CN109755027A - Composite graphite alkene film, high-energy ultracapacitor and intelligent flexible device - Google Patents
Composite graphite alkene film, high-energy ultracapacitor and intelligent flexible device Download PDFInfo
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- CN109755027A CN109755027A CN201910022830.7A CN201910022830A CN109755027A CN 109755027 A CN109755027 A CN 109755027A CN 201910022830 A CN201910022830 A CN 201910022830A CN 109755027 A CN109755027 A CN 109755027A
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Abstract
The invention discloses a kind of composite graphite alkene film, high-energy ultracapacitor and intelligent flexible devices, belong to electrochemical energy storage technical field.The present invention passes through the piece interlamellar spacing of accuracy controlling graphene film, match piece interlamellar spacing with electrolyte intermediate ion size, electrochemical energy storage process optimization is realized, and greatly improves the energy stored by capacitor, and the flexible device of Intellectual power output is constructed based on the film.Present invention process process is simply compatible with the prior art, and energy large scale preparation, the energy-storage property of device can be substantially improved, therefore have great application prospect.
Description
Technical field
The present invention relates to electrochemical energy storage technical fields, and in particular to a kind of composite graphite alkene film, the super electricity of high-energy
Container and intelligent flexible device.
Background technique
Supercapacitor has that quickly-chargeable, power are high, have extended cycle life, operating temperature range is wide, security performance is high
The advantages that, it may be used as large power supply, all have in fields such as hybrid-electric car, backup power source, portable electronic devices
Vast potential for future development.However, supercapacitor is compared to the lower energy density of the battery (energy stored in unit volume
Amount) limit its wider application range.Especially in the practical application of portable intelligent device, realize in limited bulk more
More energy storages becomes demand, i.e. promotion volume energy density.
Electrode material is the important component of supercapacitor, in recent years, the new carbons such as graphene, carbon nanotube
Discovery and application to energy storage field bring huge promotion.By taking grapheme material as an example, it is used as electrode of super capacitor
Theoretical capacity be up to 550F g-1, while there is good electric conductivity and stability.In addition, compared to transition metal material, stone
Black alkene material can under higher potential window steady operation, be provided with as high-energy, high-capacity super capacitor electrode
Huge application potential.
Currently, many work are made that research for how to improve the capacity of grapheme material, however, it is close for energy
Degree bring promotes the demand that practical application is but far not achieved.In order to realize the raising of final energy density, one from device sheet
Body angle is set out, and the preparation for material is essential.One of key factor is the operating potential of supercapacitor
Window is determined by selected electrolyte under normal conditions.Ionic liquid has the potential window of up to 4.0V, it is considered to be
Realize the good selection of high-energy density super capacitor.And a kind of electrode material how is prepared, allow to and different electricity
Liquid matching (i.e. electrode material adjustable porosity control) is solved, to realize that the optimization of performance but still suffers from huge challenge.And
In portable and wearable electronic product application, the flexibility of prepared supercapacitor is also essential.In addition,
To meet different output demands, if can make single device that alternative output may be implemented by intelligentized design
Function also still needs to solve.
Summary of the invention
The purpose of the present invention is to provide a kind of composite graphite alkene film, high-energy ultracapacitor and intelligent flexible devices
Part.Firstly, making it match the size of electrolyte intermediate ion by the pore structure for regulating and controlling electrode material, entire device is realized
High-energy density output, has reached the level of lead-acid battery and has been provided simultaneously with higher power density；Being constructed based on this can intelligence
The all-solid-state flexible device that can be exported, therefore have a vast market application prospect.
The technical solution adopted in the present invention is as follows:
A kind of composite graphite alkene film, the preparation process of the composite graphite alkene film are as follows: also by graphite oxide and thermal expansion
Former graphene is added to the water with certain proportion, obtains uniform suspension by ultrasonic disperse；Then by uniform suspension into
Row vacuum filtration obtains film and dries；After film progress hydrogen iodide steam reduction after drying promotes its electric conductivity, that is, obtain
The composite graphite alkene film；In the composite graphite alkene film, the content for thermally expanding reduced graphene is 40-60wt.%.
