JP4436121B2 - 蓄電素子および蓄電素子の製造方法 - Google Patents
蓄電素子および蓄電素子の製造方法 Download PDFInfo
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- JP4436121B2 JP4436121B2 JP2003411288A JP2003411288A JP4436121B2 JP 4436121 B2 JP4436121 B2 JP 4436121B2 JP 2003411288 A JP2003411288 A JP 2003411288A JP 2003411288 A JP2003411288 A JP 2003411288A JP 4436121 B2 JP4436121 B2 JP 4436121B2
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- polymer electrolyte
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Classifications
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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
- H01G11/50—Electrodes characterised by their material specially adapted for lithium-ion capacitors, e.g. for lithium-doping or for intercalation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0565—Polymeric materials, e.g. gel-type or solid-type
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Description
本発明は、高分子電解質と分極性電極とを備えた蓄電素子であって、前記分極性電極が前記高分子電解質との界面を備え、前記分極性電極が金属電極であり、前記分極性電極の負極電極が、前記高分子電解質との界面において、該負極電極に含まれる金属成分とのリチウム合金を有し、前記リチウム合金が可逆的な電気化学的酸化還元反応によりリチウムイオンを放出することができる合金であることを特徴とする蓄電素子である。
また、本発明は、蓄電素子の製造方法であって、無電解メッキ法により高分子電解質上に分極性電極が形成された電極−電解質構造体を得る構造体形成工程と構造体形成工程により得られた該電極−電解質構造体がリチウムイオンを含む溶液を含有する状態で該分極性電極に電圧を印加して、該分極性電極の金属成分とリチウムとを含む層を該分極性電極の負極に形成する層形成工程、とを含む蓄電素子の製造方法でもある。本発明の蓄電素子の製造方法を用いることにより、金属電極である負極と前記高分子電解質との界面において、該負極に含まれる金属成分とのリチウムとが含まれた層を有する蓄電素子を形成することができる。前記層が可逆的な電気化学的酸化還元反応によりリチウムイオンを放出することができる合金を含むことができるので、前記蓄電素子は、電気二重層容量とリチウム合金の酸化還元反応による擬似容量との両方を有するために、通常のキャパシタに比べて大きな比容量を有することができる。
本発明の蓄電素子は、高分子電解質と該高分子電解質を挟んで形成された2つの分極性電極からなる蓄電素子を積層、折畳、又は捲回させて、更にコイン型やラミネート型に形成し、これを缶又はラミネートパック等の容器に収容し、缶であれば封缶、ラミネートパックであればヒートシールする方法により、蓄電部品として組み立てることができる。また、前記方法において、容器を封缶若しくはヒートシールする前に、容器を特定の電解質溶液で充填して、蓄電部品を得ることもできる。本発明の蓄電素子を有底筒状の外装ケースに収納し、外装ケースの開口端部を弾性部材からなる封口体で封口することで、チップ部品である蓄電部品を得ることができる。本発明の蓄電素子を収納したケースには、線膨張率の小さい絶縁物質を充填しても良い。
本発明の蓄電素子は、公知のサイズとすることができ、例えば、7.3mm×4.3mm×2.0mmとすることができる。例えば、前記蓄電素子は、縦寸法を通常10mm以上、好ましくは20mm以上であり、25〜50mmとすることができ、同様に、横寸法を、通常10mm以上、好ましくは20mm以上であり、25〜50mmとすることができる。また、本発明の蓄電素子は、例えば、ケースサイズ10mmφ×16mmL、φ8×5L、4φ×7L、5φ×2.8L、または5φ×3L等の円筒形の蓄電部品とすることもできる。
乾燥時の膜厚が160μmの膜状高分子電解質(フッ素樹脂系イオン交換樹脂:パーフルオロカルボン酸樹脂、商品名「フレミオン」、旭硝子社製、イオン交換容量1.8meq/g)を膨潤溶媒であるメタノール中に20℃で30分以上浸漬した。膨潤した前記膜状高分子電解質の膜厚を測定して、乾燥膜厚に対して膨潤後の膜厚の増加した割合〔膨潤度(%)〕を算出し、膨潤度が50%となるように前記膜状高分子電解質を膨潤溶媒に浸漬した。次いで、膨潤した高分子電解質に対して、それぞれ下記(1)〜(3)の工程を6サイクル繰り返して実施し、1対の金属電極である分極性電極が形成された高分子電解質を得た。(1)吸着工程:ジクロロフェナントロリン金塩化物水溶液に12時間浸漬し、成形品内にジクロロフェナントロリン金錯体を吸着させ、(2)還元工程:亜硫酸ナトリウムを含む水溶液中で、吸着したジクロロフェナントロリン金錯体を還元して、膜状高分子電解質表面に金電極を形成させた。このとき、水溶液の温度を60〜80℃とし、亜硫酸ナトリウムを徐々に添加しながら、6時間ジクロロフェナントロリン金錯体の還元を行った。次いで、(3)洗浄工程:表面に金電極が形成した膜状高分子電解質を取り出し、70℃の水で1時間洗浄した。
