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WO2016129361A1 - Matériau actif d'électrode positive pour pile au lithium-ion, électrode positive pour pile au lithium-ion, pile au lithium-ion, et procédé de fabrication de matériau actif d'électrode positive pour pile au lithium-ion - Google Patents

Matériau actif d'électrode positive pour pile au lithium-ion, électrode positive pour pile au lithium-ion, pile au lithium-ion, et procédé de fabrication de matériau actif d'électrode positive pour pile au lithium-ion Download PDF

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Publication number
WO2016129361A1
WO2016129361A1 PCT/JP2016/051889 JP2016051889W WO2016129361A1 WO 2016129361 A1 WO2016129361 A1 WO 2016129361A1 JP 2016051889 W JP2016051889 W JP 2016051889W WO 2016129361 A1 WO2016129361 A1 WO 2016129361A1
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WIPO (PCT)
Prior art keywords
positive electrode
active material
electrode active
lithium
lithium ion
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Ceased
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PCT/JP2016/051889
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English (en)
Japanese (ja)
Inventor
友哉 田村
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JX Nippon Mining and Metals Corp
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JX Nippon Mining and Metals Corp
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Publication of WO2016129361A1 publication Critical patent/WO2016129361A1/fr
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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
    • H01M4/36—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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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
    • H01M4/36—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
    • H01M4/52—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
    • 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 positive electrode active material for a lithium ion battery, a positive electrode for a lithium ion battery, a lithium ion battery, and a method for producing a positive electrode active material for a lithium ion battery.
  • Lithium-containing transition metal oxides are generally used as positive electrode active materials for lithium ion batteries. Specifically, lithium cobaltate (LiCoO 2 ), lithium nickelate (LiNiO 2 ), lithium manganate (LiMn 2 O 4 ), etc., improved characteristics (higher capacity, cycle characteristics, storage characteristics, reduced internal resistance) In order to improve the rate characteristics and safety, it is underway to combine them. Lithium ion batteries for large-scale applications such as in-vehicle use and load leveling are required to have different characteristics from those of conventional mobile phones and personal computers.
  • Patent Document 1 discloses lithium composite oxide particles containing one or more transition metal elements of Ni, Mn, and Co and lithium, and the particle strength of one lithium composite oxide particle is 20 to 200 MPa.
  • a positive electrode active material is disclosed. And according to this, it is described that by increasing the output of the battery, it is possible to prevent cracking during electrode preparation and to prevent a decrease in electronic conductivity by improving the particle strength.
  • Patent Document 2 discloses a monolithic primary particle powdery lithium composite oxide mainly composed of one element selected from the group consisting of Co, Ni and Mn and lithium. And according to this, it describes that by making the positive electrode primary particles, cracking during pressing and charging / discharging is suppressed and cycle characteristics and load characteristics are improved.
  • Patent Document 3 discloses a positive electrode active material for a lithium secondary battery including voids having an average diameter of 10 to 60 nm and a porosity of 0.5 to 20%. And according to this, it is described that the particle strength is increased to prevent cracking and the thermal stability with the electrolytic solution can be improved.
  • positive electrode active materials have been researched and developed from various viewpoints, but there is still room for improvement in conventional positive electrode active materials from the viewpoint of improving battery characteristics.
  • This invention makes it a subject to provide the positive electrode active material for lithium ion batteries with favorable battery characteristics.
  • the inventor of the present invention relates to an average particle diameter D50, a particle strength, and a predetermined particle diameter in a positive electrode active material for a lithium ion battery having a predetermined composition. It has been found that a positive electrode active material for a lithium ion battery with good battery characteristics can be obtained by controlling the average porosity inside the particles.
  • the present invention in one aspect been completed on the basis of the above findings, the composition formula: in Li x Ni 1- (y + z ) Mn y Co z O 2 + ⁇ ( Formula, 0.9 ⁇ x ⁇ 1.2 And 0 ⁇ y + z ⁇ 0.3 and ⁇ 0.1 ⁇ ⁇ ⁇ 0.1.),
