JP6367207B2 - 低抵抗電気化学素子用電極、その製造方法及び電極を含む電気化学素子 - Google Patents
低抵抗電気化学素子用電極、その製造方法及び電極を含む電気化学素子 Download PDFInfo
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- JP6367207B2 JP6367207B2 JP2015537651A JP2015537651A JP6367207B2 JP 6367207 B2 JP6367207 B2 JP 6367207B2 JP 2015537651 A JP2015537651 A JP 2015537651A JP 2015537651 A JP2015537651 A JP 2015537651A JP 6367207 B2 JP6367207 B2 JP 6367207B2
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Images
Classifications
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/04—Processes of manufacture in general
- H01M4/0402—Methods of deposition of the material
- H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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- 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
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- H—ELECTRICITY
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Description
前記バインダー高分子は、69,000〜100,000範囲の分子量を有し得る。
前記導電材は、5nm〜100nmの一次凝集体の粒径を有し得る。
前記導電材は、30nm〜1μmの二次凝集体の粒径を有し得る。
前記活物質成分は、シリコン系化合物、スズ系化合物またはこれらの混合物であり得る。
前記バインダー高分子は、活物質の固形分含量100重量部を基準に5〜10重量部の量で使用され得る。
前記導電材は、活物質の固形分含量100重量部を基準に3〜15重量部の量で使用され得る。
本発明の他の態様によれば、上述した電極を含む電気化学素子が提供される。
前記電気化学素子は、リチウム二次電池であり得る。
前記電気化学素子は、フルセル(full cell)基準で4.2V以上の電圧領域が駆動電圧であり得る。
前記一次高剪断混合及び二次高剪断混合は、それぞれ独立して、20,000〜40,000psi範囲で行われ得る。
前記一次高剪断混合工程後、バインダー高分子は27,000〜380,000範囲の分子量を有し得る。
前記二次高剪断混合工程後のスラリーは、20mV〜100mV範囲のゼータ電位の絶対値を有し得る。
電極合剤スラリーに使用できるバインダー高分子は、活物質粒子同士を互いによく付着させ、また、活物質を集電体によく付着させなければならない。バインダー高分子の非制限的な例としては、ポリビニルアルコール(polyvinylalcohol)、カルボキシメチルセルロース(carboxymethylcellulose)、ハイドロキシプロピルセルロース(hydroxypropylcellulose)、ジアセチルセルロース(diacetylcellulose)、ポリ塩化ビニル(polyvinylchloride)、カルボキシル化されたポリ塩化ビニル(carboxylated polyvinylchloride )、ポリフッ化ビニル(polyvinylfluoride)、エチレンオキサイドを含むポリマー(polymer with ethylene oxide)、ポリビニルピロリドン(polyvinylpyrrolidone)、ポリウレタン、ポリテトラフルオロエチレン、ポリフッ化ビニリデン、ポリエチレン、ポリプロピレン、スチレン‐ブタジエンゴム、アクリル酸スチレン‐ブタジエンゴム、エポキシ樹脂、ナイロンなどが挙げられる。
前記バインダー高分子は、電極合剤スラリーに使用される活物質の固形分含量100重量部を基準に、5〜10重量部の量で使用され得る。
導電材は、電極合剤スラリーに含有される電極活物質の固形分含量100重量部を基準に、3〜15重量部の量で使用され得る。
本明細書で「高容量電池」とは、フルセル基準で4.2V以上の電圧領域を駆動電圧として作動する電池を意味する。
また、前記二次高剪断混合によって導電材の均一な分散が可能になる。
また、目標製品の求められる特性及び原資材の特性に応じて、活物質の混合においても高剪断ミキサーの適用が可能である。
電極合剤スラリーを製造した後、これを金属ホイルなどの集電体上に塗布し、乾燥及び圧延して所定のシート型電極を製造することができる。
実施例1のスラリーに導電材であるカーボンブラックを添加した後、高剪断ミキサーによって混合してパスによる粘性挙動を図4に示した。図4から、初期導電材ネットワークに湿潤が不十分である場合には粘稠化挙動を示すが、高剪断混合のパス数の増加によって、実施例1のCMCスラリーの挙動と類似の粘稠化挙動に変換されることが確認された。高剪断ミキサーとしてはMFDミキサーを使用し、100μm水準の毛細管径を通過することを基準に、スラリーに加える剪断圧力は20,000〜40,000psi水準とした。
