CN103779107A - Graphene and ionic liquid composite material, preparation method thereof and electrochemical capacitor - Google Patents
Graphene and ionic liquid composite material, preparation method thereof and electrochemical capacitor Download PDFInfo
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to a grapheme and ionic liquid composite material and a preparation method thereof. The preparation method comprises the following steps of: (a) graphene preparation; and (b) grapheme and ionic liquid composite material preparation. The invention also relates to an electrochemical capacitor which is made in a manner that the grapheme and ionic liquid composite material is adopted as an electrode material. With the grapheme and ionic liquid composite material prepared through using the preparation method of the invention adopted, agglomerations between graphene sheets are few, and the grapheme and ionic liquid composite material has high wettability with respect to an ionic liquid electrolyte, and therefore, when the grapheme and ionic liquid composite material is adopted as the electrode material of the electrochemical capacitor, the electrochemical capacitor can have high energy storage capacity. The preparation method of the grapheme and ionic liquid composite material is advantageous in simple equipment and process, operational easiness and easiness in realization of large-scale industrial production.
Description
Technical field
The present invention relates to electrochemical field, relate in particular to a kind of Graphene/ionic liquid combination electrode material and preparation method thereof.The invention still further relates to and adopt the prepared electrochemical capacitor of this Graphene/ionic liquid combination electrode material.
Background technology
Electrochemical capacitor, as a kind of novel energy-storing device, due to advantages such as its charge-discharge velocity are fast, power density is high, have extended cycle life, is the another energy storage device that has application potential and exploitation value after lithium ion battery.But energy density lower be a key factor of restriction electrochemical capacitor development and application, explore the energy density that how to improve electrochemical capacitor and be the emphasis of this area research at present.According to computing formula E=1/2 CV of energy density
2, improve energy density and mainly start with from two aspects, improve on the one hand the voltage window of electrochemical capacitor, be the specific capacity that improves electrode material on the one hand in addition, the raising of this two aspect all can bring the raising of energy density.The voltage window of electrochemical capacitor is main relevant with the withstand voltage scope of electrolyte, in order to improve the voltage window of electrochemical capacitor, start at present to adopt ionic liquid as electrolyte, its chemical window can reach 4-6V, can significantly increase the energy density of electrochemical capacitor, but ionic liquid is because viscosity is large, poor to the wettability of electrode material, this makes the more difficult raising of specific capacity of electrode material.
Graphene is as the two-dimentional monolayer material of one, there is higher specific area and higher conductivity, it is a kind of desirable electrochemical capacitor electrode material, but this material is easily reunited, cause its actual specific area little, and poor with the wettability of ionic liquid, the stored energy ratio capacity obtaining is not high.
Summary of the invention
The object of the invention is to solve the problem and shortage that above-mentioned prior art exists, provide a kind of Graphene/ionic liquid composite material and preparation method thereof the electrochemical capacitor prepared with adopting this composite material.
The technical scheme that the present invention is directed to above-mentioned technical problem and propose is: a kind of preparation method of Graphene/ionic liquid composite material, comprise the steps: that (a) prepares Graphene: graphite oxide is scattered in deionized water, after ultrasonic, add and go back original reagent agitating heating and reduce and filter and to obtain Graphene, gained Graphene is positioned in absolute ethyl alcohol and is preserved.
(b) prepare Graphene/ionic liquid composite material: described Graphene is taken out and blotted from absolute ethyl alcohol surperficial absolute ethyl alcohol, then described Graphene is placed in to ionic liquid and obtains Graphene and ionic liquid mixture, this mixture is placed 20～30 hours under the vacuum environment of 100 ° of C, finally unnecessary ionic liquid suction filtration is removed, obtained described Graphene/ionic liquid composite material.
In described step (a), it is 0.5～1mg/ml that described graphite oxide is dispersed in the solubility obtaining in deionized water; The described ultrasonic time is 1～2 hour; The described mass ratio of going back original reagent and described graphite oxide is 1-5mg:1-3mg, the reduction temperature of described heating: 80～120 ° of C, the recovery time: 2～3 hours, described in to go back original reagent be hydrazine hydrate or sodium borohydride.
