CN105609329A - Positive/negative electrode material for high-performance asymmetric capacitor and preparation method for positive/negative electrode material - Google Patents
Positive/negative electrode material for high-performance asymmetric capacitor and preparation method for positive/negative electrode material Download PDFInfo
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- CN105609329A CN105609329A CN201610102304.8A CN201610102304A CN105609329A CN 105609329 A CN105609329 A CN 105609329A CN 201610102304 A CN201610102304 A CN 201610102304A CN 105609329 A CN105609329 A CN 105609329A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/48—Conductive polymers
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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
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Abstract
The invention relates to a positive/negative electrode material for a high-performance asymmetric capacitor. The positive electrode material is a high-specific-capacity ternary composite material: polyaniline/graphene oxide/multi-wall carbon nanotube; the negative electrode material is a potassium hydroxide activated GO/MWCNT composite material with a high specific surface area and high conductivity. An electrochemical test for the ternary positive electrode material can prove that the electrochemical performance of the ternary composite material is far better than that of a binary composite material; an electrochemical test for a simple asymmetric capacitor assembled by the negative electrode material also proves that a relatively good electrochemical performance is obtained; the preparation method is simple in process, and the raw materials are free of toxins and hazards; the microcosmic ternary structure of the obtained positive electrode material represents integrated characteristics, wherein GO provides sufficient specific surface areas and are loaded with polyaniline nanorods; the MWCNT coated with polyaniline is bridged between GO pieces; and the negative electrode material shows porous and loosening characteristics, so that the positive/negative electrode material has relatively bright application prospects in the capacitor electrode materials.
Description
Technical field
The present invention relates to the preparation field of nano composite material, in particular to the asymmetric capacitor of a kind of high-performancePositive and negative electrode material and preparation method thereof.
Background technology
In the new century, need badly efficiently, energy storage device solves by energy scarcity and people high-quality is lived easilyPursue the problem causing. Thereby picture lithium ion battery, the secondary cells such as ultracapacitor, because its energy conversion efficiency is high, justIn carrying, can repeatedly reuse and be favored. Than lithium ion battery, ultracapacitor is but more concerned, because itsHaving charge-discharge velocity faster, more permanent service life, more friendly to environment. Traditional double electric layers supercapacitorHave unrivaled power density, almost having irreplaceable effect in some fields endless service life, for example,Start and braking. But, because mainly relying on the energy storage mechanism of ionic adsorption, it determines the deficiency of its energy density, this also makes itApplication is restricted. Thereby nowadays, researcher mainly concentrates on energy another kind and has the more electric capacity of high-energy-densityDevice-fake capacitance device. The electrode material of fake capacitance device mainly relies on the energy storage of redox reaction mechanism, and this has brought energy densitySignificantly lifting, but also sacrificed power density, in addition because the electric conductivity of most of this capacitor electrode materialPoor, make this defect more obvious. Be exactly that symmetric capacitor working narrows in addition, and exist energy storage material profitBy the not high problem of rate, and asymmetric capacitor improves energy density by positive electrode, and negative material keeps power density,In supplying a gap, keep as far as possible the advantage of oneself, and combine the electromotive force window voltage of positive and negative electrode, make it suitableWith wider.
Thereby, utilize the fast positive electrode of a kind of high-energy-density of preparation of simple and easy method, a kind of high power density negativeUtmost point material is very significant.
Summary of the invention
The object of the present invention is to provide positive and negative electrode material of the asymmetric capacitor of a kind of high-performance and preparation method thereof.The method agents useful for same is cheaply easy to get, simple to operate, and repeatability is good. Carry out respectively electricity at the both positive and negative polarity electrode material to makingChemical characterization, and be assembled in the electrochemical Characterization after capacitor, good chemical property all obtained.
The present invention is achieved in that first the method obtains homodisperse GO/MWCNT solution, and then this basisAbove obtain positive electrode by in-situ polymerization aniline, KOH activation obtains negative material. Concrete steps are as follows:
(1) GO/MWCNT mixed solution preparation: the GO/MWCNT mixture that is 3:2 by 50-100mg mass ratio is scattered in 50-In 100mL deionized water, stir through 6-24h, then slight ultrasonic promotion is dispersed, and prevents GO fragmentation, thenLow-speed centrifugal is got clarified solution, obtains GO/MWCNT mixed solution;
(2) positive electrode-PANI/GO/MWCNT trielement composite material preparation: in the mixed solution that will obtain in step (1)Add 0.05-0.1g non-ionic surface active agent, stir it is dissolved, obtain substrate solution; Then by 0.5-1mL aniline listBody is dissolved in 25-50mL1M sulfuric acid, slowly adds in substrate solution and obtains growth solution; Take 1.25-2.5g over cureAcid ammonium is dissolved in 25-50mL1M sulfuric acid, transfers in separatory funnel, drips speed per second join growth solution with 2-4In, keep temperature is 0-5 simultaneouslyOC, after 6-8h, filters, centrifugal, the dry trielement composite material powder that obtains.
