WO2020202745A1 - 非水電解質二次電池 - Google Patents

非水電解質二次電池 Download PDF

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Publication number
WO2020202745A1
WO2020202745A1 PCT/JP2020/002828 JP2020002828W WO2020202745A1 WO 2020202745 A1 WO2020202745 A1 WO 2020202745A1 JP 2020002828 W JP2020002828 W JP 2020002828W WO 2020202745 A1 WO2020202745 A1 WO 2020202745A1
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Prior art keywords
positive electrode
active material
electrode active
layer
aqueous electrolyte
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English (en)
French (fr)
Japanese (ja)
Inventor
貴志 神
鈴木　慎也
史治 新名
翔 鶴田
柳田　勝功
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Panasonic Intellectual Property Management Co Ltd
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Panasonic Intellectual Property Management Co Ltd
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Priority to CN202080018312.9A priority Critical patent/CN113519077B/zh
Priority to CN202411142629.XA priority patent/CN119133384A/zh
Priority to JP2021511149A priority patent/JP7523038B2/ja
Priority to US17/442,219 priority patent/US20220166007A1/en
Publication of WO2020202745A1 publication Critical patent/WO2020202745A1/ja
Anticipated expiration legal-status Critical
Priority to JP2024106638A priority patent/JP2024120970A/ja
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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
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0017—Non-aqueous electrolytes
    • H01M2300/0025—Organic electrolyte
    • 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 disclosure relates to a non-aqueous electrolyte secondary battery, and more particularly to a non-aqueous electrolyte secondary battery containing a lithium transition metal composite oxide as a positive electrode active material.
  • Patent Document 1 describes a compound of a predetermined element having a melting point of 750 ° C. or higher among the elements of Groups 4 to 6 on the particle surface of the lithium transition metal composite oxide (TiO 2, etc.).
  • Patent Document 2 it is produced by firing in a state where a boric acid compound is present on the particle surface of a lithium transition metal composite oxide, and the content of carbonate ion is 0.15% by weight or less and borate ion.
  • a positive electrode active material having a content of 0.01% by weight to 5.0% by weight is disclosed.
  • An object of the present disclosure is to provide a non-aqueous electrolyte secondary battery having a low initial resistance and capable of suppressing an increase in resistance during a high temperature cycle.
  • the non-aqueous electrolyte secondary battery is a non-aqueous electrolyte secondary battery including an electrode body including a positive electrode, a negative electrode, and a separator, and a non-aqueous electrolyte, and the positive electrode is at least positive electrode active. It has substance A.
  • the positive electrode active material A is a general formula Li a Ni b Co c Mn d Al e M f Og (in the formula, M is at least one element selected from groups 4, 5, and 6).
  • Li x M y O z (wherein, 1 ⁇ x ⁇ 4,1 ⁇ y ⁇ 5,1 ⁇ z ⁇ 12)
  • a first layer composed of the lithium metal compound and formed on the particle surface of the lithium transition metal composite oxide, and a second layer composed of the boron compound and formed on the first layer.
  • the first layer is formed on the particle surface of the lithium transition metal composite oxide over the entire area without interposing the second layer.
  • non-aqueous electrolyte secondary battery which is one aspect of the present disclosure, an increase in battery resistance during a high temperature cycle can be suppressed.
  • the particle surface of the lithium-transition metal composite oxide represented by the general formula Li x M y O represented by the presence of lithium metal compound in z is known to be reduced initial resistance of the battery. It is considered that the lithium metal compound functions as a lithium ion conductor and contributes to the reduction of the charge transfer resistance of the positive electrode. On the other hand, the presence of the lithium metal compound on the particle surface of the lithium transition metal composite oxide cannot suppress the increase in battery resistance during a high temperature cycle, and may rather increase the resistance.
  • the present inventors form a first layer composed of a lithium metal compound and a second layer composed of a boron compound and covering the first layer on the particle surface of the lithium transition metal composite oxide. Therefore, we succeeded in suppressing the increase in resistance during high-temperature cycles while reducing the initial resistance.
