JP2008085358A - 電気二重層キャパシタ電極用炭素材 - Google Patents
電気二重層キャパシタ電極用炭素材 Download PDFInfo
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- 239000003575 carbonaceous material Substances 0.000 title claims abstract description 60
- 239000003990 capacitor Substances 0.000 title claims abstract description 29
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 30
- 230000004913 activation Effects 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 20
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 14
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- 230000001590 oxidative effect Effects 0.000 claims abstract description 8
- 238000004438 BET method Methods 0.000 claims abstract description 6
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- 238000001179 sorption measurement Methods 0.000 claims description 8
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- 239000011295 pitch Substances 0.000 description 33
- 238000001994 activation Methods 0.000 description 23
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- 229910002804 graphite Inorganic materials 0.000 description 5
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- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 5
- -1 Aliphatic alcohols Chemical class 0.000 description 4
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 3
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- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 3
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- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 2
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- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 2
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 2
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- ZUOUZKKEUPVFJK-UHFFFAOYSA-N diphenyl Chemical compound C1=CC=CC=C1C1=CC=CC=C1 ZUOUZKKEUPVFJK-UHFFFAOYSA-N 0.000 description 2
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- KTHUKEZOIFYPEH-UHFFFAOYSA-N 1-benzylnaphthalene Chemical compound C=1C=CC2=CC=CC=C2C=1CC1=CC=CC=C1 KTHUKEZOIFYPEH-UHFFFAOYSA-N 0.000 description 1
- KZNJSFHJUQDYHE-UHFFFAOYSA-N 1-methylanthracene Chemical compound C1=CC=C2C=C3C(C)=CC=CC3=CC2=C1 KZNJSFHJUQDYHE-UHFFFAOYSA-N 0.000 description 1
- IYDMICQAKLQHLA-UHFFFAOYSA-N 1-phenylnaphthalene Chemical compound C1=CC=CC=C1C1=CC=CC2=CC=CC=C12 IYDMICQAKLQHLA-UHFFFAOYSA-N 0.000 description 1
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- XTHFKEDIFFGKHM-UHFFFAOYSA-N Dimethoxyethane Chemical compound COCCOC XTHFKEDIFFGKHM-UHFFFAOYSA-N 0.000 description 1
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 1
- 229910013063 LiBF 4 Inorganic materials 0.000 description 1
- 229910013684 LiClO 4 Inorganic materials 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 229910005580 NiCd Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 229920006282 Phenolic fiber Polymers 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000004809 Teflon Substances 0.000 description 1
- 229920006362 Teflon® Polymers 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003570 air Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 235000010290 biphenyl Nutrition 0.000 description 1
- 239000004305 biphenyl Substances 0.000 description 1
- 239000001273 butane Substances 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- KRVSOGSZCMJSLX-UHFFFAOYSA-L chromic acid Substances O[Cr](O)(=O)=O KRVSOGSZCMJSLX-UHFFFAOYSA-L 0.000 description 1
- 239000011335 coal coke Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
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- 239000011530 conductive current collector Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 239000011888 foil Substances 0.000 description 1
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- 239000006232 furnace black Substances 0.000 description 1
- AWJWCTOOIBYHON-UHFFFAOYSA-N furo[3,4-b]pyrazine-5,7-dione Chemical compound C1=CN=C2C(=O)OC(=O)C2=N1 AWJWCTOOIBYHON-UHFFFAOYSA-N 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 238000005087 graphitization Methods 0.000 description 1
