CN103903878A - Graphene electrode plate and preparing method thereof - Google Patents
Graphene electrode plate and preparing method thereof Download PDFInfo
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- CN103903878A CN103903878A CN201210572476.3A CN201210572476A CN103903878A CN 103903878 A CN103903878 A CN 103903878A CN 201210572476 A CN201210572476 A CN 201210572476A CN 103903878 A CN103903878 A CN 103903878A
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- 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 discloses a graphene electrode plate and a preparing method thereof. The method comprises the following steps: graphene and ionic liquid are mixed and then subjected to the ultrasonic dispersion process to obtain stable graphene suspending liquid; and the graphene suspending liquid is used as an electrolyte, two aluminum foils or copper foils which are made from a same material are inserted into the electrolyte in parallel as an anode electrode and a cathode electrode separately, a voltage is applied after electrical connection, and the cathode electrode is taken down to obtain the graphene electrode plate. According to the preparing method provided in the invention, grapheme can be better dispersed by using the ionic liquid, and the ionic liquid exists between layers of the deposited graphene, so the compatibility between the graphene and the electrolyte can be changed, and the capacity can be improved; according to the electrode plate prepared through the electro-deposition method, the complex coating process can be omitted, the process is simple, and binder does not need to be used, so the contact resistance between a current collector and an active material layer can be effectively reduced so as to reduce the equivalent series resistance of a supercapacitor, and improve the power density finally.
Description
Technical field
The present invention relates to electrochemical material field, relate in particular to a kind of Graphene electrodes sheet and preparation method thereof.
Background technology
Ultracapacitor is a kind of novel energy storage device, there is the advantages such as high power density (for the more than 10 times of common batteries), high cycle life (cycle-index can reach more than 100,000 times), fast charging and discharging performance are good, be widely used in the AC-battery power source of military field, device for mobile communication, computer and electric automobile etc.Conventionally mainly being assembled by electrode active material layer, electrolyte, barrier film, collector, shell etc. of ultracapacitor.The energy density of existing ultracapacitor is generally lower, the influencing factor of the energy density of ultracapacitor mainly contains the electric capacity of electrode material, the voltage of system, electrode material accounts for the proportion of the total weight of electrode active material layer, collector, sheathing material composition, therefore, the weight of the energy-storage property of increase electrode material and each composition material of reduction device can effectively improve the performance of device.Wherein, the quality of reduction collector is a method that effectively improves energy density.
Owing to existing very strong pi-pi accumulation and Van der Waals force in Graphene between carbon atomic layer, therefore, in the process of preparing electrode material, be easy to reunite.And due to the relation of Graphene nature, itself and il electrolyte have poor compatibility, cause it in the time using as electrode material, performance capacity is lower; 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 Graphene electrodes sheet by certain method, 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.But existing Graphene is generally and the compound electrode slice that makes of other metal collector that compound middle employing binding agent, has increased contact internal resistance between layers, make the equivalent series resistance of electrode slice higher, and power density is low.
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:
After Graphene and ionic liquid are mixed, grind, obtain mixture, then mixture is added in solvent and carry out ultrasonic dispersion, the graphene suspension that to form concentration be 0.1-5mg/ml; The mass volume ratio of described Graphene and ionic liquid is 1:1-1:5;
Using described graphene suspension as electrolyte, the Copper Foil of the identical material using diameter as 5-10cm or aluminium foil are as anode electrode and cathode electrode respectively, two electrode Parallel Symmetrics are placed in electrolyte, two die openings are 0.5-1cm, and adding the direct current of 40-80V at the two ends of two electrodes, electrophoresis 5-60min, takes off cathode electrode, dry processing, obtains Graphene electrodes sheet.
The preparation method of described Graphene electrodes sheet, preferably, described solvent is water, DMF(N, dinethylformamide), DMSO(dimethyl sulfoxide (DMSO)), DMAc(N, N-dimethylacetylamide) or NMP(N-methyl pyrrolidone).
The preparation method of described Graphene electrodes sheet, preferably, the time of described ultrasonic dispersion is 1-5h.
The preparation method of described Graphene electrodes sheet, preferably, described ionic liquid is glyoxaline ion liquid or pyrrolidines ionic liquid; Wherein, described glyoxaline ion liquid is 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate or 1-butyl-3-methylimidazole hexafluorophosphate; Described pyrrolidines ionic liquid is 1-methyl-propyl pyrrole tetrafluoroborate or 1-methyl-propyl pyrrole hexafluorophosphate.
The preparation method of described Graphene electrodes sheet, preferably, described dry processing is to carry out in the vacuum drying chamber of 100 ℃.