In described step (b), described ionic liquid is: at least one in the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole, 1-ethyl-3-methylimidazole hexafluorophosphate, 1-butyl-3-methylimidazole hexafluorophosphate.
In described step (a), described graphite oxide is adopted with the following method and is made: the graphite of purity 99.5% is joined in the mixed solution that mass fraction is 98% the concentrated sulfuric acid and the mass fraction red fuming nitric acid (RFNA) composition that is 65%, stir in backward described mixed solution and add potassium permanganate heated oxide, add again the hydrogenperoxide steam generator of mass fraction 30% to stir to remove potassium permanganate, then described mixed solution is carried out to suction filtration and obtain suction filtration thing, more obtain described graphite oxide after described suction filtration thing washing being dried with watery hydrochloric acid and deionized water successively.The mass volume ratio of described graphite, the described concentrated sulfuric acid, described red fuming nitric acid (RFNA), described potassium permanganate and described hydrogen peroxide is 1-5g:90-475ml:25-120ml:4-20g:10-30ml.In the described vacuum drying oven being dried under 60 ° of C, carry out, the described dry time is 12 hours.
The present invention also comprises Graphene/ionic liquid composite material of utilizing above-mentioned preparation method to make.
The present invention also further relates to the electrochemical capacitor that adopts this Graphene/ionic liquid composite material to prepare.Described electrochemical capacitor comprise by capacitor electrode slice, barrier film, capacitor electrode slice in order the stacked battery core forming, for installing the closed shell of described battery core, and the electrolyte of filling in described closed shell, described capacitor electrode slice comprises collector and is coated in the slurry on this collector, described slurry comprises electrode material, binding agent Kynoar and the conductive agent acetylene black that 85:5:10 mixes in mass ratio, and described electrode material is the prepared Graphene/ionic liquid composite material of above-mentioned preparation method.Wherein, described electrolyte is identical with the ionic liquid of selecting in described step (b).
Compared with prior art, utilize the prepared Graphene/ionic liquid composite material of preparation method of the present invention, reunion between graphene sheet layer is less, and there is higher wettability with il electrolyte, while making this composite material as electrochemical capacitor electrode material, there is higher stored energy capacitance.In addition, equipment, the technique of preparing this composite material are simple, and convenient operation is easy to realize large-scale industrial production.
Embodiment
Below in conjunction with embodiment, the present invention is given to elaboration further.
the preparation of Graphene/ionic liquid composite material:concrete preparation technology's flow process of Graphene/ionic liquid composite material of the present invention is as follows: graphite → graphite oxide → Graphene → Graphene/ionic liquid composite material.
Concrete preparation process is roughly divided into following steps.
(1) prepare graphite oxide: the graphite of purity 99.5% is joined in the mixed solution that mass fraction is 98% the concentrated sulfuric acid and the mass fraction red fuming nitric acid (RFNA) composition that is 65%, stir in backward described mixed solution and add potassium permanganate heated oxide, add again the hydrogenperoxide steam generator of mass fraction 30% to stir to remove potassium permanganate, then mixed solution is carried out to suction filtration and obtain suction filtration thing, after suction filtration thing being washed, is dried with watery hydrochloric acid and deionized water successively again, obtain graphite oxide, graphite oxide is dry in vacuum drying oven under 60 ° of C, and be 12 hours drying time.
Wherein, the mass volume ratio of graphite, the concentrated sulfuric acid, red fuming nitric acid (RFNA), potassium permanganate and hydrogen peroxide is: 1-5g:90-475ml:25-120ml:4-20g:10-30ml.
(2) prepare graphene oxide: prepared graphite oxide in step (1) is dispersed in deionized water, the graphite oxide solubility obtaining is 0.5～1mg/ml, graphite oxide was scattered in deionized water in ultrasonic 1～2 hour, after ultrasonic, add and go back original reagent agitating heating and reduce and filter and to obtain Graphene, gained Graphene is positioned in absolute ethyl alcohol and is preserved.
