CN101740225B - Electrode of super capacitor and manufacturing method thereof - Google Patents
Electrode of super capacitor and manufacturing method thereof Download PDFInfo
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- CN101740225B CN101740225B CN2008101749002A CN200810174900A CN101740225B CN 101740225 B CN101740225 B CN 101740225B CN 2008101749002 A CN2008101749002 A CN 2008101749002A CN 200810174900 A CN200810174900 A CN 200810174900A CN 101740225 B CN101740225 B CN 101740225B
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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 an electrode of a super capacitor and a manufacturing method thereof. The manufacturing method comprises the following steps of: firstly, providing a polyacrylonitrile fiber textile, wherein the polyacrylonitrile fiber textile comprises a plurality of polyacrylonitrile fibers with the diameters about 50-500nm; then carrying out heat treatment on the polyacrylonitrile fiber textile to form a carbon fiber textile, wherein the carbon fiber textile comprises a plurality carbon fibers with the diameters about 50-500nm, the surfaces of the carbon fibers are provided with a plurality of nanometer holes with the apertures about 1-50nm, and the total areas of the nanometer holes account for about 85-95 percent of the total areas of the carbon fibers; and finally cutting the carbon fiber textile to manufacture the electrode of the super capacitor.
Description
Technical field
Relevant a kind of electrode of the present invention and preparation method thereof, and the electrode and preparation method thereof of relevant a kind of super capacitor particularly.
Background technology
Be accompanied by development of science and technology, get over strict for the requirement of all kinds of computers, communication and electronic product usefulness.For improving the usefulness of aforementioned various product, in the before-mentioned products capacitance of employed electric capacity and stability be bound to corresponding raising, therefore the appearance of super capacitor has just been arranged.
The structure of at present common super capacitor mainly comprises pair of electrodes and is poured into the electrolyte between the electrode.The capacitance of super capacitor depends primarily on the character of electrode.One of direction of therefore, how making great efforts for present industry with the capacitance of further raising super capacitor through the Continual Improvement of electrode process.
Summary of the invention
The purpose of this invention is to provide electrode of a kind of super capacitor and preparation method thereof.
A kind of manufacture method of electrode of super capacitor is proposed according to one aspect of the present invention.At first, the polyacrylonitrile fibre fabric is provided, this polyacrylonitrile fibre fabric has the polyacrylonitrile fibre that many diameters are about 50～500nm.Then, the polyacrylonitrile fibre fabric is heat-treated, make to form the fine fabric of carbon, wherein, the fine fabric of carbon comprises the carbon fiber that many diameters are about 50～500nm.The surface of carbon fiber has the nano-pore that a plurality of apertures are about 1～50nm, and the total surface area of nano-pore accounts for 85～95% of carbon fiber total surface area.Afterwards, carry out the cutting of the fine fabric of carbon to process the electrode of super capacitor.
A kind of electrode of super capacitor is proposed according to the present invention on the other hand.This electrode comprises the carbon fiber that many diameters are about 50～500nm.The surface of carbon fiber has the nano-pore that a plurality of apertures are about 1～50nm, and the total surface area of nano-pore accounts for 85～95% of carbon fiber total surface area.
The electrode of the super capacitor of made has quite excellent specific capacitance value according to the present invention, can improve the capacitance of the super capacitor of its made.
Description of drawings
For let above and other objects of the present invention, characteristic, advantage can be more obviously understandable, below conjunction with figs. is elaborated to preferred embodiment of the present invention, wherein:
Fig. 1 is the manufacture method flow chart that illustrates according to the electrode of the described super capacitor of one embodiment of the invention.
Fig. 2 is the sectional structural map that illustrates the electrode that has fine fabric of carbon and metal current collection layer in one embodiment of the invention.
Fig. 3 illustrates electrode resulting collection of illustrative plates after current constant discharges and recharges test.
