KR101689479B1 - Active carbon for electrical-double-layer capacitor electrode and method for manufacturing the same - Google Patents
Active carbon for electrical-double-layer capacitor electrode and method for manufacturing the same Download PDFInfo
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- KR101689479B1 KR101689479B1 KR1020150144233A KR20150144233A KR101689479B1 KR 101689479 B1 KR101689479 B1 KR 101689479B1 KR 1020150144233 A KR1020150144233 A KR 1020150144233A KR 20150144233 A KR20150144233 A KR 20150144233A KR 101689479 B1 KR101689479 B1 KR 101689479B1
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- C01B31/08—
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- C01B31/083—
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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
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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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
Abstract
Description
The present invention relates to an activated carbon used for manufacturing an electrode included in an electric double layer capacitor and a method of manufacturing the same.
Activated carbon, which is used in the production of electrodes for electric double layer capacitors, is a key material of electrodes and occupies a large portion in terms of cost and performance of electric double layer capacitors.
Such activated carbon is prepared by a method of chemically activating a carbonaceous material such as petroleum coke or carbonized coconut with a solution of KOH, NaOH or the like, or activating it by passing it through water vapor at 900 to 1000 ° C.
However, there is a problem that the performance of the electric double layer capacitor is deteriorated due to presence of metal impurities or oxygen functional groups on the surface of the activated carbon. That is, metal impurities or oxygen functional groups present on the surface of activated carbon act as a factor causing a secondary chemical reaction when operating the electric double layer capacitor, thereby reducing the capacity of the electric double layer capacitor (deterioration in long-term lifetime performance).
In order to solve such problems, conventionally, there has been proposed a method of cleaning activated carbon with an acidic solution such as hydrochloric acid, sulfuric acid, nitric acid, etc. to remove metal impurities present on the surface of activated carbon, and then neutralizing the activated carbon. This method was effective in removing metal impurities existing on the surface of activated carbon. However, since oxygen functional groups such as carboxyl group, lactone group, phenol group and carbonyl group are generated during the cleaning process and the number of oxygen functional groups is increased on the surface of activated carbon, There was a limit in improving the performance of the capacitor. In addition, since the process of neutralization is additionally required, the production time and cost of activated carbon are increased.
The object of the present invention is to provide activated carbon for an electric double layer capacitor electrode in which the number of oxygen functional groups present on the surface is controlled in order to solve the above problems.
It is another object of the present invention to provide a method for producing activated carbon for the electric double layer capacitor electrode.
In order to achieve the above object, the present invention provides activated carbon for an electric double layer capacitor electrode having a surface oxygen concentration index of 0.08 or less.
Also, the present invention provides a method for producing a carbonaceous material, comprising the steps of: a) activating a carbonaceous raw material to produce a preliminarily activated carbon; b) washing the pre-activated carbon with ultrapure water; And c) heat-treating the pre-activated carbon washed with the ultrapure water in the presence of a mixed gas of a reducing gas and an inert gas. The present invention also provides a method of manufacturing activated carbon for an electric double layer capacitor electrode.
The present invention can provide an activated carbon for an electric double layer capacitor electrode in which the number of oxygen functional groups existing on the surface of activated carbon is controlled and the surface oxygen concentration index is low since activated carbon is produced through ultrapure water washing and reduction treatment.
Further, the present invention can provide an electric double layer capacitor having a high capacity, excellent cycle characteristics, and minimized self-discharge and leakage current because activated carbon having a low surface oxygen concentration index is applied to an electrode of an electric double layer capacitor.
1 is a reference diagram for explaining Experimental Example 2 of the present invention.
Hereinafter, the present invention will be described.
The present invention relates to an activated carbon used in the production of an electrode for an electric double layer capacitor and a method for producing the same, wherein the activated carbon of the present invention is characterized in that the number of oxygen functional groups present on the surface is controlled and the surface oxygen concentration index is low.
In general, when an electrode made of activated carbon containing metal impurities or oxygen functional groups is applied to an electric double layer capacitor, the performance of the electric double layer capacitor due to an incidental chemical reaction of metal impurities and / or oxygen functional groups during operation of the electric double layer capacitor There was a problem that it was deteriorated.
