 2019-05-20 | 2019-09-20 | 武汉理工大学 | A kind of photo-thermal sponge and its preparation method and application |
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