CN106098410A - Laser one-step method prepares ultracapacitor Graphene/manganese oxide flexible electrode - Google Patents
Laser one-step method prepares ultracapacitor Graphene/manganese oxide flexible electrode Download PDFInfo
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- CN106098410A CN106098410A CN201610470858.3A CN201610470858A CN106098410A CN 106098410 A CN106098410 A CN 106098410A CN 201610470858 A CN201610470858 A CN 201610470858A CN 106098410 A CN106098410 A CN 106098410A
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 163
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 106
- 238000000034 method Methods 0.000 title claims abstract description 13
- 238000002360 preparation method Methods 0.000 claims abstract description 49
- 239000011572 manganese Substances 0.000 claims abstract description 40
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 24
- 239000003990 capacitor Substances 0.000 claims abstract description 21
- 239000000758 substrate Substances 0.000 claims abstract description 19
- 150000001875 compounds Chemical class 0.000 claims abstract description 16
- 239000012298 atmosphere Substances 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 8
- 150000002697 manganese compounds Chemical class 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 4
- 238000000576 coating method Methods 0.000 claims abstract description 4
- 239000002131 composite material Substances 0.000 claims description 15
- 239000002390 adhesive tape Substances 0.000 claims description 10
- 229910002804 graphite Inorganic materials 0.000 claims description 9
- 239000010439 graphite Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229910021485 fumed silica Inorganic materials 0.000 claims description 7
- 238000009413 insulation Methods 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- 239000004642 Polyimide Substances 0.000 claims description 6
- 239000011656 manganese carbonate Substances 0.000 claims description 6
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 claims description 6
- 229910000357 manganese(II) sulfate Inorganic materials 0.000 claims description 6
- 229920001721 polyimide Polymers 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- 239000008151 electrolyte solution Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- -1 polyethylene terephthalate Polymers 0.000 claims description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 4
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 4
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 4
- 239000007832 Na2SO4 Substances 0.000 claims description 4
- 239000011889 copper foil Substances 0.000 claims description 4
- 239000011565 manganese chloride Substances 0.000 claims description 4
- IPJKJLXEVHOKSE-UHFFFAOYSA-L manganese dihydroxide Chemical compound [OH-].[OH-].[Mn+2] IPJKJLXEVHOKSE-UHFFFAOYSA-L 0.000 claims description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 4
- 229910052756 noble gas Inorganic materials 0.000 claims description 4
- 230000003647 oxidation Effects 0.000 claims description 4
- 238000007254 oxidation reaction Methods 0.000 claims description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 4
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- 239000005030 aluminium foil Substances 0.000 claims description 3
- 230000008859 change Effects 0.000 claims description 3
- 239000002608 ionic liquid Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 2
- 239000004952 Polyamide Substances 0.000 claims description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- 229910052786 argon Inorganic materials 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000001569 carbon dioxide Substances 0.000 claims description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052737 gold Inorganic materials 0.000 claims description 2
- 239000010931 gold Substances 0.000 claims description 2
- 229920002521 macromolecule Polymers 0.000 claims description 2
- 239000007769 metal material Substances 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 230000001590 oxidative effect Effects 0.000 claims description 2
- 229920003223 poly(pyromellitimide-1,4-diphenyl ether) Polymers 0.000 claims description 2
- 229920002647 polyamide Polymers 0.000 claims description 2
- 239000012286 potassium permanganate Substances 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 claims description 2
- 239000004332 silver Substances 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 3
- 230000001678 irradiating effect Effects 0.000 claims 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 1
- 150000002148 esters Chemical class 0.000 claims 1
- 239000007788 liquid Substances 0.000 claims 1
- 239000004575 stone Substances 0.000 claims 1
- 230000008901 benefit Effects 0.000 abstract description 7
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000009467 reduction Effects 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000001351 cycling effect Effects 0.000 abstract description 2
- 238000000354 decomposition reaction Methods 0.000 abstract 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 239000006181 electrochemical material Substances 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000002349 favourable effect Effects 0.000 abstract 1
- 238000011065 in-situ storage Methods 0.000 abstract 1
- 239000003792 electrolyte Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002485 combustion reaction Methods 0.000 description 3
- 238000007599 discharging Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 2
- 229910044991 metal oxide Inorganic materials 0.000 description 2
