WO2012128289A1 - Matériau actif d'électrode positive pour batterie à lithium-ion, électrode positive pour batterie à lithium-ion, et batterie à lithium-ion - Google Patents

Matériau actif d'électrode positive pour batterie à lithium-ion, électrode positive pour batterie à lithium-ion, et batterie à lithium-ion Download PDF

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Publication number
WO2012128289A1
WO2012128289A1 PCT/JP2012/057209 JP2012057209W WO2012128289A1 WO 2012128289 A1 WO2012128289 A1 WO 2012128289A1 JP 2012057209 W JP2012057209 W JP 2012057209W WO 2012128289 A1 WO2012128289 A1 WO 2012128289A1
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Prior art keywords
positive electrode
lithium
ion battery
electrode active
lithium ion
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PCT/JP2012/057209
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English (en)
Japanese (ja)
Inventor
健太郎 岡本
梶谷　芳男
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Jx日鉱日石金属株式会社
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Priority to JP2013505989A priority Critical patent/JP6026404B2/ja
Publication of WO2012128289A1 publication Critical patent/WO2012128289A1/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
    • H01M4/52—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
    • 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
    • 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, and 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: Li x Ni 1- y My O 2- ⁇ (0.8 ⁇ x ⁇ 1.3, 0 ⁇ y ⁇ 0.5, and M is Co, Mn, Fe, Cr, V, Ti, Cu, Al, Ga, Bi, Sn, Zn, Mg, It represents at least one element selected from the group consisting of Ge, Nb, Ta, Be, B, Ca, Sc and Zr, ⁇ corresponds to oxygen deficiency or oxygen excess, ⁇ 0.1 ⁇ ⁇ 0.1
  • a method for producing a positive electrode material for a lithium secondary battery characterized in that small substances are blended at a weight ratio of 0: 100 to 100: 0. And according to this, it is described that the positive electrode material for lithium secondary batteries with various balance of rate characteristics and capacity can be easily manufactured.
  • Patent Document 1 Although the lithium nickel composite oxide described in Patent Document 1 has an excessive amount of oxygen in its composition formula, there is still room for improvement as a high-quality positive electrode active material for lithium ion batteries.
  • an object of the present invention is to provide a positive electrode active material for a lithium ion battery having good battery characteristics.
  • the present inventor has found that there is a close correlation between the amount of oxygen of the positive electrode active material, the particle size of the primary particles, and the battery characteristics. That is, it has been found that good battery characteristics can be obtained by setting the positive electrode active material oxygen amount to a certain value or more and controlling the primary particle size of the positive electrode active material within an appropriate range. Further, the present inventors have found that there is a close correlation between the carbon content of the positive electrode active material and the amount of lithium carbonate that is residual alkali on the particle surface of the positive electrode active material, and the battery characteristics. That is, it has been found that particularly good battery characteristics can be obtained when the carbon content of the positive electrode active material is below a certain value or when the amount of lithium carbonate on the particle surface of the positive electrode active material is below a certain value.
  • Composition formula Li (Li x Ni 1- xy M y) O 2 + ⁇
  • M is at least one selected from Sc, Ti, V, Cr, Mn, Fe, Co, Cu, Zn, Ga, Ge, Bi, Sn, Mg, Ca, B and Zr; (0 ⁇ x ⁇ 0.1, 0 ⁇ y ⁇ 0.7, and ⁇ > 0)
  • the particle size of the primary particles is 1.6 to 2.3 ⁇ m
  • the carbon amount measured by the LECO method is 0.40% by mass or less
  • the positive electrode active material for a lithium ion battery according to the present invention has a carbon content of 0.20% by mass or less as measured by LECO method, and is a carbonic acid that is residual alkali on the particle surface as measured by neutralization titration.
  • the amount of lithium is 0.60 mass% or less.
  • the positive electrode active material for a lithium ion battery according to the present invention is at least one selected from Mn and Co.
  • the positive electrode active material for a lithium ion battery according to the present invention has ⁇ > 0.05 in the composition formula.
  • the positive electrode active material for a lithium ion battery according to the present invention has ⁇ > 0.1 in the composition formula.
  • the present invention is a positive electrode for a lithium ion battery using the positive electrode active material for a lithium ion battery according to the present invention.
  • the present invention is a lithium ion battery using the positive electrode for a lithium ion battery according to the present invention.
  • a positive electrode active material for a lithium ion battery having good battery characteristics can be provided.
  • FIG. 1 is an appearance photograph of primary particles and secondary particles of a positive electrode active material.
  • lithium cobaltate LiCoO 2
  • lithium-containing transition metal oxides such as lithium nickelate (LiNiO 2 ) and lithium manganate (LiMn 2 O 4 ).
  • the positive electrode active material for a lithium ion battery of the present invention produced using such a material is Composition formula: Li (Li x Ni 1- xy M y) O 2 + ⁇
  • M is at least one selected from Sc, Ti, V, Cr, Mn, Fe, Co, Cu, Zn, Ga, Ge, Bi, Sn, Mg, Ca, B and Zr; (0 ⁇ x ⁇ 0.1, 0 ⁇ y ⁇ 0.7, and ⁇ > 0) It is represented by
