WO2018016525A1 - リチウム金属複合酸化物粉末 - Google Patents
リチウム金属複合酸化物粉末 Download PDFInfo
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- WO2018016525A1 WO2018016525A1 PCT/JP2017/026104 JP2017026104W WO2018016525A1 WO 2018016525 A1 WO2018016525 A1 WO 2018016525A1 JP 2017026104 W JP2017026104 W JP 2017026104W WO 2018016525 A1 WO2018016525 A1 WO 2018016525A1
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- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Definitions
- the present invention relates to a lithium metal composite oxide powder and a lithium ion battery using this as a positive electrode.
- Lithium ion batteries have a long history and their commercial production began in the 1990s. However, it can be said that the development of lithium-ion batteries has been developed in earnest with the spread of mobile terminals, smartphones, electric vehicles and the like since 2000.
- Lithium ion batteries like other batteries, have a positive electrode, a negative electrode, an electrolyte, and an outer package as the main components. Among them, the positive electrode active material used for the positive electrode is an important material that affects the battery performance of the lithium ion battery. is there.
- Known positive electrode active materials used in lithium ion batteries include lithium cobaltate, ternary complex oxides, nickel complex oxides, spinel complex oxides, olivine compounds, etc., among which lithium cobaltate, Ternary composite oxides and nickel composite oxides are known as composite oxides having a large discharge capacity and a layered crystal structure.
- a positive electrode active material made of a layered composite metal oxide is manufactured by mixing powder of a composite metal hydroxide as a precursor and a lithium compound, and firing in an oxidizing atmosphere. At this time, in order to increase the crystallinity of the positive electrode active material to be produced, the ratio of lithium contained in the precursor metal to the lithium compound (lithium / metal) is generally more than 1.
- the positive electrode active material having a general layered structure an excessive amount of lithium compound remains on the surface of the active material after firing. If this lithium compound remains in a large amount, a cross-linking reaction of the binder used in manufacturing the positive electrode is caused, and the positive electrode slurry is gelled, which causes a problem that electrode coating cannot be performed. It is preferable that the content of residual lithium is small.
- the positive electrode active material having the above layered structure is characterized by a higher capacity than other active materials.
- the demand for higher capacity lithium-ion batteries is increasing with the diversification of applications, and the success of electric vehicles is directly linked to the possibility of higher capacity.
- increasing the capacity of the active material is how much active material can be filled in the electrode, that is, increasing the packing density of the active material to the electrode also increases the capacity of the lithium ion battery.
- the positive electrode active material powder when the positive electrode active material powder is compressed under high pressure under high pressure to obtain a positive electrode active material powder filled with high density, the positive electrode active material powder is increased as the load on the positive electrode active material powder increases. The constituent secondary particles are broken, voids and fine powder are generated inside the powder, and the compressive stress is reduced. By repeating the destruction of the secondary particles and the reduction of the compressive stress, a positive electrode active material that finally contains voids and fine powder and has a non-uniform particle shape is obtained by compression filling. The packing density of the powder often does not reach the target value.
- the average particle diameter D50 is 7 to 20 ⁇ m
- the volume-based cumulative diameter D10 is 50% or more of the average particle diameter D50
- the volume-based cumulative diameter D90 is 150% or less of the average particle diameter D50.
- a positive electrode active material for a lithium secondary battery characterized by comprising a mixture of 1 is disclosed.
- the present inventor made an effort to obtain a positive electrode active material having a high packing density regardless of the bimodal mixing method.
- the positive electrode active material powder having an average particle size and a BET specific surface area in a specific range, which is obtained by washing the lithium-nickel-cobalt-manganese composite oxide immediately after firing with specific conditions, under a high load compression It has been found that it exhibits high stress, that is, such a positive electrode active material powder can be filled at a higher density than the conventional product. Moreover, it has been discovered that such a positive electrode active material powder exhibits desirable quality even in the point that the amount of remaining lithium is small.
- invention 4 The lithium metal composite oxide powder for a lithium ion battery positive electrode active material according to Inventions 1 to 3, which has a packing density of 3.0 g / cm 3 or more when pressed at 127 MPa.
- invention 5 A positive electrode active material comprising the lithium metal composite oxide powder according to any one of Inventions 1 to 4.
- Invention 6) A lithium ion battery using the positive electrode active material of Invention 5.
- (Invention 7) A method for producing a lithium metal composite oxide powder according to any one of Inventions 1 to 4, comprising the following steps: (Mixing step) A nickel-cobalt-manganese composite hydroxide powder having an average particle size of 10.0 ⁇ m to less than 20.0 ⁇ m is prepared as a precursor powder, and a lithium compound powder is added to the precursor powder to prepare a mixture.
