CN102568848A - Preparation method of polyaniline/graphene oxide composite electrode material - Google Patents
Preparation method of polyaniline/graphene oxide composite electrode material Download PDFInfo
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- CN102568848A CN102568848A CN2011104314790A CN201110431479A CN102568848A CN 102568848 A CN102568848 A CN 102568848A CN 2011104314790 A CN2011104314790 A CN 2011104314790A CN 201110431479 A CN201110431479 A CN 201110431479A CN 102568848 A CN102568848 A CN 102568848A
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses a preparation method of polyaniline/graphene oxide composite electrode material, comprising the following steps: cleaning a stainless steel substrate; preparing a graphene oxide and aniline electrochemical deposition liquid; co-depositing the polyaniline/graphene oxide through the electrochemical cyclic voltammetry method by taking the stainless steel as a working electrode and adopting a three-electrode system, therefore, the polyaniline/graphene oxide composite electrode material is produced. The produced composite material has the advantages of high specific capacitance and good cycle stability and is suitable for the super capacitor electrode material.
Description
Technical field
The present invention relates to the preparation method of a kind of polyaniline/graphene oxide combination electrode material, belong to the energy storage material technical field.
Background technology
Electric chemical super capacitor is as a kind of novel energy-storing element, and is big because of its specific power, storage capacity strong, discharge and recharge that speed is fast, environmentally safe, advantage such as have extended cycle life have received widely and having paid close attention to.
People such as Hao are added to the alcohols dispersant for ultrasonic with graphite oxide and form uniform graphene oxide liquid mixture; Adding aniline again disperses; The solution of dropping oxidizing agent and inorganic acid in above-mentioned mixed liquor, low temperature stir polymerization down; Centrifugal, the washing after obtain graphene oxide/polyaniline composite material; In the water slurry of above-mentioned product, add concentrated base, heated and stirred is immersed in the composite material that obtains in the aqueous acid after the separation, separates drying and obtains graphene/polyaniline conductive composite material.
People such as Hualan Wang adopt the in-situ chemical polymerization to synthesize polyaniline and graphene oxide composite material.At first utilize Hummer method synthetic graphite olefinic oxide, the graphene oxide and the aniline monomer that obtain are mixed ultrasonic being uniformly dispersed in certain proportion, under intense stirring condition, slowly add oxidant.Keep above-mentioned solution ice bath stirring condition held one day, carry out chemical oxidising polymerisation and obtain polyaniline/graphene oxide composite material.Use the ratio electric capacity of the ultracapacitor of this Composite Preparation to be 531F/g, and the ratio capacitance of the polyaniline that the same terms prepares down have only 216F/g.(Wang?H?L，Hao?Q?L，Yang?X?J，et?al.Graphene?oxide?doped?polyaniline?for?supercapacitors[J].Electrochemistry?communications，2009，11(6)：1158-1161)。
Graphene oxide and aniline monomer system with in-situ polymerization in synthesized composite material; And performance excellent conducting performance (Tapas Kuilla; Sambhu Bhadra; Dahu Yao et al.Recent advances in graphene based polymer composites [J] .Progress in Polymer Science, 2010,35 (11): 1350-1375.).Because there is oxy radical on the graphene oxide surface, and specific area is big, makes it be easy to carry out compound with polyaniline.Bibliographical information chemical method synthesized polyaniline/graphene oxide composite material is arranged in recent years.Electrochemical co-deposition graphene oxide and polyaniline are adopted in this invention, and the result has improved the electrochemistry of polyaniline and recycled performance.
Summary of the invention
The object of the present invention is to provide the preparation method of a kind of polyaniline/graphene oxide combination electrode material, this preparation method's process is simple, quick and environmental protection.The combination electrode material that it makes has than the electric capacity height, and advantages such as good cycling stability are suitable for electrode material for super capacitor.
