JP2022549706A - 負極の前リチウム化装置及び負極の前リチウム化方法 - Google Patents
負極の前リチウム化装置及び負極の前リチウム化方法 Download PDFInfo
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- JP2022549706A JP2022549706A JP2022519321A JP2022519321A JP2022549706A JP 2022549706 A JP2022549706 A JP 2022549706A JP 2022519321 A JP2022519321 A JP 2022519321A JP 2022519321 A JP2022519321 A JP 2022519321A JP 2022549706 A JP2022549706 A JP 2022549706A
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- Prior art keywords
- negative electrode
- lithiation
- electrode structure
- prelithiation
- lithium metal
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Images
Classifications
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- H01M4/0438—Processes of manufacture in general by electrochemical processing
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Abstract
Description
本発明は、上述した負極の前リチウム化装置を用いた負極の前リチウム化方法を提供する。
また、本発明は、上述した負極の前リチウム化方法を含む二次電池の製造方法を提供する。
<負極構造体の製造>
負極活物質(黒鉛90%、SiO10%)92重量%、導電材(Denka Black)3重量%、バインダー(SBR)3.5重量%及び増粘剤(CMC)1.5重量%を水に添加して負極スラリーを製造した。
横×縦×高さが270cm×20cm×60cmのステンレススチール素材の前リチウム化反応槽を準備した。上記前リチウム化反応槽には、前リチウム化溶液を反応槽の高さの30%となるように投入した。上記前リチウム化反応槽の温度は25℃に維持した。
上記負極ロールから上記負極構造体を巻出して、1cm/minの速度で前リチウム化反応槽に投入、進行させた。上記巻取された負極構造体は含浸区間に進入して、50分間を走行されて電解液に含浸された。
横×縦×高さが50cm×20cm×60cmのステンレススチール素材の洗浄槽を準備した。前リチウム化反応槽および洗浄槽の間には、負極構造体を移送するためのロールが設置された。洗浄槽には、有機溶媒としてジメチルカーボネートが洗浄槽の高さの30%で含まれた。
前リチウム化区間でリチウム金属対極を負極構造体の走行方向に行くほど負極構造体との離隔距離が連続的に増加するように傾け、かつ前リチウム化区間のスタート地点でのリチウム金属対極と負極構造体との間の離隔距離を6mmとし、前リチウム化区間の終了地点でのリチウム金属対極と負極構造体との離隔距離を12mmとしたことを除いては、実施例1同じく負極構造体を製造した。
前リチウム化区間で、リチウム金属対極を負極構造体の走行方向に行くほど負極構造体との離隔距離が連続的に増加するように傾け、かつ前リチウム化区間のスタート地点でのリチウム金属対極と負極構造体との間の離隔距離を6mmとし、前リチウム化区間の終了地点でのリチウム金属対極と負極構造体との間の離隔距離を18mmとしたことを除いては、実施例1と同じく負極構造体を製造した。
前リチウム化区間で、図6のようにリチウム金属対極を負極構造体に平行に配置した。このとき、リチウム金属対極と負極構造体との間の距離を6mmと一定に維持した。上記事項を除いては、実施例1と同じく負極構造体を製造した。
前リチウム化区間で、図7のようにリチウム金属対極を負極構造体の走行方向に行くほど負極構造体との離隔距離が連続的に減少するように傾けた。具体的に、前リチウム化区間のスタート地点でのリチウム金属対極と負極構造体との間の離隔距離を6mmとし、前リチウム化区間の終了地点でのリチウム金属対極と負極構造体との間の離隔距離を3mmとしたことを除いては、実施例1と同じく負極構造体を製造した。
<リチウム二次電池の製造>
