CN108122682A - Arbitrary shape stacked ultracapacitor and preparation method thereof in a kind of same substrate - Google Patents
Arbitrary shape stacked ultracapacitor and preparation method thereof in a kind of same substrate Download PDFInfo
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- CN108122682A CN108122682A CN201611057486.8A CN201611057486A CN108122682A CN 108122682 A CN108122682 A CN 108122682A CN 201611057486 A CN201611057486 A CN 201611057486A CN 108122682 A CN108122682 A CN 108122682A
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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
- H01G11/10—Multiple hybrid or EDL capacitors, e.g. arrays or modules
- H01G11/12—Stacked hybrid or EDL capacitors
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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
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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 discloses arbitrary shape stacked ultracapacitors in a kind of same substrate and preparation method thereof, the capacitor is the arbitrary shape stacked ultracapacitor for integrating first layer electrode film/second layer membrane/third layer electrode film/solid electrolyte successively in a substrate.Its preparation method is lower electrode film layer of the spraying manufacture with arbitrary shape on the same base, and the then spraying manufacture graphene oxide membrane layer in lower electrode film, then upper electrode film layer is manufactured on membrane layer obtains the ultracapacitor with stacked structure.Arbitrary shape stacked ultracapacitor manufactured by the present invention can realize controlled shape and large-scale production, can be effectively compatible integrated with variety classes flexibility, portability, wearable electronic device, have extensive market application foreground.
Description
Technical field
The invention belongs to the manufacturing fields of ultracapacitor, and in particular to arbitrary shape stacked is super in a kind of same substrate
Capacitor and preparation method thereof.
Background technology
Conventional stacking type ultracapacitor by collector (substrate)/anode/membrane/cathode/collector (substrate) form
It stacks and forms.Time-consuming for the stacked ultracapacitor manufacture of this structure type, and process is complicated and its structure type is related to
Two substrates；Collector and electrode material fail to be melted into a whole, and the volume for causing conventional stacking type ultracapacitor is big, is unfavorable for
Its application in Miniaturized Integrated Circuit.
With the fast development of the electronic equipment of light, thin, flexible various shapes, people are greatly have stimulated to new
The demand of energy storage device.Current energy storage device, such as lithium electricity battery and ultracapacitor, shape are fixed, and volume is big, quality
Weight, it is difficult to meet the requirement of flexible electronic devices.Further, since the limitation of structure design and performance, such as polymer is needed to glue
The flexible energy storage device of controlled shape can not be accomplished by tying agent and additional conductive agent and the membrane of thickness, traditional power supply.
In order to overcome above-mentioned difficulties, in recent years, the graphene-based energy storage device of level-crossing finger-type causes extensive pass
Note, and be considered being expected to applying on miniature electronic chip.This planar structure causes electrode, membrane, electrolyte and afflux
Body is integrated into same substrate, is conducive to the combination of each component, the shape design of energy storage device.Although using multiple technologies,
Such as printing, photoetching development, laser ablation, the plane ultracapacitor of various shapes can be produced, but can not be realized
The manufacture of arbitrary shape ultracapacitor.
The content of the invention
In view of the above-mentioned problems, it is an object of the invention to manufacture arbitrary shape in same substrate using the method for spraying
Ultracapacitor with stacked structure, manufacturing process is simple, at low cost, has extensive market application foreground.
In order to achieve the above objectives, the technical solution adopted by the present invention is：
Arbitrary shape stacked ultracapacitor in a kind of same substrate, the capacitor are in a substrate, are stacked gradually
The arbitrary shape stacked super capacitor of first layer electrode film/second layer membrane/third layer electrode film/solid electrolyte
Device；
The first layer electrode film, third level electrode film material are：Graphene or graphene composite material；
The membrane is graphene oxide；
The solid electrolyte is that electrolyte is polyvinyl alcohol/sulfuric acid (PVA/H2SO4), polyvinyl alcohol/sodium sulphate (PVA/
Na2SO4), one kind in 1- butyl -3- methyl imidazolium tetrafluoroborates/silica solid electrolyte.
The substrate includes PET substrate (PET), polyetherimide (PEI), silicon chip, glass
Any insulating planar substrate such as glass, paper or plank.
The thickness of the electrode film is 0.1-5 μm, and the thickness of membrane is 1-3 μm.
Heretofore described first layer electrode material and third layer electrode material membrane electrode can be identical electrode
Material, or different electrode materials.
Heretofore described first layer electrode material and third layer electrode material are identical electrode material, super capacitor
Device is symmetrical ultracapacitor；First layer electrode material and third layer electrode material are different electrode materials, ultracapacitor
For Asymmetric Supercapacitor.
