JP2020167014A5

JP2020167014A5 -

Info

Publication number: JP2020167014A5
Application number: JP2019065778A
Authority: JP
Filing date: 2019-03-29
Publication date: 2022-01-18
Anticipated expiration: 2039-03-29

Description

リチウム塩としては特に指定はないが炭酸リチウム、水酸化リチウムが好ましい。ｘ＜０．６においては炭酸リチウムが好適であり、ｘが０．６以上では水酸化リチウムが適している。また、リチウム塩の粒径は、遷移金属複合化合物との反応性を考慮すると、平均粒子径で１０μｍ以下が好ましい。
The lithium salt is not particularly specified, but lithium carbonate and lithium hydroxide are preferable. When x <0.6, lithium carbonate is suitable, and when x is 0.6 or more, lithium hydroxide is suitable. The particle size of the lithium salt is preferably 10 μm or less in terms of average particle size in consideration of reactivity with the transition metal composite compound.

（実施例４２）
化学式Ｌｉ_１．００Ｎｉ_０．８０Ｃｏ_０．１５Ａｌ_０．０５Ｏ_２となるよう調整した水酸化リチウム、遷移金属複合化合物（化学式：Ｎｉ_０．８０Ｃｏ_０．１５Ａｌ_０．０５（ＯＨ）_２）に、カチオンＡとＢを含む複合酸化物としてＹ_０．３３Ｚｒ_０．６７Ｏ_１．８４をリチウム遷移金属複合酸化物に対し０．５質量％の比率になるように加え、精密混合機で乾式混合、その後、酸素ガスフローしながら６００℃で５時間、引き続き８００℃で２０時間焼成し、解砕、整粒してカチオンＡとＢが含まれたリチウム遷移金属複合酸化物を合成した。
(Example 42)
Lithium hydroxide, transition metal composite compound adjusted to have a chemical formula Li _1.00 Ni _0.80 Co _0.15 Al _0.05 O ₂ (chemical formula: Ni _0.80 Co _0.15 Al _0.05 (OH) To ₂ ), Y _0.33 Zr _0.67 O _1.84 as a composite oxide containing cations A and B was added so as to have a ratio of 0.5% by mass with respect to the lithium transition metal composite oxide, and the mixture was precisely mixed. Dry mixing with a machine, then firing at 600 ° C for 5 hours with oxygen gas flow, followed by firing at 800 ° C for 20 hours, crushing and sizing to synthesize a lithium transition metal composite oxide containing cations A and B. bottom.

（実施例４３）
化学式Ｌｉ_１．００Ｎｉ_０．８０Ｃｏ_０．１５Ａｌ_０．０５Ｏ_２となるよう調整した水酸化リチウム、遷移金属複合化合物（化学式：Ｎｉ_０．８０Ｃｏ_０．１５Ａｌ_０．０５（ＯＨ）_２）を加え、精密混合機で乾式混合、その後、酸素ガスフローしながら６００℃で５時間、引き続き８００℃で１５時間焼成し、解砕した。
続いて、カチオンＡとＢを含む複合酸化物としてＹ_０．３３Ｚｒ_０．６７Ｏ_１．８４をリチウム遷移金属複合酸化物に対し０．５質量％の比率になるように加え、精密混合機で乾式混合、
その後、酸素ガスフローしながら８００℃で５時間焼成し、解砕、整粒してカチオンＡとＢが含まれたリチウム遷移金属複合酸化物を合成した。
(Example 43)
Lithium hydroxide, transition metal composite compound adjusted to have a chemical formula Li _1.00 Ni _0.80 Co _0.15 Al _0.05 O ₂ (chemical formula: Ni _0.80 Co _0.15 Al _0.05 (OH) ₂ ) was added, dry mixing was performed with a precision mixer, and then the mixture was fired at 600 ° C. for 5 hours and then at 800 ° C. for 15 hours while flowing oxygen gas to crush it.
Subsequently, Y _0.33 Zr _0.67 O _1.84 was added as a composite oxide containing cations A and B so as to have a ratio of 0.5% by mass with respect to the lithium transition metal composite oxide, and a precision mixer was added. Dry mixing,
Then, it was calcined at 800 ° C. for 5 hours while flowing with oxygen gas, crushed and sized to synthesize a lithium transition metal composite oxide containing cations A and B.

（比較例６）
化学式Ｌｉ_１．００Ｎｉ_０．８０Ｃｏ_０．１５Ａｌ_０．０５Ｏ_２となるよう調整した水酸化リチウム、遷移金属複合化合物（化学式：Ｎｉ_０．８０Ｃｏ_０．１５Ａｌ_０．０５（ＯＨ）_２）を、精密混合機で乾式混合、その後、
酸素ガスフローしながら６００℃で５時間、引き続き８００℃で２０時間焼成し、解砕、整粒してリチウム遷移金属複合酸化物を合成した。
(Comparative Example 6)
Lithium hydroxide, transition metal composite compound adjusted to have a chemical formula Li _1.00 Ni _0.80 Co _0.15 Al _0.05 O ₂ (chemical formula: Ni _0.80 Co _0.15 Al _0.05 (OH) ₂ ) is dry-mixed with a precision mixer, and then
The lithium transition metal composite oxide was synthesized by firing at 600 ° C. for 5 hours and then at 800 ° C. for 20 hours while flowing oxygen gas, crushing and sizing.

（比較例８、比較例９）
比較例８、比較例９においては、表４に記載の成分比率となるカチオンＡとＢを含む複合酸化物（ＡＢＯｎ、ここでｎはカチオンＡとＢの価数に対し電荷中性条件を満たすように定まる値）をリチウム遷移金属複合酸化物に対し表４の質量％比率になるように加えた他は、実施例４２と同様に作製した。 (Comparative Example 8, Comparative Example 9)
In Comparative Examples 8 and 9, a composite oxide containing cations A and B having the component ratios shown in Table 4 (ABOn, where n is a charge neutrality condition with respect to the valences of the cations A and B). It was prepared in the same manner as in Example 42, except that the value determined as described above) was added to the lithium transition metal composite oxide in the mass% ratio of Table 4 .