The present invention realizes through following technical proposals: a kind of polyaniline/graphene oxide combination electrode material; This composite material is substrate with the stainless steel; Through polyaniline and graphene oxide compound sedimentary deposit on the electrochemical cyclic voltammetry codeposition, it is characterized in that comprising following process in the substrate:
1. place ethanol and deionized water for ultrasonic to clean dry for standby in 60 ℃ of baking ovens respectively stainless steel substrate;
2. the preparation of electrochemical deposition liquid
Graphene oxide is scattered in the H of mass concentration 16-50%
2SO
4In the solution, being made into concentration is the graphene oxide electrochemical deposition liquid of 1-25mg/L, and then in this electrochemical deposition liquid, adds aniline monomer 9.2 μ L by every milliliter, and ultrasonic dispersion 1-3h obtains the electrochemical deposition liquid of graphene oxide and aniline;
3. electrochemical co-deposition polyaniline and graphene oxide layer
Stainless steel with after step 1 processing is a work electrode; Platinized platinum is to electrode; Saturated Ag/AgCl electrode is a reference electrode, under the condition of ice bath ,-0.1V～1.2V voltage range interscan speed is to carry out electrochemical deposition circulation 5-25 time under the 50mV/s cyclic voltammetric condition; Deposit on the stainless steel was dried 20-24 hour in 60 ℃ of baking ovens, obtain polyaniline/graphene oxide combination electrode material.
The present invention is because of using electrochemical production polyaniline/graphene oxide combination electrode material; Do not need high temperature, high vacuum condition and special reaction kit; Simple with other preparation method's comparative preparation processes of polyaniline/graphene combination electrode material, preparation cost is cheap.The electrochemical deposition polyaniline carries out when having realized doping and polymerization.And because conditions such as solution concentration in the pattern thickness of polyaniline graphene oxide composite membrane etc. and the electrochemical reaction and reaction time exist positive correlation, so can control the oxidation state and the thickness of composite membrane easily through simple regulation and control reaction solution concentration, polymerization potential and electric weight; In addition, resulting product need not to separate, and has saved vigorous stirring, filters step, relatively environmental protection of manufacturing process.
Description of drawings:
Fig. 1 is the cyclic voltammetry curve figure of the pure polyaniline that makes in Comparative Examples 1 of the present invention.
The cyclic voltammetry curve figure of the polyaniline that Fig. 2 makes for the embodiment of the invention 3/graphene oxide combination electrode material.
The cyclic voltammetry curve figure of the polyaniline that Fig. 3 makes for the embodiment of the invention 4/graphene oxide combination electrode material.
The polyaniline that Fig. 4 makes for the embodiment of the invention 3/graphene oxide combination electrode material SEM photo.
Embodiment
Providing 4 embodiment of the present invention below, is to further specify of the present invention, rather than limits scope of the present invention.
Embodiment 1:
Stainless steel substrate places ethanol and deionized water for ultrasonic to clean dry for standby in 60 ℃ of baking ovens respectively; Measure 15mL 2mg/L graphene oxide, be scattered in 15ml mass concentration 50%H
2SO
4In the solution, pipette aniline monomer 275 μ L in above-mentioned solution with liquid-transfering gun then, after ultrasonic being uniformly dispersed, adopt three-electrode system on electrochemical workstation, to carry out codeposition, wherein work electrode adopts the stainless steel electrode of above-mentioned processing, depositional area 1cm
2, to the electrodes use platinized platinum, reference electrode adopts saturated Ag/AgCl electrode.Under the condition of ice bath;-0.1V～1.2V voltage range interscan speed is to carry out electrochemical deposition circulation 10 times under the 50mV/s cyclic voltammetric condition; Deposit was dried one day in 60 ℃ of baking ovens; Utilize AL104 precise electronic balance weighing quality, measure the quality of the composite material that deposits on the stainless steel according to the variation of quality before and after the electro-deposition.Obtain polyaniline/graphene oxide combination electrode material.As work electrode, is to electrode with platinized platinum simultaneously with the gained composite material, and saturated Ag/AgCl electrode is constructed three-electrode system as reference electrode, at the H of 1M
2SO
4It has higher ratio electric capacity to this polyaniline/graphene oxide material through the cyclic voltammetric performance measurement in the solution.