Heretofore described definite shape can be arbitrary shape, refer to from size of devices, configuration, dimension
Limitation；
Heretofore described two electrode materials, membrane, electrolyte, collector are all integrated in same substrate.
The preparation method of arbitrary shape stacked ultracapacitor, specially comprises the following steps in a kind of same substrate：
(1) in a substrate, tool effigurate the is produced by the 1 graphite spraying alkene ink of template of definite shape
Thin film electrode, the electrode layer are used as active material again as collector；
(2) by the template 2 of same shape, spraying graphene oxide ink on first layer membrane electrode in preparing second
Layer has same shape, ionic conduction and electronic isolation membrane；
(3) by the template 1 of same shape, graphite spraying alkene ink has in preparing third layer on second layer membrane layer
The membrane electrode of same shape, with first layer shape paired electrode；
(4) finally, the consolidating plus same shape on the surface of the certain electrode material/membrane/electrode material structure of shape
State electrolyte is prepared with arbitrary shape stacked ultracapacitor.
Graphene ink described in step (1) is the graphene being dispersed in dispersion liquid, the graphene body
For 0.05-10mg mL-1；
Graphene is electrochemical stripping graphene in the graphene ink, redox graphene, liquid phase remove stone
One or more in black alkene, chemical vapor deposition graphene, graphene composite material；
Dispersion liquid is isopropanol, one kind in N,N-dimethylformamide (DMF), N-Methyl pyrrolidone (NMP).
The width of heretofore described template 2 is more than 1 to 10 μm to 1000 μm of template.
The size of heretofore described graphene oxide is between 0.1-100 μm, and thickness is between 0.7-2.0nm；
Concentration is 0.5-8mg mL-1。
Heretofore described spraying manufacturing method includes mechanically spraying, electrostatic spraying.
For the nozzle diameter of heretofore described spraying between 0.2-1.0mm, gases used spraying is nitrogen, argon gas or sky
One kind in gas, spray gas pressure are 0.01-0.3M Pa.
The invention discloses the method for manufacturing arbitrary shape ultracapacitor on the same base, by using the side of spraying
Method manufactures the ultracapacitor of arbitrary shape stacked structure in same substrate.Specially spraying manufacture has on the same base
There is the lower electrode film layer of arbitrary shape, the then spraying manufacture graphene oxide membrane layer in lower electrode film, then in membrane
Upper electrode film layer is manufactured on layer, obtains the ultracapacitor with stacked structure.Its manufacturing process is simple, at low cost, and
It can realize controlled shape and large-scale production, it can be effectively compatible with variety classes flexibility, portability, wearable electronic device
It is integrated, there is extensive market application foreground.
The features of the present invention and advantage
1. of the present invention manufacture arbitrary shape stacked ultracapacitor on the same base, structure is substrate/electricity
Pole/membrane/electrode；Electrode is integrated with membrane, can realize the manufacture of arbitrary shape ultracapacitor.
2. of the present invention manufacture arbitrary shape stacked ultracapacitor, shape, size, dimension on the same base
And the thickness of device can be the ability to easily control, required equipment is simple, pertains only to a substrate, has the characteristics that manufacturing process is simple.
3. of the present invention manufacture arbitrary shape stacked ultracapacitor on the same base, make on a flexible substrate
It makes, can be effectively compatible integrated with variety classes flexibility, portability, wearable electronic device, there is the application of extensive market
Prospect.
Description of the drawings
Fig. 1 are prepared on the same base has arbitrary shape stacked ultracapacitor using crosspoint line style as representative
Schematic diagram.
Fig. 2 manufacture arbitrary shape ultracapacitor example using spraying process：With crosspoint line style ultracapacitor and not
With the cyclic voltammetry curve under sweep speed.
Fig. 3 manufacture arbitrary shape ultracapacitor example using spraying process：With square hollow ultracapacitor.
Specific embodiment
Embodiment 1
To be dispersed in electrochemical stripping graphene (the 0.1mg mL in isopropanol-1) and graphene oxide water solution (1mg
mL-1) for raw material, graphene oxide mean size is 100nm in the present embodiment, and spraying substrate is PET；Pass through the linear mould in crosspoint
Plate 1 (attached drawing 1) coating thickness is the Graphene electrodes layer of 100nm, and a diameter of 0.3mm of airbrush bore of spraying sprays nitrogen pressure
Power is 0.05MPa, removes template 1, obtains a pole of the linear ultracapacitor in crosspoint；Then the linear template 2 in crosspoint is passed through
(attached drawing 1) sprays graphene oxide water solution with the airbrush of 0.2mm, and the thickness of graphene oxide membrane layer is 1.5 μm, spraying
Nitrogen pressure is 0.1M Pa, removes template 2；Again on graphene oxide membrane layer, 0.3mm is used by the linear template 1 in crosspoint
Airbrush spraying same thickness another electrode；It is then injected into PVA/H2SO4, then encapsulate；Up to the linear symmetrical super electricity in crosspoint
Container (attached drawing 2).