- (Baking step) A step of baking the mixture obtained in the above mixing step in an air stream containing oxygen at a temperature range of 450 ° C. to 900 ° C. for 2 hours to 20 hours;
- (Washing step) A step of washing the fired product (lithium / nickel / cobalt / manganese composite oxide) with 100 ml or more of pure water per 100 g to obtain a lithium metal composite oxide powder.
- the lithium metal composite oxide powder of the present invention is washed with 100 ml or more of pure water per 100 g.
- the performance of lithium metal composite oxide powder is improved by such water washing, that is, the amount of residual lithium that is inconvenient for the positive electrode agent is reduced, the lithium metal composite oxidation that such water washing provides It is difficult to express the chemical characteristics of an object with a uniform chemical formula.
- the particles constituting the lithium metal composite oxide that has undergone such water washing are not completely uniform, and are not specified by a uniform size and shape. Therefore, as one of the features of the lithium metal composite oxide powder of the present invention, a kind of manufacturing method of “washed with 100 ml or more of pure water per 100 g” must be adopted.
- a lithium metal-based positive electrode active material having a small amount of remaining lithium and a high electrode density when used as a positive electrode for a lithium ion battery, and a lithium ion battery using the same.
- a nickel / cobalt / manganese composite hydroxide powder having an average particle diameter of 10.0 ⁇ m to less than 20.0 ⁇ m is prepared as a precursor powder.
- Lithium compound powder is added to the precursor powder.
- lithium compound lithium hydroxide or lithium carbonate is generally used.
- the mixing means for the precursor powder and the lithium compound powder is not limited as long as the mixing means applies a shearing force, and various mixers are generally used.
- the firing temperature is in the range of 450 ° C to 900 ° C, preferably in the range of 600 ° C to 850 ° C.
- the firing time is 2 hours to 20 hours, preferably 3 hours to 15 hours.
- the firing may be performed once or multiple times. When firing multiple times, the above temperature range is maintained for 2 to 30 hours in each firing.
- the first stage is fired at a temperature range of 450 ° C. to 700 ° C. for 3 hours to 6 hours
- the second stage is fired at a temperature range of 700 ° C. to 900 ° C. for 4 hours to 10 hours.
- the equipment used for firing is not limited as long as such firing conditions can be achieved.
- a tubular furnace, a muffle furnace, a rotary kiln (RK), or a roller hearth kiln (RHK) is used.
- RHK or RK is used.
- the fired product (lithium / nickel / cobalt / manganese composite oxide) is washed with 100 ml or more of pure water per 100 g to obtain the lithium metal composite oxide powder of the present invention. Cleaning is not a problem as long as the amount of cleaning water used is sufficient to satisfy the above range. Typically, pure water at 25 ° C. in an amount of 100 ml or more is added to 100 g of the fired product to bring the fired product into sufficient contact with water, and then the lithium metal composite oxide powder is separated.
- the means for contacting the fired product with water is not limited as long as the fired product is uniformly dispersed in water without destroying the particles of the fired product.
- a dispersion composed of a fired product and water is stirred in a container provided with a stirring blade.
- the lithium metal composite oxide powder is separated by filtering an aqueous dispersion slurry of the lithium metal composite oxide powder. Any filtration means may be used, and any of suction filtration, pressure filtration and the like can be used.
- the fired product separated after washing with water is dried. Drying is performed in an air stream containing oxygen, preferably in a temperature range of 200 ° C. to 800 ° C., more preferably 300 ° C. to 700 ° C., and still more preferably 400 ° C. to 600 ° C.
- the lithium metal composite oxide powder for a lithium ion battery positive electrode active material of the present invention has a high packing density, for example, a density of 3.0 g / cm 3 or more when pressed at 127 MPa.
- a preferable lithium metal composite oxide powder for a lithium ion battery positive electrode active material of the present invention is 3.2 g / cm 3 or more when pressed at 127 MPa, 3.3 g / cm 3 or more when pressed at 191 MPa, and 255 MPa. When pressed at a pressure of 3.4 g / cm 3 or more, it has a density of 3.5 g / cm 3 or more when pressed at 318 MPa.
- the lithium metal composite oxide powder for a lithium ion battery positive electrode active material of the present invention contains 10 mol% or less of one or more dopants selected from Ca, Ti, Al, Mg, W, Zr, Cr, and V. Further, it can be included. By supplying the metal compound containing these dopant atoms as an additional raw material to the mixing step and / or the firing step, such a dopant can be introduced into the lithium metal composite oxide.
