CN103219163B - Super capacitor fiber electrode and preparation method thereof - Google Patents
Super capacitor fiber electrode and preparation method thereof Download PDFInfo
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- CN103219163B CN103219163B CN201310130090.1A CN201310130090A CN103219163B CN 103219163 B CN103219163 B CN 103219163B CN 201310130090 A CN201310130090 A CN 201310130090A CN 103219163 B CN103219163 B CN 103219163B
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- 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
Abstract
The invention discloses a kind of super capacitor fiber electrode and preparation method thereof, described fiber electrode comprises conductive fiber and is deposited on the multi-layer nano particle on described conductive fiber, in cavernous structure between multi-layer nano particle.The present invention adopts electrochemical deposition, and obtain the Graphene-carbon ball layer structure of a porous on the platinum wire surface that diameter is 100 microns, it possesses good double layer capacity effect, meets the requirement making fibrous super capacitor, and has extended cycle life.
Description
Technical field
The present invention relates to super capacitor technology field, particularly relate to a kind of super capacitor fiber electrode and preparation method thereof.
Background technology
Super capacitor is according to the difference of its energy storage mode, and super capacitor is divided into the mixing electric capacity of electric double layer capacitance, fake capacitance and above two kinds of electric capacity thereof, totally three kinds.Wherein, the electrode material of electric double layer super capacitor is mainly material with carbon element, comprises and mainly contains active carbon, carbon aerogels, carbon nano-tube and graphene oxide etc.As the electrode material of electric double layer capacitance, need to possess good conductivity and area large etc., and graphite just possesses such characteristic, therefore selects graphite as super capacitance electrode material.
In prior art, super capacitor electrode preparation method mainly comprises two kinds:
1. there is carbon ball (diameter 200 nanometer utilizing hydro thermal method to prepare, and surface is with negative electrical charge) carry out functionalization, make it positively charged, carry out self assembly with surface with the graphene oxide of negative electrical charge, obtain so a kind of material to prepare the super capacitor electrode sheet of sheet;
2. useful many carbon fibers soak in the ink, are directly used in the electrode of fibrous ultracapacitor.
Prior art mainly utilizes the mode of self assembly carbon ball, graphene oxide to be combined, then sandwich construction material is obtained by ultracentrifugal mode, by this structural applications to fiber surface, fibrous super capacitor can not be made, is suitable only for plate super capacitor.
Therefore, for above-mentioned technical problem, be necessary to provide a kind of super capacitor fiber electrode and preparation method thereof.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of super capacitor fiber electrode and preparation method thereof.
To achieve these goals, the technical scheme that provides of the embodiment of the present invention is as follows:
A kind of super capacitor fiber electrode, described fiber electrode comprises conductive fiber and is deposited on the multi-layer nano particle on described conductive fiber, in cavernous structure between multi-layer nano particle.
As a further improvement on the present invention, described conductive fiber comprises platinum wire and carbon fiber.
As a further improvement on the present invention, described nano particle comprises carbon ball and flake graphite alkene.
Correspondingly, a kind of preparation method of super capacitor fiber electrode, described method comprises:
First nano particle of S1, making surface band negative electrical charge;
S2, take some first nano particles, be scattered in alcohol, and carry out ultrasonic process;
Add the second nanoparticles solution comprised with negative electrical charge in S3, solution in step s 2, and carry out ultrasonic process;
S4, get solution in step S3 and be positioned in becket, soaked in the solution by conductive fiber, conductive fiber with becket are connected positive source and the after-applied direct current of negative pole respectively, reaction terminates rear taking-up conductive fiber, and room temperature is dried;
S5, the conductive fiber in step S4 to be soaked in hydroiodic acid, and to obtain fiber electrode after carrying out heating water bath.
As a further improvement on the present invention, also comprise after described step S2: in solution in step s 2, add pure water, and carry out ultrasonic process.
As a further improvement on the present invention, in described step S1, the first nanometer grain preparation method of surface band negative electrical charge comprises hydro thermal method.
As a further improvement on the present invention, described first nano particle is carbon ball, and the second nano particle is flake graphite alkene.
