CN101278365A - Carbonaceous material for electric double layer capacitor and electric double layer capacitor - Google Patents
Carbonaceous material for electric double layer capacitor and electric double layer capacitor Download PDFInfo
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- CN101278365A CN101278365A CNA2006800360301A CN200680036030A CN101278365A CN 101278365 A CN101278365 A CN 101278365A CN A2006800360301 A CNA2006800360301 A CN A2006800360301A CN 200680036030 A CN200680036030 A CN 200680036030A CN 101278365 A CN101278365 A CN 101278365A
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- carbon
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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
Disclosed is a carbon material for electric double layer capacitors which exhibits excellent charge/discharge characteristics. Also disclosed is an electric double layer capacitor. Specifically disclosed is a carbon material for electric double layer capacitors which is characterized by having a BET specific surface area of 300-1000 m<2>/g, a distance between carbon layers of 0.360-0.380 nm, and a carbon intensity of not less than 2000 cps. This carbon material enables to form an electric double layer capacitor having such characteristics as high capacitance and low internal resistance. Also specifically disclosed is an electric double layer capacitor wherein such a carbon material is used as a polarizable active material. This electric double layer capacitor exhibits high capacitance and low internal resistance.
Description
Technical field
The present invention relates to material with carbon element, this material with carbon element is used for the polarizable active material in the double electric layer capacitor.
Background technology
Recently, developed the double electric layer capacitor that shows the internal resistance reduction and have the capacitance of increase.Expectation always is applied to for example such power supply purposes (power usage) of motor vehicle with this double electric layer capacitor.Double electric layer capacitor based on principle be, placing a pair of polarizable electrode consequently faces one another in electrolyte solution, dividing plate inserts therebetween to form positive electrode and negative electrode, make electric charge accumulate in the electric double layer, this electric double layer is formed in the interface between positive electrode and negative electrode (being polarizable electrode) and the electrolyte solution.
This double electric layer capacitor for example is disclosed in, and Japanese unexamined patent publication No. discloses among (spy opens) No.H11-317333, No.2002-25867 and the patent disclosure No.3689948.
The spy opens H11-317333 and discloses the double electric layer capacitor that uses the material with carbon element of the microcrystalline carbon that comprises similar graphite.Described material with carbon element obtains by activation processing.The interfloor distance of described microcrystalline carbon is the scope of 0.365nm-0.385nm.
The spy opens No.2002-25867 and discloses the double electric layer capacitor that uses the Karbate of the microcrystalline carbon that comprises similar graphite, and described microcrystalline carbon has 270m
2/ g or littler specific area and the interfloor distance d of microcrystalline carbon
002Be 0.360-0.380nm.
Patent No.3689948 discloses a kind of double electric layer capacitor, this capacitor comprises, negative electrode with polarizable electrode material, described polarizable electrode material mainly is made up of activated carbon, anode with material with carbon element, on described material with carbon element, can occlusion or desorb lithium ion and contains the non-aqueous electrolytic solution of lithium salts by described material with carbon element by chemical method or electrochemical method occlusion for lithium ion.
Yet the problem of existence is that the disclosed capacitor that is made by the material with carbon element that is used for double electric layer capacitor has big internal resistance among the No.H11-317333 by opening the spy.And has poor electrolyte solution diffusivity by open the disclosed material with carbon element that is used for double electric layer capacitor makes among the No.2002-25867 capacitor little specific area the spy owing to material with carbon element.Therefore, the problem of existence is that it is big that the resistance between electrolyte solution and the material with carbon element becomes, and internal resistance increases.
Summary of the invention
The present invention considers that above-mentioned condition carries out.Therefore the purpose of this invention is to provide material with carbon element that is used for double electric layer capacitor and the double electric layer capacitor (having big capacitance and little internal resistance) that can show excellent charging and discharge performance.As the result of study that addresses the above problem, the inventor has finished the invention about the material with carbon element that is used for double electric layer capacitor.
