CN105826083A - Preparation method of graphene-based electrode material and construction method of capacitor - Google Patents
Preparation method of graphene-based electrode material and construction method of capacitor Download PDFInfo
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- CN105826083A CN105826083A CN201610248510.XA CN201610248510A CN105826083A CN 105826083 A CN105826083 A CN 105826083A CN 201610248510 A CN201610248510 A CN 201610248510A CN 105826083 A CN105826083 A CN 105826083A
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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
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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
- H01G11/84—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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a preparation method of a graphene-based electrode material and a construction method of a capacitor. Graphene oxide is added into deionized water according to the mass ratio of the graphene oxide to the deionized water which ranges from 0.5:1000 to 2:1000, an obtained mixture is subjected to magnetic stirring or manual shaking for 0.5 hour to 1 hour, and a product A can be obtained; the product A stands still for 0.5 hour to 1 hour under 60 DEG C to 80 DEG C until a complete graphene oxide film is formed on the surface of a graphene oxide hydrosol, and a product B can be obtained; with the flexible film adopted as a base body, the product B is deposited on the base body, and is dried in the air, so that a product C can be obtained; a hydrogen iodide solution of which the mass fraction ranges from 55% to 58% is added into the product C, and the product C is subjected to reduction for 3 hours to 48 hours under 15 DEG C to 80 DEG, and an obtain substance is cleaned, and a product D can be obtained; and the product D is immersed in potassium permanganate of which the concentration ranges from 0.5 mmol/L to 5 mmol/L for 5 hours to 48 hours, and an obtained substance is cleaned, and a product E is obtained, namely a graphene/manganese oxide composite film deposited on the flexible base body can be obtained. The graphene-based electrode material can be directly used as an electrode material of a flexible film super capacitor. The preparation method has the advantages of simple operation, low time consumption, low material consumption and environmental friendliness. With the preparation method adopted, the graphene-based electrode material has excellent bending performance. The electrochemical performance of a capacitor formed by the electrode material is excellent.
Description
Technical field
The present invention relates to preparation and the structure of capacitor of a kind of graphene-based flexible super capacitor electrode material
Method, a kind of graphene-based thin film electrode of super capacitor of plane based on gas-liquid interface construction from part
The preparation of material and the construction method of capacitor.
Background technology
Due to the development of wearable electronic device, the requirement of flexible energy storage device is also gradually increased by people, soft
The most therefore property ultracapacitor receives much concern.Wherein, flexible super electric capacity based on two-dimensional film electrode is with it
Lightweight, miniaturization, the feature such as flexible, particularly attractive attention.Graphene is as a kind of two wieners
Rice material with carbon element, its carbon atom is with sp2Hybrid form forms the cellular planar structure of hexatomic ring, and it has superelevation
Electron mobility (200,000cm2/ V.s), great specific surface area (2630m2/ g), good heat conduction
The mechanical strength (40N/m fracture strength, 1TPa Young's modulus) of performance (5300W/mK) and excellence,
It it is a kind of preferably electrode material for super capacitor.It is huge that Graphene two-dimensional nano lamellar structure imparts it
The ratio of width to height (aspect ratio) so that it is Flexible graphene thin film can be assembled into by stacked in multi-layers,
Reasonably introducing another kind of nano material during thin film assembles if being formed, can then obtain the graphene-based multiple of flexibility
Close thin film.