As a further improvement on the present invention, described conductive fiber comprises platinum wire and carbon fiber.
As a further improvement on the present invention, in described step S2 ~ S3, the time of ultrasonic process is 1 ~ 20 minute.
As a further improvement on the present invention, in described step S4, direct current is 1 ~ 20V, and direct current application time is 1 ~ 20 minute.
As a further improvement on the present invention, also comprise after described step S4: 60 degree of baking oven inner dryings 10 ~ 60 minutes.
As a further improvement on the present invention, in described step S5, water bath heating temperature is 98 degree, and the heating water bath time is 1 ~ 3 hour.Compared with prior art, the present invention adopts electrochemical deposition, and obtain the Graphene-carbon ball layer structure of a porous in the diameter conductive fiber surfaces that is 100 microns, it possesses good double layer capacity effect, meet the requirement making fibrous super capacitor, and have extended cycle life.
Accompanying drawing explanation
In order to be illustrated more clearly in the embodiment of the present invention or technical scheme of the prior art, be briefly described to the accompanying drawing used required in embodiment or description of the prior art below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings.
Fig. 1 is the structural representation of ring electric field generation device in an embodiment of the present invention;
Fig. 2 is the C-V curve of fiber electrode in one embodiment of the invention;
Fig. 3 is the GCD curve of fiber electrode in one embodiment of the invention;
Fig. 4 is the AC impedance curve of fiber electrode in one embodiment of the invention;
Fig. 5 is the loop test curve of fiber electrode in one embodiment of the invention.
Embodiment
Technical scheme in the present invention is understood better in order to make those skilled in the art person, below in conjunction with the accompanying drawing in the embodiment of the present invention, technical scheme in the embodiment of the present invention is clearly and completely described, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, should belong to the scope of protection of the invention.
The invention discloses a kind of fiber electrode being applied to super capacitor, fiber electrode comprises conductive fiber and is deposited on poroid, the multi-layer nano grain structure on conductive fiber.Wherein, conductive fiber can be platinum wire and carbon fiber or other conductive fibers, and the length of electrode is arranged by the ring electric field of the differing heights set up, and nano particle comprises carbon ball, flake graphite alkene etc.
The present invention is Applied Electrochemistry deposition mainly, obtains the graphite-olefinic carbon ball layer structure of a porous on the platinum wire surface that diameter is 100 microns.Preparation method comprises: the diameter due to hydro-thermal reaction making is the carbon ball of 200 ran, carbon ball surface band negative electrical charge, surface of graphene oxide is also with negative electrical charge, therefore under the effect of a ring electric field, graphene oxide and carbon ball all move to the platinum wire of positive pole, and be deposited on platinum wire surface, obtain porous, multilayer carbon ball, graphene oxide structure.
As shown in Figure 1, be connected with the negative pole of DC power supply 3 by an endless metal 1, platinum wire 2 is connected with the positive pole of power supply the generation device of ring electric field, thus sets up a ring electric field.Because carbon ball 4 and graphene oxide 5 surface are all with negative electricity, therefore, under the effect of electric field, access carbon ball, the graphene oxide structure of multilayer in positive pole platinum wire surface energy, then by chemical reduction method redox graphene, obtain fiber electrode.The present invention is not limited only to platinum wire, is that conductive fiber is just passable, also comprises carbon fiber etc.The length of electrode can be arranged by the ring electric field of the differing heights set up.Ball is also not limited only to carbon ball, and ball here can be conductor or non-conductor, makes it with negative electrical charge by functionalization.
The invention also discloses a kind of preparation method of super capacitor fiber electrode, the method specifically comprises:
First nano particle of S1, making surface band negative electrical charge;
S2, take some first nano particles, be scattered in alcohol, and carry out ultrasonic process.In present embodiment, the first nano particle is carbon ball;
Add the second nanoparticles solution comprised with negative electrical charge in S3, solution in step s 2, and carry out ultrasonic process.In present embodiment, the second nano particle is graphene oxide;
S4, get solution in step S3 and be positioned in becket, soaked in the solution by conductive fiber, conductive fiber with becket are connected positive source and the after-applied direct current of negative pole respectively, reaction terminates rear taking-up conductive fiber, and room temperature is dried.Wherein, conductive fiber can be platinum wire or carbon fiber etc.;
S5, the conductive fiber in step S4 to be soaked in hydroiodic acid, and to obtain fiber electrode after carrying out heating water bath.