- the lithium metal composite oxide powder of the present invention can be expected as a positive electrode active material that provides a lithium ion battery excellent in volume capacity.
- the lithium metal composite oxide powder of the present invention can be used alone as a positive electrode active material for a lithium ion battery.
- a mixture of the lithium metal composite oxide powder of the present invention and one or more other positive electrode active materials for lithium ion batteries having different particle sizes and compositions may be used as the positive electrode active material.
- Example 1 (Mixed) Precursor nickel / cobalt / manganese composite hydroxide (composition: Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 , average particle size 12.0 ⁇ m) 653g was added and it mixed, applying a shear force, and obtained 3153g of mixtures. (Firing) The above mixture was placed in a ceramic firing mortar, heated to 180 ° C. over 30 minutes in an oxygen stream, and then heated to 480 ° C. over 4 hours. After maintaining at that temperature for 12 hours, it was cooled to room temperature. Next, the temperature was raised to 180 ° C. over 3 hours, and further raised to 800 ° C. over 2.5 hours, and then held at that temperature for 6 hours.
- a lithium metal composite oxide powder for a lithium ion battery positive electrode active material of the present invention having the composition: Li 1.02 Ni 0.8 Co 0.1 Mn 0.1 O 2 was obtained.
- the properties of the lithium metal composite oxide powder of the present invention were evaluated by the following methods. The results are shown in Table 1.
- the average particle size (D 50 ) of the lithium metal composite oxide particles was measured using a laser scattering type particle size distribution analyzer (Mastersizer LS-230).
- Lithium metal composite oxide powder was placed in a specific surface area measuring device (Microstarix Tristar), degassed at 250 ° C, and then BET method by nitrogen adsorption at liquid nitrogen temperature. The specific surface area was measured.
- pellet density 0.6 g of lithium metal composite oxide powder was placed in a pellet density measuring device (sample diameter 10 mm P / O / Weber PW10), and after applying a predetermined pressure, the thickness of the pellet was measured. .
- Example 2 (Mixed) precursor nickel / cobalt / manganese composite hydroxide (composition: Ni 0.8 Co 0.1 Mn 0.1 (OH) 2 , average particle size 17.0 ⁇ m) 1650 g of powder and lithium hydroxide powder 432 g was added and mixed while applying a shearing force to obtain 3153 g of a mixture. (Firing) The above mixture was placed in a ceramic firing mortar, heated to 180 ° C. over 30 minutes in an oxygen stream, and then heated to 480 ° C. over 4 hours. After maintaining at that temperature for 12 hours, it was cooled to room temperature. Next, the temperature was raised to 180 ° C. over 30 minutes, and further heated to 800 ° C.
- the lithium metal composite oxide powder of the present invention has a specific average particle size and specific surface area, can be filled with high density, and has a reduced amount of residual lithium.
