CN103681001A - A method for producing a graphene electrode slice - Google Patents
A method for producing a graphene electrode slice Download PDFInfo
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- CN103681001A CN103681001A CN201210361476.9A CN201210361476A CN103681001A CN 103681001 A CN103681001 A CN 103681001A CN 201210361476 A CN201210361476 A CN 201210361476A CN 103681001 A CN103681001 A CN 103681001A
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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
- Y02E60/10—Energy storage using batteries
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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 belongs to electrochemistry material field and discloses a method for producing a graphene electrode slice. The method comprises steps of: processing the surface of a conductive substrate slice; producing graphene suspension liquid the surface of which is provided with negative charges; producing positive charge graphene suspension liquid; producing a graphene film; and producing a graphene electrode slice. In the method for producing a graphene electrode slice, ionic liquid is used for providing positive charges so as to achieve a good graphene dispersing effect, to prolong distance between graphene layers, and to be beneficial to infiltration of electrode liquid and increase in capacity. The graphene film is produced by electrostatic attraction so as to eliminate a complex coating process and achieve simple technology. In addition, binder is prevented such that contact internal resistance between a current collector and an active material layer can be effectively decreased. Therefore, equivalent series resistance of a super capacitor is further effectively reduced and finally power density is increased.
Description
Technical field
The present invention relates to electrochemical material field, relate in particular to a kind of preparation method of Graphene electrodes sheet.
Background technology
Since the strong K sea nurse of the peace moral of Univ Manchester UK (Andre K.Geim) etc. was prepared grapheme material in 2004, because being subject to people, its unique structure and photoelectric property pay attention to widely.Graphene is called " nova " that is rising in material science and Condensed Matter Physics field, many novelties that it has and unique character and potential application are just attracting many scientific workers.Single-layer graphene has large specific area, good conduction, heat conductivility and low thermal coefficient of expansion.As: 1. high strength, Young mole, (1,100GPa), fracture strength: (125GPa); 2. high heat conductance, (5,000W/mK); 3. high conductivity, carrier transport rate, (200,000cm
2/ V * s); 4. high specific area, (calculated value: 2,630m
2/ g).Especially its high conductivity matter, the structural property of large specific surface character and the nanoscale of its monolayer two dimension can be used as electrode material in ultracapacitor and lithium ion battery.
Owing to existing very strong pi-pi accumulation and Van der Waals force in Graphene between carbon atomic layer, therefore, in preparing the process of electrode material, be easy to reunite.The technique that tradition is prepared electrode slice is comparatively complicated, and adds certain binding agent, the binding agent of insulation add the conductivity that has not only reduced material, also greatly reduce the specific area of material, thereby affected the capacitance characteristic of Graphene self.
Graphene can be prepared into by certain method Graphene electrodes sheet, and its high mechanical performance and high conductivity, therefore can, in the situation that not adding any binding agent and metal collector, be applied directly in electrode of super capacitor simultaneously.
Summary of the invention
Based on the problems referred to above, problem to be solved by this invention is to provide a kind of preparation method of Graphene electrodes sheet.
Technical scheme of the present invention is as follows:
A preparation method for Graphene electrodes sheet, comprises the steps:
Conductive base egative film is placed in to acetone, ethanol, the ultrasonic processing of intermediate water 20-30min successively, dry up subsequently, then conductive base egative film is immersed in the polyethyleneimine: amine aqueous solution of 1-5g/l, carry out surface chargeization and process 10-30min, after taking-up, with intermediate water, rinse and dry up, standby;
Graphene is put into the flask that concentrated acid is housed, in 60-80 ℃, add hot reflux 10-24h, subsequently at the dry 24h of 50-80 ℃ of vacuum drying chamber, obtain the Graphene of surface band negative electrical charge, then the Graphene of surface band negative electrical charge is joined and in the first solvent, carry out ultrasonic dispersion 1-5h, the graphene suspension of the surface band negative electrical charge that to form concentration be 0.1～5mg/ml;
After Graphene is mixed with ionic liquid, grind evenly, obtain mixture, then mixture is added and in the second solvent, carry out ultrasonic dispersions 1-5h, the graphene suspension of the surface band ionic liquid positive charge that formation concentration is 0.1～5mg/ml;
First conductive base egative film after surface charge is processed is immersed in the graphene suspension of the above-mentioned surface band negative electrical charge making and takes out after 5-20min, with a large amount of intermediate waters, rinse well, dry up; Then again conductive base egative film is immersed in to 5-20min in the graphene solution of the above-mentioned surface band positive charge making, with a large amount of intermediate waters, rinses well, dry up, make one deck graphene film, repeatedly repeat this step, make sandwich construction graphene film;
Described sandwich construction graphene film is placed in to protective gas environment, and with the heating rate of 5-10 ℃/min, is slowly warming up to 200-800 ℃ described sandwich construction graphene film is carried out, after heat treated 0.5-2h, obtaining Graphene electrodes sheet.