  • the presence of a second layer of boron compound covering the first layer forms a strong film containing M and boron on the particle surface of the positive electrode active material during the high temperature cycle, which causes the non-aqueous electrolyte in the positive electrode. It is considered that the side reaction and the elution of the metal in the positive electrode active material were suppressed, and the increase in battery resistance was suppressed.
  • the non-aqueous electrolyte secondary battery 10 in which the wound electrode body 14 is housed in the exterior body 11 made of a laminated sheet is illustrated, but the exterior body is not limited to this, and for example, a cylindrical shape, a square shape, and a coin. It may be an outer can of a shape or the like. Further, the electrode body may be a laminated electrode body in which a plurality of positive electrodes and a plurality of negative electrodes are alternately laminated via a separator.
  • FIG. 1 is a perspective view showing the appearance of the non-aqueous electrolyte secondary battery 10 which is an example of the embodiment.
  • the non-aqueous electrolyte secondary battery 10 includes an exterior body 11 composed of two laminated films 11A and 11B.
  • the non-aqueous electrolyte secondary battery 10 includes an electrode body 14 housed in the exterior body 11 and a non-aqueous electrolyte secondary battery 10.
  • the exterior body 11 has, for example, a substantially rectangular shape in a plan view, and includes a housing portion 12 in which an electrode body 14 and a non-aqueous electrolyte are housed, and a sealing portion 13 formed around the housing portion 12.
  • the laminated films 11A and 11B are generally composed of a resin film containing a metal layer such as aluminum.
  • the accommodating portion 12 can be provided by forming a recess capable of accommodating the electrode body 14 in at least one of the laminated films 11A and 11B.
  • the recess is formed only in the laminated film 11A.
  • the sealing portion 13 is formed by joining the peripheral portions of the laminated films 11A and 11B to each other.
  • the sealing portion 13 is formed in a frame shape having substantially the same width so as to surround the accommodating portion 12.
  • the non-aqueous electrolyte secondary battery 10 includes a pair of electrode leads (positive electrode lead 15 and negative electrode lead 16) connected to the electrode body 14.
  • the positive electrode lead 15 and the negative electrode lead 16 are pulled out from the same end portion of the exterior body 11 to the outside of the exterior body 11.
  • the non-aqueous electrolyte contains a non-aqueous solvent and an electrolyte salt dissolved in the non-aqueous solvent.
  • the non-aqueous solvent for example, esters, ethers, nitriles, amides, and a mixed solvent of two or more of these are used.
  • the non-aqueous solvent may contain a halogen substituent in which a part of hydrogen in these solvents is replaced with a halogen atom such as fluorine.
  • the non-aqueous electrolyte is not limited to the liquid electrolyte, and may be a solid electrolyte using a gel polymer or the like.
  • the electrolyte salt for example, a lithium salt such as LiPF 6 is used.
  • FIG. 2 is a perspective view of the electrode body 14 which is an example of the embodiment.
  • the electrode body 14 includes a positive electrode 20, a negative electrode 30, and a separator 40, and the positive electrode 20 and the negative electrode 30 are spirally wound through the separator 40 to form a flat winding. It is a revolving electrode body.
  • the positive electrode 20 has a positive electrode tab 21 in which a part of the electrode plate is a convex portion protruding in the axial direction of the electrode body 14.
  • the negative electrode 30 has a negative electrode tab 31 protruding in the same direction as the positive electrode tab 21.
  • a plurality of positive electrode tabs 21 and negative electrode tabs 31 are formed at regular intervals in the longitudinal direction of each electrode plate.
  • the electrode body 14 is formed by superimposing and winding the positive electrode 20 and the negative electrode 30 via the separator 40 so that the positive electrode tab 21 and the negative electrode tab 31 are alternately arranged in the longitudinal direction of the electrode plate.
  • the positive electrode tabs 21 and the negative electrode tabs 31 overlap each other, and the positive electrode tab laminated portion 22 is formed at one end in the width direction of the electrode body 14, and the negative electrode tab laminated portion 32 is formed at the other end in the width direction.
  • the positive electrode lead 15 is welded to the positive electrode tab laminated portion 22, and the negative electrode lead 16 is welded to the negative electrode tab laminated portion 32.