- 150000004706 metal oxides Chemical class 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 229920002799 BoPET Polymers 0.000 description 1
- 241000446313 Lamella Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002498 deadly effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 230000003760 hair shine Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/46—Metal oxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
-
- 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
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Nanotechnology (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention belongs to electrochemical material field, disclose a kind of method utilizing laser one step in-situ reducing graphene oxide, decomposition manganese compound to prepare Graphene/manganese oxide flexible electrode, and applied in the middle of ultracapacitor.Wherein the preparation method of Graphene/manganese oxide flexible electrode comprises the following steps: uniformly mixed with the compound of manganese by the aqueous solution of graphene oxide, and coating is on a flexible substrate；Laser is utilized to irradiate the compound film of graphene oxide/manganese prepared by above-mentioned steps under inert atmosphere protection: while graphene oxide is become Graphene by laser reduction, manganese compound decomposes obtains manganese oxide.Pure Graphene ultracapacitor is lower than electric capacity；Manganese oxide ultracapacitor cyclical stability is poor, is combined by both materials, can maximize favourable factors and minimize unfavourable ones, and gives full play to the advantage of the two, obtains good cycling stability, ultracapacitor that specific capacity is high.The invention have the advantage that a step laser reduction graphene oxide, decomposition manganese compound obtain Graphene and the manganese oxide flexible compound electrode of reduction-state, and assembling them into flexible super capacitor, preparation technology is simple, and efficiency is high, preparation process environmental protection, can be with industrialized production.
Description
Technical field
The invention belongs to electrochemical field, relate generally to a kind of Graphene/manganese oxide flexible electrode and high performance flexibility
Its preparation method of ultracapacitor.
Background technology
Owing to petroleum resources are the shortest, and the pollution of environment is more come by the internal combustion engine tail gas discharge of combustion of fossil fuels
The most serious, people substitute the novel energy device of internal combustion engine in research.Have been carried out hybrid power, fuel cell, chemistry
Battery product and the research and development of application, achieve certain effect.But the service life intrinsic due to them is short, temperature
The deadly defects such as characteristic is poor, chemical cell pollutes environment, system complex, cost are high, the most good solution.And
There is the ultracapacitor of the advantages such as high-energy-density, high power density, long circulation life, can partly or entirely substitute tradition
Chemical cell for the traction power source of vehicle and start the energy, and have and use more widely than traditional chemical cell
On the way.Equally, ultracapacitor can also be used for the energy-storage system of some Renewable resources such as wind energy, electric energy.
At present, the electrode material that can be used as ultracapacitor has carbon materials, metal-oxide, conducting polymer etc..?
In carbon materials, Graphene, with the specific surface area of its superelevation, excellent electric conductivity, starts one research boom in scientific circles.
Although Graphene is as the electrode material many merits such as have cheap, good conductivity, stable chemical performance, discharge and recharge fast,
But it is less than electric capacity, energy density is the highest.And Graphene is in macroscopic view accumulation process, congestion superposition between lamella,
The area of the effective electric double layer that can form it into reduces.If introducing semi-conductor nano particles at graphene film interlayer, will significantly
Reducing the interaction between graphene sheet layer, Graphene can be as the backing material of semi-conductor nano particles simultaneously, it is possible to rise
Effect to electron transmission passage, it is also possible to be effectively improved the electric property of semi-conducting material.
Metal-oxide has the advantage higher than electric capacity as electrode material for super capacitor, about the 10 ~ 100 of material with carbon element
Times, but cyclical stability is poor, energy attenuation is too fast, and relatively low electrical conductivity also limit its application.
At present, oneself has and prepares Graphene/manganese oxide composite material and do report and the Patents of electrochemical capacitor, but system
Preparation Method is that to use graphite oxide be presoma mostly, adds and prepares forerunner's complex containing manganese compound, enters forerunner's complex
Row prepared laminated film the most originally.Composite prepared by these methods has high electric conductivity and bigger specific capacity,
But complex process, wastes time and energy, and wastes raw material, waste material pollutes environment simultaneously.
Summary of the invention
This object of the present invention is to provide that a kind of technique simple, easily operated controls, cost of material is low, to environment
The friendly preparation method manufacturing Graphene/manganese oxide flexible electrode.
