WO2013027432A1 - Procédé de production de matière active d'électrode positive pour batteries au ion-lithium - Google Patents
Procédé de production de matière active d'électrode positive pour batteries au ion-lithium Download PDFInfo
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- WO2013027432A1 WO2013027432A1 PCT/JP2012/057203 JP2012057203W WO2013027432A1 WO 2013027432 A1 WO2013027432 A1 WO 2013027432A1 JP 2012057203 W JP2012057203 W JP 2012057203W WO 2013027432 A1 WO2013027432 A1 WO 2013027432A1
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- lithium
- positive electrode
- lithium ion
- active material
- electrode active
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Classifications
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/40—Nickelates
- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/136—Electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/51—Particles with a specific particle size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/40—Electric properties
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/021—Physical characteristics, e.g. porosity, surface area
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 method for producing a positive electrode active material for a lithium ion battery.
- This lithium ion secondary battery is composed of three basic elements: a positive electrode and a negative electrode, and a separator holding an electrolyte interposed between the two electrodes.
- the positive electrode and the negative electrode include an active material, a conductive material, a binder, A slurry obtained by mixing and dispersing a plasticizer in a dispersion medium as required is coated on a current collector such as a metal foil or a metal mesh.
- complex oxides of lithium and transition metals such as cobalt complex oxide (LiCoO 2 ), nickel complex oxide (LiNiO 2 ), manganese complex oxide (LiMn 2 O 4 ) are included.
- Various materials based on these have been proposed so far.
- the lithium composite oxide used as a positive electrode material for a lithium ion secondary battery is generally a compound of an element that is a main component of a positive electrode material for a lithium ion secondary battery (such as carbonates or oxides such as Co, Ni, and Mn). ) And a lithium compound (lithium carbonate or the like) are mixed at a predetermined ratio and heat-treated.
- Patent Document 1 discloses an aqueous solution containing one or more nitrates of Ni, Mn, or Co in a lithium carbonate suspension, or an aqueous solution containing Mg, Al, A mixed solution with an aqueous solution containing one or more of Ti, Cr, Fe, Cu or Zr nitrate is added to precipitate Li-containing composite metal carbonate, and the resulting Li-containing composite metal carbonate is solid-liquid.
- a method for producing a precursor material for a positive electrode material for a lithium ion secondary battery wherein the precursor material is fired after being separated from the solution by separation.
- the positive electrode active material for a lithium ion battery is effective for enabling rapid charge and discharge, in particular, in order to obtain good battery characteristics that the particle size is small and the particle size variation is small. For this reason, research and development have been actively conducted on a method for producing a positive electrode active material for a lithium ion battery having a particle size that is small and has little variation.
- an object of the present invention is to provide a method for efficiently producing a positive electrode active material for a lithium ion battery having a small and small variation in particle size (rapid charge / discharge characteristics) and good battery characteristics.
- the inventors of the present invention sprayed and dried a lithium metal nitrate solution slurry containing a lithium salt and a metal nitrate using a micro mist dryer to form a lithium metal salt composite powder, followed by firing.
- a positive electrode active material for a lithium ion battery having a small and small variation in particle size and good battery characteristics can be efficiently produced.
- a step of preparing a lithium metal nitrate solution slurry containing a lithium salt and a metal nitrate, and spraying the lithium metal nitrate solution slurry using a micro mist dryer A method for producing a positive electrode active material for a lithium ion battery, comprising: a step of drying to obtain a lithium metal salt composite powder; and a step of firing the powder.
- the metal contained in the metal nitrate is at least one selected from Ni, Mn, and Co.
- the metal nitrate contains at least Ni, and the molar ratio of Ni in the metal contained in the powder is 0.3 or more. is there.
- the metal salt contains at least Ni and Mn, and the molar ratio of Ni in the metal contained in the powder is Mn. Greater than molar ratio.
- the lithium salt is lithium carbonate.
- the particle size distribution of the particles becomes sharp, and the variation in the particle size can be well suppressed,
- dry powder having a particle size of 20 to 30 ⁇ m can be formed to a fine particle size of several ⁇ m. Therefore, various characteristics of the lithium ion battery using the positive electrode active material for a lithium ion battery produced by the production method according to the present invention are improved. Furthermore, drying and microparticulation can be performed at the same time, and the production efficiency is improved.
- composition of positive electrode active material for lithium ion battery As a material for the positive electrode active material for lithium ion batteries produced by the production method according to the present invention, compounds useful as a positive electrode active material for general positive electrodes for lithium ion batteries can be widely used. It is preferable to use a lithium-containing transition metal oxide such as lithium oxide (LiCoO 2 ), lithium nickelate (LiNiO 2 ), or lithium manganate (LiMn 2 O 4 ).