Wherein, described in go back original reagent and described graphite oxide mass ratio be 1-5mg:1-3mg, described in to go back original reagent be hydrazine hydrate or sodium borohydride; Described ionic liquid is: at least one in the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole, 1-ethyl-3-methylimidazole hexafluorophosphate, 1-butyl-3-methylimidazole hexafluorophosphate.
(3) prepare Graphene/ionic liquid composite material: described Graphene is taken out and blotted from absolute ethyl alcohol surperficial absolute ethyl alcohol, then described Graphene is placed in to ionic liquid and obtains Graphene and ionic liquid mixture, this mixture is placed 20～30 hours under the vacuum environment of 100 ° of C, finally unnecessary ionic liquid suction filtration is removed, obtained described Graphene/ionic liquid composite material.
The invention still further relates to the Graphene/ionic liquid composite material being made by a kind of above-mentioned preparation method.
the preparation of electrochemical capacitor:the present invention also comprises the electrochemical capacitor that adopts the prepared Graphene/ionic liquid composite material of said method to prepare as electrode material.Electrochemical capacitor comprise by capacitor electrode slice, barrier film, capacitor electrode slice in order the stacked battery core forming, for installing closed shell and the electrolyte of filling in closed shell of described battery core.
Wherein, described capacitor electrode slice comprises collector and is coated in the slurry on this collector, and described slurry comprises prepared Graphene/ionic liquid composite material, binding agent Kynoar and the conductive agent acetylene black of said method that 85:5:10 mixes in mass ratio.
Below introduce the roughly step that uses this Graphene/ionic liquid composite material to be made into electrochemical capacitor: first, the ratio that is 85:5:10 according to mass ratio, Graphene/ionic liquid composite material, Kynoar binding agent and conductive agent acetylene black are mixed, obtain slurry.
Secondly, slurry is coated on aluminium foil, drying, slicing treatment, make electrochemical capacitor electrode sheet.
Finally, by electrochemical capacitor electrode sheet, barrier film, electrochemical capacitor electrode sheet in order stack of laminations dress up battery core, use again battery housing seal battery core, in the liquid injection port on battery container, inject electrolyte subsequently, sealing liquid injection port, obtain electrochemical capacitor, electrochemical capacitor is carried out to electro-chemical test.
Wherein, wherein, described electrolyte is identical with the ionic liquid of selecting in above-mentioned steps (3).
Below execute example 1～4th, the preparation method of Graphene/ionic liquid composite material, embodiment 5～8th, the material of embodiment 1～4 preparation is as the application of electrochemical capacitor electrode material.
It is as follows that the present invention prepares the technological process of Graphene/ionic liquid composite material: graphite → graphite oxide → Graphene → Graphene/ionic liquid composite material.
embodiment 1:(1) prepare graphite oxide: take purity and be 99.5% graphite 1g and add in the mixed solution being formed by the 90ml concentrated sulfuric acid (mass fraction is 98%) and 25ml red fuming nitric acid (RFNA) (mass fraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 6g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 92ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 10ml hydrogenperoxide steam generator (mass fraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 100ml watery hydrochloric acid and 150ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens.
(2) prepare Graphene: the graphite oxide of preparation in step (1) is added in deionized water, the solubility of graphite oxide in water is 1mg/ml, to mixture ultrasonic 1 hour, hydrazine hydrate in mass ratio afterwards: graphene oxide=2mg:1mg adds hydrazine hydrate, the solubility of hydrazine hydrate is 0.5mg/ml, the temperature of mixture is risen to 100 ° of C, stir 2 hours, stir speed (S.S.) is 200 revs/min, filter, wash the solid product Graphene obtaining with deionized water, Graphene is placed in to absolute ethyl alcohol and preserves.