Wherein, also comprise after step S2: in solution in step s 2, add pure water, and carry out ultrasonic process.This step is selected according to the difference of fiber quality, and electrochemical deposition needs this step, and electrophoresis does not then need this step.
In step S1, the first nanometer grain preparation method of surface band negative electrical charge comprises hydro thermal method and other group processing methods.In present embodiment, adopt hydro-thermal reaction that the first nano grain surface can be made with negative electrical charge.
Preferably, the time of ultrasonic process in step S2 ~ S4 is 1 ~ 20 minute; In step S5, direct current is 1 ~ 20V, and direct current application time is 1 ~ 20 minute; In step S6, water bath heating temperature is 98 degree, and the heating water bath time is 1 ~ 3 hour.
Further, also can comprise after step S5: 60 degree of baking oven inner dryings 10 ~ 60 minutes.
In a specific embodiment of the present invention, the preparation method of fiber electrode is specially:
S1, hydro-thermal reaction is utilized to make the carbon ball of 200 nanometer diameters;
S2, take 5mg carbon ball, be scattered in 10mL alcohol, ultrasonic 10 minutes;
S3, in above solution, add 1mL pure water ultrasonic 10 minutes;
S4, in above solution, add the graphene oxide solution 1mL of 5mg/mL, ultrasonic 10 minutes;
S5, get above solution 5mL and be positioned in the becket of experimental facilities, soaked wherein by platinum wire, logical DC10V voltage, after 10 minutes, take out platinum wire, room temperature is dried, 60 degree, baking oven, and half an hour is dry;
S6, hydroiodic acid redox graphene, be soaked in the hydroiodic acid in beaker by above fiber platinum wire electrode, 98 degree of water-baths, 2 hours, namely obtains fibrous flexible platinum wire fiber electrode.
Electrochemical workstation three-electrode system is utilized to test its C-V curve, GCD curve, AC impedance curve and loop test curve specific as follows:
Ginseng Figure 2 shows that C-V (Cyclicvoltammograms) curve of fiber electrode in above-mentioned execution mode, and in Fig. 2, the rectangular graph that is similar to from outside to inside represents shape appearance figure when sweep speed is 160mV/s, 80mV/s, 40mV/s, 20mV/s, 10mV/s, 5mV/s respectively.
As can be seen from C-V curve, under different sweep speeds, its pattern is close to rectangle, and obvious redox peak, does not illustrate that this fiber electrode has good electric double layer capacitance effect.
Ginseng Figure 3 shows that GCD (Galvanostaticcharge/discharge) curve of fiber electrode in above-mentioned execution mode.In Fig. 3, peak value curve from left to right represents current density is respectively 5 μ A (0.1mA/cm
2), 10 μ A (0.2mA/cm
2), 20 μ A (0.4mA/cm
2), 40 μ A (0.8mA/cm
2), 80 μ A (1.6mA/cm
2), 160 μ A (3.2mA/cm
2) time GCD curve chart.
Under different current densities, all curves all present linear and symmetrical state, illustrate that this fiber electrode has typical electric double layer capacitance electrode characteristic, and have the charging and discharging effects of becoming reconciled and reciprocally charge-discharge characteristic, have good capacity effect.
Ginseng Figure 4 shows that AC impedance EIS (Electrochemicalimpedancespectroscopy) curve of fiber electrode in above-mentioned execution mode.AC impedance can be defined as alternating voltage along this system with the ratio of alternating current flowing through this system, and namely AC impedance computing generally adopts Complex Number Method.Complex impedance can represent with real Z ' and imaginary part Z ' ', and namely abscissa Z ' and ordinate Z ' ' represents real part and the imaginary part of AC impedance respectively.