- lithium oxide LiCoO 2
- LiNiO 2 lithium nickelate
- LiMn 2 O 4 lithium manganate
- the positive electrode active material for a lithium ion battery produced using such a material is Composition formula: Li x Ni 1- y My O 2 (In the above formula, M is at least one selected from Ni, Mn, and Co, 0.9 ⁇ x ⁇ 1.1, and 0 ⁇ y ⁇ 0.7.) It is represented by The ratio of lithium to the total metal in the positive electrode active material for lithium ion batteries is 0.9 to 1.1. However, when the ratio is less than 0.9, it is difficult to maintain a stable crystal structure, and when it exceeds 1.1, the capacity is high. This is because of a low.
- the positive electrode active material for a lithium ion battery produced by the production method of the present invention is an aggregate containing primary particles, and the average primary particle size is 1.0 to 3.0 ⁇ m. Considering the distance of movement of lithium ions during charging / discharging, the smaller primary particle size is advantageous for rapid charging / discharging as the conduction distance is shorter. In some cases, the possibility of the particles breaking up increases. Accordingly, there is an appropriate range for the average particle size of the primary particles, and it is desirable that the average particle size is 1.0 to 3.0 ⁇ m. If the average particle size is less than 1.0 ⁇ m, the primary particles may be destroyed by the press treatment during electrode production.
- the average particle size of the secondary particles formed by aggregation of the primary particles is desirably 5.0 to 9.0 ⁇ m. If the average particle size of the secondary particles is less than 5.0 ⁇ m, a large amount of solvent is required when applying the slurry, which is not preferable in terms of industrial production. Further, if the average particle size of the secondary particles is more than 9.0 ⁇ m, the contact area with the electrolytic solution is reduced, and rapid charge / discharge is difficult.
- the variation in particle size when the particle size distribution curve of the frequency is displayed with a general particle size distribution meter around the average particle size, it is considered that the variation is the least, and the following variation is The condition was used as an index of variation. That is, when the maximum diameter ( ⁇ m) is expressed as dmax, the average diameter ( ⁇ m) is expressed as d50, and the minimum diameter ( ⁇ m) is expressed as dmin, the common logarithm of the ratio (dmax / d50) and the common ratio (d50 / dmin) are used. If the logarithms are both less than 0.7, the particle diameter has little variation.
- the conditions can be expressed as follows: Log (maximum diameter ( ⁇ m) / average particle diameter ( ⁇ m)) ⁇ 0.70 Log (average particle diameter ( ⁇ m) / minimum diameter ( ⁇ m)) ⁇ 0.70
- a metal nitrate containing at least one metal selected from Ni, Mn, and Co is prepared.
- the metal nitrate for example, nickel nitrate, cobalt nitrate, manganese nitrate, and the like can be used.
- nitrate when nitrate is used, even if it is mixed as an impurity in the firing raw material, it can be fired as it is, so that the cleaning process can be omitted, and the function of the nitrate functioning as an oxidant and promoting the oxidation of the metal in the firing raw material.
- the respective metals contained in the metal nitrate are adjusted so as to have a desired molar ratio. Thereby, the molar ratio of each metal in the positive electrode active material is determined.
- the molar ratio of Ni in the metal is 0.3 or more. This is because when the molar ratio of Ni is less than 0.3, the absolute amount of oxygen necessary for firing 1 mol of the positive electrode material is reduced.
- the metal nitrate solution contains at least Ni and Mn, it is preferable that the molar ratio of Ni in the contained metal is larger than the molar ratio of Mn. This is because when the molar ratio of Ni is less than or equal to the molar ratio of Mn, the valence of Ni becomes bivalent, and there is no need to oxidize Ni during the heat treatment.
- lithium carbonate is suspended in pure water, and then the above metal salt solution of metal is added to prepare a lithium metal nitrate solution slurry.
- the lithium metal nitrate solution slurry is spray-dried with a micro mist dryer to obtain a lithium metal salt composite powder.
- M the metal of the metal salt
- a micro mist dryer is a spray dryer that uses a pulverizing device, and thinly spreads a lithium metal salt solution slurry by a high-speed air stream in multiple paths and
- a ⁇ m mist can be formed.
- the atomizer for example, an apparatus equipped with a four-fluid nozzle is preferable.
- the atomization apparatus provided with the four-fluid nozzle is provided with two liquid and gas system paths symmetrically with respect to the nozzle edge. For example, atomization is performed by the fluid flow surface at the edge tip and the collision focus.