Embodiment 2:
Stainless steel substrate places ethanol and deionized water for ultrasonic to clean dry for standby in 60 ℃ of baking ovens respectively; Measure 15mL 10mg/L graphene oxide, be scattered in 15ml mass concentration 50%H
2SO
4In the solution, pipette aniline monomer 275 μ L in above-mentioned solution with liquid-transfering gun then, after ultrasonic being uniformly dispersed, adopt three-electrode system on electrochemical workstation, to carry out codeposition, wherein work electrode adopts the stainless steel electrode of above-mentioned processing, depositional area 1cm
2, to the electrodes use platinized platinum, reference electrode adopts saturated Ag/AgCl electrode.Under the condition of ice bath;-0.1V～1.2V voltage range interscan speed is to carry out electrochemical deposition circulation 10 times under the 50mV/s cyclic voltammetric condition; Deposit was dried one day in 60 ℃ of baking ovens; Utilize AL104 precise electronic balance weighing quality, measure the quality of the composite material that deposits on the stainless steel according to the variation of quality before and after the electro-deposition.Obtain polyaniline/graphene oxide combination electrode material.As work electrode, is to electrode with platinized platinum simultaneously with the gained composite material, and saturated Ag/AgCl electrode is constructed three-electrode system as reference electrode, at the H of 1M
2SO
4It has higher ratio electric capacity to this polyaniline/graphene oxide material through the cyclic voltammetric performance measurement in the solution.
Comparative Examples 1
Stainless steel substrate places ethanol and deionized water for ultrasonic to clean dry for standby in 60 ℃ of baking ovens respectively; Pipette aniline monomer 275 μ L with liquid-transfering gun and be scattered in 15ml 50%H
2SO
4In the solution, after ultrasonic being uniformly dispersed, adopt three-electrode system on electrochemical workstation, to carry out codeposition, wherein work electrode adopts the stainless steel electrode of above-mentioned processing, depositional area 1cm
2, to the electrodes use platinized platinum, reference electrode adopts saturated Ag/AgCl electrode.Under the condition of ice bath;-0.1V～1.2V voltage range interscan speed is to carry out electrochemical deposition circulation 10 times under the 50mV/s cyclic voltammetric condition; Deposit was dried one day in 60 ℃ of baking ovens; Utilize AL104 precise electronic balance weighing quality, measure the quality of the composite material that deposits on the stainless steel according to the variation of quality before and after the electro-deposition.Obtain pure polyaniline electrode material.As work electrode, is to electrode with platinized platinum simultaneously with the gained material, and saturated Ag/AgCl electrode is constructed three-electrode system as reference electrode, at the H of 1M
2SO
4In the solution this polyaniline electrode material is carried out the cyclic voltammetric performance measurement.
Embodiment 3:
Stainless steel substrate places ethanol and deionized water for ultrasonic to clean dry for standby in 60 ℃ of baking ovens respectively; Measure 15mL 20mg/L graphene oxide, be scattered in 15ml 50%H
2SO
4In the solution, pipette aniline monomer 275 μ L in above-mentioned solution with liquid-transfering gun then, after ultrasonic being uniformly dispersed, adopt three-electrode system on electrochemical workstation, to carry out codeposition, wherein work electrode adopts the stainless steel electrode of above-mentioned processing, depositional area 1cm
2, to the electrodes use platinized platinum, reference electrode adopts saturated Ag/AgCl electrode.Under the condition of ice bath;-0.1V～1.2V voltage range interscan speed is to carry out electrochemical deposition circulation 10 times under the 50mV/s cyclic voltammetric condition; Deposit was dried one day in 60 ℃ of baking ovens; Utilize AL104 precise electronic balance weighing quality, measure the quality of the composite material that deposits on the stainless steel according to the variation of quality before and after the electro-deposition.Obtain polyaniline/graphene oxide combination electrode material.As work electrode, is to electrode with platinized platinum simultaneously with the gained composite material, and saturated Ag/AgCl electrode is constructed three-electrode system as reference electrode, at the H of 1M
2SO
4It has higher ratio electric capacity to this polyaniline/graphene oxide material through the cyclic voltammetric performance measurement in the solution.Circulate after 1000 times, stability is compared polyaniline and has been improved 50%.
