JP2018514073A - 電極およびその製造方法 - Google Patents
電極およびその製造方法 Download PDFInfo
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- JP2018514073A JP2018514073A JP2018503449A JP2018503449A JP2018514073A JP 2018514073 A JP2018514073 A JP 2018514073A JP 2018503449 A JP2018503449 A JP 2018503449A JP 2018503449 A JP2018503449 A JP 2018503449A JP 2018514073 A JP2018514073 A JP 2018514073A
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Abstract
Description
BMI(I/S)=BMI(Interface)/BMI(Surface)
1)活性層形成用組成物が塗布された集電体を予熱する段階;
2)前記予熱された集電体を定率蒸発させる段階;
3)減率蒸発させる段階;および
4)前記予熱段階よりも低い温度で残留溶媒を除去する段階.
BMI(I/S)=BMI(Interface)/BMI(Surface)
1)活性層形成用組成物が塗布された集電体を予熱する段階;
2)前記予熱された集電体を定率蒸発させる段階;
3)減率蒸発させる段階;および
4)前記予熱段階よりも低い温度で残留溶媒を除去する段階.
撹はん容器にPVDFバインダーと導電材および活物質を投入してプラネタリーミキサーを利用して撹はんする。ペーストの状態を肉眼で確認した後、コーティング可能な粘度となるようにN−メチルピロリドン(NMP)を少量ずつ投入して撹はんすることを繰り返して活性層形成用組成物を製造する。
コンマコーターを利用してアルミニウム集電体ホイルの上に活性層形成用組成物を塗布する。コーティングの速度とコータースリットのギャップを調節してコーティング厚さを調節する。コーティングされた電極を10個の乾燥区域を有する乾燥炉で30分間乾燥する。適当な大きさに電極を裁断した後、ロールプレスで押圧して所望の空隙率に到達するまで圧延を繰り返す。圧延が完了した電極は必要に応じて100〜150℃真空オーブンで12時間の間追加乾燥を実施する。
26×76×1mmのスライドガラスに両面テープを付着する。3Mセロハンテープの接着面が上にくるように両面テープの上に付着する。15×150mm2の大きさで裁断された電極試料をセロハンテープの接着面に付着した後、ハンドラミネーター(hand laminator)で一度押し出す。各電極サンプル当たり、3個の試料を準備して付着後すぐに測定する。物性分析器(Texture analyzer、TA)を利用して180度、0.3m/minの条件で測定する。
ダイヤモンドカッターを利用して製造された電極を傾斜切削することによって、電極の全体深さに沿った断面に露出されるようにした後、赤外線分光分析装置(ATR IR spectroscopy)を利用して吸収スペクトルに基づいて電極の深さによるバインダーの分布量をグラフで表現し、深さ別の積分強度の合算を通じてBMI(Interface)およびBMI(Surface)を計算して、BMI(I/S)を算出する。
[活性層形成用組成物の製造]
PVDFバインダー、導電材(Denka black)および活物質(バインダー:導電材:活物質=91.5:4.3:4.2)の混合物に総固形分含量が約68%程度となるようにN−メチルピロリドン(NMP)溶媒を約38.9重量部投入して活性層形成用組成物を製造した。
前記活性層形成用組成物をコンマコーターを利用してアルミニウム集電体ホイルの上に塗布する。引き続き、10個の乾燥区域を含み、電極の上下部を熱風乾燥できる熱風生成部を含む乾燥炉で、順次予熱工程(第1区域、約150℃〜180℃、風量1,200rpm〜1,600rpm)、定率蒸発工程(第2区域〜第5区域、約105℃〜130℃、風量1,200rpm〜1,600rpm)、減率蒸発工程(第6および第7区域、約90℃〜105℃、風量500rpm〜1,000rpm)および残留溶媒除去工程(第8および9区域、約130℃〜145℃、風量500rpm〜1,000rpm)を実施する。残留溶媒除去工程後、約40℃〜60℃の温度範囲で減温する工程(第10区域)を遂行し、集電体上に形成された活性層を含む電極を製造した。前記電極の活性層の集電体に対する剥離力およびBMI(I/S)値は下記の表1の通りである。