  • oxygen is expressed as O 2 + ⁇ ( ⁇ > 0) as described above in the composition formula, and is excessively contained. Battery characteristics such as rate characteristics and capacity retention are improved.
  • ⁇ is preferably ⁇ > 0.05, and more preferably ⁇ > 0.1.
  • the positive electrode active material for lithium ion batteries is composed of primary particles, secondary particles formed by aggregation of primary particles, or a mixture of primary particles and secondary particles (see FIG. 1).
  • the primary particles have a particle size of 1.6 to 2.3 ⁇ m.
  • the particle size of the primary particles is less than 1.6 ⁇ m, there arises a problem that the particles are cracked by a press during battery production or are deteriorated due to particle cracks during battery cycle.
  • the particle size of the primary particles is more than 2.3 ⁇ m, there is a problem of battery deterioration due to the withering of the electrolytic solution or increasing the amount of the electrolytic solution.
  • the particle size of the primary particles is preferably 1.8 to 2.1 ⁇ m.
  • the positive electrode active material for a lithium ion battery of the present invention has a carbon content measured by the LECO method of 0.40% by mass or less.
  • the LECO method is an inert gas melting-infrared absorption method, and is defined in, for example, JIS R 1603.
  • the amount of carbon measured by the LECO method is preferably 0.30% by mass or less, more preferably 0.20% by mass or less.
  • the carbon contained in the positive electrode material does not exist alone in the inside or on the surface of the positive electrode material, but is present as lithium carbonate (Li 2 CO 3 ).
  • Lithium carbonate is a weak alkali and lowers battery characteristics, so it is better that the residual alkali is less.
  • “the amount of carbon contained in the positive electrode active material” indicates the amount of carbon contained in the form of lithium carbonate (Li 2 CO 3 ) in the positive electrode material, and if this amount is small ( If it is 0.40 mass% or less), battery characteristics are good.
  • the amount of lithium carbonate that is residual alkali on the particle surface measured by neutralization titration is 0.70% by mass or less.
  • Neutralization titration is performed using a normal neutralization titration method using hydrochloric acid or the like as a titrant. If the amount of lithium carbonate, which is residual alkali on the particle surface, is more than 0.7% by mass, it reacts with the electrolyte solution during repeated charge and discharge, resulting in deterioration and poor battery characteristics. Moreover, when there is much alkali, gas generation
  • the amount of lithium carbonate that is residual alkali on the particle surface measured by neutralization titration is preferably 0.60% by mass or less, more preferably 0.55% by mass or less.
  • the positive electrode active material for a lithium ion battery is composed of primary particles, secondary particles formed by aggregation of primary particles, or a mixture of primary particles and secondary particles.
  • the positive electrode active material for a lithium ion battery preferably has an average particle diameter of primary particles or secondary particles of 2 to 15 ⁇ m. When the average particle size is less than 2 ⁇ m, it becomes difficult to apply to the current collector. When the average particle size is more than 15 ⁇ m, voids are likely to occur during filling, and the filling property is lowered.
  • the average particle size is more preferably 3 to 10 ⁇ m.
  • the positive electrode for a lithium ion battery includes, 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 additive, and a binder from an aluminum foil or the like.
  • the current collector has a structure provided on one side or both sides.
  • 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 metal is at least one selected from Ni and Sc, Ti, V, Cr, Mn, Fe, Co, Cu, Zn, Ga, Ge, Bi, Sn, Mg, Ca, B, and Zr.
  • the metal salt is sulfate, chloride, nitrate, acetate, etc., and nitrate is particularly preferable.
  • 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.
  • lithium carbonate is suspended in pure water, and then the metal salt solution of the metal is added to prepare a metal carbonate solution slurry. At this time, fine particles of lithium-containing carbonate precipitate in the slurry. At this time, stirring is performed in order to mix the lithium carbonate and the metal salt solution. However, the more the stirring is performed, the smaller the particles of the slurry that are generated, and the more uniform and better the reaction proceeds. The amount of lithium carbonate can be reduced, whereby the carbon content in the lithium salt composite (precursor for lithium ion battery positive electrode material) produced can be suppressed. As a stirring condition, the solution is stirred at a rotation speed of about 250 rpm using a stirring blade having a predetermined size.
  • the lithium compound does not react as a metal salt during heat treatment such as sulfate or chloride, the salt is washed with a saturated lithium carbonate solution and then filtered off.
  • a saturated lithium carbonate solution When 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. Next, the lithium-containing carbonate separated by filtration is dried to obtain a lithium salt composite (precursor for lithium ion battery positive electrode material) powder.
  • 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 firing container filled with the precursor powder for the lithium ion battery positive electrode material is transferred to a firing furnace and fired. Firing is performed by heating and holding in an oxygen atmosphere for a predetermined time. Further, it is preferable to perform baking under a pressure of 101 to 202 KPa because the amount of oxygen in the composition further increases.
  • the heating and holding temperature in the firing step affects the primary particle size of the lithium ion battery positive electrode material.
