CN106158429A - The method manufacturing graphene-based ultracapacitor - Google Patents
The method manufacturing graphene-based ultracapacitor Download PDFInfo
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- CN106158429A CN106158429A CN201610715291.1A CN201610715291A CN106158429A CN 106158429 A CN106158429 A CN 106158429A CN 201610715291 A CN201610715291 A CN 201610715291A CN 106158429 A CN106158429 A CN 106158429A
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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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- 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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- 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 method that the present invention relates to manufacture graphene-based ultracapacitor, comprises the following steps: be dissolved in dispersion liquid by graphite alkenes material；The dispersion of graphite alkenes material will be dissolved with on collector；The collector being coated with graphite alkenes material solution is dried, and obtains electrode material；Prepare the mixture of electrolyte and polymer；Described mixture is coated on described electrode material surface, is dried Preset Time；It is coated with on the electrode material of mixture described in another described electrode material is placed in, applies preset pressure and be dried.The method manufacturing graphene-based ultracapacitor that the present invention provides, electrolyte layer interpenetrates on surface with electrode material, is in close contact, thus considerably reduces the equivalent series resistance of ultracapacitor to improve the overall performance of ultracapacitor.
Description
Technical field
The present invention relates to capacitor technology field, the method being specifically related to manufacture graphene-based ultracapacitor.
Background technology
In order to solve energy crisis, the development and utilization of regenerative resource proportion shared by human lives increases day by day
Add.In prior art, the energy of the overwhelming majority is required for being converted into electric energy and just can be used effectively, therefore electrochemical energy storing device
Energy market is occupied indispensable status.Slow, the service life based on lithium ion battery product charge rate on market
Shortcoming short, that pollution environment is serious, ultracapacitor developed rapidly in the last few years.As a kind of energy storage device, super capacitor
The performance of device, between battery and ordinary capacitor, has big electric current quick charge and discharge characteristic, high-power energy density, safety
Can be high, have extended cycle life and the feature such as environmental protection.
Ultracapacitor mainly includes a few major part of collector, electrode material, electrolyte, barrier film, and encapsulating material.Weighing apparatus
The important indicator of amount ultracapacitor performance is big electric current quick charge and discharge characteristic and high-power energy density, and big electric current quickly fills
Putting characteristic and high-power energy density depends primarily on equivalent series resistance (ESR), ESR derives from and manufactures each of ultracapacitor
The summation of the resistance of portion of material, depends not only on the selection of each several part material, and closely related with manufacturing process.And it is existing
Production technology in, to using the ultracapacitor of liquid electrolyte, common method be encapsulated electrode material and collector it
After add electrolyte again；And for using the ultracapacitor of solid-state electrolytic solution, conventional way is for preparing electrode material respectively
And solid-state electrolytic solution, then it is combined layer by layer.In these techniques, between collector and electrode material, or electrode material
Fail to be fully contacted between material and electrolyte, thus cause electrode material not tight with the combination of electrolyte layer, thus increase
Add the ESR of ultracapacitor.
Summary of the invention
For defect of the prior art, it is desirable to provide the method manufacturing graphene-based ultracapacitor, so that
Obtain electrolyte layer to interpenetrate on surface with electrode material, be in close contact, thus reduce the equivalent series resistance of ultracapacitor
To improve the overall performance of ultracapacitor.
For solving the problems referred to above, the present invention provides the method manufacturing graphene-based ultracapacitor, comprises the following steps: will
Graphite alkenes material is dissolved in dispersion liquid；The dispersion of graphite alkenes material will be dissolved with on collector；To be coated with
The collector being covered with graphite alkenes material solution is dried, and obtains electrode material；Prepare the mixture of electrolyte and polymer；By institute
State mixture and be coated on described electrode material surface, be dried Preset Time；It is coated with described in another described electrode material is placed in
On the electrode material of mixture, apply preset pressure and be dried.
