JP5478882B2 - 改善された取り扱い性を有する電気化学的セル用の又は電池用のセパレータ、並びに、当該セパレータの製造方法及び該セパレータの使用 - Google Patents
改善された取り扱い性を有する電気化学的セル用の又は電池用のセパレータ、並びに、当該セパレータの製造方法及び該セパレータの使用 Download PDFInfo
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- JP5478882B2 JP5478882B2 JP2008529571A JP2008529571A JP5478882B2 JP 5478882 B2 JP5478882 B2 JP 5478882B2 JP 2008529571 A JP2008529571 A JP 2008529571A JP 2008529571 A JP2008529571 A JP 2008529571A JP 5478882 B2 JP5478882 B2 JP 5478882B2
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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
- Y02E60/10—Energy storage using batteries
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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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T29/00—Metal working
- Y10T29/49—Method of mechanical manufacture
- Y10T29/49002—Electrical device making
- Y10T29/49108—Electric battery cell making
- Y10T29/4911—Electric battery cell making including sealing
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Description
比較例:公知技術によるセパレータ
水130g及びエタノール15gに先ず、5質量%のHNO3−水溶液30g、テトラエトキシシラン10g、メチルトリエトキシシラン2.5g及びDynasilan GLYMO(Degussa AG)7.5gを添加した。先ず数時間攪拌したこのゾルに、次いで各々酸化アルミニウムMartoxid MZS−1(Martinswerke)250gを懸濁させた。この泥状物を少なくとも更に24時間電磁攪拌機で均質化したが、その際攪拌容器は、溶剤損失が起こらないように、覆っておく必要があった。
水130g及びエタノール32gに先ず、濃HNO3−溶液5g、テトラエトキシシラン10g、メチルトリエトキシシラン1g及びDynasilan GLYMO(Degussa AG)7.5gを添加した。先ず数時間攪拌したこのゾルに、次いで各々酸化アルミニウムMartoxid MZS−1(Martinswerke)250g及びPVDF−コポリマー−粉末(Kynarflex 2801;Arkema GmbH;140℃ MP)を懸濁させた。この泥状物を少なくとも更に24時間電磁攪拌機で均質化したが、その際攪拌容器は、溶剤損失が起こらないように、覆っておく必要があった。
水130g及びエタノール32gに先ず、濃HNO3−溶液5g、テトラエトキシシラン10g、メチルトリエトキシシラン1g及びDynasilan GLYMO(Degussa AG)7.5gを添加した。先ず数時間攪拌したこのゾルに、次いで各々酸化アルミニウムAlcoa社のct 3000SG230g及びポリオレフィン−コポリマー−粉末(Vestowax A616;Degussa AG;120℃ MP;d50=5−6μm)を懸濁させた。この泥状物を少なくとも更に24時間電磁攪拌機で均質化したが、その際攪拌容器は、溶剤損失が起こらないように、覆っておく必要があった。
アセトン中の3質量%Kynarflex2801の溶液を連続浸漬法で例1により得たセパレータ上に速度1m/分で塗布し、温度60℃で熱空気流中で乾燥させた。
アセトン中の0.5質量%Kynarflex2801の溶液を連続浸漬法で、例1により得たセパレータ上に速度5m/分で塗布し、温度80℃で熱空気流中で乾燥させた。
シクロヘキサン中の3質量%Vestowax A616の溶液(その際完全には溶解してなく部分架橋した非溶解性粒子を濾過器で分離した)を連続浸漬法で、例2により得たセパレータ上に速度10m/分で塗布し、温度100℃で熱空気流中で乾燥させた。
