WO2006088004A1 - Materiau d'electrode pour condensateur electrique double couche et son procede de production - Google Patents

Materiau d'electrode pour condensateur electrique double couche et son procede de production Download PDF

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Publication number
WO2006088004A1
WO2006088004A1 PCT/JP2006/302494 JP2006302494W WO2006088004A1 WO 2006088004 A1 WO2006088004 A1 WO 2006088004A1 JP 2006302494 W JP2006302494 W JP 2006302494W WO 2006088004 A1 WO2006088004 A1 WO 2006088004A1
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WO
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Prior art keywords
double layer
electric double
electrode material
layer capacitor
carbon
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PCT/JP2006/302494
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English (en)
Japanese (ja)
Inventor
Tomoya Iwasaki
Hitoshi Hashizume
Makoto Shimizu
Original Assignee
Shinano Kenshi Kabushiki Kaisha
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Priority to JP2006524165A priority Critical patent/JPWO2006088004A1/ja
Publication of WO2006088004A1 publication Critical patent/WO2006088004A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/52—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbon, e.g. graphite
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • 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
    • H01G11/36—Nanostructures, e.g. nanofibres, nanotubes or fullerenes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52—Constituents or additives characterised by their shapes
    • C04B2235/5284—Hollow fibers, e.g. nanotubes
    • C04B2235/5288—Carbon nanotubes
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
    • 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

