JP6224125B2 - 低いタップ密度を有する遷移金属前駆体及び高い粒子強度を有するリチウム遷移金属酸化物 - Google Patents
低いタップ密度を有する遷移金属前駆体及び高い粒子強度を有するリチウム遷移金属酸化物 Download PDFInfo
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Description
前駆体の平均粒径(D50)と前駆体のタップ密度(tap density)との比が下記式1の条件を満足することを特徴とする遷移金属前駆体を提供する。
0<a≦1.2、0≦x≦0.9、0≦y≦0.9、0≦z≦0.9、0≦w≦0.3、2≦a+x+y+z+w≦2.3、0≦t<0.2、
Mは、Al、Cu、Fe、Mg、B、Cr及び第2の周期の遷移金属からなる群から選択される1つ以上の金属カチオンであり、
Aは、−1または−2価の1つ以上のアニオンである。
ニッケル硫酸塩、コバルト硫酸塩及びマンガン硫酸塩をモル比で0.45:0.15:0.40の割合で混合して1.5M濃度の遷移金属水溶液を準備し、3M水酸化ナトリウム水溶液を準備した。
反応中、添加物として30%濃度のアンモニア溶液を湿式反応器に1/10〜1/5の流量を連続的に供給したこと以外は、実施例1と同様の方法で遷移金属前駆体を製造した。
反応中、攪拌機の1分当りの回転数を600〜800rpmに維持したこと以外は、実施例1と同様の方法で遷移金属前駆体を製造した。
ニッケル硫酸塩、コバルト硫酸塩、及びマンガン硫酸塩をモル比で0.45:0.15:0.40の割合で混合して1.5M濃度の遷移金属水溶液を準備し、3M水酸化ナトリウム水溶液を準備した。
反応中、添加物としてアンモニア溶液を連続的に供給しなかったこと以外は、比較例1と同様の方法で遷移金属前駆体を製造した。
実施例1〜3及び比較例1、2でそれぞれ製造された遷移金属前駆体を、SEISHIN(KYT−4000)測定機器を用いて100ccのタッピング用シリンダーに50gを入れた後、3000回タッピングを加えた。また、Microtrac(S−3500)を用いて体積基準の粉体分布度を得、D50値を測定し、D50に対するTap密度を計算した。その結果を下記表1に示す。
実施例1〜3及び比較例1、2でそれぞれ製造された遷移金属前駆体をLi/(Ni+Co+Mn)の割合が1.10モル比となるようにLi2CO3を混合した後に、5℃/分の昇温速度で加熱して、950℃で10時間焼成させることで、リチウム遷移金属酸化物粉末(正極活物質)を製造した。
実施例1〜3及び比較例1、2でそれぞれ製造された遷移金属前駆体を用いた正極活物質粉末をPDM−300 paste mixerにそれぞれ10g入れ、5mmのアルミナビーズを入れた後、公転×自転回転数(rpm)基準600×600の条件で活物質をボールミル粉砕過程を経た。このように製造された活物質粉砕品を、Microtrac(S−3500)を用いて60秒の超音波分散過程を経た後、再び体積基準の粉体分布に該当するD50値を測定した。
Claims (7)
- 遷移金属前駆体を提供するステップであって、前記遷移金属前駆体の平均粒径(D50)と前記遷移金属前駆体のタップ密度との比が下記式1の条件を満足し、前記遷移金属前駆体が下記式2で表される遷移金属水酸化物粒子である、遷移金属前駆体を提供するステップと、
前記遷移金属前駆体とリチウム前駆体を混合し、焼結してリチウム遷移金属酸化物を提供するステップであって、前記リチウム遷移金属酸化物の平均粒径(D50)と、前記リチウム遷移金属酸化物の製造のための前記遷移金属前駆体の平均粒径(D50)との比が、下記式3を満足する、リチウム遷移金属酸化物を提供するステップと、
を含む、リチウム遷移金属酸化物の製造方法であって、
前記リチウム遷移金属酸化物が、下記式4で表される化合物である、リチウム遷移金属酸化物の製造方法。
(式2)
M(OH1−x)2
上記式中、Mが、Ni、Co、Mn、Al、Cu、Fe、Mg、B、Cr及び第2の周期の遷移金属からなる群から選択される2つまたはそれ以上であり、0≦x≦0.5である。
(式4)
Li a Ni x Mn y Co z M w O 2−t A t
上記式中、
0<a≦1.2、0≦x≦0.9、0≦y≦0.9、0≦z≦0.9、0<w≦0.3、2≦a+x+y+z+w≦2.3、0<t<0.2、
Mが、Al、Cu、Fe、Mg、B、Cr及び第2の周期の遷移金属からなる群から選択される1つ以上の金属カチオンであり、
Aが、−1または−2価の1つ以上のアニオンである。 - 前記リチウム遷移金属酸化物が、2種以上の遷移金属を含んでいることを特徴とする、請求項1に記載のリチウム遷移金属酸化物の製造方法。
