JP6204581B2 - リチウム二次電池用正極活物質の製造方法 - Google Patents
リチウム二次電池用正極活物質の製造方法 Download PDFInfo
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- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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- C01G45/12—Manganates manganites or permanganates
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
- C01G45/1257—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing lithium, e.g. Li2MnO3, Li2[MxMn1-xO3
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- C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
- C01G51/44—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese
- C01G51/50—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO2]n-, e.g. Li(CoxMn1-x)O2, Li(MyCoxMn1-x-y)O2
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- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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Description
(1−x)LiM’O2−yAy −xLi2MnO3−y’Ay’(1)
前記式中、
M’は、MnaMbであり、
Mは、Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn及び2周期の遷移金属からなる群から選択される1つ以上であり、
Aは、PO4、BO3、CO3、F及びNO3のアニオンからなる群から選択される1つ以上であり、
0<x<1、0<y≦0.02、0<y’≦0.02、0.5≦a≦1.0、0≦b≦0.5、a+b=1である。
正極の製造
正極活物質としてLi 1.2 Co 0.1 Ni 0.1 Mn 0.6 O 2 を使用し、BF42.0gが溶解している100mlの溶液を前記正極活物質に付加して攪拌し、250℃の温度で熱処理した後、水で洗浄し、真空乾燥する脱リチウム化過程を行い、機械的ミリング法を用いて表面改質過程を行った正極活物質を製造した。
負極としては天然黒鉛を使用し、導電材(カーボンブラック)、バインダー(PVdF)をそれぞれ90:5:5の重量比でNMP(N−methyl−2−pyrrolidone)に入れ、ミキシングして、負極合剤を製造した。
前記負極と正極との間に分離膜(Toray、厚さ:15μm)を介在して電極組立体を製造した後、前記電極組立体をパウチ型電池ケースに収納し、エチルカーボネートとジメチルカーボネートとエチルメチルカーボネートが体積比を基準として1:1:1で混合されており、リチウム塩として1MのLiPF6を含んでいるリチウム非水系電解液を添加して、リチウム二次電池を製造した。
正極活物質の製造過程の脱リチウム化過程において、300℃の温度で熱処理した以外は、実施例1と同様の方法でリチウム二次電池を製造した。
正極活物質の製造過程の脱リチウム化過程において、400℃の温度で熱処理した以外は、実施例1と同様の方法でリチウム二次電池を製造した。
正極活物質の製造過程において、脱リチウム化過程及び表面改質過程を経ていないこと以外は、実施例1と同様の方法でリチウム二次電池を製造した。
正極活物質の製造過程において、脱リチウム化過程を経ていないこと以外は、実施例1と同様の方法でリチウム二次電池を製造した。
正極活物質の製造過程において、表面改質過程を経ていないこと以外は、実施例1と同様の方法でリチウム二次電池を製造した。
実施例1〜3及び比較例1〜3の二次電池を0.1C、5mAで3.35Vまで充電し、常温で2日、60℃で1日間保管した後、93kPaで30秒〜1分間副反応ガス除去過程を経た後、0.5Cで4.3Vまで充電した後、0.05Cまで定電圧充電し、0.5Cで2.5Vまで放電し、これを45℃の温度で250サイクル繰り返し行った後、電池のガス発生量を測定し、その結果を下記の表1に示す。
実施例1及び比較例1の二次電池を、理論容量15mAh/eaを0.5Cと算定し、17.8mAの電流を印加する充放電を通じて0.5C容量を測定し、2Cに該当する100mAhの電流を印加する充放電を通じて3C容量を測定し、2C容量/1C容量でレート特性を表現して、その結果を下記の表2に示す。
Claims (4)
- 下記化学式(1)で表される化合物から選択された1つ以上のリチウム遷移金属酸化物を、BF4が溶解している溶液に付加して撹拌し、前記リチウム遷移金属酸化物を熱処理することを含む化学的脱リチウム化過程と、
化学的脱リチウム化されたリチウム遷移金属酸化物の表面改質過程と、
を含み、
前記化学的脱リチウム化されたリチウム遷移金属酸化物の表面改質過程を機械的ミリング法で行う、リチウム二次電池用正極活物質の製造方法:
(1−x)LiM’O2−yAy−xLi2MnO3−y’Ay’ (1)
前記式中、
M’が、MnaMbであり、
Mが、Ni、Ti、Co、Al、Cu、Fe、Mg、B、Cr、Zr、Zn及び2周期の遷移金属からなる群から選択される1つ以上であり、
Aが、PO4、BO3、CO3、F及びNO3のアニオンからなる群から選択される1つ以上であり、
0<x<1、0≦y≦0.02、0≦y’≦0.02、0.5≦a≦1.0、0≦b≦0.5、a+b=1である。 - 前記熱処理を250℃以上の温度で行うことを特徴とする、請求項1に記載の製造方法。
- 前記熱処理を300℃以上の温度で行うことを特徴とする、請求項2に記載の製造方法。
- 前記熱処理を400℃以上の温度で行うことを特徴とする、請求項3に記載の製造方法。
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KR10-2013-0090956 | 2013-07-31 | ||
