CN108122685A - Stacked ultracapacitor that a kind of inkjet printing is prepared and preparation method thereof - Google Patents
Stacked ultracapacitor that a kind of inkjet printing is prepared and preparation method thereof Download PDFInfo
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- CN108122685A CN108122685A CN201611061170.6A CN201611061170A CN108122685A CN 108122685 A CN108122685 A CN 108122685A CN 201611061170 A CN201611061170 A CN 201611061170A CN 108122685 A CN108122685 A CN 108122685A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
- H01G11/52—Separators
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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
- H01G11/54—Electrolytes
- H01G11/56—Solid electrolytes, e.g. gels; Additives therein
-
- 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
Stacked ultracapacitor prepared the invention discloses a kind of inkjet printing and preparation method thereof, the capacitor is stacked ultracapacitor, in a substrate, the arbitrary shape stacked ultracapacitor of first layer electrode film/second layer membrane/third layer electrode film/solid electrolyte is integrated successively；Its preparation method comprises the following steps：(1) preparation of inkjet printing electrode slurry, the preparation of (2) graphene oxide membrane slurry, the preparation of (3) stacked ultracapacitor.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 technology fields of ultracapacitor, and in particular to the stacked that a kind of inkjet printing is prepared surpasses
Grade capacitor and preparation method thereof.
Background technology
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 invention discloses the method for manufacturing arbitrary shape stacked ultracapacitor on the same base, by using spray
The method of ink printing manufactures the ultracapacitor of arbitrary shape stacked structure in same substrate.Specially electrode material is made
It is that collector is used as active material again, passes through and first layer of the electrode material slurry with certain pattern form is printed in a substrate
Electrode thin film layer, then the second layer graphene oxide membrane layer of identical patterns is printed on first layer electrode, it is used as ion
Conductive and electronic isolation membrane realizes that membrane is integrated with electrode, so as to realize the super electricity of arbitrary shape by printing
The manufacture of container；Then printing and first layer electrode same shape and symmetrical third layer electrode on membrane layer.It reinjects solid
Body gel electrolyte, encapsulation, obtains arbitrary shape stacked ultracapacitor.
The content of the invention
It is an object of the invention to manufacture arbitrary shape in same substrate using the method for inkjet printing to have stacking
The ultracapacitor of structure, manufacturing process is simple, at low cost, has extensive market application foreground.
The stacked ultracapacitor that a kind of inkjet printing is prepared, the capacitor are in a substrate, integrate the successively
The arbitrary shape stacked ultracapacitor of one layer of electrode film/second layer membrane/third layer electrode film/solid electrolyte；
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 include PET substrate (PET), polyetherimide (PEI), paper and other
Insulating planar substrate.
The thickness of the electrode film is 0.5-100 μm, and preferred scope is 1-10 μm；The thickness of membrane is 0.1-10 μm,
Preferably 2-5 μm.
A kind of preparation method for the stacked ultracapacitor that inkjet printing is prepared, specifically includes following steps：
(1) preparation of inkjet printing electrode slurry
It disperses graphene in n,N-Dimethylformamide (DMF), then 3000rpm centrifugation 30min, take supernatant；To
In obtained supernatant, terpinol is added in, the volume ratio of supernatant and terpinol is 5-20, then rotating pressure-decreasing evaporation DMF；Gained
Graphene/the terpinol arrived is 3 by volume:1 adds in ethyl alcohol, and obtaining can be with the electrode slurry of inkjet printing；The graphite
Alkene electrode slurry concentration is 0.1-5mg mL-1；
(2) preparation of graphene oxide membrane slurry
Graphene oxide using correct hummers methods be made, graphene oxide again with mixed with propylene glycol, graphene oxide slurry
The concentration of material is 1-10mg mL-1, obtain the graphene oxide membrane slurry reciprocal between 2-4 of Weber number；
(3) preparation of stacked ultracapacitor
Printed substrates are put into printer, electrode slurry is packed into the print cartridge of printer, is beaten by computer design arbitrary graphic pattern
First layer Graphene electrodes are printed off, it can be repeatedly；Graphene oxide membrane slurry is packed into print cartridge again, in first layer electricity
The second layer graphene oxide membrane layer of identical patterns is printed on extremely, it can be repeatedly；Then on membrane layer printing with
First layer electrode is identical and symmetrical third layer electrode；Solid gel electrolyte is reinjected, encapsulates, obtains arbitrary shape stacked
Ultracapacitor.
