CN106298267A - A kind of preparation method of activated carbon composite graphite alkene foam electrode sheet - Google Patents
A kind of preparation method of activated carbon composite graphite alkene foam electrode sheet Download PDFInfo
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- CN106298267A CN106298267A CN201610675647.3A CN201610675647A CN106298267A CN 106298267 A CN106298267 A CN 106298267A CN 201610675647 A CN201610675647 A CN 201610675647A CN 106298267 A CN106298267 A CN 106298267A
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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
- H01G11/66—Current collectors
- H01G11/68—Current collectors 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
- H01G11/66—Current collectors
- H01G11/70—Current collectors characterised by their structure
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/22—Electronic properties
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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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 activated carbon 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；Activated carbon is joined in dehydrated alcohol by step (4), is ultrasonically formed suspension, then the alcohol suspension titration containing activated carbon is applied on foamy graphite alkene, is dried, 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 activated carbon composite graphite alkene foam electrode sheet
Preparation method.
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 activated carbon composite graphite alkene foam electrode sheet,
High-specific surface area, high connductivity grapheme foam compound electric pole piece prepared by the method both can serve as collector, can serve as again
Active material, can increase again the capacity of electrode after load type active carbon, can also simplify work prepared by ultracapacitor simultaneously
Skill process, reduces its process costs.
The present invention provides the preparation method of a kind of activated carbon 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.
Activated carbon is joined in dehydrated alcohol by step (4), and ultrasonic 10-30min forms suspension, then will be containing activated carbon
Alcohol suspension titration be applied on foamy graphite alkene, be dried, after cooling Kun pressure obtain 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 activated carbon alcohol suspension is 30-70%；
Further, in described step (4), ultrasonic time is 10-30min；
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 not only as collector but also make
For active material, simplify preparation technology, reduce cost；(2) activated carbon supported rear Graphene and activated carbon can play
Capacity, can be effectively increased the capacity of electrode；(3) loose structure of grapheme foam can provide effective electronics and ion to pass
Pathway, it is achieved high-energy-density and high power density；(4) electrode slice prepared by the method need not add in conventional electrodes sheet
Adding additives and conductive agent, reduce 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 dehydrated alcohol by activated carbon, it is 30% suspension that ultrasonic 10min forms mass concentration, then will contain
The alcohol suspension titration of activated carbon is applied on foamy graphite alkene, is dried, and is then placed in 200 DEG C of annealing 60min in Muffle furnace,
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 dehydrated alcohol by activated carbon, it is 70% suspension that ultrasonic 10-30min forms mass concentration, then will
Alcohol suspension titration containing activated carbon is applied on foamy graphite alkene, is dried, is then placed in 300 DEG C of annealing in Muffle furnace
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 dehydrated alcohol by activated carbon, it is 50% suspension that ultrasonic 20min forms mass concentration, then will contain
The alcohol suspension titration of activated carbon 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 dehydrated alcohol by activated carbon, it is 50% suspension that ultrasonic 15min forms mass concentration, then will contain
The alcohol suspension titration of activated carbon is applied on foamy graphite alkene, is dried, and is then placed in 220 DEG C of annealing 40min in Muffle furnace,
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 dehydrated alcohol by activated carbon, it is 60% suspension that ultrasonic 25min forms mass concentration, then will contain
The alcohol suspension titration of activated carbon is applied on foamy graphite alkene, is dried, and is then placed in 280 DEG C of annealing 35min in Muffle furnace,
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.
Preparation 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 electrode slice quality specific volume
Amount has reached 298.8-306.1 F/g.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | |
| Specific discharge capacity (F/g) | 299.1 | 298.8 | 306.1 | 302 | 304.5 |
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 an activated carbon 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；
Activated carbon is joined in dehydrated alcohol by step (4), is ultrasonically formed suspension, then by the alcohol suspension containing activated carbon
Titration is applied on foamy graphite alkene, is dried, 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.
3. the method for claim 1, it is characterised in that the quality that in described step (1), polypropylene is fine is graphite oxide
The 0.01-5% of quality.
4. 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.
5. the method for claim 1, it is characterised in that described step (1) is 1-in the concentration of graphite oxide suspension
The suspension of 20g/L.
6. 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.
7. the method for claim 1, it is characterised in that in described step (2), the atmosphere in Muffle furnace is dense containing volume
Spend the hydrogen nitrogen mixed gas of 5% hydrogen；Reaction temperature in Muffle furnace is 800-1100 DEG C, and the response time is 1-10h.
8. 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.
9. the method for claim 1, it is characterised in that in described step (4), the quality of activated carbon alcohol suspension is dense
Degree is 30-70%；Ultrasonic time is 10-30min.
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 (3)
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|---|---|---|---|---|
| CN108054028A (en) * | 2017-11-03 | 2018-05-18 | 佛山科学技术学院 | A kind of preparation method of foam electrode piece |
| CN108899215A (en) * | 2018-06-29 | 2018-11-27 | 成都三乙医疗科技有限公司 | A kind of foam nickel electrode piece preparation method |
| CN110660594A (en) * | 2019-11-18 | 2020-01-07 | 西安合容新能源科技有限公司 | Preparation method of multi-dimensional graphene-based supercapacitor electrode plate |
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