  • the average particle diameter D50 is 5 to 7 ⁇ m, and the particle strength is 60 MPa or more.
  • the ratio of the number of primary particles to the secondary particles is 40 to 75%.
  • the positive electrode active material for a lithium ion battery of the present invention has a specific surface area of 0.6 m 2 / g or less.
  • the present invention provides a positive electrode for a lithium ion battery using the positive electrode active material for a lithium ion battery of the present invention.
  • the present invention is a lithium ion battery using the positive electrode for a lithium ion battery of the present invention.
  • a step of adding a metal salt solution containing Ni, Mn and Co to a suspension in which a lithium salt is dispersed to obtain a lithium metal salt solution slurry, and the lithium metal salt A step of obtaining a positive electrode active material precursor powder which is a lithium metal salt composite by drying the solution slurry; and a step of firing the positive electrode active material precursor powder at a temperature rising rate of 200 ° C./h or more.
  • the method for producing a positive electrode active material for a lithium ion battery according to the present invention includes a step of crushing the fired powder with a pulverizer at a rotational speed of 5000 rpm or more for both the classification rotor and the grinding rotor.
  • the rotational speeds of the classification rotor and the grinding rotor of the pulverizer are both 5500 to 6500 rpm.
  • FIG. 2 is an electron microscopic observation photograph of the particle surface of Example 1.
  • FIG. 4 is an electron microscope observation photograph of the particle surface of Example 2.
  • FIG. 2 is an electron microscope observation photograph of the particle surface of Comparative Example 1.
  • 6 is an electron microscopic observation photograph of the particle surface of Comparative Example 2.
  • the positive electrode active material for a lithium ion battery of the present invention is Composition formula: in Li x Ni 1- (y + z ) Mn y Co z O 2 + ⁇ ( wherein, a 0.9 ⁇ x ⁇ 1.2, is 0 ⁇ y + z ⁇ 0.3, -0 1 ⁇ ⁇ ⁇ 0.1.)
  • the ratio of lithium to all metals in the positive electrode active material for a lithium ion battery is 0.9 to 1.2. When the ratio is less than 0.9, it is difficult to maintain a stable crystal structure. This is because the high capacity cannot be secured.
  • the composition of nickel in the positive electrode active material for lithium ion batteries is 0.7 or more and less than 1.0, the capacity, output, and safety of the lithium ion battery using the positive electrode active material for lithium ion batteries are Improve balance.
  • the composition of nickel in the positive electrode active material for a lithium ion battery is preferably 0.8 or more and less than 1.0, more preferably 0.9 or more and less than 1.0.
  • the composition of O (oxygen) in the positive electrode active material for a lithium ion battery is “O 2 + ⁇ ” ( ⁇ 0.1 ⁇ ⁇ ⁇ 0.1).
  • the value of ⁇ can be adjusted by oxygen deficiency due to the firing atmosphere, introduction of blown oxygen gas, or the like.
  • the positive electrode active material for a lithium ion battery of the present invention is composed of secondary particles formed by aggregation of primary particles, or a mixture of primary particles and secondary particles.
  • the average particle diameter D50 of secondary particles formed by aggregation of these primary particles or a mixture of primary particles and secondary particles is 5 to 7 ⁇ m.
  • the particle diameter D50 can be a 50% diameter in the particle size distribution measured with Microtrack MT3000EX II manufactured by Nikkiso Co., Ltd.
  • D50 represents the particle size at which the cumulative curve becomes 50% when the cumulative curve is obtained with the total volume of a certain powder group as 100%.
  • the positive electrode active material for a lithium ion battery of the present invention has a particle strength of 60 MPa or more. With such a configuration, cracking of particles due to pressing during electrode fabrication and cracking of particles during charging and discharging are reduced, thereby reducing DC resistance during cycling and improving life characteristics.
  • the particle strength is preferably 80 MPa or more, more preferably 100 MPa or more, and typically 60 to 150 MPa. The particle strength can be measured, for example, with a micro compression tester MCT-211 manufactured by Shimadzu Corporation.
  • the measurement is performed by placing a powder sample dispersed on a sample stage, aiming at the center of one secondary particle having an average particle diameter of D50 with a microscope, pressing an indenter with a diameter of 20 ⁇ m at a load speed of 0.532 mN / sec, and breaking.
  • the average porosity inside the particles having a particle diameter of 3 ⁇ m or more is 5% or less.
  • the particles having a particle diameter of 3 ⁇ m or more are secondary particles in which primary particles are aggregated, and by controlling the average void ratio inside the particles to 5% or less, it is possible to press the electrodes at the time of electrode preparation. Since the cracking of particles and the cracking of particles during charging and discharging are further reduced, the direct current resistance during cycling is further reduced, and the life characteristics are further improved.