The invention provides the material with carbon element that is used for double electric layer capacitor, this material with carbon element has:
At 300-1000m
2The BET specific area of/g scope,
The interfloor distance of the carbon of 0.360-0.380nm scope and
2000cps or bigger carbon intensity.
In addition, the material with carbon element that comprises of double electric layer capacitor according to the present invention has:
At 300-1000m
2The BET specific area of/g scope,
The interfloor distance of the carbon of 0.360-0.380nm scope and
2000cps or bigger carbon intensity.
Embodiment
Hereinafter, though be called execution mode, the present invention will be described more specifically.
(execution mode)
(material with carbon element that is used for double electric layer capacitor)
The material with carbon element that is used for double electric layer capacitor according to the present invention is the material with carbon element as the polarizable active material of double electric layer capacitor.
The material with carbon element that is used for double electric layer capacitor according to the present invention has the interfloor distance d of the carbon of 0.360-0.380nm scope
002, and at d
002Carbon intensity be 2000cps or bigger, and have 300-1000m
2The BET specific area of/g scope.That is, material with carbon element according to the present invention comprises the microcrystalline carbon of similar graphite, and it is kind of a high compactness material with carbon element.Simultaneously, this material with carbon element optionally has hole or impalpable structure.This hole or impalpable structure make the material with carbon element that is used for double electric layer capacitor according to the present invention can have capacitance and the same little internal resistance same big with the material with carbon element that is disclosed in above-mentioned patent documentation 1 and 2 (spy opens H11-317333 and No.2002-25867).
Because the electrode material (material with carbon element) according to polarizable electrode of the present invention has 300-1000m
2The specific area of/g scope, so internal resistance is lower than the material with carbon element that is used for double electric layer capacitor in patent documentation 1 and 2.Yet, have less than 270m in the double electric layer capacitor use
2During the material with carbon element of the BET specific area of/g, increase owing to the increase of the migration resistance in the electrolyte solution though might obtain big capacitance internal resistance.In addition, be 1000m in the BET specific area
2/ g or when bigger, because capacitance and general activated carbon is the same manifests in hole inside, therefore can not the big capacitance of acquisition.According to the present invention, the more preferably BET specific area of material with carbon element is 300-700m
2The scope of/g.
About the material with carbon element that is used for double electric layer capacitor according to the present invention, distance is the scope of 0.360-0.380nm between carbon-coating.Less than 0.360 o'clock, electrolyte was difficult to be inserted in the carbon-coating at interfloor distance, and this can cause the deterioration of capacitance and the increase of internal resistance.In addition, during greater than 0.380nm, carbon density can reduce and can not obtain high capacitance at interfloor distance.Interfloor distance is the scope of 0.365-0.375nm more preferably.
The material with carbon element of double electric layer capacitor that is used for according to the present invention is at d
002Have 2000cps or bigger carbon intensity, and it is the high compactness material with carbon element with crystallite of flourishing similar graphite.Therefore, material with carbon element according to the present invention is applicable to the polarizable electrode material that double electric layer capacitor with high capacitance is used.During less than 2000cps, therefore can not obtain big capacitance in carbon intensity because the compactness of material is low.
Manufacture method according to the material with carbon element that is used for double electric layer capacitor of the present invention is unrestricted, as long as the value of distance and carbon intensity falls in the preset range between BET surface area, carbon-coating.
For example, crystallite and comparatively unbodied low orientation petroleum asphalt or carbonization of Carboniferous System pitch and activation by having similar graphite can make the material with carbon element that is used for double electric layer capacitor according to of the present invention.Here, the BET specific area of material with carbon element is determined according to activation condition.More unbodied material with low orientation tends to form big specific area after activation processing.Have the petroleum asphalt of the crystallite of similar graphite by use, distance and carbon intensity can be in preset ranges between the carbon-coating of material.