  • the reactivity is weak compared with the case where lithium hydroxide is used as a raw material.
  • the particle size of the primary particles is controlled to 1.6 to 2.3 ⁇ m.
  • the firing temperature is lowered because the reactivity is high, and the firing time is reduced. Therefore, the primary particle size to be generated is as small as about 0.5 ⁇ m. End up.
  • the powder is taken out from the firing container and pulverized using a commercially available pulverizer or the like to obtain a positive electrode active material powder.
  • the crushing at this time is performed by appropriately adjusting the crushing strength and crushing time so that fine powder is not generated as much as possible.
  • D90 the particle diameter ( ⁇ m) at the point where the cumulative curve becomes 90%
  • D10 the particle diameter ( ⁇ m) at the point where the cumulative curve becomes 10% by the crushing
  • (D90 ⁇ D10) / 2 is adjusted to 8 ⁇ m or less. Further, it is more preferable to adjust so that (D90-D10) / 2 is 6 ⁇ m or less.
  • Examples 1 to 14 First, after suspending lithium carbonate of the input amount shown in Table 1 in 3.2 liters of pure water, 4.8 liter of metal salt solution was charged. Here, the nitrate hydrate of each metal was adjusted so that each metal might become the composition ratio of Table 1, and the total metal mole number might be set to 14 mol. Stirring was performed using a stirrer equipped with stirring blades at a rotational speed of 250 rpm. Incidentally, a suspension of lithium carbonate, the product (lithium ion secondary battery positive electrode material, i.e.
  • A is 0.9 when lithium salt reacts as a firing raw material such as nitrate or acetate, and “1” when lithium salt does not react as a firing raw material such as sulfate or chloride. 0.
  • 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).
  • a firing container was prepared, and this firing container was filled with a lithium-containing carbonate. Next, the firing container was placed in an oxygen atmosphere furnace under atmospheric pressure, heated and held at the firing temperature shown in Table 1 for 10 hours, and then cooled to obtain an oxide.
  • the obtained oxide is crushed so that the fine powder having a predetermined particle size has a predetermined particle size distribution width, and a lithium ion secondary battery is obtained.
  • a positive electrode powder was obtained.
  • Example 15 Example 15 was carried out except that each material of the raw material had the composition shown in Table 1, the metal salt was chloride, the lithium-containing carbonate was precipitated, washed with a saturated lithium carbonate solution, and filtered. The same treatment as in Examples 1 to 14 was performed.
  • Example 16 Example 16 was carried out except that each metal of the raw material had a composition as shown in Table 1, the metal salt was a sulfate, a lithium-containing carbonate was precipitated, washed with a saturated lithium carbonate solution, and filtered. The same treatment as in Examples 1 to 14 was performed.
  • Example 17 As Example 17, the same processing as in Examples 1 to 14 was performed, except that each metal of the raw material had a composition as shown in Table 1 and firing was performed under a pressure of 120 KPa instead of atmospheric pressure.
  • each metal of the raw material has a composition as shown in Table 1, the stirring condition in the reaction between lithium carbonate and the metal salt solution is 150 rpm, and the final oxide is crushed. The same processing as in Examples 1 to 14 was performed except that the adjustment as in Examples 1 to 14 was not performed.
  • Comparative Examples 4 to 5 As Comparative Examples 4 to 5, the same processing as in Comparative Example 1 was performed except that each metal of the raw material had a composition as shown in Table 1 and the firing process was performed in an air atmosphere furnace instead of an oxygen atmosphere furnace.
  • the amount of carbon in the positive electrode material was measured by the LECO method based on the provisions of JIS G1211, JIS G1215. That is, 0.1 to 0.3 g of powder of each positive electrode material was sampled, 2 g of an auxiliary combustion material not containing carbon was added and placed in a ceramic crucible, and then burned in a high frequency melting furnace. The amount of carbon was determined by detecting and quantifying the components during combustion with an infrared detector.
  • Each positive electrode material, conductive material, and binder are weighed in a ratio of 85: 8: 7, and the positive electrode material and the conductive material are mixed into a slurry in which the binder is dissolved in an organic solvent (N-methylpyrrolidone). And coated on an Al foil, dried and pressed to obtain a positive electrode. Subsequently, a 2032 type coin cell for evaluation with Li as the counter electrode was prepared, and 1M-LiPF 6 dissolved in EC-DMC (1: 1) was used as the electrolyte, and the current density was 0.2C. The discharge capacity was measured.
  • Examples 1 to 17 all had good battery characteristics. In addition, Examples 1 to 14 and 17 in which the metal salt of the raw material was nitrate had particularly good battery characteristics. Further, Example 17 in which the firing was performed under pressure rather than atmospheric pressure had the best battery characteristics. In Comparative Examples 1 to 3, the composition of the metal used as the raw material was excessive oxygen as in the present invention, but the battery characteristics were poor due to the stirring conditions and crushing conditions. . In Comparative Examples 4 to 5, the composition of the metal used as the raw material was outside the scope of the present invention, and the battery characteristics were poor due to the stirring conditions and the crushing conditions.