例1から5並びに比較例で製造したセパレータを下記に記載したように特性付けした。結果は第3表にまとめた。
このために30℃で先ずコンダクトメータ(Metrohm)を用いて純粋な電解質(炭酸プロピレン中のLiClO4の0.01モル溶液)の伝導率LF1を測定した。次いでセパレータを電解質で浸漬し、同じく伝導率LF2を測定した。MacMullin数はこの二つの伝導率の比LF1/LF2である。
バブルポイント(BP)は、完全に湿潤した膜(セパレータ)を通って気泡が生じる際の圧力(バール)である。これは膜中の最大孔又は瑕疵箇所の大きさの目安である。BPが小さければそれだけ最大孔又は最大瑕疵(穴)は大きい。
Gurley数をBPと同じ装置で測定した。しかしGurley数を測定する際に6.45cm2の平面(気体の31cmの水柱の圧力)を通って流れるために100mlの気体容量が必要とする時間tを測定した。
耐屈曲性の測定は、試験すべきセパレータを折り曲げ、生じる屈折上に質量1kgを有しかつ直径10cmの円形底面を有する重りを1分間載せることによって行う。その際、重りは重りの直径が丁度屈折上に位置するように載せる。重りを取り除いた後、セパレータを広げ、皺をのばし、スイッチをいれた蛍光板上に載せた。そこで光学顕微鏡を用いて折れ目の重りで重しをかけた場所を精査した。蛍光板の光がセパレータを通って妨げられずに進むことができた、従って屈曲によって穴が生じた屈折場所に印を付けた(盲検試料用に各セパレータを先ず折り曲げる場所で蛍光板を用いて屈曲前に穴/瑕疵場所が存在するか試験することができる)。こうして印を付けた屈曲の長さを合計した。印を付けた長さが1cmより少ない場合は、耐屈曲性は良好と評価した。印を付けた長さが1〜5cmである場合は対屈曲性は平均的と評価した。印を付けた長さが5cmより多い(50%)場合には耐屈曲性は不良と評価した。
Claims (22)
- 非電導性材料から成る繊維を有する支持体上及び当該支持体の間隙中に、無機接着剤によって相互に接着しかつ前記支持体と接着した、Al2O3、ZrO2及びSiO2から選択した少なくとも1種の酸化物を有する酸化物粒子から成る多孔性の非電導性塗膜を有する、電気化学的セル用又は電池用のセパレータであって、セラミック塗膜中にAl2O3、ZrO2及び/又はSiO2の酸化物粒子の他にポリマー粒子も存在していることを特徴とするセパレータ。
- 前記ポリマー粒子が、100℃より大きい溶融温度を有することを特徴とする、請求項1に記載のセパレータ。
- 該セパレータ中で前記酸化物粒子対前記ポリマー粒子の容量割合が2対1から100対1であることを特徴とする、請求項1又は2に記載のセパレータ。
- 前記ポリマー粒子が、前記酸化物粒子の平均粒度の0.1〜30倍に相応する平均粒度を有することを特徴とする、請求項1から3までのいずれか1項に記載のセパレータ。
- 該セパレータが、当該セパレータの厚さの0.5倍より小さい平均粒度を有するポリマー粒子だけを有することを特徴とする、請求項4に記載のセパレータ。
- 前記支持体が、ポリアクリロニトリル、ポリアミド、ポリエステル及び/又はポリオレフィンの繊維から選択されるポリマー繊維を有する、ポリマーフリースであることを特徴とする、請求項1から5までのいずれか1項に記載のセパレータ。
- 前記無機接着剤が、元素Al、Si及び/又はZrの酸化物から選択したものであることを特徴とする、請求項1から6までのいずれか1項に記載のセパレータ。
- 前記セラミック塗膜が、その表面上に可溶性ポリマーを有することを特徴とする、請求項1から7までのいずれか1項に記載のセパレータ。
- 前記の可溶性ポリマーで構成される膜が厚さ10nm〜5μmを有することを特徴とする、請求項8項に記載のセパレータ。
- 請求項1から9までのいずれか1項に記載の電気化学的セル用又は電池用のセパレータを製造するための方法であって、
非電導性材料から成る繊維を有しかつ当該繊維の間に間隙がある支持体にセラミック塗膜を設け、このために前記支持体上及びその中に懸濁液を施与し、これを少なくとも1回加熱することによって前記支持体上及びその中で固化させ、その際、前記懸濁液は、ゾルと、当該ゾル中に懸濁させた粒子の少なくとも二つのフラクションとを有し、それらフラクションのうちの第1フラクションは、元素Al、Zr及び/又はSiの酸化物から選択した酸化物粒子を有し、かつ、それらフラクションのうちの第2フラクションはポリマー粒子を有することを特徴とする、方法。 - 前記の第1フラクションで使用される酸化物粒子対前記の第2フラクションで使用されるポリマー粒子の容量割合が2対1から100対1であることを特徴とする、請求項10に記載の方法。
- 前記第1フラクションにおいては、平均粒度が0.1〜10μmの酸化物粒子が少なくとも1種使用されることを特徴とする、請求項10又は11に記載の方法。