  • the positive electrode 20, the negative electrode 30, and the separator 40 constituting the electrode body 14 will be described in detail, particularly the positive electrode 20.
  • the positive electrode 20 has a positive electrode core body and a positive electrode mixture layer provided on the surface of the positive electrode core body.
  • a foil of a metal such as aluminum that is stable in the potential range of the positive electrode 20, a film in which the metal is arranged on the surface layer, or the like can be used.
  • the positive electrode mixture layer contains a positive electrode active material, a conductive material, and a binder, and is preferably provided on both sides of the positive electrode core body excluding the portion to which the positive electrode lead 15 is connected.
  • a positive electrode mixture slurry containing a positive electrode active material, a conductive material, a binder, and the like is applied to the surface of a positive electrode core, the coating film is dried, and then compressed to form a positive electrode mixture layer. It can be manufactured by forming it on both sides of the core body.
  • Examples of the conductive material contained in the positive electrode mixture layer include carbon materials such as carbon black, acetylene black, ketjen black, and graphite.
  • Examples of the binder contained in the positive electrode mixture layer include fluororesins such as polytetrafluoroethylene (PTFE) and polyvinylidene fluoride (PVdF), polyacrylonitrile (PAN), polyimide, acrylic resin, and polyolefins. These resins may be used in combination with cellulose derivatives such as carboxymethyl cellulose (CMC) or salts thereof, polyethylene oxide (PEO) and the like.
  • the positive electrode mixture layer has at least positive electrode active material A as the positive electrode active material.
  • the positive electrode active material A is composed of a lithium transition metal composite oxide and a lithium metal compound, and is composed of a first layer formed on the particle surface of the lithium transition metal composite oxide and a boron compound, and is a first layer. Includes a second layer formed on top.
  • the positive electrode active material A is a secondary particle in which primary particles are aggregated.
  • the first layer is formed on the particle surface of the lithium transition metal composite oxide over the entire area without interposing the second layer.
  • the positive electrode active material A contains a lithium transition metal composite oxide / a first layer / a second layer in order from the inside of the particles. That is, it can be said that the positive electrode active material A is a core-shell particle in which a shell composed of a first layer and a second layer is formed on the surface of the core particle made of a lithium transition metal composite oxide.
  • a first layer made of a lithium metal compound on the surface of secondary particles of a lithium transition metal composite oxide, the initial resistance of the battery can be reduced, and a second layer made of a boron compound covering the first layer can be formed. By forming it, it is possible to suppress an increase in battery resistance during a high temperature cycle.
  • Lithium transition metal composite oxide constituting the positive electrode active material A (hereinafter referred to as "lithium-transition metal complex oxide A") of the general formula Li a Ni b Co c Mn d Al e M f O g (wherein Among them, M is at least one element selected from Group 4, Group 5, and Group 6, 0.8 ⁇ a ⁇ 1.2, b ⁇ 0.82, 0 ⁇ c ⁇ 0.08, 0.05. It is a composite oxide represented by ⁇ d ⁇ 0.12, 0 ⁇ e ⁇ 0.05, 0.01 ⁇ f ⁇ 0.05, 1 ⁇ g ⁇ 2).
  • the content of Ni is preferably 82 to 92 mol%, more preferably 82 to 90 mol%, based on the total number of moles of the metal element excluding Li.
  • the content of Co is preferably 3 to 8 mol%, more preferably 5 to 8 mol%, based on the total number of moles of the metal elements excluding Li. If the Co content exceeds 8 mol%, the increase in resistance during the high temperature cycle cannot be suppressed.
  • the Mn content is preferably 6 to 10 mol% with respect to the total number of moles of the metal element excluding Li. If the Mn content is less than 5 mol%, the increase in resistance during the high temperature cycle cannot be suppressed.
  • the lithium transition metal composite oxide A may contain an element other than Li, Ni, Co, Mn, and M as long as the object of the present disclosure is not impaired.
  • the first layer (wherein, 1 ⁇ x ⁇ 4,1 ⁇ y ⁇ 5,1 ⁇ z ⁇ 12) the general formula Li x M y O z composed of lithium metal compound represented by the.
