JP2020526894A - ニッケル酸リチウム複合酸化物の正極活物質粒子粉末及び非水電解質二次電池 - Google Patents
ニッケル酸リチウム複合酸化物の正極活物質粒子粉末及び非水電解質二次電池 Download PDFInfo
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Abstract
【解決手段】 層状構造のニッケル酸リチウム複合酸化物Li1+aNi1−b−cCobMcO2(Mは元素Mn、Al、B、Mg、Ti、Sn、Zn、Zrのうち少なくとも1種、−0.1≦a≦0.2、0.05≦b≦0.5、0.01≦c≦0.4)を芯粒子Xとし、元素Al、Mg、Zr、Ti、Siのうち少なくとも1種含む被覆化合物Yを有した正極活物質粒子粉末であって、前記被覆化合物Yの平均膜厚が0.2〜5nm、結晶化度が50〜95%、エピタキシャル成長度が50〜95%、被覆率が50〜95%であることを特徴とする正極活物質粒子粉末。
【選択図】なし
Description
本発明に係るニッケル酸リチウム複合酸化物の正極活物質粒子粉末は、気相成長法とその後の熱処理で形成されたエピタキシャル成長性の被覆化合物Yを有している。該被覆化合物Yは非常に薄く、高結晶化度、高エピタキシャル成長度、及び高被覆率を備えるため、二次電池の充放電の繰り返し時の際に、高い容量を示しつつ、生じる副反応を抑制する。結果として、高エネルギー密度で充放電繰り返し特性に優れた正極活物質粒子粉末、及び二次電池として好適である。
前駆体であるコバルト含有水酸化ニッケルNi0.84Co0.16(OH)2は水溶媒中のアンモニア錯体を経由した晶析法で数日間かけて得られた。該水酸化物と水酸化リチウム・一水塩LiOH・H2Oと水酸化アルミニウムAl(OH)3を、モル比でLi:Ni:Co:Al=1.02:0.81:0.15:0.04になるよう所定量を計量後、ハイスピードミキサーで混合し、ローラーハースキルンにおいて酸素雰囲気下770℃で芯粒子Xとなり得るニッケル酸リチウム複合酸化物を得た。
K.Tsutsumi等、 JEOL News、Vol.49、2014年、59−72頁
実施例1で得られた芯粒子Xとなり得る層状構造のニッケル酸リチウム複合酸化物Li1.02Ni0.81Co0.15Al0.04O2を用い、原子層堆積法で被覆化合物Yを形成させた。同法での処理条件は実施例1と同様で、用いた原料ガスAはトリメチルアルミニウムAl(CH3)3、原料ガスBはH2Oであり、180℃で4サイクルの処理であった。その後、大気中350℃−2時間で被覆化合物Yの結晶化度を高めた。得られた粒子粉末はエピタキシャル成長度の高い被覆化合物Yを有するニッケル酸リチウム複合酸化物粒子粉末であった。得られた酸化物粒子粉末を正極活物質粒子粉末として、以下、評価した。
実施例1で得られた芯粒子Xとなり得る層状構造のニッケル酸リチウム複合酸化物Li1.02Ni0.81Co0.15Al0.04O2を、表面処理することなく正極活物質粒子粉末として用いた。表3に示すように、得られた粉体特性において、LiOH含有量は0.5を超えており、Li2CO3/LiOHの強度比は0.9未満であり、電極スラリーのゲル化が起こりやすい特性であった。STEM観察で前記活物質粒子表面の10粒子をランダムに選び、EDS分析したところ、過剰なAlの存在は確認できなかった。従って被覆化合物Yの被覆率は0%であった。また、電池特性では初期放電容量は高いものの、140サイクルの放電容量維持率が90%未満であり141サイクルの放電容量維持率は85%未満であり、特性は低かった。
実施例1の途中の製造工程から抜き取った試料、即ち、原子層堆積法での処理後の試料を正極活物質として用いた。STEM観察で前記活物質粒子表面の10粒子をランダムに選び、EDS分析したところ、過剰なAlの存在は高い頻度で確認できた。表3に粉体特性及び電池特性を示すように、高い水酸化リチウムの含有量を示し、2%粉体pHも高く、二次電池のサイクル特性は低かった。
実施例1に用いた芯粒子Xとなり得るニッケル酸リチウム複合酸化物を、空気:CO2=3:1(体積比)の混合ガス条件下、250℃−2時間処理した。原子層堆積法での処理は行わなかった。残存するLiOH量は0.5未満と低いものの、二次電池のサイクル特性は良好であるとは言い難いものであった。
Claims (5)
- 層状構造のニッケル酸リチウム複合酸化物Li1+aNi1−b−cCobMcO2(Mは元素Mn、Al、B、Mg、Ti、Sn、Zn、Zrのうち少なくとも1種、−0.1≦a≦0.2、0.05≦b≦0.5、0.01≦c≦0.4)を芯粒子Xとし、元素Al、Mg、Zr、Ti、Siのうち少なくとも1種含む被覆化合物Yを有した正極活物質粒子粉末であって、前記被覆化合物Yの平均膜厚が0.2〜5nm、結晶化度が50〜95%、エピタキシャル成長度が50〜95%、被覆率が50〜95%であることを特徴とする正極活物質粒子粉末。
- 請求項1記載の正極活物質粒子粉末であって、前記被覆化合物Yにおける元素Niに対する被覆化合物Yに含まれる元素Al、Mg、Zr、Ti、Siの総原子数比の平均値が0.5以上である正極活物質粒子粉末。