  • the average porosity inside the particles having a particle diameter of 3 ⁇ m or more is preferably 3% or less, more preferably 1% or less, and typically 1 to 5%.
  • the said average porosity is about the porosity inside a particle
  • the porosity inside the particle is the ratio of the area of the void inside the particle to the area of the particle having a particle diameter of 3 ⁇ m or more. Then, these observations are performed for 10 observation fields for one sample, the average value thereof is calculated, and this is set as the average porosity inside the particles.
  • Patent Document 3 Japanese Patent Laid-Open No. 2012-4109 discloses the idea that the positive electrode active material affects the battery characteristics by controlling the porosity.
  • Patent Document 3 it is the idea about the porosity in the whole positive electrode active material.
  • particles having a particle diameter of 3 ⁇ m or more are further controlled to improve battery characteristics by controlling the porosity inside the particles. It has been found that it has a big influence.
  • the average particle diameter D50 is preferably controlled to 5 to 7 ⁇ m, and the ratio of the number of primary particles in the secondary particles is preferably controlled to 40 to 75%.
  • the particles constituting the positive electrode active material are in a state closer to a single particle, and particle cracking due to pressing during electrode production and particle cracking during charge and discharge are further reduced, thereby reducing the cycle time.
  • the direct current resistance is further reduced, and the life characteristics are further improved.
  • the ratio of the number of primary particles in the secondary particles is more preferably controlled to 50 to 75%, and more preferably 60 to 75%.
  • the ratio of the number of primary particles and secondary particles is evaluated as follows. First, 30 secondary particles are selected at random in an observation photograph taken with an electron microscope in which a sample powder is embedded in a resin and photographed multiple times in an observation field of 50 ⁇ m ⁇ 70 ⁇ m.
  • the secondary particles are defined as one gray lump separated by black as a resin portion, for example, as in the SEM image of FIG.
  • the positive electrode active material for a lithium ion battery of the present invention preferably has a specific surface area of 0.6 m 2 / g or less. When the specific surface area exceeds 0.6 m 2 / g, the surface resistance may increase and the cycle characteristics may deteriorate.
  • the specific surface area is preferably 0.5 m 2 / g or less, more preferably 0.45 m 2 / g or less, and typically 0.45 to 0.6 m 2 / g.
  • the positive electrode for a lithium ion battery comprises, for example, a positive electrode mixture prepared by mixing a positive electrode active material for a lithium ion battery having the above-described configuration, a conductive material, and a binder, such as an aluminum foil. It has a structure provided on one side or both sides of the current collector. Moreover, the lithium ion battery which concerns on embodiment of this invention is equipped with the positive electrode for lithium ion batteries of such a structure.
  • a metal salt solution is prepared.
  • the metals are Ni, Mn and Co.
  • the metal salt is sulfate, chloride, nitrate, acetate, etc., and nitrate is particularly preferable. This is because even if it is mixed as an impurity in the firing raw material, it can be fired as it is, so that the washing step can be omitted, and nitrate functions as an oxidant, and promotes the oxidation of the metal in the firing raw material.
  • Each metal contained in the metal salt is adjusted so as to have a desired molar ratio. Thereby, the molar ratio of each metal in the positive electrode active material is determined.
  • a suspension in which lithium carbonate is dispersed in pure water is prepared, and then the metal salt solution of the metal is added to prepare a metal carbonate solution slurry.
  • fine particles of lithium-containing carbonate precipitate in the slurry.
  • the lithium compound does not react during heat treatment such as sulfate or chloride as a metal salt, it is washed with a saturated lithium carbonate solution and then filtered off.
  • the lithium compound reacts as a lithium raw material during the heat treatment, such as nitrate or acetate, it can be used as a calcined precursor by washing and drying as it is without washing.
  • the lithium-containing carbonate separated by filtration is dried to obtain a powder of a lithium metal salt complex (a precursor for a lithium ion battery positive electrode material).
  • a firing container having a predetermined capacity is prepared, and this firing container is filled with a precursor powder for a lithium ion battery positive electrode material.
  • the surface structure of the positive electrode active material is controlled by moving the firing container filled with the precursor powder for the lithium ion battery positive electrode material to a firing furnace and firing at a temperature rising rate of 200 ° C./h or more. .
