JP6490101B2 - チタン酸リチウム粒子と炭素質物質の複合体の製造方法 - Google Patents
チタン酸リチウム粒子と炭素質物質の複合体の製造方法 Download PDFInfo
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Description
本発明の好ましい実施形態におけるチタン酸リチウム粒子と炭素質物質の複合体は、チタン酸リチウム粒子の表面の一部又は全部が炭素質物質で被覆されていることを特徴とする。
本発明の原料混合物は、リチウム化合物、並びにアルカリ可溶性樹脂のオリゴマー及び/又は原料モノマーを用いて製造された炭素質物質の前駆体により、表面の一部又は全部が被覆されたチタン化合物である。本発明の原料混合物を準備する工程は、例えば、溶媒、チタン化合物、リチウム化合物及びアルカリ可溶性樹脂のオリゴマーを混合し、得られた混合物を乾燥することで得る方法;溶媒、チタン化合物、リチウム化合物及びアルカリ可溶性樹脂の原料モノマーを混合し、得られた混合物を乾燥する方法がある。これらの中でも、チタン化合物の分散性の観点から、溶媒、チタン化合物、リチウム化合物及びアルカリ可溶性樹脂の原料モノマーを混合し、得られた混合物を乾燥する方法が好ましい。
加熱処理の雰囲気としては非酸化性雰囲気下であれば特に制限はなく、好ましくは窒素、アルゴン等の不活性ガス雰囲気下、又は不活性ガス中に微量の酸素が存在するような実質的に不活性な雰囲気下で行うことができる。
本発明の複合体は、優れた電気的特性を有していることから、カーボンブラック等の導電剤、フッ素樹脂等のバインダー等とともに混練、成形することで、電気化学デバイスの電極として好適に使用することができる。前述の電極を用いることができる電気化学デバイスとしては、例えば電気二重層キャパシタ、リチウムイオンキャパシタ、リチウムイオン電池等が挙げられる。
フェノール類化合物としてレゾルシノール(0.4mol)、アルデヒド類化合物として37質量%ホルムアルデヒド水溶液(0.7mol)及び溶媒として水(8.9mol)をビーカーに加え5分間混合した。
フェノール類化合物をフェノール(0.4mol)、アルデヒド類化合物を37質量%ホルムアルデヒド水溶液(0.9mol)に変更した以外は実施例1と同様の方法でチタン酸リチウム粒子と炭素質物質の複合体を得た。
フェノール類化合物をm−クレゾール(0.4mol)に変更した以外は実施例1と同様の方法でチタン酸リチウム粒子と炭素質物質の複合体を得た。
アルデヒド類化合物をヘキサメチレンテトラミン(0.04mol)に変更した以外は実施例1と同様の方法でチタン酸リチウム粒子と炭素質物質の複合体を得た。
チタン化合物を含水水酸化チタン粒子(1.8mol、平均一次粒子径10nm)に変更した以外は実施例1と同様の方法でチタン酸リチウム粒子と炭素質物質の複合体を得た。
チタン化合物をアナターゼ型酸化チタン(IV)粒子(1.8mol、平均一次粒子径150nm)に変更した以外は実施例1と同様の方法でチタン酸リチウム粒子と炭素質物質の複合体を得た。図3に得られた複合体のSEM写真を示す。写真の倍率は10万倍である。
リチウム化合物を水酸化リチウム(0.5mol)に変更した以外は実施例1と同様の方法でチタン酸リチウム粒子と炭素質物質の複合体を得た。
リチウム化合物として酢酸リチウム(1.5mol)及び溶媒として水(8.9mol)をビーカーに加えて混合し、酢酸リチウムが完全に溶解するまで10分間混合した。
実施例1の複合体と、結着剤としてSBRゴム(BM400B、日本ゼオン社製)とを、複合体とSBRゴムの質量比が97.5:2.5となるように微量の水と共に乳鉢で混合してスラリー状にして電極組成物を調製した。この電極組成物をアルミニウム集電体上に塗布、乾燥することで電極を得た。
上記で得られた半電池の初期放電容量と放電容量維持率を評価し、結果を表1に示した。初期放電容量と放電容量維持率は以下のように行った。
25℃にて電池評価を行った。対極(リチウム電極)に対して10Cに相当する電流で1.0Vまで充電した。放電はリチウム極に対して10Cに相当する電流で2.5Vまで行い初期放電容量を測定した。容量は、用いたチタン酸リチウムの重量当たりに換算した。
リチウム電極に対して100Cに相当する電流で1.0Vまで充電し、放電をリチウム電極に対して100Cに相当する電流で2.5Vまで行い初期放電容量を測定した。以下の式に示すように、100Cにおける放電容量の10Cにおける放電容量に対する比として放電容量維持率を算出し、レート特性を評価した。
Claims (3)
- チタン酸リチウム粒子と炭素質物質の複合体を製造する方法であって、
チタン化合物、リチウム化合物、並びにアルカリ可溶性樹脂のオリゴマー及び/又は原料モノマーを含む原料混合物を準備する工程と、
前記原料混合物を非酸化性雰囲気下で加熱処理して、前記複合体を製造する工程と
を備え、
前記チタン化合物の平均一次粒子径が、1〜99nmであり、前記アルカリ可溶性樹脂のオリゴマー及び/又は原料モノマーに、ホルムアルデヒド、アセトアルデヒド、ブチルアルデヒド、サリチルアルデヒド、ベンズアルデヒド、パラホルムアルデヒド、トリオキサン、及びヘキサメチレンテトラミンから選ばれる少なくとも1種が含まれることを特徴とするチタン酸リチウム粒子と炭素質物質の複合体の製造方法。 - 前記アルカリ可溶性樹脂が、主鎖又は側鎖に水酸基、フェノール性水酸基及び/又はカルボキシル基を有していることを特徴とする請求項1に記載のチタン酸リチウム粒子と炭素質物質の複合体の製造方法。
- 前記加熱処理の温度が、800〜1000℃であることを特徴とする請求項1又は2に記載のチタン酸リチウム粒子と炭素質物質の複合体の製造方法。
