CN106548875A - A kind of transparent ultracapacitor of all-solid-state flexible and its prepare and apply - Google Patents
A kind of transparent ultracapacitor of all-solid-state flexible and its prepare and apply Download PDFInfo
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- CN106548875A CN106548875A CN201610953706.9A CN201610953706A CN106548875A CN 106548875 A CN106548875 A CN 106548875A CN 201610953706 A CN201610953706 A CN 201610953706A CN 106548875 A CN106548875 A CN 106548875A
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes 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
- H01G11/54—Electrolytes
- H01G11/56—Solid electrolytes, e.g. gels; Additives therein
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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 present invention relates to a kind of transparent ultracapacitor of all-solid-state flexible and its prepare and apply, ultracapacitor is that, with flexible transparent film as electrode, electrolyte is solid gel electrolyte.Single electrode of the flexible transparent film as ultracapacitor, high molecular polymer are solid gel electrolyte, prepare assembling with reference to Technology designs such as LBL self-assembly, laser ablation or templates and obtain flexible and transparent ultracapacitor.The present invention has the advantages that in preparation technology quick, easily operated, equipment requirements are low, is suitable to large area, preparing on a large scale, have the advantages that strong light transmission, flexibility, chemical property are good in product feature, all solid state capacitor of assembling can be widely applied to the fields such as wearable electrochemical energy storage, electronical display.
Description
Technical field
The invention belongs to capacitor and its prepare and application, the transparent super capacitor of more particularly to a kind of all-solid-state flexible
Device and its preparation and application.
Background technology
With the discovery and utilization of cleaning new energy (solar energy, wind energy, heat energy etc.), people need a kind of energy storage to set
It is standby to store and change these valuable energy.Ultracapacitor has higher cycle life and high charge-discharge speed, while gathering around
There are simple structure, characteristic stable in properties, be allowed on high-power energy conversion, portable electronic device, micro-current power supply unit
There is extensive utilization.
Univ Manchester UK Andre Geim in 2004 et al. are found that Graphene, cause extensive concern and grind
Study carefully, while greatly having promoted the research of two-dimensional material.Two-dimensional material is the lamellar with high aspect ratio or banded structure, its
Thickness is only one or several atomic layer level thickness.Therefore, such material there is larger specific surface area to be applied to and prepares with height
The membrane electrode of performance.
New transparent flexible super capacitor not only can visually meet the electronic information epoch to aesthetic requirement,
Its larger area specific capacitance can provide enough energy stores support performances simultaneously, meet Modern Information, change with oneself energy
Source supply is required.
The content of the invention
The technical problem to be solved be to provide a kind of transparent ultracapacitor of all-solid-state flexible and its prepare and
Using the present invention is prepared with high performance, the flexible electrochemical energy storage device that vision can be saturating；The present invention utilizes lamellar two
The excellent electrochemical energy storage characteristic of dimension material, quickly transmits the advantage of electronics in integrally very as network skeleton with reference to conductive fiber
Good solves this technical problem.Wherein lamellar two-dimensional material is reducing its fiber contacts resistance, while network of fibers is made
Quick and sufficient discharge and recharge approach is provided for rapid electric charge transportation system, the flexibility prepared with efficient high transparency is complete
Solid-state super capacitor, can be widely applied to the energy supply device of the electronic equipment such as wearable, portable.
A kind of transparent ultracapacitor of all-solid-state flexible of the present invention, the ultracapacitor is to be with flexible transparent film
Electrode, electrolyte are solid gel electrolyte；Wherein flexible transparent film electrode is by macromolecule flexible and transparent substrate and is supported on
The ink composition of substrate surface；Wherein solid gel electrolyte is conductive polymer polymer gel.
The load capacity of flexible transparent film electrode ink inside is 5-200mg/cm2, the light transmittance for loading rear film is 40-
90%.
The macromolecule flexible and transparent substrate is polyethylene terephthalate (PET) substrate or polydimethylsiloxane
(PDMS) substrate；Ink is the mixed of the dispersion liquid and conductive fiber solution of the two-dimensional material of graphene oxide and class graphene-structured
Close liquid.The two-dimensional material of class graphene-structured is the one kind in graphene oxide, molybdenum bisuphide, tungsten disulfide, manganese dioxide etc.
Or it is several；Conductive fiber is one or more in nano silver wire (AgNWs), CNT (CNTs) etc.；Lamella knot in ink
The concentration of the two-dimensional material of structure is 1～50mg/mL, and the concentration of conductive fiber is 1～10mg/mL；The solvent of ink is water or second
Alcohol.