The preparation method of described Graphene electrodes sheet, wherein, described conductive base egative film is indium tin oxide glass, aluminium zinc oxide glass or indium-zinc oxide glass.
The preparation method of described Graphene electrodes sheet, wherein, described in to dry up be to adopt nitrogen to dry up.
The preparation method of described Graphene electrodes sheet, wherein, described concentrated acid is that volume ratio is the concentrated sulfuric acid of 1:1-3:1 and the mixed acid that red fuming nitric acid (RFNA) forms.
The preparation method of described Graphene electrodes sheet, wherein, described the first solvent and the second solvent are DMF, dimethyl sulfoxide (DMSO), DMA or 1-METHYLPYRROLIDONE.
The preparation method of described Graphene electrodes sheet, wherein, described ionic liquid is glyoxaline ion liquid or pyrrolidines ionic liquid.
The preparation method of described Graphene electrodes sheet, wherein, described glyoxaline ion liquid is 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate or 1-butyl-3-methylimidazole hexafluorophosphate.
The preparation method of described Graphene electrodes sheet, wherein, described pyrrolidines ionic liquid is 1-methyl-propyl pyrrole tetrafluoroborate or 1-methyl-propyl pyrrole hexafluorophosphate.
The preparation method of described Graphene electrodes sheet, wherein, described protective gas is that volume ratio is the nitrogen of 95:5～90:10 and the mist of hydrogen.
The preparation method of Graphene electrodes sheet provided by the invention, uses ionic liquid that positive charge is provided, and can reach the effect of good dispersed graphite alkene simultaneously, and its existence increase graphene layer spacing, is conducive to the infiltration of electrode solution, is conducive to raising capacity; By electrostatic attraction, prepare graphene film, can save complicated coating process, technique is simple, and without binding agent, therefore can effectively reduce the internal resistance that contacts between collector and active material layer, and then reduce the equivalent series resistance of ultracapacitor, finally improve power density.
Accompanying drawing explanation
Fig. 1 is preparation technology's flow chart of Graphene electrodes sheet of the present invention.
Embodiment
Preparation technology's flow process of Graphene electrodes sheet provided by the invention, as shown in Figure 1, comprises the steps:
(1), the surface treatment of conductive base egative film: conductive base egative film is placed in to acetone, ethanol, the ultrasonic processing of intermediate water 20-30min successively, after processing totally, with a large amount of intermediate waters, rinse, nitrogen dries up, again conductive base egative film is immersed in and in polymine (PEI) aqueous solution of 1-5g/l, carries out surface chargeization and process 10-30min, then take out, again with intermediate water rinse conductive base egative film and with nitrogen dry up, standby; Conductive base egative film surface band positive electricity now; Wherein, described conductive base egative film is indium tin oxide glass (abbreviation ito glass), aluminium zinc oxide glass (being called for short AZO glass) or indium-zinc oxide glass (being called for short IZO glass); Ito glass comprises substrate of glass, and by the conductive layer that magnetron sputtering technique is prepared on surface of glass, material is ITO; AZO glass and IZO category of glass seemingly, do not repeat them here;
(2), the preparation of surface band negative electrical charge graphene suspension: Graphene is put into the concentrated acid (mixed solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) is housed, wherein both volume ratios are 1:1-3:1) flask in 60-80 ℃, add hot reflux 10-24h, and at the dry 24h of 50-80 ℃ of vacuum drying chamber, obtain the Graphene of surface band negative electrical charge, joined and in the first solvent, carried out ultrasonic dispersion 1-5h, the graphene suspension of the surface band negative electrical charge that to form concentration be 0.1～5mg/ml; Wherein, the first solvent is DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO), DMA (DMAc) or 1-METHYLPYRROLIDONE (NMP);
(3), the preparation of positive charge graphene suspension: will grind 5-20min with agate mortar after Graphene and ionic liquid mixing, then mixture is added and in the second solvent, carry out ultrasonic dispersion 1-5h, the graphene suspension of the surface band ionic liquid positive charge that to form concentration be 0.1～5mg/ml; Wherein, the second solvent is DMF (DMF), dimethyl sulfoxide (DMSO) (DMSO), DMA (DMAc) or 1-METHYLPYRROLIDONE (NMP); Ionic liquid is glyoxaline ion liquid or pyrrolidines ionic liquid;
Glyoxaline ion liquid is 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate or 1-butyl-3-methylimidazole hexafluorophosphate; Preferably pyrrolidines ionic liquid is 1-methyl-propyl pyrrole tetrafluoroborate or 1-methyl-propyl pyrrole hexafluorophosphate;
Preferably, ionic liquid is 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate and 1-methyl-propyl pyrrole tetrafluoroborate.
