WO2009139493A1 - 導電性接着剤ならびにそれを用いた電気二重層キャパシタ用電極および電気二重層キャパシタ - Google Patents
導電性接着剤ならびにそれを用いた電気二重層キャパシタ用電極および電気二重層キャパシタ Download PDFInfo
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- WO2009139493A1 WO2009139493A1 PCT/JP2009/059234 JP2009059234W WO2009139493A1 WO 2009139493 A1 WO2009139493 A1 WO 2009139493A1 JP 2009059234 W JP2009059234 W JP 2009059234W WO 2009139493 A1 WO2009139493 A1 WO 2009139493A1
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- WIPO (PCT)
- Prior art keywords
- electric double
- conductive adhesive
- double layer
- electrode
- layer capacitor
- Prior art date
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- 239000011976 maleic acid Substances 0.000 description 1
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- XJRBAMWJDBPFIM-UHFFFAOYSA-N methyl vinyl ether Chemical compound COC=C XJRBAMWJDBPFIM-UHFFFAOYSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- XGTQXAMURMYHPC-UHFFFAOYSA-N n,n-dimethylformamide;thiolane 1,1-dioxide Chemical compound CN(C)C=O.O=S1(=O)CCCC1 XGTQXAMURMYHPC-UHFFFAOYSA-N 0.000 description 1
- OGHYBWBUSLSBBT-UHFFFAOYSA-N n-[4-[acetyl(ethenyl)amino]butyl]-n-ethenylacetamide Chemical compound CC(=O)N(C=C)CCCCN(C=C)C(C)=O OGHYBWBUSLSBBT-UHFFFAOYSA-N 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- YCWSUKQGVSGXJO-NTUHNPAUSA-N nifuroxazide Chemical group C1=CC(O)=CC=C1C(=O)N\N=C\C1=CC=C([N+]([O-])=O)O1 YCWSUKQGVSGXJO-NTUHNPAUSA-N 0.000 description 1
- LYGJENNIWJXYER-UHFFFAOYSA-N nitromethane Chemical compound C[N+]([O-])=O LYGJENNIWJXYER-UHFFFAOYSA-N 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 229920000582 polyisocyanurate Polymers 0.000 description 1
- 239000011495 polyisocyanurate Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 230000000717 retained effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005488 sandblasting Methods 0.000 description 1
- 229940047670 sodium acrylate Drugs 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- PNGLEYLFMHGIQO-UHFFFAOYSA-M sodium;3-(n-ethyl-3-methoxyanilino)-2-hydroxypropane-1-sulfonate;dihydrate Chemical compound O.O.[Na+].[O-]S(=O)(=O)CC(O)CN(CC)C1=CC=CC(OC)=C1 PNGLEYLFMHGIQO-UHFFFAOYSA-M 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 150000005621 tetraalkylammonium salts Chemical class 0.000 description 1
- 125000005497 tetraalkylphosphonium group Chemical group 0.000 description 1
- CBXCPBUEXACCNR-UHFFFAOYSA-N tetraethylammonium Chemical class CC[N+](CC)(CC)CC CBXCPBUEXACCNR-UHFFFAOYSA-N 0.000 description 1
- SZWHXXNVLACKBV-UHFFFAOYSA-N tetraethylphosphanium Chemical class CC[P+](CC)(CC)CC SZWHXXNVLACKBV-UHFFFAOYSA-N 0.000 description 1
- QEMXHQIAXOOASZ-UHFFFAOYSA-N tetramethylammonium Chemical class C[N+](C)(C)C QEMXHQIAXOOASZ-UHFFFAOYSA-N 0.000 description 1
- BXYHVFRRNNWPMB-UHFFFAOYSA-N tetramethylphosphanium Chemical class C[P+](C)(C)C BXYHVFRRNNWPMB-UHFFFAOYSA-N 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 235000005074 zinc chloride Nutrition 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/10—Multiple hybrid or EDL capacitors, e.g. arrays or modules
- H01G11/12—Stacked hybrid or EDL capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/38—Carbon pastes or blends; Binders or additives therein
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/74—Terminals, e.g. extensions of current collectors
-
- 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 a conductive adhesive used for an electrode for an electric double layer capacitor
- the present invention relates to an electric double layer capacitor electrode and an electric double layer capacitor using the same.
- electric double-layer capacitors that can be charged and discharged with a large current are promising as storage devices with high charging and discharging frequency, such as auxiliary power sources for electric vehicles, auxiliary power sources for solar cells, and auxiliary power sources for wind power generation. Therefore, an electric double layer capacity with high energy density, rapid charge / discharge, and excellent durability is desired.
- the electric double layer capacitor has a structure in which a pair of polarizable electrode layers are opposed to each other through a separator and serve as a positive electrode and a negative electrode.
- Each polarizable electrode layer is impregnated with an aqueous electrolyte solution or a non-aqueous electrolyte solution, and each polarizable electrode layer is bonded to a current collector.
