CN103456508B - Method for manufacturing graphene composite electrode - Google Patents
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Abstract
The invention relates to the technical field of graphene, and provides a method for manufacturing a graphene composite electrode. The method includes steps of respectively providing poly(3,4-ethylenedioxythiophene), polystyrene sulfonate aqueous solution and aqueous solution dispersion containing graphene and cationic surfactants; immersing current collectors into polyethylenimine aqueous solution to obtain current collectors with surfaces which are subjected to charge processing; immersing the current collectors with the surfaces which are subjected to charge processing into the poly(3,4-ethylenedioxythiophene), the polystyrene sulfonate aqueous solution and aqueous solution dispersion containing the graphene and the cationic surfactants, and then sequentially immersing the current collectors into the poly(3,4-ethylenedioxythiophene), the polystyrene sulfonate aqueous solution and aqueous solution dispersion containing the graphene and the cationic surfactants again to obtain a graphene polymer modified electrode; drying the graphene polymer modified electrode under the vacuum condition at the temperature ranging from 100 DEG C to 180 DEG C to obtain the graphene composite electrode. The method has the advantages that a technology for manufacturing the graphene composite electrode is simple, operation is simple and feasible, and the graphene composite electrode can be easily manufactured on a large scale.
Description
Technical field
The invention belongs to energy storage device technical field, and in particular to a kind of preparation method of graphene combination electrode.
Background technology
Since strong K seas nurse (Andre K.Geim) of the peace moral of Univ Manchester UK etc. prepared stone in 2004
Black alkene material, widely payes attention to as its unique structure and photoelectric property receive people.Graphene is called material science
" nova " risen with Condensed Matter Physics field, its have many novel and the property of uniqueness and potential application are inhaled
Many scientific workers are drawn.Single-layer graphene has a big specific surface area, excellent conduction, heat conductivility and low thermal expansion
Coefficient, such as：1. high intensity, Young mole, (1,100GPa), fracture strength：(125GPa)；2. high heat conductance, (5,000W/
mK)；3. high conductivity, carrier transport rate, (200,000cm2/V*s)；4. high specific surface area, (calculated value：2,
630m2/g).Especially the nanoscale of its high connductivity property, big specific surface property and its monolayer two dimension is structural
Matter, can be used as electrode material in ultracapacitor and lithium ion battery.However, as the Ultrahigh of material with carbon element is limited, base
It is in the capacitive property of the ultracapacitor of grapheme material and unsatisfactory.
Conducting polymer polythiophene (PTh), has good photoelectric properties, with other conjugated polymers such as polyaniline
(PANI), polypyrrole (PPY) etc. has compared more preferable chemical stability.Especially its derivant poly- (3,4- ethylenedioxy thiophenes)
(PEDOT) with easily preparation, electro-chemical activity height, good electric conductivity and environmental stability, relative height ratio capacity etc. after doping
Advantage, has larger application in terms of ultracapacitor and li-ion electrode materials.But it also with other conducting polymers one
Sample, is inevitably present framing structure destructible, capacity attenuation obviously situation.
Usual ultracapacitor all positive and negative electrode pieces, the technique that tradition prepares electrode slice are complex, and add certain
Binding agent, increase the equivalent series resistance of electrode, in theory the maximum power density P of ultracapacitormax=V2/ 4R tables
Show, wherein V is the voltage of ultracapacitor, and R is the equivalent series resistance of ultracapacitor, reduces the power of ultracapacitor
Density.
The content of the invention
The technical problem to be solved is the defect for overcoming prior art, there is provided a kind of graphene combination electrode
Preparation method.