At present, existing many documents report assembling and the preparation process of graphene-based flexible thin film, and this is to structure
Build flexible super capacitor based on graphene membrane electrode and establish good working foundation.Wherein, vacuum
Suction method and chemical vapour deposition technique are the common technologies preparing graphene film, but obtained by these methods
Graphene film is the most all deposited on hard substrate (such as: Woelm Alumina filter membrane, Copper Foil, silicon chip)
On, therefore directly as the electrode material of flexible film super capacitor, and can not must pass through loaded down with trivial details base
The graphene film being deposited on hard substrate is transferred to flexible substrate (such as: poly-diformazan by body transfer step
Radical siloxane (Polydimethylsiloxane, PDMS) or polyethylene terephthalate
On (Poly (ethylene terephthalate), PET), matrix transfer process typically requires hard base
Body etches away, and the flexible substrate used is typically polymeric matrix, is eventually deposited on polymeric matrix
Graphene film just can be directly as the electrode material of flexible super capacitor；It addition, chemical vapour deposition technique
It is commonly used for preparing pure graphene film, it is difficult to be used for preparing graphene-based laminated film.Thin based on Graphene
Its configuration of the flexible super capacitor of membrane electrode mainly includes tradition " sandwich " configuration and plane configuration, its
Midplane configuration is more beneficial for the miniaturization of ultracapacitor volume and minimizing of thickness of detector.Utilize
It is thin that LBL self-assembly and chemical vapour deposition technique deposited multi-layer graphene at quartz substrate and copper foil surface respectively
Film and single-layer graphene film, and the plane super capacitor based on two kinds of graphene membrane electrode design constructions
Device, the good chemical property that two kinds of plane ultracapacitors show, its area ratio capacity is respectively
394μF/cm2With 80 μ F/cm2。(J.J.Yoo,K.Balakrishnan,J.Huang,et al.Nano
Letters 2011,11, (4), 1423-1427.) but, it is usual that LBL self-assembly prepares graphene film
Need to utilize positively charged nano material and electronegative graphene oxide solution as presoma, utilize
Electrostatic adelphotaxy between the two, carry out matrix in two kinds of nanomaterial solution repeatedly immersing-
The cyclic process cleaned-be dried, until it reaches required film thickness, therefore LBL self-assembly process is suitable
Time-consumingly complexity, and the graphene film obtained is often laminated film；Although chemical vapor deposition processes
There is in terms of preparing pure graphene film significant advantage, but its preparation process relates to high temperature high heat so
Power consumption process, and be difficult to a step and realize the controlled preparation of graphene-based laminated film.System discussed above
Two kinds of common methods of standby graphene-based thin film, its most critical issue is that the Graphene obtained by two kinds of methods is thin
Film is all deposited directly upon on hard substrate, it is impossible to directly apply to flexible super capacitor, only by multiple
Miscellaneous matrix transfer step, could deposit on flexible substrate, so by obtained graphene-based thin film transfer
And, thin film is transferred to from hard substrate this transfer step on flexible substrate to be needed to use severe corrosive examination
Hard substrate is dissolved by agent, and whole process is very time-consuming, consumptive material, not environmentally.
Summary of the invention
It is an object of the invention to, it is provided that the preparation of a kind of graphene-based electrode material and the structure side of capacitor
Method.Prepared graphene-based electrode material can directly as the electrode material of flexible film super capacitor,
Easy and simple to handle, the shortest, consumptive material is few, environmental protection, the most also has good bending property, pliability is good.
And with electrode material of the present invention build plane ultracapacitor chemical property good, area ratio capacity exists
1000μF/cm2Above, it is possible not only to build plane flexible super capacitor, it is also possible to build traditional three
Mingzhi's type flexible super capacitor, is simultaneously also beneficial to the miniaturization of device and lightening.
The present invention realizes by the following technical solutions: the preparation method of a kind of graphene-based electrode material, including
Following steps:
1, it is that 0.5-2:1000 adds oxidation in deionized water by the mass ratio of graphite oxide Yu deionized water
Graphite, stirring, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtain A product；
2, A product are at a temperature of 60-80 DEG C, stand 0.5-1h, until graphene oxide hydrosol surface is formed
Complete graphene oxide film, obtains B product；
3, employing fexible film is as matrix, i.e. B product are deposited on this flexible substrate, dry in the air by flexible substrate
Dry, obtain C product；
4, in C product, the hydrogen iodide solution that mass fraction is 55-58% is added, reduction 3-48h at 15-80 DEG C,
Clean through ethanol and distilled water, obtain D product；
5, D product are put into immersion 5-48h in the potassium permanganate of 0.5-5mmol/L, clear through ethanol and distilled water
Wash, obtain E product, the Graphene must being deposited on flexible substrate/Mn oxide laminated film.