The polyvinyl alcohol that the conductive polymer polymer is-sulphuric acid PVA-H2SO4Gel or polyvinyl alcohol-phosphoric acid PVA-
H3PO4Gel；Concentration is 0.5-1mmol/mL.
A kind of preparation method of the transparent ultracapacitor of all-solid-state flexible of the present invention, including：
(1) two-dimensional material of lamellar structure is carried out after pretreatment, dispersion in a solvent, obtains lamellar structure two-dimensional material
Dispersion liquid, as electrode active material ink, then mix with conductive fiber solution, obtain ink；
(2) macromolecule flexible and transparent substrate is carried out into pretreatment, be placed on warm table (heating-up temperature less than flexible substrates it is soft
Change temperature), ink is then loaded, flexible transparent film is obtained；
(3) using step (2) flexible transparent film as ultracapacitor single electrode (being all negative electrode and anode), macromolecule
Polymer is solid gel electrolyte, is then assembled into the tool of flexible transparent film/solid gel electrolyte/flexible transparent film
There is the all-solid-state supercapacitor of sandwich structure；
Or by the electrode (being all negative electrode and anode) that step (2) flexible transparent film is ultracapacitor, using laser incising
Flexible transparent film is etched or is sprayed out the positive pole being interspersed with negative pole (same flat by erosion technology or mask plate spraying process
Face), conductive polymer polymer is solid electrolyte, assembles and obtains all solid state super capacitor for referring to slotting formula structure with plane
Device.
In step (1) pretreatment be carry out intercalation lift-off technology, activation in one or two, make the two dimension of lamellar structure
Material is more readily dispersed in water or ethanol；It is separated into：20～120min of ultrasound, 0～60min of cell pulverization；Wherein it is dispersed in molten
Centrifugation 0～10 time is carried out after in agent, centrifugation rate is 500rpm～10000rpm.
The absorbance of step (1) active material dispersion liquid is 20～95%.
In the step (2), to be dried after being cleaned by ultrasonic again, then process for modifying surface is processed, wherein surface for pretreatment
Modification technology is processed as：Plasma gass, ozone etc..
Step (2) pretreatment is specially：(polyethylene terephthalate (PET) is poly- for macromolecule flexible and transparent substrate
Dimethyl siloxane (PDMS) etc.) respectively through ethanol, the ultrasonic cleaning successively of ultra-pure water, drying temperature be 27 DEG C (room temperature)～
60 DEG C, recycle the process for modifying surface such as plasma gass, ozone that pretreatment is carried out to substrate surface, the time is 5～30min.
In the step (2), the heating-up temperature of warm table is 30～65 DEG C.
In the step (2), carrying method is for spraying or brushes, and the volume for loading ink is 5～100mL.
The structure of the transparent ultracapacitor of gained all-solid-state flexible is that traditional sandwich structure and plane refer to slotting formula structure.
A kind of application of the transparent ultracapacitor of all-solid-state flexible of the present invention, is applied to wearable electrochemical energy storage, electricity
Son shows.
The capacitor of the present invention is that traditional sandwich inserts two kinds of structures of formula, the work with two-dimensional material as electrode with new finger
Property material, conductive fiber for electrode active material skeleton, macromolecule flexible transparent film be substrate, using spraying or spread coating
Prepare transparent electrode thin film, solid electrolyte of the high-molecular gel for capacitor, with reference to LBL self-assembly, laser ablation or template
The Technology designs such as method prepare assembling and obtain flexible and transparent ultracapacitor.
Two-dimensional material is the lamellar with high aspect ratio or banded structure, and its thickness is only one or several atomic layers thicks
Degree.Therefore, such material there is larger specific surface area to be applied to and prepares with high performance membrane electrode.Conductive fiber conduct
Framing structure in flexible transparent electrode provide efficient electric transmission approach and reduce two-dimensional material between stack degree so as to
Reduce absorbance.With reference to masking techniques such as spraying, brushings, fast and effectively prepare complete with the flexible high-performance of high transmission rate
Solid state energy memory device, can be widely applied to multiple kinds of energy conversion and application.