Embodiment 4:
Stainless steel substrate places ethanol and deionized water for ultrasonic to clean dry for standby in 60 ℃ of baking ovens respectively; Measure 15mL 50mg/L graphene oxide, be scattered in 15ml 50%H
2SO
4In the solution, pipette aniline monomer 275 μ L in above-mentioned solution with liquid-transfering gun then, after ultrasonic being uniformly dispersed, adopt three-electrode system on electrochemical workstation, to carry out codeposition, wherein work electrode adopts the stainless steel electrode of above-mentioned processing, depositional area 1cm
2, to the electrodes use platinized platinum, reference electrode adopts saturated Ag/AgCl electrode.Under the condition of ice bath;-0.1V～1.2V voltage range interscan speed is to carry out electrochemical deposition circulation 10 times under the 50mV/s cyclic voltammetric condition; Deposit was dried one day in 60 ℃ of baking ovens; Utilize AL104 precise electronic balance weighing quality, measure the quality of the composite material that deposits on the stainless steel according to the variation of quality before and after the electro-deposition.Obtain polyaniline/graphene oxide combination electrode material.As work electrode, is to electrode with platinized platinum simultaneously with the gained composite material, and saturated Ag/AgCl electrode is constructed three-electrode system as reference electrode, at the H of 1M
2SO
4It has higher ratio electric capacity to this polyaniline/graphene oxide material through the cyclic voltammetric performance measurement in the solution.
Claims (1)
1. polyaniline/graphene oxide combination electrode material, this composite material is substrate with the stainless steel, through polyaniline and graphene oxide compound sedimentary deposit on the electrochemical cyclic voltammetry codeposition, it is characterized in that comprising following process in the substrate:
1). place ethanol and deionized water for ultrasonic to clean dry for standby in 60 ℃ of baking ovens respectively stainless steel substrate;
2). graphene oxide is scattered in the H of mass concentration 16-50%
2SO
4In the solution, being made into concentration is the graphene oxide electrochemical deposition liquid of 1-25mg/L, and then in this electrochemical deposition liquid, adds aniline monomer 9.2 μ L by every milliliter, and ultrasonic dispersion 1-3h obtains the electrochemical deposition liquid of graphene oxide and aniline;
3). the stainless steel with after the step 1) processing is a work electrode; Platinized platinum is to electrode; Saturated Ag/AgCl electrode is a reference electrode, under the condition of ice bath ,-0.1V～1.2V voltage range interscan speed is to carry out electrochemical deposition circulation 5-25 time under the 50mV/s cyclic voltammetric condition; Deposit on the stainless steel was dried 20-24 hour in 60 ℃ of baking ovens, obtain polyaniline/graphene oxide combination electrode material.
