JP6757894B2 - 電気化学デバイスの製造方法および電気化学デバイス - Google Patents
電気化学デバイスの製造方法および電気化学デバイス Download PDFInfo
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Description
上記第1乾燥工程、第2乾燥工程におけるCO2パージの効果を確認するために、以下の3つのセル(セルA1、セルB1、セルX1)を作成した。以下、特に説明がない限り、3つのセルの構成および作製方法は、共通である。
正極用の集電体(第1の集電体)として、2cm×2cmの平面形状のAl箔を用いた。1mol/lのアニリンモノマーと2mol/lの硫酸を含む水溶液を電解重合液として、定電流電解重合法により、Al箔の表裏両面にポリアニリンを合成した。電解重合後、蒸留水で洗浄、乾燥した。正極電極層の厚みは、どちらも60μmとした。
負極用の集電体(第2の集電体)として、2cm×2cmの平面形状のCu箔を用いた。ハードカーボン97wt%、カルボキシルメチルセルロース1wt%、スチレンブタジエンゴム2wtを混合した混合粉末と水とを重量比で40:60の割合で混練したカーボンペーストを作製し、これをCu箔の片面上に塗布、乾燥することにより、厚さ35μmの負極電極層を形成した。
セパレータについては、厚さ35μmのセルロースシートを所定のサイズに切り出し、これも110℃に加熱し、12時間保持する乾燥工程を行った後、常温に戻し、露点が−40℃以下のドライエアをパージして常圧に戻した。
プロピレンカーボネート(PC)とジメチルカーボネート(DMC)とを重量比1:1で混合した溶液に対して、0.2wt%のビニレンカーボネート(VC)を添加した。これを溶媒として、電解質としてLiPF6を1mol/l含む溶液を電解液とした。
これらの正極、負極、セパレータを、正極電極層および負極電極層がセパレータを介して対向するように積層することにより電気化学素子を作製した。すなわち、正極、負極およびセパレータを、負極/セパレータ/正極/セパレータ/負極の順に積層した構成とした。
電気化学素子を、3辺が予め封止された2枚のAlラミネートシートからなる外装体内に挿入した。次に、真空容器内にて常温で30分間保持する乾燥工程を行った後、それぞれ異なるガスをパージして常圧に戻した。すなわち、パージ用のガスとして、セルA1およびB1ではCO2を、セルX1では露点が−40℃以下のドライエアを用いた。
作製したセルを電流容量の10倍の電流値(10C)の条件で3.0Vにした後、3.0Vで30分間の定電圧を維持した。その後、露点−40℃以下の雰囲気下で外装体から電気化学素子を取り出し、正極、負極、セパレータに分解した後、正極をDMCで洗浄して電解液成分を除去した。そのように処理した正極を真空乾燥してDMCを除去した後、FT−IRにて各セルの正極電極層について分析を行った。なお、FT−IRは、ATR法にて測定した。
次に、実験1における正極および負極のサイズを2cm×2cmの平面形状から4cm×5cmの平面形状に変えた以外はセルA1、B1およびX1と同様にして、セルA2、B2およびX2をそれぞれ作製した。作製したセルについて、60℃で、3.5Vの電圧を印加した状態で、時間経過とともに容量(静電容量)、直流抵抗の変化率、および、外装体内のガスの変化量(ガス発生量)を評価するフロート試験を行った。結果を図3に示す。
次に、上記の実施形態で説明した巻回型のセルを作成し、実験2と同様のフロート試験を行った。負極電極層の炭素材料としてソフトカーボンを使用する以外は、上記の実施形態と同様に電気化学素子を作製し、直径1.25cm、長さ4cmの外装体内に封止した。その他の正極、負極の作製条件は実験1と同様であり、電気化学素子の乾燥後のパージをCO2で行ったセルB3(正極のみの乾燥後のパージはドライエアで行った。)と、正極および電気化学素子のどちらの乾燥後のパージもドライエアで行ったセルX3を作製した。2つのセルについて、実験2と同様に、フロート試験を行った。結果を図4に示す。
2 外装体
3 封口部材
3a、3b 貫通孔
4 正極
4a 第1の集電体
4b 正極電極層
5 負極
5a 第2の集電体
5b 負極電極層
6 セパレータ
7、8 リード線
Claims (8)
- 第1の集電体と導電性高分子を含む正極電極層とを含む正極を準備する工程と、
第2の集電体と負極電極層とを含む負極を準備する工程と、
前記正極と前記負極と電解液とを外装体内に封入する工程と、を備え、
前記正極を準備する工程は、前記正極を減圧雰囲気中に保持した後、前記減圧雰囲気中にCO2を主体とするガスを導入する工程を含む、
電気化学デバイスの製造方法。 - 第1の集電体と導電性高分子を含む正極電極層とを含む正極を準備する工程と、
第2の集電体と負極電極層とを含む負極を準備する工程と、
前記正極と前記負極とを含む積層体を準備する工程と、
前記正極と前記負極と電解液とを外装体内に封入する工程と、を備え、
前記積層体を準備する工程は、前記積層体を減圧雰囲気中に保持した後、前記減圧雰囲気中にCO2を主体とするガスを導入する工程を含む、
電気化学デバイスの製造方法。 - 前記負極電極層は、リチウムイオンの吸蔵および放出が可能な材料を含む、
請求項1または2に記載の電気化学デバイスの製造方法。 - 前記ガスを導入する際の温度は、15℃以上120℃以下の範囲である、
請求項1〜3のいずれかに記載の電気化学デバイスの製造方法。 - 前記導電性高分子はポリアニリンまたはその誘導体を含む、
請求項1〜4のいずれかに記載の電気化学デバイスの製造方法。 - 第1の集電体と導電性高分子を含む正極電極層とを含む正極と、
第2の集電体と負極電極層とを含む負極と、
電解液と、を備え、
前記正極電極層は、赤外分光法によって計測される吸収スペクトルにおいて、800cm−1での吸収強度と800cm−1付近での近接ピーク吸収強度との比が0.30より大きく、1085cm−1での吸収強度と1085cm−1付近での近接ピーク吸収強度との比が0.21より大きく、および、1340cm−1での吸収強度と1340cm−1付近での近接ピーク吸収強度との比が0.70より大きい、
電気化学デバイス。 - 前記正極と前記負極との間に介在されたセパレータをさらに含み、
前記負極電極層は、リチウムイオンが吸蔵された材料を含み、
前記電解液は、リチウムイオン及びアニオンを含む、
請求項6に記載の電気化学デバイス。 - 前記導電性高分子はポリアニリンまたはその誘導体を含む、
請求項6又は7に記載の電気化学デバイス。
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