JP2007243153A - 電気二重層キャパシタ用正電極及び電気二重層キャパシタ - Google Patents
電気二重層キャパシタ用正電極及び電気二重層キャパシタ Download PDFInfo
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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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
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Abstract
【解決手段】結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20%以上である、電気二重層キャパシタの電極活物質用炭素質材料。
【選択図】なし
Description
R(%)=(I(101−R)/I(101−H))×100 (1)
[式中、I(101−R)はX線結晶回折スペクトルにおける菱面体晶(101)面に帰属するピークの積分強度であり、I(101−H)はX線結晶回折スペクトルにおける六方晶(101)面に帰属するピークの積分強度である。]
で示す構造を有する。ピロリジニウム化合物塩は公知であり、当業者に知られた方法で合成されたものであればよい。
黒鉛粒子1は、黒鉛をメディアを用いて摩砕することにより平均粒子径が5ミクロン程度となるように調整された薄片化黒鉛粒子である。
黒鉛粒子2〜5は、黒鉛1を更に磨砕することで、菱面体晶の割合を表3のように調整したものである。
黒鉛粒子6〜10は、菱面体晶の割合が表3のようになるようにあらかじめ調整された人造黒鉛である。
(1)X線結晶解析
X線回折装置(株式会社リガク製「RINT-UltimaIII」)を用い、黒鉛粒子を測定した。得られたX線回折スペクトルを分析して、(002)面の結晶格子定数(C0(002))、平均面間隔d002(オングストローム)及び(002)ピーク(2θ=26.5°付近にあるピーク)の半値幅を決定した。ターゲットをCuKαとし、40kV,50mA(:今一度確認させてください。)にて測定を行った。
ラマン分光装置(日本分光株式会社製「レーザラマン分光光度計NRS−3100」)を用い、黒鉛粒子を下記条件にて測定した。
(1)黒鉛複合粒子
A)CVDによる処理:900から1100℃に昇温された炉内の石英製キュベットに黒鉛粒子5を静置し、これにアルゴンガスをキャリアとしてベンゼン蒸気を導入し、キシレンを黒鉛上に析出炭化させる。析出炭素量を種々変更し実施した。
B)樹脂被覆処理1:ベークライト樹脂の溶液(群栄化学:レジトップ)を種々の濃度に調整した。次に黒鉛粒子5をこれら溶液に浸し、乾燥した。窒素気流中にて600℃で焼成し、樹脂を炭化した。
C)樹脂被覆処理2:キシレン溶解性の石炭ピッチの溶液(新日鐵化学)を溶剤にて種々の濃度に調整した。次に黒鉛粒子5をこれら溶液に浸し、乾燥した。窒素気流中にて600℃で焼成し、樹脂分を炭化した。
(2)非多孔性炭素複合粒子
A)黒鉛粒子5の代わりに非多孔性炭素粒子1を用いること以外は黒鉛−炭素複合粒子の場合と同様にして、CVDによる処理を行なった。
(3)活性炭複合粒子
A)黒鉛粒子5の代わりに活性炭粒子1を用いること以外は黒鉛−炭素複合粒子の場合と同様にして、CVDによる処理を行なった。
(1)炭素電極の製造
炭素粒子1を3g、アセチレンブラック(電気化学工業製)1g、ポリテトラフルオロエチレン粉末(三井・デュポンフロロケミカル製)0.3gを混合し、めのう乳鉢を用いて混練した。成形装置を用いて、混練物を0.4mmの均一な厚みのシート状に成形して正電極を得た。
活性炭(関西熱化学製「MSP20」)、アセチレンブラック(電気化学工業製)、及びポリビニリデンフロリド(PVDF)のn-メチルピロリドン溶液(クレハ化学製)を適量混合し、めのう乳鉢を用いて混練した。成形装置を用いて、混練物を0.4mmの均一な厚みのシート状に成形して、負電極を得た。
組み立てた電気二重層キャパシタにパワーシステム製充放電試験装置「CDT−RD20」を接続し、5mAにて7200秒間の定電流充電を行い、設定電圧に到達した後、5mAにての定電流放電を行った。設定電圧は3.5Vとし、3サイクル実施し3サイクル目のデータを採用した。