Embodiment
The making of the electrode of super capacitor
Fig. 1 is the manufacture method flow chart that illustrates according to the electrode of the described super capacitor of one embodiment of the invention.At first, carry out step 110, the polyacrylonitrile fibre fabric is provided, this polyacrylonitrile fibre fabric can be weaved by polyacrylonitrile fibre and form.The diameter of aforementioned polyacrylonitrile fibre is about 50～500nm, and polyacrylonitrile fibre can be made via method of electrostatic spinning.
Then, carry out step 120, the polyacrylonitrile fibre fabric is heat-treated, make polyacrylonitrile fibre be reacted into carbon fiber and form the fine fabric of carbon.The fine fabric of carbon comprises the carbon fiber that diameter is about 50～500nm, and the surface of carbon fiber has the nano-pore that the aperture is about 1～50nm, and the total surface area of nano-pore accounts for 85～95% of carbon fiber total surface area.
Particularly, the heat treated step of aforementioned polyacrylonitrile fibre fabric comprises two stage heating stepses.At first, the polyacrylonitrile fibre fabric is heated to 200～300 ℃, and kept temperature 60～120 minutes, so that the polyacrylonitrile fibre fabric is carried out oxidation processes.Afterwards, heat with 800～1000 ℃ temperature again, and kept temperature 3～9 minutes, make to form the fine fabric of carbon.
After the fine fabric of aforesaid carbon completes, can directly carry out cutting of the fine fabric of carbon to process the electrode that super capacitor is used.Certainly, also can be as shown in Figure 1, carry out step 130, further on the fine fabric of carbon, form the metal current collection layer, have more low-impedance electrode with formation.
Please refer to Fig. 2, it is the sectional structural map that illustrates the electrode that has fine fabric of carbon and metal current collection layer in one embodiment of the invention.Electrode 200 has fine fabric 240 of carbon and metal current collection layer 250.The material of metal current collection layer 250 for example can be platinum, titanium, gold, silver, copper, aluminium, chromium, iron or aforesaid combination, and its generation type for example can be feasible modes such as applying, sputter.If adopt the mode of fitting to form metal current collection layer 250, will there be one deck following layer (not illustrating) between the fine fabric 240 of metal current collection layer 250 and carbon.
Example of making
It is said to according to the above embodiment of the present invention, and the fine fabric example of making of the carbon E1～E3 of the electrode making that is applied to super capacitor is provided.Wherein, the fibre diameter < 500nm in the employed polyacrylonitrile fibre fabric.The temperature of oxidation processes is about 260 ℃, and heating rate is about 2 ℃/>minute.The heating-up temperature of second stage is about 1000 ℃, keeps temperature-time to be respectively 3 minutes (E1), 6 minutes (E2) and 9 minutes (E3).
Specific surface area analysis
The fine fabric of the carbon that above-mentioned example of making E1～E3 accomplished carries out adsorption experiment respectively to analyze the specific area of the fine fabric of carbon.Show a series of fine fabric specific areas of measured carbon that go out.
Table one specific surface area analysis
| E1 | E2 | E3 | |
| Specific area (m 2/g) | 343 | 494 | 1104 |
Can know that by table one along with the raising (E1 v.s E2v.s E3) that keeps temperature-time in high-temperature process (e.g1000 ℃) process, specific area can obtain to improve.The raising of specific area can improve the capacitance of the super capacitor of follow-up made.
Be further to analyze the distribution scenario of the surface area on the fine fabric of carbon, the surface area of the fine fabric of further being accomplished with regard to example of making E3 of carbon is analyzed.By learning in analyzing that (specific area is 1104m to the fine fabric of E3 carbon
2/ g) in macropore (Kong Jing>Surface area 50nm) accounts for 10% long-pending (110.092m of the fine fabric face of carbon
2/ g).Because the surface area of the carbon fiber in the fine fabric of example of making E3 carbon mainly is the contribution that comes from the hole, therefore can further estimates and learn that (aperture is that 1～50nm) surface area contributed is about 90% to nano-pore.