(4), the preparation of graphene film: first the conductive base egative film by above-mentioned steps (1) after surface treatment is immersed in the graphene solution of the surface band negative electrical charge that concentration that step (2) makes is 0.1～5mg/ml and takes out after 5-20min, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, and then conductive base egative film is immersed in to 5-20min in the graphene solution of the surface band positive charge that concentration that step (3) makes is 0.1～5mg/ml, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, obtain one deck graphene film; Repeatedly repeat this step, make sandwich construction graphene film;
By soaking for the first time, in the conductive layer surface electric charge suction-operated of conductive base egative film, electronegative Graphene is adsorbed onto on conductive base egative film, form ground floor graphene layer; By soaking for the second time, conductive base egative film utilizes the Graphene of adsorption, electronegative Graphene adsorption band positive charge, forms second layer graphene layer; At two kinds, so repeatedly alternately soak in the graphene solution of different electric charges, just can obtain on the surface of conductive base egative film the graphene film of sandwich construction.
(5) preparation of Graphene electrodes sheet: by the conductive base egative film of the graphene film with sandwich construction of step (4) gained, put into tube furnace, pass into the inert gas (mist that comprises nitrogen, argon gas or nitrogen and argon gas, be preferably nitrogen) drive the air in stove away, then pass into the mist (in hydrogen, the percentage by volume of mist is 5-10%) of nitrogen and hydrogen, heating rate with 5-10 ℃/min, slowly be warming up to 200-800 ℃, heat treated 0.5-2h at this temperature, obtains Graphene electrodes sheet on conductive base egative film surface.
The preparation method of Graphene electrodes sheet provided by the invention, uses ionic liquid that positive charge is provided, and can reach the effect of good dispersed graphite alkene simultaneously, and its existence increase graphene layer spacing, is conducive to the infiltration of electrode solution, is conducive to raising capacity; By electrostatic attraction, prepare graphene film, can save complicated coating process, technique is simple, and without binding agent, therefore can effectively reduce the internal resistance that contacts between collector and active material layer, and then reduce the equivalent series resistance of ultracapacitor, finally improve power density.
Below in conjunction with accompanying drawing, preferred embodiment of the present invention is described in further detail.
Preparation technology's flow process of the Graphene electrodes sheet that the present invention is synthetic is as follows:
(1), the surface treatment of ito glass: the ito glass of cutting out is placed in to acetone, ethanol, the ultrasonic processing of intermediate water 20min successively, after processing totally, with a large amount of intermediate waters, rinse, nitrogen dries up, again ito glass is immersed in to 10min in polymine (PEI) aqueous solution of 1g/l and carries out surface charge processing, after taking-up, with intermediate water, rinse and dry up with nitrogen standby, ito glass surface band positive electricity now.
(2), the surperficial preparation with negative electrical charge graphene suspension: Graphene is put into the concentrated acid (mixed solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) is housed, wherein both volume ratios are 1:1) flask in 80 ℃, add hot reflux 10h, and at the dry 24h of 50 ℃ of vacuum drying chambers, obtain the Graphene of surface band negative electrical charge, joined in DMF and carry out ultrasonic dispersion 1h, the surface that formation concentration is 0.1mg/ml is with the graphene suspension of negative electrical charge;
(3), the preparation of positive charge graphene suspension: will grind 5min with agate mortar after Graphene and the mixing of 1-ethyl-3-methylimidazole tetrafluoroborate, then mixture is added in DMF solvent and carry out ultrasonic dispersion 1h, the surface that formation concentration is 0.1mg/ml is with the graphene suspension of positive charge.
(4), the preparation of graphene film: first the ito glass by step (1) after surface treatment is immersed in the graphene solution of the surface band negative electrical charge that concentration that step (2) makes is 0.1mg/ml and takes out after 5min, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, 5min in the graphene solution of the surface band positive charge that to be then immersed in concentration that step (3) makes be 0.1mg/ml, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, obtain the preparation of one deck graphene film; Repeat this step 20 time, make 20 layer graphene films;
(5) preparation of Graphene electrodes sheet: by 20 layer graphene films of step (4) gained, put into tube furnace, pass into nitrogen and drive the air in stove away, then pass into the mist of nitrogen and hydrogen (5%), heating rate with 5 ℃/min, delay and be warming up to 200 ℃, at this temperature, heat 2h, obtain Graphene electrodes sheet.