- a water-based electrolyte solution can increase the capacitance density and reduce the resistance value, but the working voltage must be less than the voltage at which water electrolysis occurs, so the energy density is increased.
- a non-aqueous electrolyte is used for.
- a sheet forming (rolling) method and a coating method as a method of manufacturing a polarizable electrode.
- a thin electrode can be produced by a relatively easy operation, but it is possible to coat a current collector such as an aluminum foil.
- the electrode density cannot be increased because pressing is performed after the tinting.
- the sheet forming method compared with the coating method, produces a sheet electrode formed at a higher density and then joins it to a current collector such as an aluminum foil. It is a joining method.
- Japanese Patent Laid-Open No. 2 0 0 5 — 1 3 6 4 0 1 discloses a structure including a carbonaceous electric double layer forming material (activated carbon, etc.), a carbon material for securing conductivity, and a binder.
- a polarizable porous sheet made of a material is an electric double-layer capacitor electrode formed by integrating a conductive intermediate layer on at least one side of a current collector via a conductive intermediate layer, the conductive intermediate layer being Synthetic rubbers and those containing two or more types of carbon materials with different particle sizes have been proposed. According to the electrode for the electric double layer capacitor, the internal resistance is low, the electric capacity is high, and the high output density can be achieved.
- Japanese Laid-Open Patent Publication No. 2 0 3-3 5 3 0 7 4 describes that a specific poly-N-vinylacetamide is used as a binder for electrode paces for electric double layer capacitors. Yes.
- Japanese Patent Application Laid-Open No. Heisei 2 0 0 2 1 3 5 3 0 7 4 discloses that a binder containing poly-N-pinylacetamide is bonded to a polarizable electrode layer and a sheet-like current collector. There is no description or suggestion about using as a conductive adhesive
- a conductive adhesive for joining a polarizable electrode layer and a sheet-like current collector has been a mixture of polyvinyl alcohol (PVA) and conductive material, styrene-butadiene rubber (SBR) and There is a mixture of conductive materials.
- PVA polyvinyl alcohol
- SBR styrene-butadiene rubber
- non-aqueous electric double layer capacitor electrodes It is necessary to perform a drying treatment before it is used for the conductive adhesive, and the conductive adhesive is required to have heat resistant adhesiveness that can withstand the drying treatment.
- an object of the present invention is to provide a conductive adhesive that achieves higher thermal resistance while maintaining low internal resistance.
- a conductive adhesive comprising a system binder.
- An electrode for an electric double layer capacitor in which a polarizable electrode layer is joined to at least one side of a sheet-like current collector via a conductive adhesive.
- the conductive adhesive is the conductive adhesive described in any one of (1) to (6).
- An electric double-layer capacitor comprising the electrode for an electric double-layer capacitor according to any one of (7) to (9) is provided.
- FIG. 1 is a partially enlarged schematic cross-sectional view showing an example of an electric double layer capacitor electrode according to the present invention.
- Fig. 2 shows the electric double layer capacitor electrode and the separator of the present invention. It is a schematic perspective view which shows the structure combined.
- FIG. 3 is a schematic perspective view showing a state in which a plurality of components of the electric double layer capacitor are arranged side by side.
- FIG. 4 is a partially cutaway schematic perspective view showing the configuration of the electric double layer capacitor fabricated in the example (invention example).
- the conductive adhesive according to the present invention is a conductive adhesive for joining a polarizable electrode layer of an electric double layer capacitor electrode and a sheet-like current collector, and is composed of a conductive material and a poly (N-vinylacetamide). Contains a binder.
- Poly N_vinylacetamide has the following formula (1):
- R 1 and R 2 each independently represent a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, preferably 1 to 6 alkyl groups. May include an ether bond, an ester bond, a thioether bond or an amide bond.
- a polymer containing a repeating structural unit having an amide structure represented by R 1 and R 2 are preferably a hydrogen atom, a methyl group, an ethyl group, a propyl group, an isopropyl group, a butyl group, a 2-methylpropyl group, a t-butyl group, or a methoxymethyl group, and R 1 is a hydrogen atom. More preferably, it is an atom, and R 2 is a methyl group or an ethyl group.
- R 1 and R 2 each independently represent a hydrogen atom or an alkyl group having 1 to 10 carbon atoms, preferably 1 to 6 carbon atoms. A bond, an ester bond, a chain bond or an amide bond), and a polymer obtained by polymerizing the compound is preferably used.
- R 1 and R 2 are preferably a hydrogen atom, a methyl group, an ethyl group, a propyl group, an isopropyl group, a butyl group, a 2-methylpropyl group, a t-butyl group, or a methoxymethyl group, and further R 1 More preferably, is a hydrogen atom, and R 2 is a methyl group or an ethyl group.
- the N-vinylacetamide polymer means an N-vinylacetamide homopolymer and an N-vinylacetamide copolymer.