The composite graphite alkene film with a thickness of between 10-200 microns.
The composite graphite alkene film is made of graphite oxide and thermal expansion reduced graphene, thermally expands reduced graphene piece
It is dispersed in graphite oxide；By regulation graphite oxide and thermally expand ratio (the i.e. adjustment graphite between reduced graphene
The mode that alkene lamella stacks), the piece interlamellar spacing of graphene can be adjusted.
The composite graphite alkene film is used as electrode active material, can due to its design feature with self-supporting
Directly as working electrode without using additional collector.High-energy super capacitor is constructed using composite graphite alkene film
Following two mode can be used in device:
First way are as follows: with composite graphite alkene film directly as working electrode, according to the suitable of electrode/membrane/electrode
Sequence assembly, and ionic liquid is injected as electrolyte, it is assembled into the supercapacitor of high-energy density；The diaphragm is three-layered node
The polypropylene-polyethylene of structure-polypropylene composite materials diaphragm, single-layer polypropylene film, monolayer polyethylene film, fibreglass diaphragm or fiber
Plain diaphragm；
The second way are as follows: with composite graphite alkene film directly as working electrode, without using diaphragm, using solid-state electricity
Xie Zhi is assembled according to electrode-solid electrolyte-electrode sequence, is then encapsulated, that is, be made with high potential window with encapsulating material
The all-solid-state flexible supercapacitor of mouth；Wherein: the encapsulating material is polyethylene terephthalate, polydimethylsiloxanes
Alkane, ethylene-vinyl acetate copolymer or polyvinyl butyral resin；The all-solid-state flexible with high potential window assembled
Supercapacitor can realize 0-180 ° and bend at any angle.
The present invention further constructs intelligent flexible device using the composite graphite alkene film, specifically: with composite graphite
Alkene film is assembled into electrode-solid electrolyte-electrode structure using solid electrolyte directly as working electrode；It will be described
Electrode-solid electrolyte-electrode structure is then sealed with encapsulating material as a unit by stacking multiple units again
Dress, acquisition have the regulatable all solid state intelligent flexible capacitor element of output.
During above-mentioned building high-energy ultracapacitor and intelligent flexible device, the solid electrolyte refer to from
Sub- liquid is conducting medium, using polyvinylidene fluoride-hexafluoropropylene copolymer as the gel state electrolyte of matrix, specifically by from
Sub- liquid, acetone and polyvinylidene fluoride-hexafluoropropylene copolymer mixed material are cured rear acquired.
The ionic liquid is 1- ethyl-3-methylimidazole tetrafluoroborate, 1- ethyl-3-methylimidazole hexafluorophosphoric acid
Bis- (trifluoromethyl sulfonyl) imines of salt, 1- ethyl-3-methylimidazole quinoline, 1- butyl -3- methyl imidazolium tetrafluoroborate, 1- fourth
Two (trimethyl fluoride sulfonyl) acid imide of base -3- methylimidazole hexafluorophosphate or 1- butyl -3- methylimidazole.
During above-mentioned building high-energy ultracapacitor and intelligent flexible device, in the composite graphite alkene film
Graphene film interlamellar spacing with matched using the size of ionic liquid, i.e., in composite graphite alkene film graphene film interlamellar spacing have
There is the pore structure to match with object ion liquid.Described interlamellar spacing refers to the spacing in film between graphene film, " phase
Matching " refer to piece interlamellar spacing equal or close to ion size, the difference of the ion size of graphene film interlamellar spacing and ionic liquid
Less than 0.1nm.