Present invention provides the manufacture method of a kind of Graphene/manganese oxide flexible super capacitor, this Graphene/oxidation
Manganese flexible super capacitor good cycling stability, energy density are high.
Technical scheme disclosed by the invention includes:
First aspect present invention utilizes laser one-step method to prepare the preparation side of ultracapacitor Graphene/manganese oxide flexible electrode
Method, comprises the following steps:
A the compound water of graphene oxide Yu manganese is configured to mixed liquor by (), coating is on a flexible substrate；
B () irradiates the film of the oxide of coating graphene oxide/manganese on a flexible substrate under inert atmosphere protection with laser,
To prepare Graphene/manganese oxide composite electrodes.
According to the preparation method of above-mentioned Graphene/manganese oxide flexible electrode, the present invention step can prepare Graphene/oxygen
Change manganese flexible electrode, overcome the preparation method that conventional graphite alkene/manganese oxide composite electrodes is loaded down with trivial details, substantially increase production effect
Rate.
In the described embodiment of the present invention: the compound of described graphene oxide with manganese is used water as dispersant and is configured to
Mixed liquor.
The compound of the manganese described in the described embodiment of the present invention can be MnSO4、MnCl2、MnCO3、Mn(OH)2、Mn3
(PO3)2、Mn3(BO3)2、Mn(CH3COO)2Deng the compound of the manganese in water soluble or acid, but cannot be Mn (NO3)2、
KMnO4、Mn(ClO)4Compound etc. strong oxidizing property manganese.
The mass ratio of the compound of graphene oxide described in the mixed liquor of some described embodiments of the present invention and manganese
For graphene oxide: the compound=1:0.05 ~ 1:40 of manganese.
In preparation method described in some described embodiments of the present invention, the compound of described manganese can be MnSO4、
MnCl2、MnCO3、Mn(OH)2、Mn3(PO3)2、Mn3(BO3)2、Mn(CH3COO)2In any one or a combination thereof.
In the preparation method of the Graphene/manganese oxide flexible electrode described in some described embodiments of the present invention, institute
Flexible substrates can be polyethylene terephthalate (PET), polyimides (PI), polyamide (PAN), Merlon
(PC) and the macromolecule of the insulation such as ultra-thin glass or inorganic material, it is also possible to be the flexible aluminium foil of conduction, titanium foil, native gold, silver
Any one in the metal materials such as paper tinsel, Copper Foil, nickel foil, stainless steel substrates or graphite paper.
In the preparation method of the Graphene/manganese oxide flexible electrode described in some described embodiments of the present invention, institute
Stating the noble gas described in step (b) is that nitrogen, argon, carbon dioxide etc. do not have the one in the gas of oxidation, reproducibility
Or several mixed gas.
In the preparation method of the Graphene/manganese oxide flexible electrode described in some described embodiments of the present invention, profit
With inert atmosphere protection, with the film of the oxide of the graphene oxide/manganese in laser irradiation flexible substrates.Described noble gas
Flow be 0.1 ~ 10 liter/per minute.
In the preparation method of the Graphene/manganese oxide flexible electrode in some described embodiments of the present invention, described step
Suddenly the laser power described in (b) is 100mW ~ 10W, and sweep speed is 1 ~ 100 cm per minute.
Used by second aspect present invention embodiment Graphene/manganese oxide composite material by according to a first aspect of the present invention
The Graphene of embodiment/manganese oxide flexible electrode preparation method prepare.
The preparation method of the Graphene of third aspect present invention embodiment/manganese oxide composite material flexible electrode includes following
Two kinds: in described insulation flexible substrate, on the Graphene/manganese oxide composite electrodes of preparation, connect colelctor electrode；Electric conductivity flexibility base
, the Graphene/manganese oxide composite electrodes of preparation need not connect further colelctor electrode at the end.
In some embodiments of the invention, the Graphene/manganese oxide compound electric of preparation in described insulation flexible substrate
Colelctor electrode is connected on extremely.
In some embodiments of the invention, at the suprabasil Graphene/manganese oxide composite material of described insulation flexible
Stickup conductive tape in side is using as described colelctor electrode, and described conductive tape includes copper adhesive tape, the Copper Foil of subsidiary binding agent or aluminum
Any one in paper tinsel, conductive fabric.