  • the first layer may be formed so as to cover the entire surface of the secondary particles of the lithium transition metal composite oxide A, or may be scattered on the particle surface.
  • M in the above general formula is at least one element selected from Group 4, Group 5, and Group 6, and is preferably at least one element selected from Ti, Nb, W, and Zr. That is, the lithium transition metal composite oxide A preferably contains at least one selected from Ti, Nb, W, and Zr. Further, the lithium metal compound constituting the first layer preferably contains at least one selected from Ti, Nb, W, and Zr.
  • Suitable lithium metal compounds are, for example, Li 2 TiO 3 , Li 4 Ti 5 O 12 , LiTIO 4 , Li 2 Ti 2 O 5 , LiTIO 2 , Li 3 NbO 4 , LiNbO 3 , Li 4 Nb 2 O 7 , Li 8 Nb 6 O 19 , Li 2 ZrO 3 , LiZrO 2 , Li 4 ZrO 4 , Li 2 WO 4 , Li 4 WO 5 .
  • the content of the first layer is preferably 0.001 to 1 mol% based on the element of M in the above general formula, preferably 0.01 to the total number of moles of the metal elements excluding Li of the positive electrode active material A. 0.5 mol% is more preferable.
  • the content of the first layer is within the above range, it becomes easy to suppress an increase in battery resistance during a high temperature cycle.
  • the second layer is composed of a boron compound and is formed on the first layer.
  • the second layer preferably covers the entire area of the first layer. That is, it is preferable that the first layer is not exposed on the surface of the positive electrode active material A.
  • a part of the second layer may be formed directly on the particle surface of the lithium transition metal composite oxide A.
  • the second layer may be formed, for example, by covering the entire surface of the secondary particle surface of the lithium transition metal composite oxide A including the region where the first layer is formed.
  • the second layer was not formed between the surface of the secondary particles of the lithium transition metal composite oxide A and the first layer, but faced opposite to the lithium transition metal composite oxide A of the first layer. It is formed only on the surface. Further, the lithium metal compound constituting the first layer and the boron compound constituting the second layer do not coexist with each other, and the boundary between the first layer and the second layer can be confirmed by, for example, XPS.
  • the boron compound constituting the second layer may be a compound containing B, and is not particularly limited, but is preferably an oxide or a lithium oxide.
  • Examples of the boron compound include boron oxide (B 2 O 3 ) and lithium borate (Li 2 B 4 O 7 ).
  • the content of the second layer is preferably 0.1 to 1.5 mol%, preferably 0.5 to 1.0, based on the total number of moles of metal elements excluding Li of the positive electrode active material A, based on the boron element. More preferably mol%. When the content of the second layer is within the above range, it becomes easy to suppress an increase in battery resistance during a high temperature cycle.
  • the average primary particle size of the positive electrode active material A is, for example, 100 nm to 1000 nm.
  • the average particle size (average secondary particle size) of the positive electrode active material A is, for example, 8 ⁇ m to 15 ⁇ m.
  • the particle size of the positive electrode active material A is substantially equal to the particle size of the lithium transition metal composite oxide A.
  • the average primary particle size of the positive electrode active material is determined by analyzing the SEM image of the particle cross section observed by a scanning electron microscope (SEM). For example, the positive electrode 20 or the positive electrode active material is embedded in the resin, a cross section is prepared by cross section polisher (CP) processing, and the cross section is photographed by SEM. Thirty primary particles are randomly selected from the SEM image, and the grain boundaries of the primary particles are observed. Then, after specifying the outer shape of the primary particles, the major axis (longest diameter) of each of the 30 primary particles is obtained, and the average value thereof is taken as the average primary particle diameter.
  • SEM scanning electron microscope
  • the average secondary particle size is also obtained from the SEM image of the particle cross section. Specifically, 30 secondary particles are randomly selected from the SEM image, and the grain boundaries of the selected 30 secondary particles are observed. Then, after specifying the outer shape of the secondary particles, the major axis (longest diameter) of each of the 30 secondary particles is obtained, and the average value thereof is taken as the average secondary particle diameter.
  • the positive electrode active material A is produced, for example, by the following process.