The present invention provides a kind of preparation method of graphene combination electrode, and which comprises the steps：
Poly- (3,4- ethylenedioxy thiophenes) is provided respectively:Poly styrene sulfonate aqueous solution, graphene-containing and cation form
The aqueous dispersion of face activating agent；
Collector is immersed in aq. polyethyleneimine, the collector that surface chargeization is processed is obtained；
The collector of surface chargeization process is immersed in into poly- (the 3,4- ethylenedioxy thiophenes):Polystyrene sulphur
In acid salt aqueous solution, then it is immersed in the aqueous dispersion of the graphene-containing and cationic surfactant, then successively
Repetition is immersed in poly- (the 3,4- ethylenedioxy thiophenes):Poly styrene sulfonate aqueous solution and the graphene-containing and sun from
The step of aqueous dispersion of sub- surfactant, obtain graphene polymer modified electrode；
The graphene polymer is vacuum dried at 100～180 DEG C, the graphene combination electrode is obtained.
The preparation method of the graphene combination electrode of the present invention, different from the preparation method of conventional electrodes piece, does not adopt viscous
Knot agent, therefore, it is possible to effectively reduce the contact internal resistance between collector and active material layer, and then reduces ultracapacitor
Equivalent series resistance, it is possible to increase power density；Additionally, its preparation process is simple, operating simple and feasible, and production cost
It is low, it is easy to accomplish batch production；Further, derivant of the present invention by Graphene with polythiophene is combined, and is realizing high specific volume
In the case of, it is effectively increased the stable circulation performance of composite.
Description of the drawings
Fig. 1 is the preparation technology flow chart of graphene combination electrode of the present invention.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, it is below in conjunction with drawings and Examples, right
The present invention is further elaborated.It should be appreciated that specific embodiment described herein is only to explain the present invention, and
It is not used in the restriction present invention.
The embodiment of the present invention provides a kind of preparation method of graphene combination electrode, as shown in figure 1, which includes following step
Suddenly：
S01：Poly- (3,4- ethylenedioxy thiophenes) is provided respectively:Poly styrene sulfonate aqueous solution, graphene-containing and sun from
The aqueous dispersion of sub- surfactant；
S02：Collector is immersed in aq. polyethyleneimine, the collector that surface chargeization is processed is obtained；
S03：The collector of surface chargeization process is immersed in into poly- (the 3,4- ethylenedioxy thiophenes):Polyphenyl second
In alkene sulfonic acid saline solution, then it is immersed in the aqueous dispersion of the graphene-containing and cationic surfactant, then
It is repeated in being immersed in poly- (the 3,4- ethylenedioxy thiophenes):Poly styrene sulfonate aqueous solution and the graphene-containing and
The step of aqueous dispersion of cationic surfactant, obtain graphene polymer modified electrode；
S04：The graphene polymer modified electrode is vacuum dried at 100～180 DEG C, the Graphene is obtained multiple
Composite electrode.
Specifically, in above-mentioned steps S01, poly- (3,4-ethylene dioxythiophene):Poly styrene sulfonate（PEDOT:PSS）
By commercially available acquisition, or can be prepared using existing method.Preferably, PEDOT:The concentration of PSS aqueous solutions be 0.1～
5mg/mL.Wherein, PEDOT:The preparation of PSS preferably adopts following step：
PSS is dissolved in the water, after being configured to the solution that concentration is 0.1～5mg/mL, EDOT monomers is added, wherein, PSS
Mol ratio with EDOT monomers is 1:1～2:1, stir 5～10 minutes, Deca hydrochloric acid, the pH value range of control system is 2～3.
Then the mol ratio of Deca Ammonium persulfate., Ammonium persulfate. and EDOT monomers is 1:1～2:1, quick 12～24h of stirring reaction, obtain
Obtain the PEDOT of 0.1～5mg/mL:PSS solution.
The preparation of the aqueous dispersion of graphene-containing and cationic surfactant is by Graphene and cationic surface
Activating agent is added to the water, 1～5h of ultrasonic disperse, forms Graphene of the surface with positive charge that concentration is 0.1～5mg/mL
Suspension.Wherein, the mass ratio of Graphene and cationic surfactant is 1:1～1:2.Preferably, the cationic surface
Activating agent is alcohol salt, quaternary ammonium salt surface active agent.Alcohol salt can be diethanol ammonium, triethanol ammonium.It is highly preferred that
The cationic surfactant is quaternary ammonium salt, this is because the dissolubility of quaternary ammonium salt is preferable.