KR20130090956 | 2013-07-31 | ||
PCT/KR2014/007021 WO2015016621A1 (ko) | 2013-07-31 | 2014-07-31 | 리튬 이차전지용 양극 활물질의 제조방법 |
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JP6204581B2 true JP6204581B2 (ja) | 2017-09-27 |
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US (1) | US10008720B2 (ja) |
JP (1) | JP6204581B2 (ja) |
KR (1) | KR101623719B1 (ja) |
CN (1) | CN105264695B (ja) |
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KR20160112766A (ko) * | 2015-03-20 | 2016-09-28 | 주식회사 엘지화학 | 고전압 리튬 이차전지용 양극 활물질 및 이를 포함하는 리튬 이차전지 |
CN107394199A (zh) * | 2017-07-20 | 2017-11-24 | 北京理工大学 | 一种高镍三元正极材料存放后电化学性能的恢复方法 |
KR102617870B1 (ko) * | 2018-07-25 | 2023-12-22 | 주식회사 엘지에너지솔루션 | 리튬 이차전지용 리튬 금속의 전처리 방법 |
KR102530216B1 (ko) * | 2020-06-05 | 2023-05-09 | 포항공과대학교 산학협력단 | 리튬 이차전지용 양극 활물질의 전기화학적 특성을 활성화시키는 방법 및 리튬 이차전지용 양극 활물질 |
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KR100528455B1 (ko) * | 2004-03-19 | 2005-11-15 | 한국과학기술연구원 | 고성능 리튬이차전지 양극 활성물질 제조방법 및 상기방법을 이용하여 제조한 양극 활성 물질을 사용한리튬이차전지 |
JP2006228704A (ja) * | 2005-01-18 | 2006-08-31 | Nissan Motor Co Ltd | 二次電池用電極及びこれを用いた非水電解液二次電池 |
EP2067198A2 (en) * | 2006-09-25 | 2009-06-10 | Board of Regents, The University of Texas System | Cation-substituted spinel oxide and oxyfluoride cathodes for lithium ion batteries |
US8835027B2 (en) | 2007-09-21 | 2014-09-16 | Uchicago Argonne, Llc | Positive electrodes for lithium batteries |
JP5505608B2 (ja) * | 2008-09-10 | 2014-05-28 | 戸田工業株式会社 | 非水電解質二次電池用Li−Ni複合酸化物粒子粉末及びその製造方法、並びに非水電解質二次電池 |
WO2010039732A2 (en) | 2008-09-30 | 2010-04-08 | Envia Systems, Inc. | Fluorine doped lithium rich metal oxide positive electrode battery materials with high specific capacity and corresponding batteries |
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JP5791877B2 (ja) * | 2009-09-30 | 2015-10-07 | 三洋電機株式会社 | 正極活物質、この正極活物質の製造方法、及び、正極活物質を用いた非水電解質二次電池 |
JP2011134670A (ja) * | 2009-12-25 | 2011-07-07 | Toyota Motor Corp | リチウム二次電池用正極活物質 |
JP5627142B2 (ja) * | 2010-02-24 | 2014-11-19 | エルジー ケム. エルティーディ. | 高容量の正極活物質およびこれを含むリチウム二次電池 |
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EP2680347B1 (en) | 2011-02-21 | 2015-09-16 | LG Chem, Ltd. | Positive electrode active material having improved output characteristics, and lithium secondary battery comprising same |
JP5516463B2 (ja) * | 2011-03-15 | 2014-06-11 | 株式会社豊田自動織機 | リチウムイオン二次電池用正極活物質の製造方法 |
JP2012234772A (ja) * | 2011-05-09 | 2012-11-29 | Mitsubishi Chemicals Corp | リチウム二次電池正極材料用リチウム遷移金属系化合物粉体及びその製造方法、並びにそれを用いたリチウム二次電池用正極及びリチウム二次電池 |
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US20160133931A1 (en) | 2016-05-12 |
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US10008720B2 (en) | 2018-06-26 |
CN105264695B (zh) | 2018-10-02 |
CN105264695A (zh) | 2016-01-20 |
KR20150015412A (ko) | 2015-02-10 |
KR101623719B1 (ko) | 2016-05-24 |
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