- the produced mist is dried in a drying chamber in a micro mist dryer to produce a dry powder of a lithium metal nitrate complex having a fine particle size (several ⁇ m) mainly composed of the compound on the right side of the above formula.
- a micro mist dryer to produce a dry powder of a lithium metal nitrate complex having a fine particle size (several ⁇ m) mainly composed of the compound on the right side of the above formula.
- the average droplet diameter can be controlled by changing the gas-liquid ratio.
- the particle size distribution of the particles becomes sharp, and the variation in the particle size is satisfactorily suppressed.
- Nozzle clogging that has occurred in the external mixing method is suppressed, enabling continuous spraying for a long time.
- the required spray amount can be easily obtained by adjusting the edge length.
- a dry powder having a particle size of 20 to 30 ⁇ m in normal drying can be formed into a fine particle size of several ⁇ m.
- Drying and microparticulation can be performed at the same time, resulting in good production efficiency.
- the dry powder is filled in a baking container of a predetermined size so as to have a predetermined thickness, and is subjected to an oxidation treatment in which heat is maintained for a predetermined time under atmospheric pressure in an atmosphere that can maintain oxidizing properties such as in the air.
- the powder of a positive electrode active material is obtained by grind
- the reaction at this time is represented by the following chemical formula when the metal of the metal salt is represented by “M”. In either formula, there is an oxygen term on the right side, indicating that oxygen is generated from the firing raw material.
- the lithium metal nitrate solution slurry is spray-dried using a micro mist dryer, so that the particle size distribution of the particles becomes sharp and the variation in the particle size can be well suppressed, and the normal drying is performed. Then, a dry powder having a particle diameter of 20 to 30 ⁇ m can be formed into a fine particle diameter of several ⁇ m. Therefore, various characteristics of the lithium ion battery using the positive electrode active material for a lithium ion battery produced by the production method according to the present invention are improved. Furthermore, drying and microparticulation can be performed at the same time, and the production efficiency is improved.
- Example 1 First, 517 g of lithium carbonate was suspended in 1.06 liter of pure water, and then 4.8 liter of a metal salt solution was added.
- the metal salt solution is prepared by adjusting nickel nitrate, cobalt nitrate and manganese nitrate hydrates so that Ni, Mn and Co are in a predetermined ratio, and the total number of moles of Ni, Mn and Co. was adjusted to 14 mol.
- a metal nitrate solution was added to the lithium carbonate suspension thus prepared to form a slurry.
- this slurry was spray-dried with a micro mist dryer (MDL-100M) manufactured by Fujisaki Electric Co., Ltd. to obtain 2800 g of a dry powder of lithium metal nitrate composite (precursor material for lithium ion secondary battery positive electrode material). From the XRD diffraction of this composite, it was confirmed that the composite was formed from lithium nitrate (LiNO 3 ) and basic metal nitrate ⁇ M 3 (NO 3 ) 2 (OH) 4 : M is a metal component ⁇ .
- MDL-100M micro mist dryer
- the composite was filled and oxidized in an air atmosphere at a temperature of 980 ° C. for 12 hours.
- the obtained oxide was pulverized with a ball mill to obtain a powder of a lithium ion secondary battery positive electrode material.
- BCL-20 type hot air circulation
- Example 2 First, 517 g of lithium carbonate was suspended in 1.06 liter of pure water, and then 4.8 liter of a metal salt solution was added.
- the metal salt solution is prepared by adjusting nickel nitrate, cobalt nitrate and manganese nitrate hydrates so that Ni, Mn and Co are in a predetermined ratio, and the total number of moles of Ni, Mn and Co. was adjusted to 14 mol.
- a metal nitrate solution was added to the lithium carbonate suspension thus prepared to form a slurry. Subsequently, this slurry was spray-dried with a micro mist dryer (MDL-100M) manufactured by Fujisaki Electric Co., Ltd. to obtain 2800 g of a dry powder of lithium metal nitrate composite (precursor material for lithium ion secondary battery positive electrode material). From the XRD diffraction of this composite, it was confirmed that the composite was formed from lithium nitrate (LiNO 3 ) and basic metal nitrate ⁇ M 3 (NO 3 ) 2 (OH) 4 : M is a metal component ⁇ .
- the composite was filled and oxidized in an air atmosphere at a temperature of 870 ° C. for 12 hours.
- the obtained oxide was pulverized with a ball mill to obtain a powder of a lithium ion secondary battery positive electrode material.