(3) negative material-KOH activation GO/MWCNT composite preparation: the mixed solution that will obtain in step (1)In add KOH solid, GO/MWCNT is wadded a quilt with cotton from solution heavy, through filtration, dry after mixing KOH solid, then lazyUnder property gas shield respectively to it 400OC calcines 0.5-1h, 800OC calcines 2.5-4h, and finally by overpickling, washing is dryThe dry product that obtains.
In the present invention, GO/MWCNT is mono-layer graphite oxide alkene/multi-walled carbon nano-tubes, PANI/GO/MWCNT be polyaniline/Mono-layer graphite oxide alkene/multi-walled carbon nano-tubes.
Tool of the present invention has the following advantages and good effect:
1. adsorb then growth in situ, PANI(polyaniline by monomer) at GO(mono-layer graphite oxide alkene) surperficial with nanometer suedeHair shape exists, and not only makes itself and GO adsorb more firm, strengthens stability, and has increased the overall specific area of material;
2. introduce MWCNT(multi-walled carbon nano-tubes) solve reduction GO and be easy to the problem of reuniting, ensure electric conductivity, in addition simultaneouslyMWCNT can also intert, and bridge joint composite various piece obtains an integrated structure;
3. gather materials on the spot, it is heavy that GO/MWCNT wads a quilt with cotton by KOH, and activation, had both ensured mixed effect homogeneous, do not introduce again that other is newImpurity, and with respect to conventional common carbon electrode, it shows more excellent chemical property.
4. this method is simple, and reagent is easy to get, favorable reproducibility, and can large-scale production.
Brief description of the drawings
Fig. 1 shows that positive and negative pole material of the present invention synthesizes simple process figure;
Fig. 2 shows positive electrode XRD collection of illustrative plates of the present invention;
Fig. 3 shows positive electrode XPS collection of illustrative plates of the present invention;
Fig. 4 shows positive electrode ac impedance spectroscopy in various embodiments of the present invention;
Fig. 5 shows positive electrode cyclic voltammetric collection of illustrative plates in various embodiments of the present invention;
Fig. 6 shows positive electrode constant current charge-discharge collection of illustrative plates in various embodiments of the present invention;
Fig. 7 shows the selected positive and negative pole material cyclic voltammetric of the present invention comparison diagram;
Fig. 8 shows the simple and easy capacitor schematic diagram of assembling;
Fig. 9 shows the different electromotive force window of capacitor testing cyclic voltammogram spectrum;
Figure 10 shows capacitor constant current charge-discharge collection of illustrative plates under different current densities;
Figure 11 shows the power density of capacitor and the relation of energy density;
Figure 12 shows capacitor stability.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail. Be understandable that, described hereinConcrete case study on implementation only for explaining the application, but not restriction to the application.
The present invention realizes schematic diagram as shown in Figure 1, and in deionized water, Monodispersed GO/MWCNT mixture, wherein,MWCNT interts, and bridges between GO lamella. For positive electrode, adopt the method for in-situ polymerization, and utilize π-π active force,To on GO lamella evenly, the closely polyaniline nano post of growth, and the MWCNT connecting material of being wrapped up by polyaniline each is smallLamella, not only strengthens electric conductivity, and makes it present integrated feature, and forms the increasing that three-dimensional structure has been brought specific areaAdd. For negative material, we gather materials on the spot, heavy to the wadding of GO/MWCNT mixed liquor by electrolyte, then with KOH activation,Obtain one and be uniformly dispersed, porous, the material of good conductivity.
Embodiment 1
(1) GO/MWCNT mixed solution preparation: the GO/MWCNT mixture that is 3:2 by 50mg mass ratio be scattered in 50mL go fromIn sub-water, stir through 12h, then slight ultrasonic 10min promotion is dispersed, and prevents GO fragmentation, then 2000r/Min low-speed centrifugal is got clarified solution, obtains GO/MWCNT mixed solution;
(2) positive electrode-PANI/GO/MWCNT trielement composite material preparation: in the mixed solution that will obtain in step (1)Add 0.1g non-ionic surface active agent PVP (polyvinylpyrrolidone (polyvinylpyrrolidone) be called for short PVP) orOP-10, stirs it is dissolved, and obtains substrate solution; Then 0.5mL aniline monomer is dissolved in 25mL1M sulfuric acid, slowSlowly add in substrate solution and obtain growth solution; Take 1.25g ammonium persulfate and be dissolved in 25mL1M sulfuric acid, transfer to pointIn liquid funnel, drip speed per second join in growth solution with 2-4, keep temperature is 0-5 simultaneouslyOC, after 6h, mistakeFilter, centrifugal, the dry trielement composite material powder PAGM that obtains. Its XRD as shown in Figure 2, has represented the feature of typical polyanilinePeak; As shown in Figure 3, oxygen element is that graphene oxide is introduced to XPS, and nitrogen element is that polyaniline is introduced. Illustrate that composite is prepared intoMerit.