Preparation technology's flow process of the Graphene that the present invention is synthetic is as follows:
(1), the surface treatment of AZO glass: the AZO glass of cutting out is placed in to acetone, ethanol, the ultrasonic processing of intermediate water 30min successively.After processing totally, with a large amount of intermediate waters, rinse, nitrogen dries up, then AZO glass is immersed in to 30min in polymine (PEI) aqueous solution of 51g/L and carries out surface charge processing, after taking-up, with intermediate water, rinse and dry up with nitrogen standby, AZO glass surface positively charged now.
(2)/surperficial preparation with negative electrical charge graphene suspension: Graphene is put into the concentrated acid (mixed solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) is housed, wherein both volume ratios are 3:1) flask in 60 ℃, add hot reflux 24h, and at the dry 24h of 80 ℃ of vacuum drying chambers, obtain surface with negative electrical charge Graphene, be added to the water and carry out ultrasonic dispersion 5h, the surface that formation concentration is 5mg/ml is with the graphene suspension of negative electrical charge.
(3) preparation of positive charge graphene suspension: by Graphene and 1-butyl-3-methylimidazole hexafluorophosphate, after mixing, with agate mortar, grind 20min, then mixture is added in DMSO solvent and carry out ultrasonic dispersion 5h, the surface that formation concentration is 5mg/ml is with the graphene suspension of ionic liquid positive charge.
(4) preparation of graphene film: first the AZO glass by step (1) after surface treatment be immersed in the graphene solution of the surface band negative electrical charge that concentration that step (2) makes is 5mg/ml and take out after 20min, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, be immersed in again 20min in the graphene solution of surface band positive charge of the 5mg/ml that step (3) makes, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, obtain the preparation of one deck graphene film, repeat this step 40 time, obtain 40 layer graphene films;
(5), the preparation of Graphene electrodes sheet: 40 layer graphene films of step (4) gained are put into tube furnace, pass into nitrogen and drive the air in stove away, then pass into the mist of nitrogen and hydrogen (10%), heating rate with 10 ℃/min, slowly be warming up to 500 ℃, at this temperature, heat 1.5h, obtain Graphene electrodes sheet.
Preparation technology's flow process of the Graphene electrodes sheet that the present invention is synthetic is as follows:
(1), the surface treatment of IZO glass: the IZO glass of cutting out is placed in to acetone, ethanol, the ultrasonic processing of intermediate water 25min successively.After processing totally, with a large amount of intermediate waters, rinse, nitrogen dries up, then substrate sheet is immersed in to 20min in polymine (PEI) aqueous solution of 3g/l and carries out surface charge processing, after taking-up, with intermediate water, rinse and dry up with nitrogen standby, IZO glass surface positively charged now.
(2) the surperficial preparation with negative electrical charge graphene suspension: Graphene is put into the concentrated acid (mixed solution of the concentrated sulfuric acid and red fuming nitric acid (RFNA) is housed, wherein both volume ratios are 2:1) flask in 70 ℃, add hot reflux 17h, and at the dry 24h of 65 ℃ of vacuum drying chambers, obtain surface with negative electrical charge Graphene, be added to the water and carry out ultrasonic dispersion 3h, the surface that formation concentration is 3mg/ml is with the graphene suspension of negative electrical charge.
(3) preparation of positive charge graphene suspension: will grind 13min with agate mortar after Graphene and the mixing of 1-methyl-propyl pyrrole tetrafluoroborate, then mixture is added in nmp solvent and carry out ultrasonic dispersion 3h, the surface that formation concentration is 3mg/ml is with the graphene suspension of ionic liquid positive charge.
(4) preparation of graphene film: first the IZO glass by step (1) after surface treatment be immersed in the graphene solution of the surface band negative electrical charge that concentration that step (3) makes is 3mg/ml and take out after 13min, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, 13min in the graphene solution of the surface band positive charge that to be immersed in concentration that step (4) makes be 3mg/ml again, with a large amount of intermediate waters, rinse well, with rubber pipette bulb, dry up, obtain the preparation of one deck graphene film, repeat this step 100 time, make 100 layer graphene films.