  • Nickel cobalt manganese composite hydroxide is calcined at 400 ° C. to 600 ° C. to obtain nickel cobalt manganese composite oxide.
  • the composite oxide, a lithium compound such as lithium hydroxide, and a compound containing a metal element selected from Group 4, Group 5, and Group 6 are mixed at a predetermined molar ratio to form oxygen. atmosphere, and fired under the conditions of 700 ° C. ⁇ 900 ° C., a lithium transition metal composite oxide of lithium metal compound represented by Li x M y O z on the surface of the particles of the (first layer) is stuck precursor obtain.
  • the precursor and the boron compound are mixed at a predetermined molar ratio and calcined in an oxygen atmosphere under the conditions of 150 ° C. to 400 ° C.
  • the positive electrode 20 preferably has a positive electrode active material A and a positive electrode active material B as the positive electrode active material.
  • the positive electrode active material B is preferably secondary particles in which primary particles are aggregated.
  • the average primary particle size of the positive electrode active material B is 0.5 ⁇ m or more, and is larger than the average primary particle size of the positive electrode active material A.
  • the average primary particle size of the positive electrode active material B is, for example, 0.5 ⁇ m to 4 ⁇ m.
  • the average secondary particle size of the positive electrode active material B is 2 ⁇ m to 7 ⁇ m, which is smaller than the average secondary particle size of the positive electrode active material A.
  • the positive electrode active material B may be composed of only primary particles instead of secondary particles.
  • Lithium transition metal composite oxide constituting the positive electrode active material B (hereinafter sometimes referred to as “lithium-transition metal composite oxide B”) has the general formula Li a Ni b Co c Mn d M e O f (wherein, M is at least one element selected from Group 4, Group 5, and Group 6, 0.8 ⁇ a ⁇ 1.2, b ⁇ 0.80, 0 ⁇ c ⁇ 0.15, 0 ⁇ d ⁇ 0 .15, 0 ⁇ e ⁇ 0.05, 1 ⁇ f ⁇ 2).
  • the lithium transition metal composite oxide B may have the same composition as the lithium transition metal composite oxide A.
  • the amount of Co in the positive electrode active material B is preferably equal to or larger than the amount of Co in the positive electrode active material A.
  • the positive electrode active material B is (wherein, 1 ⁇ x ⁇ 4,1 ⁇ y ⁇ 5,1 ⁇ z ⁇ 12) the general formula Li x M y O z is composed of lithium metal compound represented by the lithium transition metal It is preferable to include a surface layer formed on the surface of the secondary particles of the composite oxide B.
  • the surface layer is a layer corresponding to the first layer of the positive electrode active material A, and may be formed so as to cover the entire surface of the secondary particles of the lithium transition metal composite oxide B, and may be formed as a point on the particle surface. It may be present.
  • M in the above general formula is at least one element selected from Group 4, Group 5, and Group 6, and is preferably at least one element selected from Ti, Nb, W, and Zr.
  • Suitable lithium metal compounds are Li 2 TiO 3 , Li 4 Ti 5 O 12 , Li IO 4 , Li 2 Ti 2 O 5 , LiTIO 2 , Li 3 NbO 4 , LiNbO 3 , Li 4 Nb 2 O 7 , Li 8 Nb. 6 O 19 , Li 2 ZrO 3 , LiZrO 2 , Li 4 ZrO 4 , Li 2 WO 4 , Li 4 WO 5 .
  • the content of the surface layer in the positive electrode active material B is preferably lower than the content of the first layer in the positive electrode active material A.
  • the content of the surface layer is preferably 0.001 to 1.0 mol%, preferably 0.01 to 1.0 mol%, based on the element of M in the above general formula, with respect to the total number of moles of metal elements excluding Li of the positive electrode active material B. 0.5 mol% is more preferable.
  • the ratio of the content of the first layer in the positive electrode active material B to the content of the first layer in the positive electrode active material A is preferably 1.1 or more.
  • the positive electrode active material B preferably further contains a second surface layer formed on the surface layer.
  • the second surface layer is a layer corresponding to the second layer of the positive electrode active material A, and is composed of a boron compound.
