CN108010744A - The preparation method of graphene coated molecular sieve combination electrode material - Google Patents
The preparation method of graphene coated molecular sieve combination electrode material Download PDFInfo
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- CN108010744A CN108010744A CN201711295936.1A CN201711295936A CN108010744A CN 108010744 A CN108010744 A CN 108010744A CN 201711295936 A CN201711295936 A CN 201711295936A CN 108010744 A CN108010744 A CN 108010744A
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—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 present invention relates to technical field of inorganic material, and in particular to a kind of preparation method of graphene coated molecular sieve combination electrode material.The preparation method of graphene coated molecular sieve combination electrode material, includes the following steps：（1）Prepare GO；（2）Prepare 4A/RGO combination electrode materials；（3）Prepare 4A/RGO electrodes.The three-dimensional compound 4A/RG electrode materials preparation method of the present invention is easy, which is expected to be applied to extensive preparation, is a kind of electrode material for super capacitor for having potential using value.
Description
Technical field
The present invention relates to technical field of inorganic material, and in particular to a kind of graphene coated molecular sieve combination electrode material
Preparation method.
Background technology
Ultracapacitor has the advantages that energy density is high, has extended cycle life as a kind of novel green energy storage device,
It is used widely in the fields such as wind-power electricity generation, storage backup, the high-power equipment of military project and track traffic.Wherein, electrode material is
Influence the key factor of ultracapacitor chemical property.Studying three kinds of more electrode material for super capacitor at present is respectively
Carbon material, metal oxide and conducting polymer.Research shows, above-mentioned variety classes electrode material is compound, the collaboration of generation
Effect not only can overcome the disadvantages that homogenous material deficiency, but also can realize that material property has complementary advantages.Therefore, combination electrode material has become
The research hotspot in ultracapacitor field.For example, electrochemical deposition method prepares graininess Mn02/ graphene complex, concurrently
Its maximum specific capacitance is 378 F/g under present l mV/s sweep speeds.Such as using chemical graft process fabricated in situ graphene/poly-
Pyrroles's compound, its specific capacitance is up to 284 F/g.
Graphene is a kind of carbon material with honeycomb shape special construction, its theoretical specific surface area (2630 m2/ g) and
Electrical conductivity (7200 S/m) is far above other carbon materials.Therefore, graphene is the electrochemical energy storage materials of most attraction.But
It is that Van der Waals force can make graphene that irreversible reunion occur, so that its specific surface area and specific capacity are reduced, simple Graphene electrodes
The actual specific capacity of ultracapacitor be only capable of reaching 200 F/g or so.Although molecular sieve is with high specific surface area and uniformly
Porosity, but its poorly conductive, it is impossible to be directly used as electrode material.
The content of the invention
It is contemplated that in view of the above-mentioned problems, propose a kind of preparation side of graphene coated molecular sieve combination electrode material
Method.
Technical program of the present invention lies in：
The preparation method of graphene coated molecular sieve combination electrode material, includes the following steps：
（1）Prepare GO；
（2）Prepare 4A/RGO combination electrode materials；
（3）Prepare 4A/RGO electrodes.
The detailed process for preparing GO is：The concentrated sulfuric acid of 40 mL, 98wt% is pipetted, is placed in 250 mL beakers, adds
Entering 6 g potassium sulfates and 6 g P205, magnetic agitation is uniform, and into mixed liquor plus 10 g of crystalline flake graphite, 0 DEG C of ice-water bath stir, and 75
DEG C reaction 5 h, be cooled to room temperature, stand overnight, filtering supernatant, then 45 DEG C drying；The above-mentioned pre-oxidation graphite powders of 2 g are taken to add
Entering the 100 mL concentrated sulfuric acids, 0 DEG C of stirring of ice-water bath, adds 20 g potassium permanganate, continues to stir 20 min, then 40 DEG C of 4 h of reaction,
1000 mL distilled water are finally poured into, add dropwise 30 mL hydrogen peroxide, solution reaction is golden yellow to presenting；Finally, will
Solution centrifuges, and dialysis washing is precipitated to neutrality, product GO.