Definitions

  • the present invention relates to an electric double layer capacitor electrode material, a manufacturing method thereof, and an electric double layer capacitor.
  • An electric double layer capacitor has been used as a small power storage device for a backup power source such as a portable device.
  • high power density capacitors are required for hybrid vehicles and fuel cell vehicles from the viewpoint of environmental issues.
  • a conductive material such as carbon black is added to the activated carbon material as a polarizable electrode material to increase the conductivity and decrease the internal resistance.
  • attempts have been made to reduce internal resistance by increasing the electrical conductivity by adding carbon nanofibers as a conductive material (Japanese Patent Laid-Open No. 2001-135554).
  • Patent Document 1 JP 2001-135554
  • the present invention has been made to solve the above-described problems, and the object of the present invention is to provide an electric double layer suitable for high-current high-speed charge / discharge, which can uniformly disperse force-bonded nanofibers, reduce internal resistance, and It is in providing a capacitor electrode material and a manufacturing method thereof.
  • the electrode material for an electric double layer capacitor according to the present invention is in a solution in which a polymer substance in which an atom group containing a helium atom such as nitrogen, oxygen or sulfur is present in the main chain or side chain is dissolved. Carbon nanofibers are dispersed, the dispersion solution is dried, and the dried product is also baked in a non-acidic atmosphere at 500 to 3,000 ° C. to obtain a composite carbon material force.
  • the composite carbon material is subjected to activation treatment, and a large number of pores are formed on the surface. It is characterized by.
  • the electrode material for the electric double layer capacitor is characterized by having a granularity of 1 ⁇ m to 1000 m.
  • the amount of carbon nanofibers relative to the polymer material is 1-30 wt%.
  • the polymer substance is characterized by comprising an amino acid, a protein having an amino acid strength, or a peptide.
  • the polymer material is also characterized by a silk material strength.
  • the composite carbon material includes a nitrogen element.
  • the carbon nanofiber is a single-layer, double-layer, or multi-layer carbon nanotube, a cap-stacked carbon nanotube, or a carbon nanohorn.
  • the electric double layer capacitor according to the present invention is a pair of electrode bodies made of a current collector and a polarizable electrode, a separator, and an electric double layer capacitor made of electrolytic solution. 9. An electrode material for an electric double layer capacitor as set forth in any one of 9 above.
  • the method for producing an electric double layer capacitor according to the present invention includes a polymer in which a polymer substance in which an atomic group containing a hetero atom such as nitrogen, oxygen, or sulfur is present in a main chain or a side chain is dissolved.
  • the method includes a step of dispersing carbon nanofibers in a solution derived from a substance, a step of drying the dispersion solution, and a step of firing a dried product to form a composite carbon material.
  • the dried product is preferably pulverized and then calcined.
  • the composite carbon material formed by firing the dried product may be crushed into particles.
  • carbon nanofibers are dispersed in an amount of 1 to 30 wt% with respect to the polymer substance.
  • the carbon nanofibers are uniformly dispersed and the carbide derived from the polymer material and the carbon nanofibers 1 are in close contact with each other, so that the internal resistance can be sufficiently reduced, and a high-current, high-speed Suitable for charging / discharging, high output electric double layer capacitor can be obtained.
  • FIG. 1 is a Raman spectrum diagram of a fired product when coarse-grained silk is fired at a high temperature of 2000 ° C.
  • FIG. 2 Raman spectrum of fired product when coarse silk is fired at a high temperature of 700 ° C.
  • FIG. 3 Raman spectrum of the fired product when coarse silk is fired at a high temperature of 1000 ° C.
  • FIG. 6 is a graph showing measured values of powder resistance of a composite carbon material.
  • FIG. 7 is a graph showing capacitor characteristics (volume capacity) of Examples and Comparative Examples.
  • the electric double layer capacitor is composed of a pair of electrode bodies composed of a current collector and a polarizable electrode, a separator, and an electrolyte (the structure itself can take various known structures and is not particularly shown).
  • This embodiment is characterized by the electrode material included in the polarizable electrode.
  • carbon nanofibers are dispersed in a solution in which a polymer substance in which atomic groups containing heteroatoms such as nitrogen, oxygen, and sulfur are present in the main chain or side chain is dissolved,
  • the dispersion solution is dried, and the dried product is composed of a composite carbon material fired in a non-oxidizing atmosphere at 500 ° C. to 3000 ° C.
  • a silk material can be used for the polymer material.
  • the silk material is a general term for woven fabrics, knitted fabrics, powders, cotton, yarns, etc., which are rabbits or barbaric. These can be used alone or in combination.
  • These silk materials have a higher-order protein structure, and there are coordinating groups containing various amino acid residues on the surface (including the folded inner surface).
  • a polymer material in addition to the silk material described above, a polymer material in which an atomic group containing donor atoms such as nitrogen, oxygen, and sulfur is present in the main chain or side chain can be used.
  • proteins such as keratin, milk protein, corn protein and collagen can also be used.
  • carbon nanofibers are added to a solution in which the above polymer material is dissolved and dispersed well.
  • To disperse the carbon nanofibers apply ultrasonic vibration.
  • the amount of carbon nanofiber added to the polymer material is preferably about 1 to 30 wt%.
  • the carbon nanofiber single-walled, double-walled, or multi-walled carbon nanotubes, cap-stacked carbon nanotubes, or carbon nanohorns can be used.
  • the mixed solution is naturally dried or heated to about 80 ° C. to remove moisture and dried.
  • this dried product is fired at a temperature of 500 ° C. to 3000 ° C. to obtain a composite carbon material.
  • an activation treatment is performed in which this composite carbon material is exposed to high-temperature steam at about 700 ° C.
  • This activation treatment a large number of pores are formed on the surface of the carbide derived from the polymer material in the composite carbon material.
  • the surface area is increased, which is suitable as an electrode material for the electric double layer capacitor.
  • the pores are extremely small with a diameter of 1 Onm or less, and as a result, the composite carbon material has a surface area as large as 100 to 3000 m 2 Zg.
  • the activated composite carbon material is pulverized to a size of about 1 ⁇ to 1000 / ⁇ m, preferably about 5 m to 10 m.
  • a polarizable electrode By pulverizing in this way, it is possible to obtain a polarizable electrode by binding with a binder such as PTFE (polytetrafluoroethylene).
  • the dried product dried in the above drying step may be pulverized and fired.
  • the polarizable electrode only the composite carbon material formed in the above-mentioned granular shape may be used, but other conductive materials such as activated carbon and carbon black may be used in combination.