  • the second surface layer preferably covers the entire surface layer (hereinafter, referred to as "first surface layer"). When the first surface layer is scattered on the particle surface of the lithium transition metal composite oxide B, a part of the second surface layer may be formed directly on the particle surface of the lithium transition metal composite oxide B.
  • the second surface layer was not formed between the surface of the secondary particles of the lithium transition metal composite oxide B and the first surface layer, and faced the opposite side to the lithium transition metal composite oxide A of the first surface layer. It is formed only on the surface. That is, the first surface layer is formed on the particle surface of the lithium transition metal composite oxide B over the entire area without passing through the second surface layer.
  • the boron compound constituting the second surface layer may be a compound containing B, and is not particularly limited, but is preferably an oxide or a lithium oxide.
  • Examples of the boron compound include boron oxide (B 2 O 3 ) and lithium borate (Li 2 B 4 O 7 ).
  • the content of the second surface layer in the positive electrode active material B may be lower than the content of the second layer in the positive electrode active material A.
  • the content of the second layer is preferably 0.1 to 1.5 mol% based on the boron element with respect to the total number of moles of the metal element excluding Li of the positive electrode active material B, and is 0.5 to 1. 0 mol% is more preferable.
  • the positive electrode active material B is produced, for example, by the following process.
  • Nickel cobalt manganese composite hydroxide is calcined at 400 ° C. to 600 ° C. to obtain nickel cobalt manganese composite oxide.
  • the composite oxide, a lithium compound such as lithium hydroxide, and a compound containing a metal element selected from Group 4, Group 5, and Group 6 are mixed at a predetermined molar ratio, and further. by adding an alkali component such as potassium hydroxide at a predetermined concentration, an oxygen atmosphere, and fired under the conditions of 650 ° C.
  • ⁇ 850 ° C. is represented by Li x M y O z on the particle surface of the lithium-transition metal composite oxide A precursor to which the lithium metal compound (first surface layer) is adhered is obtained. (3) The precursor and the boron compound are mixed at a predetermined molar ratio and calcined in an oxygen atmosphere under the conditions of 150 ° C. to 400 ° C.
  • the negative electrode 30 has a negative electrode core body and a negative electrode mixture layer provided on the surface of the negative electrode core body.
  • a foil of a metal such as copper that is stable in the potential range of the negative electrode 30, a film on which the metal is arranged on the surface, or the like can be used.
  • the negative electrode mixture layer contains a negative electrode active material and a binder, and is preferably provided on both sides of the negative electrode core body excluding the portion to which the negative electrode lead 16 is connected, for example.
  • a negative electrode mixture slurry containing a negative electrode active material, a binder, and the like is applied to the surface of the negative electrode core, the coating film is dried, and then compressed to form a negative electrode mixture layer of the negative electrode core. It can be produced by forming it on both sides.
  • the negative electrode mixture layer contains, for example, a carbon-based active material that reversibly occludes and releases lithium ions as a negative electrode active material.
  • Suitable carbon-based active materials are natural graphite such as scaly graphite, massive graphite, earthy graphite, and graphite such as artificial graphite such as massive artificial graphite (MAG) and graphitized mesophase carbon microbeads (MCMB).
  • a Si-based active material composed of at least one of Si and a Si-containing compound may be used, or a carbon-based active material and a Si-based active material may be used in combination.
  • the binder contained in the negative electrode mixture layer fluororesin, PAN, polyimide, acrylic resin, polyolefin or the like can be used as in the case of the positive electrode 20, but styrene-butadiene rubber (SBR) is used. Is preferable.
  • the negative electrode mixture layer preferably further contains CMC or a salt thereof, polyacrylic acid (PAA) or a salt thereof, polyvinyl alcohol (PVA) and the like. Above all, it is preferable to use SBR in combination with CMC or a salt thereof, PAA or a salt thereof.
  • the separator 40 a porous sheet having ion permeability and insulating property is used. Specific examples of the porous sheet include a microporous thin film, a woven fabric, and a non-woven fabric.
  • the material of the separator 40 polyolefins such as polyethylene and polypropylene, cellulose and the like are suitable.