(3) prepare Graphene/ionic liquid composite material: Graphene is taken out from absolute ethyl alcohol, blot surperficial absolute ethyl alcohol with filter paper, Graphene is immersed in to two fluoroform sulfimide salt [the EMIM] [Tf of 1-ethyl-3-methylimidazole completely
2n] in ionic liquid, then mixture is placed in to lower 24 hours of the vacuum environment of 100 ° of C, finally unnecessary ionic liquid suction filtration is removed, obtain Graphene/ionic liquid composite material.
embodiment 2:(1) prepare graphite oxide: take purity and be 99.5% graphite 5g and add in the mixed solution being formed by the 475ml concentrated sulfuric acid (mass fraction is 98%) and 120ml red fuming nitric acid (RFNA) (mass fraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 20g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 92ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 30ml hydrogenperoxide steam generator (mass fraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 300ml watery hydrochloric acid and 450ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens.
(3) prepare Graphene: the graphite oxide of preparation in step (1) is added in deionized water, the solubility of graphite oxide in water is 0.5mg/ml, to mixture ultrasonic 1 hour, sodium borohydride in mass ratio afterwards: graphene oxide=5mg:3mg adds sodium borohydride, the solubility of sodium borohydride is 0.3mg/ml, the temperature of mixture is risen to 80 ° of C, stir 3 hours, stir speed (S.S.) is 200 revs/min, filter, wash the solid product Graphene obtaining with deionized water, Graphene is placed in to absolute ethyl alcohol and preserves.
(3) prepare Graphene/ionic liquid composite material: Graphene is taken out from absolute ethyl alcohol, blot surperficial absolute ethyl alcohol with filter paper, Graphene is immersed in to 1-ethyl-3-methylimidazole hexafluorophosphate [EMIM] PF completely
6in ionic liquid, then mixture is placed in to lower 24 hours of the vacuum environment of 100 ° of C, finally unnecessary ionic liquid suction filtration is removed, obtain Graphene/ionic liquid composite material.
embodiment 3:(1) prepare graphite oxide: take purity and be 99.5% graphite 2g and add in the mixed solution being formed by the 170ml concentrated sulfuric acid (mass fraction is 98%) and 48ml red fuming nitric acid (RFNA) (mass fraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 8g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 92ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 16ml hydrogenperoxide steam generator (mass fraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 250ml watery hydrochloric acid and 300ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens.
(2) prepare Graphene: the graphite oxide of preparation in step (1) is added in deionized water, the solubility of graphite oxide in water is 2mg/ml, to mixture ultrasonic 2 hours, hydrazine hydrate in mass ratio afterwards: graphene oxide=4mg:1mg adds hydrazine hydrate, the solubility of hydrazine hydrate is 0.5mg/ml, the temperature of mixture is risen to 120 ° of C, stir 3 hours, stir speed (S.S.) is 200 revs/min, filter, wash the solid product Graphene obtaining with deionized water, Graphene is placed in to absolute ethyl alcohol and preserves.
(3) Graphene/ionic liquid composite material: Graphene is taken out from absolute ethyl alcohol, blot surperficial absolute ethyl alcohol with filter paper, Graphene is immersed in two fluoroform sulfimide salt [BMIM] [TFSI] ionic liquids of 1-butyl-3-methylimidazole completely, then mixture is placed in to lower 24 hours of the vacuum environment of 100 ° of C, finally unnecessary ionic liquid suction filtration is removed, obtained Graphene/ionic liquid composite material.
embodiment 4: (1) prepares graphite oxide: take purity and be 99.5% graphite 1g and add in the mixed solution being made up of the 90ml concentrated sulfuric acid (mass fraction is 98%) and 25ml red fuming nitric acid (RFNA) (mass fraction is 65%), mixture is placed under frozen water mixing bath environment and is stirred 20 minutes, in mixture, add 4g potassium permanganate at leisure again, stir 1 hour, then mixture is heated to 85 ° of C and keeps 30 minutes, add afterwards 92ml deionized water to continue to keep 30 minutes under 85 ° of C, finally add 9ml hydrogenperoxide steam generator (mass fraction 30%), stir 10 minutes, mixture is carried out to suction filtration, with 100ml watery hydrochloric acid and 150ml deionized water, solids is washed respectively successively again, wash altogether three times, last solid matter is the dry graphite oxide that obtains for 12 hours in 60 ° of C vacuum drying ovens.
