CN103745834B - A kind of carbon nano-tube/poly pyrroles/graphite felt combination electrode and preparation method thereof - Google Patents
A kind of carbon nano-tube/poly pyrroles/graphite felt combination electrode and preparation method thereof Download PDFInfo
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- CN103745834B CN103745834B CN201410011800.3A CN201410011800A CN103745834B CN 103745834 B CN103745834 B CN 103745834B CN 201410011800 A CN201410011800 A CN 201410011800A CN 103745834 B CN103745834 B CN 103745834B
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Abstract
The invention discloses a kind of carbon nano-tube/poly pyrroles/graphite felt combination electrode and its preparation method and application, using oxidation pre-treatment graphite felt as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the mixed solution of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles, as electrolyte, utilizes electrochemistry cyclic voltammetric oxidative polymerization to prepare carbon nano-tube/poly pyrroles/graphite felt combination electrode.Combination electrode prepared by the present invention not only has higher ratio electric capacity and more excellent cyclical stability, and preparation condition is gentle, technique simple, it is controlled to operate, and has significant social and economic effects.
Description
Technical field
The invention belongs to the preparation field of electrode for super capacitor, be specifically related to a kind of carbon nano-tube/poly pyrroles/graphite felt combination electrode and its preparation method and application.
Background technology
Preparation is simple, it is reversible to adulterate, environmental friendliness, conductivity high, bigger than electric capacity, film property is excellent and receives much concern with it for polypyrrole.Meanwhile, nano-carbon material can improve mechanics and the electric property of polypyrrole further.P.M.Ajayan(P.M.Ajayan, O.Stephan, C.Colliex, D.Trauth.Science, 1994, 26:1212-1214), GaoyiHan(GaoyiHan, JinyingYuan, GaoquanShi, FeiWei.ThinSolidFilms, 2005, 474:64-69), HamedArami(HamedArami, MahyarMazloumi, RaziehKhalifehzadeh, ShahriarHojjatiEmami, S.K.Sadrnezhaad.MaterialsLetters, 2007, 61:4412-4415), Yeon-KyeongLee(Yeon-KyeongLee, Keum-JuLee, Dae-SungKim, Dong-JinLee, Jin-YeolKim.SyntheticMetals, 2010, 160:814-818) and J.Li(J.Li;H.Q.Xie, Y.Li.AdvancedMaterialsResearch, 2012,399-401:1415-1418) etc. be prepared for the multiple Pt/Polypyrrole composite material containing nano-carbon material.Research finds, the Pt/Polypyrrole composite material containing nano-carbon material has broad application prospects in the inverting element electrode material such as ultracapacitor, secondary cell field.
Polypyrrole combination electrode material containing nano-carbon material can be prepared by multiple method.E.Frackowiak(E.Frackowiak, V.Khomenko, K.Jurewicz, K.Lota, F.B é guin.JournalofPowerSources, 2006,153:413-418) find that the polypyrrole carbon nano tube compound material prepared by chemical method has excellent cyclical stability, in the voltage range of 0.4V, when cycle charge-discharge is more than 3000 cycles, can stably at 160F g than electric capacity-1.Ren Xiangzhong (Ren Xiangzhong, Zhao Qi, Liu Jianhong, Gu Yi. polymer material science and engineering, 2008,24(10) electrochemical process: 29-32) is adopted to synthesize PPy/MWCNT conductive composite film, it has been found that compared with pure PPy film, PPy/MWCNT conductive composite film surface is more coarse, loose, has more excellent electron transmission behavior.YuepingFang(YuepingFang, JianweiLiu, DeokJinYu, JamesP.Wicksted, KaanKalkan, C.OzgeTopal, BretN.Flanders, JudyWu, JunLi.JournalofPowerSources, 2010,195:674-679) by the method for pulse electrodeposition, polypyrrole painting is formed uniform thin film on the carbon nanotubes, obtain the MWCNT-PPy thin film of self-supporting, reach 427F g than electric capacity-1.Q.Fu(Q.Fu, B.Gao, H.Dou, L.Hao, X.Lu, K.Sun, J.Jiang, X.Zhang.SyntheticMetals, 2011,161:373-378) adopt the nano composite material of in-situ chemical route synthesis sulfonation multi-walled carbon nano-tubes and polypyrrole, it has been found that this material has stable ratio electric capacity, reaches 357F g-1, after the cycle charge-discharge in 1000 cycles, only lose 3% than electric capacity.
At present, Pt/Polypyrrole composite material containing nano-carbon material has good electric conductivity, stability, environment friendly and mechanical performance, but composite material preparation process is complicated, more relatively low than electric capacity, significantly limit its application on electrode material for super capacitor, it is still necessary to strengthen research further.