Graphite alkenes material is dissolved in solution, the solution being dissolved with graphite alkenes material is coated on collector it
On, then be dried, form the graphite alkenes electrode material for super capacitor with loose structure；Electrode material is super as composition
Level capacitor key components, decide the main performance index of ultracapacitor, as energy density, power density and
Cycle life etc.；Up to now, activated carbon, CNT, metal-oxide and conducting polymer etc. are all applied to super
The electrode material of capacitor, but the performance of the ultracapacitor obtained still awaits improving；The present invention selects graphite alkenes material
Material, because it has the electric conductivity of excellence, the specific surface area of superelevation, mechanical property and stability, such that it is able to reduce target
The equivalent series resistance of thing；By the mixture of the electrolyte of preparation with polymer, the graphite alkenes being coated on loose structure is super
Capacitor electrode material surface, before mixture is completely dried, by the graphite alkenes electrode of super capacitor of another loose structure
Material is superimposed on the mixture of the graphite alkenes electrode material for super capacitor being coated on loose structure, and applying pressure also will
It is dried, thus obtains, by dry one-step shaping, the integrated device that electrode material combines with electrolyte；Employing the method can
So that the graphite alkenes electrode material for super capacitor of electrolyte and the mixture of polymer and two loose structures is in close contact,
Forming thin polymer film between two-layer electrode material through being dried, this thin polymer film could be formed with the ion of effect and leads to
Road, and play the effect of barrier film；Use the mixture coating of electrolyte and polymer, i.e. select integrated electrolyte and be polymerized
Thing, thus replace the addition of extra barrier film so that the method for the present invention simply efficiently and alleviates the weight of the product prepared
Amount.
It is to say, the method manufacturing graphene-based ultracapacitor that the present invention provides, electrolyte layer and electrode material
Interpenetrate on surface, be in close contact, thus the equivalent series resistance considerably reducing ultracapacitor is super to improve
The overall performance of capacitor.
In the further embodiment of the present invention, described applying preset pressure also also includes after drying: by described applying
Preset pressure dried product are packaged in pvc material.
In the further embodiment of the present invention, described Preset Time is 2～8 hours；Described preset pressure is
50psi。
In the further embodiment of the present invention, described graphite alkenes material is that graphene microchip, graphene oxide are micro-
Sheet or redox graphene microchip.
In the further embodiment of the present invention, described dispersion liquid is water, organic solvent, has the macromolecule of cohesive
Solution, conductive polymer solution, curable monomer solution, the mixture comprising metal-oxide or comprise other material with carbon elements
Mixture.
In the further embodiment of the present invention, described polymer is polyvinyl alcohol, polyvinylidene fluoride, polyethylene,
Polypropylene, politef, polystyrene, polymethyl methacrylate, hemacol, polyacrylamide or
Polyimides
In the further embodiment of the present invention, described electrolyte is that 1～3mol/L acid solution, 3～6mol/L alkali are molten
Liquid, 1～3mol/L inorganic salt solution, 1～5mol/L organic slat solution or 1～5mol/L organic solvent.
In the further embodiment of the present invention, described acid solution is sulphuric acid or phosphorus aqueous acid；Described aqueous slkali
For potassium hydroxide or the aqueous solution of sodium hydroxide；Described inorganic salt solution is sodium chloride, potassium chloride, lithium chloride, sodium fluoride, fluorination
The aqueous solution of potassium, sodium nitrate, potassium nitrate, lithium nitrate, sodium sulfate, potassium sulfate or lithium sulfate；Described organic slat solution is triethyl group
Methyl ammonium tetrafluoroborate, tetraethyl ammonium tetrafluoroborate, iodate triethylammonium tetrakis or pyrrolidine tetrafluoroborate；Described organic solvent is four
Hydrogen furan, dimethylformamide, acetonitrile, N-Methyl pyrrolidone, Allyl carbonate, ethylene carbonate, dimethyl carbonate, carbonic acid
The mixed solvent of one or more in methyl ethyl ester.