  • the separator 40 may have either a single-layer structure or a laminated structure. A heat-resistant layer or the like may be formed on the surface of the separator.
  • the precursor and boric acid (H 3 BO 3 ) are mixed so that the total amount of Ni, Co and Mn and the molar ratio of B to B are 1: 0.01, and this mixture is mixed in an oxygen atmosphere.
  • a positive electrode active material A in which the surface of the lithium metal compound (first layer) was covered with a boron compound (second layer) was obtained.
  • the composition of the positive electrode active material A was Li 1.03 Ni 0.85 Co 0.08 Mn 0.07 Zr 0.01 O 2 .
  • the positive electrode active material A had an average primary particle diameter of 800 nm and an average particle diameter (average secondary particle diameter) of 12.1 ⁇ m.
  • Positive electrode active material A, acetylene black, and polyvinylidene fluoride (PVdF) are mixed at a mass ratio of 96.3: 2.5: 1.2, and N-methyl-2-pyrrolidone (NMP) is used as a dispersion medium.
  • NMP N-methyl-2-pyrrolidone
  • the positive electrode mixture slurry is applied to both sides of the positive electrode core made of aluminum foil, the coating film is dried and compressed, and then cut into a predetermined electrode size to form positive electrode mixture layers on both sides of the positive electrode core.
  • the positive electrode was prepared.
  • Negative electrode active material sodium salt of carboxymethyl cellulose (CMC-Na), and styrene-butadiene rubber (SBR) are mixed at a mass ratio of 100: 1: 1 and water is used as a dispersion medium to prepare a negative electrode mixture.
  • a slurry was prepared.
  • the negative electrode mixture slurry is applied to both sides of the negative electrode core made of copper foil, the coating film is dried and compressed, and then cut into a predetermined electrode size to form negative electrode mixture layers on both sides of the negative electrode core.
  • the negative electrode was prepared.
  • LiPF 6 is dissolved at a concentration of 1 mol / L in a mixed solvent in which ethylene carbonate (EC), ethyl methyl carbonate (EMC), and dimethyl carbonate (DMC) are mixed in a volume ratio of 3: 3: 4. did. Further, vinylene carbonate (VC) was dissolved in this mixed solvent at a concentration of 2% by mass to prepare a non-aqueous electrolyte solution.
  • EC ethylene carbonate
  • EMC ethyl methyl carbonate
  • DMC dimethyl carbonate
  • the positive electrode to which the aluminum positive electrode lead is attached and the negative electrode to which the nickel negative electrode lead is attached are spirally wound through a polyethylene separator and molded into a flat shape to form a wound electrode body. Made.
  • This electrode body was housed in an exterior body made of aluminum laminate, and after injecting the non-aqueous electrolyte solution, the opening of the exterior body was sealed to prepare a 650 mAh non-aqueous electrolyte secondary battery.
  • Example 2 In the synthesis of the positive electrode active material A, titanium oxide (TiO 2 ) was used instead of ZrO 2 , and nickel cobalt-manganese composite oxide, lithium hydroxide, and titanium oxide (TiO 2 ) were used as Ni, Co, and Mn.
  • TiO 2 titanium oxide
  • Ni, Co, and Mn nickel cobalt-manganese composite oxide, lithium hydroxide, and titanium oxide (TiO 2 ) were used as Ni, Co, and Mn.
  • a non-aqueous electrolyte secondary battery was produced in the same manner as in Example 1 except that the total amount of Li was mixed so that the molar ratio of Li and Ti was 1: 1.08: 0.03.
  • Example 3 A non-aqueous electrolyte secondary battery was produced in the same manner as in Example 1 except that niobium oxide (Nb 2 O 5 ) was used instead of ZrO 2 in the synthesis of the positive electrode active material A.
  • niobium oxide Nb 2 O 5
  • Example 4 A non-aqueous electrolyte secondary battery was produced in the same manner as in Example 1 except that tungsten oxide (WO 3 ) was used instead of ZrO 2 in the synthesis of the positive electrode active material A.