Accordingly, in order to remove metal impurities present in activated carbon, activated carbon was washed with an acidic solution and neutralized to adjust the pH to about 7 to 8 to prepare activated carbon. However, when activated carbon is washed with an acidic solution, an oxygen functional group such as a carboxyl group, a lactone group, a phenol group or a carbonyl group is generated ( Langmuir 2004, 20, 2233-2242, Journal of Hazardous Materials 2008, 159, 523-527 ) There is a problem that the oxygen concentration on the surface of the honeycomb structure increases. Accordingly, in order to lower the oxygen concentration of the activated carbon having the increased oxygen concentration on the surface, the activated carbon which has not been cleaned with the acid solution has to be heat-treated at a temperature higher than the heat treatment temperature. However, although the oxygen concentration can be lowered by the heat treatment as described above, the high heat treatment results in a problem that the capacity of the electric double layer capacitor is reduced.
That is, when the activated carbon is produced by the conventional method, an additional treatment process is required to remove the oxygen functional groups generated in the cleaning process, thereby decreasing the production efficiency of the activated carbon, and it is difficult to remove the oxygen functional groups even after the additional treatment process There is a limit in obtaining activated carbon having physical properties.
Accordingly, the present invention solves the problems of conventional methods by washing activated carbon with ultrapure water and performing reduction treatment, which will be described in detail as follows.
One. Electric double layer Activated carbon for capacitor electrodes
The activated carbon for the electric double layer capacitor electrode of the present invention (hereinafter referred to as 'activated carbon') has a surface oxygen concentration index of 0.08 or less (specifically, 0.01 to 0.07). The surface oxygen concentration index refers to the ratio (O1s / C1s) of peak intensity of C1s to peak intensity of C1s obtained by analyzing activated carbon by X-ray photoelectron spectroscopy (XPS). When the electrode made of activated carbon of the present invention having a surface oxygen concentration index of 0.08 or less is applied to the electric double layer capacitor, the cycle characteristics of the electric double layer capacitor can be improved, and the self discharge and leakage current can be remarkably reduced .
The specific surface area and the surface oxygen functional group of the present activated carbon of the present invention are not particularly limited. However, considering the performance of the electric double layer capacitor, the specific surface area is preferably 500 to 3000 m 2 / g and the surface oxygen functional group is preferably 0.4 meq / g or less .
2. Electric double layer Method for producing activated carbon for capacitor electrode
The present invention provides a method for producing the activated carbon. That is, the present invention provides a method for producing activated carbon having a low surface oxygen concentration index, that is, 0.08 or less, by controlling the number of oxygen functional groups existing on the surface.
a) Activation
First, the activated carbon is activated by activating the carbonaceous raw material. The carbonaceous raw material is not particularly limited, but includes, for example, petroleum coke, coal coke, pitch, carbonized plants (such as palm), synthetic resin Carbon nanotubes, carbon onions, and the like. The method for activating the carbonaceous raw material is not particularly limited, but examples thereof include chemical activation using KOH or NaOH, activation using high temperature steam, and the like.
On the other hand, the particle size of the preliminarily activated carbon is not particularly limited, but may be D 10 / D 50 / D 90 (1 to 4 μm / 5 to 11 μm / 12 to 20 μm).
b) Cleaning
The pre-activated carbon prepared above is washed with deionized water (> 10 MΩ · cm). The temperature of the ultrapure water is not particularly limited, but is preferably 60 to 80 ° C. If the cleaning temperature is less than 60 ° C, the cleaning effect of the pre-activated carbon may be deteriorated. If the cleaning temperature exceeds 80 ° C, the energy cost for maintaining the high temperature may increase. Also, it is preferable that the process of cleaning with ultra-pure water is performed from 1 to 3 times in consideration of the cleaning efficiency.
When the preliminarily activated carbon is washed with the ultra pure water, the metal impurity (for example, potassium) present in the preliminarily activated carbon can be efficiently removed without increasing the oxygen concentration of the preliminarily activated carbon.
On the other hand, it is preferable that the preliminary activated carbon cleaned with the ultrapure water is subjected to a drying process so that the heat treatment described below can be performed well.
c) Heat treatment
The pre-activated carbon cleaned with the ultrapure water is heat-treated in the presence of a mixed gas in which a reducing gas and an inert gas are mixed. When the preliminarily activated carbon is heat-treated in the presence of the mixed gas in which the reducing gas is mixed, a high reduction efficiency can be obtained even when the heat treatment is performed at a relatively low temperature. Specifically, the temperature for the heat treatment is not particularly limited, but is preferably 700 to 1300 ° C. The time for the heat treatment is not particularly limited, but is preferably 30 minutes to 2 hours.
On the other hand, the reducing gas is not particularly limited, but hydrogen is exemplified as a non-limiting example. The inert gas is not particularly limited, and examples thereof include nitrogen, helium, and argon. Here, the mixing ratio of the reducing gas and the inert gas is not particularly limited, but it is preferable that the hydrogen gas is 1 to 4% by volume and the inert gas is 96 to 99% by volume based on 100% by volume of the mixed gas.