放電電力より正極活物質重量あたりの容量(mAh/g)を算出した。結果を表4に示す。
正電極の炭素質材料として、黒鉛粒子1の代わりに黒鉛粒子2〜10を用いること以外は実施例1と同様にして電気二重層キャパシタを製造し、試験した。試験結果を表4に示す。
黒鉛粒子1の代わりに黒鉛粒子5及び6、非多孔性炭素1及び2を用いること以外は実施例1と同様にして正電極を製造した。そして、これと同じ方法により、負電極をも製造した。得られた正電極および負電極を用いること以外は実施例1と同様にして、電気二重層キャパシタを製造し、試験した。試験結果を表4に示す。
正電極の炭素質材料として、表5に示す炭素複合粒子を用い、負電極の炭素質材料、および電解液の種類を表5に示すように変更すること以外は実施例1と同様にして電気二重層キャパシタを製造し、試験し、容量を算出した。
表5
炭素1:非多孔性炭素1
SBPPF6:スピロビピロリジニウム六フッ化燐塩のプロピレンカーボネート溶液(2.0モル%)
EMIPF6:エチルメチルイミダゾリウム六フッ化燐塩のプロピレンカーボネート溶液(2.0モル%)
TEMAPF6:トリエチルメチルアンモニウム六フッ化燐塩のプロピレンカーボネート溶液(2.0モル%)
表5の続き
炭素1:非多孔性炭素1
SBPPF6:スピロビピロリジニウム六フッ化燐塩のプロピレンカーボネート溶液(2.0モル%)
EMIPF6:エチルメチルイミダゾリウム六フッ化燐塩のプロピレンカーボネート溶液(2.0モル%)
TEMAPF6:トリエチルメチルアンモニウム六フッ化燐塩のプロピレンカーボネート溶液(2.0モル%)
2…トップカバー、
3…スプリング、
4、8…集電極、
5、7…炭素質電極、
6…セパレータ、
9…ガイド、
10、13…Oリング、
12…本体、
14…押え板、
15…参照電極、
16…ボトムカバー。
Claims (10)
- 炭素の結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20%以上である、電気二重層キャパシタの電極活物質用炭素質材料。
- 電極活物質として、炭素の結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20%以上である炭素質材料を含有する電気二重層キャパシタ用正電極。
- 電極活物質として、炭素の結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20%以上である炭素質材料を含有する正電極;及び電極活物質として活性炭を含有する負電極;を有する電気二重層キャパシタ。
- 電極活物質として、炭素の結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20%以上である炭素質材料を含有する正電極;及び電極活物質として、炭素の結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20%以上である炭素質材料を含有する負電極;を有する電気二重層キャパシタ。
- 非水溶媒中に溶質を溶解させた電解液中に、炭素の結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20%以上である炭素質材料を含有する炭素質正電極、及び炭素質負電極が浸されてなる電気二重層キャパシタ。
- 前記炭素の結晶構造中に存在する六方晶系構造に対する菱面体晶系構造の割合が20〜90%である請求項3〜5のいずれかに記載の電気二重層キャパシタ。
- 前記炭素質材料が黒鉛又は非多孔性炭素である請求項3〜5のいずれかに記載の電気二重層キャパシタ。
- 前記黒鉛が、ラマン分光法によるI(1360)/I(1580)の比が0.15から1.2の範囲のものである請求項7に記載の電気二重層キャパシタ。
- 前記溶質が、四級アンモニウム及びその誘導体の四フッ化ホウ酸塩、及び四級アンモニウム及びその誘導体の六フッ化リン酸塩からなる群から選択される少なくとも一種の電解質である請求項5に記載の電気二重層キャパシタ。
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