The Graphene electrodes sheet that the present invention also provides above-mentioned either method to make.
The preparation method of Graphene electrodes sheet provided by the invention, uses ionic liquid dispersed graphite alkene preferably, and post-depositional Graphene, and interlayer exists certain ionic liquid, is conducive to change the compatibility of Graphene and electrode solution, is conducive to raising capacity; The electrode slice of preparing by the method for electro-deposition, can save complicated coating process, and 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
The preparation method of a kind of Graphene electrodes sheet provided by the invention, formed by graphene film and collector, by Graphene is dispersed in ionic liquid, obtain stable graphene suspension, again graphene suspension is deposited on collector by the method for electro-deposition, obtains Graphene electrodes sheet.
As shown in Figure 1, a kind of preparation technology's flow process of Graphene electrodes sheet is as follows:
(1) preparation of graphene suspension:
Will Graphene and ionic liquid grind 5-20min with agate mortar after mixing, then mixture is added and in solvent, carries out ultrasonic dispersions 1-5h, the graphene suspension that formation concentration is 0.1-5mg/ml;
Wherein, solvent can be water, DMF, DMSO, DMAc or NMP; Ionic liquid can be glyoxaline ion liquid, or pyrrolidines ionic liquid; Glyoxaline ion liquid has: 1-ethyl-3-methylimidazole tetrafluoroborate, 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-butyl-3-methylimidazole hexafluorophosphate; Pyrrolidines ionic liquid: 1-methyl-propyl pyrrole tetrafluoroborate, 1-methyl-propyl pyrrole hexafluorophosphate.
(2) preparation of Graphene electrodes sheet:
By the graphene suspension in (1) as electrolyte, the Copper Foil of the identical material using diameter as 5-10cm or aluminium foil are as anode electrode and cathode electrode respectively, two electrode Parallel Symmetrics are placed in electrolyte, two die openings are 0.5-1cm, the direct current that adds 40-80V at the two ends of amount electrode, electrophoresis 5-60min, takes off cathode electrode, dry in the vacuum drying chamber of 100 ℃, obtain Graphene electrodes sheet.
The preparation method of Graphene electrodes sheet provided by the invention, uses ionic liquid dispersed graphite alkene preferably, and post-depositional Graphene, and interlayer exists certain ionic liquid, is conducive to change the compatibility of Graphene and electrode solution, is conducive to raising capacity; The electrode slice of preparing by the method for electro-deposition, can save complicated coating process, and 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 synthetic Graphene electrodes sheet of the present invention is as follows:
(1) preparation of graphene suspension: by 1g Graphene, 1g1-ethyl-3-methylimidazole tetrafluoroborate, after mixing, grind 5min with agate mortar, then mixture is added and in DMF solvent, carry out ultrasonic dispersion 5h, the graphene suspension that to form concentration be 0.1mg/ml.
(2) preparation of Graphene electrodes sheet: by the graphene suspension in (1) as electrolyte, get the Copper Foil of two 5cm diameters respectively as anode electrode and cathode electrode, two electrode Parallel Symmetrics are placed in electrolyte, two electrode die openings are 0.5cm, add the direct current of 40V at the two ends of electrode, electrophoresis 5min, takes off the Copper Foil as negative electrode, dry in the vacuum drying chamber of 100 ℃, obtain Graphene electrodes sheet.
(1) preparation of graphene suspension: by 1g Graphene, 3g1-butyl-3-methylimidazole hexafluorophosphate, after mixing, grind 20min with agate mortar, then mixture is added and in DMSO solvent, carry out ultrasonic dispersion 5h, the graphene suspension that to form concentration be 2mg/ml.
(2) preparation of Graphene electrodes sheet: by the graphene suspension in (1) as electrolyte, get aluminium foil that two diameters are 10cm respectively as anode electrode and cathode electrode, two electrode Parallel Symmetrics are placed in electrolyte, two electrode spacings are 0.5cm, add the direct current of 80V at the two ends of electrode, electrophoresis 20min, using as the aluminium foil of negative electrode, it takes off, dry in the vacuum drying chamber of 100 ℃, obtain Graphene electrodes sheet.
Embodiment 3
Preparation technology's flow process of the synthetic Graphene electrodes sheet of the present invention is as follows:
(1) preparation of graphene suspension: by 1g Graphene, after mixing, 5g1-methyl-propyl pyrrole tetrafluoroborate grinds 60min with agate mortar, then mixture is added and in nmp solvent, carry out ultrasonic dispersion 1h, the graphene suspension that to form concentration be 5mg/ml.