  • the mixing ratio of the electrode material is not particularly limited.
  • the composite carbon material of the present embodiment 15 to 90 wt%, conductive material such as carbon black 3 to 15 wt%, PTFE3 to 2 Owt%, CMC ( (Carboxymethylcellulose) 3 to 20 wt% is preferable.
  • the firing temperature is more preferable as the firing is performed at a higher temperature because the carbide derived from the polymer material becomes graphite and the conductivity is improved. Specifically, when it is fired at 1400 ° C or higher, it becomes a carbide with good conductivity.
  • the dispersibility of the carbon nanofibers becomes uniform.
  • the silk material was baked alone and the physical properties of the fired product were examined.
  • the firing temperature of the silk material is about 500 ° C to 3000 ° C.
  • the firing atmosphere is performed in an inert gas atmosphere such as nitrogen gas or argon gas or in a vacuum to prevent the silk material from burning and ashing.
  • an inert gas atmosphere such as nitrogen gas or argon gas or in a vacuum to prevent the silk material from burning and ashing.
  • firing it is preferable that firing is performed in a plurality of stages while avoiding rapid firing.
  • the firing conditions are the same when firing the composite material.
  • the first firing temperature for example, 500 ° C
  • the temperature is raised at a moderate temperature increase rate of 0 ° C. or less, preferably 50 ° C. or less per hour, and the primary calcination is carried out at this primary calcination temperature for several hours.
  • a secondary firing temperature e.g., 700 ° C
  • the secondary firing is performed for several hours at the secondary firing temperature.
  • a third firing for example, 2000 ° C. of final firing
  • the firing conditions are not limited to the above, and can be changed as appropriate depending on the type of silk material, the function of the desired carbon material, and the like.
  • firing is performed in multiple stages, and by heating at a moderate temperature rise rate and firing, dozens of amino acids are involved in an amorphous structure and a crystalline structure. However, rapid degradation of protein conformation is avoided.
  • Figure 1 shows the Raman spectrum of the fired product when coarse-grained silk is fired at a high temperature of 2000 ° C (final stage firing temperature). 2681cm _1 , It is understood that graphitized since the peak is observed at the 1335cm _1.
  • FIG. 5 is a Raman spectrum diagram of a fired product when fired with C. When the firing temperature is 1400 ° C, the peak value is low, but the peaks at the above three locations are observed.
  • IX 10 is _5 ( ⁇ ⁇ ⁇ ), but does not extend to the graphite (4 ⁇ 7 ⁇ 10-7 ⁇ -m), become a better resistivity carbon (4 X 10- 5), good electrical conductivity It turns out that it has sex.
  • Table 1 shows the results of elemental analysis (semi-quantitative analysis results) using an electron microanalyzer of the fired product obtained by firing a silk knitted silk fabric at 700 ° C in a nitrogen atmosphere.
  • Measurement conditions are acceleration voltage: 15 kV, irradiation current: 1 ⁇ , and probe diameter: 100 m.
  • the values in the table indicate the tendency of the detected elements and are not guaranteed values.
  • Example 1 As described above, when the silk material is fired, a large amount of elements such as nitrogen element remain, which is suitable as an electrode material for a capacitor.
  • Example 1 As described above, when the silk material is fired, a large amount of elements such as nitrogen element remain, which is suitable as an electrode material for a capacitor.
  • a 65 wt% aqueous solution 11 of calcium chloride dihydrate 11 of calcium chloride dihydrate, 240 g of silk raw material was added, and the solution was heated and dissolved for 6 hours while maintaining the solution temperature at 95 ° C. After filtering the dissolved solution after the decomposition, the undissolved material was filtered off, and the filtrate was further desalted using a dialysis membrane with a molecular fraction of 300 to further dilute the sylk protein solution to 3 wt%.
  • Silk protein aqueous solution was used. Carbon nanofibers were mixed with 3 ml of this 3 wt% silk protein aqueous solution, and the carbon nanofibers were dispersed by applying ultrasonic waves and dried at room temperature.
  • FIG. 5 is an SEM photograph of the composite carbon material obtained in this way. It can be seen that the carbon nanofibers are bound by the carbide derived from the polymer material, and that the carbon nanofibers protrude in the shape of spines. When the electrode material is used, the protruding carbon nanofibers come into contact with each other, and high conductivity is obtained.
  • Example 6 shows a powder of a composite carbon material formed using DWCNT and MWCNT as the carbon nanofiber and a composite carbon material (comparative example) formed using carbon black instead of the carbon nanofiber. This is a graph of measured resistance. Using this composite carbon material 75wt%, PTFE 15wt%, CMC 10wt%, a polarizable electrode material was formed.
  • Example 2
  • Carbon nanofibers were mixed with 3 ml of a 3 wt% silk protein aqueous solution, and the carbon nanofibers were dispersed by applying ultrasonic waves and dried at 80 ° C. After drying, it was pulverized and calcined at 700 ° C in a nitrogen atmosphere to obtain a composite carbon material powder. This material was steam activated at 700 ° C to obtain a high surface area composite carbon material. Using this composite carbon material 75wt%, PTFE 15wt%, CMC 10wt%, a polarizable electrode material was formed.
  • Carbon nanofibers were mixed in 3 ml of a 3 wt% silk amino acid aqueous solution, and the carbon nanofibers were dispersed by applying ultrasonic waves and dried at 80 ° C. After drying, it was pulverized and calcined at 700 ° C in a nitrogen atmosphere to obtain a composite carbon material powder. This material was steam activated at 700 ° C to obtain a high surface area composite carbon material. Using this composite carbon material 75wt%, PTFE 15wt%, CMC 10wt%, a polarizable electrode material was formed.
  • Example 4 Example 4
  • Carbon nanofibers were mixed in 3 ml of a 3 wt% silk amino acid aqueous solution, and the carbon nanofibers were dispersed by applying ultrasonic waves and dried at 80 ° C. After drying, it was pulverized and calcined at 700 ° C in a nitrogen atmosphere to obtain a composite carbon material powder. This material was steam activated at 700 ° C to obtain a high surface area composite carbon material. Using this composite carbon material 75wt%, PTFE 15wt%, CMC 10wt%, a polarizable electrode material was formed.
  • Example 5 Example 5
  • Carbon nanofibers were mixed in 3 ml of a 3 wt% silk amino acid aqueous solution, and the carbon nanofibers were dispersed by applying ultrasonic waves and dried at room temperature. After drying, it was pulverized and fired at 700 ° C in a nitrogen atmosphere to obtain a composite carbon material powder. This material Furthermore, it was fired at 2000 ° C. in a nitrogen atmosphere to obtain a low resistance composite carbon material. Using this, a polarizable electrode material was obtained using 80 wt% activated carbon, 10 wt% low resistance composite carbon material, and 10 wt% PTFE.
  • a commercially available carbon black was used in place of the low resistance composite carbon material, and a silk amino acid aqueous solution was dried and the dried product was crushed without adding carbon nanofibers or carbon black.
  • a polarizable electrode material using a carbon material fired under the above conditions was obtained.