- Monomers copolymerizable with N-vinylacetamide include (meth) acrylic acid or salts thereof, (meth) methyl acrylate, (meth) acrylic acid ethyl, (meth) acrylic acid (iso) propyl, (meth) Ptyl acrylate, octyl (meth) acrylate, 2-methyhexyl (meth) acrylate, methoxytyl (meth) acrylate, 2 — hydroxetyl (meth) acrylate, 2-hydroxypropyl (meta) ) (Meth) acrylic acid monomers such as acrylate, polyoxyalkylene glycol mono (meth) acrylate; Mid, N, N—Dimethyl (meth) acrylamide, N, N—Jetyl (meth) acrylamide, N—
- the proportion of the copolymerizable monomer used is generally 60% by mass or less, preferably 40% by mass or less, to the extent that the target performance of the present invention is not impaired with respect to the total amount of the polymerizable monomers. Preferably it is 30% by mass or less.
- the polymer of N-vinylacetamide is a three-dimensional crosslinked product containing a three-dimensional crosslinked structure in the presence of a crosslinking agent having two or more polymerizable double bonds in one molecule.
- a polymer obtained by polymerization crosslinking of N-vinylacetamide together with the above-mentioned other comonomers or an uncrosslinked precursor polymer is produced in advance, and this is reacted with a functional group in the polymer to form a chemical bond. It is produced by a method of forming, for example, a method of cross-linking with radiation or peroxide.
- Crosslinkers with two or more polymerizable double bonds in one molecule used for crosslinking here are tetraaryloxetane, pen erythritol tetraaryl ether, pen erythritol tart.
- crosslinking agent such as or a compound having a (meth) acrylic group; divinylbenzene, divinyl ether, (meth) acrylic acid aryl, and the like can be used. These crosslinking agents may be used alone or in combination. It can also be used above.
- the amount of the crosslinking agent used is preferably 10% by mass or less, more preferably 6% by mass or less, based on the total amount of the polymerizable monomer containing N-vinylacetamide.
- crosslinking agent that can react with a functional group (for example, a hydroxyl group, an amino group, a carboxyl group, etc.) in an uncrosslinked precursor polymer to form a chemical bond, depending on the functional group, polyglycidyl ether, Examples thereof include polyisocyanurate, polyamine, polyol, and polystrepturonic acid.
- the amount of these cross-linking agents used is usually based on the total amount of cross-linked precursor polymer, and the ratio of polymer: cross-linking agent is 90: 10-9.99 9: 9. The range is preferable, and the range of 9 5: 5 to 9 9.99 95: 0.05 is more preferable.
- the molecular weight of the N-vinylacetamide polymer is preferably not less than 500,000, more preferably not less than 500,000 and not more than 100,000, and more preferably not less than 30,000 and not more than 100,000. More preferably, 1 million or more
- Particularly preferred is 5 million or less.
- the molecular weight is too small, the heat resistant adhesiveness is lowered, and the mechanical strength is also reduced, which is not preferable. If the molecular weight is too high, the liquid viscosity of the produced conductive adhesive becomes too high, which is not preferable.
- N-pinylacetamide polymer of the present invention examples include poly-N-vinylacetamide manufactured by Showa Denko, for example, NA- 1 5 0 F, NA 0 1 OF, NA— 0 1 0 S, non-crosslinked type GE— 1 9 1, GE— 1 9 1 LH, GE— 1 9 1 L, GE 1 1 9 1 LL, GE-1 9 1 L 3 4, and GE— 1 6 7, GE— 1 6 7 L, GE-1 6 3 LM (sodium acrylate copolymer), and XGC— 3 3 0 (vinyl acetate copolymer), and XGC— 2
- the conductive material contained in the conductive adhesive according to the present invention includes graphite having high conductivity due to the presence of delocalized ⁇ electrons; a spherical structure in which several layers of graphitic carbon crystallites gather to form a turbulent structure Carbon black as an aggregate (acetylene black, ketjen black, other furnace blacks, channel blacks, thermal lamp blacks, etc.); a blackboard that becomes a substrate by vapor-phase pyrolysis of hydrocarbons such as methane, propane, and acetylene Examples include pyrolytic black lead deposited on a thin film.
- artificial graphite particularly high-purity artificial graphite
- acetylene black is preferred.
- “high purity” means that the ash content is 0.5 mass% or less.
- the conductive material it is preferable to use two or more types having different particle diameters in combination because it is easy to achieve both the low internal swelling of the conductive adhesive and the heat resistant adhesiveness.
- a mixture of high-purity artificial graphite powder and acetylene black can be suitably used.
- the particle diameter of acetylene black is an average particle diameter (primary particle diameter) and is usually about 10 to 50 nm. Further, it is preferable to use a high-purity artificial graphite having an average particle size of 0.5 to 20 ⁇ m, and more preferably 1 to 10 m.