The detailed process for preparing 4A/RGO combination electrode materials is：Claim 4A to be placed in 250 mL beakers, add 50
GO gels scattered mL, after 10~15 min of ultrasonic dissolution, 30 min of strong stirring, obtains unit for uniform suspension；Suspension 80
DEG C evaporation moisture is stirred continuously, gained pastel is placed in 45 DEG C of drying, 320 DEG C of calcinations 2 under nitrogen protective condition in baking oven
H, obtained product cooled to room temperature, up to 4A/RGO combination electrode materials.
The detailed process for preparing 4A/RGO electrodes is：Nickel foam is collector, with acetone, ethanol and distilled water according to
Secondary ultrasonic cleaning nickel foam, vacuum drying are stand-by；Ethanol in proper amount ultrasound point will be added in 4A/RGO, acetylene black and Nafion solution
Dissipate, 60 DEG C of magnetic agitations are coated in cleaned nickel foam, tablet press machine keeps 2 min to press with 10 MPa pressure into plasticity slurry
Flakiness electrode, 45 DEG C of 12 h of vacuum drying, obtains 4A/RGO electrodes.
The mixing quality ratio of the 4A/RGO, acetylene black and Nafion solution are 8：1：1.
The technical effects of the invention are that：
The three-dimensional compound 4A/RG electrode materials preparation method of the present invention is easy, which is expected to be applied to extensive preparation, is one
Kind has the electrode material for super capacitor of potential using value.
Embodiment
The preparation method of graphene coated molecular sieve combination electrode material, includes the following steps：
（1）Prepare GO：
The concentrated sulfuric acid of 40 mL, 98wt% is pipetted, is placed in 250 mL beakers, 6 g potassium sulfates is added and 6 g P205, magnetic force stirs
Mix uniformly, into mixed liquor plus 10 g of crystalline flake graphite, 0 DEG C of ice-water bath stir, and 75 DEG C of 5 h of reaction, are cooled to room temperature, stood
Night, filtering supernatant, then 45 DEG C of drying；The above-mentioned pre-oxidation graphite powders of 2 g are taken to add the 100 mL concentrated sulfuric acids, 0 DEG C of ice-water bath stirs
Mix, add 20 g potassium permanganate, continue to stir 20 min, then 40 DEG C of 4 h of reaction, finally pour into 1000 mL distilled water, then by
30 mL hydrogen peroxide are added dropwise in drop, and solution reaction is golden yellow to presenting；Finally, solution is centrifuged, during dialysis washing is precipitated to
Property, product GO.
（2）Prepare 4A/RGO combination electrode materials
Title 4A is placed in 250 mL beakers, GO gels scattered 50 mL of addition, after 10~15 min of ultrasonic dissolution, is strongly stirred
30 min are mixed, obtain unit for uniform suspension；80 DEG C of suspension is stirred continuously evaporation moisture, and gained pastel is placed in baking oven 45 DEG C
Drying, 320 DEG C of 2 h of calcination under nitrogen protective condition, obtained product cooled to room temperature, up to 4A/RGO combination electrodes
Material.
（3）Prepare 4A/RGO electrodes：
Nickel foam is collector, is cleaned by ultrasonic nickel foam successively with acetone, ethanol and distilled water, vacuum drying is stand-by；By 4A/
Ethanol in proper amount ultrasonic disperse is added in RGO, acetylene black and Nafion solution, 60 DEG C of magnetic agitations are coated in cleaning into plasticity slurry
In good nickel foam, tablet press machine keeps 2 min to be pressed into thin electrode with 10 MPa pressure, and 45 DEG C of 12 h of vacuum drying, obtain 4A/
RGO electrodes.
Wherein, the mixing quality ratio of the 4A/RGO, acetylene black and Nafion solution is 8：1：1.
Claims (6)
1. the preparation method of graphene coated molecular sieve combination electrode material, it is characterised in that：Include the following steps：
（1）Prepare GO；
（2）Prepare 4A/RGO combination electrode materials；
（3）Prepare 4A/RGO electrodes.