Step S02 is specifically, after will be collection liquid surface process clean, being immersed in aq. polyethyleneimine, taking out, use
Water is rinsed and is dried up with nitrogen, obtains the collector that surface chargeization is processed, standby.Wherein, the collector is Copper Foil, aluminum
The sheet metals such as paper tinsel, nickel foil；The thickness of the collector is 6～20 μm；The concentration of the aq. polyethyleneimine is 1～5g/
L；The surface treatment can adopt following methods：By collector be sequentially placed in acetone, ethanol, water supersound process 20～
30min, is then cleaned with water, and nitrogen is dried up.
Step S03 is specifically, be immersed in poly- (3,4-ethylene dioxythiophene) by the collector of surface chargeization process:
In poly styrene sulfonate aqueous solution, take out after 5～20min, rinsed well with water, then dried up, be then immersed in the stone again
In the aqueous solution of black alkene and cationic surfactant, 5～20min is soaked, rinsed with water, then dried up, be repeated in being soaked in
PEDOT:The step of PSS and graphene-containing and aqueous solution of cationic surfactant active dispersion, repeat 3～10 times, obtain graphite
Alkene polymer modified electrode.
Step S04 specifically, the graphene polymer modified electrode is put in vacuum drying oven, at 100～180 DEG C
Lower vacuum drying, 0.5～2h are cooled to room temperature, rinse surface with water, are dried to obtain graphene combination electrode.
A kind of preparation method of graphene combination electrode provided in an embodiment of the present invention, which passes through electrostatic attraction and prepares stone
Black alkene combination electrode, electrode material are directly adsorbed on electrode by electrostatic attraction, can save the coating process of complexity, technique
Simply, and without binding agent, therefore, it is possible to effectively reduce the contact internal resistance between collector and active material layer, and then reduce
The equivalent series resistance of ultracapacitor, finally improves power density；By the compound of Graphene and PEDOT, realize it is high
In the case of specific capacitance, the stable circulation performance of composite can be effectively increased；Graphene combination electrode prepared by the method
Can be applicable in ultracapacitor and lithium ion cell electrode.
Implementing for the present invention is described in detail below in conjunction with specific embodiment.
Embodiment 1：
Prepare PEDOT:PSS aqueous solutions：PSS is dissolved in a certain amount of deionized water, concentration is configured to for 0.1mg/
The solution of mL, thereto Deca EDOT（Wherein PSS is 1 with the mol ratio of EDOT monomers:1）, it is slowly stirred 5 minutes, Deca salt
Acid, the pH value of control system is 2, is then slowly added dropwise Ammonium persulfate. [(NH4)2S2O8] solution, which is 1 with the mol ratio of EDOT:
1, quick stirring reaction 12h obtains the PEDOT/PSS solution of 0.1mg/mL.
Prepare the aqueous dispersion of Graphene and compositions comprising cationic surfactants：By Graphene and trimethyl
Ammonium chloride is 1 according to mass ratio:1 be added to distilled water in carry out ultrasonic disperse 1h, form Graphene concentration for 0.1mg/mL
The aqueous solution of Graphene and quaternary ammonium salt.
6 μm of Copper Foils are sequentially placed into into supersound process 20min in acetone, ethanol, secondary water, after processing totally, with a large amount of two
Secondary water is rinsed, and nitrogen is dried up, then soaks 10min during substrate sheet to be immersed in polyethyleneimine (PEI) aqueous solution of 1g/L, is carried out
Surface chargeization process, is rinsed and is dried up with nitrogen with secondary water after taking-up, standby.