In some embodiments of the invention, in described electric conductivity flexible substrates, the Graphene/manganese oxide of preparation is combined
Electrode need not connect further colelctor electrode.
The Graphene of fourth aspect present invention embodiment/manganese oxide composite and flexible electrode, is according to a third aspect of the present invention
The preparation method of the Graphene of embodiment/manganese oxide composite and flexible prepares.
The preparation method of the Graphene of fifth aspect present invention embodiment/manganese oxide flexible super capacitor, including following
Step: the flexible electrical that the preparation method of the Graphene of embodiment according to a third aspect of the present invention/manganese oxide flexible electrode is obtained
Pole is packaged and irrigates electrolyte solution, is then packaged, to obtain described Graphene/manganese oxide flexible super electric capacity
Device.
In some embodiments of the invention, the preparation method of described Graphene/manganese oxide flexible super capacitor, its
Being characterised by, described Graphene/manganese oxide flexible electrode is packaged by package adhesive tape or optic-solidified adhesive, described encapsulating material
Including any one in Kapton adhesive tape, adhesive tape, tape, stationery adhesive tape, insulating tape or optic-solidified adhesive.
In some embodiments of the invention, the preparation method of described Graphene/manganese oxide flexible super capacitor, its
Being characterised by, described electrolyte solution includes Na2SO4/ fumed silica system, ionic liquid/fumed silica system.
In some embodiments of the invention, the preparation method of described Graphene/manganese oxide flexible super capacitor, its
Being characterised by, Graphene/manganese oxide flexible electrode is as positive pole, and graphite, activated carbon etc. are as negative pole, and composition asymmetrical type is super
Capacitor；Or grouped by itself is symmetry ultracapacitor.
The Graphene of sixth aspect present invention embodiment/manganese oxide flexible super capacitor, according to a fifth aspect of the present invention
The preparation method of the described Graphene/manganese oxide flexible super capacitor of embodiment prepares.
The additional aspect of the present invention and advantage will part be given in the following description, and part will become from the following description
Obtain substantially, or recognized by the practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or the additional aspect of the present invention and advantage are from combining the accompanying drawings below description to embodiment and will become
Substantially with easy to understand, wherein:
Fig. 1 is the technique Making programme figure of the Graphene/manganese oxide flexible electrode of the embodiment of the present invention.
Fig. 2 is the schematic appearance of the Graphene/manganese oxide electrode of according to embodiments of the present invention 1；
Fig. 3 is the perspective view of the Graphene/manganese oxide ultracapacitor of according to embodiments of the present invention 3；
Fig. 4 is the charging and discharging curve of the Graphene/manganese oxide ultracapacitor of according to embodiments of the present invention 3.
Detailed description of the invention
Embodiment 1
Use the Hummer method improved to prepare graphene oxide (GO), take GO 0.1g, MnSO40.2g, adds distilled water
In, mixing stirring, obtain mixed liquor；
The mixed liquor obtained is evenly coated on PET film, dries, obtain electrode precursor；
At the N that flow is 1 liter/min2Under atmosphere, employing power is 300mW, and sweep speed is that the laser of 8 cels shines
Penetrate reduction, the irradiation route of laser can be arranged as required to, while GO is reduced by laser irradiation, MnSO4It is broken down into oxidation
Manganese, obtains Graphene/manganese oxide flexible electrode；
Embodiment 2
Use the Hummer method improved to prepare GO, take GO 0.1g, MnCO30.3g, adds in distilled water, mixing stirring,
Obtain mixed liquor；
The mixed liquor obtained is evenly coated on polyimides (PI) film, dries, obtain electrode precursor；
At the N that flow is 0.5 liter/min2Under atmosphere, employing power is 200mW, and sweep speed is that the laser of 6 cels is carried out
Irradiate reduction, the irradiation route of laser can be arranged as required to, while GO is reduced by laser irradiation, MnCO3It is broken down into oxygen
Change manganese, obtain Graphene/manganese oxide flexible electrode；
Embodiment 3
Both positive and negative polarity all uses the Graphene/manganese oxide flexible electrode obtained in embodiment 1, uses Na2SO4The conduct of/fumed silica
Electrolyte, encapsulation, obtain symmetric form ultracapacitor.As shown in Fig. 3, Graphene/manganese oxide ultracapacitor includes: graphite
Alkene/manganese oxide C1 and C2 (i.e. the Graphene of embodiment 1 gained/manganese oxide electrode)；Packaging part K and electrolyte solution
(not shown).