2. the preparation method of high-performance quantum dot point coded magnetic microballoon according to claim 1, it is characterised in that：Described
The detailed process for preparing the aqueous dispersions of the magnetic polystyrene microsphere of the amine-modified carboxyl modified of polyethyleneimine is：By 30mg carboxylics
The magnetic polystyrene microsphere of base modification is placed in centrifuge tube, and Magneto separate removes supernatant, cleans 3 times with MES buffer solutions, magnetic
It is separated off supernatant；3mg/mL carbodiimides and 80mg/mL polyethyleneimines are added to the magnetic polyphenyl of carboxyl modified
In ethene microballoon, be vortexed simultaneously ultrasonic disperse, and after revolving reaction 3h, Magneto separate removes supernatant, is cleaned 3 times with ultra-pure water, disperses
In ultra-pure water, the aqueous dispersions of the magnetic polystyrene microsphere of the amine-modified carboxyl modified of polyethyleneimine are obtained.
3. the preparation method of high-performance quantum dot point coded magnetic microballoon according to claim 2, it is characterised in that：Described
The specific mistake of quantum dot is loaded on the aqueous dispersions surface of the magnetic polystyrene microsphere of the amine-modified carboxyl modified of polyethyleneimine
Cheng Wei：The aqueous dispersions of the magnetic polystyrene microsphere of the amine-modified carboxyl modified of 3mg polyethyleneimines are taken, Magneto separate water removal, is used
Washes of absolute alcohol 3 times；Chloroform/butanol solution is prepared, adds 1mL Se deposits/ZnS quantum dots solution to polyethylene
In the aqueous dispersions of the magnetic polystyrene microsphere of the carboxyl modified of imines modification, vortex is uniformly dispersed, lucifuge revolving reaction 0.5
Magneto separate removes supernatant after h, adds washes of absolute alcohol 3 times, is scattered in ultra-pure water, obtains MS@polyethyleneimines@
QDS aqueous dispersions.
4. the preparation method of high-performance quantum dot point coded magnetic microballoon according to claim 3, it is characterised in that：Described
The detailed process of water removal is：Magneto separate removes the water in MS@Ju Yixiyaan@QDS aqueous dispersions, adds 1 mL 9mg/mL
Polyethylenimine solution, be vortexed scattered rear lucifuge revolving reaction 0.5h, and Magneto separate removes supernatant, after cleaning 3 times with ultra-pure water
It is scattered in ultra-pure water, obtains cadmium sulfide/ZnS quantum dots coded magnetic microballoon.
5. the preparation method of high-performance quantum dot point coded magnetic microballoon according to claim 4, it is characterised in that：Described
The concentration of MES buffer solutions is 10 mmol/L.
6. the preparation method of high-performance quantum dot point coded magnetic microballoon according to claim 5, it is characterised in that：Described
The volume ratio of chloroform/butanol solution is 1：20.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108232142A (en) * | 2017-12-22 | 2018-06-29 | 中国科学院福建物质结构研究所 | A kind of zinc sulphide/graphene composite material, preparation method and application |
| CN108630459A (en) * | 2018-05-10 | 2018-10-09 | 河北工业大学 | A kind of preparation method of all solid state multilevel hierarchy transparent flexible ultracapacitor of low cost |
| CN110429289A (en) * | 2019-08-19 | 2019-11-08 | 北京林业大学 | A kind of preparation method of the catalyst for direct lignin alkaline fuel cell anode |
-
2017
- 2017-12-08 CN CN201711295936.1A patent/CN108010744A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108232142A (en) * | 2017-12-22 | 2018-06-29 | 中国科学院福建物质结构研究所 | A kind of zinc sulphide/graphene composite material, preparation method and application |
| CN108232142B (en) * | 2017-12-22 | 2020-10-27 | 中国科学院福建物质结构研究所 | Zinc sulfide/graphene composite material, and preparation method and application thereof |
| CN108630459A (en) * | 2018-05-10 | 2018-10-09 | 河北工业大学 | A kind of preparation method of all solid state multilevel hierarchy transparent flexible ultracapacitor of low cost |
| CN110429289A (en) * | 2019-08-19 | 2019-11-08 | 北京林业大学 | A kind of preparation method of the catalyst for direct lignin alkaline fuel cell anode |
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Application publication date: 20180508 |