Copper Foil after surface treatment is immersed in into PEDOT:In PSS aqueous solutions, take out after 5min, use a large amount of secondary waters
Rinse well, dried up with rubber pipette bulb.5min in the aqueous solution of Graphene and cationic surfactant is immersed in again, with a large amount of two
Secondary water is rinsed well, is dried up with rubber pipette bulb, completes the preparation of one layer graphene/PEDOT thin film, repeats above step 3 times, is prepared
Three layer graphenes adsorbed on collector/PEDOT thin film, obtain graphene polymer modified electrode.
The graphene polymer modified electrode of acquisition is put in vacuum drying oven, is vacuum dried at 100～180 DEG C
0.5h, is cooled to room temperature, rinses surface with water, is dried to obtain graphene combination electrode.
Embodiment 2：
Prepare PEDOT:PSS aqueous solutions：PSS is dissolved in a certain amount of deionized water, concentration is configured to for 5mg/mL
Solution, Deca EDOT thereto（The mol ratio of wherein PSS and EDOT is 2:1）, it is slowly stirred 10 minutes, Deca hydrochloric acid, controls
The pH value of system processed is 3, is then slowly added dropwise Ammonium persulfate. [(NH4)2S2O8] solution, which is 2 with the mol ratio of EDOT:1, soon
Fast stirring reaction 12h, obtains the PEDOT/PSS solution of 5mg/mL.
Prepare the aqueous dispersion of Graphene and compositions comprising cationic surfactants：By Graphene and triethanol ammonium according to matter
Amount is than being 1:1 be added to distilled water in carry out ultrasonic disperse 5h, formed Graphene concentration be 5mg/mL Graphene and three ethanol
The aqueous solution of ammonium.
20 μm of aluminium foils are sequentially placed into into supersound process 30min in acetone, ethanol, secondary water, after processing totally, with a large amount of two
Secondary water is rinsed, and nitrogen is dried up, then soaks 10min during substrate sheet to be immersed in polyethyleneimine (PEI) aqueous solution of 5g/L, is carried out
Surface chargeization process, is rinsed and is dried up with nitrogen with secondary water after taking-up, standby.
Copper Foil after surface treatment is immersed in into PEDOT:In PSS aqueous solutions, take out after 5min, use a large amount of secondary waters
Rinse well, dried up with rubber pipette bulb.5min is soaked in being immersed in the aqueous solution of Graphene and cationic surfactant again, with greatly
Amount secondary water is rinsed well, is dried up with rubber pipette bulb, completes the preparation of one layer graphene/PEDOT thin film, repeats above step 7 times,
Seven layer graphenes/PEDOT the thin film adsorbed on collector is prepared, graphene polymer modified electrode is obtained.
The graphene polymer modified electrode of acquisition is put in vacuum drying oven, is vacuum dried at 100～180 DEG C
2h, is cooled to room temperature, rinses surface with water, is dried to obtain graphene combination electrode.
Embodiment 3：
Prepare PEDOT:PSS aqueous solutions：PSS is dissolved in a certain amount of deionized water, concentration is configured to for 0.1mg/
The solution of mL, thereto Deca EDOT（The mol ratio of wherein PSS and EDOT is 2:1）, it is slowly stirred 7 minutes, Deca hydrochloric acid, controls
The pH value of system processed is 3, is then slowly added dropwise Ammonium persulfate. [(NH4)2S2O8] solution, which is 2 with the mol ratio of EDOT:1, soon
Fast stirring reaction 12h, obtains the PEDOT/PSS solution of 0.1mg/mL.
Prepare the aqueous dispersion of Graphene and compositions comprising cationic surfactants：By Graphene and diethanol ammonium according to matter
Amount is than being 2：1. ultrasonic disperse 1h is carried out in being added to distilled water, form Graphene and diethyl that Graphene concentration is 0.1mg/mL
The aqueous solution of alcohol ammonium.
20 μm of nickel foils are sequentially placed into into supersound process 20min in acetone, ethanol, secondary water, after processing totally, with a large amount of two
Secondary water is rinsed, and nitrogen is dried up, then soaks 30min during substrate sheet to be immersed in polyethyleneimine (PEI) aqueous solution of 5g/L, is carried out
Surface chargeization process, is rinsed and is dried up with nitrogen with secondary water after taking-up, standby.