The preparation method of aforesaid graphene-based electrode material, the graphite oxide described in step 1 presses following step
Suddenly it is prepared:
A. after potassium peroxydisulfate and phosphorus pentoxide being mixed for 1:1 in mass ratio, at 75-85 DEG C, by over cure
Acid potassium: dense H2SO4Ratio for 15g:80-150ml adds dense H2SO4, stir 20-30min, until molten
Liquid is limpid, obtains mixed solution；In mixed solution, add graphite powder, stir under 75-85 DEG C of water bath condition
4-5h, is cooled to room temperature, continues to add deionized water in mixed solution, and vacuum filtration method is by mixed solution
In solid sample clean and collect, during vacuum filtration use deionized water clean sample, until filter
Liquid is neutral, and the solid sample after being cleaned by sucking filtration is dried, and obtains the powdered graphite of pre-oxidation；
B. the powdered graphite pre-oxidized adds dense H2SO4In, stir under the conditions of the ice-water bath of 0-5 DEG C,
Potassium permanganate powder it is slowly added in solution, after then stirring 3-5h under the water-bath of 30-40 DEG C, then
0-5 DEG C of ice-water bath continues stirring 10-20min, is slow added into deionized water, continue stirring 2-3h, then
Adding mass fraction is the hydrogenperoxide steam generator of 30%, stirring while adding, stands 12h, collect solid after adding
Sample, cleans with the dilute hydrochloric acid solution that mass fraction is 4-5%, is centrifuged repeatedly cleaning, until cleanout fluid
Till pH value becomes neutrality, then it is vacuum dried 45-50h, obtains graphite oxide powder.
The preparation method of aforesaid graphene-based electrode material, presses graphite oxide and deionized water in step 1
Mass ratio is that 1:1000 adds graphite oxide in deionized water.
The preparation method of aforesaid graphene-based electrode material, in step 2, time of repose is 0.8h.
The preparation method of aforesaid graphene-based electrode material, in step 4, the recovery time is 28h.
The preparation method of aforesaid graphene-based electrode material, step 5 is that D product are put into the height of 3mmol/L
Potassium manganate soaks 28h, obtains E product, the Graphene must being deposited on flexible substrate/Mn oxide THIN COMPOSITE
Film.
The preparation method of aforesaid graphene-based electrode material, described fexible film is poly terephthalic acid second
Diol ester, i.e. PET matrix or polydimethylsiloxane, i.e. PDMS matrix.
The preparation method of aforesaid graphene-based electrode material, described dense H2SO4Mass fraction be 98%.
The method have the advantages that
1, prepared graphene-based electrode material can be directly as the electrode material of flexible film super capacitor
Material, it is not necessary to loaded down with trivial details matrix transfer step, is not related to the power consumption processes such as High Temperature High Pressure, it is not required that complicated
LBL self-assembly process, the shortest, consumptive material is few, environmental protection.
2, electrode material of the present invention builds and obtains capacitor.The capacitor obtained has general flexible super electric capacity
The performance of device, chemical property is good, and area ratio capacity is at 1000 μ F/cm2Above, at wearable electronic device
Field can use as flexible energy storage component.
3, prepared graphene-based electrode material has good bending property, finds through test, this graphite
Thiazolinyl electrode material remains in that fabulous integrity at the rear film of 1000 bendings of experience.It is possible not only to structure
Build plane flexible super capacitor, it is also possible to build traditional sandwich type flexible super capacitor.
4, when air liquid interface is assembled out by the present invention with flexiplast as matrix, it is not necessary to will without
The graphene-based thin-film package of support is inside flexiplast matrix.
5, the miniaturization of device and lightening is conducive to.Graphene aqueous dispersions sucking filtration is typically directly used to obtain
Graphene film, thin film is thicker.The present invention graphene oxide film obtained with air liquid interface construction from part,
The thickness of the graphene-based thin film obtained by again after reduction only has tens to hundreds of nanometer.
6, the inventive method is prepared the graphite oxide of gained and is had higher degree of oxidation, has excellent water-soluble
Property, it is not necessary to ultrasonic wave added can make graphite oxide dispersion form homogeneous phase aqueous solution in aqueous, is conducive to
Obtain the graphene oxide lamella of big lamella, contribute to reduce the later stage prepare graphene-based flexible membrane electrode
Internal resistance.
Further illustrate the present invention by the following examples, but not as limitation of the present invention
Detailed description of the invention
Embodiment 1.
The preparation method of a kind of graphene-based electrode material, comprises the following steps:
1, it is that 1:1000 adds graphite oxide in deionized water by the mass ratio of graphite oxide Yu deionized water,
In magnetic agitation or manually rock 0.8h, until solution is to stablize homogeneous graphene oxide hydrosol solution,
Obtain A product；
2, A product are at a temperature of 60-80 DEG C, stand 0.8h, until graphene oxide hydrosol surface has been formed
Whole graphene oxide film, obtains B product；
3, use fexible film as matrix, B product are deposited on this matrix, dry, obtain C product；Described
Fexible film is polyethylene terephthalate, i.e. PET matrix；
4, the hydrogen iodide solution that mass fraction is 57%, reductase 12 8h, warp at 15-80 DEG C are added to C kind
Ethanol and distilled water clean, and obtain D product；
5, D product are put into immersion 28h in the potassium permanganate of 3mmol/L, cleans through ethanol and distilled water,
E product, the Graphene must being deposited on flexible substrate/Mn oxide laminated film.
