CN103771397A - Preparation method for graphene and super capacitor - Google Patents
Preparation method for graphene and super capacitor Download PDFInfo
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- CN103771397A CN103771397A CN201210407636.9A CN201210407636A CN103771397A CN 103771397 A CN103771397 A CN 103771397A CN 201210407636 A CN201210407636 A CN 201210407636A CN 103771397 A CN103771397 A CN 103771397A
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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 relates to a preparation method for graphene. The method includes the steps of: adding graphite oxide into water and conducting ultrasonic dispersion to obtain an graphene oxide suspension; adding nitric acid with a mass concentration of 50%-70% into the graphene oxide suspension, conducting ultrasonic reaction under room temperature for 0.5-2 hours, and performing filtering to obtain advanced graphene oxide; and subjecting the advanced graphene oxide to ultrasonic dispersion in an organic solvent to form an advanced graphene oxide suspension, subjecting the advanced graphene oxide suspension to stirring reaction for 2-10 hours under irradiation of a high pressure mercury lamp, and conducting filtering to obtain graphene. The graphene prepared by the method can improve the specific capacity of a super capacitor. The invention also provides a preparation method of the super capacitor.
Description
Technical field
The present invention relates to a kind of preparation method of Graphene and the preparation method of ultracapacitor.
Background technology
Graphene is a kind of two-dimentional unimolecular layer material, has excellent physical properties, as high theoretical specific surface area, excellent physical strength, good snappiness and high specific conductivity etc., is subject to investigator's extensive concern.Graphene has high specific surface area, fabulous electroconductibility, good thermal conductivity, and the cost performance of the Graphene obtaining by graphite oxide reduction method is higher, and good stability, is the ideal electrode material of ultracapacitor.
But existing Graphene is during as the electrode materials of ultracapacitor, the specific storage of ultracapacitor is lower.
Summary of the invention
Based on this, be necessary the preparation method of the Graphene that a kind of specific storage that improves ultracapacitor is provided and the preparation method of ultracapacitor.
A preparation method for Graphene, comprises the steps:
Graphite oxide is added to the water to ultrasonic dispersion and forms graphene oxide suspension;
Be 50% ~ 70% nitric acid to adding mass concentration in described graphene oxide suspension, under room temperature, ultrasonic reaction 0.5 hour ~ 2 hours, obtains deep oxidation Graphene after filtration; And
Ultrasonic described deep oxidation Graphene being dispersed in formed to deep oxidation graphene suspension in organic solvent, described deep oxidation graphene suspension stirring reaction 2 hours ~ 10 hours under the irradiation of high voltage mercury lamp, obtains Graphene after filtration.
In an embodiment, described in described graphene oxide suspension, the concentration of graphene oxide is 0.1mg/mL ~ 2mg/mL therein.
In an embodiment, the graphene oxide in described graphene oxide suspension and the solid-to-liquid ratio of described nitric acid are 1mg:1ml ~ 1mg:10ml therein.
In an embodiment, described organic solvent is selected from least one in DMF, ethylene glycol, N-Methyl pyrrolidone and tetrahydrofuran (THF) therein.
In an embodiment, the power of described high voltage mercury lamp is 300W ~ 600W therein.
In an embodiment, described stirring is magnetic agitation therein.
In an embodiment, described in described deep oxidation graphene suspension, the concentration of deep oxidation Graphene is 0.5mg/mL ~ 2mg/mL therein.
A preparation method for ultracapacitor, comprises the following steps:
Graphene is provided, and described Graphene is prepared by the preparation method of above-mentioned Graphene;
After described Graphene, binding agent and conductive agent are mixed, add in solvent and make slurry, described slurry coating is prepared to electrode slice on collector; And
By being soaked in electrolytic solution after described electrode slice and barrier film assembling, obtain ultracapacitor.
In an embodiment, the mass ratio of described Graphene, described binding agent and described conductive agent is 88 ~ 92:5 ~ 10:2 ~ 3 therein.
In an embodiment, the material of described collector is aluminium, stainless steel or nickel therein.
The preparation method of above-mentioned Graphene and ultracapacitor, simple to operate; By using nitric acid to carry out deep oxidation to graphene oxide, make the hydroxyl in graphene oxide be converted into carbonyl, thereby make the edge of the Graphene of final preparation contain a large amount of carbonyls, can bring into play fake capacitance, two graphene sheet layers can provide double-layer capacitance, thereby when Graphene is applied to the electrode materials of electrical condenser, can improve the specific storage of ultracapacitor.