(5) preparation of Graphene electrodes sheet: 100 layer graphene films of step (4) gained are put into tube furnace, pass into nitrogen and drive the air in stove away, then pass into the mist of nitrogen and hydrogen (8%), heating rate with 7 ℃/min, slowly be warming up to 800 ℃, at this temperature, heat 0.5h, obtain Graphene electrodes sheet.
Chemical property detects.When chemical property detects, electrode slice need to be assemblied on ultracapacitor.
The preparation of pole piece: the electrode slice that the various embodiments described above are made carries out roll-in, carries out roll extrusion by the pole piece of gained with roller mill;
Cut-parts: the pole piece of roll-in is broken into the circular pole piece that diameter is 10mm with card punch, accurately weigh;
The assembling of battery: barrier film and electrolyte are assembled into ultracapacitor according to cell making process, its septation is celgard2000, electrolyte is 1-ethyl-3-methylimidazole tetrafluoro boric acid salting liquid, assembled and within latter standing one day, carried out constant current charge-discharge test, wherein voltage range is 0-3.0V, electric current is that 1A/g carries out constant current charge-discharge, and testing result is as table 1.
Table 1
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| Power density kw/kg | 24.3 | 25.7 | 26.4 |
| Capacity F/g | 132 | 143 | 148 |
Should be understood that, the above-mentioned statement for preferred embodiment of the present invention is comparatively detailed, can not therefore think the restriction to scope of patent protection of the present invention, and scope of patent protection of the present invention should be as the criterion with claims.
Claims (9)
1. a preparation method for Graphene electrodes sheet, is characterized in that, comprises the steps:
Conductive base egative film is placed in to acetone, ethanol, the ultrasonic processing of intermediate water 20-30min successively, dry up subsequently, then conductive base egative film is immersed in the polyethyleneimine: amine aqueous solution of 1-5g/l, carry out surface chargeization and process 10-30min, after taking-up, with intermediate water, rinse and dry up, standby;
Graphene is put into the flask that concentrated acid is housed, in 60-80 ℃, add hot reflux 10-24h, subsequently at the dry 24h of 50-80 ℃ of vacuum drying chamber, obtain the Graphene of surface band negative electrical charge, then the Graphene of surface band negative electrical charge is joined and in the first solvent, carry out ultrasonic dispersion 1-5h, the graphene suspension of the surface band negative electrical charge that to form concentration be 0.1～5mg/ml;
After Graphene is mixed with ionic liquid, grind evenly, obtain mixture, then mixture is added and in the second solvent, carry out ultrasonic dispersions 1-5h, the graphene suspension of the surface band ionic liquid positive charge that formation concentration is 0.1～5mg/ml;
First conductive base egative film after surface charge is processed is immersed in the graphene suspension of the above-mentioned surface band negative electrical charge making and takes out after 5-20min, with a large amount of intermediate waters, rinse well, dry up; Then again conductive base egative film is immersed in to 5-20min in the graphene solution of the above-mentioned surface band positive charge making, with a large amount of intermediate waters, rinses well, dry up, make one deck graphene film, repeatedly repeat this step, make sandwich construction graphene film;
Described sandwich construction graphene film is placed in to protective gas environment, and with the heating rate of 5-10 ℃/min, is slowly warming up to 200-800 ℃ described sandwich construction graphene film is carried out, after heat treated 0.5-2h, obtaining Graphene electrodes sheet.
2. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, described conductive base egative film is indium tin oxide glass, aluminium zinc oxide glass or indium-zinc oxide glass.
3. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, described in to dry up be to adopt nitrogen to dry up.
4. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, described concentrated acid is that volume ratio is the concentrated sulfuric acid of 1:1-3:1 and the mixed acid that red fuming nitric acid (RFNA) forms.
5. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, described the first solvent and the second solvent are DMF, dimethyl sulfoxide (DMSO), DMA or 1-METHYLPYRROLIDONE.
6. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, described ionic liquid is glyoxaline ion liquid or pyrrolidines ionic liquid.
7. the preparation method of Graphene electrodes sheet according to claim 5, it is characterized in that, described glyoxaline ion liquid is 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate or 1-butyl-3-methylimidazole hexafluorophosphate.
8. the preparation method of Graphene electrodes sheet according to claim 5, is characterized in that, described pyrrolidines ionic liquid is 1-methyl-propyl pyrrole tetrafluoroborate or 1-methyl-propyl pyrrole hexafluorophosphate.
9. the preparation method of Graphene electrodes sheet according to claim 5, is characterized in that, described protective gas is that volume ratio is the nitrogen of 95:5～90:10 and the mist of hydrogen.
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