JP2006093401A - 電気二重層キャパシタの電極用炭素材の原料炭組成物 - Google Patents
電気二重層キャパシタの電極用炭素材の原料炭組成物 Download PDFInfo
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- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910000831 Steel Inorganic materials 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
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- 238000004438 BET method Methods 0.000 description 1
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- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 description 1
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- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
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- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- 229910001942 caesium oxide Inorganic materials 0.000 description 1
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- 229920006037 cross link polymer Polymers 0.000 description 1
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 description 1
- 238000011549 displacement method Methods 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
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- 229940021013 electrolyte solution Drugs 0.000 description 1
- 238000000921 elemental analysis Methods 0.000 description 1
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 description 1
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- ZTOMUSMDRMJOTH-UHFFFAOYSA-N glutaronitrile Chemical compound N#CCCCC#N ZTOMUSMDRMJOTH-UHFFFAOYSA-N 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
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- 229910052700 potassium Inorganic materials 0.000 description 1
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- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 1
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- 229910052715 tantalum Inorganic materials 0.000 description 1
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- 239000011269 tar Substances 0.000 description 1
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- 239000010936 titanium Substances 0.000 description 1
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Classifications
-
- 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
-
- Y02T10/7022—
Landscapes
- Carbon And Carbon Compounds (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
【解決手段】 賦活処理を施されることで、電気二重層キャパシタの電極用炭素材となる原料炭組成物であって、マイクロ強度の値が5〜30%であり、揮発分が1.3質量%以上6質量%未満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の原料炭組成物。
【選択図】 なし
Description
JIS M8813「石炭類及びコークス類−元素分析方法」に記載の方法に準拠して測定した。
IP 143/90「Determination of Asphaltenes ( Heptane Insolubles )」に記載の方法に準拠して測定した。
JIS M8812「石炭類及びコークス類−工業分析法」に記載の方法に準拠して測定した。
試料(原料炭組成物)に対して15%のシリコン粉末を混合して測定用セルに充填し、CuKα線を線源とし、X線回折装置(理学電機株式会社製、商品名:RINT1400VX)を用いて反射式ディフラクトメーター法によって広角X線回折線を測定し、学振法に基づき(002)面の平均層間距離(d002)を求めた。
顕微鏡に偏光板としてポラライザーとアナライザーを用い、これらの振動方向を直交させた直交ニコル下で検体を観察した。検体が等方性ならば、載物台に載せた検体視野は暗く、検体を回転しても何の変化がなく、一方、光学的に異方性の場合であれば、載物台を回転すると、明暗が規則的に変化する。
(i)原料炭組成物の製造
石油重質油の流動接触分解装置のボトム油90Vol%に減圧蒸留装置の残渣油を10Vol%ブレンドした(硫黄分0.17質量%、アスファルテン量0.9質量%)。この重質油混合物を500℃、1.0時間で炭素化(コーキング)させることにより、揮発分5.8質量%、マイクロ強度7%の原料炭組成物を得た。なお、このようにして得られた原料炭組成物は、偏光顕微鏡観察*で、組織を観察すると光学的異方性組織で流れ模様が主体であった。また、微結晶炭素の平均層間距離d002は0.346nmであり、気孔率は22%であった。
上記の原料炭組成物100質量部に対して水酸化カリウムが200質量部となるように混合し、窒素ガス雰囲気中、750℃で1時間賦活反応を進行させ、反応後に水洗及び酸洗浄(HClを使用)して炭素材に残存ずる金属カリウムを除去し、乾燥して電気二重層キャパシタの電極用炭素材を得た。この炭素材の比表面積は1980m2/gであった。また、細孔容積は0.95cm3/g、細孔直径は1.9nmであった。