In the further embodiment of the present invention, the thickness of described electrode material is 100-200 micron.
Accompanying drawing explanation
Fig. 1 is the flow chart of the method manufacturing graphene-based ultracapacitor in the embodiment of the present invention；
Fig. 2 is the schematic diagram of the graphene-based ultracapacitor that the embodiment of the present invention obtains.
Detailed description of the invention
Below in conjunction with accompanying drawing, embodiments of the invention are described in detail.Following example are only used for clearer
Explanation technical scheme, be therefore only used as example, and can not limit the scope of the invention with this.
Fig. 1 is the flow chart of the method manufacturing graphene-based ultracapacitor in the embodiment of the present invention；Fig. 2 is the present invention
The schematic diagram of the graphene-based ultracapacitor that embodiment obtains.
As Figure 1-Figure 2, the present invention provides the method manufacturing graphene-based ultracapacitor, comprises the following steps:
S101: graphite alkenes material is dissolved in dispersion liquid.Wherein, described graphite alkenes material be graphene microchip,
Graphene oxide microplate or redox graphene microchip；Described dispersion liquid is water, organic solvent, has the high score of cohesive
Sub-solution, conductive polymer solution, curable monomer solution, the mixture comprising metal-oxide or comprise the mixed of material with carbon element
Compound.
S102: the dispersion of graphite alkenes material will be dissolved with on collector.
S103: the collector being coated with graphite alkenes material solution is dried, and obtains electrode material.Wherein, described electrode
The thickness of material is 100-200 micron.
Graphite alkenes material is dissolved in solution, the solution being dissolved with graphite alkenes material is coated on collector it
On, then be dried, form the graphite alkenes electrode material for super capacitor with loose structure；Electrode material is super as composition
Level capacitor key components, decide the main performance index of ultracapacitor, as energy density, power density and
Cycle life etc.；Up to now, activated carbon, CNT, metal-oxide and conducting polymer etc. are all applied to super
The electrode material of capacitor, but the performance of the ultracapacitor obtained still awaits improving；The present invention selects graphite alkenes material
Material, because it has the electric conductivity of excellence, the specific surface area of superelevation, mechanical property and stability, such that it is able to reduce target
The equivalent series resistance of thing.
S104: prepare the mixture of electrolyte and polymer.Wherein, described electrolyte be 1～3mol/L acid solution, 3～
6mol/L aqueous slkali, 1～3mol/L inorganic salt solution, 1～5mol/L organic slat solution or 1～5mol/L organic solvent.Use 1
～3mol/L acid solution, 3～6mol/L aqueous slkali, 1～3mol/L inorganic salt solution, 1～5mol/L organic slat solution or 1～
5mol/L organic solvent as electrolyte, electrolyte penetrance in the film can be improved, and improve graphene-based super
The use power of capacitor；Select organic electrolyte can improve the running voltage of graphene-based ultracapacitor.Described acid is molten
Liquid is sulphuric acid or phosphorus aqueous acid；Described aqueous slkali is the aqueous solution of potassium hydroxide or sodium hydroxide；Described inorganic salt solution
For sodium chloride, potassium chloride, lithium chloride, sodium fluoride, potassium fluoride, sodium nitrate, potassium nitrate, lithium nitrate, sodium sulfate, potassium sulfate or sulphuric acid
The aqueous solution of lithium；Described organic slat solution is triethyl methyl ammonium tetrafluoroborate, tetraethyl ammonium tetrafluoroborate, iodate triethylammonium tetrakis or
Pyrrolidine tetrafluoroborate；Described organic solvent is oxolane, dimethylformamide, acetonitrile, N-Methyl pyrrolidone, carbonic acid
Propylene, ethylene carbonate, dimethyl carbonate, the mixed solvent of one or more in Ethyl methyl carbonate.Described polymer is
Polyvinyl alcohol, polyvinylidene fluoride, polyethylene, polypropylene, politef, polystyrene, polymethyl methacrylate, poly-first
Base hydroxyethyl acrylate, polyacrylamide or polyimides.