Electrovolumetric analysis
The fine fabric of the carbon that above-mentioned example of making E1～E3 (1000 ℃ heat treatment time 3,6 and 9 minutes) is accomplished can further cut processing electrode, and in the three-pole electro-chemical systems, charges and discharge the capacitance of electrical method (galvanostatic charge and discharge method) and cyclic voltammetry (cyclic voltammetric method) measurement electrode respectively with current constant.
Reference electrode in the aforementioned three-pole electro-chemical systems (reference electrode) is saturated dried mercury electrode; Work electrode (working electrode) is the made electrode of the fine fabric of E1～E3 carbon, and comparative electrode (counterelectrode) is a graphite electrode.Electrolyte is the sulfuric acid solution of 1M.
Current constant discharges and recharges test
The made electrode of aforementioned example of making E1～E3 carries out current constant and discharges and recharges test in the three-pole electro-chemical systems, wherein employed electric current is 1mA, and the voltage range that discharges and recharges is 0～0.75V.
(I)
Fig. 3 illustrates electrode resulting collection of illustrative plates after current constant discharges and recharges test.By the collection of illustrative plates collocation formula I that test is obtained, can calculate the ratio capacitance of electrode.Wherein the C among the formula I is specific capacitance (F/g), and I is an electric current, and Δ T is the time difference, and Δ V is a potential difference, and m is test piece (electrode) weight.
Table two is that the electrode of listing the fine fabric made of E1～E3 carbon discharges and recharges the ratio capacitance that is drawn after the test through current constant.Wherein, the fine fabric of the carbon of example of making E1～E3 is distinctly processed three electrodes and is carried out three tests, and the specific capacitance value that three tests are obtained averages.
Table two current constant discharges and recharges test
Commercially available article 1: platform carbon scientific & technical corporation activated carbon fiber cloth
Commercially available article 2: select can carbon element scientific & technical corporation activated carbon fiber cloth
By can knowing in the table two, the electrode of the fine fabric made of example of making E1～E3 carbon discharges and recharges the average charge that test draws and is about 174～274F/g than capacitance via aforementioned currents is constant, and discharge is about 187～298F/g than capacitance.The made electrode of the fine fabric of example of making E1～E3 carbon significantly improves 70～170% compared to the ratio capacitance of commercially available article, has excellent specific capacitance value, can promote the capacitance of the super capacitor of follow-up making.
The cyclic voltammetry test
For further confirming the capacitance of the electrode that the fine fabric of aforementioned example of making E1～E3 carbon is made, be to adopt cyclic voltammetry to carry out the measured capacitance value of electrode.Wherein, the sweep speed in the cyclic voltammetry is 6mV/s, and the voltage of test is 0～0.75V.
Table three is ratio capacitances that the electrode of listing example of making E1～E3 made is drawn after the cyclic voltammetry test.Wherein, the fine fabric of the carbon of example of making E1～E3 is distinctly processed three electrodes and is carried out three tests, and the specific capacitance value that three tests are obtained averages.
The test of table three cyclic voltammetry
Can know that by table three electrode of the fine fabric made of example of making E1～E3 carbon is respectively 182F/g, 274F/g and 287F/g via the measured average discharge of cyclic voltammetry than capacitance, with the constant measured close in value of test that discharges and recharges of aforementioned currents.Via the result of cyclic voltammetry test, can reaffirm that the fine fabric made of example of making E1 of the present invention～E3 carbon electrode has the high specific capacitance value.
Though the present invention discloses as above with embodiment; Yet it is not in order to limit the present invention; Anyly be familiar with this technical staff; Do not breaking away from the spirit and scope of the present invention, when can doing various changes that are equal to or replacement, so protection scope of the present invention is when looking accompanying being as the criterion that the application's claim scope defined.
