JP2021501977A - 負極活物質、前記負極活物質を含む負極、及び前記負極を含む二次電池 - Google Patents
負極活物質、前記負極活物質を含む負極、及び前記負極を含む二次電池 Download PDFInfo
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Abstract
Description
本出願は、2017年11月9日付で出願された韓国特許出願第10−2017−0148839号に基づいた優先権の利益を主張し、当該韓国特許出願の文献に開示されている全ての内容は、本明細書の一部として含まれる。
実施例1:電池の製造
(1)負極活物質の製造
最大粒径(Dmax)が45μmのシリコン(Si)10gとLiF 0.2gをイソプロパノール30gに添加して混合溶液を製造した。その後、ジルコニア材質のビーズ(平均粒径:0.3mm)を利用して、1,200rpmのビーズ回転速度で30時間前記混合物を粉砕した。このとき、生成されたシリコンの平均粒径(D50)は100nmで、前記シリコンの表面に形成されたSiO2の厚さは10nmであり、前記SiO2上に配置されたLiFの厚さは0.01nmから10nmであった。
前記製造された負極活物質、導電材である微粒黒鉛、バインダーであるポリアクリロニトリル(Polyacrylonitrile)を7:2:1の重量比で混合して混合物0.2gを製造した。溶媒であるN−メチル−2−ピロリドン(NMP)3.1gを前記混合物に添加して負極スラリーを製造した。前記負極スラリーを厚さが20μmの負極集電体である銅(Cu)金属薄膜に塗布、乾燥した。この時に循環される空気の温度は80℃であった。次いで、圧延(roll press)し、130℃の真空オーブンで12時間乾燥して負極を製造した。
製造された負極を1.7671cm2の円形に切断したリチウム(Li)金属薄膜を正極とした。前記正極と負極の間に多孔性ポリエチレンのセパレータを介在し、メチルエチルカーボネート(EMC)とエチレンカーボネート(EC)の混合体積比が7:3である混合溶液に0.5重量%で溶解されたビニレンカーボネートを溶解させ、1M濃度のLiPF6が溶解された電解液を注入してリチウムコインハーフセル(coin half−cell)を製造した。
(1)負極活物質の製造
最大粒径(Dmax)が45μmのシリコン(Si)10gとLiF 2.5gをイソプロパノール30gに添加して混合溶液を製造した。その後、ジルコニア材質のビーズ(平均粒径:0.3mm)を利用して、1,200rpmのビーズ回転速度で30時間前記混合物を粉砕した。このとき、生成されたシリコンの平均粒径(D50)は100nmで、前記シリコンの表面に形成されたSiO2の厚さは10nmであり、前記SiO2上に配置されたLiFの厚さは1nmから30nmであった。
前記で製造された負極活物質を用いたことを除き、実施例1と同様の方法で負極及び二次電池を製造した。
(1)負極活物質の製造
最大粒径(Dmax)が45μmのシリコン(Si)10gとLiF 0.1gをイソプロパノール30gに添加して混合溶液を製造した。その後、ジルコニア材質のビーズ(平均粒径:0.3mm)を利用して、1,200rpmのビーズ回転速度で30時間前記混合物を粉砕した。このとき、生成されたシリコンの平均粒径(D50)は100nmで、前記シリコンの表面に形成されたSiO2の厚さは10nmであり、前記SiO2上に配置されたLiFの厚さは0.01nmから5nmであった。
前記で製造された負極活物質を用いたことを除き、実施例1と同様の方法で負極及び二次電池を製造した。
(1)負極活物質の製造
実施例1の負極活物質の製造ステップにおいて、スラリーの製造時にLiFを添加していないことを除き、実施例1と同様の方法で負極活物質を製造した。
前記負極活物質を用いて、実施例1と同様の方法で負極及び二次電池を製造した。
実施例1から3及び比較例1の電池に対して充電/放電を行い、放電容量、初期効率、容量維持率及び電極(負極)厚さ変化率を評価し、これを下記表1に記載した。
充電条件:CC(定電流)/CV(定電圧)(5mV/0.005C current cut−off)
放電条件:CC(定電流)条件 1.5V
初期効率(%)=(1回放電後の放電容量/1回の充電容量)×100
容量維持率(%)=(49回の放電容量/1回の放電容量)×100
電極厚さ変化率(%)=(最終の負極厚さ変化量/最初の負極厚さ)×100
Claims (10)
- 複数のナノ粒子を含む炭素質マトリックスを含んでなり、
前記ナノ粒子は、
シリコンコアと、
前記シリコンコア上に配置されてSiOx(0<x≦2)を含む酸化膜層と、
前記酸化膜層の表面の少なくとも一部を覆ってLiFを含むコーティング層とを含む負極活物質。 - 前記シリコンコアの平均粒径(D50)は40nmから400nmである、請求項1に記載の負極活物質。
- 前記酸化膜層の厚さは0.01nmから20nmである、請求項1に記載の負極活物質。
- 前記LiFは、前記負極活物質の全重量を基準に0.1重量%から25重量%で含まれる、請求項1に記載の負極活物質。
- 前記コーティング層の厚さは0.01nmから50nmである、請求項1に記載の負極活物質。
- 前記炭素質マトリックスは、前記負極活物質の全重量を基準に5重量%から50重量%で含まれる、請求項1に記載の負極活物質。
- 前記酸化膜層がリチウムシリケートをさらに含む、請求項1に記載の負極活物質。
- 前記リチウムシリケートは、Li2SiO3、Li4SiO4及びLi2Si2O5のうち少なくともいずれか一つを含む、請求項7に記載の負極活物質。
- 請求項1から請求項8のいずれか一つに記載の負極活物質を含む負極。
- 請求項9に記載の負極と、
正極と、
前記正極と前記負極の間に介在されたセパレータと、
電解質とを含む二次電池。
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KR10-2017-0148839 | 2017-11-09 | ||
PCT/KR2018/013658 WO2019093830A1 (ko) | 2017-11-09 | 2018-11-09 | 음극 활물질, 상기 음극 활물질을 포함하는 음극, 및 상기 음극을 포함하는 이차 전지 |
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US20200266424A1 (en) | 2020-08-20 |
WO2019093830A1 (ko) | 2019-05-16 |
KR20190052953A (ko) | 2019-05-17 |
JP2022125285A (ja) | 2022-08-26 |
CN111316483B (zh) | 2023-07-04 |
ES2943089T3 (es) | 2023-06-08 |
JP7438599B2 (ja) | 2024-02-27 |
PL3694031T3 (pl) | 2023-05-29 |
JP7164123B2 (ja) | 2022-11-01 |
CN111316483A (zh) | 2020-06-19 |
EP3694031B1 (en) | 2023-03-29 |
HUE061829T2 (hu) | 2023-08-28 |
EP3694031A1 (en) | 2020-08-12 |
KR102244953B1 (ko) | 2021-04-27 |
EP3694031A4 (en) | 2020-12-09 |
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