JP2022516664A - リチウム二次電池用の負極活物質及びそれを含むリチウム二次電池 - Google Patents
リチウム二次電池用の負極活物質及びそれを含むリチウム二次電池 Download PDFInfo
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Abstract
Description
C.S.[nm]=K・λ/B・cosθ
C.S.[nm]=K・λ/B・cosθ
C.S.[nm]=K・λ/B・cosθ
ケイ素粉末と二酸化ケイ素粉末(SiO2)が1:1のモル比になり、ケイ素粉末とMg粉末が1:0.5のモル比になるようにケイ素粉末、二酸化ケイ素粉末(SiO2)及びMg粉末を混合した混合物を反応器に入れた。前記ケイ素粉末と二酸化ケイ素粉末(SiO2)とMg粉末との混合物を真空下で-100torrの減圧雰囲気で1,500℃に加熱し、前記ケイ素粉末及び二酸化ケイ素粉末(SiO2)の混合粉末による酸化ケイ素蒸気とマグネシウム蒸気とを同時に発生させることで気相反応させた後、冷却して800℃でケイ素-酸化ケイ素-マグネシウムシリケート複合体を析出した。続いて、前記ケイ素-酸化ケイ素-マグネシウムシリケート複合体をジェットミルで平均粒径(D50)5μmに粉砕した後、ケイ素-酸化ケイ素-マグネシウムシリケート複合体粒子粉末を回収した。この際、ケイ素-酸化ケイ素-マグネシウムシリケート複合体粒子の重量基準でMg含量は10.2%であった。
混合粉末の熱処理温度を1400℃にして製造したことを除いては、実施例1と同様の方法でケイ素-酸化ケイ素-マグネシウムシリケート複合体粒子粉末を製造した。
酸化ケイ素蒸気とマグネシウム蒸気とを同時に発生させることで気相反応させた後の冷却温度を600℃にしたことを除いては、実施例1と同様の方法でケイ素-酸化ケイ素-マグネシウムシリケート複合体粒子を製造した。
ケイ素粉末と二酸化ケイ素粉末(SiO2)が1:1のモル比になり、またケイ素粉末とMg粉末が1:0.5のモル比になるようにケイ素粉末、二酸化ケイ素粉末(SiO2)及びMg粉末を混合した混合物を反応器に入れた。前記ケイ素粉末と二酸化ケイ素粉末(SiO2)とMg粉末との混合物を真空下で-100torrの減圧雰囲気で1,500℃に加熱し、前記ケイ素粉末及び二酸化ケイ素粉末(SiO2)の混合粉末による酸化ケイ素蒸気とマグネシウム蒸気とを同時に発生させることで気相反応させた後、400℃で冷却してケイ素-酸化ケイ素-マグネシウムシリケート複合体を析出した。
最終段階において、アルゴン(Ar)雰囲気下、1200℃で5時間の熱処理をさらに行うことを除いては、比較例1と同様の方法でケイ素-酸化ケイ素-マグネシウムシリケート複合体粒子粉末を製造した。
前記実施例1~2及び比較例1~3で製造した試料の各々を負極活物質として使用し、導電材としてSuper-P black、バインダーとしてポリアクリル酸(Poly Acrylic acid;PAA)を重量基準にして80:10:10の比になるようにN-メチルピロリドンと混合してスラリー状の組成物を製造した。
前記実施例1~2及び比較例1~3の各々で製造された試料に対するX線回折分析結果を下記の表1に示した。
C.S.[nm]=K・λ/B・cosθ
C.S.[nm]=K・λ/B・cosθ
C.S.[nm]=K・λ/B・cosθ
前記実施例1~2及び比較例1~3の各々のケイ素-酸化ケイ素-マグネシウムシリケート複合体の粒子粉末を用いて製作したコインセルを、0.05Cの定電流で電圧が0.01Vになるまで充電し、0.05Cの定電流で電圧が1.5Vになるまで放電して、放電容量及び初期効率を求めた。
初期効率:100×(1回サイクルにおける放電容量)/(1回サイクルにおける充電容量)
Claims (10)
- リチウム二次電池用の負極活物質であって、
酸化ケイ素(SiOx,0<x≦2)マトリクスと、前記酸化ケイ素マトリクスに存在するケイ素(Si)結晶粒、MgSiO3結晶粒及びMg2SiO4結晶粒と、を含むケイ素-酸化ケイ素-マグネシウムシリケート複合体を含み、
前記ケイ素-酸化ケイ素-マグネシウムシリケート複合体において、MgSiO3結晶粒が5~30nmの範囲の結晶サイズを有し、Mg2SiO4結晶粒が20~100nmの範囲の結晶サイズを有し、
MgSiO3結晶粒とMg2SiO4結晶粒の含量比が、2:1~1:1の範囲の重量比で含まれる、リチウム二次電池用の負極活物質。 - 前記ケイ素結晶粒、MgSiO3結晶粒及びMg2SiO4結晶粒が、酸化ケイ素マトリクス内に埋め込まれている、請求項1に記載のリチウム二次電池用の負極活物質。
- 前記MgSiO3結晶粒が、5~25nmの範囲の結晶サイズを有する、請求項1または2に記載のリチウム二次電池用の負極活物質。
- 前記Mg2SiO4結晶粒が、20~50nmの範囲の結晶サイズを有する、請求項1から3のいずれか一項に記載のリチウム二次電池用の負極活物質。