Claims (7)
1. the manufacture method of the electrode of a super capacitor comprises at least:
One polyacrylonitrile fibre fabric is provided, and this polyacrylonitrile fibre fabric has many polyacrylonitrile fibres that diameter is 50～500nm;
Direct heating this polyacrylonitrile fibre fabric to 200～300 ℃, and kept temperature 60～120 minutes, so that this polyacrylonitrile fibre fabric is carried out oxidation processes;
Further directly heat this polyacrylonitrile fibre fabric to 800～1000 ℃; And kept temperature 3～9 minutes; Make to form the fine fabric of carbon, wherein the fine fabric of this carbon comprises the many carbon fibers that diameter is 50～500nm, and described carbon fiber surface has a plurality of nano-pores that the aperture is 1～50nm; And the total surface area of described nano-pore accounts for 85～95% of described carbon fiber total surface area; And
Cut the fine fabric of this carbon to process this electrode.
2. the manufacture method of the electrode of super capacitor according to claim 1 is characterized in that described polyacrylonitrile fibre is to be made with method of electrostatic spinning.
3. the manufacture method of the electrode of super capacitor according to claim 1 is characterized in that also comprising formation one metal current collection layer on the fine fabric of this carbon.
4. the manufacture method of the electrode of super capacitor according to claim 3 is characterized in that this metal current collection layer is the surface that is formed at the fine fabric of this carbon with the mode of sputter.
5. the electrode of a super capacitor; Comprise diameter and be the fine fabric of carbon that the many carbon fibers of 50～500nm are formed; Wherein said carbon fiber surface has a plurality of nano-pores that the aperture is 1～50nm, and the total surface area of described nano-pore accounts for 85～95% of described carbon fiber total surface area.
6. the electrode of super capacitor according to claim 5 is characterized in that also comprising a metal current collection layer, is positioned on the described carbon fiber.
7. the electrode of super capacitor according to claim 6, the material that it is characterized in that this metal current collection layer are to be selected from by platinum, titanium, gold, silver, copper, aluminium, chromium, iron and group that aforesaid combination constituted.
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| CN2008101749002A CN101740225B (en) | 2008-11-11 | 2008-11-11 | Electrode of super capacitor and manufacturing method thereof |
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| CN2008101749002A CN101740225B (en) | 2008-11-11 | 2008-11-11 | Electrode of super capacitor and manufacturing method thereof |
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| CN101740225A CN101740225A (en) | 2010-06-16 |
| CN101740225B true CN101740225B (en) | 2012-04-25 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US8576541B2 (en) * | 2010-10-04 | 2013-11-05 | Corning Incorporated | Electrolyte system |
| KR20150032221A (en) * | 2013-09-17 | 2015-03-25 | 주식회사 아모그린텍 | Capacitive Deionization Electrode Module, Manufacturing Method thereof and Deionization Equipment using the Same |
| KR101655363B1 (en) * | 2013-11-21 | 2016-09-07 | 주식회사 아모그린텍 | Deionization Equipment |
| CN104240973A (en) * | 2014-09-22 | 2014-12-24 | 复旦大学 | Transparent flexible supercapacitor fabric and preparation method thereof |
| EP4075551A1 (en) * | 2019-12-10 | 2022-10-19 | Dalian Institute Of Chemical Physics, Chinese Academy Of Sciences | Electrode material having fiber structure, and preparation and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1354292A (en) * | 2001-12-10 | 2002-06-19 | 梁继选 | Continuous preparation method of active carbon fibre matting and cloth |
| US6413633B1 (en) * | 2001-04-18 | 2002-07-02 | Francis Patrick McCullough | Activated biregional fiber(s) |
| CN101290835A (en) * | 2007-04-16 | 2008-10-22 | 韩国科学技术研究院 | Electrode for supercapacitor and the fabrication method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6413633B1 (en) * | 2001-04-18 | 2002-07-02 | Francis Patrick McCullough | Activated biregional fiber(s) |
| CN1354292A (en) * | 2001-12-10 | 2002-06-19 | 梁继选 | Continuous preparation method of active carbon fibre matting and cloth |
| CN101290835A (en) * | 2007-04-16 | 2008-10-22 | 韩国科学技术研究院 | Electrode for supercapacitor and the fabrication method thereof |
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