Copper Foil after surface treatment is immersed in into PEDOT:In PSS aqueous solutions, take out after 20min, use a large amount of secondary
Water is rinsed well, is dried up with rubber pipette bulb.20min is soaked in being immersed in the aqueous solution of Graphene and cationic surfactant again,
Rinsed well with a large amount of secondary waters, dried up with rubber pipette bulb, complete the preparation of one layer graphene/PEDOT thin film, repeat above step
10 times, the ten layer graphenes/PEDOT thin film adsorbed on collector is prepared, obtain graphene polymer modified electrode.
The graphene polymer modified electrode of acquisition is put in vacuum drying oven, is vacuum dried at 100～180 DEG C
0.5h, is cooled to room temperature, rinses surface with water, is dried to obtain graphene combination electrode.
Performance detection：
Graphene combination electrode prepared by above-described embodiment 1～3 is carried out into roll-in, cut-parts, will roll-in to cross Graphene multiple
Composite electrode card punch breaks into the circular pole piece of a diameter of 10mm, correct amount.
The assembling of battery：Barrier film and electrolyte are assembled into into ultracapacitor according to cell making process, its septation is
Celgard 2000, electrolyte are 0.5mol/L H2SO4Solution, standing after being completed carries out a constant current charge-discharge test in,
Wherein voltage range is 0～2.0V, and electric current carries out constant current charge-discharge for 1A/g.
Table 1 is that graphene combination electrode prepared by embodiment 1～3 is used in capacitor carrying out the result of electro-chemical test,
Good performance is shown, with higher power density.
Table 1
| Embodiment 1 | Embodiment 2 | Embodiment 3 | |
| Power density kw/kg | 22.6 | 21.7 | 20.3 |
Presently preferred embodiments of the present invention is the foregoing is only, not to limit the present invention, all essences in the present invention
Any modification, equivalent and improvement made within god and principle etc., should be included within the scope of the present invention.
Claims (9)
1. a kind of preparation method of graphene combination electrode, it is characterised in that comprise the steps：
Poly- (3,4- ethylenedioxy thiophenes) is provided respectively:Poly styrene sulfonate aqueous solution, graphene-containing and cationic surface are lived
The aqueous dispersion of property agent；
Collector is immersed in aq. polyethyleneimine, the collector that surface chargeization is processed is obtained；
The collector of surface chargeization process is immersed in into poly- (the 3,4- ethylenedioxy thiophenes):Poly styrene sulfonate
In aqueous solution, then it is immersed in the aqueous dispersion of the graphene-containing and cationic surfactant, is then repeated in
It is immersed in poly- (the 3,4- ethylenedioxy thiophenes):Poly styrene sulfonate aqueous solution and the graphene-containing and cation form
The step of aqueous dispersion of face activating agent, obtain graphene polymer modified electrode；
The graphene polymer modified electrode is vacuum dried at 100～180 DEG C, the graphene combination electrode is obtained.
2. the preparation method of graphene combination electrode as claimed in claim 1, it is characterised in that poly- (3, the 4- ethylenes two
Oxygen thiophene):The concentration of poly styrene sulfonate aqueous solution is 0.1～5mg/mL；Graphene in the aqueous dispersion
Concentration is 1 for the mass ratio of 0.1～5mg/mL, the Graphene and cationic surfactant:1～2:1.
3. the preparation method of graphene combination electrode as claimed in claim 1, it is characterised in that the surface chargeization is processed
Collector be immersed in poly- (3,4- ethylenedioxy thiophenes):Time in poly styrene sulfonate aqueous solution is 5～20min；Institute
The collector for stating surface chargeization process is immersed in the aqueous dispersion of the graphene-containing and cationic surfactant
Time be 5～20min.