- the conductive intermediate layer obtained from the conductive adhesive has a conductive material in which high-purity artificial graphite having such an average particle size and acetylene black are used in combination, thereby increasing the conductivity of the conductive intermediate layer itself. On the other hand, it is possible to ensure excellent bonding strength and internal resistance reduction effect by allowing a part of the conductive intermediate layer to enter the pores of the polarizable electrode layer described later.
- the use of a car pump rack such as acetylene black and artificial graphite as the conductive material is exposed by peeling off W or the current collector, and from the diffraction intensity curve obtained by the X-ray diffraction method on the exposed surface, the crystalline diffraction line shape based on artificial graphite and the non-based state based on carbon black A crystalline diffraction line shape is observed, which can be confirmed.
- the mixing ratio of acetylene black and high purity artificial graphite is preferably 1:10 to 1: 1 by mass ratio, more preferably 1: 3 to 1: 1. With such a mixing ratio, sufficient adhesiveness and a high internal resistance reduction effect can be ensured at the same time.
- the average particle size of the high-purity artificial graphite is a value measured by a laser particle size distribution measuring device (“SALD—200” manufactured by Shimadzu Corporation).
- SALD—200 laser particle size distribution measuring device
- the acetylene black having an average particle size within the above range may be selected according to the nominal value of the acetylene black manufacturer.
- these conductive materials have an ash content of 0.5% or less regardless of the type.
- an electrode using a carbon material having such a low ash content is applied to an electric double layer capacitor, the life of the capacitor can be extended.
- the total amount of the conductive material in the conductive adhesive is preferably 3% by mass or more and 30% by mass or less. More preferably, it is 5 mass% or more and 15 mass% or less.
- the amount of the conductive material is below the above range, the conductivity of the conductive intermediate layer may be insufficient.
- the above range is exceeded, the amount balance with the binder for forming the conductive intermediate layer (the above poly-N-vinylacetamide) is lost, and the adhesiveness tends to be lowered.
- the amount of poly 1 N-vinylacetamide in the conductive adhesive is preferably 15% by mass or less, and more preferably 10% by mass or less. If the amount of poly-N-vinylacetamide exceeds the above range, the internal resistance may increase too much.
- the amount of poly (N-vinylacetamide) in the conductive adhesive is preferably 0.5% by mass or more, and more preferably 2% by mass or more. More preferred.
- the conductive adhesive of the present invention employs a structure containing two or more kinds of conductive materials having different particle diameters, so that the conductive material having a small particle diameter that can enter the pores of the polarizable electrode layer satisfactorily.
- carbon black such as acetylene black
- a conductive material having a large particle size for example, high-purity artificial graphite
- the surface of the poly (N-vinylacetamide) particle in the dispersion medium is made of a conductive material having a small particle size. Covering can be suppressed, and when the conductive intermediate layer is formed, good heat-resistant adhesiveness can be secured.
- a polarizable electrode layer which is a component of an electrode for an electric double layer capacitor, is mixed with an electric double layer forming material (carbon electrode material) and a conductive material and a binder for ensuring conductivity. It is a porous sheet obtained by roll-rolling or roll-extrusion with ethanol or oil added.
- the electric double layer forming material used as the raw material of the polarizable electrode layer is not particularly limited as long as it is a carbonaceous material capable of forming the electric double layer, but activated carbon is typical.
- activated carbon various activated carbons generally used for carbon electrodes can be used. Specifically, charcoal, coconut husk charcoal, lignite, uncarburized materials such as sawdust, activated with a gas such as steam or carbon dioxide, or activated with chemicals such as zinc chloride, etc. Can be used.
- the shape may be powder or granular. Thus, since activated carbon has a specific surface area that is significantly increased by activation, an electrode having a large electric capacity per unit volume can be formed.
- the electric double layer forming material may be graphite-like microcrystalline carbon produced by subjecting a carbon material to activation treatment.
- This microcrystalline carbon forms an electric double layer by allowing ions or the like to enter between crystal layers when a voltage is applied.
- the microcrystalline carbon is obtained in accordance with the technique disclosed in Japanese Patent Application Laid-Open No. 11-31273-33. be able to.
- the carbon material for ensuring conductivity is not particularly limited, and for example, various conductive materials exemplified for the conductive adhesive can be used.
- fluorine resins such as polytetrafluoroethylene (PTFE), polyvinylidene fluoride (PVDF), ethylene-tetrafluoroethylene copolymer; and cellulose resins such as carboxymethylcellulose are generally used.
- PTFE polytetrafluoroethylene
- PVDF polyvinylidene fluoride
- cellulose resins such as carboxymethylcellulose
- the average pore diameter of the polarizable electrode layer is preferably 0.1 ⁇ m or more and 5 X m or less, and more preferably 0.5 m or more.
- the conductive adhesive component may not easily enter the pores of the polarizable electrode layer.
- the conductive adhesive component may be separated.
- the conductive intermediate layer that penetrates deep into the pores of the polar electrode layer and remains at the interface between the current collector and the polarizable electrode layer may become very thin, resulting in a decrease in bonding strength.