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JP2014253676 | 2014-12-16 | ||
JP2014253676 | 2014-12-16 | ||
PCT/JP2015/084015 WO2016098608A1 (ja) | 2014-12-16 | 2015-12-03 | チタン酸リチウム粒子と炭素質物質の複合体の製造方法及びチタン酸リチウム粒子と炭素質物質の複合体 |
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JPWO2016098608A1 JPWO2016098608A1 (ja) | 2017-09-28 |
JP6490101B2 true JP6490101B2 (ja) | 2019-03-27 |
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US (1) | US10665360B2 (ja) |
EP (1) | EP3236522A4 (ja) |
JP (1) | JP6490101B2 (ja) |
KR (1) | KR102003140B1 (ja) |
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US2909505A (en) * | 1954-06-14 | 1959-10-20 | Johnson & Son Inc S C | Alkali soluble resins and compositions containing the same |
EP2181964B1 (en) * | 2007-08-30 | 2014-05-14 | Ishihara Sangyo Kaisha, Ltd. | Titanic acid compound, process for producing the titanic acid compound, electrode active material containing the titanic acid compound, and storage device using the electrode active material |
DE102008050692B4 (de) | 2008-10-07 | 2014-04-03 | Süd-Chemie Ip Gmbh & Co. Kg | Kohlenstoffbeschichteter Lithiumtitan-Spinell |
WO2010052950A1 (ja) | 2008-11-04 | 2010-05-14 | 国立大学法人岩手大学 | 不定比チタン化合物、その炭素複合体、それら化合物の製造方法、及びそれら化合物を含むリチウムイオン二次電池用負極活物質、並びにそれを用いたリチウムイオン二次電池 |
CN102201570B (zh) | 2010-03-25 | 2013-11-06 | 清华大学 | 锂电池电极材料的制备方法 |
JP5450284B2 (ja) | 2010-06-28 | 2014-03-26 | 株式会社日立製作所 | チタン酸リチウム粒子およびその製造方法、リチウムイオン電池用負極、ならびにリチウム電池 |
KR20140050016A (ko) | 2011-06-30 | 2014-04-28 | 코넬 유니버시티 | 하이브리드 물질 및 나노복합체 물질, 이들의 제조 방법, 및 이들의 사용 |
US10950849B2 (en) | 2011-06-30 | 2021-03-16 | Cornell University | Hybrid materials and nanocomposite materials, methods of making same, and uses thereof |
KR101451899B1 (ko) * | 2012-10-05 | 2014-10-21 | 동국대학교 산학협력단 | 리튬이차전지의 스피넬 리튬 티타늄 옥사이드 나노섬유 음극활물질의 제조방법 |
CN103456939B (zh) | 2013-07-24 | 2015-12-23 | 湖南大学 | 利用偏钛酸制备锂离子电池负极材料碳包覆钛酸锂的方法 |
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WO2016098608A1 (ja) | 2016-06-23 |
KR20170097648A (ko) | 2017-08-28 |
CA2969306C (en) | 2020-01-07 |
TWI645606B (zh) | 2018-12-21 |
US20170346131A1 (en) | 2017-11-30 |
US10665360B2 (en) | 2020-05-26 |
KR102003140B1 (ko) | 2019-07-23 |
JPWO2016098608A1 (ja) | 2017-09-28 |
EP3236522A1 (en) | 2017-10-25 |
TW201630234A (zh) | 2016-08-16 |
CA2969306A1 (en) | 2016-06-23 |
EP3236522A4 (en) | 2018-08-29 |
CN107004848A (zh) | 2017-08-01 |
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