Made all solid state intelligent capacitor device can be according to the difference of connection type to realize different output demands, i.e.,
When external circuit connects two structural units in a series arrangement, the output purpose for increasing potential window can reach；When external circuit with
When parallel way connects two structural units, the output purpose for increasing capacity can reach.
Design principle of the present invention is as follows:
By the piece interlamellar spacing in regulation graphene film, realize the effect of entire electrode material porosity.When
When the pore-size of electrode material and the ion size of electrolyte match, the space utilization of hole has reached optimization, thus
Maximise volume energy density.In the design of all-solid-state flexible supercapacitor, graphene membrane electrode material itself is good
Bending performance also ensure the flexibility of entire device.It is by changing external circuit connection according to demand in intelligent device design
Mode realizes different output effects.
It advantages of the present invention and has the beneficial effect that:
1, the self-supporting graphene film itself in the ultracapacitor device that the present invention is assembled, as active material
Working electrode be can be used as without using additional collector.
2, the spacing that the present invention designs is adjusted graphene film structure and can effectively control the porosity of material,
To realize the matching with electrolyte, and then maximise the energy density of device.
3, the method and process of the present invention for realizing that porosity is adjusted is simple, and repeatability is strong, and is easy to extensive
Amplification production.
4, present invention self-supporting spacing produced, which is adjusted graphene film and applies, has popularity, can be effectively used for
The supercapacitor of different electrolytes system constructs, such as flexible all-solid state equipment.
5, the present invention intelligent all-solid-state flexible device produced can change connection type according to demand, increase electricity to reach
Position window or the output purpose for increasing capacity.
Detailed description of the invention
Fig. 1 is that the present invention uses graphite oxide and thermal expansion reduced graphene presoma to make self-supporting graphene film
Schematic diagram.
Fig. 2 is to use the performance for the film that different proportion presoma is produced after regulation.
Fig. 3 is close for the symmetrical supercapacitor energy energy achieved that the graphene film using optimization is assembled into
The comparison of degree and power density and different type energy storage device.
Fig. 4 is the composed structure schematic diagram and its photo of made intelligent all-solid-state flexible device.
Fig. 5 is the schematic diagram for the different connection types of intelligent device and has corresponding constant current charge-discharge curve.
Specific embodiment
The present invention is illustrated with reference to the accompanying drawings and embodiments.
The preparation process of self-supporting graphene film used in following embodiment will be made in advance first as shown in Figure 1:
Standby graphite oxide is added to the water with thermal expansion reduced graphene with certain proportion, obtains uniform solution by ultrasonic disperse；With
Vacuum filtration obtains film and dries afterwards；Carried out further hydrogen iodide steam reduction again to be promoted after electric conductivity using workmanship
Make electrode.
The process that the hydrogen iodide steam reduction promotes electric conductivity can refer to (the document 1:Direct reduction of document 1
of graphene oxide films into highly conductive and flexible grapheme films by
Hydrohalic acids, Carbon, 2010,48,4466-4474).
The thermal expansion reduced graphene is to obtain using graphene oxide as raw material by High-Temperature Deoxygenation and rapid expanding
Thermal expansion redox graphene (Thermal-shock Reduced Graphene-oxide), can refer to document 2-3 (text
Offer 2:Fabrication of graphene/polyaniline composite paper via in situ anodic
Electropolymerization for high-performance flexible electrode, ACS Nano2009,3,
1745-1752；Document 3:J.Mater.Chem.A, 2017,5,24686-24694).
The solid electrolyte refers to will be dissolved with polyvinylidene fluoride-hexafluoropropylene copolymer acetone of ionic liquid point
Obtained electrolyte gel after dispersion liquid solidification.