Accompanying drawing explanation
Fig. 1 is the preparation method's of the Graphene of an embodiment schema;
Fig. 2 is the preparation method's of the ultracapacitor of an embodiment schema.
Embodiment
For above-mentioned purpose of the present invention, feature and advantage can be become apparent more, below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.A lot of details are set forth in the following description so that fully understand the present invention.But the present invention can implement to be much different from alternate manner described here, and those skilled in the art can do similar improvement without prejudice to intension of the present invention in the situation that, and therefore the present invention is not subject to the restriction of following public concrete enforcement.
Refer to Fig. 1, the preparation method of the Graphene of an embodiment, comprises the steps:
Step S110, graphite oxide is added to the water to ultrasonic dispersion forms graphene oxide suspension.
Preferably, graphite oxide makes by improved Hummers method (selecting from JACS, 1958,80,1339), and vacuum-drying is dewatered for 24 hours at 120 ℃.
Preferably, in graphene oxide suspension, the concentration of graphene oxide is 0.1mg/mL ~ 2mg/mL.
Step S120, be 50% ~ 70% nitric acid to adding mass concentration in graphene oxide suspension, under room temperature, ultrasonic reaction 0.5 hour ~ 2 hours, obtains deep oxidation Graphene after filtration.
In this step, graphene oxide can make can carbon oxidized containing oxygen official in graphene oxide in the nitric acid of strong oxidizing property, hydroxyl, epoxy group(ing) etc. in graphene oxide is oxidized to carbonyl, carboxyl, carbonic acid gas etc., oxygen-containing functional group can form defect and hole after forming gas in graphene sheet layer, defect in graphene oxide can be torn in ultrasonic cavatition simultaneously, graphene oxide edge after tearing is also connecting oxygen-containing functional group, obtains deep oxidation Graphene.Functional group in deep oxidation Graphene be the content of carbonyl and carboxyl compared with the height of graphene oxide, the content of hydroxyl and epoxy group(ing) is few compared with graphene oxide.
Preferably, the solid-to-liquid ratio of the graphene oxide in graphene oxide suspension and nitric acid is 1mg:1ml ~ 1mg:10ml.
Preferably, the temperature of ultrasonic reaction is room temperature.
Preferably, the deep oxidation Graphene obtaining after filtration uses deionized water wash final vacuum dry 24 hours ~ 48 hours.
Step S130, ultrasonic deep oxidation Graphene being dispersed in formed to deep oxidation graphene suspension in organic solvent, deep oxidation graphene suspension stirring reaction 2 hours ~ 10 hours under the irradiation of high voltage mercury lamp, obtains Graphene after filtration.
In this step, oxygen-containing functional group in deep oxidation Graphene is under the irradiation of high voltage mercury lamp, the energy producing is reduced oxygen-containing functional group on deep oxidation Graphene upper skeleton, after irradiation after a while, inner oxygen-containing functional group major part is reduced, generate carbonic acid gas and remove, but inside still exists part carbonyl, carboxyl not to be reduced, and is connected to Graphene edge.
Preferably, organic solvent is selected from least one in DMF (DMF), ethylene glycol, N-Methyl pyrrolidone (NMP) and tetrahydrofuran (THF) (THF).
Preferably, the power of high voltage mercury lamp is 300W ~ 600W.
Preferably, stir as magnetic agitation.
Preferably, in deep oxidation graphene suspension, the concentration of deep oxidation Graphene is 0.5mg/mL ~ 2mg/mL.
The preparation method of above-mentioned Graphene, simple to operate; By using nitric acid to carry out deep oxidation to graphene oxide, make the hydroxyl in graphene oxide be converted into carbonyl, thereby make the edge of the Graphene of final preparation contain a large amount of carbonyls, can bring into play fake capacitance, two graphene sheet layers can provide double-layer capacitance, thereby when Graphene is applied to the electrode materials of electrical condenser, can improve the specific storage of electrical condenser.
Refer to Fig. 2, the preparation method of the ultracapacitor of an embodiment, comprises the steps:
Step S210, provide Graphene.
Wherein, Graphene is prepared by the preparation method of above-mentioned Graphene.
Step S220, add in solvent after Graphene, binding agent and conductive agent are mixed and make slurry, slurry coating is prepared on collector to electrode slice.
Preferably, Graphene, binding agent and conductive agent are according to mass ratio 88 ~ 92:5 ~ 10:2 ~ 3.
Preferably, solvent is selected from least one in N-Methyl pyrrolidone NMP, dehydrated alcohol and anhydrous propanone.
Preferably, slurry coating, on collector, drying, is rolled to film, is made into electrode slice after cutting.