(double electric layer capacitor)
Double electric layer capacitor of the present invention uses the above-mentioned material with carbon element of double electric layer capacitor that is used for as the polarizable electrode material.According to the present invention, the device that the electric capacity of double electric layer capacitor is represented is that being situated between, a pair of polarizing electrode staggered relatively forms positive pole and negative pole by the dividing plate in electrolyte solution.Electric charge accumulates on the electric double layer, and this electric double layer is formed in the interface of at least one electrode (polarizing electrode) and electrolyte solution.That is, capacitor of the present invention comprises so-called mixed capacitor (hybrid capacitor), and this mixed capacitor antianode uses different materials with negative electrode.The capacitor that is used for double electric layer capacitor of the present invention has big capacitance and has little internal resistance.
According to the present invention,, can use the above-mentioned material with carbon element that is used for double electric layer capacitor in the pair of electrodes at least one.That is, double electric layer capacitor of the present invention can the two all uses top material with carbon element to constitute by only target or anode or target and anode.In addition, above the two all uses at target and anode be used for the material with carbon element of double electric layer capacitor the time, the value more than can be different in distance and the carbon intensity between the BET specific area of negative electrode and anode, carbon-coating.
Except that electrode material, can form by the known materials of routine according to double electric layer capacitor of the present invention.For example, it can be placed in the container with electrolyte solution by the manufacturing pellet electrode and via dividing plate and be prepared.
For example, can be by following formation pellet electrode.At first, with the particle size of material with carbon element crushing into about 5-100 μ m.Then, add and mix as the carbon black of conduction adminicle with as the polytetrafluoroethylene (PTFE) of adhesive, so that give the material with carbon element powder high conductivity.At last, be sheet material with rolling rod with the gained forming materials.As the conduction adminicle, can use (for example acetylene blacks) such as powder graphite of de-carbon infrablack.As adhesive, can use polyvinylidene fluoride (PVDE), polyethylene (PE) or polypropylene (PP) except that PTFE.In this case, the proportioning between material with carbon element (activated carbon), conduction adminicle (carbon black) and the adhesive (PTFE) is generally 10: 0.5-1.0: 0.5-0.25.
Collector is mounted to the gained electrode and these electrodes are arranged to form positive pole and negative pole via dividing plate.Immerse and comprise electrolytical organic solvent with the assembling double electric layer capacitor thereafter.
As the organic solvent that is used for double electric layer capacitor, can use for example carbonates such as dimethyl carbonate, diethyl carbonate, ethylene carbonate and propylene carbonate, nitrile such as acetonitrile and propionitrile, lactone such as gamma-butyrolacton, Alpha-Methyl-gamma-butyrolacton, Beta-methyl-gamma-butyrolacton, gamma-valerolactone and 3-methyl-gamma-valerolactone, sulfoxide class such as dimethyl sulfoxide (DMSO) and diethyl sulfoxide, amide-type such as dimethyl formamide and diethylformamide, ethers such as oxolane and dimethoxy-ethane, dimethylsulfolane (dimethyl sulfolan) and sulfolane.These organic solvents can be used as independent solvent and use or use as two or more mixed solvents.