(2) prepare Graphene: the graphite oxide of preparation in step (1) is added in deionized water, the solubility of graphite oxide in water is 1mg/ml, to mixture ultrasonic 1 hour, sodium borohydride in mass ratio afterwards: graphene oxide=1mg:1mg adds sodium borohydride, the solubility of sodium borohydride is 1mg/ml, the temperature of mixture is risen to 90 ° of C, stir 3 hours, stir speed (S.S.) is 200 revs/min, filter, wash the solid product Graphene obtaining with deionized water, Graphene is placed in to absolute ethyl alcohol and preserves.
(3) prepare Graphene/ionic liquid composite material: Graphene is taken out from absolute ethyl alcohol, blot surperficial absolute ethyl alcohol with filter paper, Graphene is immersed in to 1-butyl-3-methylimidazole hexafluorophosphate [BMIM] PF completely
6in ionic liquid, then mixture is placed in to lower 24 hours of the vacuum environment of 100 ° of C, finally unnecessary ionic liquid suction filtration is removed, obtain Graphene/ionic liquid composite material.
In the step (3) of above each embodiment, mixture is placed in to lower 24 hours of the vacuum environment of 100 ° of C, under this environment, ionic liquid has displaced the water in graphene sheet layer, under the vacuum environment of 100 ° of C, water in graphene sheet layer evaporates, and ionic liquid has entered graphene sheet layer, has so just formed Graphene/ionic liquid composite material.Therefore the reunion between prepared Graphene/ionic liquid composite material graphene sheet layer is less, and has higher wettability with il electrolyte, while making this composite material as electrochemical capacitor electrode material, there is higher stored energy capacitance.
embodiment 5:(1) ratio that is 85:5:10 according to mass ratio, Graphene/ionic liquid composite material prepared by embodiment 1, Kynoar binding agent and conductive agent acetylene black mix, and obtain slurry.
(2) slurry is coated on aluminium foil, through the dry 2 hours slicing treatment of dry 2 hours, the 250 ° C of 80 ° of C, makes electrochemical capacitor electrode sheet.
(3) by the electrochemical capacitor electrode sheet obtaining in the electrochemical capacitor electrode sheet obtaining in step (2), barrier film, (2) in order stack of laminations dress up battery core, use again battery housing seal battery core, in battery container, inject two fluoroform sulfimide salt [the EMIM] [Tf of 1-ethyl-3-methylimidazole by the liquid injection port on battery container subsequently
2n] ionic liquid, sealing liquid injection port, obtains electrochemical capacitor.
Electrochemical capacitor to assembling in (3) carries out charge-discharge test, and voltage window is 4V.
Embodiment 6～8 is identical with the method for embodiment 5, and the electrode material just adopting is respectively that embodiment 2～4 is out prepared, and the electrolyte of employing ionic liquid used when preparing composite material in this embodiment is identical.
table 1 is embodiment 1-4 key process parameter.
table 2 is embodiment 5~
8 carry out the specific capacity of charge-discharge test under 0.5A/g electric current.
| ? | Specific capacity (F/g) |
| Embodiment 5 | 245 |
| Embodiment 6 | 236 |
| Embodiment 7 | 228 |
| Embodiment 8 | 254 |
The specific capacity of Graphene/ionic liquid composite material prepared by employing this method under 0.5A/g current density all, more than 220F/g, is up to 254F/g, has excellent energy-storage property.
Compared with prior art, utilize the reunion between the prepared Graphene/ionic liquid composite material graphene sheet layer of preparation method of the present invention less, and there is higher wettability with il electrolyte, while making this composite material as electrochemical capacitor electrode material, there is higher stored energy capacitance.In addition, equipment, the technique of preparing this composite material are simple, and convenient operation is easy to realize large-scale industrial production.
Foregoing; it is only preferred embodiment of the present invention; not for limiting embodiment of the present invention; those of ordinary skills are according to main design of the present invention and spirit; can carry out very easily corresponding flexible or modification, therefore protection scope of the present invention should be as the criterion with the desired protection range of claims.