S105: described mixture is coated on described electrode material surface, is dried Preset Time.Wherein, described default time
Between be 2～8 hours.
S106: be coated with on the electrode material of mixture described in being placed in by another described electrode material, applies to preset pressure
Power is also dried.Wherein, described preset pressure is 50psi.
By the electrolyte of preparation and the mixture of polymer, it is coated on the graphite alkenes electrode of super capacitor of loose structure
Material surface, is dried Preset Time, i.e. before mixture is completely dried, by the graphite alkenes ultracapacitor of another loose structure
Electrode material is superimposed on the mixture of the graphite alkenes electrode material for super capacitor being coated on loose structure, applies pressure
And be dried, thus obtain, by dry one-step shaping, the integrated device that electrode material combines with electrolyte；Use the party
Method can make the graphite alkenes electrode material for super capacitor of electrolyte and the mixture of polymer and two loose structures tight
Contact, forms thin polymer film through being dried between two-layer electrode material, and this thin polymer film could be formed with effect
Ion channel, and play the effect of barrier film；Use the mixture coating of electrolyte and polymer, i.e. select the electrolyte of integration
With polymer, thus replace the addition of extra barrier film so that the method for the present invention simply efficiently and alleviates the product prepared
The weight of product.Figure it is seen that use the graphene-based ultracapacitor prepared of method of the present invention, electrolyte layer with
Electrode material interpenetrates on surface, is in close contact, thus reduces the equivalent series resistance of ultracapacitor to improve super electricity
The overall performance of container.
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment one
The graphene microchip of 40mg/mL is dissolved in polyacrylic acid；This solution is spread evenly across in current collector aluminum foil,
Under an atmospheric pressure, it is dried 24 hours at 25 DEG C；After treating the polyacrylic acid volatilization in solution, obtain filmy graphite alkene
Electrode material and the conglomerate of collector, i.e. electrode material, its thickness is about 200 microns.By 1mol/L sulfuric acid solution and 10%
Polyvinyl alcohol uniformly prepares solid electrolyte solution, is coated in dry electrode material surface, at one atm, 25 DEG C
Under be dried 2 hours；When solid electrolyte is not yet completely dried, another the electrode material being dried is placed in and is coated with mixture
Electrode material i.e. solid electrolyte polyvinyl alcohol/sulphuric acid on, and apply the pressure of 50psi, continue to be dried 24 at 25 DEG C
Hour；Finally give the ultracapacitor of integration.With polrvinyl chloride (PVC) as plastic packaging material, described applying is preset
Pressure dried product are packaged in pvc material, are assembled into ultracapacitor.
The ultracapacitor that the present embodiment assembles is 0～1.2V in voltage range, when electric current density is 0.5A/g, and quality
Being 126F/g than electric capacity, energy density is 18Wh/kg, power density be 400W/kg.ESR be 50m Ω.
Embodiment two
The graphene oxide microplate of 30mg/mL is dissolved in polyurethane；This solution is spread evenly across copper foil of affluxion body
On, under an atmospheric pressure, it is dried 6 hours at 40 DEG C；After treating the polyurethane volatilization in solution, obtain filmy graphite alkene
Electrode material and the conglomerate of collector, i.e. electrode material, its thickness is about 150 microns.By 6mol/LKOH and 10% polyethylene
Alcohol mix homogeneously prepares solid electrolyte solution, is coated in dry electrode material surface, at one atm, is dried at 25 DEG C
2 hours；When solid electrolyte is not yet completely dried, another the electrode material being dried is placed in the electrode being coated with mixture
On material i.e. solid electrolyte polyvinyl alcohol/sulphuric acid, and apply the pressure of 50psi, continue to be dried 24 hours at 25 DEG C；?