Comparative example 1
In above-mentioned graphene film preparation process, following dispersion liquid: (1) pure oxygen graphite is used respectively；(2) stone is aoxidized
Ink-thermal expansion graphene (25wt.% thermally expands graphene)；(3) (75wt.% thermally expands stone to graphite oxide-thermal expansion graphene
Black alkene).Obtained film is assembled in 1- ethyl-3-methylimidazole tetrafluoro boric acid salt electrolyte and obtains symmetrical super capacitor
Device, and charge-discharge test is carried out to it.As a result it as shown in Fig. 2, maximum volumetric capacitance is not implemented in above-mentioned 3 samples, says
The interstitial space not up to optimized in its bright thermal energy storage process utilizes.
Embodiment 1
In above-mentioned graphene film preparation process, using graphite oxide-thermal expansion graphene, (50wt.% thermally expands stone
Black alkene) dispersion liquid, and obtained film is assembled to acquisition pair in 1- ethyl-3-methylimidazole tetrafluoro boric acid salt electrolyte
Claim supercapacitor, carries out charge-discharge test.As a result as shown in Figure 2, it is possible to find compared with graphene film made of this ratio
3 samples in above-mentioned comparative example 1 show higher volumetric capacitance, illustrate that it has similar sample in thermal energy storage process
The interstitial space of middle optimization utilizes.
Embodiment 2
Using self-supporting graphene film most outstanding in above-described embodiment 1 as working electrode, and pass through vacuum filtration
When be added more dispersion liquids mode adjust its unit area load capacity to be commercialized standard 10mg cm-2, then in 1- ethyl-
Assembling obtains symmetrical supercapacitor in 3- methyl imidazolium tetrafluoroborate electrolyte, and calculates the volume energy of obtained device entirety
Metric density.As a result as shown in figure 3, can reach 90.1Wh L by super capacitor energy density prepared by this method-1, not only far
Higher than conventional commercial supercapacitor (5-8Wh L-1), it has been even up to level (the 50-90Wh L of lead-acid battery-1), and simultaneously
Have more than the two higher power densities of magnitude.Illustrate the energy storage that production device can be substantially improved through the invention
Energy.
Embodiment 3
Using graphene film prepared in embodiment 1 as working electrode, using dissolved with ionic liquid (1- ethyl -3- first
Base tetrafluoroborate) polyvinylidene fluoride-hexafluoropropylene copolymer as solid electrolyte, and use poly- terephthaldehyde
Sour glycol ester is encapsulating material, makes all solid state intelligent flexible device with construction shown in Fig. 4 (a), obtained device is real
Object figure photo can be found in Fig. 4 (b).The all solid state intelligent flexible device can be by changing connection type to meet different input need
It asks.As shown in Fig. 5 (a), due to the difference of connection type, device successively realizes the effect of series connection output and parallel output, point
Do not achieved the purpose that increase potential window and increased capacity (as shown in the charging and discharging curve in Fig. 5 (b)).
Claims (11)
1. a kind of composite graphite alkene film, it is characterised in that: the preparation process of the composite graphite alkene film are as follows: by graphite oxide with
Thermal expansion reduced graphene is added to the water with certain proportion, obtains uniform suspension by ultrasonic disperse；It then will be uniform
Suspension is filtered by vacuum to obtain film and be dried；Film after drying carries out hydrogen iodide steam reduction and promotes its electric conductivity
Afterwards, that is, the composite graphite alkene film is obtained；In the composite graphite alkene film, the content for thermally expanding reduced graphene is 40-
60wt.%.
2. composite graphite alkene film according to claim 1, it is characterised in that: the composite graphite alkene film with a thickness of
Between 10-200 microns.
3. composite graphite alkene film according to claim 1, it is characterised in that: the composite graphite alkene film is by oxidation stone
Ink is dispersed in graphite oxide with thermal expansion reduced graphene composition, thermal expansion reduced graphene piece；It is aoxidized by regulation
Ratio between graphite and thermal expansion reduced graphene, can adjust the piece interlamellar spacing of graphene.