Preferably, the material of collector is aluminium, stainless steel or nickel, and namely collector is aluminium foil, nickel foil or stainless steel substrates.
Preferably, binding agent is polyvinylidene difluoride (PVDF) (PVDF), and conductive agent is acetylene black.
Step S230, by being soaked in electrolytic solution after the assembling of electrode slice and barrier film, obtain ultracapacitor.
Preferably, electrolytic solution is that concentration is the tetraethyl ammonium a tetrafluoro borate (TEABF of 0.5mol/L ~ 1.5mol/L
4) acetonitrile (AN) solution.
Preferably, diaphragm clip is held in stacked composition battery core between two electrode slices, then uses capacitor casing sealed electrical core, finally injects electrolytic solution by the spout being arranged in capacitor casing, and sealing spout can obtain ultracapacitor.
The preparation method of above-mentioned ultracapacitor is comparatively simple; The specific storage of the ultracapacitor of preparation is higher.
Further illustrate below in conjunction with specific embodiment.
Embodiment 1
(1) graphite: purity 99.5%;
(2) graphite oxide: make graphite oxide by improved Hummers method (selecting from JACS, 1958,80,1339), 120 degree vacuum-dryings 24 hours, obtain dehydration graphite oxide;
(3) nitric acid oxidation: will obtain graphite oxide and put into water, the graphene oxide suspension of ultrasonic formation 0.1mg/L, then stir the nitric acid (add-on of nitric acid is 1mL:1mg with graphite oxide ratio) that adds 50%, ultrasonic reaction 0.5h at ambient temperature, obtains deep oxidation Graphene after filtration;
(4) reduction: the dispersion of materials that (3) are obtained is at DMF(dimethyl formamide) ultrasonic 0.5h obtains the deep oxidation graphene suspension that concentration is 0.5mg/ml in solution, again the suspension obtaining is placed on magnetic stirring apparatus, at the irradiation lower magnetic force stirring reaction 10h of high voltage mercury lamp (300W), after photo catalytic reduction, filter and obtain grapheme material.
Embodiment 2
(1) graphite: purity 99.5%;
(2) graphite oxide: make graphite oxide by improved Hummers method (selecting from JACS, 1958,80,1339), 120 degree vacuum-dryings 24 hours, obtain dehydration graphite oxide;
(3) nitric acid oxidation: will obtain graphite oxide and put into water, the graphene oxide suspension of ultrasonic formation 2mg/L, then stir the nitric acid (add-on of nitric acid is 1mL:1mg with graphite oxide ratio) that adds 70%, ultrasonic reaction 2h at ambient temperature, obtains deep oxidation Graphene after filtration;
(4) reduction: the dispersion of materials that (3) are obtained obtains 2mg/ml at ethylene glycol organic solvent for ultrasonic 0.5 ~ 2h, again the suspension obtaining is placed on magnetic stirring apparatus, at the irradiation lower magnetic force stirring reaction 2h of high voltage mercury lamp (600W), after photo catalytic reduction, filter and obtain grapheme material.
Embodiment 3
(1) graphite: purity 99.5%;
(2) graphite oxide: make graphite oxide by improved Hummers method (selecting from JACS, 1958,80,1339), 120 degree vacuum-dryings 24 hours, obtain dehydration graphite oxide;
(3) nitric acid oxidation: will obtain graphite oxide and put into water, the graphene oxide suspension of ultrasonic formation 0.5mg/L, then stir the nitric acid (add-on of nitric acid is 1mL:1mg with graphite oxide ratio) that adds 60%, ultrasonic reaction 1h at ambient temperature, obtains deep oxidation Graphene after filtration;
(4) reduction: the dispersion of materials that (3) are obtained is at NMP(N-methyl-2-pyrrolidone) organic solvent for ultrasonic 1h obtains 1mg/ml, again the suspension obtaining is placed on magnetic stirring apparatus, at the irradiation lower magnetic force stirring reaction 7h of high voltage mercury lamp (400W), after photo catalytic reduction, filter and obtain grapheme material.
Embodiment 4
(1) graphite: purity 99.5%;
(2) graphite oxide: make graphite oxide by improved Hummers method (selecting from JACS, 1958,80,1339), 120 degree vacuum-dryings 24 hours, obtain dehydration graphite oxide;
(3) nitric acid oxidation: will obtain graphite oxide and put into water, the graphene oxide suspension of ultrasonic formation 1mg/L, then stir the nitric acid (add-on of nitric acid is 1mL:1mg with graphite oxide ratio) that adds 65%, ultrasonic reaction 1.5h at ambient temperature, obtains deep oxidation Graphene after filtration;
(4) reduction: the dispersion of materials that (3) are obtained is at THF(tetrahydrofuran (THF)) organic solvent for ultrasonic 1.5h obtains 1.5mg/ml, again the suspension obtaining is placed on magnetic stirring apparatus, at the irradiation lower magnetic force stirring reaction 4h of high voltage mercury lamp (500W), after photo catalytic reduction, filter and obtain grapheme material.
