CN103680975A - Graphene/ionic liquid composite electrode, preparation method thereof and capacitor - Google Patents
Graphene/ionic liquid composite electrode, preparation method thereof and capacitor Download PDFInfo
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- CN103680975A CN103680975A CN201210362588.6A CN201210362588A CN103680975A CN 103680975 A CN103680975 A CN 103680975A CN 201210362588 A CN201210362588 A CN 201210362588A CN 103680975 A CN103680975 A CN 103680975A
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Abstract
The invention relates to a graphene/ionic liquid composite electrode and a preparation method thereof. The preparation method comprises the following steps: (a) preparing a graphene and ionic liquid mixture; and (b) preparing a graphene and ionic liquid composite electrode. The invention further relates to a capacitor prepared by adopting the graphene and ionic liquid composite electrode as electrode material. According to the preparation method of the invention, ionic liquid which is solid at room temperature is used as solvent to prepare graphene through a microwave stripping method in a heating state, the preparation efficiency is improved, and grapheme is enabled to have good dispersion performance; an ionic liquid membrane is used as a separating membrane and a high-polymer separating membrane is not adopted, which is conducive to improvement of the proportion of active materials and the energy density and reduction of the size of the capacitor; ionic liquid and graphene are mixed to prepare the composite electrode and are in close contact with each other, which is more conducive to electronic conduction; and a thermal spraying method is adopted to prepare a current collector, which can help to reduce the contact resistance of the electrode material and the current collector and improve the power density.
Description
Technical field
The present invention relates to electrochemical field, relate in particular to a kind of Graphene/ionic liquid combination electrode and preparation method thereof.The invention still further relates to and adopt this Graphene/ionic liquid combination electrode as the prepared capacitor of electrode material.
Background technology
Graphene is a kind of Two-dimensional Carbon atomic crystal of the discoveries such as the strong K sea nurse of the peace moral of Univ Manchester UK in 2004 (Andre K.Geim), and obtains the physics Nobel Prize in 2010, again causes material with carbon element research boom.Because its unique structure and photoelectric property become the study hotspot in the fields such as material with carbon element, nanometer technology, Condensed Matter Physics and functional material, many scientific workers have been attracted.Graphene has good conduction, heat conductivility and low thermal coefficient of expansion, can be used for electrode material, composite material etc.In current preparation method, have graphite oxide reducing process, this method can cause the destruction of graphene-structured, and uses the poisonous chemical reagent that has pollution, and environment is caused to bad impact; Also have by pyrolysis carbon source and prepare Graphene, this method yields poorly, cost is higher.Ultracapacitor has good circulation useful life and high power density, has wide practical use.When Graphene is for electrode material for super capacitor at present, need to add binding agent, this can cause the proportion of active material to decline, and affects the performance of capacity, also can increase internal resistance, affects the performance of power density.
Summary of the invention
The object of the invention is to solve the problem and shortage that above-mentioned prior art exists, a kind of preparation method of Graphene/ionic liquid combination electrode is provided and adopts in the prepared capacitor of this Graphene/ionic liquid combination electrode, utilize under room temperature and make solvent for solid-state ionic liquid, under heated condition, by microwave stripping method, prepare Graphene, improved preparation efficiency, and Graphene has been had to fine dispersiveness.
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 combination electrode, comprises the steps.
(a) prepare Graphene and ionic liquid mixture: get intercalated graphite and join in the container that ionic liquid is housed, peel off after ultrasonic, obtain Graphene and ionic liquid mixture.
(b) prepare Graphene/ionic liquid combination electrode: get described Graphene and ionic liquid mixture and be put in mould, to constant the applying of mould, press rear this pressure that keeps until be cooled to room temperature, take out sample, the metal film that is 2～5um at arbitrary coating thickness of described sample again, obtains blocky graphite alkene/ionic liquid combination electrode of single face spraying matel coated film.
Described intercalated graphite preparation method is as follows: graphite is pressed into graphite flake as work electrode, using stereotype as to electrode, Hg/Hg2SO4 is as reference electrode, intercalator is as electrolyte, by described work electrode, described electrode, described reference electrode put into electrolytic cell and be fully immersed in described electrolyte, and adopt stainless steel substrates as collector, and under the current density of 5～100mA/cm2, react 1～20 hour, after cleaning-drying, can obtain pure intercalated graphite.
Described graphite is a kind of in native graphite, Delanium, expanded graphite, and described graphite flake is of a size of 75 * 40 * 7mm3.