4. the preparation method of graphene combination electrode as claimed in claim 1, it is characterised in that obtain the Graphene polymerization
In the step of thing modified electrode, the collector is immersed in poly- (3,4-ethylene dioxythiophene):Poly styrene sulfonate water
In solution and be immersed in the graphene-containing and cationic surfactant aqueous dispersion number of repetition be 3～10
It is secondary.
5. the preparation method of graphene combination electrode as claimed in claim 1, it is characterised in that the cation surface activating
Agent is alcohol salt and/or quaternary ammonium salt.
6. the preparation method of the graphene combination electrode as described in claim 1 or 5, it is characterised in that the cationic surface
Activating agent is quaternary ammonium salt.
7. the preparation method of graphene combination electrode as claimed in claim 1, it is characterised in that poly- (3, the 4- ethylenes two
Oxygen thiophene):The preparation steps of poly styrene sulfonate aqueous solution are：
Poly styrene sulfonate is dissolved in the water, after being configured to the solution that concentration is 0.1～5mg/mL, 3,4- ethylenes two is added
Oxygen thiophene, obtains mixed solution, wherein, poly styrene sulfonate is 1 with the mol ratio of 3,4-ethylene dioxythiophene:1～2:1；
Stir the mixed solution 5～10 minutes, the pH value with acid adjustment mixed solution is 2～3, adds Ammonium persulfate., over cure
Sour ammonium is 1 with the mol ratio of 3,4- ethylenedioxy thiophenes:1～2:1, continue the stirring mixed solution, mixing time is 12～
24h, obtains poly- (3,4-ethylene dioxythiophene):Poly styrene sulfonate aqueous solution.
8. the preparation method of graphene combination electrode as claimed in claim 1, it is characterised in that the polyethyleneimine is water-soluble
The concentration of liquid is 1～5g/L, and the collector is immersed in the time in aq. polyethyleneimine for 5～10min.
9. the preparation method of graphene combination electrode as claimed in claim 1, it is characterised in that the vacuum drying time
For 0.5～2h.
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| JP6436101B2 (en) * | 2014-01-29 | 2018-12-12 | 日本ゼオン株式会社 | Electrode for electrochemical element and electrochemical element |
| CN104300111B (en) * | 2014-10-16 | 2017-02-15 | 佛山市盈通黑金碳材料股份有限公司 | Electrode material and preparation method of electrode material |
| CN105375035B (en) * | 2015-12-21 | 2018-03-20 | 东莞新能源科技有限公司 | A kind of collector, its preparation method and the lithium ion battery containing the collector |
| WO2018123778A1 (en) * | 2016-12-27 | 2018-07-05 | 東レ株式会社 | Method for manufacturing electrode material, electrode material, and electrode for secondary battery |
| CN109244418B (en) * | 2018-09-29 | 2021-02-05 | 湖北文理学院 | Surface-coated lithium ion battery positive electrode material, preparation method and lithium ion battery |
| CN110148750A (en) * | 2019-04-08 | 2019-08-20 | 东莞天予天正新能源科技有限公司 | A kind of cathode material of lithium ion battery and preparation method thereof |
| CN110320259A (en) * | 2019-07-11 | 2019-10-11 | 山西大学 | A kind of preparation method and application of aptamers electrochemical sensor |
| CN111370665A (en) * | 2020-03-19 | 2020-07-03 | 西安越遴新材料研究院有限公司 | Preparation method of high-specific-capacity multi-sheet-layer stacked silicon-carbon composite material |
| CN111431498B (en) * | 2020-03-31 | 2023-09-01 | 中国科学院宁波材料技术与工程研究所 | Conductive polymer solution for crystal resonator and application thereof |
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| CN101587778A (en) * | 2009-06-18 | 2009-11-25 | 天津大学 | Poly(3,4-ethylenedioxythiophene) aligned array layer thin-film electrode material and preparing method thereof |
| CN102484204A (en) * | 2009-11-26 | 2012-05-30 | Dic株式会社 | Material For Photoelectric Conversion Element, And Photoelectric Conversion Element |
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