(2) preparation of Graphene electrodes sheet: by the graphene suspension in (1) as electrolyte, get Copper Foil that two diameters are 10cm respectively as anode electrode and cathode electrode, two electrode Parallel Symmetrics are placed in electrolyte, two electrode spacings are 0.5cm, add the direct current of 80V at the two ends of electrode, electrophoresis 60min, takes off the Copper Foil as negative electrode, dry in the vacuum drying chamber of 100 ℃, obtain Graphene electrodes sheet.
Performance Detection:
The preparation of pole piece: above-mentioned electrode slice is carried out to roll-in: the pole piece of gained roller mill is carried out to roll extrusion; 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, assemble rear leaving standstill and within one day, carried out constant current charge-discharge test, wherein voltage range is 0-3.0V, and electric current is that 1A/g carries out constant current charge-discharge.
Table 1 is that embodiment (1) to (3) carries out Electrochemical results.
Table 1
| ? | |
|
Embodiment 3 |
| Power density kw/kg | 19.3 | 20.7 | 21.4 |
| Capacity F/g | 152 | 157 | 160 |
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 (8)
1. a preparation method for Graphene electrodes sheet, is characterized in that, comprises the steps:
After Graphene and ionic liquid are mixed, grind, obtain mixture, then mixture is added in solvent and carry out ultrasonic dispersion, the graphene suspension that to form concentration be 0.1-5mg/ml; The mass ratio of described Graphene and ionic liquid is 1:1-1:5;
Using described graphene suspension as electrolyte, the Copper Foil of the identical material using diameter as 5-10cm or aluminium foil are as anode electrode and cathode electrode respectively, two electrode Parallel Symmetrics are placed in electrolyte, two die openings are 0.5-1cm, and adding the direct current of 40-80V at the two ends of two electrodes, electrophoresis 5-60min, takes off cathode electrode, dry processing, obtains Graphene electrodes sheet.
2. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, described solvent is water, DMF, dimethyl sulfoxide (DMSO), DMA or 1-METHYLPYRROLIDONE.
3. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, the time of described ultrasonic dispersion is 1-5h.
4. 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.
5. the preparation method of Graphene electrodes sheet according to claim 4, 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.
6. the preparation method of Graphene electrodes sheet according to claim 4, is characterized in that, described pyrrolidines ionic liquid is 1-methyl-propyl pyrrole tetrafluoroborate or 1-methyl-propyl pyrrole hexafluorophosphate.
7. the preparation method of Graphene electrodes sheet according to claim 1, is characterized in that, described dry processing is to carry out in the vacuum drying chamber of 100 ℃.
8. the Graphene electrodes sheet that the arbitrary described method of claim 1 to 7 makes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105140465A (en) * | 2015-09-21 | 2015-12-09 | 上海展枭新能源科技有限公司 | One-step method for preparing adhesive-free graphene electrode and used device |
| CN107527746A (en) * | 2017-08-04 | 2017-12-29 | 湖南国盛石墨科技有限公司 | A kind of graphene negative electricity pole piece and its preparation method and application |
| CN111017911A (en) * | 2019-12-26 | 2020-04-17 | 南开大学 | Reduced graphene oxide and preparation method and application thereof |
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| CN102021633A (en) * | 2009-09-09 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of graphene thin film field emission material |
| CN102142294A (en) * | 2010-01-29 | 2011-08-03 | 海洋王照明科技股份有限公司 | Graphene-ionic liquid composite material and preparation method thereof |
| CN102507696A (en) * | 2011-10-19 | 2012-06-20 | 浙江大学 | Ion-selective electrode based on graphene electrode and preparation method thereof |
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| CN102021633A (en) * | 2009-09-09 | 2011-04-20 | 中国科学院金属研究所 | Preparation method of graphene thin film field emission material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105140465A (en) * | 2015-09-21 | 2015-12-09 | 上海展枭新能源科技有限公司 | One-step method for preparing adhesive-free graphene electrode and used device |
| CN105140465B (en) * | 2015-09-21 | 2017-07-28 | 上海展枭新能源科技有限公司 | One-step method prepares the method and equipment therefor of the Graphene electrodes of binder free |
| CN107527746A (en) * | 2017-08-04 | 2017-12-29 | 湖南国盛石墨科技有限公司 | A kind of graphene negative electricity pole piece and its preparation method and application |
| CN111017911A (en) * | 2019-12-26 | 2020-04-17 | 南开大学 | Reduced graphene oxide and preparation method and application thereof |
| CN111017911B (en) * | 2019-12-26 | 2021-07-30 | 南开大学 | Reduced graphene oxide and preparation method and application thereof |
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Application publication date: 20140702 |