Described intercalator is at least one in formic acid, acetic acid, propionic acid, nitric acid, nitromethane.
In step (a), the mass volume ratio of described intercalated graphite and described ionic liquid is 1g:(10～100) ml; The temperature of described ionic liquid is 150～300 ℃; Described ultrasonic power is that 1000～2000w, splitting time are 10～100 minutes.
Described ionic liquid is: 1-ethyl-3-methylimidazole bromine salt, 1-ethyl-3-methylimidazole villaumite, 1-ethyl-3-methylimidazole salt compounded of iodine, 1-ethyl-2,3-methylimidazole fluoroform sulphonate, 1,2-diethyl-3-methylimidazole fluoroform sulphonate, 1,2-dimethyl-3-ethyl imidazol(e) bromine salt, 1,2-dimethyl-3-ethyl imidazol(e) villaumite, 1, at least one in 2-dimethyl-3-ethyl imidazol(e) tetrafluoroborate.
In step (b), the described Graphene of choosing and the weight of ionic liquid mixture are 20～60g, and the length and width size of described mould is respectively 200mm * 300mm, and described metal film is copper film or aluminium film.
The present invention also comprises the Graphene/ionic liquid combination electrode that utilizes above-mentioned preparation method to make.
Above-mentioned Graphene/ionic liquid combination electrode can be used as electrode material and is applied in capacitor, this capacitor comprise by combination electrode, ionic liquid film, combination electrode in order the stacked battery core forming, for installing the closed shell of described battery core, and filling is at the electrolyte of closed shell, the one side that described compound electric pole piece does not spray described metal film contacts with described ionic liquid film, and described compound electric pole piece is above-mentioned nitrating Graphene/ionic liquid combination electrode.
Described ionic liquid film adopts thin film coated device to be prepared from, and thickness is 3～10um, and length and width are 300mm * 200mm; The material of preparing described ionic liquid film is identical with the ionic liquid of selecting in described step (a).
Compared with prior art,, there is following advantage in Graphene/ionic liquid combination electrode of the present invention and preparation method thereof:
1. utilize under room temperature and make solvent for solid-state ionic liquid, under heated condition, by microwave stripping method, prepare Graphene, improved preparation efficiency, and Graphene is had to fine dispersiveness.
2. adopt ionic liquid film to serve as barrier film, and do not use polymer separators, be conducive to improve active material proportion and energy density, also can reduce the volume of capacitor; Ionic liquid is mixed with into combination electrode with Graphene, and the two close contact is more conducive to electrical conductivity.
3. adopt the mode of thermal spraying, can reduce contact resistance, the raising power density of electrode material and collector.
4. in preparing the process of Graphene, reduced size mixing, the technology for preparing electrode such as batch mixing, coating, further optimized the manufacturing process of chemical capacitor, reduced manufacturing cost.In preparation, needed raw material source is wide, and cost is low, and preparation technology is simple, is easy to realize suitability for industrialized production.
Embodiment
Below in conjunction with embodiment, the present invention is given to elaboration further.
The preparation process of Graphene collector of the present invention is roughly divided into following steps.
(1) prepare intercalated graphite: graphite is pressed into and is of a size of 75 * 40 * 7mm
3, be about 2g graphite flake as work electrode, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, intercalator is as electrolyte, by work electrode, electrode, reference electrode are put into electrolytic cell and be fully immersed in electrolyte, and adopts stainless steel substrates as collector, at 5～100mA/cm
2current density under react 1～20 hour, through washed with de-ionized water, vacuum drying chamber, in 60～80 ℃, can obtain pure intercalated graphite after dry 12～24 hours.
(2) preparing Graphene and ionic liquid mixture: by mass volume ratio, be 1g:(10～100) intercalated graphite is joined to temperature is in 150～300 ℃ of ionic liquids to ml, after ultrasonic under the power of 1000～2000w, peel off 10～100 minutes, obtain Graphene and ionic liquid mixture.
(3) prepare Graphene/ionic liquid combination electrode: get 20～60g Graphene and ionic liquid mixture and be put into length and width and be respectively in 300mm * 200mm mould, add die cover, to the constant pressure that applies 20MPa of mould, until die cover is no longer after mold bottom motion, mould keeps this pressure until be cooled to room temperature, open mould, take out the sample in mould, in arbitrary, sample, adopt the metal film that the mode coating thickness of heat spray is 2～5um again, obtain blocky graphite alkene/ionic liquid combination electrode of single face spraying matel coated film.Metal film can be copper film or aluminium film.