- the pores of the activated carbon are covered with the conductive adhesive component, which may reduce the capacitor performance.
- the average pore diameter referred to in the present specification is a value measured using a mercury intrusion type porosimeter (“Pore Sizer 9 3 10” manufactured by Micrometrics).
- the porosity of the polarizable electrode layer is preferably 40% or more and 90% or less, and more preferably 60% or more and 80% or less. If the porosity falls below the above range, a sufficient amount of electrolysis is required when used in a capacitor. The liquid may not be retained and internal resistance may increase. In addition, since the amount of the conductive adhesive component that can enter the pores of the polarizable electrode layer is reduced, the above-described anchor effect and internal resistance reduction effect may not be sufficiently ensured. On the other hand, when the porosity exceeds the above range, if the amount of the conductive adhesive is insufficient, there will be many voids where the conductive intermediate layer has not entered. The anchor effect may be insufficient.
- an air layer in the case of a capacitor, an electrolyte is injected to form a liquid phase portion
- an air layer in the case of a capacitor, an electrolyte is injected to form a liquid phase portion
- the above-described internal resistance reduction effect cannot be sufficiently ensured.
- the conductive intermediate layer penetrates deeply into the pores of the polarizable electrode layer. Therefore, when activated carbon is used for the polarizable electrode layer, most of the pores of the activated carbon are covered with the component, which reduces the specific surface area of the activated carbon, causing a decrease in capacity performance.
- activated carbon is used for the polarizable electrode layer, most of the pores of the activated carbon are covered with the component, which reduces the specific surface area of the activated carbon, causing a decrease in capacity performance.
- the porosity (%) in this specification is expressed as the ratio of the void volume (V.) to the total volume (V) of the polarizable electrode layer [(V.ZV) X1 0 0]. This is the required value.
- the void volume is the true density of the polarizable electrode layer (
- V 0 V-(W / p)
- the porosity and average pore size of the polarizable electrode layer can be adjusted by the type of the electric double layer forming material that is a constituent material of the polarizable electrode layer, the amount of binder, the roll pressure at the time of preparing the polarizable electrode layer, etc. .
- the thickness of the polarizable electrode layer is generally from 0.05 to 1 mm, and more preferably from 0.08 to 0,5 mm.
- the polarizable electrode layer can be manufactured by the following method. Necessary for the above-mentioned electric double layer forming material, carbon material for securing conductivity, and binder Depending on the molding aid [water, alcohol (methanol, ethanol, etc.), oil (petroleum, other oils, etc.)] added and mixed, this is rolled, extruded, etc. to form into a sheet shape. The agent can be removed to form a polarizable electrode layer.
- the mixing ratio is determined based on the electric double layer forming material: 100 parts by mass, the carbon material: 3 to 15 parts by mass, and the binder: 5 to 1. 5 parts by mass, ethanol: 50-300 parts by mass, temperature: 50-: L 00 ° C, roll-extruded, polarizable electrode having the above average pore diameter and porosity A layer can be obtained.
- the sheet-like current collector which is a component of the electric double layer capacitor electrode, but aluminum is electrically conductive. It is particularly preferable because of its excellent stability and high stability (it does not dissolve and precipitate in the electrolyte) and its cost is low. These metals can be used in any shape of foil, plate, and sheet.
- the sheet-like current collector may have a surface roughened so that irregularities are formed on the surface.
- the effect of the present invention is that the sheet-like current collector is in the form of a sheet such as a plane aluminum foil having a smooth surface. In the case of a current collector, it becomes more prominent.
- air gaps can be reduced by filling the voids that may exist at the interface for point contact between the sheet-shaped current collector and the polarizable electrode layer with the conductive intermediate layer.
- the bonding strength can be improved by the anchor effect.
- the method is not particularly limited, and known methods such as sandblasting and etching (electrolytic etching, chemical etching, etc.) can be employed. Among them, according to chemical etching using chemicals, the sheet-shaped current collector surface It is preferable because the pores and irregularities formed on the surface can be easily controlled to a shape suitable for the anchor effect of the adhesive.
- the thickness of the current collector (when the surface is roughened, the thickness before the treatment) is
- 1 to 1 0 0 111 is generally preferable, and 2 0 to 50 0 m is more preferable.
- the electrode for an electric double layer capacitor according to the present invention can be manufactured as follows. First, the conductive adhesive is applied to the polarizable electrode layer and the surface (bonding surface) of the Z or sheet current collector.
- the coated surface may be a bonded surface of either the polarizable electrode layer or the sheet-like current collector, but may be applied to both.
- the polarizable electrode layer and the sheet-like current collector are laminated so that the applied conductive adhesive is interposed.
- the laminating method may be simply overlapping and bonding, but it is preferable to pressurize and compress after bonding. By using the latter method, the bonding can be made more reliable, and a part of the conductive adhesive can be surely press-fitted into the holes of the polarized electrode layer. In addition, since the polarizable electrode layer is compressed and densified, the capacity of the polarizable electrode layer can be increased.