Obtain the ultracapacitor of integration eventually.With polrvinyl chloride (PVC) as plastic packaging material, by described applying preset pressure and do
Product after dry is packaged in pvc material, is assembled into ultracapacitor.
The ultracapacitor that the present embodiment assembles is 0～1.2V in voltage range, when electric current density is 0.5A/g, and quality
Be 145F/g than electric capacity, energy density be 22Wh/kg, ESR be 80m Ω.
Embodiment three
The redox graphene microchip of 30mg/mL is dissolved in polyvinyl alcohol；This solution is spread evenly across collection
On fluid aluminium foil, under an atmospheric pressure, it is dried 20 hours at 40 DEG C；After treating the polyvinyl alcohol volatilization in solution, obtain
Filmy graphite alkene electrode material and the conglomerate of collector, i.e. electrode material, its thickness is about 100 microns.By 1mol/L sulfur
Acid solution and 10% polyvinyl alcohol uniformly prepare solid electrolyte solution, are coated in dry electrode material surface, at one
Under atmospheric pressure, it is dried 8 hours at 25 DEG C；When solid electrolyte is not yet completely dried, another the electrode material being dried is put
In being coated with on the electrode material i.e. solid electrolyte polyvinyl alcohol/sulphuric acid of mixture, and apply the pressure of 50psi, 25
Continue at DEG C to be dried 24 hours；Finally give the ultracapacitor of integration.With polrvinyl chloride (PVC) as plastic packaging material,
Described applying preset pressure dried product are packaged in pvc material, are assembled into ultracapacitor.
The ultracapacitor that the present embodiment assembles is 0～1.2V in voltage range, when electric current density is 0.5A/g, and quality
Be 167F/g than electric capacity, energy density be 25Wh/kg, ESR be 46m Ω.
Certainly, situation about enumerating except embodiment one to embodiment three, other Preset Times, graphite alkenes material, dispersion
The thickness of liquid, polymer, electrolyte, the concentration of electrolyte and electrode material is also possible；Simply in embodiment one to reality
Executing in the case of example three enumerates, it is more thorough that electrolyte layer and electrode material interpenetrate on surface, and contact is tightr, obtains
The equivalent series resistance of ultracapacitor is less and various aspects of performance is more preferable.
The method manufacturing graphene-based ultracapacitor that the present invention provides, electrolyte layer and electrode material are mutual on surface
Infiltration, is in close contact, thus considerably reduces the equivalent series resistance of ultracapacitor to improve the whole of ultracapacitor
Body performance.
In describing the invention, it is to be understood that term " first ", " second " are only used for describing purpose, and can not
It is interpreted as instruction or hint relative importance or the implicit quantity indicating indicated technical characteristic.Thus, define " the
One ", the feature of " second " can express or implicitly include one or more this feature.In describing the invention,
" multiple " are meant that two or more, unless otherwise expressly limited specifically.
In the description of this specification, reference term " embodiment ", " some embodiments ", " example ", " specifically show
Example " or the description of " some examples " etc. means to combine this embodiment or example describes specific features, structure, material or spy
Point is contained at least one embodiment or the example of the present invention.In this manual, to the schematic representation of above-mentioned term not
Identical embodiment or example must be directed to.And, the specific features of description, structure, material or feature can be in office
One or more embodiments or example combine in an appropriate manner.Additionally, in the case of the most conflicting, the skill of this area
The feature of the different embodiments described in this specification or example and different embodiment or example can be tied by art personnel
Close and combination.
Although above it has been shown and described that embodiments of the invention, it is to be understood that above-described embodiment is example
Property, it is impossible to being interpreted as limitation of the present invention, those of ordinary skill in the art within the scope of the invention can be to above-mentioned
Embodiment is changed, revises, replaces and modification.