平均粒径10μmに粉砕した上記炭素材80質量部にカーボンブラックを10質量部、ポリテトラフルオロエチレン粉末を10質量部加え、乳鉢でペースト状となるまで混錬した。次いで、得られたペーストを180kPaのローラープレスで圧延して、厚さ200μmの電極シートを作製した。
上記電極シートから直径16mmの円盤状ディスクを2枚打ち抜き、120℃、0.1Torrで2時間真空乾燥した後、露点−85℃の窒素雰囲気下のグローブボックス中にて、有機電解液(トリエチルメチルアンモニウムテトラフルオロボレートのプロピレンカーボネート溶液、濃度:1モル/リットル)を真空含浸せしめた。次に、2枚の電極を各々正極、負極とし、両極間にガラス繊維セパレータ(ADVANTEC社製、商品名:GA−200、厚さ:200μm)、両端にはアルミ箔の集電体を取り付け、宝泉社製の2極式セルに組み込んで電気二重層キャパシタ(コイン型セル)を作製した。
上記コイン型セルに1F当たり10mAの定電流で2.7Vまで充電した。充電終了後12時間2.7Vに保持した後、10mAの定電流放電を行なった。そして、放電時のエネルギー量から以下の式:
合計放電エネルギーW[W・s]={静電容量C[F]×(放電開始電圧V[V])2}/2
に従って静電容量を算出した。
実施例1の原料炭組成物をさらに不活性ガス雰囲気で、650℃で1時間処理し、揮発分3.3質量%、マイクロ強度13%の原料炭組成物を得た。また、微結晶炭素の平均層間距離d002は0.344nmであり、気孔率は24%であった。その後、実施例1と同様にアルカリ賦活処理して電極用炭素材を得た。この炭素材の比表面積は900m2/g、細孔容積は0.47cm3/g、細孔直径は2.0nmであった。この炭素材を用いて、実施例1と同様に電極を作製し、セルを組み立て、静電容量を測定した結果、単位体積当たりの静電容量(F/cc)は34F/ccであった。
実施例1の原料炭組成物を不活性ガス雰囲気で、さらに750℃で1時間処理し、揮発分1.7質量%、マイクロ強度18%の原料炭組成物を得た。また、微結晶炭素の平均層間距離d002は0.343nmであり、気孔率は25%であった。その後、実施例1と同様にアルカリ賦活処理して電極用炭素材を得た。この炭素材の比表面積は600m2/g、細孔容積は0.30cm3/g、細孔直径は2.1nmであった。)この炭素材を用いて、実施例1と同様に電極を作製し、セルを組み立て、静電容量を測定した結果、単位体積当たりの静電容量(F/cc)は35F/ccであった。
実施例1の原料組成物を用い、原料炭組成物100質量部に対して水酸化ナトリウムが200質量部となるように混合し、窒素ガス雰囲気中、600℃で1時間賦活反応を進行させた、
その後、実施例1と同様にアルカリ賦活処理して電極用炭素材を得た。この炭素材の比表面積は800m2/g、細孔容積は0.45cm3/g、細孔直径は2.2nmであった。この炭素材を用いて、実施例1と同様に電極を作製し、セルを組み立て、静電容量を測定した結果、単位体積当たりの静電容量(F/cc)は40F/ccであった。
石油重質油の流動接触分解装置のボトム油90Vol%に減圧蒸留装置の残渣油を10Vol%ブレンドし、この重質混合油を470℃で1時間処理して炭素化させることにより、揮発分11質量%、マイクロ強度3%、気孔率17%、d0020.350の原料炭組成物を得た。なお、このようにして得られた原料炭組成物は、偏光顕微鏡観察で、組織を観察すると光学的異方性組織で流れ模様が主体であった。
石油重質油の流動接触分解装置のボトム油10Vol%に減圧蒸留装置の残渣油を90Vol%ブレンドし(硫黄分4.5質量%、アスファルテン量15.0質量%)、500℃で炭素化させることにより、揮発分6.3質量%,マイクロ強度22%の原料炭組成物を得た。なお、このようにして得られた原料炭組成物は、偏光顕微鏡観察で、組織を観察すると光学的異方性組織でモザイク模様が主体であった。
比較例1の原料炭組成物を不活性ガス雰囲気で、650℃で1時間処理し、揮発分3.6質量%,マイクロ強度4%、気孔率39%の原料炭組成物を得た。実施例1と同様にして、セルを組み立て、静電容量を測定した結果、単位体積当たりの静電容量(F/cc)は25F/ccであった。
実施例1の原料炭組成物を不活性ガス雰囲気で、さらに900℃で1時間処理し、揮発分1.0質量%、マイクロ強度25%、気孔率35%、d0020.343の原料炭組成物を得た。その後、実施例1と同様にアルカリ賦活して比表面積50m2/gの電極用炭素材を得た。実施例1と同様にして、セルを組み立て、静電容量を測定した結果、単位体積当たりの静電容量(F/cc)は15F/ccであった。
Claims (7)
- 賦活処理を施されることで、電気二重層キャパシタの電極用炭素材となる原料炭組成物であって、
マイクロ強度の値が5〜30%であり、揮発分が1.3質量%以上6質量%未満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の原料炭組成物。 - 黒鉛類似の微結晶炭素を有することを特徴とする請求項1記載の原料炭組成物。
- 気孔率が20〜30%であることを特徴とする請求項1記載の原料組成物。
- 請求項1〜3のいずれかに記載の原料炭組成物を賦活処理することにより得られる電気二重層キャパシタの電極用炭素材。
- 前記賦活処理がアルカリ金属化合物を用いた賦活処理であることを特徴とする請求項4記載の電気二重層キャパシタの電極用炭素材。
- 前記アルカリ金属化合物が水酸化ナトリウムであることを特徴とする請求項5記載の電気二重層キャパシタの電極用炭素材。
- 請求項4〜6のいずれかに記載の電極用炭素材を含む電極を備えることを特徴とする電気二重層キャパシタ。
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JP2008181949A (ja) * | 2007-01-23 | 2008-08-07 | Hitachi Chem Co Ltd | 電気二重層キャパシタ用電極材及び電気二重層キャパシタ |
JP2009013012A (ja) * | 2007-07-04 | 2009-01-22 | Nippon Oil Corp | 電気二重層キャパシタ電極用活性炭の製造方法 |
WO2011152426A1 (ja) * | 2010-05-31 | 2011-12-08 | Jx日鉱日石エネルギー株式会社 | リチウムイオン二次電池負極材料用原料炭組成物 |
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JP2008181949A (ja) * | 2007-01-23 | 2008-08-07 | Hitachi Chem Co Ltd | 電気二重層キャパシタ用電極材及び電気二重層キャパシタ |
JP2009013012A (ja) * | 2007-07-04 | 2009-01-22 | Nippon Oil Corp | 電気二重層キャパシタ電極用活性炭の製造方法 |
WO2011152426A1 (ja) * | 2010-05-31 | 2011-12-08 | Jx日鉱日石エネルギー株式会社 | リチウムイオン二次電池負極材料用原料炭組成物 |
JP5728475B2 (ja) * | 2010-05-31 | 2015-06-03 | Jx日鉱日石エネルギー株式会社 | リチウムイオン二次電池負極材料用原料炭組成物 |
KR101821838B1 (ko) * | 2010-05-31 | 2018-01-24 | 제이엑스티지 에네루기 가부시키가이샤 | 리튬 이온 이차 전지 부극 재료용 원료탄 조성물 |
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