As the electrolyte that is dissolved in these organic solvents, can use for example tetrafluoro boric acid salt such as tetrafluoro boric acid etamon, the tetrafluoro boric acid tetramethylammonium, the tetrafluoro boric acid tetrapropylammonium, the tetrafluoro boric acid tetrabutylammonium, tetrafluoro boric acid trimethyl ethyl ammonium, tetrafluoro boric acid triethyl group ammonium methyl, tetrafluoro boric acid diethyl-dimethyl ammonium, tetrafluoro boric acid N-ethyl-N-crassitude, tetrafluoro boric acid N, N-tetramethylene pyrrolidines, tetrafluoro boric acid 1-ethyl-3-methylimidazole, perchloric acid salt such as perchloric acid etamon, the perchloric acid tetramethylammonium, the perchloric acid tetrapropylammonium, the perchloric acid tetrabutylammonium, perchloric acid trimethyl ethyl ammonium, perchloric acid triethyl group ammonium methyl, perchloric acid diethyl-dimethyl ammonium, perchloric acid N-ethyl-N-crassitude, perchloric acid N, N-tetramethylene pyrrolidines, perchloric acid 1-ethyl-3-methylimidazole, hexafluorophosphoric acid salt such as hexafluorophosphoric acid etamon, the hexafluorophosphoric acid tetramethylammonium, the hexafluorophosphoric acid tetrapropylammonium, the hexafluorophosphoric acid tetrabutylammonium, hexafluorophosphoric acid trimethyl ethyl ammonium, hexafluorophosphoric acid triethyl group ammonium methyl, hexafluorophosphoric acid diethyl-dimethyl ammonium.In addition, in that one of electrode in the capacitor is used can occlusion or during the material with carbon element of desorb lithium ion, wish to use for example LiClO of lithium salts
4, LiCF
3, SO
3, LiBF
4, LiPF
4, LiAsF
6, LiSbF
6, LiCF
3CO
2, LiN (CF
3SO
2)
2As electrolyte.
The concentration of preferred electrolyte is the scope of 0.5-5mol/L.More preferably, it should be the scope of 1.0-2.5mol/L.When electrolyte concentration was lower than 0.5mol/L, capacitance was because electrolytical shortage and deterioration.In addition, when using as the such ion fluid of 1-ethyl-3-methylimidazole, this fluid should in statu quo use or it should be mixed use with electrolytic solution.
Embodiment
The present invention is described in detail with reference to embodiment below.
(preparation of material with carbon element)
As embodiments of the invention, make the material with carbon element that is used for double electric layer capacitor by following method, i.e. sample 1-5.
(being used for the preparation of the material with carbon element of double electric layer capacitor)
As raw material, preparation has the crystallite of similar graphite and comparatively unbodied low orientation Carboniferous System pitch.Then, under the pressure condition of 0.1-0.5MPa, with 5 ℃/minute speed temperature is risen to 300-500 ℃ predetermined temperature.Thereafter, with this material heating 1 to 5 hour and carry out preliminary carbonization treatment.
Then, under 0.2MPa or littler pressure condition, with 5 ℃/minute speed temperature is risen to 700-900 ℃ predetermined temperature.Thereafter with this material heating 1-5 hour and carry out carbonization treatment.
After carbonization treatment, use alkali cpd (alkali metal hydroxide, alkali carbonate) to carry out activation processing.In this activation processing, the carbide of use and the amount of alkali cpd make that the ratio of amount by weight is 1: 1 to 1: 5.With temperature maintenance 700-900 (preferred 800 ℃) 4-10 hour.It should be noted, at nitrogen atmosphere or contain in the nitrogen atmosphere of steam and carry out activation processing.Then, water fully washs it and is crushed to average particle size particle size D50=5-50nm.
At last, under the nitrogen atmosphere of the hydrogen that contains the 3-100% ratio, calcine with preparation according to the material with carbon element that is used for double electric layer capacitor of the present invention, i.e. sample 1-5 at 700-900 ℃ (preferred 800 ℃).In addition, make the material with carbon element that is used for double electric layer capacitor by regulating above-mentioned each condition, i.e. sample 1-5.
In addition, when preparation was used for the material with carbon element of double electric layer capacitor, the amorphous materials that will have low orientation after preliminary carbonization was used for sample 1-3.And in sample 4-5, use compactness material with high orientation.Can carry out relatively crystal orientation by X-ray diffraction peak at d002.The results are shown in the table 1.About method of measurement, (Rigakudenkisha makes, Rint-2500) to use x-ray diffractometer.Measuring condition is listed as follows, tubular lamp bulb; Cu (K α), tube voltage: 40kV, tube current: 40mA, temperature range: 8-68 ℃.