Beneficial effect
(1) present invention has in preparation technology that quick, easily operated, equipment requirements are low, be suitable to large area, extensive makes
The advantage such as standby；
(2) the transparent two-dimensional material base transparent flexible electrode prepared by the present invention, has light transmission in product feature
By force, it is flexible, the advantages of chemical property is good；
(3) all-solid-state supercapacitor based on transparent flexible electrode prepared by the present invention, with high area specific capacitance,
High light transmission rate, the flexible advantage carried with can be widely used in the fields such as portable, wearable electronic device.
Description of the drawings
Digital photograph figures of the Fig. 1 for molybdenum bisuphide aqueous dispersions used by embodiment 1；
Digital photograph figures of the Fig. 2 for graphene oxide aqueous dispersions used by embodiment 4；
Fig. 3 is the digital photograph of the flexible transparent film electrode prepared by embodiment 1；
Fig. 4 is the flexible transparent film electrode stereoscan photograph prepared by embodiment 1；
Fig. 5 is the digital photograph of the flexible transparent film electrode prepared by embodiment 4；
Fig. 6 is the flexible transparent film electrode stereoscan photograph prepared by embodiment 4；
Fig. 7 is the slotting formula all-solid-state flexible of finger assembled as single electrode with flexible transparent film electrode prepared by embodiment 2
The digital photograph of device；
Fig. 8 is the structural representation of the transparent sandwich structure ultracapacitor of all-solid-state flexible prepared by embodiment 1；
Fig. 9 is the transparent structural representation for referring to the formula of inserting structure ultracapacitor of all-solid-state flexible prepared by embodiment 4；
Figure 10 is the uv-visible absorption spectra curve of the flexible transparent electrode prepared by embodiment 1-4；
Figure 11 is that the cyclic voltammetric of the transparent ultracapacitor of all-solid-state flexible of the sandwich structure prepared by embodiment 1 is bent
Line；
Figure 12 is the circulation of the slotting formula flexible and transparent ultracapacitor of all solid state finger that the finger prepared by embodiment 2 inserts formula structure
Volt-ampere curve；
Figure 13 is that the cyclic voltammetric of the transparent ultracapacitor of all-solid-state flexible of the sandwich structure prepared by embodiment 3 is bent
Line；
Figure 14 is the circulation of the slotting formula flexible and transparent ultracapacitor of all solid state finger that the finger prepared by embodiment 4 inserts formula structure
Volt-ampere curve.
Specific embodiment
With reference to specific embodiment, by taking graphene oxide with molybdenum bisuphide as an example, the present invention is expanded on further.Ying Li
Solution, these embodiments are only illustrative of the invention and is not intended to limit the scope of the invention.In addition, it is to be understood that reading this
After the content of bright instruction, those skilled in the art can be made various changes or modifications to the present invention, and these equivalent form of values are same
Fall within the application appended claims limited range.
Embodiment 1
The molybdenum disulfide nano sheet powder body of few layer is obtained using lithium ion graft process, 50mg molybdenum disulfide nano sheets is weighed and is surpassed
Sound 30min, cell pulverization 10min are allowed to be dispersed in 20mL ultra-pure waters, then 8min is centrifuged under 1000rpm, dispel stripping
Incomplete block molybdenum bisuphide, obtains 2.5mg/mL molybdenum bisuphide aqueous dispersions.By AgNWs (2mg/mL) ethanol solution with it is upper
Molybdenum bisuphide aqueous dispersions are stated by 2：1 volume ratio is mixed, and is stood.
Flexible PDMS substrates are passed sequentially through into ethanol, ultra-pure water is cleaned by ultrasonic 5min respectively, argon again after drying at room temperature
Process 5min is modified under gas plasma.The flexible substrates handled well are placed on warm table and are heated to 50 DEG C, use brush pen
Brush is directly brushed dispersion liquid in flexible substrates, and the uniform 20mL that brushes obtains flexible transparent film as electrode.Using biography
System sandwich structure (structure as shown in Figure 8), 1M PVA-H2SO4For gel electrolyte, the transparent super electricity of assembling all-solid-state flexible
Container.
The digital photograph of molybdenum bisuphide aqueous dispersions used is shown in Fig. 1, the transparent molybdenum bisuphide/silver nanoparticle of the flexibility of preparation
The digital photograph of line membrane electrode is as shown in figure 3, respective surfaces stereoscan photograph is as shown in figure 4, uv-visible absorption spectra
As shown in Figure 10.The circulation of the capacitor of all solid state transparency electrode of the traditional sandwich structure assembled as single electrode with this electrode
As shown in figure 11, wherein scanning speed is 0.2mV/s to volt-ampere curve.