(3) electrode preparation: the slurry preparing (proportioning is active material: conductive black: binding agent=8:1:1) is evenly coated withOverlay on (100 orders, 1*1cm) on stainless (steel) wire, through compressing, after being dried, obtain electrode, testing electrolyte used is 1M sulphurAcid. Its ac impedance measurement as shown in Figure 4, has represented obvious high frequency, intermediate frequency, and low frequency three parts, at HFS and real axisFocus and initial point approach be probably 1.5 ohm, illustrate that electrode internal resistance is lower, the electrode that therefore we prepare is reliable; InFrequently part is a semi-circular structure, and it is less that the electronics of less radius explanation electrode material shifts resistance; Low frequency part is and voidAlmost parallel curve of axle, illustrates that electrode material ion diffusional resistance is less. Cyclic voltammetry as shown in Figure 5, has represented poly-The more symmetrical characteristic peak of three couples of aniline, and the area that volt-ampere curve surrounds is larger, and the ratio electric capacity calculating is 696Fg-1(sweep speed is 20mVs-1). Constant current charge-discharge is tested as shown in Figure 6, compare little ohmmic drop, top and AC impedanceTest is echoed mutually, and discharge curve is more level and smooth, illustrates that electrode material internal structure is even, and discharge time is longer, further illustrates thisElectrode material has larger ratio electric capacity. (without the following electrode preparation method of specified otherwise all for this reason)
Embodiment 2
According to the reactions steps of embodiment 1 and process, just change the mixed liquor of GO/MWCNT into pure GO liquid, what obtain is compoundMaterial PAG. This routine its XRD of gained positive electrode PAG, XPS, as Fig. 2, shown in 3, little with PAGM difference, illustrate similarStructure, element composition. Its electrochemical Characterization, as Fig. 4, shown in 5,6, represents similar curvilinear structures to PAGM, has proved institute aboveState, provide good electric conductivity for no other reason than that lacked MWCNT, make poor compared to PAGM performance of its chemical property.
Embodiment 3
According to the reactions steps of embodiment 1 and process, just change the mixed liquor of GO/MWCNT into pure MWCNT liquid, obtainComposite PAM. This routine its XRD of gained positive electrode PAG, XPS, as Fig. 2, shown in 3, little with PAGM difference, phase has been describedLike structure, element composition. Its electrochemical Characterization, as Fig. 4, shown in 5,6, represents similar curvilinear structures to PAGM, before having provedDescribed in face, provide bigger serface for no other reason than that lacked GO, make poor compared to PAGM performance of its chemical property.
Embodiment 4
Negative material-KOH activation GO/MWCNT composite preparation: will add 50 in the mixed solution obtaining in step (1)MgKOH solid wads a quilt with cotton GO/MWCNT heavy from solution, through filtration, and the dry KOH solid that mixes again 300mg afterwards, thenUnder inert gas shielding respectively to it 400OC calcines 1h, 800OC calcines 3h, and finally by overpickling, washing and drying obtainsTo product A-GM. This routine its cyclic voltammetric of gained negative material A-GM characterizes as shown in Figure 7, has shown very symmetrical curve,And the area that curve surrounds is larger, the electric conductivity of the electrode material excellence of preparation is described, porosity and looseness has obtained larger ratio tableArea.
Embodiment 5
To the easily assembled capacitor PAGM//A-GM of positive and negative pole material, as shown in Figure 8. Because negative material is compared to positive electrodeMaterials are more, thus by it as for concentrically ringed outside. The capacitor electrode test chemical of assembling is as Fig. 9, and 10,11, shown in 12. ItsIn, explore the test of capacitor electromotive force window voltage as shown in Figure 9, show the electromotive force window electricity higher than independent positive and negative pole materialPress, reached 1.6V. Capacitor constant current charge-discharge is tested as shown in figure 10, has shown within the scope of compared with high current densityGood berth. In given current density range, power density, the relation of energy density as shown in figure 11, within the scope of this, is shownLarger power density, energy density. Capacitor job stability as shown in figure 12, after periodic duty 3000 times, can alsoKeep more than 85%, having shown good stability.
Above-described embodiment is illustrative principle of the present invention and effect only, but not for limiting the present invention. Any familiarThe personage of this technology all can, under spirit of the present invention and category, modify or change above-described embodiment. Therefore,Such as in affiliated technical field, have and conventionally know that the knowledgeable completes not departing under disclosed spirit and technological thoughtAll modifications or change, still covered by claim of the present invention.