上記製造例により得られた電極−電解質構造体を、ビス(トリフルオロメチル)スルホニルイミドリチウム(Li(CF3SO2)2N)の0.5mol/L水溶液に12時間浸漬した後に、該電極−電解質構造体を120分間真空乾燥した。乾燥された該電極−電解質構造体にビス(トリフルオロメチル)スルホニルイミドリチウム(Li(CF3SO2)2N)の1.0mol/Lのプロピレンカーボネイト溶液に12時間浸漬した。プロピレンカーボネイト溶液を含む該電極−電解質構造体の一対の分極性電極に、負極電圧が−5.0Vとなるように、分極性電極のそれぞれに対して電圧を12時間印加して、実施例1の蓄電素子を得た。得られた蓄電素子は、負極が黒色状に変色し、電極−高分子電解質界面においてリチウムと金との合金を備えた。また、実施例1の蓄電素子に含まれるイオン種は(CF3SO2)2N−とLi+であった。
上記製造例により得られた電極−電解質構造体を、イオン交換水に12時間浸漬した後に、該電極−電解質構造体120分間真空乾燥した。HNO3の1.0mol/L水溶液に浸漬した。HNO3水溶液を含む該電極−電解質構造体の一対の分極性電極に、負極電圧が−5.0Vとなるように、分極性電極のそれぞれに対して電圧を12時間印加して、比較例1の蓄電素子を得た。比較例1の蓄電素子に含まれるイオン種は、H+、NO3 −であった。比較例1の蓄電素子は、電気二重層キャパシタである。
上記製造例により得られた電極−電解質構造体を、(C2H5)4NBF4の0.5mol/L水溶液に12時間浸漬した後に、該電極−電解質構造体120分間真空乾燥した。ついで、(C2H5)4NBF4の1.0mol/Lプロピレンカーボネート溶液に浸漬した。(C2H5)4NBF4プロピレンカーボネイト溶液を含む該電極−電解質構造体の一対の分極性電極に、負極電圧が−5.0Vとなるように、分極性電極のそれぞれに対して電圧を12時間印加して、比較例2の蓄電素子を得た。比較例2の蓄電素子に含まれるイオン種は、(C2H5)4N−とBF4 +であった。比較例2の蓄電素子は電気二重層キャパシタである。
(比容量)
実施例1並びに比較例1及び2について、2電極の定電流放電法により得た実測値を表1に示す。定電流放電法によるの比容量の実測値は、商品名「HJ−201B」(北斗電工社製)を用いて、上記規格番号EIAJ RC−2377に準拠して測定した値である。なお、この方法で静電容量を測定する場合には、測定対象物である高分子電解質を切断して、膨潤状態で10mm×10mmの大きさの蓄電素子とした。なお、得られた実施例1並びに比較例1及び2の蓄電素子の乾燥した状態における膜厚は、160μmであった。なお、表中においてPCはプロピレンカーボネイトの略である。
本発明の蓄電素子である実施例1の蓄電素子は、定電流放電法で測定された比容量が20F/cm3という大きな比容量を示した。これは、充電時においては、負極では電気化学的酸化還元反応により分極性電極の金属成分である金とリチウムとの合金がチウムイオンが含まれる層として負極界面に形成され、正極においては(CF3SO2)2N−により電気二重層が形成される。そのために、レドックス反応による擬似容量と電気二重層による電気二重層容量を足し合わせた値を比容量として有すると考えられる。実施例1の蓄電素子は、電気二重層キャパシタとハイブリッドキャパシタとの特徴を兼ね備えたハイブリッドキャパシタとして機能しているものと考えられる。
Circuit)カード等の薄型の半導体装置、強誘電体を用いたFeRAM、有機EL素子の発光素子アレイ、ICカードなどのICチップ、強誘電体蓄電素子を有する半導体装置、並びに電力変換を行うスイッチング素子に好適に用いることができる。
Claims (7)
- 蓄電素子の製造方法であって、
無電解メッキ法により高分子電解質上に分極性電極が形成された電極−電解質構造体を得る構造体形成工程と
構造体形成工程により得られた該電極−電解質構造体がリチウムイオンを含む溶液を含有する状態で、該分極性電極に電圧を印加して、該分極性電極の金属成分とリチウムとを含む層を該分極性電極の負極に形成する層形成工程、
とを含む蓄電素子の製造方法。 - リチウムイオンを含む溶液を前記電極−電解質構造体の高分子電界質に含有させることを、前記層形成工程の前工程として、若しくは前記層形成工程と同時に行うことを特徴とする請求項1に記載の蓄電素子の製造方法。
- 前記高分子電解質がイオン交換樹脂膜であり、前記無電解メッキ法が、イオン交換樹脂に金属錯体を吸着させる吸着工程と、吸着工程により金属錯体が吸着したイオン交換樹脂に還元剤溶液を接触させて金属を析出させる還元工程とを含む方法である請求項1または2に記載の蓄電素子の製造方法。
- 前記金属錯体が金、鉛、錫及び亜鉛からなる群より選ばれた1種以上の金属を含む請求項1乃至3のいずれかに記載の蓄電素子の製造方法。
- 高分子電解質と分極性電極とを備えた蓄電素子であって、
高分子電解質に無電解メッキ法を施して分極性電極が形成された電極−電解質構造体を得た後に、該電極−電解質構造体がリチウムイオンを含む溶液を含有する状態で該分極性電極に電圧を印加することにより、該分極性電極の負極に該分極性電極の金属成分とリチウムとが結合した層を形成することにより得られた蓄電素子。 - 前記高分子電解質がイオン交換樹脂膜であり、前記無電解メッキ法が、イオン交換樹脂に金属錯体を吸着させる吸着工程と、吸着工程により金属錯体が吸着したイオン交換樹脂に還元剤溶液を接触させて金属を析出させる還元工程とを含む方法である請求項5に記載の蓄電素子。