- a lithium metal composite oxide powder of the present invention is used as a positive electrode active material of a lithium ion lithium ion battery, gelation during the application of the positive electrode agent is suppressed, and high output of the battery is expected.
- the lithium metal composite oxide powder of the present invention can contribute to the production of a high-quality positive electrode agent and a lithium ion battery having a large volume capacity using the positive electrode agent.
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Abstract
Description
(発明1)組成:LiaNibCocMndO2(0.8≦a≦1.2、0.7≦b≦0.95、0.05≦c≦0.33、0.05≦d≦0.33、b+c+d=1)を有するリチウム・ニッケル・コバルト・マンガン複合酸化物の粒子からなり、
上記粒子の平均粒径(体積基準平均径)が10.0μmを超え16.0μm未満であり、
上記粒子の窒素吸着によるBET法での比表面積が0.5m2/gを超え2.0m2/g未満であり、
その100gあたり100ml以上の量の純水によって洗浄されたものであり、残存水酸化リチウム量が0.3重量%以下に低減されている、
リチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。
(発明2)上記粒子の窒素吸着によるBET法での比表面積が1.0m2/gを超え2.0m2/g未満である、発明1のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。
(発明3)10モル%以下の、Ca,Ti,Al,Mg,W,Zr,Cr,Vから選ばれる1種以上のドーパントを更に含む、発明1または2のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。
(発明4)127MPaで加圧した際に3.0g/cm3以上の充填密度を有する、発明1~3のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。
(発明5)発明1~4のいずれかのリチウム金属複合酸化物粉末を含む正極活物質。
(発明6)発明5の正極活物質を用いたリチウムイオン電池。
(発明7)以下の工程を有する、発明1~4のいずれかのリチウム金属複合酸化物粉末の製造方法;
(混合工程)平均粒径が10.0μm~20.0μm未満のニッケル・コバルト・マンガン複合水酸化物の粉末を前駆体粉末として用意し、この前駆体粉末にリチウム化合物の粉末を加えて混合物を得る工程であって、ここで上記前駆体粉末と上記リチウム化合物粉末との量比は、元素Li、Ni、Co、Mnが組成:LiaNibCocMndO2(0.8≦a≦1.2、0.7≦b≦0.95、0.05≦c≦0.33、0.05≦d≦0.33、b+c+d=1)を満たす割合で含まれる混合物が得られるような範囲にある;
(焼成工程)上記混合工程で得られた混合物を、酸素を含む気流中で、450℃~900℃の温度範囲で、2時間~20時間、焼成する工程;
(水洗工程)焼成物(リチウム・ニッケル・コバルト・マンガン複合酸化物)を、その100gあたり100ml以上量の純水によって洗浄して、リチウム金属複合酸化物粉末を得る工程。
本発明のリチウム金属複合酸化物粉末の製造方法を以下に述べる。
本発明のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末は、10.0μmを超え16.0μm未満、好ましくは10μmを超え15.0μm未満の平均粒径(体積基準平均径)を有し、0.5m2/gを超え2.0m2/g未満、好ましくは1.0m2/gを超え2.0m2/g未満、更に好ましくは、1.0m2/gを超え1.5m2/g未満の窒素吸着によるBET法での比表面積を有する。その残存LiOHは0.3重量%以下に低減されている。さらに本発明のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末は高い充填密度、例えば、127MPaで加圧した際に3.0g/cm3以上の密度を有する。好ましい本発明のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末は、127MPaで加圧した際に3.2g/cm3以上、191MPaで加圧した際に3.3g/cm3以上、255MPaで加圧した際に3.4g/cm3以上、318MPaで加圧した際に3.5g/cm3以上の密度を有する。
更に、本発明のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末は、10モル%以下の、Ca,Ti,Al,Mg,W,Zr,Cr,Vから選ばれる1種以上のドーパントを更に含むことができる。これらドーパント原子を含む金属化合物を上記混合工程及び/又は上記焼成工程に追加原料として供給することにより、このようなドーパントを上記リチウム金属複合酸化物に導入することができる。
本発明のリチウム金属複合酸化物粉末は体積容量に優れたリチウムイオン電池をもたらす正極活物質として期待できる。本発明のリチウム金属複合酸化物粉末を単独でリチウムイオン電池の正極活物質として用いることができる。本発明のリチウム金属複合酸化物粉末と、粒径や組成の異なる1種以上の他のリチウムイオン電池用正極活物質との混合物を正極活物質として用いてもよい。
(混合)前駆体であるニッケル・コバルト・マンガン複合水酸化物(組成:Ni0.8Co0.1Mn0.1(OH)2、平均粒径12.0μm)粉末2500gに水酸化リチウム粉末653gを加え、せん断力を掛けながら混合し、混合物3153gを得た。(焼成) 上記混合物をセラミックス製焼成匣鉢にとり、酸素気流中で180℃まで30分かけて昇温し、その後480℃まで4時間掛けて昇温した。そのままの温度で12時間保持した後、室温まで冷却した。次に180℃まで3時間かけて昇温し、更にその後800℃まで2.5時間かけて昇温した後、そのままの温度で6時間保持した。室温まで冷却後、解砕を行って焼成物を得た。(水洗) 上記焼成物100gを取り100mlの水と混合し、25℃で5分間攪拌し、吸引濾過してリチウム金属複合酸化物を分離した。このリチウム金属複合酸化物を100℃で20時間減圧乾燥して水分を除き、さらに酸素気流中500℃で20時間焼成した。