- 前記第2フラクションにおいては、前記の懸濁される酸化物粒子の平均粒度の0.1〜30倍に相応する平均粒度を有するポリマー粒子が使用されることを特徴とする、請求項10から12までのいずれか1項に記載の方法。
- 前記支持体上に塗布する前に、前記の使用される懸濁液に付加的に定着剤を添加し、ここで、当該定着剤は、有機官能性シラン類のうちの1種であることを特徴とする、請求項10から13までのいずれか1項に記載の方法。
- 前記支持体として、ポリアクリロニトリル、ポリエステル、ポリアミド及び/又はポリオレフィンから選択した繊維を有するポリマーフリースを使用することを特徴とする、請求項10から14までのいずれか1項に記載の方法。
- 前記の使用されるゾルを、元素Al、Zr又はSiの前駆物質化合物を、水を用いてか又は水で希釈した酸を用いて加水分解することによって得ることを特徴とする、請求項10から15までのいずれか1項に記載の方法。
- 前記の支持体上及びその中に存在する懸濁液を、50〜350℃に加熱することによって固化させることを特徴とする、請求項10から16までのいずれか1項に記載の方法。
- 前記の懸濁液の固化後に生成するセラミック塗膜を先ず可溶性ポリマーの溶液で処理し、次いで溶剤を除去することを特徴とする、請求項10から17までのいずれか1項に記載の方法。
- 請求項10から18までのいずれか1項に記載の方法により得られることを特徴とする、請求項1から9までのいずれか1項に記載のセパレータ。
- 請求項1から9までのいずれか1項に記載のセパレータ又は請求項19に記載のセパレータの、電気化学的セル又は電池中のセパレータとしての使用。
- 請求項1から9までのいずれか1項に記載のセパレータ又は請求項19に記載のセパレータを有するリチウム電池。
- 請求項21に記載のリチウム電池を有する乗物。
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DE102005042215A DE102005042215A1 (de) | 2005-09-05 | 2005-09-05 | Separator mit verbesserter Handhabbarkeit |
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PCT/EP2006/062915 WO2007028662A1 (de) | 2005-09-05 | 2006-06-06 | Separator mit verbesserter handhabbarkeit |
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-
2005
- 2005-09-05 DE DE102005042215A patent/DE102005042215A1/de not_active Withdrawn
- 2005-10-26 CN CN2005101216856A patent/CN1929164B/zh not_active Expired - Fee Related
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- 2006-06-06 EP EP06763519.3A patent/EP1925047B1/de not_active Not-in-force
- 2006-06-06 US US12/063,626 patent/US10566593B2/en not_active Expired - Fee Related
- 2006-08-30 TW TW095132064A patent/TW200727526A/zh unknown
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US10566593B2 (en) | 2020-02-18 |
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WO2007028662A1 (de) | 2007-03-15 |
KR101276906B1 (ko) | 2013-06-20 |
EP1925047A1 (de) | 2008-05-28 |
US20100279173A1 (en) | 2010-11-04 |
US20140212727A1 (en) | 2014-07-31 |
CN1929164A (zh) | 2007-03-14 |
DE102005042215A1 (de) | 2007-03-08 |
EP1925047B1 (de) | 2015-07-29 |
KR20080049029A (ko) | 2008-06-03 |
CN1929164B (zh) | 2010-12-22 |
JP2009507353A (ja) | 2009-02-19 |
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