The method for producing activated carbon of the present invention is characterized in that the step of washing with an acidic solution is excluded. That is, the present invention uses ultrapure water without using an acidic solution when cleaning the preliminary activated carbon, so that the present invention can control the number of oxygen functional groups present in the activated carbon to easily produce activated carbon having a low surface oxygen sensitivity index have.
Therefore, when the activated carbon is produced by the production method of the present invention, the time and cost consumed in manufacturing the activated carbon is reduced, which is economical. In addition, since activated carbon is washed using ultrapure water, waste water is not generated unlike the conventional method using an acidic solution, which is eco-friendly. In addition, since the pH of the activated carbon is neutralized by washing the activated carbon with ultra pure water, which is not an acidic solution, it is possible to minimize the corrosion of the current collector during the production of the electrode.
3. Electric double layer Electrodes for capacitors
The present invention provides an electrode for an electric double layer capacitor comprising the activated carbon. Specifically, the electrode for an electric double layer capacitor of the present invention includes a conductive material, a binder, and a current collector in addition to the above-described activated carbon.
The conductive material is not particularly limited as long as it is a material known in the art, and examples thereof include carbon black, graphite, and carbon nanotubes. The binder is not particularly limited as long as it is a material known in the art and includes, but not limited to, polytetrafluoroethylene (PTFE), carboxymethylcellulose (CMC), polyvinyl alcohol (PVA), polyvinylidene fluoride (PVDF), polyvinylpyrrolidone (PVP), methylcellulose , Styrene butadiene rubber (SBR), ethylene-vinyl chloride copolymer resin, vinylidene chloride latex, chlorinated resin, vinyl acetate resin, polyvinyl butyral, polyvinyl formal, bisphenol-based epoxy resin, butadiene rubber, isoprene rubber, nitrile butadiene Rubber, urethane rubber, silicone rubber, acrylic rubber and the like can be used.
Such an electrode for an electric double layer capacitor of the present invention is not particularly limited as long as it is a method known in the art.
4. Electric double layer Capacitor
The present invention provides an electric double layer capacitor including the electrode for the electric double layer capacitor. Specifically, the electric double layer capacitor of the present invention has a structure in which the above-described electrode is disposed as a cathode and an anode through a separator, and the anode and the anode are impregnated with the electrolyte.
Since the electric double layer capacitor of the present invention includes the electrode made of the activated carbon described above, it has a high capacity and excellent cycle characteristics, and the self discharge and leakage current are minimized.
Hereinafter, the present invention will be described in detail with reference to examples. However, the following examples are illustrative of the present invention, and the present invention is not limited by the following examples.
[ Example One]
The chemically activated petroleum coke was washed and filtered three times with ultra-pure water at 70 DEG C and then dried at 150 DEG C for 12 hours. At this time, the mixing ratio (weight ratio) of petroleum coke to ultrapure water was 3: 7, and the cleaning time was 30 minutes per one time. Then, the washed petroleum coke was heat-treated at 700 ° C for 1 hour in the presence of a mixed gas of 2 vol% of hydrogen and 98 vol% of nitrogen, thereby preparing activated carbon.
[ Example 2]
Activated carbon was prepared in the same manner as in Example 1 except that the washed petroleum coke was heat-treated at 850 ° C.
[ Example 3]
Activated carbon was prepared in the same manner as in Example 1, except that the washed petroleum coke was heat-treated at 1000 ° C.
[ Example 4]
The carbonized coconut was activated with water vapor and then washed and filtered three times with ultrapure water at 70 DEG C and dried at 150 DEG C for 12 hours. At this time, the mixing ratio (weight ratio) of coconut and ultrapure water was 3: 7, and the cleaning time was 30 minutes. The washed coconut was washed with 700 캜 For 1 hour to produce activated carbon.
[ Example 5]
Activated carbon was prepared in the same manner as in Example 4 except that the washed coconut was heat-treated at 850 ° C.
[ Example 6]
Activated carbon was prepared in the same manner as in Example 4 except that the washed coconut was heat-treated at 1000 ° C.
[ Comparative Example One]
The chemically activated petroleum coke was washed with 3% hydrochloric acid (HCl). Next, the petroleum coke washed with hydrochloric acid was washed and filtered three times with ultra-pure water at 70 ° C., and then dried at 150 ° C. for 12 hours to produce activated carbon.