Wherein, Graphene/manganese oxide electrode C1 and C2 is Graphene/manganese oxide electrode that embodiment 1 obtains, and centre is filled out
Having Na2SO4/ fumed silica electrolyte (not shown), electrode is isolated by electrolyte the most naturally, thus it is super to eliminate tradition
The diaphragm element of level capacitor.
K encapsulating material shown in Fig. 3 (optic-solidified adhesive), plays solidification, envelope to described Graphene/manganese oxide electrode C1 and C2
Pretend use, thus form symmetric form ultracapacitor.
Fig. 4 shows the discharge and recharge of the 3 single Graphene/manganese oxide ultracapacitors prepared according to embodiments of the present invention
Curve.
Wherein, for the Graphene/manganese oxide symmetric form ultracapacitor be given by such as Fig. 3, charging/discharging voltage window 0
～0.8V, charging and discharging currents is 1mA, is calculated the appearance of this Graphene/manganese oxide ultracapacitor by formula according to discharge curve
Amount is 90.5mF.
On the other hand, being computed, single electrode effective area is 1cm2.Thus, it is converted into area ratio
Electric capacity understands, and is 362mF/cm according to the ratio electric capacity of the prepared Graphene/manganese oxide ultracapacitor of embodiment 32
Embodiment 4
Both positive and negative polarity all uses the Graphene/manganese oxide flexible electrode obtained in embodiment 2, uses ionic liquid/fumed silica conduct
Electrolyte, encapsulation, obtain symmetric form ultracapacitor.
Table 1 is the cyclical stability test result of the ultracapacitor of embodiment 3 and example 4 preparation.
| Embodiment 3 | Embodiment 4 | |
| 1000 times | 83% | 87% |
Table 1 is the capacitor charge and discharge test result of the ultracapacitor of embodiment 3 and example 4 preparation.
| Embodiment 3 | Embodiment 4 | |
| Specific capacity (area) | 362mF/cm<sup>2</sup> | 335mF/cm<sup>2</sup> |
By above-mentioned, according to the Graphene/manganese oxide ultracapacitor of the present invention, there is simple in construction, electrical property
The advantages such as energy is good, preparation technology is simple, with low cost, can be widely used for the every field of electric energy storage.
Above-mentioned specific embodiment, simply the preferential description implemented to the present invention, can not constitute present invention protection
The restriction of scope.Various changes that technical scheme is made by those skilled in the art, revise, replace and modification, all
Should fall in the protection domain that claims of invention determine.
Claims (16)
1. utilizing laser one-step method to prepare the preparation method of ultracapacitor Graphene/manganese oxide flexible electrode, its feature exists
In, comprise the following steps:
A the compound water of graphene oxide Yu manganese is configured to mixed liquor by (), be then coated with on a flexible substrate；
B () irradiates the film of the oxide of coating graphene oxide/manganese on a flexible substrate under inert atmosphere protection with laser,
To prepare Graphene/manganese oxide composite and flexible electrode.
2. the preparation method of the Graphene as described in claim 1/manganese oxide flexible electrode, it is characterised in that described step
A () including: the compound water of described graphene oxide Yu manganese is configured to mixed liquor；The compound of described manganese can be
MnSO4、MnCl2、MnCO3、Mn(OH)2、Mn3(PO3)2、Mn3(BO3)2、Mn(CH3COO)2Change in the manganese in water soluble or acid
Compound, but cannot be Mn (NO3)2、KMnO4、Mn(ClO)4Compound etc. strong oxidizing property manganese.
3. the preparation method of the Graphene as described in claim 2/manganese oxide flexible electrode, it is characterised in that in described mixing
Graphene oxide described in liquid is graphene oxide with the mass ratio of the compound of manganese: the compound=1:0.05 ~ 1:40 of manganese.