- the pressurizing method is not particularly limited, but for example, a method of passing between a pair of rolls is relatively simple. At this time, the clearance between the rolls with respect to the total thickness of the laminate is, for example, preferably 30 to 90%, and more preferably 50 to 70%.
- the capacity of the polarizable electrode layer can be increased. If the clearance is less than the above range, the current collector may be deformed and the polarizable electrode layer may be peeled off. Next, volatile components (such as dispersion medium) in the conductive adhesive are removed. Removal Although the leaving method is not particularly limited, for example, a hot air drying method is suitable. The hot air temperature is preferably near the boiling point of the dispersion medium. By removing the dispersion medium, a conductive intermediate layer is formed from the conductive adhesive, and the electric double layer capacitor electrode of the present invention as shown in FIG. 1 is obtained.
- Figure 1 the leaving method is not particularly limited, for example, a hot air drying method is suitable. The hot air temperature is preferably near the boiling point of the dispersion medium.
- Electrode 1 0 is a polarizable electrode layer 1 consisting of a carbonaceous electric double layer forming material, a carbon material for ensuring conductivity, and a constituent material including a binder on both sides of current collector 1 1 2 Bonded via conductive intermediate layer 1 3.
- the polarizable electrode layer 12 made of the above-described constituent material is a porous body, and a part of the conductive intermediate layer 13 enters the pores 12 a.
- the electric double layer capacitor according to the present invention uses the electric double layer capacitor electrode according to the present invention.
- a non-aqueous electrode for an electric double layer capacitor needs to be dried to remove moisture from the electrode before it is used in a capacitor.
- the electrode 10 of the present invention and the separate night 15 are combined alternately, and the drying treatment is performed in a state where a plurality of these combinations are arranged side by side as shown in FIG. Can be applied.
- the drying temperature can be set to 20 ° C. or higher, preferably 25 ° C. or higher, in order to increase the productivity of the electric double layer capacitor.
- a case (metal case, etc.) having an upper lid 21 and a current collecting lead 23 is accommodated in the combination of the above electrode and separate overnight, and further the electrode
- An electric double layer capacitor can be obtained by filling electrolyte 2 2 between 10 and separator 15.
- PTFE polyethylene, polypropylene and other porous sheets made hydrophilic Examples include porous sheets obtained from colander;
- Electrolyte electrolytes include tetrafluoroboric acid, hexafluorophosphoric acid, hexafluoroarsenic acid
- Fluorine-containing acids such as hexafluoroantimonic acid and trifluoroalkylsulfonic acid; Chlorine-containing acids such as perchloric acid and tetrachloroaluminic acid; Acids such as alkali metal salts (sodium salt, strength lithium) Salts), alkaline earth metal salts (magnesium salts, calcium salts, etc.)
- Ammonium salt tetraalkyl ammonium salt (tetramethylammonium salt, tetraethylammonium salt, etc.), tetraalkylphosphonium salt (tetramethylphosphonium salt, tetraethylphosphonium salt, etc.) ) Can be illustrated.
- 9 is a current collecting terminal attached to the current collector, and a current collecting lead (not shown) is attached to this current collecting terminal 9. Also, among the plurality of electrodes arranged side by side, For what is provided in the
- the electrode for electric double layer capacity of the present invention since the electrode for electric double layer capacity of the present invention that achieves a lower internal resistance than before is used, the internal resistance is low, the electric capacity is high, and the output is high. Can demonstrate density
- Activated carbon powder (“YP-1 17” manufactured by Kuraray Chemical Co., Ltd., specific surface area: 1500 m 2 / g, average particle size: 8 xm): 85 parts by mass, Ketjen Black (Ketjen Blackin Yu National Corporation) EC: 600 JD ”)): 7 parts by mass, PTFE powder: 8 parts by mass of ethanol: 100 parts by mass of ethanol, kneaded and subjected to squeeze rolling, width: 1 0 0 A long polarizable electrode layer was obtained with mm, thickness: 0.15 mm, porosity: 65%, and average pore diameter: 0.8 m.
- plain aluminum two-foil width: 150 mm, thickness: 30 m, “A1N30H-H18” manufactured by Nihon Foil Co., Ltd. was used.
- high-purity artificial graphite with an average particle size of 8 (“SP — 2 70” manufactured by Nippon Graphite Industries Co., Ltd.) and average particle size (primary particle size) of acetylene black of 35 ⁇ m (Electrochemical Industry) “Denka Black” manufactured by the company was used.
- Poly N-vinylacetamide (“P NVA G E 1 9 1 — 2 0 3” manufactured by Showa Denko KK) was used as the binder. These were mixed so as to have the composition shown in Table 1 to obtain a conductive adhesive.
- a conductive adhesive was applied to both sides of the current collector using an application roll.
- the coating amount is 12 g / m 2 per side (approx. 2 g / m 2 after drying) It was.