  • voids (pores) in the positive electrode active material are reduced, and the particle strength is improved. That is, when a composite oxide such as nitrate is used as a precursor, pores are included in the particles due to NO x volatilization during firing.
  • nuclei are formed from the surface of the particles when the precursor becomes a ternary positive electrode active material.
  • the heating rate during firing is less than 200 ° C./h, the escape of gas components is worsened by the nuclei formed on the surface, but in the present invention, the temperature rate is 200 ° C./h or more, so Before the nucleation of the gas ends, gas generation occurs, and pores due to the contained gas are reduced.
  • the heating rate is preferably 250 ° C./h or more, and typically 200 to 300 ° C./h.
  • both the classification rotor and the grinding rotor are pulverized at a rotational speed of 5000 rpm or more by the pulverizer, so that the powder becomes a state close to primary particles, and the average voids inside the particles having an average particle diameter D50 and a particle diameter of 3 ⁇ m or more.
  • the volume ratio of the primary particles to the secondary particles can be controlled. This also eliminates the encapsulated pores and further increases the particle strength.
  • the rotational speeds of the classification rotor and the grinding rotor of the pulverizer are both preferably 5500 to 6500 rpm, and more preferably both 6000 to 6500 rpm.
  • Examples 1 to 8 First, nitrates adjusted so that each metal contained in the metal salt had a molar ratio shown in Table 1 were prepared. Next, after suspending lithium carbonate in pure water, this metal salt solution was added. By this treatment, fine particles of lithium-containing carbonate were precipitated in the solution, and this precipitate was filtered off using a filter press. Subsequently, the precipitate was dried to obtain a lithium-containing carbonate (a precursor for a lithium ion battery positive electrode material). Next, a firing container was prepared, and this firing container was filled with a lithium-containing carbonate. Next, after baking the baking container on the baking conditions of Table 1 under atmospheric pressure, it cooled and the oxide was obtained.
  • this metal salt solution was added. By this treatment, fine particles of lithium-containing carbonate were precipitated in the solution, and this precipitate was filtered off using a filter press. Subsequently, the precipitate was dried to obtain a lithium-containing carbonate (a precursor for a lithium ion battery positive electrode material). Next,
  • the obtained oxide was pulverized by using a pulverizer manufactured by Hosokawa Micron Corporation with the classification rotor and the pulverization rotor set to the pulverization rotation speeds shown in Table 1 to obtain a lithium ion secondary battery positive electrode material.
  • a pulverizer manufactured by Hosokawa Micron Corporation with the classification rotor and the pulverization rotor set to the pulverization rotation speeds shown in Table 1 to obtain a lithium ion secondary battery positive electrode material.
  • the raw material charged into the pulverizer is first crushed by a rotating crushing rotor. Thereafter, the finely divided raw material powder is collected through the gaps of the classification rotor, and the large and heavy raw material powder is pulverized by the crushing rotor that rotates again without passing through the classification rotor.
  • the adjustment of the rotational speeds of the two rotors is a condition for efficiently recovering the powder crushed to a desired particle size.
  • Comparative Examples 1 to 7 As Comparative Examples 1 to 7, each metal contained in the metal salt had a composition as shown in Table 1, and the same treatment as in Examples 1 to 8 was performed except for the firing conditions and the crushing conditions.
  • the average particle diameter D50 was a 50% diameter in the particle size distribution measured with Microtrack MT3000EX II manufactured by Nikkiso Co., Ltd.
  • the average particle diameter D50 is 5 to 7 ⁇ m, the particle strength is 60 MPa or more, and the average porosity inside the particles having a particle diameter of 3 ⁇ m or more is 5% or less.
  • the discharge capacity was good.
  • the average particle diameter D50 is outside the range of 5 to 7 ⁇ m, the particle strength is less than 60 MPa, and the average porosity inside the particles having a particle diameter of 3 ⁇ m or more is more than 5%.
  • the cycle characteristics were poor.
  • the average particle diameter D50 was outside the range of 5 to 7 ⁇ m, the average porosity inside the particles having a particle diameter of 3 ⁇ m or more was more than 5%, and both the cycle characteristics and the discharge capacity were poor. It was.
  • FIG. 1 shows an electron microscope observation photograph of the particle surface of Example 1.
  • FIG. 2 the electron microscope observation photograph of the particle
  • FIG. 3 the electron microscope observation photograph of the particle
  • FIG. 4 the electron microscope observation photograph of the particle

