JP5295564B2 - 緻密な混合チタンリチウム酸化物の粉末状化合物、該化合物の製造方法および該化合物を含んでなる電極 - Google Patents
緻密な混合チタンリチウム酸化物の粉末状化合物、該化合物の製造方法および該化合物を含んでなる電極 Download PDFInfo
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Description
− 粉末状の混合されたチタンリチウム酸化物を合成する工程、
− 該酸化物を、遊星ミルで24時間〜48時間粉砕し、1μm以下の直径を有する微粒子と、該微粒子の凝集により形成され、100μm以下の直径を有する、少なくとも10体積%の粒状体とを形成する工程、
− 温度450℃〜600℃で熱処理する工程
を含んでなる方法により、達成される。
− 混合されたチタンリチウム酸化物の前駆物質を1〜2時間粉砕する工程、
− 900℃に達する温度で熱処理する工程
を含んでなる。
− Li4Ti5O12またはLi4Ti5O12の誘導体の単一微粒子(unitary particle)により形成された第一の粒度群、および
− 特定数の該単一微粒子が凝集して形成された粒状体により形成された第二の粒度群
からなる。
2.06Li2CO3+5TiO2→Li4Ti5O12+2.06CO2+0.06Li2O
− 第一温度増加を毎分2℃の処理速度で行い、500℃の第一の一定温度域に達した後、15時間保持し、
− 第二温度増加を毎分2℃の処理速度で行い、680℃の第二の一定温度域に達した後、15時間保持し、
− 第三温度増加を毎分2℃の処理速度で行い、900℃の最終的な一定温度域に達した後、5時間保持する。
− Nが小さい程、電流は強く、充電および放電サイクルが速いこと、
− 弱い条件、例えばC/10、では、バッテリーは公称容量160mAh/gに達すること、
− すべての電流条件(C/10〜20C)に対して、リチウムバッテリーの挙動は安定していること、
− 強い条件、例えば20C、でも、リチウム貯蔵バッテリーの容量は、なお約60mAh/g、すなわち弱い条件下で得られる公称容量の40%であること
が分かる。
Claims (14)
- ‐ 1μm以下の直径を有する凝集していないチタンリチウム酸化物の微粒子(1)からなる第一の群と、
‐ 1μm以下の直径を有する複数の前記チタンリチウム酸化物の微粒子(1)の凝集により形成され、かつそれぞれが100μm以下の直径を有する粒状体(2)からなる第二の群とからなる、混合されたチタンリチウム酸化物の粉末状化合物であって、前記第二の群が前記粉末状化合物の総体積に対して10〜50体積%含まれ、
前記混合されたチタンリチウム酸化物の粉末状化合物が1g/cm 3 以上の充填密度を有することを特徴とする、混合されたチタンリチウム酸化物の粉末状化合物。 - 凝集により形成される前記粒状体(2)の比率が、前記化合物の総体積に対して30〜50体積%である、請求項1に記載の化合物。
- 前記微粒子(1)の直径が0.1μm〜0.5μmである、請求項1または2に記載の化合物。
- 前記化合物の不純物の割合が、チタン1モルあたり1%以下である、請求項1〜3のいずれか一項に記載の化合物。
- 前記化合物の実験式がLi4Ti5O12およびその誘導体から選択される、請求項1〜4のいずれか一項に記載の化合物。
- 前記Li4Ti5O12の誘導体が、Li(4−x)MxTi5O12およびLi4Ti(5−y)NyO12から選択され、ここでxおよびyが、それぞれ0〜0.2であり、MおよびNが、それぞれNa、K、Mg、Nb、Al、Ni、Co、Zr、Cr、Mn、Fe、Cu、Zn、SiおよびMoから選択された化学元素である、請求項5に記載の化合物。
- 比表面積が5〜30m2/gである、請求項1〜6のいずれか一項に記載の化合物。
- 請求項1〜7のいずれか一項に記載の混合されたチタンリチウム酸化物の粉末状化合物を製造する方法であって、少なくとも下記の連続的な工程、すなわち
− 粉末状の混合されたチタンリチウム酸化物を合成する工程、
− 前記酸化物を、遊星ミルで24時間〜48時間粉砕し、1μm以下の直径を有する微粒子(1)と、前記微粒子(1)の凝集により形成され、かつ100μm以下の直径を有する、少なくとも10体積%の粒状体(2)とを形成する工程、および
− 温度450℃〜600℃で熱処理する工程
を含んでなる、方法。 - 前記酸化物を粉砕する工程が、混合されたチタンリチウム酸化物の総体積に対して5体積%未満の有機溶剤と共に行われる、請求項8に記載の方法。
- 前記混合されたチタンリチウム酸化物の合成工程が、少なくとも
− 前記混合されたチタンリチウム酸化物の前駆物質を1〜2時間粉砕する工程、
− 900℃に達する温度で熱処理する工程
を含んでなる、請求項8または9に記載の方法。 - 前記混合されたチタンリチウム酸化物の前駆物質がTiO2およびLi2CO3である、請求項10に記載の方法。
- 前記粉砕工程の際に、Na、K、Mg、Nb、Al、Ni、Co、Zr、Cr、Mn、Fe、Cu、Zn、SiおよびMoから選択された化学元素の前駆物質が、混合されたチタンリチウム酸化物の前駆物質に加えられる、請求項10または11に記載の方法。
- 請求項1〜7のいずれか一項に記載の混合されたチタンリチウム酸化物の粉末状化合物を少なくとも含んでなる、電気化学的エネルギー貯蔵装置用の電極。
- 前記粉末状化合物の、少なくとも一種の導電性添加剤および/または重合体結合剤とのナノ−分散物からなる、請求項13に記載の電極。
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FR0409207 | 2004-08-31 | ||
FR0409207A FR2874603B1 (fr) | 2004-08-31 | 2004-08-31 | Compose pulverulent d'oxyde mixte de titane et de lithium dense, procede de fabrication d'un tel compose et electrode comportant un tel compose |