When material was the black such high orientation of image-stone (high-crystallinity) material, for example diffraction maximum demonstrated rapid initial rising usually.Here, contrast is used for diffracted intensity and the half width of the material of sample 1-3 and sample 4-5 at d002, and the material of sample 1-3 demonstrates than lower diffracted intensity of the material of sample 4-5 and wideer half width at d002.The material of sample 1-3 also demonstrates the diffraction maximum wideer than the material of sample 4-5.This shows that the material that is used for this embodiment is comparatively amorphous and has low orientation.In addition, will be understood that equally that this material tends to have between wide carbon-coating distance and its crystal grain tends to be fine particle by this fact.
Measured distance and carbon intensity between BET specific area about the material with carbon element that is used for double electric layer capacitor of the sample 1-5 that makes, carbon-coating.The result is shown in the table 2.
(Quantachrome makes, and NOVA-3000) measures the BET specific area, and calculates by the BET method with the distribution of pores measuring instrument.(Rigakudenkisha makes, and Rint-2500) measures distance and diffracted intensity between the carbon-coating of d002 with x-ray diffractometer.Measuring condition is as follows, tubular lamp bulb; Cu (K α), tube voltage: 40kV, tube current: 40mA, measuring range: 8-68 °.Record distance and diffracted intensity (cps) between the carbon-coating of d002 by diffraction maximum at d002.
(electric double-layer capacitors prepared)
Use the material with carbon element that is used for double electric layer capacitor of sample 1-5 to make double electric layer capacitor as the polarizable active material of electrode.
At first, as active material, (120 ℃, 0.133Pa (10 with the material with carbon element vacuumize of sample 1-5
-3Torr)), preparation is as active material carbon black (the Cabot manufacturing of conduction adminicle then, VURCAN-XC72R) and as the PVDF of adhesive (KurehaKagakusha makes, #9210), the amount of preparation makes that the ratio of amount by weight is 9: 1: 2, and mixes with N-methyl pyrrolidone (NMP) as solvent.After it is adjusted to moderate viscosity, material is carried out the vacuum kneading to form slurry.The gained slurry is applied to the aluminium foil of collected current, pushes to form the square of 50 * 50mm, thickness t=50 μ m, used as electrode slice with roll squeezer.
(product of Advantech Toyosha, (at 120 ℃, 0.133Pa (10 GA-100) this electrode slice to be carried out vacuumize with glass fiber filter paper
-3Torr), 2-6 hour).Glove box in carry out vacuum impregnation thereafter.Then, use EMI-BF
4Be the tetrafluoroborate of 1-ethyl-3-methylimidazole, it is an ionic liquid, as electrolyte.The dipping after, with gained material Vacuum Package in the aluminum laminated bag to make the capacitor battery of the material with carbon element that has used sample 1-5.
(evaluation of capacitor)
The charging and the discharge performance of the capacitor that just makes are estimated.Also monitor the rising that accumulates to the voltage of capacitor with electric charge by constant current charge, the charging and the discharge performance of capacitor are estimated.That is, the constant current charge by 10mA (or 5mA) is also for example kept this voltage during 3.75V when voltage reaches predetermined value in positive pole and negative pole, and it becomes the constant voltage charge mode and electric current begins to weaken.When process is scheduled to charging interval T (normally being 4500 seconds), change the polarity of electrode.By constant current mode it is discharged, constant current is 10mA (or 5mA), till voltage becomes 0V.After this operation, (normally being 180 seconds) at certain intervals repeated constant current charge again and discharged 1 to 3 time by above-mentioned.Then, applied voltage is reduced to the 3.3V and the limiting voltage that will discharge and is made as 0.5V.With identical electric current, carry out cycle detection.Use can make charging that 8 passages carry out simultaneously and discharge equipment, and (Hokutodenko produces, and HJ1001SM8) measures.With this result and the measurement result (capacitance, internal resistance) that obtains together shown in the table 2.
Detect as a comparison, use sample 6-8 from cocos active carbon to prepare electric capacity in the same way and estimate.The result is also shown in the table 2.And, also shown cocos active carbon, be distance and carbon intensity between the BET specific area, carbon-coating of sample 6-8.