4. the preparation method of the Graphene as described in claim 3/manganese oxide flexible electrode, it is characterised in that the change of described manganese
Compound includes MnSO4、MnCl2、MnCO3、Mn(OH)2、Mn3(PO3)2、Mn3(BO3)2、Mn(CH3COO)2In any one or its group
Close.
5. the preparation method of the Graphene as according to any one of claim 2 ~ 4/manganese oxide flexible electrode, it is characterised in that
Described step (a) including: being coated with on a flexible substrate by described mixed liquor, described flexible substrates is polyethylene terephthalate
The macromolecule or inorganic of the insulation such as ester (PET), polyimides (PI), polyamide (PAN), Merlon (PC) and ultra-thin glass
Material, it is also possible to be metal material or the graphite such as the flexible aluminium foil of conduction, titanium foil, native gold, native silver, Copper Foil, nickel foil, stainless steel substrates
Any one in paper.
6. the preparation method of the Graphene as described in claim 1/manganese oxide flexible electrode, it is characterised in that described step
B () including: under inert atmosphere protection, the film of the oxide of the graphene oxide/manganese being coated with on a flexible substrate is carried out laser
Irradiating, the flow of described noble gas is 0.1 ~ 10 liter/per minute.
7. the preparation method of the Graphene as described in claim 1/manganese oxide flexible electrode, it is characterised in that described step
B () including: under inert atmosphere protection, the film of the oxide of the graphene oxide/manganese being coated with on a flexible substrate is carried out laser
Irradiating, described noble gas is that nitrogen, argon, carbon dioxide etc. do not have the one in the gas of oxidation, reproducibility or several
The mixed gas planted.
8. the preparation method of the Graphene as described in claim 1/manganese oxide flexible electrode, it is characterised in that described step
B the laser power described in () is 100mW ~ 10W, sweep speed is 1 ~ 100 cm per minute.
9. Graphene/manganese oxide flexible electrode, it is characterised in that according to the graphite described in any one of claim 1 ~ 8
The preparation method of alkene/manganese oxide flexible electrode prepares.
10. the preparation method of Graphene/manganese oxide flexible electrode as claimed in claim 9, it is characterised in that in described insulation
Colelctor electrode is connected on the Graphene/manganese oxide composite electrodes of preparation in flexible substrates；The graphite of preparation in electric conductivity flexible substrates
Alkene/manganese oxide composite electrodes need not connect further colelctor electrode.
The preparation method of 11. Graphene electrodes as claimed in claim 10, it is characterised in that in described insulation flexible substrate
The side of graphene composite material paste conductive tape using as described colelctor electrode, described conductive tape includes copper adhesive tape, attached
Any one in Copper Foil with binding agent or aluminium foil, conductive fabric.
The preparation method of 12. 1 kinds of Graphene/manganese oxide flexible super capacitors, it is characterised in that comprise the following steps: by root
The flexible electrode obtained according to the preparation method of Graphene described in claim 8 ~ 11/manganese oxide flexible electrode is packaged and irrigates
Electrolyte solution, is then packaged, to obtain described Graphene/manganese oxide flexible super capacitor.
The preparation method of 13. Graphene/manganese oxide flexible super capacitors as claimed in claim 12, it is characterised in that institute
Stating Graphene/manganese oxide flexible electrode to be packaged by package adhesive tape or optic-solidified adhesive, described encapsulating material includes Kapton
Any one in adhesive tape, adhesive tape, tape, stationery adhesive tape, insulating tape or optic-solidified adhesive.
The preparation method of the 14. Graphene/manganese oxide flexible super capacitors as described in claim 12, it is characterised in that institute
State electrolyte solution and include Na2SO4/ fumed silica system, ionic liquid/fumed silica system.
The preparation method of 15. Graphene/manganese oxide flexible super capacitors as claimed in claim 12, it is characterised in that stone
Ink alkene/manganese oxide flexible electrode is as positive pole, and graphite, activated carbon etc., as negative pole, form asymmetrical type ultracapacitor；Or
Grouped by itself is symmetry ultracapacitor.
16. 1 kinds of Graphene/manganese oxide flexible super capacitors, it is characterised in that described in any one of claim 11 ~ 15
Graphene/manganese oxide flexible super capacitor preparation method prepare.
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