JP6517326B2 - リチウム二次電池用負極活物質の製造方法 - Google Patents
リチウム二次電池用負極活物質の製造方法 Download PDFInfo
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- JP6517326B2 JP6517326B2 JP2017513514A JP2017513514A JP6517326B2 JP 6517326 B2 JP6517326 B2 JP 6517326B2 JP 2017513514 A JP2017513514 A JP 2017513514A JP 2017513514 A JP2017513514 A JP 2017513514A JP 6517326 B2 JP6517326 B2 JP 6517326B2
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- negative electrode
- active material
- polycrystalline silicon
- electrode active
- lithium secondary
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- 229910052744 lithium Inorganic materials 0.000 title claims description 45
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Description
本出願は、2014年10月2日付韓国特許出願第2014−0133430号及び2015年9月30日付韓国特許出願第2015−0137454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た全ての内容は本明細書の一部として含まれる。
本発明は、リチウム二次電池用負極活物質、この製造方法、及びこれを含むリチウム二次電池に関する。
N=(logz/log2)+1 (1)
LixMyM’zO2 (1)
(前記化学式(1)で、前記M及びM’はそれぞれ独立的にFe、Ni、Co、Mn、Cr、Zr、Nb、Cu、V、Mo、Ti、Zn、Al、Ga、Mg、B及びこれらの組合せからなる群より選択される元素であり、前記x、y、zはそれぞれ独立的な酸化物組成元素等の原子分率であって、0<x≦1、0<y≦1、0<z≦1、0<x+y+z≦2である。)
平均粒径(D50)が5μmである多結晶ケイ素粉末(気孔度:<1体積%、平均結晶粒の大きさ:49nm)を1350℃でアルゴン(Ar)の非活性雰囲気下に1時間の間熱処理して結晶粒界に不純物を凝集させた後、蒸溜水(DIW)に含浸して10分間に亘って20〜25℃まで急速冷却し、塩酸0.5M濃度の水溶液中に30分間含浸して酸処理した。その結果として、金属不純物が除去された多孔性の多結晶ケイ素粉末を収得し、これを負極活物質として用いた。
前記実施例1で製造した多孔性の多結晶ケイ素粉末をスクロース(sucrose)粉末2gとともに蒸溜水240gに混合した。その結果として収得した混合液を噴霧乾燥器に注入した後、噴霧乾燥(spray drying)して前記多孔性の多結晶ケイ素粉末上にスクロース粉末をコーティングした。このとき、噴霧乾燥器内の注入口(in−let)の温度は200℃、排出口(out−let)の温度は120℃にそれぞれ設定し、また前記混合液の裝入速度は20ml/分とした。前記噴霧乾燥工程の結果として、スクロース粉末がコーティングされた多孔性の多結晶ケイ素粉末を収得し、これをアルゴン雰囲気下に500℃の焼成炉で2時間の間焼成及び炭化した。その結果として、非晶質炭素がコーティングされた多孔性の多結晶ケイ素粉末を収得し、これを負極活物質として用いた。このとき、前記非晶質炭素コーティング層の含量は、負極活物質の総重量に対して5重量%であった。
前記実施例1で用いた平均粒径(D50)が5μmである多結晶ケイ素粉末(気孔度:<1体積%、平均結晶粒の大きさ:49nm)10gを、5Mフッ酸溶液300mlと0.015Mの硝酸銀溶液700mlを混合して製造した50℃のエッチング溶液に30分間浸漬した。このとき、硝酸銀溶液のAg+イオンがケイ素から電子を受けてケイ素粉末の表面に吸着され、電子を奪われたSi+をフッ酸(HF)に溶かすことによりエッチングが行われる。エッチングが完了した多孔性ケイ素粉末を蒸溜水を用いて中和させた後、20%硝酸溶液に浸漬して表面に吸着されたAgを除去し、再び中和して多孔性の多結晶ケイ素粉末を製造し、これを負極活物質として用いた。