- a long polar electrode layer was layered on the conductive adhesive application surface (both sides) of the current collector, and a laminated sheet was passed through a compression roll (clearance: 70%).
- the laminated sheet was passed through a continuous hot air dryer set at a temperature of 1550 ° C. in 3 minutes, and the dispersion medium was removed from the conductive adhesive to obtain a long electrode.
- a plurality of electrodes were punched out of the long electrode so that the electrode adhesion part had a square shape of 10 cm and the current collector part had a shape of 2 cm ⁇ 10 cm. After that, 15 pairs of these electrodes and separators as shown in Fig. 2 were stacked. In addition, in the separator evening, the separator porous evening made from the stretched porous PTFE membrane (“BSP 0 1 0 2 5 6 0-2” manufactured by Japan Gore-Tex, Inc.), thickness: 25 ⁇ m, porosity: 60%) was used. These electrode groups were vacuum dried at 25 ° C. for 72 hours for Example and Comparative Example 3, dried for 2 hours at 20 ° C. for Comparative Example 1, and 150 ° C. for Comparative Example 2.
- the product was stored in an aluminum case, and then a current collecting lead was attached to each current collecting terminal, and a positive electrode terminal and a negative electrode terminal were further attached to the current collecting leads.
- a tetrapropylammonium tetrafluoroborate propylene carbonate solution (concentration: lmo 1 / L) is injected into the case as an electrolyte, and the case is sealed by attaching the top lid. Electric double layer capacity was obtained.
- a slit is made in the shape of a grid on the polarizable electrode layer part (one eye is 5 X 5 mm, 144).
- Adhesive tape (made by Nitto Denko “Dump mouth” Nice II ”) was applied and pressed with enough fingers to remove air bubbles between the polarizable electrode layer and the adhesive tape, and then the tape was peeled off, and the peeled state of the polarizable electrode layer was observed.
- Example 3 An electrode and an electric double layer capacitor were prepared and evaluated in the same manner as in Example 1 except that the configuration of the conductive adhesive was changed as shown in Table 1. The results are shown in Table 2 and Table 3. Example 3
- Example 2 For the conductive adhesive, an electrode and an electric double layer capacitor were prepared in the same manner as in Example 1 except that carboxymethyl cellulose (“CMC Daicel” manufactured by Daicel Chemical Industries, Ltd.) was used instead of PNVA. Evaluation was performed. The results are shown in Table 2 and Table 3.
- CMC Daicel carboxymethyl cellulose
- thermosetting polyimide (“U-varnish” manufactured by Ube Industries, Ltd.) was used instead of PNVA. Fabricated and evaluated. The results are shown in Tables 2 and 3.
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
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CN2009801178282A CN102027555A (zh) | 2008-05-13 | 2009-05-13 | 导电性粘接剂以及使用该粘接剂的双电层电容器用电极和双电层电容器 |
KR1020107025428A KR101162464B1 (ko) | 2008-05-13 | 2009-05-13 | 도전성 접착제 및 그것을 이용한 전기 이중층 캐패시터용 전극 및 전기 이중층 캐패시터 |
US12/990,638 US8456802B2 (en) | 2008-05-13 | 2009-05-13 | Conductive adhesive and electrode for electric double layer capacitor and electric double layer capacitor employing it |
EP09746699.9A EP2278597A4 (en) | 2008-05-13 | 2009-05-13 | CONDUCTIVE ADHESIVE, ELECTRODE WITH DOUBLE-LAYER ELECTRICAL CAPACITOR USING THE SAME, AND DOUBLE-LAYER ELECTRICAL CAPACITOR |
Applications Claiming Priority (2)
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JP2008126077A JP2009277783A (ja) | 2008-05-13 | 2008-05-13 | 導電性接着剤ならびにそれを用いた電気二重層キャパシタ用電極および電気二重層キャパシタ |
JP2008-126077 | 2008-05-13 |
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PCT/JP2009/059234 WO2009139493A1 (ja) | 2008-05-13 | 2009-05-13 | 導電性接着剤ならびにそれを用いた電気二重層キャパシタ用電極および電気二重層キャパシタ |
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US (1) | US8456802B2 (ja) |
EP (1) | EP2278597A4 (ja) |