Embodiment 5
1, prepare super capacitor electrode slice
First, select Graphene prepared by embodiment 1 as active material;
Secondly, the ratio that is 88:10:2 according to mass ratio, Graphene prepared by embodiment 1, polyvinylidene difluoride (PVDF) binding agent and conductive agent acetylene black mix, and obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Order stack of laminations according to pole piece, barrier film, pole piece is dressed up battery core, then uses battery housing seal battery core, subsequently toward injecting 1mol/L tetraethyl ammonium a tetrafluoro borate (TEABF by the spout being arranged on battery container in battery container
4) acetonitrile (AN) solution as electrolytic solution, sealing spout, obtain ultracapacitor.
Embodiment 6
1, prepare super capacitor electrode slice
First, select Graphene prepared by embodiment 2 as active material;
Secondly, the ratio that is 88:10:2 according to mass ratio, Graphene prepared by embodiment 2, polyvinylidene difluoride (PVDF) binding agent and conductive agent acetylene black mix, and obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Order stack of laminations according to pole piece, barrier film, pole piece is dressed up battery core, then uses battery housing seal battery core, subsequently toward injecting 0.5mol/L tetraethyl ammonium a tetrafluoro borate (TEABF by the spout being arranged on battery container in battery container
4) acetonitrile (AN) solution as electrolytic solution, sealing spout, obtain ultracapacitor.
Embodiment 7
1, prepare super capacitor electrode slice
First, selecting Graphene prepared by embodiment 3 is active material;
Secondly, the ratio that is 88:10:2 according to mass ratio, Graphene prepared by embodiment 3, polyvinylidene difluoride (PVDF) binding agent and conductive agent acetylene black mix, and obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Order stack of laminations according to pole piece, barrier film, pole piece is dressed up battery core, then uses battery housing seal battery core, subsequently toward injecting 1.5mol/L tetraethyl ammonium a tetrafluoro borate (TEABF by the spout being arranged on battery container in battery container
4) acetonitrile (AN) solution as electrolytic solution, sealing spout, obtain ultracapacitor.
Embodiment 8
1, prepare super capacitor electrode slice
First, select Graphene prepared by embodiment 4 as active material;
Secondly, the ratio that is 88:10:2 according to mass ratio, Graphene prepared by embodiment 4, polyvinylidene difluoride (PVDF) binding agent and conductive agent acetylene black mix, and obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Order stack of laminations according to pole piece, barrier film, pole piece is dressed up battery core, then uses battery housing seal battery core, subsequently toward injecting 0.8mol/L tetraethyl ammonium a tetrafluoro borate (TEABF by the spout being arranged on battery container in battery container
4) acetonitrile (AN) solution as electrolytic solution, sealing spout, obtain ultracapacitor.
Comparative example 1
(1) graphite: purity 99.5%;
(2) graphite oxide: make graphite oxide by improved Hummers method (selecting from JACS, 1958,80,1339), 120 degree vacuum-dryings 24 hours, obtain dehydration graphite oxide;
(3) Graphene: the graphite oxide obtaining is put into retort furnace, reduce 30s under 1050 ℃ of high temperature under argon gas inert atmosphere.
Comparative example 2
1, prepare super capacitor electrode slice
First, select grapheme material prepared by comparative example 1 as active material;
Secondly, the ratio that is 88:10:2 according to mass ratio, Graphene prepared by comparative example 1, polyvinylidene difluoride (PVDF) binding agent and conductive agent acetylene black mix, and obtain slurry;
Finally, slurry is coated on aluminium foil, drying, roll film, trimming processing, make the pole piece of ultracapacitor.
2, the assembling of ultracapacitor
Order stack of laminations according to pole piece, barrier film, pole piece is dressed up battery core, use again battery housing seal battery core, subsequently toward by be arranged on spout on battery container toward acetonitrile (AN) solution that injects 1mol/L tetraethyl ammonium a tetrafluoro borate (TEABF4) in battery container as electrolytic solution, sealing spout, obtains ultracapacitor.
Be under the current density of 0 ~ 2.7V, 0.5A/g in voltage range, the ultracapacitor that utilizes charge-discharge test instrument to prepare embodiment 5 ~ 8 and comparative example 2 carries out constant current charge-discharge test, and its performance data is listed in the table below.