PCT/FR2005/002052 WO2006027449A2 (fr) | 2004-08-31 | 2005-08-08 | Compose pulverulent d'oxyde mixte de titane et de lithium dense, procede de fabrication d'un tel compose et electrode comportant un tel compose |
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US (1) | US7682596B2 (ja) |
EP (1) | EP1784358B1 (ja) |
JP (2) | JP5295564B2 (ja) |
KR (1) | KR101245418B1 (ja) |
CN (1) | CN101035743B (ja) |
AT (1) | ATE496870T1 (ja) |
DE (1) | DE602005026133D1 (ja) |
ES (1) | ES2356923T3 (ja) |
FR (1) | FR2874603B1 (ja) |
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JP4957911B2 (ja) * | 2005-03-30 | 2012-06-20 | 株式会社Gsユアサ | Al含有チタン酸リチウムからなるリチウムイオン電池用活物質及びリチウムイオン電池 |
JP4957912B2 (ja) * | 2005-03-30 | 2012-06-20 | 株式会社Gsユアサ | Mg含有チタン酸リチウムからなるリチウムイオン電池用活物質及びリチウムイオン電池 |
JP4580949B2 (ja) * | 2006-06-02 | 2010-11-17 | 株式会社東芝 | 非水電解質電池、電池パック及び充電式掃除機 |
DE102008026580A1 (de) * | 2008-06-03 | 2009-12-10 | Süd-Chemie AG | Verfahren zur Herstellung von Lithiumtitan-Spinell und dessen Verwendung |
KR101122135B1 (ko) * | 2009-06-19 | 2012-03-15 | 주식회사 이아이지 | 리튬 티탄 복합산화물을 포함하는 리튬이차전지 음극, 이를 이용한 리튬이차전지, 전지팩 및 자동차 |
CN101944609A (zh) * | 2009-07-07 | 2011-01-12 | 清华大学深圳研究生院 | 锌掺杂的钛酸锂材料及其制备方法 |
FR2948232B1 (fr) | 2009-07-16 | 2011-08-26 | Commissariat Energie Atomique | Electrolyte liquide pour accumulateur au lithium, comprenant un melange de solvants organiques non aqueux |
WO2011024353A1 (ja) * | 2009-08-31 | 2011-03-03 | 株式会社村田製作所 | 電極活物質およびその製造方法、ならびにそれを備えた非水電解質二次電池 |
DE102009049470A1 (de) * | 2009-10-15 | 2011-04-28 | Süd-Chemie AG | Verfahren zur Herstellung von feinteiligen Lithiumtitan-Spinellen und deren Verwendung |
JP4920803B2 (ja) * | 2010-03-29 | 2012-04-18 | パナソニック株式会社 | 非水電解質二次電池用負極、およびその製造方法、ならびに非水電解質二次電池 |
KR101286761B1 (ko) * | 2010-06-01 | 2013-07-16 | 주식회사 엘앤에프신소재 | 전이금속 화합물 전구체, 이를 이용한 리튬 전이금속 화합물, 상기 리튬 전이금속 화합물을 포함하는 양극 활물질 및 상기 양극 활물질을 포함하는 리튬 이온 이차전지 |
JP5674357B2 (ja) * | 2010-07-01 | 2015-02-25 | エナックス株式会社 | リチウムイオン二次電池 |
JP5230713B2 (ja) | 2010-10-29 | 2013-07-10 | 株式会社東芝 | 電池用活物質、非水電解質電池及び電池パック |
KR101312271B1 (ko) * | 2011-03-25 | 2013-09-25 | 삼성에스디아이 주식회사 | 티탄산리튬, 티탄산리튬을 포함하는 음극 및 이를 포함하는 리튬 이차 전지 |
JP5569980B2 (ja) * | 2011-12-26 | 2014-08-13 | 太陽誘電株式会社 | リチウムチタン複合酸化物、それを用いた電池用電極およびリチウムイオン二次電池 |
JP2015046218A (ja) * | 2011-12-28 | 2015-03-12 | パナソニック株式会社 | 非水電解質二次電池用電極およびそれを用いた非水電解質二次電池 |
CN104170149B (zh) * | 2012-04-17 | 2017-07-18 | 株式会社Lg 化学 | 具有优异性能的锂二次电池 |
KR101542050B1 (ko) * | 2012-04-17 | 2015-08-06 | 주식회사 엘지화학 | 낮은 함습성의 전극 활물질 및 이를 포함하는 리튬 이차전지 |
