JP7094943B2 - 二次電池用のシリコン系活物質粒子及びその製造方法 - Google Patents
二次電池用のシリコン系活物質粒子及びその製造方法 Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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Description
また、機械的圧縮及び剪断応力が大きすぎると、シリコン粒子が微細粒子化され、活物質として十分な容量が得られないため、粉砕法における応力制御が必要となる。
平均直径約5μmの市販のポリシリコン粉末を用意して、95重量%のエタノールに対して、α-リポ酸、オクテン、没食子酸プロピル、トコフェロール、グルタチオン、ブチルヒドロキルアニソール、及びフェノールをそれぞれ5重量%含む分散用溶媒中に分散させることによって、粉砕前混合物を調製した。
平均直径約5μmの市販のポリシリコン粉末を用意し、当該ポリシリコン粉末を100重量%のエタノールを含む分散用溶媒中に溶解して粉砕前混合物を調製した。前記粉砕前混合物に圧縮応力及び剪断応力を加えることができる時間制御ミル粉砕プロセスを少なくとも1回繰り返し、それによってシリコン系活物質粒子を調製した。
実施例及び比較例におけるシリコン負極活物質を含むサンプルについて電池特性を評価
した。実施例及び比較例におけるシリコン負極活物質粒子を使用して作製したハーフセル
を用いることにより、酸素含有量(%)、重量当たりの容量(capacity)(mA
h/g)、及び初期効率(%)の大きさを評価した。測定した実験結果を以下の表1に示
す。特に、充電/放電速度は0.5Cであった。基準初期容量は4,200mAh/gで
あり、これはシリコンの理論容量である。
SC シリコン粒子
PS 平面状の表面
CS 導電層
CO 化学酸化物層
SEP シリコン系活物質複合体
CM カーボンマトリックス
Claims (12)
- シリコン系活物質粒子の調製方法であって、
シリコン粉末を提供する工程と、
水、脱イオン水又はアルコール溶媒以外である酸化防止剤を含有する分散用溶媒中に前記シリコン粉末が分散された、粉砕前混合物を提供する工程と、
前記粉砕前混合物の前記シリコン粉末に機械的圧縮及び剪断応力を加えて前記シリコン粉末を粒状にし、それによって前記酸化防止剤により制御された酸素含有量を有するシリコン粒子を形成する工程と、
前記シリコン粒子を含む生成物を乾燥して、シリコン系活物質粒子を得る工程と、を備える調製方法。 - 前記酸化防止剤は、α-リポ酸、オクテン、没食子酸プロピル、トコフェロール、グルタチオン、ブチルヒドロキシアニソール、ブチル化ヒドロキシトルエン、tert-ブチルヒドロキノン、ノルジヒドログアイアレチン酸、セサモール、ビタミンE、ビタミンC、及びケルセチンからなる群から選択される、請求項1に記載の方法。
- 前記酸化防止剤は、前記シリコン粉末の重量に対して1重量%~10重量%の量で使用される、請求項1に記載の方法。
- 前記分散用溶媒は、水、脱イオン水、アルコール溶媒、又はそれらの2種以上の混合物をさらに含む、請求項1に記載の方法。
- 前記アルコール溶媒は、エチルアルコール、メチルアルコール、グリセリン、プロピレングリコール、イソプロピルアルコール、イソブチルアルコール、ポリビニルアルコール、シクロヘキサノール、オクチルアルコール、デカノール、ヘキサデカノール、エチレングリコール、1,2-オクタンジオール、1,2-ドデカンジオール、及び1,2-ヘキサデカンジオール、又はそれらの混合物、からなる群から選択されるいずれか1種を含む、請求項4に記載の方法。
- 機械的圧縮及び剪断応力を加える前記工程が、回転研磨プレートと固定プレートとの間に前記粉砕前混合物を供給しながらプレス及び研磨を行う研削によって達成される、請求項1に記載の方法。
- 前記シリコン系活物質粒子は、シリコン粒子のコア上に形成された化学酸化物層を含む、請求項1に記載の方法。
- 前記シリコン系活物質粒子中、前記シリコン粒子の前記コア及び前記化学酸化物層の総重量に対する前記酸素含有量は、5重量%~15重量%の範囲又は6重量%~10重量%の範囲内に制限される、請求項7に記載の方法。
- 前記化学酸化物層は、前記機械的圧縮及び剪断応力を加える工程の間、前記酸化防止剤を含む前記分散用溶媒によって低い温度で形成された酸化シリコン層である、請求項7に記載の方法。
- 前記シリコン粒子の前記コアは、低い結晶性を有する又は非晶質である、請求項7に記載の方法。
- 前記シリコン系活物質粒子の平均粒子径は、30nm~300nmの範囲又は30nm~200nmの範囲内である、請求項1に記載の方法。
- 前記シリコン粒子を含む前記生成物と炭素前駆体溶媒とを混合して分散溶液を形成する工程と、
前記分散溶液由来の炭素前駆体マトリックス内に、前記シリコン粒子が分散された固体二次粒子を形成する工程と、
前記固体二次粒子を熱処理して前記炭素前駆体マトリックスを炭化し、それによってシリコン系二次活物質粒子を形成する工程をさらに備える、請求項1に記載の方法。
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KR1020160106853A KR101773719B1 (ko) | 2016-08-23 | 2016-08-23 | 2 차 전지용 실리콘계 활물질 입자 및 이의 제조 방법 |
KR10-2016-0106853 | 2016-08-23 | ||
PCT/KR2017/009223 WO2018038538A1 (ko) | 2016-08-23 | 2017-08-23 | 2 차 전지용 실리콘계 활물질 입자 및 이의 제조 방법 |
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EP3560891A4 (en) | 2020-01-22 |
CN109843799B (zh) | 2022-10-14 |
CN109843799A (zh) | 2019-06-04 |
JP2019533273A (ja) | 2019-11-14 |
US11171332B2 (en) | 2021-11-09 |
EP3560891A1 (en) | 2019-10-30 |
US20190190020A1 (en) | 2019-06-20 |
KR101773719B1 (ko) | 2017-09-01 |
WO2018038538A1 (ko) | 2018-03-01 |
EP3560891B1 (en) | 2021-05-05 |
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