Claims (8)
1. a preparation method for the positive electrode material of the asymmetric capacitor of high-performance, is characterized in that, comprises the following steps:
(1) GO/MWCNT mixed solution preparation: the GO/MWCNT mixture that is 3:2 by 50-100mg mass ratio is scattered in 50-In 100mL deionized water, through stirring, then slight ultrasonic promotion is dispersed, and prevents GO fragmentation, then low speed fromThe heart is got clarified solution, obtains GO/MWCNT mixed solution;
(2) positive electrode-PANI/GO/MWCNT trielement composite material preparation: in the mixed solution that will obtain in step (1)Add 0.05-0.1g non-ionic surface active agent, stir it is dissolved, obtain substrate solution; Then by 0.5-1mL aniline listBody is dissolved in 25-50mL1M sulfuric acid, slowly adds in substrate solution and obtains growth solution; Take 1.25-2.5g over cureAcid ammonium is dissolved in 25-50mL1M sulfuric acid, transfers in separatory funnel, drips speed per second join growth solution with 2-4In, keep temperature is 0-5 simultaneouslyOC, after 6-8h, filters, centrifugal, the dry trielement composite material powder that obtains.
2. preparation method according to claim 1, is characterized in that, in step (1), mixing time is 8-24h, when ultrasonicBetween be 5-10min.
3. preparation method according to claim 1, is characterized in that, the non-ionic surface active agent described in step (2)For PVP or OP-10.
4. the positive electrode material of the asymmetric capacitor of high-performance being made by method described in claim 1.
5. a preparation method for the negative electrode material of the asymmetric capacitor of high-performance, is characterized in that, comprises the following steps:
(1) GO/MWCNT mixed solution preparation: the GO/MWCNT mixture that is 3:2 by 50-100mg mass ratio is scattered in 50-In 100mL deionized water, through stirring, then slight ultrasonic promotion is dispersed, and prevents GO fragmentation, then low speed fromThe heart is got clarified solution, obtains GO/MWCNT mixed solution;
(2) negative material-KOH activation GO/MWCNT composite preparation: will add in the mixed solution obtaining in step (1)Enter KOH solid, GO/MWCNT is wadded a quilt with cotton from solution heavy, through filtering, after being dried, mix again KOH solid, then at indifferent gasUnder body protection respectively to it 400OC calcines 0.5-1h, 800OC calcines 2.5-4h, finally by overpickling, and washing and dryingObtain product.
6. preparation method according to claim 5, is characterized in that, described in step (2), adds for the first time KOH solid to be50-100mg, adding for the second time KOH solid masses is GO/MWCNT5-10 times.
7. preparation method according to claim 5, is characterized in that, the inert gas described in step (2) is nitrogen.
8. the negative electrode material of the asymmetric capacitor of high-performance being made by method described in claim 5.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106169379A (en) * | 2016-09-28 | 2016-11-30 | 唐山学院 | A kind of method preparing graphite paper/CNT graphene/polyaniline flexible compound electrode |
| CN106904697A (en) * | 2017-04-25 | 2017-06-30 | 上海丁香环境科技有限公司 | A kind of asymmetric capacitive deionization device preparation method of graphene-based electrode |
| CN109830684A (en) * | 2019-01-22 | 2019-05-31 | 东莞市创明电池技术有限公司 | Cell positive electrode and preparation method thereof and lithium ion battery |
| CN110289176A (en) * | 2019-02-25 | 2019-09-27 | 常州大学 | A kind of preparation method for the polyaniline grafted redox graphene/multi-wall carbon nano-tube composite material can be used for electrochemical energy storage |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106169379A (en) * | 2016-09-28 | 2016-11-30 | 唐山学院 | A kind of method preparing graphite paper/CNT graphene/polyaniline flexible compound electrode |
| CN106904697A (en) * | 2017-04-25 | 2017-06-30 | 上海丁香环境科技有限公司 | A kind of asymmetric capacitive deionization device preparation method of graphene-based electrode |
| CN106904697B (en) * | 2017-04-25 | 2019-07-19 | 上海丁香环境科技有限公司 | A kind of preparation method of the graphene-based electrode of asymmetry capacitive deionization device |
| CN109830684A (en) * | 2019-01-22 | 2019-05-31 | 东莞市创明电池技术有限公司 | Cell positive electrode and preparation method thereof and lithium ion battery |
| CN110289176A (en) * | 2019-02-25 | 2019-09-27 | 常州大学 | A kind of preparation method for the polyaniline grafted redox graphene/multi-wall carbon nano-tube composite material can be used for electrochemical energy storage |
| CN110289176B (en) * | 2019-02-25 | 2021-07-02 | 常州大学 | Preparation method of polyaniline grafted reduced graphene oxide/multi-walled carbon nanotube composite material for electrochemical energy storage |
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