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KR101796233B1 (ko) * | 2013-05-23 | 2017-12-01 | 주식회사 포스코 | 이종 금속이 도핑된 리튬 티탄 복합 산화물의 제조 방법, 및 이에 의하여 제조된 이종 금속이 도핑된 리튬 티탄 복합 산화물 |
JP6415902B2 (ja) * | 2014-08-28 | 2018-10-31 | 株式会社吉野工業所 | プリフォーム及びボトルの製造方法 |
KR101766870B1 (ko) * | 2014-10-31 | 2017-08-09 | 주식회사 엘지화학 | 리튬 이차전지용 음극활물질, 이를 포함한 음극 및 리튬 이차전지 |
KR101847769B1 (ko) * | 2016-02-05 | 2018-04-10 | 주식회사 엘지화학 | 음극 활물질, 이를 포함하는 음극 및 리튬 이차전지 |
WO2017135758A1 (ko) * | 2016-02-05 | 2017-08-10 | 주식회사 엘지화학 | 음극 활물질, 이를 포함하는 음극 및 리튬 이차전지 |
CN105914357B (zh) * | 2016-06-22 | 2018-05-15 | 河北师范大学 | 一种含铁和钾的锂离子电池钛酸锂负极材料的制备方法 |
CN109565044B (zh) * | 2017-03-21 | 2022-07-12 | 株式会社Lg新能源 | 具有高输出特性的负极活性材料和包含其的锂二次电池 |
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JP3625680B2 (ja) * | 1999-03-25 | 2005-03-02 | 三洋電機株式会社 | リチウム二次電池 |
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JP4623786B2 (ja) * | 1999-11-10 | 2011-02-02 | 住友電気工業株式会社 | 非水二次電池 |
JP4763884B2 (ja) * | 2000-09-21 | 2011-08-31 | 東芝電池株式会社 | 非水電解質二次電池 |
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JP2002175805A (ja) * | 2000-12-06 | 2002-06-21 | Chuo Denki Kogyo Co Ltd | 電池用活物質とその製造方法および電池 |
US7211350B2 (en) * | 2001-01-29 | 2007-05-01 | Rutgers University Foundation | Nanostructure lithium titanate electrode for high cycle rate rechargeable electrochemical cell |
JP4949561B2 (ja) * | 2001-03-27 | 2012-06-13 | 東邦チタニウム株式会社 | リチウムイオン二次電池電極活物質製造原料としての二酸化チタン粉、リチウムイオン二次電池電極活物質としてのチタン酸リチウムおよびその製造方法 |
ATE285379T1 (de) * | 2001-07-20 | 2005-01-15 | Altair Nanomaterials Inc | Verfahren zur herstellung von lithiumtitanat |
JP4153192B2 (ja) * | 2001-10-31 | 2008-09-17 | チタン工業株式会社 | 電極用チタン酸リチウム及びその用途 |
JP2003203632A (ja) * | 2002-01-09 | 2003-07-18 | Hitachi Ltd | リチウム二次電池用正極活物質とその製造法及びそれを用いたリチウム二次電池並びに組電池モジュール |
US7316862B2 (en) * | 2002-11-21 | 2008-01-08 | Hitachi Maxell, Ltd. | Active material for electrode and non-aqueous secondary battery using the same |
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KR101245418B1 (ko) | 2013-03-19 |
FR2874603A1 (fr) | 2006-03-03 |
CN101035743A (zh) | 2007-09-12 |
JP2013144639A (ja) | 2013-07-25 |
KR20070047810A (ko) | 2007-05-07 |
WO2006027449A3 (fr) | 2006-06-01 |
FR2874603B1 (fr) | 2006-11-17 |
EP1784358B1 (fr) | 2011-01-26 |
US7682596B2 (en) | 2010-03-23 |
PL1784358T3 (pl) | 2011-06-30 |
ATE496870T1 (de) | 2011-02-15 |
US20080031798A1 (en) | 2008-02-07 |
DE602005026133D1 (de) | 2011-03-10 |
ES2356923T3 (es) | 2011-04-14 |
EP1784358A2 (fr) | 2007-05-16 |
JP2008511528A (ja) | 2008-04-17 |
WO2006027449A2 (fr) | 2006-03-16 |
CN101035743B (zh) | 2012-07-18 |
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