[ Comparative Example 2]
The chemically activated petroleum coke was washed with 3% hydrochloric acid (HCl). Next, the petroleum coke washed with hydrochloric acid was washed and filtered three times with ultra-pure water at 70 DEG C, and then dried at 150 DEG C for 12 hours. Then, the dried coconut was heat-treated at 700 ° C for 1 hour in the presence of a mixed gas of 2% by volume of hydrogen and 98% by volume of nitrogen, thereby preparing activated carbon.
[ Experimental Example 1] Evaluation of physical properties of activated carbon
The properties of the activated carbon prepared in Examples 1 to 6 and Comparative Examples 1 and 2 were evaluated by the following methods. The results are shown in Table 1 below.
1. Specific surface area (m 2 / g): 0.5 g of activated carbon was dried at 200 ° C. for 12 hours to completely remove moisture in pores present on the surface of activated carbon and activated carbon, and adsorbed nitrogen (N 2 ) The amount of gas was measured.
2. Surface Oxygen Functional Group (meq / g): After mixing bases having different pKa values with activated carbon, react with acidic functional groups (carboxyl group, lactone group, phenol group) on the surface of activated carbon, (Base used: 0.1 N NaOH) to determine the amount by back-titration in solution.
3. Surface Oxygen Concentration Index (O1s / C1s): The ratio of the peak intensity of C1s to the peak intensity of O1s obtained by analyzing activated carbon made by X-ray photoelectron spectroscopy (analyzer: Thermo Scientific MultiLab 2000) was calculated.
Temperature
Functional group
Concentration index
Ultrapure water
Ultrapure water
Referring to Table 1, it can be confirmed that the specific surface area, surface oxygen functional group and surface oxygen concentration index of the activated carbon of Examples 1 to 6 are produced in the range required in the present invention.
[ Manufacturing example 1 to 6 and Comparative Manufacturing Example 1 to 2] Electric double layer Capacitor manufacturing
Acetylene black, a binder CMC (Carboxymethylcellulose) and SBR (Styrene Butadiene Rubber), prepared in Examples 1 to 6 and Comparative Examples 1 and 2, were mixed in a Planetary Mixer in a ratio of 90: 5: 1.5 : 3.5, and then mixed to prepare a slurry. The prepared slurry was comma coated on the Al foil to prepare an electrode. The electrode was wound with a separator (NKK, 35 μm thick pulp material) to produce a cylindrical electric double layer capacitor of 18Φ × 40 mm. At this time, 1M TEABF4 (tetraethylammonium tetrafluoroborate) contained in organic acetonitrile was used as the electrolyte solution.
[ Experimental Example 2] Electric double layer Evaluation of physical properties of capacitors
The properties of the electrical double-layer capacitors of Production Examples 1 to 6 and Comparative Production Examples 1 and 2 were evaluated by the following methods, and the results are shown in Table 2 below.
1. Cell capacity (F): The cell was charged to 2.7 V with a current of 0.5 A, followed by a constant voltage charge for 10 minutes and then discharged to 0 V with 0.5 A again. At this time, the capacity in the range of 80% to 40% of the discharge interval is referred to as a cell capacity, and is calculated by the following equation.
C (Capacitance) = discharge current (0.5 A) x (? Time) / (? Voltage)
2. High Temperature Storage (%): The cell was charged to 2.85 V and maintained at constant voltage charge at 85 C for 36 hours. Thereafter, the cell capacity was measured by cooling to room temperature, and the capacity retention ratio (%) with respect to the initial capacity was calculated.
3. Cycle characteristics (%): The cell was charged to 2.85 V and then cycled from a condition of 2.85 V to 1.425 V (half voltage) once per minute (see FIG. 1). The cycle condition was 10000 cycles at 85 ° C. After 10,000 cycles, the cells were cooled to room temperature, and the cell capacity was measured to calculate the capacity retention ratio (%) based on the initial capacity.
4. Self-discharge (ΔV): The cell was charged to 2.7 V and then subjected to a constant voltage charge at room temperature for 12 hours. Thereafter, it was left to discharge in the Rest mode for 12 hours, and the difference between the discharged voltage and the initial 2.7 V (Δ) was calculated.
5. Leakage current (mA): The cell was charged to 2.7 V and a constant voltage charge was applied for 12 hours at room temperature, and the applied current was measured at the end of 12 hours.
Referring to Table 2, it can be confirmed that the properties of the electric double layer capacitors are superior to those of Comparative Production Examples 1 and 2 in the case of using the activated carbon of the present invention.