Summary of the invention
It is an object of the invention to provide a kind of carbon nano-tube/poly pyrroles/graphite felt combination electrode and its preparation method and application, combination electrode prepared by the present invention not only has higher ratio electric capacity and more excellent cyclical stability, and there is preparation condition gentleness, technique is simple, operate the advantages such as controlled, possesses significant social and economic effects.
For achieving the above object, the present invention adopts the following technical scheme that
A kind of carbon nano-tube/poly pyrroles/graphite felt combination electrode is using oxidation pre-treatment graphite felt as carrier, using CNT and DBSA radical ion codope polypyrrole as electrode operation material.
The method preparing carbon nano-tube/poly as above pyrroles/graphite felt combination electrode comprises the following steps:
(1) 20 ~ 200mg oxide/carbon nanometer tube (Xin Yudong, Liu Xiaodong are weighed；Cabonic acid oxidation modification. East China Institute of Technology's journal (natural science edition), 2010,33(1): 75-78) it is placed in 100mL deionized water, ultrasonic 1 ~ 10h, add DBSA and dodecylbenzene sodium sulfonate, ultrasonic 10 ~ 40min, controlling DBSA ion concentration in solution is 0.05 ~ 0.3mol/L；Adding pyrroles, the mol ratio controlling pyrroles and DBSA radical ion is 2 ~ 0.5:1, and ultrasonic 10 ~ 40min obtains the mixed solution of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles；
(2) adopting three-electrode system, with oxidation pre-treatment graphite felt, (Mulberry business is refined, Tan Ning, Liu Suqin, Chen Liquan for Li Xiaogang, Huang Kelong；Catalysis of graphite felt electrode treated with electrochemical oxidation VO2+/VO2 +Electricity to catalysis activity. functional material, 2006,37(7): 1084-1086) as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the mixed solution that step (1) prepares is as electrolyte, carry out electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range is-0.2V ~ 1.5V, and sweep speed is 10 ~ 100mV/s, and scan round 20 ~ 80 is enclosed, take out working electrode, repeatedly rinse with ethanol and deionized water, vacuum drying, obtain described carbon nano-tube/poly pyrroles/graphite felt combination electrode.
Described carbon nano-tube/poly pyrroles/graphite felt combination electrode is primarily adapted for use in and prepares ultracapacitor.
The preparation condition having the great advantage that the present invention of the present invention is gentle, technique is simple, it is controlled to operate, obtained high specific capacitance polypyrrole/graphite felt composite electrode is when charging and discharging currents density respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 809F/g, 617F/g, 468F/g and 354F/g, after discharge and recharge 1000 times, than capacitance fade 12.8%.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph (15000 times) of carbon nano-tube/poly pyrroles/graphite felt composite.
Fig. 2 is the scanning electron microscope (SEM) photograph (5000 times) of carbon nano-tube/poly pyrroles/graphite felt composite.
Fig. 3 is the scanning electron microscope (SEM) photograph (1000 times) of carbon nano-tube/poly pyrroles/graphite felt composite.
Detailed description of the invention
Embodiment 1
(1) preparation of the aqueous solution of the mixture of CNT, DBSA, dodecylbenzene sodium sulfonate and pyrroles: weigh 200mg oxide/carbon nanometer tube and be placed in 100mL deionized water, ultrasonic 10h, prepares finely dispersed carbon nano-tube aqueous solutions；Adding the mixture that mol ratio is the DBSA of 1:1 and dodecylbenzene sodium sulfonate, ultrasonic 20min in above-mentioned aqueous solution, controlling DBSA ion concentration in aqueous solution is 0.1mol/L；Weigh and be placed in above-mentioned aqueous solution with the pyrroles that DBSA radical ion mol ratio is 1:1, ultrasonic 20min, obtain the aqueous solution of the mixture of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles.
(2) preparation of carbon nano-tube/poly pyrroles/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) prepares is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range-0.2V ~ 1.5V, sweep speed 50mV/s, scan round 40 is enclosed, take out working electrode, repeatedly rinse with ethanol and deionized water, vacuum drying obtains using oxidation pre-treatment graphite felt as carrier, using CNT and DBSA radical ion codope polypyrrole as the combination electrode of electrode operation material, it is described high specific capacitance carbon nano-tube/poly pyrroles/graphite felt combination electrode.