上記実施例および比較例で製造された負極構造体を図8のように幅方向に3等分して区間(区間a~c)を設定し、各区間でコインセルのサイズでそれぞれ負極を打ち抜きした。すなわち、区間bは、負極構造体の幅方向の中央部の部分であり、区間a及び区間cは、負極構造体での幅方向を基準として無地部に隣接した両側縁の部分である。
上記のように製造されたコイン型ハーフセルを電気化学充放電器を用いて可逆性テストを行った。充電時に0.005V(vsLi/Li+)の電圧まで0.1Cのシーレート(C-rate)の電流密度で電流を加えて充電し、放電時に同じ電流密度で1.5Vの電圧まで放電を行った。このとき、下記式1のように、充電容量対比放電容量の比で初期可逆性を確認し、その結果を表1に図示した。
初期効率(%)= {(初期放電容量)/(初期充電容量)} × 100
Claims (16)
- 含浸区間、前リチウム化区間及びエージング区間に順次的に区画され、
内部に負極構造体が走行される前リチウム化溶液が収容された前リチウム化反応槽と、
前記前リチウム化溶液の外部に配置され、走行前の負極構造体が巻取される負極ロールと、
前記前リチウム化区間の前リチウム化溶液内に配置され、かつ前リチウム化溶液内で走行する負極構造体と対向するように、前記負極構造体から所定の間隔が離隔されて配置されるリチウム金属対極と、
前記負極構造体およびリチウム金属対極に連結される充放電部とを含み、
前記リチウム金属対極は、負極構造体の走行方向に行くほど負極構造体との離隔距離が連続的に増加するように傾けられた、負極の前リチウム化装置。 - 前記リチウム金属対極は、前記前リチウム化区間に配置される、請求項1に記載の負極の前リチウム化装置。
- 前記前リチウム化区間の終了地点でのリチウム金属対極と負極構造体との間の離隔距離は、前リチウム化区間のスタート地点でのリチウム金属対極と負極構造体との間の離隔距離の1.2倍~5倍である、請求項2に記載の負極の前リチウム化装置。
- 前記前リチウム化区間のスタート地点でのリチウム金属対極と負極構造体との離隔距離は1~20mmである、請求項3に記載の負極の前リチウム化装置。
- 前記負極構造体は、負極集電体の少なくとも一面に負極活物質層が形成され、かつ負極活物質層の幅方向の少なくとも一側に無地部が形成されたものである、請求項1に記載の負極の前リチウム化装置。
- 前記リチウム金属対極は、負極活物質層のみに対面する状態で配置される、請求項5に記載の負極の前リチウム化装置。
- 有機溶媒を含む洗浄槽をさらに含む、請求項1に記載の負極の前リチウム化装置。
- 前記洗浄槽を通過した負極構造体を乾燥する乾燥部および前記乾燥部に移送された負極構造体を巻取および巻出し得る回収ロールをさらに含む、請求項7に記載の負極の前リチウム化装置。
- 請求項1に記載の負極の前リチウム化装置および負極構造体を準備するステップと、
前記負極構造体を前リチウム化反応槽内の含浸区間を走行させながら、前リチウム化溶液に含浸させるステップと、
含浸された負極構造体を前リチウム化区間の前リチウム化溶液の内部を走行させながら前リチウム化するステップと、
前リチウム化された負極構造体をエージング区間でエージングするステップと、を含み、
前記前リチウム化は、負極構造体と離隔されるように配置されたリチウム金属対極を前リチウム化区間に配置し、前記負極構造体を電気化学充填して行い、
前記リチウム金属対極は、負極構造体の走行方向に行くほど負極構造体との離隔距離が連続的に増加するように傾けられた、負極の前リチウム化方法。 - 前記前リチウム化区間の終了地点でのリチウム金属対極と負極構造体との間の離隔距離は、前リチウム化区間のスタート地点でのリチウム金属対極と負極構造体との間の離隔距離の1.2倍~5倍である、請求項9に記載の負極の前リチウム化方法。
- 前記前リチウム化区間のスタート地点でのリチウム金属対極と負極構造体との間の離隔距離は1~20mmである、請求項9に記載の負極の前リチウム化方法。
- 前記負極構造体は、負極集電体の少なくとも一面に負極活物質層が形成され、かつ負極活物質層の幅方向の少なくとも一側に無地部が形成されたものである、請求項9に記載の負極の前リチウム化方法。
- エージングされたリチウム金属対極は、負極活物質層のみに対向する状態で配置される、請求項9に記載の負極の前リチウム化方法。
- 前記負極構造体を前リチウム化反応槽から取り出して洗浄するステップをさらに含む、請求項9に記載の負極の前リチウム化方法。
- 前記洗浄された負極構造体を乾燥させるステップをさらに含む、請求項14に記載の負極の前リチウム化方法。
- 請求項9から15の何れか一項に記載の負極の前リチウム化方法を含む、二次電池の製造方法。
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