- BCL-20 type hot air circulation
- Example 3 First, 517 g of lithium carbonate was suspended in 1.06 liter of pure water, and then 4.8 liter of a metal salt solution was added.
- the metal salt solution is prepared by adjusting nickel nitrate, cobalt nitrate and manganese nitrate hydrates so that Ni, Mn and Co are in a predetermined ratio, and the total number of moles of Ni, Mn and Co. was adjusted to 14 mol.
- a metal nitrate solution was added to the lithium carbonate suspension thus prepared to form a slurry.
- this slurry was spray-dried with a micro mist dryer (MDL-100M) manufactured by Fujisaki Electric Co., Ltd. to obtain 2800 g of a dry powder of lithium metal nitrate composite (precursor material for lithium ion secondary battery positive electrode material). From the XRD diffraction of this composite, it was confirmed that the composite was formed from lithium nitrate (LiNO 3 ) and basic metal nitrate ⁇ M 3 (NO 3 ) 2 (OH) 4 : M is a metal component ⁇ .
- MDL-100M micro mist dryer
- the composite was filled and oxidized in an air atmosphere at a temperature of 820 ° C. for 12 hours.
- the obtained oxide was pulverized with a ball mill to obtain a powder of a lithium ion secondary battery positive electrode material.
- BCL-20 type hot air circulation
- Example 1 to 3 the primary particles are large, the secondary particles are small, the particle size variation, in particular, the minimum and average particle size variations are well suppressed, and a particle size distribution suitable for rapid charge / discharge is shown. It was. Both discharge capacity and rate characteristics were good. In Comparative Examples 1 to 3, the distribution of the primary particles was small and the secondary particles were large, the particle size variation was large, and both the discharge capacity and the rate characteristics were bad.
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Abstract
L'invention porte sur un procédé pour produire de manière efficace une matière active d'électrode positive pour batteries au ion-lithium ayant de bonnes caractéristiques de batterie, ladite matière active d'électrode positive ayant de très petits diamètres de particule avec moins de variation. Ce procédé de production d'une matière active d'électrode positive pour batteries au ion-lithium comprend : une étape dans laquelle une bouillie de solution de sel de nitrate de métal et de lithium contenant un sel de lithium et un sel de nitrate de métal est préparée; une étape dans laquelle une poudre d'un composite d'un sel de métal et de lithium est obtenue par pulvérisation et séchage de la bouillie de solution de sel de nitrate de métal et de lithium à l'aide d'un sécheur à micro-brouillard; et une étape dans laquelle la poudre est cuite.
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JP2013523400A JP5567742B2 (ja) | 2011-08-23 | 2012-03-21 | リチウムイオン電池用正極活物質の製造方法 |
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JP2011-181837 | 2011-08-23 | ||
JP2011181837 | 2011-08-23 |
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JP (1) | JP5567742B2 (fr) |
TW (1) | TWI460906B (fr) |
WO (1) | WO2013027432A1 (fr) |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JP6023587B2 (ja) * | 2011-03-29 | 2016-11-09 | Jx金属株式会社 | リチウムイオン電池用正極活物質の製造方法 |
WO2020116649A1 (fr) * | 2018-12-07 | 2020-06-11 | 住友化学株式会社 | Précurseur pour matériaux actifs d'électrode positive de batterie secondaire au lithium, procédé de production de précurseur pour matériaux actifs d'électrode positive de batterie secondaire au lithium, et procédé de production de composé métallique composite de lithium |
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TWI651271B (zh) * | 2016-05-27 | 2019-02-21 | 比利時商烏明克公司 | 小粒徑的鎳鋰金屬複合氧化物粉體的製造方法 |
US11963287B2 (en) | 2020-09-24 | 2024-04-16 | 6K Inc. | Systems, devices, and methods for starting plasma |
KR20230095080A (ko) | 2020-10-30 | 2023-06-28 | 6케이 인크. | 구상화 금속 분말을 합성하는 시스템 및 방법 |
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- 2012-03-21 JP JP2013523400A patent/JP5567742B2/ja active Active
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WO2020116649A1 (fr) * | 2018-12-07 | 2020-06-11 | 住友化学株式会社 | Précurseur pour matériaux actifs d'électrode positive de batterie secondaire au lithium, procédé de production de précurseur pour matériaux actifs d'électrode positive de batterie secondaire au lithium, et procédé de production de composé métallique composite de lithium |
JP2020092070A (ja) * | 2018-12-07 | 2020-06-11 | 住友化学株式会社 | リチウム二次電池正極活物質用前駆体、リチウム二次電池正極活物質用前駆体の製造方法及びリチウム複合金属化合物の製造方法 |
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