Wherein, graphite is a kind of in native graphite, Delanium, expanded graphite, and intercalator is at least one in formic acid, acetic acid, propionic acid, nitric acid, nitromethane.
Ionic liquid is 1-ethyl-3-methylimidazole bromine salt (chemical formula EtMeImBr), 1-ethyl-3-methylimidazole villaumite (chemical formula EtMeImCl), 1-ethyl-3-methylimidazole salt compounded of iodine (chemical formula EtMeImI), 1-ethyl-2,3-methylimidazole fluoroform sulphonate (Chemical formula 1-Et-2,3-Me
2imCF
3sO
3), 1,2-diethyl-3-methylimidazole fluoroform sulphonate (Chemical formula 1,2-Et
2-3-MeImCF
3sO
3), 1,2-dimethyl-3-ethyl imidazol(e) bromine salt (Chemical formula 1,2-Me
2-3-EtImBr), 1,2-dimethyl-3-ethyl imidazol(e) villaumite (Chemical formula 1,2-Me
2-3-EtImCl), 1,2-dimethyl-3-ethyl imidazol(e) tetrafluoroborate (Chemical formula 1,2-Me
2-3-EtImBF
4) at least one.
The present invention also comprises the Graphene/ionic liquid combination electrode that utilizes above-mentioned preparation method to make, and this Graphene/ionic liquid combination electrode can be used as electrode material and is applied in capacitor.
This capacitor comprise by Graphene/ionic liquid combination electrode, ionic liquid film, Graphene/ionic liquid combination electrode in order the stacked battery core forming, for installing the closed shell of battery core, and annotate at the electrolyte of closed shell, the compound electric pole piece not one side of spray metal film contacts with ionic liquid film.
This method of preparing capacitor is: by Graphene/ionic liquid combination electrode, ionic liquid film, Graphene/ionic liquid combination electrode in order lamination be placed on battery container, wherein Graphene/ionic liquid combination electrode of spray metal film one side does not contact with ionic liquid film, sealing, obtains ultracapacitor.
Wherein, the ionic liquid film that serves as barrier film effect adopts thin film coated device to be prepared from, and ionic liquid film thickness is 3～10um, and length and width are 300mm * 200mm, and the material of preparing ionic liquid film is identical with the ionic liquid of selecting in above-mentioned steps (2).
With 1～3 pair of Graphene/ionic liquid combination electrode of the present invention of embodiment and the preparation process of applying the capacitor of this combination electrode, be specifically described below.
Embodiment 1
(1) prepare intercalated graphite: native graphite is pressed into and is of a size of 75 * 40 * 7mm
3natural graphite flakes (about 2g) as work electrode, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, intercalator formic acid is as electrolyte, by work electrode, electrode, reference electrode are put into electrolytic cell and be fully immersed in electrolyte, and adopts stainless steel substrates as collector, at 5mA/cm
2current density under react 20 hours, can obtain intercalated graphite.Through washed with de-ionized water, vacuum drying chamber, in 60 ℃, can obtain pure intercalated graphite after dry 24 hours.
(2) prepare Graphene and ionic liquid mixture: by mass volume ratio 1g:10ml, intercalated graphite being joined to temperature is in 150 ℃ of 1-ethyl-3-methylimidazole bromine salt liquid, after ultrasonic under the power of 2000w, peel off 10 minutes, obtain Graphene and 1-ethyl-3-methylimidazole bromine salt liquid mixture.
(3) prepare Graphene/ionic liquid combination electrode: get 30g Graphene and 1-ethyl-3-methylimidazole bromine salt ion liquid mixture and be put into length and width and be respectively in 300mm * 200mm mould, add die cover, to the constant pressure that applies 20MPa of mould, until die cover is no longer after mold bottom motion, mould keeps this pressure until be cooled to room temperature, open mould, take out the sample in mould, the aluminium film that is 3um at arbitrary coating thickness of sample again, obtains blocky graphite alkene/1-ethyl-3-methylimidazole bromine salt combination electrode of single face spraying aluminising film.
The method of utilizing Graphene/1-ethyl-3-methylimidazole bromine salt combination electrode to prepare capacitor is: with thin film coated device, prepare the 1-ethyl-3-methylimidazole bromine salt ion liquid film that thickness is 5um, by Graphene/1-ethyl-3-methylimidazole bromine salt combination electrode, 1-ethyl-3-methylimidazole bromine salt ion liquid film, Graphene/1-ethyl-3-methylimidazole bromine salt combination electrode in order lamination is placed on battery container, Graphene/1-ethyl-3-methylimidazole bromine salt combination electrode the one side that does not wherein spray aluminium film contacts with 1-ethyl-3-methylimidazole bromine salt ion liquid film, sealing, obtain capacitor.
