JP2015532632A - リチウムリン酸鉄ナノ粉末の製造方法 - Google Patents
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Abstract
Description
本発明では、液相法のうち一つのグリコサーマル方法を利用したリチウムリン酸鉄ナノ粉末の製造方法を提供し、具体的には反応溶媒としてグリセロール(glycerol)を用いることにより、従来の水熱合成法及び超臨界水法と比べる時、相対的な低圧条件で反応を進めさせることができ、また従来のグリコサーマル方法と比べて粒子の大きさ及び粒度分布が効果的に制御されたリチウムリン酸鉄ナノ粉末を製造することができるようになる。
併せて、本発明では前記オリビン結晶構造のリチウムリン酸鉄ナノ粉末を含む正極活物質を提供することができる。前記正極活物質には、前記リチウムリン酸鉄粉末以外にも選択的に導電剤、バインダー及び充填剤などをさらに含んで構成されることがある。
リチウムヒドロキシドハイドレート(LiOH・H2O)0.42g、クエン酸第二鉄水和物(FeC6H5O7・nH2O)2.45g及びリン酸(H3PO4)0.98gをグリセロール50mlに入れて充分に撹拌させて混合溶液を製造した。
Claims (20)
- (a)グリセロール(glycerol)溶媒にリチウム前駆体、鉄前駆体及びリン前駆体を入れて混合溶液を製造する段階;及び
(b)前記混合溶液を反応器に投入して加熱し、10から100barの圧力条件下でリチウムリン酸鉄ナノ粉末を合成する段階;を含むリチウムリン酸鉄ナノ粉末の製造方法。 - (c)前記合成されたリチウムリン酸鉄ナノ粉末を熱処理し、前記ナノ粉末の個別粒子表面の一部または全体にコーティング層を形成する段階;をさらに含む請求項1に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記(b)段階で合成されたリチウムリン酸鉄ナノ粉末は、洗浄段階及び乾燥段階を順次に経る請求項1または請求項2に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記(b)段階は、グリセロール(glycerol)の沸点以下の温度で進められる請求項1から請求項3のいずれか一項に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記(b)段階は、150〜290℃の温度範囲内で進められる請求項1から請求項4のいずれか一項に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記(b)段階は、1〜48時間の間進められる請求項1から請求項5のいずれか一項に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リチウム前駆体は、リチウムアセテートジハイドレート(CH3COOLi・2H2O)、リチウムヒドロキシドモノハイドレート(LiOH・H2O)、リチウムヒドロキシド(LiOH)、リチウムカーボネート(Li2CO3)、リチウムホスフェート(Li3PO4)、リチウムホスフェートドデカハイドレート(Li3PO4・12H2O)及びリチウムオキサレート(Li2C2O4)からなる群から選ばれた1または2以上の混合物である請求項1から請求項6のいずれか一項に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記鉄前駆体は、クエン酸第2鉄(FeC6H5O7)、クエン酸第2鉄水和物(FeC6H5O7・nH2O)、硫酸第1鉄7水和物(FeSO4・7H2O)、シュウ酸鉄2水和物(FeC2O4・2H2O)、鉄アセチルアセトネート(Fe(C5H7O2)3)、リン酸第2鉄2水和物(FePO4・2H2O)及び水酸化第2鉄(FeO(OH))からなる群から選ばれた1または2以上の混合物である請求項1から請求項7のいずれか一項に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記リン前駆体は、トリ−アンモニウムホスフェートトリハイドレート((NH4)3PO4・3H2O)、アンモニウムホスフェート((NH4)2HPO4)、アンモニウムジヒドロゲンホスフェート(NH4H2PO4)、及びリン酸(H3PO4)からなる群から選ばれた1または2以上の混合物である請求項1から請求項8のいずれか一項に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記熱処理は、400〜900℃の温度範囲で加熱して進められることである請求項2に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 前記乾燥段階は、20〜160℃の温度で2〜40時間の間乾燥する請求項3に記載のリチウムリン酸鉄ナノ粉末の製造方法。
- 請求項1から請求項11のいずれか一項に記載のリチウムリン酸鉄ナノ粉末の製造方法によって製造されたリチウムリン酸鉄ナノ粉末は、オリビン結晶構造を有する粒子を含むリチウムリン酸鉄ナノ粉末。
- 前記リチウムリン酸鉄ナノ粉末の粒径は、30〜300nmである請求項12に記載のリチウムリン酸鉄ナノ粉末。
- 前記リチウムリン酸鉄ナノ粉末の粒度分布は、粒径平均値の50%以下である請求項12または請求項13に記載のリチウムリン酸鉄ナノ粉末。
- 前記リチウムリン酸鉄ナノ粉末の粒子は、表面に炭素コーティング層またはガラス質リチウム化合物コーティング層をさらに含む請求項12から請求項14のいずれか一項に記載のリチウムリン酸鉄ナノ粉末。
- 前記炭素コーティング層または前記ガラス質リチウム化合物コーティング層の厚さは10nm以下である請求項15に記載のリチウムリン酸鉄ナノ粉末。
- 請求項12から請求項15のいずれか1項に記載のリチウムリン酸鉄ナノ粉末を含む正極活物質。
- 請求項17に記載の正極活物質は、導電剤、バインダー及び充填剤をさらに含む正極活物質。
- 請求項17または請求項18に記載の正極活物質を含むリチウム二次電池用正極。
- 請求項19に記載の正極と負極、分離膜及びリチウム塩含有非水電解液を含むリチウム二次電池。
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KR1020140002569A KR101561374B1 (ko) | 2013-01-10 | 2014-01-08 | 리튬 인산철 나노분말 제조방법 |
KR10-2014-0002569 | 2014-01-08 | ||
PCT/KR2014/000267 WO2014109576A1 (ko) | 2013-01-10 | 2014-01-09 | 리튬 인산철 나노분말 제조방법 |
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Cited By (4)
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JP2015530344A (ja) * | 2013-01-10 | 2015-10-15 | エルジー・ケム・リミテッド | 炭素コーティングリチウムリン酸鉄ナノ粉末の製造方法 |
JP2016531069A (ja) * | 2013-08-15 | 2016-10-06 | 江蘇華東▲リ▼電技術研究院有限公司Jiangsu Huadong Institute Of Li−Ion Battery Co.Ltd. | リン酸鉄リチウムの製造方法 |
US9543582B2 (en) | 2013-01-10 | 2017-01-10 | Lg Chem, Ltd. | Method for preparing lithium iron phosphate nanopowder |
US9627685B2 (en) | 2013-01-10 | 2017-04-18 | Lg Chem, Ltd. | Method for preparing lithium iron phosphate nanopowder |
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