As can be seen from the above table, use the ultracapacitor of the Graphene of embodiment 1 ~ 4 preparation to have obvious lifting than the capacity of the ultracapacitor of the Graphene that uses conventional hot reducing method to prepare.
The above embodiment has only expressed several embodiment of the present invention, and it describes comparatively concrete and detailed, but can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (10)
1. a preparation method for Graphene, is characterized in that, comprises the steps:
Graphite oxide is added to the water to ultrasonic dispersion and forms graphene oxide suspension;
Be 50% ~ 70% nitric acid to adding mass concentration in described graphene oxide suspension, under room temperature, ultrasonic reaction 0.5 hour ~ 2 hours, obtains deep oxidation Graphene after filtration; And
Ultrasonic described deep oxidation Graphene being dispersed in formed to deep oxidation graphene suspension in organic solvent, described deep oxidation graphene suspension stirring reaction 2 hours ~ 10 hours under the irradiation of high voltage mercury lamp, obtains Graphene after filtration.
2. the preparation method of Graphene according to claim 1, is characterized in that, described in described graphene oxide suspension, the concentration of graphene oxide is 0.1mg/mL ~ 2mg/mL.
3. the preparation method of Graphene according to claim 1, is characterized in that, the graphene oxide in described graphene oxide suspension and the solid-to-liquid ratio of described nitric acid are 1mg:1ml ~ 1mg:10ml.
4. the preparation method of Graphene according to claim 3, is characterized in that, described organic solvent is selected from least one in DMF, ethylene glycol, N-Methyl pyrrolidone and tetrahydrofuran (THF).
5. the preparation method of Graphene according to claim 1, is characterized in that, the power of described high voltage mercury lamp is 300W ~ 600W.
6. the preparation method of Graphene according to claim 1, is characterized in that, described stirring is magnetic agitation.
7. the preparation method of Graphene according to claim 1, is characterized in that, described in described deep oxidation graphene suspension, the concentration of deep oxidation Graphene is 0.5mg/mL ~ 2mg/mL.
8. a preparation method for ultracapacitor, is characterized in that, comprises the following steps:
Graphene is provided, and described Graphene is prepared by the preparation method of the Graphene described in claim 1-7 any one;
After described Graphene, binding agent and conductive agent are mixed, add in solvent and make slurry, described slurry coating is prepared to electrode slice on collector; And
By being soaked in electrolytic solution after described electrode slice and barrier film assembling, obtain ultracapacitor.
9. the preparation method of ultracapacitor according to claim 8, is characterized in that, the mass ratio of described Graphene, described binding agent and described conductive agent is 88 ~ 92:5 ~ 10:2 ~ 3.
10. the preparation method of ultracapacitor according to claim 8, is characterized in that, the material of described collector is aluminium, stainless steel or nickel.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20160196893A1 (en) * | 2015-01-05 | 2016-07-07 | National Chiao Tung University | Method for preparing two-dimensional material |
| CN104036971B (en) * | 2014-05-29 | 2017-01-18 | 浙江大学 | Preparation method for graphene/carbon nano-tube composite fibre-based super capacitor |
| CN107416804A (en) * | 2017-05-26 | 2017-12-01 | 东莞市悉达纳米科技有限公司 | A kind of method that graphene is produced using suspension technology |
| CN110164711A (en) * | 2018-02-05 | 2019-08-23 | 山东佳星环保科技有限公司 | The preparation method of graphene-based capacitor with ultra high energy density |
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| CN102167314A (en) * | 2011-05-23 | 2011-08-31 | 浙江大学 | Method for preparing graphene |
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| CN201870466U (en) * | 2010-10-21 | 2011-06-22 | 宓建君 | Glass pot cover |
| CN102126720A (en) * | 2011-04-14 | 2011-07-20 | 中国科学院理化技术研究所 | Method for synthesizing graphene |
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| CN104036971B (en) * | 2014-05-29 | 2017-01-18 | 浙江大学 | Preparation method for graphene/carbon nano-tube composite fibre-based super capacitor |
| US20160196893A1 (en) * | 2015-01-05 | 2016-07-07 | National Chiao Tung University | Method for preparing two-dimensional material |
| CN107416804A (en) * | 2017-05-26 | 2017-12-01 | 东莞市悉达纳米科技有限公司 | A kind of method that graphene is produced using suspension technology |
| CN110164711A (en) * | 2018-02-05 | 2019-08-23 | 山东佳星环保科技有限公司 | The preparation method of graphene-based capacitor with ultra high energy density |
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