実施例1のスラリーに導電材であるカーボンブラックを添加した後、高剪断ミキサーによって混合してパスによる粘性挙動を図4に示した。図4から、初期導電材ネットワークに湿潤が不十分である場合には粘稠化挙動を示すが、高剪断混合のパス数の増加によって、実施例1のCMCスラリーの挙動と類似の粘稠化挙動に変換されることが確認された。高剪断ミキサーとしてはMFDミキサーを使用し、100μm水準の毛細管径を通過することを基準に、スラリーに加える剪断圧力は20,000〜40,000rpm水準とした。
一般に市販される黒鉛及び高容量材料であるSi系材料を重量比9:1で使用して負極活物質とし、アセチレンブラック、CMC、及びSBRをそれぞれ8:1:1の重量比で混合し、溶媒であるN‐メチルピロリドンに入れ、MFDミキサーを用いるが、100μm水準の毛細管径を通過することを基準に、スラリーに加える剪断圧力を18,000psi以下の水準にして高剪断混合を行った。負極合剤スラリーを厚さ10μmの銅箔にドクターブレード法で塗布して半乾燥させた後、所定の大きさに裁断した。このとき、セルの組み立ての前に真空状態で120℃で約一日間乾燥させた。
一般に市販される黒鉛及び高容量材料であるSi系材料を重量比9:1で使用して負極活物質とし、アセチレンブラック、CMC、及びSBRをそれぞれ8:1:1の重量比で混合し、溶媒であるN‐メチルピロリドンに入れ、MFDミキサーを用いるが、100μm水準の毛細管径を通過することを基準に、スラリーに加える剪断圧力を18,000rpm以下の水準にして高剪断混合を行った。負極合剤スラリーを厚さ10μmの銅箔にドクターブレード法で塗布して半乾燥させた後、所定の大きさに裁断した。このとき、セルの組み立ての前に真空状態で120℃で約一日間乾燥させた。
エチレンカーボネート(EC):ジメチルカーボネート(DMC):エチルメチルカーボネート(EMC)を3:4:3の重量比で混合して溶媒として使用し、6フッ化リン酸リチウム(LiPF6)を1.2mol/Lの濃度で溶解させて電解液を製造した。
製造された正極と負極との間に分離膜を挿入して積層型セルを製造し、ラミネートフィルムからなる収納ケースに電解液とともに含浸させた形態で密封して約24時間放置した。
高剪断混合の代りに、一般の混合条件、すなわちプラネタリー分散ミキサーを適用した混合方式で最大RPMを約2000〜3000程度の水準にした。この方式の場合、導電材の分散が不十分であり得、このため、μm大きさの活物質が後続工程で亀裂する恐れが内在する。高剪断混合の代りに上述した一般の混合条件を利用したことを除き、実施例1と同じ方式でバインダースラリーを製造してその粘性挙動を図3に示した。
高剪断混合の代りに上述した一般の混合条件で混合したことを除き、実施例2と同じ方式でスラリーを製造し、その粘性挙動を図4に示した。
前記実施例3で一般の混合条件が適用されたことを除き、前記実施例3と同じ方法で正極合剤スラリーと負極合剤スラリーを製造して電気化学素子を製造した。
実施例3で組み立てられたセルを定電流で4.6V〜2.0Vの条件でフォーメーション(Formation)した。製造された単層パウチ型セル(single layer pouch cell)を4.5〜2.0V範囲で充放電して充放電容量を測定し、その結果を図5に示した。
Claims (4)
- 電極の製造方法であって、
バインダー高分子と、溶媒とを混合し、バインダー高分子が分散されたスラリーを用意する段階と、
前記スラリーを一次高剪断混合する段階と、
前記スラリーに導電材を添加して二次高剪断混合を行う段階と、
得られたスラリーに電極活物質を添加し、分散させて電極合剤スラリーを得る段階と、及び
前記電極合剤スラリーを集電体に塗布して乾燥させる段階とを含んでなり、
前記バインダー高分子が、活物質の固形分含量100重量部を基準として、5〜10重量部の量で使用されてなり、
前記導電材が、活物質の固形分含量100重量部を基準として、3〜15重量部の量で使用されてなり、
前記バインダー高分子が、ポリテトラフルオロエチレン、ポリフッ化ビニリデン及びアクリル酸スチレン‐ブタジエンゴムからなる群より選択された一種又は二種以上の混合物、若しくは、カルボキシメチルセルロース、スチレン‐ブタジエンゴム、ポリテトラフルオロエチレン、及び液状シリコーンゴムからなる群より選択された一種又は二種以上の混合物であり、
前記溶媒が、N‐メチルピロリドン、メタノール、エタノール、n‐プロパノール、イソプロパノール、又はこれらの混合物或いは水であり、
前記一次高剪断混合及び前記二次高剪断混合が、それぞれ独立して、マイクロフルダイザー(microfludizer)により、100μm水準の毛細管径を通過することを基準に、前記スラリーを少なくとも20,000psiで剪断混合し、前記スラリーに剪断圧力を加えることを特徴とする、電極の製造方法。 - 前記導電材が、5nm〜100nmの一次凝集体の粒径を有するものであり、及び/又は、
前記導電材が、30nm〜1μmの二次凝集体の粒径を有することを特徴とする、請求項1に記載の電極。 - 前記一次高剪断混合及び前記二次高剪断混合が、それぞれ独立して、20,000〜40,000psiで行われることを特徴とする、請求項1又は2に記載の電極の製造方法。
- 前記二次高剪断混合工程後に、前記スラリーのゼータ電位の絶対値が、20mV〜100mVであることを特徴とする、請求項1〜3の何れか一項に記載の電極の製造方法。
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US10270102B2 (en) | 2019-04-23 |
JP2015532519A (ja) | 2015-11-09 |
EP2908370B1 (en) | 2018-11-28 |
EP2908370A4 (en) | 2016-10-05 |
CN104854743A (zh) | 2015-08-19 |
KR20140114799A (ko) | 2014-09-29 |
EP2908370A1 (en) | 2015-08-19 |
US20150270552A1 (en) | 2015-09-24 |
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