4. a kind of high-energy ultracapacitor containing composite graphite alkene film described in claim 3, it is characterised in that: with compound
Graphene film is assembled into high-energy ultracapacitor directly as working electrode, according to following two mode；
First way are as follows: according to the assembled in sequence of electrode/membrane/electrode, and inject ionic liquid as electrolyte, be assembled into
The supercapacitor of high-energy density；
The second way are as follows: without using diaphragm, using solid electrolyte, according to electrode-solid electrolyte-electrode sequence group
Dress, is then encapsulated with encapsulating material, that is, the all-solid-state flexible supercapacitor with high potential window is made；Wherein: described solid
State electrolyte refers to using ionic liquid as conducting medium, using polyvinylidene fluoride-hexafluoropropylene copolymer as the gel state of matrix
Electrolyte；
In first way and the second way, graphene film interlamellar spacing in the composite graphite alkene film and electrolysis is used
The ion size of liquid matches.
5. high-energy ultracapacitor according to claim 4, it is characterised in that: the diaphragm is poly- the third of three-decker
Alkene-polyethylene-polypropylene composite diaphragm, single-layer polypropylene film, monolayer polyethylene film, fibreglass diaphragm or cellulosic separator.
6. high-energy ultracapacitor according to claim 4, it is characterised in that: the encapsulating material is poly- terephthaldehyde
Sour glycol ester, dimethyl silicone polymer, ethylene-vinyl acetate copolymer or polyvinyl butyral resin.
7. high-energy ultracapacitor according to claim 4, it is characterised in that: what the second way was assembled has height
The all-solid-state flexible supercapacitor of potential window can realize 0-180 ° and bend at any angle.
8. high-energy ultracapacitor according to claim 4, it is characterised in that: the ionic liquid is 1- ethyl -3-
Methyl imidazolium tetrafluoroborate, 1- ethyl-3-methylimidazole hexafluorophosphate, the bis- (trifluoromethyls of 1- ethyl-3-methylimidazole quinoline
Sulfonyl) imines, 1- butyl -3- methyl imidazolium tetrafluoroborate, 1- butyl -3- methylimidazole hexafluorophosphate or 1- butyl -
3- methylimidazole two (trimethyl fluoride sulfonyl) acid imide.
9. a kind of intelligent flexible device constructed using composite graphite alkene film described in claim 3, it is characterised in that: with compound
Graphene film is assembled into electrode-solid electrolyte-electrode structure using solid electrolyte directly as working electrode；It will
Electrode-solid electrolyte-electrode structure as a unit, by stack multiple units then again with encapsulating material into
Row encapsulation, acquisition have the regulatable all solid state intelligent flexible capacitor element of output.
10. intelligent flexible device according to claim 9, it is characterised in that: the solid electrolyte refers to ionic liquid
Body is conducting medium, using polyvinylidene fluoride-hexafluoropropylene copolymer as the gel state electrolyte of matrix, the composite graphite alkene
Film has the pore structure to match with used ionic liquid.
11. intelligent flexible device according to claim 9, it is characterised in that: made all solid state intelligent capacitor device
It can be according to the difference of connection type to realize different output demands, i.e., when external circuit connects two structural units in a series arrangement
When, it can reach the output purpose for increasing potential window；When external circuit connects two structural units with parallel way, increasing can reach
Add the output purpose of capacity.
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| CN110225691A (en) * | 2019-06-05 | 2019-09-10 | 南京理工大学 | A kind of production method for strengthening the carbon-based composite membrane that radiates |
| CN110828198A (en) * | 2019-11-05 | 2020-02-21 | 中国科学院合肥物质科学研究院 | Laminated interdigital electrochemical capacitor and preparation method thereof |
| CN110828197A (en) * | 2019-11-05 | 2020-02-21 | 中国科学院合肥物质科学研究院 | Solid laminated interdigital electrochemical capacitor and preparation method thereof |
| CN112542329A (en) * | 2020-11-17 | 2021-03-23 | 伊诺福科光学技术有限公司 | High energy density super capacitor |
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