Claims (10)
Wherein the surface oxygen concentration index is a ratio (O1s / C1s) of peak intensity of O1s to peak intensity of C1s obtained by analyzing the activated carbon by X-ray photoelectron spectroscopy.
b) washing the pre-activated carbon with ultrapure water; And
c) heat-treating the pre-activated carbon washed with the ultrapure water in the presence of a mixed gas of a reducing gas and an inert gas.
Wherein the step of cleaning the pre-activated carbon with an acidic solution is excluded.
Wherein the ultra pure water has a temperature of 60 to 80 占 폚.
Wherein the mixed gas is 1 to 4% by volume of hydrogen gas and 96 to 99% by volume of inert gas based on 100% by volume of the mixed gas.
Wherein the pre-activated carbon cleaned with the ultrapure water is heat-treated at a temperature of 700 to 1300 ° C.
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| KR1020150144233A KR101689479B1 (en) | 2015-10-15 | 2015-10-15 | Active carbon for electrical-double-layer capacitor electrode and method for manufacturing the same |
| CN201510810264.8A CN107021481A (en) | 2015-10-15 | 2015-11-20 | Activated carbon for electric double layer capacitor electrode and its manufacture method |
| JP2015240341A JP2017076767A (en) | 2015-10-15 | 2015-12-09 | Active carbon for electric double-layer capacitor electrode and manufacturing method of the same |
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| JP2001237149A (en) * | 1999-12-17 | 2001-08-31 | Honda Motor Co Ltd | Activated carbon for electric dipole layer capacitor |
| KR101311389B1 (en) * | 2012-04-16 | 2013-09-25 | 주식회사 동양탄소 | A method for preparing anthracite-based powdered activated carbon with high specific surface area from anthracites |
| JP5400892B2 (en) * | 2008-11-04 | 2014-01-29 | コーニング インコーポレイテッド | Method for producing porous activated carbon |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JPH07142295A (en) * | 1993-11-16 | 1995-06-02 | Fuji Elelctrochem Co Ltd | Electric double layer capacitor and manufacture of active carbon for its electrode |
| JP4762424B2 (en) * | 2001-03-12 | 2011-08-31 | 昭和電工株式会社 | Activated carbon, manufacturing method thereof, and electric double layer capacitor using the activated carbon |
| JP4392223B2 (en) * | 2003-10-31 | 2009-12-24 | Ｊｆｅケミカル株式会社 | Activated carbon manufacturing method and manufacturing apparatus thereof |
| JP2006024747A (en) * | 2004-07-08 | 2006-01-26 | Mitsubishi Gas Chem Co Inc | Carbon material for electric double-layer capacitor electrode, and its production method |
| JP2008195559A (en) * | 2007-02-09 | 2008-08-28 | Mitsubishi Gas Chem Co Inc | Activated carbon for electric double-layer capacitor electrode and method for producing the activated carbon |
| JP5676074B2 (en) * | 2008-10-31 | 2015-02-25 | 関西熱化学株式会社 | Method for reforming activated carbon |
| JP5246697B2 (en) * | 2008-12-05 | 2013-07-24 | 株式会社明電舎 | Method for manufacturing electrode for electric double layer capacitor |
| CN101700885B (en) * | 2009-11-04 | 2012-01-18 | 大连理工大学 | Method for preparing activated carbon with high specific surface area |
| JP2013157554A (en) * | 2012-01-31 | 2013-08-15 | Daihatsu Motor Co Ltd | Method of manufacturing electrode and electrode |
| US20120177923A1 (en) * | 2012-03-20 | 2012-07-12 | Haycarb PLC | Low ash activated carbon and methods of making same |
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- 2015-10-15 KR KR1020150144233A patent/KR101689479B1/en active IP Right Grant
- 2015-11-20 CN CN201510810264.8A patent/CN107021481A/en active Pending
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100204257B1 (en) * | 1995-10-02 | 1999-06-15 | 마스다 노부유키 | Heat treated activated carbon for denitration process for preparing the same method of denitration using the same and system of denitration using the same |
| JP2001237149A (en) * | 1999-12-17 | 2001-08-31 | Honda Motor Co Ltd | Activated carbon for electric dipole layer capacitor |
| JP5400892B2 (en) * | 2008-11-04 | 2014-01-29 | コーニング インコーポレイテッド | Method for producing porous activated carbon |
| KR101311389B1 (en) * | 2012-04-16 | 2013-09-25 | 주식회사 동양탄소 | A method for preparing anthracite-based powdered activated carbon with high specific surface area from anthracites |
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