- 前記金属成分が金、鉛、錫及び亜鉛からなる群より選ばれた1種以上の金属を含む請求項5または6に記載の蓄電素子。
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EP2393090A1 (en) * | 2010-06-01 | 2011-12-07 | Nxp B.V. | Highly-integrated thin film capacitor with amorphous cathode |
US8920731B2 (en) * | 2010-09-20 | 2014-12-30 | Kimberly-Clark Worldwide, Inc. | Nonwoven-based chemi-capacitive or chemi-resistive gas sensor |
JP5670168B2 (ja) * | 2010-12-13 | 2015-02-18 | Udトラックス株式会社 | 蓄電セル及び蓄電装置 |
US9786947B2 (en) * | 2011-02-07 | 2017-10-10 | Sila Nanotechnologies Inc. | Stabilization of Li-ion battery anodes |
CN102249380B (zh) * | 2011-05-20 | 2012-11-28 | 华东师范大学 | 一种高效液流式膜电容脱盐装置 |
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JPS60161611A (ja) * | 1984-02-01 | 1985-08-23 | エルナ−株式会社 | 電気二重層キヤパシタ |
JPS60220574A (ja) * | 1984-04-17 | 1985-11-05 | Matsushita Electric Ind Co Ltd | 充電可能な電気化学装置 |
US5366829A (en) * | 1993-06-14 | 1994-11-22 | Valence Technology, Inc. | Method of forming an anode material for lithium-containing solid electrochemical cells |
US5953204A (en) * | 1994-12-27 | 1999-09-14 | Asahi Glass Company Ltd. | Electric double layer capacitor |
JPH118153A (ja) | 1997-06-13 | 1999-01-12 | Matsushita Electric Ind Co Ltd | 高分子薄膜の製造方法とコンデンサの製造方法 |
JP3812098B2 (ja) * | 1997-11-04 | 2006-08-23 | 三菱化学株式会社 | 電気二重層キャパシター |
JP3800799B2 (ja) * | 1998-04-10 | 2006-07-26 | 三菱化学株式会社 | 電気二重層キャパシター |
US6797428B1 (en) * | 1999-11-23 | 2004-09-28 | Moltech Corporation | Lithium anodes for electrochemical cells |
US6426863B1 (en) * | 1999-11-25 | 2002-07-30 | Lithium Power Technologies, Inc. | Electrochemical capacitor |
GB0016057D0 (en) * | 2000-06-30 | 2000-08-23 | Aea Technology Plc | A method of assembling a cell |
JP3726649B2 (ja) * | 2000-07-21 | 2005-12-14 | Jsr株式会社 | 重合体組成物および複合膜 |
KR100388906B1 (ko) * | 2000-09-29 | 2003-06-25 | 삼성에스디아이 주식회사 | 리튬 2차 전지 |
-
2003
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2004
- 2004-12-09 US US10/582,548 patent/US20070117017A1/en not_active Abandoned
- 2004-12-09 CN CN2004800367509A patent/CN1890769B/zh not_active Expired - Fee Related
- 2004-12-09 WO PCT/JP2004/018384 patent/WO2005057597A1/ja active Application Filing
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EP1693866A4 (en) | 2009-08-05 |
WO2005057597A1 (ja) | 2005-06-23 |
EP1693866A1 (en) | 2006-08-23 |
CN1890769B (zh) | 2010-10-06 |
CN1890769A (zh) | 2007-01-03 |
JP2005175107A (ja) | 2005-06-30 |
US20070117017A1 (en) | 2007-05-24 |
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