Embodiment 2
(1) prepare intercalated graphite: Delanium is pressed into and is of a size of 75 * 40 * 7mm
3artificial stone ink sheet (about 2g) as work electrode, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, intercalator acetic acid is as electrolyte, by work electrode, electrode, reference electrode are put into electrolytic cell and be fully immersed in electrolyte, and adopts stainless steel substrates as collector, at 20mA/cm
2current density under react 1 hour, can obtain intercalated graphite.Through washed with de-ionized water, vacuum drying chamber, in 70 ℃, can obtain pure intercalated graphite after dry 20 hours.
(2) prepare Graphene and ionic liquid mixture: by mass volume ratio 1g:100ml, intercalated graphite being joined to temperature is in the 1-ethyl-3-methylimidazole villaumite ionic liquid of 300 ℃, after ultrasonic under the power of 1000w, peel off 100 minutes, obtain Graphene and 1-ethyl-3-methylimidazole villaumite ionic liquid mixture.
(3) prepare Graphene/ionic liquid combination electrode: get 20g Graphene and 1-ethyl-3-methylimidazole villaumite ionic liquid mixture and be put into length and width and be respectively in 300mm * 200mm mould, add die cover, to the constant pressure that applies 20MPa of mould, until die cover is no longer after mold bottom motion, mould keeps this pressure until be cooled to room temperature, open mould, take out the sample in mould, the aluminium film that is 2um at arbitrary coating thickness of sample again, obtains blocky graphite alkene/1-ethyl-3-methylimidazole villaumite combination electrode of single face spraying aluminising film.
The method of utilizing Graphene/1-ethyl-3-methylimidazole villaumite combination electrode to prepare capacitor is: with thin film coated device, prepare the 1-ethyl-3-methylimidazole villaumite ionic liquid film that thickness is 3um, by Graphene/1-ethyl-3-methylimidazole villaumite combination electrode, / 1-ethyl-3-methylimidazole villaumite ionic liquid film, Graphene/1-ethyl-3-methylimidazole villaumite combination electrode in order lamination is placed on battery container, Graphene/1-ethyl-3-methylimidazole villaumite combination electrode the one side that does not wherein spray aluminium film contacts with 1-ethyl-3-methylimidazole villaumite ionic liquid film, sealing, obtain ultracapacitor.
Embodiment 3
(1) prepare intercalated graphite: expanded graphite is pressed into and is of a size of 75 * 40 * 7mm
3expanded graphite sheet (about 2g) as work electrode, using stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, propionic acid is as electrolyte, by work electrode, electrode, reference electrode are put into electrolytic cell and be fully immersed in electrolyte, and adopts stainless steel substrates as collector, at 50mA/cm
2current density under react 15 hours, can obtain intercalated graphite.Through washed with de-ionized water, vacuum drying chamber, in 80 ℃, can obtain pure intercalated graphite after dry 12 hours.
(2) prepare Graphene and ionic liquid mixture: by mass volume ratio 1g:50ml by intercalated graphite join temperature be 210 ℃ 1, in 2-diethyl-3-methylimidazole fluoroform sulphonate, after ultrasonic under the power of 1200w, peel off 50 minutes, obtain the mixture of Graphene and 1,2-diethyl-3-methylimidazole fluoroform sulphonate ionic liquid.
(3) prepare Graphene/ionic liquid combination electrode: get 60g Graphene and 1, the mixture of 2-diethyl-3-methylimidazole fluoroform sulphonate ionic liquid is put into length and width and is respectively in 300mm * 200mm mould, add die cover, to the constant pressure that applies 20MPa of mould, until die cover is no longer after mold bottom motion, mould keeps this pressure until be cooled to room temperature, open mould, take out the sample in mould, the copper film that is 5um at arbitrary coating thickness of sample again, obtain blocky graphite alkene/1 of one side spraying copper film, 2-diethyl-3-methylimidazole fluoroform sulphonate combination electrode.