  • tungsten oxide WO 3
  • the composition of the positive electrode active material B was confirmed by ICP to be Li 1.03 Ni 0.85 Co 0.08 Mn 0.07 Ti 0.03 O 2 .
  • the positive electrode active material B had an average primary particle size of 2 ⁇ m and an average secondary particle size of 5 ⁇ m.
  • the non-aqueous electrolyte 2 is the same as in Example 2 except that the positive electrode active material A and the positive electrode active material B are mixed at a mass ratio of 7: 3 and used as the positive electrode active material. The next battery was manufactured.
  • Example 6> In the synthesis of the positive electrode active material B, the molar ratio of nickel-cobalt-manganese composite oxide, lithium hydroxide, titanium oxide, the total amount of Ni, Co, and Mn, and Li and Ti is 1: 1.08.
  • a non-aqueous electrolyte secondary battery was produced in the same manner as in Example 4 except that the mixture was mixed so as to have a ratio of 0.01.
  • the precursor and H 3 BO 3 were mixed so that the total amount of Ni, Co, and Mn and the molar ratio of B were 1: 0.01, and this mixture was mixed in an oxygen atmosphere at 300 ° C.
  • the positive electrode active material B whose surface of the lithium metal compound (first surface layer) was covered with the boron compound (second surface layer) was obtained.
  • the positive electrode active material B had an average primary particle size of 2 ⁇ m and an average secondary particle size of 5 ⁇ m.
  • the non-aqueous electrolyte 2 is the same as in Example 2 except that the positive electrode active material A and the positive electrode active material B are mixed at a mass ratio of 7: 3 and used as the positive electrode active material. The next battery was manufactured.
  • a non-aqueous electrolyte secondary battery was produced in the same manner as in Example 2 except that in the synthesis of the positive electrode active material A, TiO 2 was not mixed, H 3 BO 3 was not mixed, and the subsequent firing was not performed.
  • the positive electrode active material A had an average primary particle diameter of 740 nm and an average secondary particle diameter of 11.1 ⁇ m.
  • a non-aqueous electrolyte secondary battery was produced in the same manner as in Example 2 except that TiO 2 was not mixed in the synthesis of the positive electrode active material A.
  • the positive electrode active material A had an average primary particle diameter of 740 nm and an average secondary particle diameter of 11.1 ⁇ m.
  • a non-aqueous electrolyte secondary battery was produced in the same manner as in Example 2 except that H 3 BO 3 was not mixed and subsequently fired in the synthesis of the positive electrode active material A.
  • the positive electrode active material A had an average primary particle size of 740 nm and an average secondary particle size of 12.1 ⁇ m.
  • the total amount of nickel-cobalt-manganese composite oxide, lithium hydroxide, H 3 BO 3 and Ni, Co, and Mn, and the molar ratio of Li and B are 1: 1.
  • a positive electrode active material precursor in which a boron compound was adhered to the particle surface of a lithium transition metal composite oxide was prepared by mixing the mixture so as to have a ratio of .08: 0.01 and firing in an oxygen atmosphere at 300 ° C. for 3 hours. Obtained.
  • the precursor and titanium oxide are mixed so that the total amount of Ni, Co, and Mn and the molar ratio of Ti are 1: 0.03, and this mixture is mixed in an oxygen atmosphere at 300 ° C. for 3 hours.
  • the positive electrode active material A was obtained by firing under the conditions of.
  • a non-aqueous electrolyte secondary battery was produced in the same manner as in Example 2 except that the positive electrode was produced using the positive electrode active material A.
  • a cycle test was conducted under the following conditions, the resistance value after 150 cycles was obtained by the above method, and the rate of increase in the resistance value after 150 cycles with respect to the resistance value before the cycle test was calculated.
  • the evaluation results are shown in Table 1 as relative values with the rate of increase of the battery of Example 1 as 100.
  • Non-aqueous electrolyte secondary battery 11 Exterior body 12 Containment part 13 Sealing part 14 Electrode body 15 Positive electrode lead 16 Negative electrode lead 20 Positive electrode 21 Positive electrode tab 22 Positive electrode tab laminated part 30 Negative electrode 31 Negative electrode tab 32 Negative electrode tab laminated part 40 Separator

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