Abstract

La présente invention décrit un matériau d'électrode destiné aux condensateurs électriques double couche, dans lequel sont uniformément dispersées des nanofibres de carbone. Ledit matériau permet de réduire la résistance interne, il convient également pour les opérations de charge/décharge haut débit, avec un courant important. L'invention décrit plus particulièrement un matériau d'électrode pour des condensateurs électriques double couche, composé d'un matériau composite de carbone obtenu en dispersant des nanofibres de carbone dans une solution ; un matériau polymère ayant un groupe atomique comprenant un hétéroatome comme un atome d'azote, d'oxygène ou de soufre dans une chaîne principale ou une chaîne latérale est dissous, ce qui sèche la solution de dispersion, puis entraîne la détonation du matériau séché à 500-3 000 °C dans une atmosphère non oxydante.
PCT/JP2006/302494 2005-02-21 2006-02-14 Materiau d'electrode pour condensateur electrique double couche et son procede de production WO2006088004A1 (fr)

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JP2006524165A JPWO2006088004A1 (ja) 2005-02-21 2006-02-14 電気二重層キャパシタ電極材料およびその製造方法

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JP2005044573 2005-02-21

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008285658A (ja) * 2007-04-16 2008-11-27 Shinano Kenshi Co Ltd 炭素粉配合ゴム組成物とその製造方法
JP2011230969A (ja) * 2010-04-28 2011-11-17 Toyo Univ ポリアミノ酸が施与されたカーボンナノチューブおよびその製造方法

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001239157A (ja) * 2000-02-28 2001-09-04 Rengo Co Ltd 無機イオン交換体−親水性高分子活性炭複合体およびその製造方法
JP2003160323A (ja) * 2001-09-11 2003-06-03 Showa Denko Kk 活性炭及びその製造方法並びにその用途
JP2005001969A (ja) * 2003-06-13 2005-01-06 Nippon Steel Chem Co Ltd 低内部抵抗炭素微粉の製造方法及び電気二重層キャパシタ

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2001239157A (ja) * 2000-02-28 2001-09-04 Rengo Co Ltd 無機イオン交換体−親水性高分子活性炭複合体およびその製造方法
JP2003160323A (ja) * 2001-09-11 2003-06-03 Showa Denko Kk 活性炭及びその製造方法並びにその用途
JP2005001969A (ja) * 2003-06-13 2005-01-06 Nippon Steel Chem Co Ltd 低内部抵抗炭素微粉の製造方法及び電気二重層キャパシタ

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2008285658A (ja) * 2007-04-16 2008-11-27 Shinano Kenshi Co Ltd 炭素粉配合ゴム組成物とその製造方法
JP2011230969A (ja) * 2010-04-28 2011-11-17 Toyo Univ ポリアミノ酸が施与されたカーボンナノチューブおよびその製造方法

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