Graphite oxide described in step 1 is prepared in the steps below:
A. by 15g potassium peroxydisulfate and 15g phosphorus pentoxide P2O5Join in the round bottom beaker of 550mL,
The dense H of 115mL is added under 75-85 DEG C of bath temperature2SO4, make mixed solution mix under magnetic stirring
25min, mixed solution becomes limpid；22g powdered graphite is joined in solution mixed above so that it is
It is stirred 4.5h under 75-85 DEG C of water bath condition, afterwards mixed solution temperature is slowly lowered to room temperature, the most slowly
Slowly add 1.7L deionized water, finally use vacuum filtration method to be cleaned also by the solid sample in mixed solution
Collect, use deionized water to clean sample during vacuum filtration, until filtrate is neutral, sucking filtration is clear
Solid sample after washing is dried, and obtains the powdered graphite of pre-oxidation；
B. in the powdered graphite of pre-oxidation, add 750mL concentrated sulphuric acid, quilt under the conditions of the ice-water bath of 0-5 DEG C
Stir, then 100g potassium permanganate powder is slowly added in flask, treat that potassium permanganate powder adds it
After, obtain reactant liquor；Reactant liquor is transferred in the water bath of 35-40 DEG C, after continuing to be stirred 4h, and reaction
Liquid transfers to continue in 0-5 DEG C of ice-water bath to stir, more slowly adds the deionized water of 750mL in reactant liquor,
And continue to stir 2.5h under the conditions of ice-water bath；It is the hydrogenperoxide steam generator of 30% by 40mL mass fraction
Join in reactant liquor, stirring while adding, add rear reactant liquor and stand 12h, collect and deposit to drag
Solid sample, then use vacuum filtration method be 4.5% by the solid sample 3L mass fraction of collection
Dilute hydrochloric acid solution filters and cleans to react away the manganese dioxide impurity in solid sample, is finally centrifuged repeatedly cleaning
Sample is until the pH value of cleanout fluid becomes neutrality, and product carries out being vacuum dried 48h the most at last, is dried temperature
Spend 20-30 DEG C and obtain graphite oxide powder；Described dense H2SO4Mass fraction be 98%.
Embodiment 2.
The preparation method of a kind of graphene-based electrode material, comprises the following steps:
1, it is that 2:1000 adds graphite oxide in deionized water by the mass ratio of graphite oxide Yu deionized water,
In magnetic agitation or manually rock 1h, until solution is to stablize homogeneous graphene oxide hydrosol solution,
A product；
2, A product are at a temperature of 60-80 DEG C, stand 1h, until graphene oxide hydrosol surface is formed completely
Graphene oxide film, obtain B product；
3, use fexible film as matrix, B product are deposited on this matrix, dry, obtain C product；Described
Fexible film is polydimethylsiloxane, i.e. PDMS matrix；
4, add, to C kind, the hydrogen iodide solution that mass fraction is 58%, reduction 48h, warp at 15-80 DEG C
Ethanol and distilled water clean, and obtain D product；
5, D product are put into immersion 48h in the potassium permanganate of 5mmol/L, cleans through ethanol and distilled water,
E product, the Graphene must being deposited on flexible substrate/Mn oxide laminated film.
The preparation method of the graphite oxide described in step 1 is with embodiment 1.
Embodiment 3.
The preparation method of a kind of graphene-based electrode material, comprises the following steps:
1, by the mass ratio of graphite oxide Yu deionized water be 0.5:1000 add in deionized water oxidation stone
Ink, in magnetic agitation or manually rock 0.5h, until solution is to stablize the water-soluble peptization of homogeneous graphene oxide
Liquid, obtains A product；
2, A product are at a temperature of 60-80 DEG C, stand 0.5h, until graphene oxide hydrosol surface has been formed
Whole graphene oxide film, obtains B product；
3, use fexible film as matrix, B product are deposited on this matrix, dry, obtain C product；Described
Fexible film is polyethylene terephthalate, i.e. PET matrix；
4, add, to C kind, the hydrogen iodide solution that mass fraction is 55%, reduction 3h, warp at 15-80 DEG C
Ethanol and distilled water clean, and obtain D product；
5, D product are put into immersion 5h in the potassium permanganate of 0.5mmol/L, cleans through ethanol and distilled water,
E product, the Graphene must being deposited on flexible substrate/Mn oxide laminated film.