Electro-chemical test shows the voltage window of the linear ultracapacitor in the crosspoint of gained as 0.8V, in cyclic voltammetric
Test sweep speed is 2mV s-1When, electrode surface specific volume is 0.88mF cm-2。
Embodiment 2
To be dispersed in electrochemical stripping graphene (the 0.5mg mL in isopropanol-1) and graphene oxide water solution (1.5mg
mL-1) for raw material, graphene oxide mean size is 1 μm in the present embodiment, and spraying substrate is PET；Pass through square hollow template 1
Coating thickness is the Graphene electrodes layer of 170nm, and a diameter of 0.5mm of airbrush bore of spraying, spraying nitrogen pressure is 0.2MPa,
Template 1 is removed, obtains a pole of square hollow ultracapacitor；Then by square hollow template 2, sprayed with the airbrush of 0.3mm
Graphene oxide water solution is applied, the thickness of graphene oxide membrane layer is 1 μm, and spraying nitrogen pressure is 0.1M Pa, removes template
2；Again on graphene oxide membrane layer, another electricity of same thickness is sprayed with the airbrush of 0.5mm by square hollow template 1
Pole；It is then injected into PVA/H2SO4, then encapsulate；Up to the symmetrical ultracapacitor of square hollow (attached drawing 3).
Electro-chemical test shows that the voltage window of the square hollow ultracapacitor of gained for 0.8V, is surveyed in cyclic voltammetric
Examination sweep speed is 2mV s-1When, electrode surface specific volume is 1.2mF cm-2。
Embodiment 3
With redox graphene (the 2mg mL being dispersed in isopropanol-1) and graphene oxide water solution (4mg mL-1)
For raw material, graphene oxide mean size is 1 μm in the present embodiment, and spraying substrate is PET；It is sprayed by alphabetical " A " shape template 1
Thickness is 1 μm of Graphene electrodes layer, and a diameter of 0.3mm of airbrush bore of spraying, spraying nitrogen pressure is 0.1MPa, removes mould
Plate 1 obtains a pole of alphabetical " A " shape ultracapacitor；Then by alphabetical " A " shape template 2, oxygen is sprayed with the airbrush of 0.3mm
Graphite aqueous solution, the thickness of graphene oxide membrane layer is 2 μm, and spraying nitrogen pressure is 0.1M Pa, removes template 2；Again
On graphene oxide membrane layer, another electrode of same thickness is sprayed with the airbrush of 0.3mm by alphabetical " A " shape template 1；So
After inject PVA/H2SO4, then encapsulate；Up to the symmetrical ultracapacitor of alphabetical " A " shape.
Electro-chemical test shows that the voltage window of letter " A " shape ultracapacitor of gained for 0.8V, is surveyed in cyclic voltammetric
Examination sweep speed is 2mV s-1When, electrode surface specific volume is 8.9mF cm-2。
Embodiment 4
Graphene (1.5mg mL are removed with the liquid phase being dispersed in DMF-1) and graphene oxide water solution (6mg mL-1)
For raw material, graphene oxide mean size is 100nm in the present embodiment, and spraying substrate is PET；It is sprayed by number " 1 " shape template 1
The Graphene electrodes layer that thickness is 5 μm is applied, a diameter of 0.3mm of airbrush bore of spraying, spraying nitrogen pressure is 0.2MPa, is removed
Template 1 obtains a pole of digital " 1 " shape ultracapacitor；Then by digital " 1 " shape template 2, sprayed with the airbrush of 0.3mm
Graphene oxide water solution, the thickness of graphene oxide membrane layer is 3 μm, and spraying nitrogen pressure is 0.1M Pa, removes template 2；
Again on graphene oxide membrane layer, another electrode of same thickness is sprayed with the airbrush of 0.3mm by digital " 1 " shape template 1；
It is then injected into PVA/H2SO4, then encapsulate；Up to the symmetrical ultracapacitor of digital " 1 " shape.