The stereoscan photograph of carbon nano-tube/poly pyrroles/graphite felt composite is as Figure 1-3.It can be seen that the CNT of the about 60nm of diameter and the uniform compound of polypyrrole, meanwhile, CNT and Pt/Polypyrrole composite material are wrapped in again graphite felt fibres surface.
Using 0.5mol/L dilute sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 450F/g, 308F/g, 213F/g and 142F/g, after discharge and recharge 1000 times, than capacitance fade 23.2%.
Embodiment 2
(1) preparation of the aqueous solution of the mixture of CNT, DBSA, dodecylbenzene sodium sulfonate and pyrroles: weigh 120mg oxide/carbon nanometer tube and be placed in 100mL deionized water, ultrasonic 8h, prepares finely dispersed carbon nano-tube aqueous solutions；Adding the mixture that mol ratio is the DBSA of 1:1 and dodecylbenzene sodium sulfonate, ultrasonic 20min in above-mentioned aqueous solution, controlling DBSA ion concentration in aqueous solution is 0.1mol/L；Weigh and be placed in above-mentioned aqueous solution with the pyrroles that DBSA radical ion mol ratio is 1:1, ultrasonic 20min, obtain the aqueous solution of the mixture of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles.
(2) preparation of carbon nano-tube/poly pyrroles/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) prepares is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range-0.2V ~ 1.5V, sweep speed 50mV/s, scan round 40 is enclosed, take out working electrode, repeatedly rinse with ethanol and deionized water, vacuum drying obtains using oxidation pre-treatment graphite felt as carrier, using CNT and DBSA radical ion codope polypyrrole as the combination electrode of electrode operation material, it is described high specific capacitance carbon nano-tube/poly pyrroles/graphite felt combination electrode.
Using 0.5mol/L dilute sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 679F/g, 541F/g, 413F/g and 293F/g, after discharge and recharge 1000 times, than capacitance fade 15.2%.
Embodiment 3
(1) preparation of the aqueous solution of the mixture of CNT, DBSA, dodecylbenzene sodium sulfonate and pyrroles: weigh 80mg oxide/carbon nanometer tube and be placed in 100mL deionized water, ultrasonic 6h, prepares finely dispersed carbon nano-tube aqueous solutions；Adding the mixture that mol ratio is the DBSA of 1:1 and dodecylbenzene sodium sulfonate, ultrasonic 20min in above-mentioned aqueous solution, controlling DBSA ion concentration in aqueous solution is 0.1mol/L；Weigh and be placed in above-mentioned aqueous solution with the pyrroles that DBSA radical ion mol ratio is 1:1, ultrasonic 20min, obtain the aqueous solution of the mixture of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles.
(2) preparation of carbon nano-tube/poly pyrroles/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) prepares is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range-0.2V ~ 1.5V, sweep speed 50mV/s, scan round 40 is enclosed, take out working electrode, repeatedly rinse with ethanol and deionized water, vacuum drying obtains using oxidation pre-treatment graphite felt as carrier, using CNT and DBSA radical ion codope polypyrrole as the combination electrode of electrode operation material, it is described high specific capacitance carbon nano-tube/poly pyrroles/graphite felt combination electrode.
Using 0.5mol/L dilute sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 809F/g, 617F/g, 468F/g and 354F/g, after discharge and recharge 1000 times, than capacitance fade 12.8%.
Embodiment 4
(1) preparation of the aqueous solution of the mixture of CNT, DBSA, dodecylbenzene sodium sulfonate and pyrroles: weigh 40mg oxide/carbon nanometer tube and be placed in 100mL deionized water, ultrasonic 5h, prepares finely dispersed carbon nano-tube aqueous solutions；Adding the mixture that mol ratio is the DBSA of 1:1 and dodecylbenzene sodium sulfonate, ultrasonic 20min in above-mentioned aqueous solution, controlling DBSA ion concentration in aqueous solution is 0.1mol/L；Weigh and be placed in above-mentioned aqueous solution with the pyrroles that DBSA radical ion mol ratio is 1:1, ultrasonic 20min, obtain the aqueous solution of the mixture of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles.
(2) preparation of carbon nano-tube/poly pyrroles/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) prepares is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range-0.2V ~ 1.5V, sweep speed 50mV/s, scan round 40 is enclosed, take out working electrode, repeatedly rinse with ethanol and deionized water, vacuum drying obtains using oxidation pre-treatment graphite felt as carrier, using CNT and DBSA radical ion codope polypyrrole as the combination electrode of electrode operation material, it is described high specific capacitance carbon nano-tube/poly pyrroles/graphite felt combination electrode.
Using 0.5mol/L dilute sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 717F/g, 553F/g, 414F/g and 325F/g, after discharge and recharge 1000 times, than capacitance fade 11.3%.