- 前記Mg2SiO4結晶粒が、前記MgSiO3結晶粒の1倍から2倍の結晶サイズを有する、請求項1から4のいずれか一項に記載のリチウム二次電池用の負極活物質。
- 前記ケイ素-酸化ケイ素-マグネシウムシリケート複合体粒子の重量を基準として、全Mg金属が4~20重量%の量で含まれる、請求項1から5のいずれか一項に記載のリチウム二次電池用の負極活物質。
- MgSiO3結晶粒とMg2SiO4結晶粒の含量比が、1.4:1~1:1範囲の重量比で含まれる、請求項1から6のいずれか一項に記載のリチウム二次電池用の負極活物質。
- 請求項1から7のいずれか一項に記載のリチウム二次電池用の負極活物質を含む、リチウム二次電池用の負極。
- 請求項8に記載のリチウム二次電池用の負極を含む、リチウム二次電池。
- 請求項1に記載のケイ素-酸化ケイ素-マグネシウムシリケート複合体の製造方法であって、
ケイ素粉末と二酸化ケイ素粉末(SiO2)のモル比が1:0.5~1:1.5になり、ケイ素粉末とMg粉末のモル比が1:0.01~1:1になるようにケイ素粉末、二酸化ケイ素粉末(SiO2)及びMg粉末を混合した混合物を反応器に入れる段階(S1)と、
前記ケイ素粉末と二酸化ケイ素粉末(SiO2)とMg粉末との混合物を真空雰囲気で1,000~1,800℃に加熱し、前記ケイ素粉末及び二酸化ケイ素粉末(SiO2)の混合粉末による酸化ケイ素蒸気とマグネシウム蒸気とを同時に発生させることで気相反応させた後、650~900℃に冷却してケイ素-酸化ケイ素-マグネシウムシリケート複合体を析出する段階(S2)と、
前記析出されたケイ素-酸化ケイ素-マグネシウムシリケート複合体を平均粒径0.1~20μmに粉砕する段階(S3)と、を含む、方法。
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KR102002136B1 (ko) | 2017-07-11 | 2019-07-24 | 주식회사 지파워 | 피부 관리 시스템 및 이의 제어 방법 |
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2020
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- 2020-01-20 US US17/420,592 patent/US11942640B2/en active Active
- 2020-01-20 WO PCT/KR2020/000961 patent/WO2020149724A1/ko unknown
- 2020-01-20 EP EP20740917.8A patent/EP3902035A4/en active Pending
- 2020-01-20 CN CN202080009651.0A patent/CN113728465A/zh active Pending
Patent Citations (2)
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JP2018519648A (ja) * | 2015-06-15 | 2018-07-19 | デジュ・エレクトロニック・マテリアルズ・カンパニー・リミテッドDaejoo Electronic Materials Co., Ltd. | 非水電解質二次電池用負極材、その製造方法、及びこれを含む非水電解質二次電池 |
JP2018156922A (ja) * | 2017-03-20 | 2018-10-04 | デジュ・エレクトロニック・マテリアルズ・カンパニー・リミテッドDaejoo Electronic Materials Co., Ltd. | リチウム二次電池陰極材用シリコン複合酸化物及びその製造方法 |
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WO2024024273A1 (ja) * | 2022-07-29 | 2024-02-01 | パナソニックエナジー株式会社 | 二次電池 |
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KR20200090058A (ko) | 2020-07-28 |
US20220077467A1 (en) | 2022-03-10 |
JP7239712B2 (ja) | 2023-03-14 |
EP3902035A4 (en) | 2022-03-16 |
EP3902035A1 (en) | 2021-10-27 |
US11942640B2 (en) | 2024-03-26 |
WO2020149724A1 (ko) | 2020-07-23 |
CN113728465A (zh) | 2021-11-30 |
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