Electro-chemical test shows that the voltage window of number " 1 " shape ultracapacitor of gained for 0.8V, is surveyed in cyclic voltammetric
Examination sweep speed is 2mV s-1When, electrode surface specific volume is 7.1mF cm-2。
Embodiment 5
To be dispersed in electrochemical stripping graphene (the 10mg mL in NMP-1) and graphene oxide water solution (3mg mL-1)
For raw material, graphene oxide mean size is 1 μm in the present embodiment, and spraying substrate is paper；It is sprayed by number " 1 " shape template 1
Thickness is 2 μm of Graphene electrodes layer, and a diameter of 0.3mm of airbrush bore of spraying, spraying nitrogen pressure is 0.1MPa, removes mould
Plate 1 obtains a pole of digital " 1 " shape ultracapacitor；Then by digital " 1 " shape template 2, oxygen is sprayed with the airbrush of 0.5mm
Graphite aqueous solution, the thickness of graphene oxide membrane layer is 3 μm, and spraying nitrogen pressure is 0.1M Pa, removes template 2；Again
On graphene oxide membrane layer, another electrode of same thickness is sprayed with the airbrush of 0.3mm by digital " 1 " shape template 3；So
After inject PVA/H2SO4, then encapsulate；Up to the symmetrical ultracapacitor of digital " 1 " shape.
Electro-chemical test shows that the voltage window of number " 1 " shape ultracapacitor of gained for 0.8V, is surveyed in cyclic voltammetric
Examination sweep speed is 2mV s-1When, electrode surface specific volume is 13.6mF cm-2。
Embodiment 6
To be dispersed in electrochemical stripping graphene (the 2mg mL in isopropanol-1) and graphene oxide water solution (3mg mL-1) for raw material, graphene oxide mean size is 100nm in the present embodiment, and spraying substrate is silicon chip；Pass through alphabetical " A " shape template
1 coating thickness is the Graphene electrodes layer of 700nm, and a diameter of 0.3mm of airbrush bore of spraying, spraying nitrogen pressure is
0.1MPa removes template 1, obtains a pole of alphabetical " A " shape ultracapacitor；Then by alphabetical " A " shape template 2,0.2mm is used
Airbrush spraying graphene oxide water solution, the thickness of graphene oxide membrane layer is 1 μm, and spraying nitrogen pressure is 0.1M Pa,
Remove template 2；Again on graphene oxide membrane layer, same thickness is sprayed by the alphabetical airbrush of 0.3mm of " A " shape template 1
Another electrode；It is then injected into PVA/Na2SO4, then encapsulate；Up to the symmetrical ultracapacitor of alphabetical " A " shape.
Electro-chemical test shows that the voltage window of letter " A " shape ultracapacitor of gained for 0.8V, is surveyed in cyclic voltammetric
Examination sweep speed is 2mV s-1When, electrode surface specific volume is 6.4mF cm-2。
Embodiment 7
With grapheme/polyaniline composite material (the 0.5mg mL being dispersed in isopropanol-1), the electricity that is dispersed in isopropanol
Chemical stripping graphene (1mg mL-1) and graphene oxide water solution (3mg mL-1) for raw material, graphite oxide in the present embodiment
Alkene mean size is 100nm, and spraying substrate is PET；It is compound for 1 μm of graphene/polyaniline by 1 coating thickness of square template
Material electrodes layer, a diameter of 0.5mm of airbrush bore of spraying, spraying nitrogen pressure are 0.15MPa, remove template 1, obtain square
One pole of ultracapacitor；Then by square template 2, graphene oxide water solution, graphite oxide are sprayed with the airbrush of 0.2mm
The thickness of alkene membrane layer is 2 μm, and spraying nitrogen pressure is 0.1M Pa, removes template 2；Again on graphene oxide membrane layer, lead to
The electrochemical stripping Graphene electrodes that the airbrush coating thickness of 0.5mm is 2 μ m thicks of square template 1 are crossed, are formed asymmetric super
Grade capacitor, is then injected into PVA/H2SO4, then encapsulate；Up to square Asymmetric Supercapacitor.
