JP7206250B2 - アノード上にsei層を形成する方法 - Google Patents
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Description
本出願は、2017年7月10日に出願された米国仮出願第62/530,609号明細書の恩典を主張する。上記出願の全教示は、参照により本明細書に組み込まれる。
(a)アノードの1サイクル目の不可逆的損失以上の用量までアノードを予備アルカリ化するステップ。アノードは、黒鉛、コークス、その他の炭素、スズ、酸化スズ、ケイ素、酸化ケイ素、アルミニウム、リチウム活性金属、合金化金属材料、およびこれらの混合物であり得る。
(b)予備アルカリ化アノード、カソード、セパレータ、および電解質を密閉セルに組み立てるステップ。
(c)SEI層を形成するのに十分な条件および時間でセルを浸漬するステップ。
(d)任意選択的にセルを脱気するステップ。
a.アノードの不可逆的損失以上の用量までアノードを予備アルカリ化するステップと、
b.予備アルカリ化アノード、カソード、セパレータ、および電解質を密閉セルに組み立てるステップと、
c.外部電圧または電流を印加せずにセルを浸漬することによってSEI層を形成するステップと、
d.任意選択的にセルを脱気するステップと、
を含む方法である。
以下は、半セルでテストされた、予備アルカリ化アノードを有するセルの非電気化学的形成の詳細な例である。使用されたアノードは、およそ10.5%の不可逆的容量損失を有し、これをその総容量のおよそ15%まで予備アルカリ化した。ケイ素-黒鉛混合物からなるアルカリ化アノードを、およそ1.5×1.5cmの所望のサイズに打ち抜いた。次いで、パウチセルアセンブリ内でほぼ同じサイズのリチウム金属に対してアノード電極を組み立てた。使用したセパレータはCelgard2320であった。使用した電解質は、水分レベルが10ppm未満で2%のVCおよび10%のFECを有する3:7(EC:EMC)の1MのLiPF6であった。存在する気体を除去して電極およびセパレータの濡れを改善するために、密閉中にセルに真空を印加した。室温または40℃で、24、48、または72時間にわたり、外部から電圧または電流を印加せずに、各セルを浸漬した。26℃に制御されたカスタムメイドの環境チャンバ内で、全ての電池テストを実行した。パウチセルをテストするために、Maccorモデル4300電池テスタを使用した。各セルを、形成サイクルと類似の低サイクル速度で動作させた。比較のために、非アルカリ化アノードを有する類似のセルを構築した。形成されたSEIの量をセルの初期不可逆性から予測できることは、当業者によく知られている。予備アルカリ化アノードの不可逆的損失を非アルカリ化アノードの不可逆的損失から差し引くことによって、予備アルカリ化アノードを有するセル内の非電気化学的形成を介して形成されたSEIを推定できる。
以下は、フルセルの調製および処理の詳細な例である。ケイ素-黒鉛混合物からなる予備アルカリ化アノードを、およそ3×5cmの所望のサイズに打ち抜いた。使用されたアノードは、およそ10.5%の不可逆的容量損失を有し、これをその総容量のおよそ15%まで予備アルカリ化した。次いで、パウチセルアセンブリ内でほぼ同じサイズのNCMカソードに対してアノード電極を組み立てた。使用したセパレータはCelgard2320であった。使用した電解質は、水分レベルが10ppm未満で2%のVCおよび10%のFECを有する3:7(EC:EMC)の1MのLiPF6であった。存在する気体を除去して電極およびセパレータの濡れを支援するために、密閉中にセルに真空を印加した。セルを室温で24時間浸漬した。この後、パウチの過度に小さな切り込みを入れ、真空を印加して、真空下でセルに最終密閉を施した。26℃に制御されたカスタムメイドの環境チャンバ内で、全ての電池テストを実行した。パウチセルをテストするために、Maccorモデル4300電池テスタを使用した。開始時に従来の電気化学的形成サイクルを使用せず、通常のサイクル速度で1つのセルを動作させた。比較のために、開始時に2回の低速電気化学的形成サイクルを使用した後、通常のサイクル速度で別のセルを動作させた。
以下は、アノードの調製および処理の詳細な例である。厚さ25ミクロンの銅箔を、油分および破片を除去するためにイソプロピルアルコールおよびKimberly-ClarkのKimwipesで洗浄し、その後空気中で乾燥させた。Arkema Fluoropolymers Div.の1,000,000重量PVDF2.1グラムをAldrich Chemicalの乾燥NMP溶媒95mlに加えて、溶液を調製した。PVDF材料を完全に溶解するために、溶液を撹拌棒で一晩混合した。光感受性の溶媒が反応するのを防ぐために、溶液を暗所に保管した。次いで、33.9mlのこのPVDF溶液を、Conoco PhilipsのCPreme G5黒鉛15グラムおよびアセチレンブラック0.33グラムに加え、混合玉を使わずに600RPMのボールミル内で2時間撹拌した。加熱機能を有する真空押えプレートを使用して、得られたスラリーを銅箔上にキャストした。キャストして120℃で乾燥した後の完成した黒鉛の厚さは、約100ミクロンまたは14mg/cm2であった。次いで、アノードシートを15mm径のディスクに打ち抜き、その後、2032ボタン電池アセンブリで使用するために約3000psiおよび120℃で加圧した。その後、銅/黒鉛アノードディスクを、National Appliance Companyのモデル5851真空オーブン内で125℃および1mTorrで、少なくとも12時間真空焼成した。
Claims (9)
- 充電式金属イオン電池のアノード上にSEI層を形成する方法であって、
a.アノードの不可逆的損失以上の用量まで前記アノードを予備アルカリ化するステップと、
b.予備アルカリ化した前記アノードと、カソードと、セパレータと、電解質とを密閉セルに組み立てるステップと、
c.外部電圧または電流を印加せずに前記密閉セルを浸漬することによってSEI層を形成するステップと、
d.任意選択的に前記密閉セルを脱気するステップと、
を含む方法。 - 予備アルカリ化するステップはリチウム化を含む、請求項1に記載の方法。
- 前記アノードは、黒鉛またはその他の炭素、ケイ素、スズ、ケイ素合金、酸化ケイ素、金属酸化物、またはこれらの組み合わせを含む、請求項1に記載の方法。
- SEI層を形成するステップは、前記密閉セルを1時間から10日間浸漬することによって実行される、請求項1に記載の方法。
- SEI層を形成するステップは、前記密閉セルを1時間から2日間浸漬することによって実行される、請求項4に記載の方法。
- 前記SEI層は周囲温度で形成される、請求項5に記載の方法。
- 前記SEI層は約10℃から60℃の間の温度で形成される、請求項5に記載の方法。
- 前記SEI層は、前記密閉セルを1時間から2日間浸漬することによって形成される、請求項7に記載の方法。
- 充電式金属イオン電池の形成方法であって、
a.アノードの不可逆的損失以上の用量まで前記アノードを予備アルカリ化するステップと、
b.予備アルカリ化した前記アノードと、カソードと、セパレータと、電解質とを密閉セルに組み立てるステップと、
c.外部電圧または電流を印加せずに前記密閉セルを浸漬することによってSEI層を化学的に形成するステップと、
d.任意選択的に前記密閉セルを脱気するステップと、
e.外部電圧および/または電流の印加を通じて前記アノードを充電するステップと、
を含む方法。
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US20240194849A1 (en) | 2024-06-13 |
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US20220376219A1 (en) | 2022-11-24 |
US11380879B2 (en) | 2022-07-05 |
EP3652795A4 (en) | 2021-03-10 |
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