The preparation method of the graphite oxide described in step 1 is with embodiment 1.
Embodiment 4.
The preparation method of a kind of graphene-based electrode material, comprises the following steps:
1, by the mass ratio of graphite oxide Yu deionized water be 1.7:1000 add in deionized water oxidation stone
Ink, in magnetic agitation or manually rock 0.9h, until solution is to stablize the water-soluble peptization of homogeneous graphene oxide
Liquid, obtains A product；
2, A product are at a temperature of 60-80 DEG C, stand 0.9h, until graphene oxide hydrosol surface has been formed
Whole graphene oxide film, obtains B product；
3, use fexible film as matrix, B product are deposited on this matrix, dry, obtain C product；Described
Fexible film is polydimethylsiloxane, i.e. PDMS matrix.
4, add, to C kind, the hydrogen iodide solution that mass fraction is 57%, reduction 3-48h at 15-80 DEG C,
Clean through ethanol and distilled water, obtain D product；
5, D product are put into immersion 40h in the potassium permanganate of 4mmol/L, cleans through ethanol and distilled water,
E product, the Graphene must being deposited on flexible substrate/Mn oxide laminated film.
The preparation method of the graphite oxide described in step 1 is with embodiment 1.
Embodiment 5.
The preparation method of a kind of graphene-based electrode material, comprises the following steps:
1, by the mass ratio of graphite oxide Yu deionized water be 0.9:1000 add in deionized water oxidation stone
Ink, in magnetic agitation or manually rock 0.6h, until solution is to stablize the water-soluble peptization of homogeneous graphene oxide
Liquid, obtains A product；
2, A product are at a temperature of 60-80 DEG C, stand 0.6h, until graphene oxide hydrosol surface has been formed
Whole graphene oxide film, obtains B product；
3, use fexible film as matrix, B product are deposited on this matrix, dry, obtain C product；Described
Fexible film is polyethylene terephthalate, i.e. PET matrix.
4, add, to C kind, the hydrogen iodide solution that mass fraction is 56%, reduction 10h, warp at 15-80 DEG C
Ethanol and distilled water clean, and obtain D product；
5, D product are put into immersion 10h in the potassium permanganate of 1mmol/L, cleans through ethanol and distilled water,
E product, the Graphene must being deposited on flexible substrate/Mn oxide laminated film.
The preparation method of the graphite oxide described in step 1 is with embodiment 1.
Claims (8)
1. the preparation method of a graphene-based electrode material, it is characterised in that: comprise the following steps:
(1) it is that 0.5-2:1000 adds oxygen in deionized water by the mass ratio of graphite oxide Yu deionized water
Graphite, stirring, until solution is to stablize homogeneous graphene oxide hydrosol solution, obtain A product；
(2) A product are at a temperature of 60-80 DEG C, stand 0.5-1h, until graphene oxide hydrosol surface shape
Become complete graphene oxide film, obtain B product；
(3) employing fexible film is as matrix, i.e. B product are deposited on this flexible substrate by flexible substrate,
Dry, obtain C product；
(4) in C product, add the hydrogen iodide solution that mass fraction is 55-58%, reduce at 15-80 DEG C
3-48h, after ethanol and distilled water clean, obtains D product；
(5) D product are put into immersion 5-48h in the potassium permanganate of 0.5-5mmol/L, through ethanol and distilled water
After cleaning, obtain E product, the Graphene must being deposited on flexible substrate/Mn oxide laminated film.