Electro-chemical test shows that the voltage window of the square figure super capacitor of gained for 1.4V, is swept in cyclic voltammetry
Rate is retouched as 10mV s-1When, electrode surface specific volume is 15.8mF cm-2。
Embodiment 8
To be dispersed in electrochemical stripping graphene (the 0.3mg mL in isopropanol-1) and graphene oxide water solution (1.5mg
mL-1) for raw material, graphene oxide mean size is 100nm in the present embodiment, and spraying substrate is PET；It is sprayed by square template 1
The electrochemical stripping Graphene electrodes layer that thickness is 1 μm, a diameter of 0.5mm of airbrush bore of spraying are applied, spraying nitrogen pressure is
0.15MPa removes template 1, obtains a pole of square figure super capacitor；Then by square template 2, sprayed with the airbrush of 0.2mm
Graphene oxide water solution is applied, the thickness of graphene oxide membrane layer is 2 μm, and spraying nitrogen pressure is 0.1M Pa, removes template
2；Again on graphene oxide membrane layer, pass through the electrochemistry that the airbrush coating thickness of 0.5mm is 1 μ m thick of square template 1
Graphene electrodes are removed, 1- butyl -3- methyl imidazolium tetrafluoroborates/silica dielectric liquid is then injected into, then encapsulates；To obtain the final product
Square symmetrical ultracapacitor.
Electro-chemical test shows that the voltage window of the square figure super capacitor of gained for 3V, is scanned in cyclic voltammetry
Rate is 50mV s-1When, electrode surface specific volume is 1.2mF cm-2。
Claims (9)
1. arbitrary shape stacked ultracapacitor on the same base, it is characterised in that the capacitor be in a substrate, according to
The arbitrary shape stacked of secondary integrated first layer electrode film/second layer membrane/third layer electrode film/solid electrolyte is super
Capacitor；
The first layer electrode film, third level electrode film material are：Graphene or graphene composite material；
The membrane is graphene oxide；
The solid electrolyte is that electrolyte is polyvinyl alcohol/sulfuric acid, polyvinyl alcohol/sodium sulphate, 1- butyl -3- methylimidazoles four
One kind in borofluoride/silica solid electrolyte.
2. the stacked ultracapacitor of arbitrary shape on the same base described in accordance with the claim 1, it is characterised in that：It is described
Substrate include PET substrate (PET), polyetherimide (PEI), silicon chip, glass, paper or plank etc.
Any insulating planar substrate.
3. the stacked ultracapacitor of arbitrary shape on the same base described in accordance with the claim 1, it is characterised in that：It is described
The thickness of electrode film is 0.1-5 μm, and the thickness of membrane is 1-3 μm.
4. the preparation method of the stacked ultracapacitor of arbitrary shape on the same base described in accordance with the claim 1, special
Sign is to specifically include following steps：
(1) in a substrate, it is thin that the first layer with the shape is produced by the 1 graphite spraying alkene ink of template of definite shape
Membrane electrode, the electrode layer are used as active material again as collector；
(2) by the template 2 of same shape, spraying graphene oxide ink is in preparing second layer tool on first layer membrane electrode
There is same shape, ionic conduction and electronic isolation membrane；
(3) by the template 1 of same shape, graphite spraying alkene ink in prepared on the second layer membrane layer third layer have it is identical
The membrane electrode of shape, with first layer shape paired electrode；
(4) finally, on the surface of the certain electrode material/membrane/electrode material structure of shape plus the solid-state electricity of same shape
Liquid is solved, is prepared with arbitrary shape stacked ultracapacitor.
It is 5. special according to the preparation method of the stacked ultracapacitor of arbitrary shape on the same base described in claim 4
Sign is：Graphene ink described in step (1) is the graphene being dispersed in dispersion liquid, and the graphene body is
0.05-10mg mL-1；
The graphene is electrochemical stripping graphene, redox graphene, liquid phase remove graphene, chemical vapor deposition stone
One or more in black alkene or graphene composite material；
The dispersion liquid is one kind in isopropanol, N,N-dimethylformamide (DMF) or N-Methyl pyrrolidone (NMP).
It is 6. special according to the preparation method of the stacked ultracapacitor of arbitrary shape on the same base described in claim 4
Sign is：The width of the template 2 is 10 μm~1000 μm bigger than the width of template 1.
It is 7. special according to the preparation method of the stacked ultracapacitor of arbitrary shape on the same base described in claim 4
Sign is：The size of step (2) graphene oxide is between 0.1-100 μm, and thickness is between 0.7-2.0nm；It is dense
It spends for 0.5-8mg mL-1。
It is 8. special according to the preparation method of the stacked ultracapacitor of arbitrary shape on the same base described in claim 4
Sign is：The spraying method includes mechanically spraying or electrostatic spraying.
9. according to the arbitrary shape stacked ultracapacitor of manufacture on the same base described in claim 4, it is characterised in that：
It is described spraying design parameter be：Nozzle diameter is 0.2-1.0mm, the gases used one kind in nitrogen, argon gas or air of spraying,
Spray gas pressure is 0.01-0.3M Pa.
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