(混合)前駆体であるニッケル・コバルト・マンガン複合水酸化物(組成:Ni0.8Co0.1Mn0.1(OH)2、平均粒径17.0μm)粉末1650gに水酸化リチウム粉末432gを加え、せん断力を掛けながら混合し、混合物3153gを得た。(焼成) 上記混合物をセラミックス製焼成匣鉢にとり、酸素気流中で180℃まで30分かけて昇温し、その後480℃まで4時間かけて昇温した。そのままの温度で12時間保持した後、室温まで冷却した。次に180℃まで30分かけて昇温し、更にその後800℃まで2.5時間かけて昇温した後、そのままの温度で6時間保持した。室温までを行ってリチウム金属複合酸化物焼成体を得た。(水洗)実施例1と同様に行った。こうして組成:Li1.02Ni0.8Co0.1Mn0.1O2を有する本発明のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末を得た。その性状を表1に示す。
[比較例3]実施例1と同じ条件で原料を混合、焼成、冷却、解砕してリチウム金属複合酸化物焼成体を得た。これを水洗することなく比較用のリチウム金属複合酸化物粉末に用いた。これは組成:Li1.02Ni0.8Co0.1Mn0.1O2を有する。その評価結果を表1に示す。
Claims (7)
- 組成:LiaNibCocMndO2(0.8≦a≦1.2、0.7≦b≦0.95、0.05≦c≦0.33、0.05≦d≦0.33、b+c+d=1)を有するリチウム・ニッケル・コバルト・マンガン複合酸化物の粒子からなり、
上記粒子の平均粒径(体積基準平均径)が10.0μmを超え16.0μm未満であり、
上記粒子の窒素吸着によるBET法での比表面積が0.5m2/gを超え2.0m2/g未満であり、
その100gあたり100ml以上の量の純水によって洗浄されたものであり、残存水酸化リチウム量が0.3重量%以下に低減されている、
リチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。 - 上記粒子の窒素吸着によるBET法での比表面積が1.0m2/gを超え2.0m2/g未満である、請求項1に記載のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。
- 10モル%以下の、Ca,Ti,Al,Mg,W,Zr,Cr,Vから選ばれる1種以上のドーパントを更に含む、請求項1または2に記載のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。
- 127MPaで加圧した際に3.0g/cm3以上の充填密度を有する、請求項1~3のいずれかに記載のリチウムイオン電池正極活物質用リチウム金属複合酸化物粉末。
- 請求項1~4のいずれかに記載のリチウム金属複合酸化物粉末を含む正極活物質。
- 請求項5に記載の正極活物質を用いたリチウムイオン電池。
- 以下の工程を有する、請求項1~4のいずれかに記載のリチウム金属複合酸化物粉末の製造方法;
(混合工程)平均粒径が10.0μm~20.0μm未満のニッケル・コバルト・マンガン複合水酸化物の粉末を前駆体粉末として用意し、この前駆体粉末にリチウム化合物の粉末を加えて混合物を得る工程であって、ここで上記前駆体粉末と上記リチウム化合物粉末との量比は、元素Li、Ni、Co、Mnが組成:LiaNibCocMndO2(0.8≦a≦1.2、0.7≦b≦0.95、0.05≦c≦0.33、0.05≦d≦0.33、b+c+d=1)を満たす割合で含まれる混合物が得られるような範囲にある;
(焼成工程)上記混合工程で得られた混合物を、酸素を含む気流中で、450℃~900℃の温度範囲で、2時間~20時間、焼成する工程;
(水洗工程)焼成物(リチウム・ニッケル・コバルト・マンガン複合酸化物)を、その100gあたり100ml以上量の純水によって洗浄して、リチウム金属複合酸化物粉末を得る工程。
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JP2021530085A (ja) * | 2018-06-28 | 2021-11-04 | ビーエイエスエフ・ソシエタス・エウロパエアBasf Se | Niの多い電極活物質の製造方法 |
US20210376318A1 (en) * | 2018-06-28 | 2021-12-02 | Basf Se | Method for processing ni-rich electrode active materials |
CN109713228B (zh) * | 2019-01-04 | 2021-07-23 | 南通瑞翔新材料有限公司 | 一种锂离子电池三元材料可循环的水洗降碱方法 |
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JP7455871B2 (ja) | 2020-02-07 | 2024-03-26 | 富士フイルム株式会社 | 無機固体電解質含有組成物、全固体二次電池用シート及び全固体二次電池並びに、全固体二次電池用シート及び全固体二次電池の製造方法 |
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KR20220045813A (ko) * | 2020-10-06 | 2022-04-13 | 주식회사 엘지화학 | 고함량의 니켈 함유 리튬 복합전이금속 산화물 양극 활물질 입자 혼합물의 제조방법 |
KR102587970B1 (ko) | 2020-10-06 | 2023-10-10 | 주식회사 엘지화학 | 고함량의 니켈 함유 리튬 복합전이금속 산화물 양극 활물질 입자 혼합물의 제조방법 |
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TW201806867A (zh) | 2018-03-01 |
JPWO2018016525A1 (ja) | 2019-06-13 |
US20190288284A1 (en) | 2019-09-19 |
CN109643795A (zh) | 2019-04-16 |
EP3490041A4 (en) | 2020-01-08 |
KR102236601B1 (ko) | 2021-04-07 |
EP3490041A1 (en) | 2019-05-29 |
KR20190032452A (ko) | 2019-03-27 |
TWI654140B (zh) | 2019-03-21 |
JP7041620B2 (ja) | 2022-03-24 |
CN109643795B (zh) | 2022-01-04 |
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