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000004898 kneading Methods 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
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- 238000002844 melting Methods 0.000 description 1
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- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
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- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
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- 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
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
-
- 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
-
- 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
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/60—Other road transportation technologies with climate change mitigation effect
- Y02T10/70—Energy storage systems for electromobility, e.g. batteries
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- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
【解決手段】窒素吸着BET法により求めた比表面積が1000m2/g以上1900m2/g以下、X線回折法により求められる平均層面間隔が0.36nm以下である炭素材を、好ましくはピッチを原料として得られた熱に対し不融性の多孔性のピッチ系炭素前駆体に酸化性ガス雰囲気下700℃以上1500℃以下で賦活処理を施すことにより形成する。
【選択図】 図1
Description
「窒素吸着BET法による表面積」:BETの式から誘導された近似式
Vm=1/{V(1−x)}
を用いて液体窒素温度における、窒素吸着による1点法(相対圧力x=0.3)によりVmを求め、次式により試料の比表面積を計算した。
ここに、Vmは試料表面に単分子層を形成するに必要な吸着量(cm3/g)、Vは実測される吸着量(cm3/g)、xは相対圧力である。具体的には、MICROMERITICS社製「Flow Sorb II 2300」を用いて、以下のようにして液体窒素温度における炭素材への窒素の吸着量を測定した。粒子径約5〜50μmに粉砕した炭素材を試料管に充填し、窒素ガスを30モル%濃度で含有するヘリウムガスを流しながら、試料管を−196℃に冷却し、炭素材に窒素を吸着させる。つぎに試料管を室温に戻す。このとき試料から脱離してくる窒素量を熱伝導度型検出器で測定し、吸着ガス量Vとした。
軟化点210℃、キノリン不溶分1重量%、H/C原子比0.63の石油系ピッチ68kgと、ナフタレン32kgとを、撹拌翼のついた内容積300リットルの耐圧容器に仕込み、190℃で加熱溶融混合を行った後、80〜90℃に冷却して押し出し、径約500μmの紐状成形体を得た。次いで、この紐状成形体を直径と長さの比が約1.5になるように破砕し、得られた破砕物を93℃に加熱した0.53重量%のポリビニルアルコール(ケン化度88%)を溶解した水溶液中に投入し、撹拌分散し、冷却して球状ピッチ成形体スラリーを得た。大部分の水をろ過により除いた後、球状ピッチ成形体の約6倍量の重量のn−ヘキサンでピッチ成形体中のナフタレンを抽出除去した。この様にして得た多孔性球状ピッチを、流動床を用いて、加熱空気を通じながら、260℃まで昇温し、260℃に1時間保持して酸化し、熱に対して不融性の多孔性球状ピッチ成形体を得た。得られた熱に対して不融性の多孔性ピッチ成形体を流動床を用いて、H2Oを50モル%含有する窒素と水蒸気の混合ガス中、300℃〜900℃まで200℃/時間で昇温し、900℃で120分間水蒸気賦活処理を行い比表面積が1000m2/gの球状炭素材(活性炭)を得た。得られた球状炭素材を平均粒径約30μmに粉砕し、電極用炭素材とした。
水蒸気賦活時間を140分とした以外、実施例1と同様にして電極用炭素材を調製した。
水蒸気賦活時間を200分とした以外、実施例1と同様にして電極用炭素材を調製した。
水蒸気賦活時間を240分とした以外、実施例1と同様にして電極用炭素材を調製した。
水蒸気賦活時間を60分とした以外、実施例1と同様にして電極用炭素材を調製した。
水蒸気賦活時間を270分とした以外、実施例1と同様にして電極用炭素材を調製した。
石炭コークスをアルカリ賦活し調製した高比表面積活性炭(「30SPD」、関西熱化学株式会社製)を電極用炭素材として使用した。
フェノール樹脂から調製した活性炭(「BP12」、鐘紡株式会社製)を電極用炭素材として使用した。
フェノール樹脂から調製した活性炭(「BP25」、鐘紡株式会社製)を電極用炭素材として使用した。
実施例及び比較例で得られた各炭素材を用いて、以下のようにして電気二重層キャパシタを作製し、その性能評価を行った。
静電容量(F)=2×合計放電エネルギー(W・s)/(放電開始電圧(V))2
の関係式を用いて評価セルの静電容量を求め、この静電容量を分極性電極材料の炭素材重量(正極+負極:g)で除し値を単位重量当たりの静電容量(F/g)とした。単位重量当たりの静電容量の値に分極性電極材料の嵩密度(g/cm3)を乗じた値を単位容積当たりの静電容量(F/cm3)とした。
2 負極
3 ガラスフィルター
4 容器
5 電解液
6 上ぶた
7 スプリング
8 正極集電体
9 Oリング
Claims (2)
- 酸化性ガス雰囲気下700℃以上1500℃以下での賦活処理を経て得られた窒素吸着BET法により求めた比表面積が1000m2/g以上1900m2/g以下、X線回折法により求められる平均層面間隔が0.36nm以下であることを特徴とする電気二重層キャパシタ電極用炭素材。
- 熱に対し不融性の多孔性のピッチ系炭素前駆体の賦活処理により得られた請求項1記載の電気二重層キャパシタ電極用炭素材。
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JP2010177284A (ja) * | 2009-01-27 | 2010-08-12 | Toyota Central R&D Labs Inc | 蓄電デバイス |
JP2015130479A (ja) * | 2013-12-02 | 2015-07-16 | 株式会社佐藤工務所 | 電気二重層キャパシタの製造方法 |
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JPH05139712A (ja) * | 1991-11-19 | 1993-06-08 | Koa Oil Co Ltd | 導電性多孔質炭素材の製造方法 |
JPH09241930A (ja) * | 1996-03-01 | 1997-09-16 | Petoca:Kk | 活性炭素繊維成形体の製造方法および活性炭素繊維成形体 |
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JPH05139712A (ja) * | 1991-11-19 | 1993-06-08 | Koa Oil Co Ltd | 導電性多孔質炭素材の製造方法 |
JPH09241930A (ja) * | 1996-03-01 | 1997-09-16 | Petoca:Kk | 活性炭素繊維成形体の製造方法および活性炭素繊維成形体 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2010177284A (ja) * | 2009-01-27 | 2010-08-12 | Toyota Central R&D Labs Inc | 蓄電デバイス |
JP2015130479A (ja) * | 2013-12-02 | 2015-07-16 | 株式会社佐藤工務所 | 電気二重層キャパシタの製造方法 |
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