JP (1) | JP2009277783A (ja) |
KR (1) | KR101162464B1 (ja) |
CN (1) | CN102027555A (ja) |
WO (1) | WO2009139493A1 (ja) |
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WO2012027102A1 (en) * | 2010-08-23 | 2012-03-01 | Corning Incorporated | Dual-layer method of fabricating ultracapacitor current collectors |
WO2011149807A3 (en) * | 2010-05-27 | 2012-03-01 | Corning Incorporated | Multi-layered electrode for ultracapacitors |
JP2015095275A (ja) * | 2013-11-08 | 2015-05-18 | 株式会社豊田自動織機 | 集電体の製造方法 |
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US8200466B2 (en) | 2008-07-21 | 2012-06-12 | The Board Of Trustees Of The Leland Stanford Junior University | Method for tuning patient-specific cardiovascular simulations |
US9405886B2 (en) | 2009-03-17 | 2016-08-02 | The Board Of Trustees Of The Leland Stanford Junior University | Method for determining cardiovascular information |
WO2011024798A1 (ja) * | 2009-08-27 | 2011-03-03 | 大日精化工業株式会社 | 水系の炭素フィラー分散塗工液、導電性付与材料、蓄電装置用電極板、蓄電装置用電極板の製造方法及び蓄電装置 |
US8315812B2 (en) | 2010-08-12 | 2012-11-20 | Heartflow, Inc. | Method and system for patient-specific modeling of blood flow |
EE05629B1 (et) * | 2010-09-06 | 2013-02-15 | O� Skeleton Technologies | Meetod suure eriv?imsuse ja energiatihendusega superkondensaatori elektrokeemilise süsteemi valmistamiseks, sellele vastav superkondensaator ja meetod selle valmistamiseks |
FR2977364B1 (fr) * | 2011-07-01 | 2015-02-06 | Hutchinson | Collecteur de courant et procede de fabrication correspondant |
KR101994705B1 (ko) * | 2011-11-22 | 2019-07-17 | 삼성전기주식회사 | 에너지 저장체의 전극 및 에너지 저장체의 전극 제조방법 |
JP2013211345A (ja) | 2012-03-30 | 2013-10-10 | Nihon Gore Kk | 電気二重層キャパシタ用の分極性電極 |
US9595398B2 (en) | 2013-08-30 | 2017-03-14 | Corning Incorporated | Low resistance ultracapacitor electrode and manufacturing method thereof |
JP6743699B2 (ja) * | 2014-08-11 | 2020-08-19 | 株式会社Gsユアサ | 非水電解質蓄電素子用正極板、及び非水電解質蓄電素子 |
KR102272893B1 (ko) * | 2016-11-07 | 2021-07-05 | 쥐알에스티 인터내셔널 리미티드 | 전지용 애노드 슬러리의 제조 방법 |
JP2017118136A (ja) * | 2017-02-22 | 2017-06-29 | 日本ゴア株式会社 | 電気二重層キャパシタ用の分極性電極 |
CN108565382A (zh) * | 2018-04-28 | 2018-09-21 | 上海恩捷新材料科技股份有限公司 | 一种水性涂层锂离子电池隔膜及其制备方法 |
TW202022063A (zh) * | 2018-09-13 | 2020-06-16 | 日商昭和電工股份有限公司 | 導電性墨及碳配線基板 |
KR102239685B1 (ko) | 2018-09-20 | 2021-04-14 | (주) 퓨리켐 | 활성탄으로 이루어진 도전성 접착제, 이를 이용한 전극 집전체, 슈퍼커패시터용 전극 및 고온 성능이 우수한 슈퍼커패시터 |
JP6712758B2 (ja) * | 2019-01-16 | 2020-06-24 | 日本ゴア合同会社 | 電気二重層キャパシタ用の分極性電極 |
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JPH11154630A (ja) * | 1997-09-22 | 1999-06-08 | Japan Gore Tex Inc | 分極性電極体及びその製造方法 |
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- 2009-05-13 EP EP09746699.9A patent/EP2278597A4/en not_active Withdrawn
- 2009-05-13 WO PCT/JP2009/059234 patent/WO2009139493A1/ja active Application Filing
- 2009-05-13 US US12/990,638 patent/US8456802B2/en not_active Expired - Fee Related
- 2009-05-13 CN CN2009801178282A patent/CN102027555A/zh active Pending
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WO2011149807A3 (en) * | 2010-05-27 | 2012-03-01 | Corning Incorporated | Multi-layered electrode for ultracapacitors |
US8687346B2 (en) | 2010-05-27 | 2014-04-01 | Corning Incorporated | Multi-layered electrode for ultracapacitors |
WO2012027102A1 (en) * | 2010-08-23 | 2012-03-01 | Corning Incorporated | Dual-layer method of fabricating ultracapacitor current collectors |
US8840687B2 (en) | 2010-08-23 | 2014-09-23 | Corning Incorporated | Dual-layer method of fabricating ultracapacitor current collectors |
JP2015095275A (ja) * | 2013-11-08 | 2015-05-18 | 株式会社豊田自動織機 | 集電体の製造方法 |
Also Published As
Publication number | Publication date |
---|---|
KR101162464B1 (ko) | 2012-07-04 |
EP2278597A1 (en) | 2011-01-26 |
US20110043966A1 (en) | 2011-02-24 |
JP2009277783A (ja) | 2009-11-26 |
CN102027555A (zh) | 2011-04-20 |
US8456802B2 (en) | 2013-06-04 |
KR20110002476A (ko) | 2011-01-07 |
EP2278597A4 (en) | 2013-11-06 |
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