The graphene is electrochemical stripping graphene, redox graphene, liquid phase remove graphene, chemical gaseous phase
Deposit the one or more in graphene, graphene composite material.
The Graphene electrodes slurry concentration is 0.1-5mg mL-1, preferably 0.5-2mg mL-1。
The second layer graphene oxide interlayer is identical with first layer electrode pattern shape, second layer graphene oxide every
Layer is more than 10 μm~500 μm than the width of first layer electrode, and preferred scope is 100 μm~500 μm.
The concentration of the graphene oxide slurry is 1-10mg mL-1, preferably 6-10mg mL-1。
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 duplicate printing number is 1-10 times, is preferably 1-5 times.
Heretofore described two electrode materials, membrane, electrolyte, collector are all integrated in same substrate.
The features of the present invention and advantage
1. inkjet printing of the present invention manufactures arbitrary shape stacked ultracapacitor, electrode is integrated with membrane,
It can realize the manufacture of arbitrary shape ultracapacitor.
2. inkjet printing of the present invention manufactures arbitrary shape stacked ultracapacitor, required equipment is simple, only relates to
And a substrate, have the characteristics that manufacturing process is simple.
3. inkjet printing of the present invention manufactures arbitrary shape stacked ultracapacitor, 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 inkjet printings manufacture square stacked ultracapacitor schematic diagram.Left figure electrode layer, right figure graphene oxide
Layer.
Digital " 1 " stacked ultracapacitor schematic diagram of Fig. 2 inkjet printings manufacture.Left figure electrode layer, right figure graphite oxide
Alkene layer.
Digital " A " stacked ultracapacitor schematic diagram of Fig. 3 inkjet printings manufacture.Left figure electrode layer, right figure graphite oxide
Alkene layer.
Specific embodiment
Embodiment 1
Electrochemical stripping graphene slurry (0.5mg mL-1) and graphene oxide slurry (8mg mL-1) for raw material, this reality
It is A4 paper to apply printed substrates in example；It is square (Fig. 1) that computer, which sets shape, design graphene oxide layer than 100 μm of electrode slice width,
Prevent first layer electrode from contacting directly short circuit with third layer electrode；First on paper first layer Graphene electrodes are printed according to design
Layer, duplicate printing 2 times, first layer thickness of electrode are 1.4 μm；Then according to design printing second layer oxidation on first layer electrode
Graphene layer, duplicate printing 3 times, second layer membrane thicknesses are about 2.6 μm；The printing and first on graphene oxide membrane layer again
Graphene electrodes layer as layer, is repeated twice.It is then injected into PVA/H2SO4, then encapsulate；Up to square symmetrical ultracapacitor.
Electro-chemical test shows that the voltage window of the square symmetrical ultracapacitor of gained for 0.8V, is surveyed in cyclic voltammetric
Examination sweep speed is 5mV s-1When, electrode surface specific volume is 13.4mF cm-2。
Embodiment 2
Electrochemical stripping graphene slurry (1mg mL-1) and graphene oxide slurry (6mg mL-1) for raw material, this implementation
Printed substrates are A4 paper in example；Computer design shape is digital " 1 " shape (Fig. 2), and design graphene oxide layer is than electrode slice width 300
μm, prevent first layer electrode from contacting directly short circuit with third layer electrode；First on paper the first layer graphene is printed according to design
Electrode layer, duplicate printing 1 time, first layer thickness of electrode are 0.9 μm；Then on first layer electrode the second layer is printed according to design
Graphene oxide layer, duplicate printing 3 times, second layer membrane thicknesses are about 2.1 μm；Again on graphene oxide membrane layer printing with
The same Graphene electrodes layer of first layer, duplicate printing 1 time.It is then injected into PVA/Na2SO4, then encapsulate；Up to digital " 1 " shape pair
Claim ultracapacitor.
Electro-chemical test shows that the voltage window of the symmetrical ultracapacitor of number " 1 " shape of gained for 0.8V, is lied prostrate in Xun Huan
Peace test sweep speed is 5mV s-1When, electrode surface specific volume is 8.9mF cm-2。
Embodiment 3
Electrochemical stripping graphene slurry (2mg mL-1) and graphene oxide slurry (10mg mL-1) for raw material, this implementation
Printed substrates are A4 paper in example；Computer design shape is alphabetical " A " shape (Fig. 3), graphene oxide layer than 300 μm of electrode slice width,
Prevent first layer electrode from contacting directly short circuit with third layer electrode；First on paper first layer Graphene electrodes are printed according to design
Layer, duplicate printing 1 time, first layer thickness of electrode are 2.2 μm；Then according to design printing second layer oxidation on first layer electrode
Graphene layer, duplicate printing 3 times, second layer membrane thicknesses are about 3.6 μm；The printing and first on graphene oxide membrane layer again
Graphene electrodes layer as layer, duplicate printing 1 time.It is then injected into PVA/H2SO4, then encapsulate；Symmetrically surpass up to letter " A " shape
Grade capacitor.