- 請求項1記載の正極活物質粒子粉末であって、水酸化リチウムLiOHの含有量が0.50重量%以下、炭酸リチウムLi2CO3の含有量が0.65重量%以下、水酸化リチウム含有量に対する炭酸リチウム含有量の重量比が0.9以上である正極活物質粒子粉末。
- 請求項1記載の正極活物質粒子粉末であって、BET比表面積が0.05〜0.70m2/g、凝集粒子メジアン径D50が1〜30μm、2%粉体pHが11.6以下である正極活物質粒子粉末。
- 請求項1記載の正極活物質粒子粉末を、正極活物質の少なくとも一部に用いた非水電解質二次電池。
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HUE064649T2 (hu) * | 2019-12-03 | 2024-04-28 | Lg Energy Solution Ltd | Eljárás pozitív elektróda aktív anyag elõállítására lítium szekunder akkumulátorhoz, és az azzal elõállított pozitív elektróda aktív anyag |
US20210336240A1 (en) * | 2020-04-22 | 2021-10-28 | Uchicago Argonne, Llc | Modification of lithium ion electrode materials via atomic layer deposition techniques |
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US10615414B2 (en) * | 2016-01-15 | 2020-04-07 | Toda Kogyo Corp. | Lithium nickelate-based positive electrode active substance particles and process for producing the same, and non-aqueous electrolyte secondary battery |
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US20160351910A1 (en) * | 2015-06-01 | 2016-12-01 | Energy Power Systems Llc. | Nano-engineered coatings for anode active materials, cathode active materials, and solid-state electrolytes and methods of making batteries containing nano-engineered coatings |
WO2017025957A1 (en) * | 2015-08-11 | 2017-02-16 | Technion Research & Development Foundation Limited | Metal fluoride coated lithium intercalation material and methods of making same and uses thereof |
JP2018206747A (ja) * | 2016-07-05 | 2018-12-27 | 株式会社半導体エネルギー研究所 | 正極活物質、正極活物質の作製方法、および二次電池 |
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WO2022259755A1 (ja) * | 2021-06-10 | 2022-12-15 | 三井金属鉱業株式会社 | 活物質及びその製造方法 |
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EP3652113B1 (en) | 2023-09-20 |
EP3652113A1 (en) | 2020-05-20 |
US20200119342A1 (en) | 2020-04-16 |
ES2961786T3 (es) | 2024-03-13 |
CN110785380A (zh) | 2020-02-11 |
KR102515290B1 (ko) | 2023-03-29 |
JP7148874B2 (ja) | 2022-10-06 |
US20200185708A1 (en) | 2020-06-11 |
WO2019012497A1 (en) | 2019-01-17 |
KR20200029397A (ko) | 2020-03-18 |
PL3652113T3 (pl) | 2024-03-18 |
HUE064235T2 (hu) | 2024-02-28 |
CN110785380B (zh) | 2022-12-13 |
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