The preparation method of graphene-based electrode material the most according to claim 1, it is characterised in that:
Graphite oxide described in step (1) is prepared in the steps below:
A. after potassium peroxydisulfate and phosphorus pentoxide being mixed for 1:1 in mass ratio, at 75-85 DEG C, by over cure
Acid potassium: dense H2SO4Ratio for 15g:80-150ml adds dense H2SO4, stir 20-30min, until molten
Liquid is limpid, obtains mixed solution；In mixed solution, add graphite powder, stir under 75-85 DEG C of water bath condition
4-5h, is cooled to room temperature, continues to add deionized water in mixed solution, and vacuum filtration method is by mixed solution
In solid sample clean and collect, during vacuum filtration use deionized water clean sample, until filter
Liquid is neutral, and the solid sample after being cleaned by sucking filtration is dried, and obtains the powdered graphite of pre-oxidation；
B. the powdered graphite pre-oxidized adds dense H2SO4In, stir under the conditions of the ice-water bath of 0-5 DEG C,
Potassium permanganate powder it is slowly added in solution, after then stirring 3-5h under the water-bath of 30-40 DEG C, then
0-5 DEG C of ice-water bath continues stirring 10-20min, is slow added into deionized water, continue stirring 2-3h, then
Adding mass fraction is the hydrogenperoxide steam generator of 30%, stirring while adding, stands 12h, collect solid after adding
Sample, cleans with the dilute hydrochloric acid solution that mass fraction is 4-5%, is centrifuged repeatedly cleaning, until cleanout fluid
Till pH value becomes neutrality, then it is vacuum dried 45-50h, obtains graphite oxide powder.
The preparation method of graphene-based electrode material the most according to claim 1, it is characterised in that: step
Suddenly in (1) by the mass ratio of graphite oxide Yu deionized water be 1:1000 add in deionized water oxidation stone
Ink.
The preparation method of graphene-based electrode material the most according to claim 1, it is characterised in that: step
Suddenly in (2), time of repose is 0.8h.
The preparation method of graphene-based electrode material the most according to claim 1, it is characterised in that: step
Suddenly in (4), the recovery time is 28h.
The preparation method of graphene-based electrode material the most according to claim 1, it is characterised in that: step
Suddenly soak 28h during (5) are the potassium permanganate that D product are put into 3mmol/L, obtain E product, must be deposited on soft
Graphene/Mn oxide laminated film on property matrix.
The preparation method of graphene-based electrode material the most according to claim 1, it is characterised in that: institute
Stating fexible film is polyethylene terephthalate, i.e. PET matrix or polydimethylsiloxane, i.e. PDMS
Matrix.
The preparation method of graphene-based electrode material the most according to claim 2, it is characterised in that institute
State dense H2SO4Mass fraction be 98%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10014124B1 (en) | 2017-09-27 | 2018-07-03 | King Saud University | Composite electrode material for supercapacitors |
| CN109368634A (en) * | 2018-11-14 | 2019-02-22 | 贵州大学 | A kind of preparation method and applications of graphene-based material precursor |
| CN112010290A (en) * | 2020-08-26 | 2020-12-01 | 兰州大学 | Method for industrially preparing graphene film |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549864A (en) * | 2009-04-30 | 2009-10-07 | 上海大学 | Method for simply and innoxiously preparing single-layer graphene |
| CN101894679A (en) * | 2009-05-20 | 2010-11-24 | 中国科学院金属研究所 | Method for preparing graphene-based flexible super capacitor and electrode material thereof |
| CN102709061A (en) * | 2012-07-03 | 2012-10-03 | 电子科技大学 | Graphene-cladding manganese dioxide combination electrode material and method for producing same |
-
2016
- 2016-04-21 CN CN201610248510.XA patent/CN105826083B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101549864A (en) * | 2009-04-30 | 2009-10-07 | 上海大学 | Method for simply and innoxiously preparing single-layer graphene |
| CN101894679A (en) * | 2009-05-20 | 2010-11-24 | 中国科学院金属研究所 | Method for preparing graphene-based flexible super capacitor and electrode material thereof |
| CN102709061A (en) * | 2012-07-03 | 2012-10-03 | 电子科技大学 | Graphene-cladding manganese dioxide combination electrode material and method for producing same |
Non-Patent Citations (1)
| Title |
|---|
| XIAOCHEN DONG , XUEWAN WANG , JING WANG. ETC.: "Synthesis of a MnO¬2–graphene foam hybrid with controlled MnO2 particle shape and its use as a supercapacitor electrode", 《CARBON》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10014124B1 (en) | 2017-09-27 | 2018-07-03 | King Saud University | Composite electrode material for supercapacitors |
| CN109368634A (en) * | 2018-11-14 | 2019-02-22 | 贵州大学 | A kind of preparation method and applications of graphene-based material precursor |
| CN112010290A (en) * | 2020-08-26 | 2020-12-01 | 兰州大学 | Method for industrially preparing graphene film |
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