AC impedance is also one of main method of research chemical property, can evaluate its performance by impedance spectrum map analysis electrode for capacitors process.For desirable porous electrode, Nyquist curve is a straight line perpendicular to axis of abscissas, and for typical actual porous electrode, due to the uneven distribution of decentralized capacitance effect and hole electrolyte inside resistance, when applying high frequency ac signal to electrochemical system, electric double layer only can being formed close in the hole of electrode surface; Reduce with AC signal frequency, electrolyte ion is gradually toward electrode hole internal migration, and the real axis of Nyquist curve reduces gradually by the impact of frequency, finally shows as a straight line vertical with real axis.Like this, Nyquist curve is divided into three parts: Part I is the semicircle being positioned at high frequency region, the contact resistance of the intercept difference expression system of semicircle; Part II is positioned at intermediate frequency zone (Warburg impedance area), the general straight line in 45 ° of slopes, and it represents that electrolyte ion is at the intrapore diffusion resistance of electrode; Part III is be positioned at the low frequency range straight line vertical with axis of abscissas, and this part represents pure capacitance behavior.
ESI curve as can be seen from Fig. 4, curve has typical semicircle-rectilinear form, illustrates that fiber electrode is porous loose structure.In senior middle school frequency zones, there is semi-circular shape, in low frequency range, there is linear pattern.Semicircle explanation electrode has fine charge transport capability, illustrates that electrolyte has good diffusivity in the electrodes with real axis close to 45 degree of angle linear patterns.This fiber electrode is typical porous loose structure as seen from Figure 4.
Ginseng Figure 5 shows that the loop test curve of fiber electrode in above-mentioned execution mode.
Stability test is one of important indicator of electrode practicality.As can be seen from Figure 5, although there is the decay of about 7% in front 50 cycles, tend towards stability afterwards, after 2000 these cycle periods, pattern and the area thereof of C-V curve do not change substantially, and remain on the capacity of more than 90%, illustrate that electrode has good stability.
In sum, fiber electrode prepared by present embodiment has supercapacitor properties, may be used for super capacitor.
In other embodiments, the first nano particle and the second nano particle also can select metal or the inorganic particle of other surface band negative electrical charges.
In preparation process, the ultrasonic time in step S2 ~ S4 is set to 1 ~ 20 minute, also can obtain the test data similar with above-described embodiment; The temperature of oven drying temperature, drying time and heating water bath and heating time also can be different, can obtain the similar test data of above-described embodiment equally, can meet the electrology characteristic of electrode in super capacitor.
In addition, by changing the ratio of carbon ball and graphene oxide, the porosity of sandwich construction can also be controlled in other embodiments; By changing direct voltage and conduction time, the thickness of sandwich construction can be controlled.
As can be seen from the above technical solutions, the present invention adopts electrochemical deposition, and obtain the graphene oxide-carbon ball layer structure of a porous on the platinum wire surface that diameter is 100 microns, it possesses good double layer capacity effect, meet the requirement making fibrous super capacitor, and have extended cycle life.
To those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.Any Reference numeral in claim should be considered as the claim involved by limiting.
In addition, be to be understood that, although this specification is described according to execution mode, but not each execution mode only comprises an independently technical scheme, this narrating mode of specification is only for clarity sake, those skilled in the art should by specification integrally, and the technical scheme in each embodiment also through appropriately combined, can form other execution modes that it will be appreciated by those skilled in the art that.
Claims (11)
1. a super capacitor fiber electrode, it is characterized in that, described fiber electrode comprises conductive fiber and is deposited on the multi-layer nano particle on described conductive fiber, and described nano particle comprises carbon ball and flake graphite alkene, in cavernous structure between described multi-layer nano particle.
2. super capacitor fiber electrode according to claim 1, is characterized in that, described conductive fiber comprises platinum wire and carbon fiber.