As shown in table 2, what observe is, uses the capacitor of the material with carbon element of sample 1-3 to have high capacitance and low internal resistance, and distance and carbon intensity fall in the preset range between the BET specific area of described material with carbon element, carbon-coating.
What also observe is, the capacitance of having used the capacitor of sample 4-5 to have to improve, but internal resistance poor than the capacitor of sample 1-3, and distance and carbon intensity fall in the preset range between the carbon-coating of described sample 4-5, but the BET specific area is littler than preset range.
The capacitor of sample 6, the BET specific area of described sample 6 falls in the preset range, but distance and carbon strength ratio preset range are big between carbon-coating, the capacitor of sample 7, distance and carbon strength ratio preset range are big between the BET specific area of described sample 7, carbon-coating, the perhaps capacitor of sample 8, distance falls in the preset range between the carbon-coating of described sample 8, but BET specific area and carbon intensity do not fall into preset range, these capacitors have little internal resistance, but capacitance is compared serious deterioration with the capacitor of sample 1-3.
That is, what observe is, the capacitor of sample 1-3 has high capacitance and low internal resistance, and distance and carbon intensity fall in the preset range between the BET specific area of the material with carbon element that described sample 1-3 uses, carbon-coating.This high-performance derives from the material with carbon element of the polarizable active material that is used for electrode.Be understandable that the material with carbon element that distance and carbon intensity fall in the preset range between its BET specific area, carbon-coating shows these effects.
In other words, according to the material with carbon element of the sample 1-3 of present embodiment, comprise the microcrystalline carbon of similar graphite, and they are high compactness material with carbon elements.Simultaneously, this material with carbon element optionally has hole or impalpable structure.Therefore, this material with carbon element have with patent documentation 1-2 in the same high capacitance of the material with carbon element described, and have low internal resistance.
Claims (2)
1. the material with carbon element that is used for double electric layer capacitor, this material with carbon element has:
At 300-1000m
2The BET specific area of/g scope;
Distance between the carbon-coating of 0.360-0.380nm scope; With
2000cps or bigger carbon intensity.
2. the double electric layer capacitor that comprises described material with carbon element, described material with carbon element has:
At 300-1000m
2The BET specific area of/g scope;
Distance between the carbon-coating of 0.360-0.380nm scope; With
2000cps or bigger carbon intensity.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2005288616 | 2005-09-30 | ||
| JP288616/2005 | 2005-09-30 | ||
| JP321362/2005 | 2005-11-04 |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201110173035.1A Division CN102336402B (en) | 2005-09-30 | 2006-09-28 | Carbon material for electric double layer capacitor and electric double layer capacitor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101278365A true CN101278365A (en) | 2008-10-01 |
Family
ID=39996582
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2006800360301A Pending CN101278365A (en) | 2005-09-30 | 2006-09-28 | Carbonaceous material for electric double layer capacitor and electric double layer capacitor |
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| Country | Link |
|---|---|
| CN (1) | CN101278365A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102859625A (en) * | 2010-04-21 | 2013-01-02 | 康宁股份有限公司 | Electrochemical capacitor having lithium containing electrolyte |
| CN114322662A (en) * | 2021-12-13 | 2022-04-12 | 中国科学技术大学 | Energy collection-storage wearable protective equipment and preparation method thereof |
-
2006
- 2006-09-28 CN CNA2006800360301A patent/CN101278365A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102859625A (en) * | 2010-04-21 | 2013-01-02 | 康宁股份有限公司 | Electrochemical capacitor having lithium containing electrolyte |
| CN102859625B (en) * | 2010-04-21 | 2016-02-17 | 康宁股份有限公司 | There is the electrochemical capacitor containing lithium electrolyte |
| CN114322662A (en) * | 2021-12-13 | 2022-04-12 | 中国科学技术大学 | Energy collection-storage wearable protective equipment and preparation method thereof |
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Open date: 20081001 |