前記実施例1で用いた平均粒径(D50)が5μmである多結晶ケイ素粉末(気孔度:<1体積%、平均結晶粒の大きさ:49nm)を負極活物質として用いた。
前記実施例1及び2で製造した負極活物質をそれぞれ用いてリチウム二次電池を製造した。
前記比較例1で製造した負極活物質を走査電子顕微鏡(SEM)を用いて観察した。その結果を図1に示した。
前記実施例1での負極活物質の製造時に、熱処理前と後の多結晶ケイ素粉末の断面を走査電子顕微鏡(SEM)を用いて観察した。その結果を図2a及び図2bに示した。
前記実施例1での負極活物質の製造時に、熱処理された多結晶ケイ素粉末に対する酸処理前/後の金属不純物の含量変化を誘導結合プラズマ−原子放出分光器(Inductively Coupled Plasma−Atomic Emission Spectrometer,ICP−AES)を用いて分析した。その結果を表1に示した。
前記実施例1、比較例1、2の負極活物質に対して気孔度及び平均結晶粒の大きさをそれぞれ測定した。その結果を下記表2に示した。
前記実施例1、2及び比較例1、2の負極活物質を用いて半分電池を製造した後、初期充放電特性、容量維持率及び負極厚さ膨張抑制効果を評価した。その結果を下記表3に示した。
厚さ膨張率=[(50番目の充放電サイクルでの満充電された負極の厚さ−初期負極の厚さ)/(初期負極の厚さ−銅の集電体の厚さ)] (2)
Claims (5)
- 金属不純物を含む多結晶シリコンを熱処理した後、冷却し、結晶粒界に前記金属不純物を含む多結晶シリコンを準備する段階、及び
前記結晶粒界に金属不純物を含む多結晶シリコンを酸処理して前記金属不純物を溶出させることにより、結晶粒界に気孔が形成された多孔性の多結晶シリコンを製造する段階
を含み、
前記熱処理が、750℃から1400℃での温度で行われるものであり、
前記冷却が、20℃から30℃の温度まで10分以内の時間の間に亘って冷却させることにより行われるものであり、
前記多結晶シリコンの原料物質の金属不純物の含量が、7,458〜100,000ppmであり、
前記結晶粒界に気孔が形成された多孔性の多結晶シリコンの気孔度が、5体積%から18体積%である、
リチウム二次電池用負極活物質の製造方法。 - 前記金属不純物が、Ni、Sc、Ti、V、Cr、Mn、Fe、Co、Cu、Zn、Y、Zr、Nb、Mo、Ru、Rh、Pd、La、Hf、Ta、W、Re、Os、Mg、Ca、P、Al、Ge、Sn、Sb、Bi、及びLiからなる群より選択されるいずれか一つまたは二つ以上の混合物を含むものである請求項1に記載のリチウム二次電池用負極活物質の製造方法。
- 前記酸は、フッ酸、塩酸、硫酸、硝酸及びリン酸からなる群より選択されるいずれか一つまたは二つ以上の混合物を含むものである請求項1に記載のリチウム二次電池用負極活物質の製造方法。
- 前記多孔性の多結晶シリコンの製造後、前記多孔性の多結晶シリコンの表面上に、炭素系物質を含むコーティング層を形成する段階をさらに含む請求項1に記載のリチウム二次電池用負極活物質の製造方法。
- 前記炭素系物質が、非晶質炭素を含むものである請求項4に記載のリチウム二次電池用負極活物質の製造方法。
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- 2015-10-01 CN CN201580053723.0A patent/CN107112519B/zh active Active
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- 2015-10-01 EP EP15846949.4A patent/EP3203550B1/en active Active
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US10637051B2 (en) | 2020-04-28 |
EP3203550A4 (en) | 2017-08-09 |
EP3203550B1 (en) | 2019-07-03 |
PL3203550T3 (pl) | 2019-11-29 |
US20170309902A1 (en) | 2017-10-26 |
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KR101766535B1 (ko) | 2017-08-10 |
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