Embodiment 5
(1) preparation of the aqueous solution of the mixture of CNT, DBSA, dodecylbenzene sodium sulfonate and pyrroles: weigh 20mg oxide/carbon nanometer tube and be placed in 100mL deionized water, ultrasonic 2h, prepares finely dispersed carbon nano-tube aqueous solutions；Adding the mixture that mol ratio is the DBSA of 1:1 and dodecylbenzene sodium sulfonate, ultrasonic 20min in above-mentioned aqueous solution, controlling DBSA ion concentration in aqueous solution is 0.1mol/L；Weigh and be placed in above-mentioned aqueous solution with the pyrroles that DBSA radical ion mol ratio is 1:1, ultrasonic 20min, obtain the aqueous solution of the mixture of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles.
(2) preparation of carbon nano-tube/poly pyrroles/graphite felt combination electrode: adopt three-electrode system, using oxidation pre-treatment graphite felt as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the aqueous solution that step (1) prepares is as electrolyte, utilize electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range-0.2V ~ 1.5V, sweep speed 50mV/s, scan round 40 is enclosed, take out working electrode, repeatedly rinse with ethanol and deionized water, vacuum drying obtains using oxidation pre-treatment graphite felt as carrier, using CNT and DBSA radical ion codope polypyrrole as the combination electrode of electrode operation material, it is described high specific capacitance carbon nano-tube/poly pyrroles/graphite felt combination electrode.
Using 0.5mol/L dilute sulfuric acid as electrolyte, record this combination electrode when charging and discharging currents density respectively 1g/A, 2g/A, 4g/A and 10g/A, than electric capacity respectively up to 625F/g, 476F/g, 363F/g and 287F/g, after discharge and recharge 1000 times, than capacitance fade 10.0%.
The foregoing is only presently preferred embodiments of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to the covering scope of the present invention.
Claims (2)
1. carbon nano-tube/poly pyrroles/graphite felt combination electrode, it is characterised in that: described combination electrode is using oxidation pre-treatment graphite felt as carrier, using CNT and DBSA radical ion codope polypyrrole as electrode operation material；Concretely comprising the following steps of preparation method:
Specifically comprise the following steps that
(1) weigh 20 ~ 200mg oxide/carbon nanometer tube and be placed in 100mL deionized water, ultrasonic 1 ~ 10h, add DBSA and dodecylbenzene sodium sulfonate, ultrasonic 10 ~ 40min, controlling DBSA ion concentration in solution is 0.05 ~ 0.3mol/L；Adding pyrroles, the mol ratio controlling pyrroles and DBSA radical ion is 2 ~ 0.5:1, and ultrasonic 10 ~ 40min obtains the mixed solution of oxide/carbon nanometer tube, DBSA, dodecylbenzene sodium sulfonate and pyrroles；
(2) three-electrode system is adopted, using oxidation pre-treatment graphite felt as working electrode, platinum filament is as to electrode, saturated calomel electrode is as reference electrode, the mixed solution that step (1) prepares is as electrolyte, carry out electrochemistry cyclic voltammetric oxidative polymerization, voltage scan range is-0.2V ~ 1.5V, sweep speed is 10 ~ 100mV/s, scan round 20 ~ 80 is enclosed, and takes out working electrode, repeatedly rinses with ethanol and deionized water, vacuum drying, obtains described carbon nano-tube/poly pyrroles/graphite felt combination electrode.
2. the application of carbon nano-tube/poly pyrroles/graphite felt combination electrode as claimed in claim 1, it is characterised in that: described carbon nano-tube/poly pyrroles/graphite felt combination electrode is used for preparing ultracapacitor.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4076900A (en) * | 1975-11-20 | 1978-02-28 | Compagnie Generale D'electricite S.A. | Sodium-sulphur type electric cell |
| CN103401008A (en) * | 2013-07-31 | 2013-11-20 | 华南理工大学 | Method and device for storing bioelectrical energy by virtue of capacitive anode |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4076900A (en) * | 1975-11-20 | 1978-02-28 | Compagnie Generale D'electricite S.A. | Sodium-sulphur type electric cell |
| CN103401008A (en) * | 2013-07-31 | 2013-11-20 | 华南理工大学 | Method and device for storing bioelectrical energy by virtue of capacitive anode |
Non-Patent Citations (1)
| Title |
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| "聚吡咯/多壁碳纳米管的合成及电化学行为";任祥忠等;《高分子材料科学与工程》;20081015;第24卷(第10期);第29-32页 * |
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