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| CN102760888A (en) * | 2012-07-16 | 2012-10-31 | 北京工业大学 | Preparation and application of graphene/substrate electrode and polyaniline-graphene/substrate electrode |
| CN102786705A (en) * | 2012-09-04 | 2012-11-21 | 江南大学 | Method for preparing graphene/polyaniline laminated films on basis of layer-by-layer self-assembly technique |
| CN102800493A (en) * | 2012-08-18 | 2012-11-28 | 中北大学 | Micro-capacitor with asymmetric 3D structure and producing method thereof |
| CN103310995A (en) * | 2013-06-08 | 2013-09-18 | 江苏悦达墨特瑞新材料有限公司 | Preparation method for composite nanomaterial of graphene and poly acetanilide nanowires |
| CN103367766A (en) * | 2013-07-31 | 2013-10-23 | 华南理工大学 | Preparation method for graphene/ conductive polymer anode for microbial fuel cell |
| CN103680973A (en) * | 2012-09-14 | 2014-03-26 | 海洋王照明科技股份有限公司 | Polyaniline/graphene/carbon nanotube composite and preparation method thereof, as well as electrode plate and capacitor |
| CN104211958A (en) * | 2014-09-19 | 2014-12-17 | 江苏科技大学 | Sulfonated graphene and polyaniline hybridized membrane and electrochemical preparation method thereof |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102220597A (en) * | 2011-05-20 | 2011-10-19 | 湖南大学 | Preparation method of conducting polymer-graphene composition |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102220597A (en) * | 2011-05-20 | 2011-10-19 | 湖南大学 | Preparation method of conducting polymer-graphene composition |
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| CN102800493B (en) * | 2012-08-18 | 2015-04-08 | 中北大学 | Micro-capacitor with asymmetric 3D structure and producing method thereof |
| CN102800493A (en) * | 2012-08-18 | 2012-11-28 | 中北大学 | Micro-capacitor with asymmetric 3D structure and producing method thereof |
| CN102786705A (en) * | 2012-09-04 | 2012-11-21 | 江南大学 | Method for preparing graphene/polyaniline laminated films on basis of layer-by-layer self-assembly technique |
| CN103680973A (en) * | 2012-09-14 | 2014-03-26 | 海洋王照明科技股份有限公司 | Polyaniline/graphene/carbon nanotube composite and preparation method thereof, as well as electrode plate and capacitor |
| CN103310995A (en) * | 2013-06-08 | 2013-09-18 | 江苏悦达墨特瑞新材料有限公司 | Preparation method for composite nanomaterial of graphene and poly acetanilide nanowires |
| CN103367766A (en) * | 2013-07-31 | 2013-10-23 | 华南理工大学 | Preparation method for graphene/ conductive polymer anode for microbial fuel cell |
| CN104681281B (en) * | 2013-12-02 | 2017-12-12 | 天津大学 | With excellent high rate performance combination electrode material and preparation method thereof |
| CN104681281A (en) * | 2013-12-02 | 2015-06-03 | 天津大学 | Composite electrode material having excellent rate performance and preparation method thereof |
| CN104211958A (en) * | 2014-09-19 | 2014-12-17 | 江苏科技大学 | Sulfonated graphene and polyaniline hybridized membrane and electrochemical preparation method thereof |
| CN104465121A (en) * | 2014-11-28 | 2015-03-25 | 天津大学 | Graphene oxide-polyaniline composite electrode material with three-dimensional structure and manufacturing method thereof |
| CN106783206B (en) * | 2014-11-28 | 2018-04-03 | 天津大学 | The preparation method of the graphene oxide polyaniline composite electrode material of three-dimensional structure |
| CN106449146A (en) * | 2014-11-28 | 2017-02-22 | 天津大学 | Application of three-dimensional oxidized graphene-polyaniline composite material in capacitor electrode material |
| CN104465121B (en) * | 2014-11-28 | 2017-05-03 | 天津大学 | Graphene oxide-polyaniline composite electrode material with three-dimensional structure and manufacturing method thereof |
| CN106783206A (en) * | 2014-11-28 | 2017-05-31 | 天津大学 | The preparation method of the graphene oxide polyaniline composite electrode material of three-dimensional structure |
| CN105905985B (en) * | 2016-04-18 | 2019-02-19 | 济南大学 | The preparation and application of a kind of GO/PEDOT:PSS applied to heterogeneous electric Fenton-like system modified graphite felt electrode |
| CN105905985A (en) * | 2016-04-18 | 2016-08-31 | 济南大学 | Preparation and application of GO/PEDOT:PSS modified graphite felt electrode applied to heterogeneous Electro-Fenton system |
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Application publication date: 20120711 |