Electro-chemical test shows that the voltage window of the symmetrical ultracapacitor of letter " A " shape of gained for 0.8V, is lied prostrate in Xun Huan
Peace test sweep speed is 5mV s-1When, electrode surface specific volume is 20.8mF cm-2。
Embodiment 4
Electrochemical stripping graphene slurry (1.5mg mL-1) and graphene oxide slurry (8mg mL-1) for raw material, this reality
It is PET to apply printed substrates in example；Computer design shape is alphabetical " A " shape (Fig. 3), graphene oxide layer than 500 μm of electrode slice width,
Prevent first layer electrode from contacting directly short circuit with third layer electrode；First on paper first layer Graphene electrodes are printed according to design
Layer, duplicate printing 1 time, first layer thickness of electrode are 1.8 μm；Then according to design printing second layer oxidation on first layer electrode
Graphene layer, duplicate printing 3 times, second layer membrane thicknesses are about 3 μm；Printing and first layer on graphene oxide membrane layer again
The same Graphene electrodes layer, duplicate printing 1 time.It is then injected into PVA/H2SO4, then encapsulate；It is symmetrically super up to alphabetical " A " shape
Capacitor.
Electro-chemical test shows that the voltage window of the symmetrical ultracapacitor of letter " A " shape of gained for 0.8V, is lied prostrate in Xun Huan
Peace test sweep speed is 5mV s-1When, electrode surface specific volume is 15.3mF cm-2。
Embodiment 5
Electrochemical stripping graphene slurry (1mg mL-1), graphene/polyaniline composite mortar (0.8mg mL-1) and oxidation
Graphene slurry (8mg mL-1) for raw material, printed substrates are A4 paper in the present embodiment；Computer design shape is alphabetical " A " shape (figure
3), graphene oxide layer prevents first layer electrode from contacting directly short circuit with third layer electrode than 500 μm of electrode slice width；Exist first
First layer Graphene electrodes layer, duplicate printing 3 times are printed according to design on paper, first layer thickness of electrode is 1.8 μm；Then
Second layer graphene oxide layer is printed according to design on one layer of electrode, duplicate printing 3 times, second layer membrane thicknesses are about 3 μm；Again
Third layer graphene/polyaniline electrode layer is printed with graphene/polyaniline composite mortar on graphene oxide membrane layer, is repeated
Printing 2 times, third layer thickness are 1.2 μm.It is then injected into PVA/H2SO4, then encapsulate；Up to the asymmetric super capacitor of alphabetical " A " shape
Device.
Electro-chemical test shows that the voltage window of letter " A " shape Asymmetric Supercapacitor of gained for 1.2V, is cycling
Volt-ampere test sweep speed is 5mV s-1When, electrode surface specific volume is 23.6mF cm-2。
Embodiment 6
Electrochemical stripping graphene slurry (1mg mL-1) and graphene oxide slurry (6mg mL-1) for raw material, this implementation
Printed substrates are A4 paper in example；Computer design shape is digital " 1 " shape (Fig. 2), and design graphene oxide layer is than electrode slice width 300
μm, prevent first layer electrode from contacting directly short circuit with third layer electrode；First on paper the first layer graphene is printed according to design
Electrode layer, duplicate printing 2 times, first layer thickness of electrode are 1.3 μm；Then on first layer electrode the second layer is printed according to design
Graphene oxide layer, duplicate printing 3 times, second layer membrane thicknesses are about 2.1 μm；Again on graphene oxide membrane layer printing with
The same Graphene electrodes layer of first layer, duplicate printing 2 times.It is then injected into 1- butyl -3- methyl imidazolium tetrafluoroborates/dioxy
SiClx, then encapsulate；Up to the symmetrical ultracapacitor of digital " 1 " shape.
Electro-chemical test shows that the voltage window of the symmetrical ultracapacitor of number " 1 " shape of gained for 2.0V, is lied prostrate in Xun Huan
Peace test sweep speed is 10mV s-1When, electrode surface specific volume is 4.6mF cm-2。
Claims (7)
1. a kind of stacked ultracapacitor that inkjet printing is prepared, 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 polyvinyl alcohol/sulfuric acid, polyvinyl alcohol/sodium sulphate, 1- butyl -3- methylimidazole tetrafluoro boric acids
One kind in salt/silica solid electrolyte.