3. a preparation method for super capacitor fiber electrode, described super capacitor fiber electrode is the super capacitor fiber electrode described in claim 1, it is characterized in that, comprises the following steps:
First nano particle of S1, making surface band negative electrical charge;
S2, take some first nano particles, be scattered in alcohol, and carry out ultrasonic process;
Add the second nanoparticles solution comprised with negative electrical charge in S3, solution in step s 2, and carry out ultrasonic process;
S4, get solution in step S3 and be positioned in becket, soaked in the solution by conductive fiber, conductive fiber with becket are connected positive source and the after-applied direct current of negative pole respectively, reaction terminates rear taking-up conductive fiber, and room temperature is dried;
S5, the conductive fiber in step S4 to be soaked in hydroiodic acid, and to obtain fiber electrode after carrying out heating water bath.
4. the preparation method of super capacitor fiber electrode according to claim 3, is characterized in that, also comprises after described step S2: add pure water in solution in step s 2, and carries out ultrasonic process.
5. the preparation method of super capacitor fiber electrode according to claim 3, is characterized in that, in described step S1, the first nanometer grain preparation method of surface band negative electrical charge comprises hydro thermal method.
6. the preparation method of super capacitor fiber electrode according to claim 3, is characterized in that, described first nano particle is carbon ball, and the second nano particle is flake graphite alkene.
7. the preparation method of super capacitor fiber electrode according to claim 3, is characterized in that, described conductive fiber comprises platinum wire and carbon fiber.
8. the preparation method of super capacitor fiber electrode according to claim 3, is characterized in that, the time of ultrasonic process in described step S2 ~ S3 is 1 ~ 20 minute.
9. the preparation method of super capacitor fiber electrode according to claim 3, is characterized in that, in described step S4, direct current is 1 ~ 20V, and direct current application time is 1 ~ 20 minute.
10. the preparation method of super capacitor fiber electrode according to claim 3, is characterized in that, also comprises after described step S4: 60 degree of baking oven inner dryings 10 ~ 60 minutes.
The preparation method of 11. super capacitor fiber electrode according to claim 3, is characterized in that, in described step S5, water bath heating temperature is 98 degree, and the heating water bath time is 1 ~ 3 hour.
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| CN104152971B (en) * | 2014-08-01 | 2018-06-01 | 天津工业大学 | A kind of method in insulation non-woven material surface deposition nano particle |
| CN105185600B (en) * | 2015-09-25 | 2018-05-15 | 东华大学 | A kind of method that electrophoresis prepares Graphene electrodes material |
| WO2019059238A1 (en) * | 2017-09-25 | 2019-03-28 | 国立大学法人千葉大学 | Porous conductor having conductive nanostructure and electricity storage device using same |
| CN110752095B (en) * | 2019-11-15 | 2020-11-10 | 重庆大学 | Method for synthesizing metal oxide array on conductive fiber, fiber structure metal oxide composite electrode and application |
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| CN101661839A (en) * | 2009-09-11 | 2010-03-03 | 华东师范大学 | Metal fiber-nanometer carbon fiber-carbon aerogel composite material and preparation method and use thereof |
| CN102509643A (en) * | 2011-11-29 | 2012-06-20 | 西北师范大学 | Graphene/carbon ball composite material, and preparation and application thereof |
| CN102544459A (en) * | 2012-01-09 | 2012-07-04 | 上海交通大学 | Method for preparing graphene-coated carbon microsphere material by coating graphene oxide on carbon microsphere |
| CN103003902A (en) * | 2010-06-15 | 2013-03-27 | 应用奈米结构公司 | Electrical devices containing carbon nanotube-infused fibers and methods for production thereof |
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| CN101661839A (en) * | 2009-09-11 | 2010-03-03 | 华东师范大学 | Metal fiber-nanometer carbon fiber-carbon aerogel composite material and preparation method and use thereof |
| CN103003902A (en) * | 2010-06-15 | 2013-03-27 | 应用奈米结构公司 | Electrical devices containing carbon nanotube-infused fibers and methods for production thereof |
| CN102509643A (en) * | 2011-11-29 | 2012-06-20 | 西北师范大学 | Graphene/carbon ball composite material, and preparation and application thereof |
| CN102544459A (en) * | 2012-01-09 | 2012-07-04 | 上海交通大学 | Method for preparing graphene-coated carbon microsphere material by coating graphene oxide on carbon microsphere |
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