- 前記式4において、x>y及びx>zの条件を満足することを特徴とする、請求項1に記載のリチウム遷移金属酸化物の製造方法。
- 請求項1から3のいずれか1項に記載の製造方法により製造されたリチウム遷移金属酸化物を含む正極、負極、及び前記正極と負極との間に高分子膜が介在している単位セルを電池ケースに内蔵させるステップを含む、リチウム二次電池の製造方法。
- 前記リチウム二次電池が、リチウムイオン電池であることを特徴とする、請求項4に記載のリチウム二次電池の製造方法。
- 前記リチウム二次電池が、リチウムイオンポリマー電池であることを特徴とする、請求項4に記載のリチウム二次電池の製造方法。
- 前記リチウム二次電池が、リチウムポリマー電池であることを特徴とする、請求項4に記載のリチウム二次電池の製造方法。
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KR1020130015206A KR101575024B1 (ko) | 2013-02-13 | 2013-02-13 | 낮은 탭 밀도를 갖는 전이금속 전구체 및 높은 입자 강도를 가진 리튬 전이금속 산화물 |
KR10-2013-0015206 | 2013-02-13 | ||
PCT/KR2014/001107 WO2014126373A1 (ko) | 2013-02-13 | 2014-02-11 | 낮은 탭 밀도를 갖는 전이금속 전구체 및 높은 입자 강도를 가진 리튬 전이금속 산화물 |
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JP7262230B2 (ja) * | 2019-01-22 | 2023-04-21 | 株式会社田中化学研究所 | 非水電解質二次電池用複合水酸化物小粒子 |
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- 2014-02-11 US US14/441,580 patent/US11577969B2/en active Active
- 2014-02-11 JP JP2015545387A patent/JP6224125B2/ja active Active
- 2014-02-11 WO PCT/KR2014/001107 patent/WO2014126373A1/ko active Application Filing
- 2014-02-11 BR BR112015013932A patent/BR112015013932B8/pt active IP Right Grant
- 2014-02-11 CN CN201480003552.6A patent/CN104884390B/zh active Active
- 2014-02-11 IN IN3943DEN2015 patent/IN2015DN03943A/en unknown
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TWI606632B (zh) | 2017-11-21 |
WO2014126373A1 (ko) | 2014-08-21 |
EP2902364A1 (en) | 2015-08-05 |
US11577969B2 (en) | 2023-02-14 |
EP2902364A4 (en) | 2016-06-29 |
EP2902364B1 (en) | 2018-06-06 |
CN104884390B (zh) | 2018-01-23 |
BR112015013932A2 (pt) | 2017-07-11 |
CN104884390A (zh) | 2015-09-02 |
KR101575024B1 (ko) | 2015-12-07 |
US20160002063A1 (en) | 2016-01-07 |
BR112015013932B1 (pt) | 2021-11-23 |
IN2015DN03943A (ja) | 2015-10-02 |
US20220135428A1 (en) | 2022-05-05 |
JP2016500048A (ja) | 2016-01-07 |
BR112015013932B8 (pt) | 2023-01-17 |
KR20140102367A (ko) | 2014-08-22 |
TW201448332A (zh) | 2014-12-16 |
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