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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)

Abstract

L'invention concerne un matériau actif d'électrode positive pour une batterie à lithium-ion qui présente d'excellentes caractéristiques de batterie. Le matériau actif d'électrode positive pour la batterie à lithium-ion est représenté par la formule de composition Li (Lix Ni1-x-y My) O2+α (dans la formule, M est un ou plusieurs des éléments sélectionnés parmi : Sc, Ti, V, Cr, Mn, Fe, Co, Cu, Zn, Ga, Ge, Bi, Sn, Mg, Ca, B et Zr, avec 0 ≤ x ≤ 0,1, 0 < y ≤ 0,7 et α > 0). La taille de particule primaire est de 1,6 à 2,3 µm, la teneur en carbone telle que mesurée par le procédé LECO est de 0,40 % en masse ou moins, et la teneur en carbonate de lithium qui est l'alcalin résiduel des surfaces de particules telle que mesurée par titrage par neutralisation est de 0,70 % en masse ou moins.
PCT/JP2012/057209 2011-03-24 2012-03-21 Matériau actif d'électrode positive pour batterie à lithium-ion, électrode positive pour batterie à lithium-ion, et batterie à lithium-ion WO2012128289A1 (fr)

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Cited By (4)

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JP2016072071A (ja) * 2014-09-30 2016-05-09 住友金属鉱山株式会社 非水系電解質二次電池用正極活物質、その製造に用いられる分散液及びそれらの製造方法
JP2016072072A (ja) * 2014-09-30 2016-05-09 住友金属鉱山株式会社 非水系電解質二次電池用正極活物質の製造方法、および該非水系電解質二次電池用正極活物質
CN108956850A (zh) * 2017-05-17 2018-12-07 北大先行科技产业有限公司 一种快速评价三元正极材料表面残碱相对含量的检测方法
CN110233244A (zh) * 2019-06-28 2019-09-13 北京科技大学 一种高镍三元正极材料颗粒表面稳定化处理方法

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JP2003017054A (ja) * 2001-06-29 2003-01-17 Sony Corp 正極活物質及び非水電解質電池の製造方法
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2016072071A (ja) * 2014-09-30 2016-05-09 住友金属鉱山株式会社 非水系電解質二次電池用正極活物質、その製造に用いられる分散液及びそれらの製造方法
JP2016072072A (ja) * 2014-09-30 2016-05-09 住友金属鉱山株式会社 非水系電解質二次電池用正極活物質の製造方法、および該非水系電解質二次電池用正極活物質
CN108956850A (zh) * 2017-05-17 2018-12-07 北大先行科技产业有限公司 一种快速评价三元正极材料表面残碱相对含量的检测方法
CN110233244A (zh) * 2019-06-28 2019-09-13 北京科技大学 一种高镍三元正极材料颗粒表面稳定化处理方法

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