Claims (9)
1. a preparation method for Graphene/ionic liquid composite material, is characterized in that, comprises the steps:
(a) prepare Graphene: graphite oxide is scattered in deionized water, adds after ultrasonic and go back original reagent agitating heating and reduce and filter and to obtain Graphene, gained Graphene is positioned in absolute ethyl alcohol and is preserved;
(b) prepare Graphene/ionic liquid composite material: described Graphene is taken out and blotted from absolute ethyl alcohol surperficial absolute ethyl alcohol, then described Graphene is placed in to ionic liquid and obtains Graphene and ionic liquid mixture, this mixture is placed 20～30 hours under the vacuum environment of 100 ° of C, finally unnecessary ionic liquid suction filtration is removed, obtained described Graphene/ionic liquid composite material.
2. preparation method according to claim 1, is characterized in that, in described step (a), it is 0.5～1mg/ml that described graphite oxide is dispersed in the solubility obtaining in deionized water; The described ultrasonic time is 1～2 hour; The described mass ratio of going back original reagent and described graphite oxide is 1-5mg:1-3mg, the reduction temperature of described heating: 80～120 ° of C, the recovery time: 2～3 hours, described in to go back original reagent be hydrazine hydrate or sodium borohydride.
3. preparation method according to claim 1, it is characterized in that, in described step (b), described ionic liquid is: at least one in the two fluoroform sulfimide salt of 1-ethyl-3-methylimidazole, the two fluoroform sulfimide salt of 1-butyl-3-methylimidazole, 1-ethyl-3-methylimidazole hexafluorophosphate, 1-butyl-3-methylimidazole hexafluorophosphate.
4. preparation method according to claim 1, it is characterized in that, in described step (a), described graphite oxide is adopted with the following method and is made: the graphite of purity 99.5% is joined in the mixed solution that mass fraction is 98% the concentrated sulfuric acid and the mass fraction red fuming nitric acid (RFNA) composition that is 65%, stir in backward described mixed solution and add potassium permanganate heated oxide, add again the hydrogenperoxide steam generator of mass fraction 30% to stir to remove potassium permanganate, then described mixed solution is carried out to suction filtration and obtain suction filtration thing, after described suction filtration thing washing being dried with watery hydrochloric acid and deionized water successively again, obtain described graphite oxide.
5. preparation method according to claim 5, is characterized in that, the mass volume ratio of described graphite, the described concentrated sulfuric acid, described red fuming nitric acid (RFNA), described potassium permanganate and described hydrogen peroxide is 1-5g:90-475ml:25-120ml:4-20g:10-30ml.
6. preparation method according to claim 5, is characterized in that, in the described vacuum drying oven being dried under 60 ° of C, carries out, and the described dry time is 12 hours.
7. Graphene/the ionic liquid composite material that the arbitrary described preparation method of claim 1 to 6 makes.
8. an electrochemical capacitor, comprise by capacitor electrode slice, barrier film, capacitor electrode slice in order the stacked battery core forming, for installing the closed shell of described battery core, and the electrolyte of filling in described closed shell, described capacitor electrode slice comprises collector and is coated in the slurry on this collector, described slurry comprises electrode material, binding agent Kynoar and the conductive agent acetylene black that 85:5:10 mixes in mass ratio, it is characterized in that, described electrode material is Graphene/ionic liquid composite material claimed in claim 7.
9. electrochemical capacitor according to claim 8, is characterized in that, described electrolyte is identical with the ionic liquid of selecting in described step (b).
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| CN105597819A (en) * | 2015-12-30 | 2016-05-25 | 浙江大学 | Graphite oxide immobilized acidic ionic liquid catalyst and preparation and application thereof |
| CN105869913A (en) * | 2016-04-06 | 2016-08-17 | 清华大学 | Super capacitor and preparation method thereof |
| CN108363221A (en) * | 2018-01-22 | 2018-08-03 | 北京大学 | Adjustable long wave flow-through optical filter based on graphene |
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