2. the stacked ultracapacitor that a kind of inkjet printing described in accordance with the claim 1 is prepared, it is characterised in that：It is described
Substrate includes PET substrate (PET), polyetherimide (PEI), paper and other insulating planar substrates.
3. the stacked ultracapacitor that a kind of inkjet printing described in accordance with the claim 1 is prepared, it is characterised in that：It is described
The thickness of electrode film is 0.5-100 μm, and the thickness of membrane is 0.1-10 μm.
4. the preparation method for the stacked ultracapacitor that a kind of inkjet printing is prepared, which is characterized in that specifically include following
Step：
(1) preparation of inkjet printing electrode slurry
It disperses graphene in n,N-Dimethylformamide (DMF), then 3000rpm centrifugation 30min, take supernatant；To obtaining
Supernatant in, add in terpinol, the volume ratio of supernatant and terpinol is 5-20, then rotating pressure-decreasing evaporation DMF；It is obtained
Graphene/terpinol is 3 by volume:1 adds in ethyl alcohol, and obtaining can be with the electrode slurry of inkjet printing；The graphene electricity
Pole slurry concentration is 0.1-5mg mL-1；
(2) preparation of graphene oxide membrane slurry
Graphene oxide using correct hummers methods be made, graphene oxide again with mixed with propylene glycol, graphene oxide slurry
Concentration is 1-10mg mL-1, obtain the graphene oxide membrane slurry reciprocal between 2-4 of Weber number；
(3) preparation of stacked ultracapacitor
Printed substrates are put into printer, electrode slurry is packed into the print cartridge of printer, is printed by computer design arbitrary graphic pattern
First layer Graphene electrodes, can be repeatedly；Graphene oxide membrane slurry is packed into print cartridge again, on first layer electrode
The second layer graphene oxide membrane layer of identical patterns is printed, it can be repeatedly；Then the printing and first on membrane layer
Layer electrode be identical and symmetrical third layer electrode；Solid gel electrolyte is reinjected, encapsulates, it is super to obtain arbitrary shape stacked
Capacitor.
It is 5. special according to the preparation method for the stacked ultracapacitor that a kind of inkjet printing described in claim 4 is prepared
Sign is：The graphene is electrochemical stripping graphene, redox graphene, liquid phase remove graphene, chemical gaseous phase
Deposit the one or more in graphene, graphene composite material.
It is 6. special according to the preparation method for the stacked ultracapacitor that a kind of inkjet printing described in claim 4 is prepared
Sign is：The second layer graphene oxide interlayer is identical with first layer electrode pattern shape, second layer graphene oxide every
Layer is 10 μm~500 μm bigger than the width of first layer electrode.
It is 7. special according to the preparation method for the stacked ultracapacitor that a kind of inkjet printing described in claim 4 is prepared
Sign is：The duplicate printing number is 1-10 times.
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Cited By (4)
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| CN109637819A (en) * | 2018-12-07 | 2019-04-16 | 中国科学院大连化学物理研究所 | A kind of integrated plane supercapacitor and preparation method thereof |
| CN110895998A (en) * | 2019-11-22 | 2020-03-20 | 西安交通大学 | Electrode material ink, preparation method and method for preparing miniature super capacitor by using electrode material ink |
| CN110911177A (en) * | 2019-12-04 | 2020-03-24 | 苏州大学 | Preparation method of asymmetric molybdenum disulfide/graphene micro supercapacitor |
| WO2021040722A1 (en) * | 2019-08-29 | 2021-03-04 | Hewlett-Packard Development Company, L.P. | Flexible printed articles |
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| WO2021040722A1 (en) * | 2019-08-29 | 2021-03-04 | Hewlett-Packard Development Company, L.P. | Flexible printed articles |
| CN110895998A (en) * | 2019-11-22 | 2020-03-20 | 西安交通大学 | Electrode material ink, preparation method and method for preparing miniature super capacitor by using electrode material ink |
| CN110911177A (en) * | 2019-12-04 | 2020-03-24 | 苏州大学 | Preparation method of asymmetric molybdenum disulfide/graphene micro supercapacitor |
| CN110911177B (en) * | 2019-12-04 | 2021-05-14 | 苏州大学 | Preparation method of asymmetric molybdenum disulfide/graphene micro supercapacitor |
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| CN108122685B (en) | 2020-11-10 |
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