Embodiment 2
The molybdenum disulfide nano sheet powder body of few layer is obtained using lithium ion graft process, 50mg molybdenum disulfide nano sheets is weighed and is surpassed
Sound 60min, cell pulverization 10min are allowed to be dispersed in 10mL ultra-pure waters, then 8min are centrifuged under 1000rpm, dispel stripping
Incomplete block molybdenum bisuphide, obtains the molybdenum bisuphide aqueous dispersions of 5mg/mL.By CNTs (2mg/mL) ethanol solution with it is upper
Molybdenum bisuphide aqueous dispersions are stated by 2：1 volume ratio is mixed, and is stood.
Flexible PET base is passed sequentially through into ethanol, ultra-pure water is cleaned by ultrasonic 20min respectively, dried in 50 DEG C of baking oven
It is modified process 10min afterwards again under ozone.The flexible substrates handled well are placed on warm table and are heated to 50 DEG C, use air brush
Directly dispersion liquid is sprayed on flexible base board, is uniformly sprayed 10mL and flexible transparent film is obtained as electrode.Using laser
Engraving technology etches transparency electrode with the both positive and negative polarity (structure as shown in Figure 9) for referring to that slotting formula plane is interspersed, 1MPVA-
H2PO4For gel electrolyte, the transparent ultracapacitor of assembling all-solid-state flexible.
Uv-visible absorption spectra curve using the transparent single electrode thin film obtained after brushing is as shown in Figure 10, this
Digital photograph of the single electrode after laser ablation is as shown in Figure 7.The new finger that assembling is obtained inserts all solid state of formula structure
As shown in figure 12, wherein scanning speed is 0.2mV/s to the cyclic voltammetry curve of bright ultracapacitor.
Embodiment 3
Large-sized graphene oxide powder is prepared using Hummer ' s methods are improved, 20mg graphene oxides are weighed, ultrasound
60min, cell pulverization 10min are allowed to be dispersed in 5mL ultra-pure waters, then 5min is centrifuged under 1000rpm, dispel and cannot disperse completely
Full graphene oxide, obtains the graphene oxide aqueous dispersions of 4mg/mL.By CNTs (2mg/mL) ethanol solution and above-mentioned two
Molybdenum sulfide aqueous dispersions press 1：1 volume ratio is mixed, and is stood.
Flexible PET base is passed sequentially through into ethanol, ultra-pure water is cleaned by ultrasonic 10min respectively, dried in 40 DEG C of baking oven
It is modified process 15min afterwards again under ozone.The flexible substrates handled well are placed on warm table and are heated to 50 DEG C, use writing brush type brush
Directly mixed ink is uniformly brushed on flexible base board, uniform 40mL mixed inks of brushing obtain flexible transparent film
As electrode.Using traditional sandwich structure, 0.5M PVA-H2PO4For gel electrolyte, all-solid-state flexible is assembled transparent super
Capacitor.
Wherein the uv-visible absorption spectra curve of single electrode transparent membrane is as shown in Figure 10, all solid state super after assembling
As shown in figure 13, wherein scanning speed is 0.2mV/s to the cyclic voltammetry curve of capacitor.
Embodiment 4
Large-sized graphene oxide powder is prepared using Hummer ' s methods are improved, graphene oxide prepared by 20mg is surpassed
Sound 30min, cell pulverization 10min are allowed to be dispersed in 10mL ultra-pure waters, then 5min is centrifuged under 800rpm, dispel dispersion not
Completely graphene oxide, obtains the graphene oxide aqueous dispersions of 2mg/mL.By AgNWs (5mg/mL) ethanol solution with it is above-mentioned
Molybdenum bisuphide aqueous dispersions press 2：1 volume ratio is mixed, and is stood.
Flexible PET base is passed sequentially through into ethanol, ultra-pure water is cleaned by ultrasonic 20min respectively, dried in 50 DEG C of baking oven
It is modified process 15min afterwards again under ozone.The flexible substrates handled well are placed on warm table and are heated to 55 DEG C, use air brush
Directly dispersion liquid is sprayed on flexible base board, is uniformly sprayed 20mL mixed inks and flexible transparent film is obtained as electrode.
Transparency electrode is etched with the both positive and negative polarity for referring to that slotting formula plane is interspersed, 1M PVA-H using laser-engraving technique2SO4For
Gel electrolyte, the transparent ultracapacitor of assembling all-solid-state flexible.