Utilize Graphene/1, the method that 2-diethyl-3-methylimidazole fluoroform sulphonate combination electrode is prepared capacitor is: with thin film coated device, preparing thickness is 1 of 10um, 2-diethyl-3-methylimidazole fluoroform sulphonate ionic liquid film, by Graphene/1, 2-diethyl-3-methylimidazole fluoroform sulphonate combination electrode, 1-ethyl-2, 3-methylimidazole fluoroform sulphonate ionic liquid film, Graphene/1, 2-diethyl-3-methylimidazole fluoroform sulphonate combination electrode in order lamination is placed on battery container, wherein do not spray Graphene/1 of copper film, 2-diethyl-3-methylimidazole fluoroform sulphonate combination electrode one side is with 1, the contact of 2-diethyl-3-methylimidazole fluoroform sulphonate ionic liquid film, sealing, obtain ultracapacitor.
Table 1 is the design parameter of embodiment 1～11, and wherein the operating procedure of embodiment 4～11 is identical with embodiment 1～3, just with reference to table 1, has carried out parameter transformation, at this, its preparation process is repeated no more.
Table 1
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 (10)
1. a preparation method for Graphene/ionic liquid combination electrode, is characterized in that, comprises the steps:
(a) prepare Graphene and ionic liquid mixture: get intercalated graphite and join in the container that ionic liquid is housed, peel off after ultrasonic, obtain Graphene and ionic liquid mixture;
(b) prepare Graphene/ionic liquid combination electrode: get described Graphene and ionic liquid mixture and be put in mould, to constant the applying of mould, press rear this pressure that keeps until be cooled to room temperature, take out sample, the metal film that is 2～5um at arbitrary coating thickness of described sample again, obtains blocky graphite alkene/ionic liquid combination electrode of single face spraying matel coated film.
2. preparation method according to claim 1, is characterized in that, described intercalated graphite preparation method is as follows: graphite is pressed into graphite flake as work electrode, usings stereotype as to electrode, Hg/Hg
2sO
4as reference electrode, intercalator is as electrolyte, by described work electrode, described electrode, described reference electrode are put into electrolytic cell and be fully immersed in described electrolyte, and adopts stainless steel substrates as collector, at 5～100mA/cm
2current density under react 1～20 hour, after cleaning-drying, can obtain pure intercalated graphite.
3. preparation method according to claim 2, is characterized in that, described graphite is a kind of in native graphite, Delanium, expanded graphite, and described graphite flake is of a size of 75 * 40 * 7mm
3.
4. preparation method according to claim 2, is characterized in that, described intercalator is at least one in formic acid, acetic acid, propionic acid, nitric acid, nitromethane.
5. preparation method according to claim 1, is characterized in that, in step (a), the mass volume ratio of described intercalated graphite and described ionic liquid is 1g:(10～100) ml; The temperature of described ionic liquid is 150～300 ℃; Described ultrasonic power is that 1000～2000w, splitting time are 10～100 minutes.
6. preparation method according to claim 1, it is characterized in that, described ionic liquid is: 1-ethyl-3-methylimidazole bromine salt, 1-ethyl-3-methylimidazole villaumite, 1-ethyl-3-methylimidazole salt compounded of iodine, 1-ethyl-2,3-methylimidazole fluoroform sulphonate, 1,2-diethyl-3-methylimidazole fluoroform sulphonate, 1,2-dimethyl-3-ethyl imidazol(e) bromine salt, 1,2-dimethyl-3-ethyl imidazol(e) villaumite, 1, at least one in 2-dimethyl-3-ethyl imidazol(e) tetrafluoroborate.
7. preparation method according to claim 1, it is characterized in that, in step (b), the described Graphene of choosing and the weight of ionic liquid mixture are 20～60g, the length and width size of described mould is respectively 200mm * 300mm, and described metal film is copper film or aluminium film.
8. Graphene/ionic liquid combination electrode that the arbitrary described preparation method of a claim 1 to 7 makes.
9. a capacitor, comprise by combination electrode, ionic liquid film, combination electrode in order the stacked battery core forming, for installing the closed shell of described battery core, and filling is at the electrolyte of closed shell, the one side that described compound electric pole piece does not spray described metal film contacts with described ionic liquid film, it is characterized in that, described compound electric pole piece is the prepared Graphene/ionic liquid combination electrode of claim 8.
10. capacitor according to claim 9, is characterized in that, described ionic liquid film adopts thin film coated device to be prepared from, and thickness is 3～10um, and length and width are 300mm * 200mm; The material of preparing described ionic liquid film is identical with the ionic liquid of selecting in described step (a).
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Application publication date: 20140326 |