Claims (9)
1. the method manufacturing graphene-based ultracapacitor, it is characterised in that comprise the following steps:
Graphite alkenes material is dissolved in dispersion liquid；
The dispersion of graphite alkenes material will be dissolved with on collector；
The collector being coated with graphite alkenes material solution is dried, and obtains electrode material；
Prepare the mixture of electrolyte and polymer；
Described mixture is coated on described electrode material surface, is dried Preset Time；
It is coated with on the electrode material of mixture described in another described electrode material is placed in, applies preset pressure and be dried.
The method of the graphene-based ultracapacitor of manufacture the most according to claim 1, it is characterised in that
Described applying preset pressure also also includes after drying: described applying preset pressure dried product are packaged in polychlorostyrene
In vinyl material.
The method of the graphene-based ultracapacitor of manufacture the most according to claim 1, it is characterised in that
Described Preset Time is 2～8 hours；Described preset pressure is 50psi.
The method of the graphene-based ultracapacitor of manufacture the most according to claim 1, it is characterised in that
Described graphite alkenes material is graphene microchip, graphene oxide microplate or redox graphene microchip.
The method of the graphene-based ultracapacitor of manufacture the most according to claim 1, it is characterised in that
Described dispersion liquid is water, organic solvent, has the macromolecular solution of cohesive, conductive polymer solution, curable list
Liquid solution, the mixture comprising metal-oxide or comprise the mixture of material with carbon element.
The method of the graphene-based ultracapacitor of manufacture the most according to claim 1, it is characterised in that
Described polymer is polyvinyl alcohol, polyvinylidene fluoride, polyethylene, polypropylene, politef, polystyrene, poly-first
Base acrylic acid methyl ester., hemacol, polyacrylamide or polyimides.
The method of the graphene-based ultracapacitor of manufacture the most according to claim 1, it is characterised in that
Described electrolyte is 1～3mol/L acid solution, 3～6mol/L aqueous slkali, 1～3mol/L inorganic salt solution, 1～5mol/L
Organic slat solution or 1～5mol/L organic solvent.
The method of the graphene-based ultracapacitor of manufacture the most according to claim 7, it is characterised in that
Described acid solution is sulphuric acid or phosphorus aqueous acid；
Described aqueous slkali is the aqueous solution of potassium hydroxide or sodium hydroxide；
Described inorganic salt solution is sodium chloride, potassium chloride, lithium chloride, sodium fluoride, potassium fluoride, sodium nitrate, potassium nitrate, lithium nitrate,
The aqueous solution of sodium sulfate, potassium sulfate or lithium sulfate；
Described organic slat solution is triethyl methyl ammonium tetrafluoroborate, tetraethyl ammonium tetrafluoroborate, iodate triethylammonium tetrakis or pyrrolidine
Tetrafluoroborate；
Described organic solvent is oxolane, dimethylformamide, acetonitrile, N-Methyl pyrrolidone, Allyl carbonate, ethylene
Alkene ester, dimethyl carbonate, the mixed solvent of one or more in Ethyl methyl carbonate.
9. according to the method manufacturing graphene-based ultracapacitor described in any one of claim 1～8, it is characterised in that
The thickness of described electrode material is 100-200 micron.
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| CN109326459A (en) * | 2018-11-09 | 2019-02-12 | 南京邮电大学 | A kind of preparation method and application of metalloporphyrin frame/titanium carbide composite and flexible all-solid-state supercapacitor |
| CN109461596A (en) * | 2018-11-09 | 2019-03-12 | 南京邮电大学 | A kind of preparation method and application of the flexible ultra-thin all-solid-state supercapacitor based on titanium carbide |
| CN109755038A (en) * | 2019-01-14 | 2019-05-14 | 南京邮电大学 | The preparation method and application of flexible all-solid-state supercapacitor based on two-dimensional drape metalloporphyrin frame ultrathin nanometer piece |
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