The digital photograph of the aqueous dispersions of graphene oxide used is shown in Fig. 2, and the transparent graphene oxide of the flexibility of preparation/
The digital photograph of nano silver wire membrane electrode is as shown in figure 5, respective surfaces stereoscan photograph is as shown in fig. 6, ultraviolet-visible is inhaled
Receive the curve of spectrum as shown in Figure 10.The capacitor of all solid state transparency electrode of formula is inserted with the new finger that this electrode is assembled as single electrode
Cyclic voltammetry curve as shown in figure 14, wherein scanning speed is 0.2mV/s.
Claims (10)
1. the transparent ultracapacitor of a kind of all-solid-state flexible, it is characterised in that：The ultracapacitor is with flexible transparent film
For electrode, electrolyte is solid gel electrolyte；Wherein flexible transparent film electrode is by macromolecule flexible and transparent substrate and load
Constitute in the ink of substrate surface；Wherein solid gel electrolyte is conductive polymer polymer gel.
2. the transparent ultracapacitor of a kind of all-solid-state flexible according to claim 1, it is characterised in that：Flexible transparent film
The load capacity of electrode ink inside is 5-200mg/cm2, load rear film light transmittance is 40-90%.
3. the transparent ultracapacitor of a kind of all-solid-state flexible according to claim 1, it is characterised in that：The macromolecule is soft
Property transparent substrates be polyethylene terephtalate substrate or polydimethylsiloxane substrate；Ink is tied for lamella
The mixed liquor of the dispersion liquid and conductive fiber solution of structure two-dimensional material.
4. the transparent ultracapacitor of a kind of all-solid-state flexible according to claim 3, it is characterised in that：The two of lamellar structure
Dimension material is graphene oxide, molybdenum bisuphide, tungsten disulfide, one or more in manganese dioxide；Conductive fiber is silver nanoparticle
One or more in line (AgNWs), CNT (CNTs) etc.；In ink the concentration of the two-dimensional material of lamellar structure be 1～
50mg/mL, the concentration of conductive fiber is 1～10mg/mL；The solvent of ink is water and/or ethanol.
5. the transparent ultracapacitor of a kind of all-solid-state flexible according to claim 1, it is characterised in that：The macromolecule is led
Electric polymer is polyvinyl alcohol-sulphuric acid PVA-H2SO4Gel or polyvinyl alcohol-phosphoric acid PVA-H3PO4Gel.
6. the preparation method of the transparent ultracapacitor of a kind of all-solid-state flexible as described in claim 1-5 is arbitrary, including：
(1) two-dimensional material of lamellar structure is carried out after pretreatment, dispersion in a solvent, obtains dividing for lamellar structure two-dimensional material
Dispersion liquid, is then mixed with conductive fiber solution, obtains ink；
(2) macromolecule flexible and transparent substrate is carried out into pretreatment, is placed on warm table, then loaded ink, obtain flexible and transparent
Thin film；
(3) using step (2) flexible transparent film as ultracapacitor single electrode, high molecular polymer be solid gel electrolysis
Matter, be then assembled into flexible transparent film/solid gel electrolyte/flexible transparent film with all solid state of sandwich structure
Ultracapacitor；
Or by the electrode that step (2) flexible transparent film is ultracapacitor, using laser etching techniques or mask plate spraying process,
Flexible transparent film is etched or is sprayed out the positive pole and negative pole being interspersed, conductive polymer polymer is solid electrolyte,
Assembling is obtained with the all-solid-state supercapacitor for referring to the formula of inserting structure.
7. the preparation method of the transparent ultracapacitor of a kind of all-solid-state flexible according to claim 6, it is characterised in that：Step
Suddenly in (1) pretreatment be carry out intercalation, activation in one or two；It is separated into：Ultrasound, cell pulverization.
8. the preparation method of the transparent ultracapacitor of a kind of all-solid-state flexible according to claim 6, it is characterised in that：Institute
Pretreatment is stated in step (2) to be dried after being cleaned by ultrasonic again, then process for modifying surface is processed；The heating-up temperature of warm table is
30～65 DEG C.
9. the preparation method of the transparent ultracapacitor of a kind of all-solid-state flexible according to claim 6, it is characterised in that：Institute
Load in stating step (2) is spraying or brushing.
10. the application of the transparent ultracapacitor of a kind of all-solid-state flexible as described in claim 1-5 is arbitrary, it is characterised in that：
It is applied to wearable electrochemical energy storage, electronical display.
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