活性層形成用組成物が塗布された集電体を10個の乾燥区域で約130℃の温度で一定に乾燥する段階を実施したことを除いては、実施例1と同じ方式で電極を製造した。比較例1による電極の活性層の集電体に対する剥離力およびBMI(I/S)値は下記の表1の通りである。
活性層形成用組成物が塗布された集電体を予熱工程(第1および第2乾燥区域、約130℃〜135℃、風量約50Nm3/min)、定率蒸発工程(第3〜第8乾燥区域、約120℃〜125℃、風量約100Nm3/min)および減率蒸発工程(第9および第10乾燥区域、約135℃〜140℃、風量約70Nm3/min)の温度範囲で遂行したことを除いては、実施例1と同じ方式で電極を製造した。比較例2による電極の活性層の集電体に対する剥離力およびBMI(I/S)値は下記の表1の通りである。
200:集電体
300:活性層
Claims (19)
- 集電体;および
前記集電体上に形成され、バインダーを有する活性層を含み、
下記の式1で表示されるBMI(I/S)が0.018〜0.300の範囲内にある電極:
[式1]
BMI(I/S)=BMI(Interface)/BMI(Surface)
式1において、BMI(Interface)は活性層に存在する全体バインダーの量対比、活性層の集電体と接する面を基準として、活性層の厚さ方向に0%〜15%に該当する領域に存在するバインダーの量(%)を意味し、BMI(Surface)は活性層に存在する全体バインダーの量対比、活性層の集電体と接する面を基準として、活性層の厚さ方向に85%〜100%に該当する領域に存在するバインダーの量(%)を表わす。 - BMI(Interface)は0.8%〜6.0%の範囲内にある、請求項1に記載の電極。
- BMI(Surface)は22.0%〜42.3%の範囲内にある、請求項1に記載の電極。
- 集電体はステンレススチール、ニッケル、チタン、焼成炭素、銅またはアルミニウムである、請求項1に記載の電極。
- バインダーはアクリル系バインダーまたはフッ素系バインダーである、請求項1に記載の電極。
- 活性層は導電材および活物質をさらに含む、請求項1に記載の電極。
- 活性層は安定化剤、分散剤、界面活性剤、脱泡剤および架橋剤のうち選択されるいずれか一つ以上の添加剤をさらに含む、請求項1に記載の電極。
- 活性層は15×150mm2大きさの電極試片を常温で0.3m/minの剥離速度および180度の剥離角度で測定した集電体に対する剥離力が30gf/cm以上である、請求項1に記載の電極。
- 集電体上にバインダー、導電材および活物質を含む活性層形成用組成物を塗布した後、乾燥する段階を含む、請求項1に記載された電極の製造方法。
- 乾燥する段階は下記の1)〜4)の段階を含む、請求項9に記載の電極の製造方法:
1)活性層形成用組成物が塗布された集電体を予熱する段階;
2)前記予熱された集電体を定率蒸発させる段階;
3)減率蒸発させる段階;および
4)前記予熱段階よりも低い温度で残留溶媒を除去する段階。 - 段階1)は150℃〜180℃の範囲内で遂行される、請求項10に記載の電極の製造方法。
- 段階2)は段階1)対比25℃〜60℃範囲の低い温度で遂行される、請求項10に記載の電極の製造方法。
- 段階2)を終了した後電極内の残留溶媒は1重量%〜5重量%の範囲内にある、請求項10に記載の電極の製造方法。
- 段階3)は90℃〜105℃の範囲内で遂行される、請求項10に記載の電極の製造方法。
- 段階3)を終了した後電極内の残留溶媒は0.05重量%〜0.8重量%の範囲内にある、請求項10に記載の電極の製造方法。
- 段階4)は130℃〜145℃の範囲内で遂行される、請求項10に記載の電極の製造方法。
- 段階4)を終了した後電極内の残留溶媒は0.05重量%以下である、請求項10に記載の電極の製造方法。
- 乾燥する段階は、段階4)の以後に前記段階4)の温度より50℃〜100℃範囲の低い温度で減温する段階をさらに含む、請求項10に記載の電極の製造方法。
- 請求項1に記載された電極を含む、電池。
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