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)
  • Secondary Cells (AREA)

Abstract

L'invention concerne un matériau actif d'électrode positive pour une pile au lithium-ion ayant d'excellentes caractéristiques de cellule. L'invention concerne un matériau actif d'électrode positive pour une pile au lithium-ion, le matériau actif d'électrode positive étant représenté par la formule de composition LixNi1 - (y + z)MnyCozO2 + α (dans la formule, 0,9 ≤ x ≤ 1,2, 0 < y + z ≤ 0,3, -0,1 ≤ α ≤ 0,1), le diamètre de particule moyen D50 faisant 5-7 μm, la résistance de particule étant de 60 MPa ou plus, et la porosité moyenne dans l'intérieur de particules ayant un diamètre de particule de 3 µm ou plus étant de 5 % ou moins.
PCT/JP2016/051889 2015-02-12 2016-01-22 Matériau actif d'électrode positive pour pile au lithium-ion, électrode positive pour pile au lithium-ion, pile au lithium-ion, et procédé de fabrication de matériau actif d'électrode positive pour pile au lithium-ion Ceased WO2016129361A1 (fr)

Applications Claiming Priority (2)

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JP2015025702A JP6407754B2 (ja) 2015-02-12 2015-02-12 リチウムイオン電池用正極活物質、リチウムイオン電池用正極、リチウムイオン電池、及び、リチウムイオン電池用正極活物質の製造方法
JP2015-025702 2015-02-12

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WO2019098384A1 (fr) * 2017-11-20 2019-05-23 住友化学株式会社 Matériau actif d'électrode positive pour batterie secondaire au lithium, électrode positive pour batterie secondaire au lithium et batterie secondaire au lithium
WO2019177032A1 (fr) * 2018-03-13 2019-09-19 住友化学株式会社 Poudre d'oxyde composite de métal au lithium, matière active d'électrode positive pour batterie secondaire au lithium, électrode positive, et batterie secondaire au lithium
WO2019177014A1 (fr) * 2018-03-13 2019-09-19 住友化学株式会社 Poudre d'oxyde composite de métal au lithium, matière active d'électrode positive pour batterie secondaire au lithium, électrode positive, et batterie secondaire au lithium
WO2020059471A1 (fr) * 2018-09-21 2020-03-26 株式会社田中化学研究所 Matériau actif d'électrode positive pour accumulateur et procédé destiné à le produire
JP2020053386A (ja) * 2018-09-21 2020-04-02 株式会社田中化学研究所 二次電池用正極活物質及びその製造方法
JP2020083750A (ja) * 2019-10-07 2020-06-04 住友化学株式会社 リチウム金属複合酸化物粉末、リチウム二次電池用正極活物質、正極、及びリチウム二次電池
JP2020087879A (ja) * 2018-11-30 2020-06-04 住友化学株式会社 リチウム金属複合酸化物粉末、リチウム二次電池用正極活物質、正極、及びリチウム二次電池
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JP2023091568A (ja) * 2021-12-20 2023-06-30 プライムプラネットエナジー＆ソリューションズ株式会社 正極活物質、およびこれを用いた非水電解質二次電池

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JP6587044B1 (ja) 2017-12-27 2019-10-09 日立金属株式会社 リチウムイオン二次電池用正極活物質及びリチウムイオン二次電池用正極活物質の製造方法、並びにリチウムイオン二次電池
JP7198170B2 (ja) * 2019-07-30 2022-12-28 Ｊｘ金属株式会社 全固体リチウムイオン電池用正極活物質、全固体リチウムイオン電池用正極活物質の製造方法及び全固体リチウムイオン電池
JP7366487B2 (ja) 2020-06-15 2023-10-23 エルジー・ケム・リミテッド 正極活物質の製造方法
WO2022019273A1 (fr) * 2020-07-21 2022-01-27 住友金属鉱山株式会社 Méthode de production d'hydroxyde contenant du nickel, méthode de production de matériau actif d'électrode positive pour batteries secondaires au lithium-ion, matériau actif d'électrode positive pour batteries secondaires au lithium-ion et batterie secondaire au lithium-ion
WO2022060207A1 (fr) * 2020-09-21 2022-03-24 주식회사 엘지화학 Matériau actif d'électrode positive fabriqué par synthése en phase solide, et son procédé de fabrication
KR102558390B1 (ko) * 2020-10-26 2023-07-24 주식회사 에코프로비엠 양극 활물질 및 이를 포함하는 리튬 이차전지
CN118221179B (zh) * 2024-05-24 2024-09-10 广东邦普循环科技有限公司 三元正极材料前驱体、制备方法及应用

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CN113165907A (zh) * 2018-11-30 2021-07-23 住友化学株式会社 锂金属复合氧化物、锂二次电池用正极活性物质、正极以及锂二次电池
KR20210095149A (ko) * 2018-11-30 2021-07-30 스미또모 가가꾸 가부시끼가이샤 리튬 금속 복합 산화물, 리튬 이차 전지용 정극 활물질, 정극, 및 리튬 이차 전지
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JP7222866B2 (ja) 2019-10-07 2023-02-15 住友化学株式会社 リチウム金属複合酸化物粉末、リチウム二次電池用正極活物質、正極、及びリチウム二次電池
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