WO2023120048A1 - 二次電池用正極およびその製造方法、ならびに二次電池 - Google Patents

二次電池用正極およびその製造方法、ならびに二次電池 Download PDF

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WO2023120048A1
WO2023120048A1 PCT/JP2022/043753 JP2022043753W WO2023120048A1 WO 2023120048 A1 WO2023120048 A1 WO 2023120048A1 JP 2022043753 W JP2022043753 W JP 2022043753W WO 2023120048 A1 WO2023120048 A1 WO 2023120048A1
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positive electrode
active material
secondary battery
phosphorus compound
organic phosphorus
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French (fr)
Japanese (ja)
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充朗 白髪
雪尋 沖
千咲希 長谷川
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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 CN202280083444.9A priority Critical patent/CN118435388A/zh
Priority to EP22910766.9A priority patent/EP4456199A4/en
Priority to JP2023569207A priority patent/JPWO2023120048A1/ja
Priority to US18/722,906 priority patent/US20250054968A1/en
Publication of WO2023120048A1 publication Critical patent/WO2023120048A1/ja
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    • H—ELECTRICITY
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    • 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
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
    • C07F9/02—Phosphorus compounds
    • C07F9/28—Phosphorus compounds with one or more P—C bonds
    • C07F9/38—Phosphonic acids [RP(=O)(OH)2]; Thiophosphonic acids ; [RP(=X1)(X2H)2(X1, X2 are each independently O, S or Se)]
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    • H01M10/052—Li-accumulators
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    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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    • H01M4/0402—Methods of deposition of the material
    • H01M4/0404—Methods of deposition of the material by coating on electrode collectors
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    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
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    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
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    • 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
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—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
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    • 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
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    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
    • H—ELECTRICITY
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    • 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
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    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H—ELECTRICITY
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    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • H—ELECTRICITY
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    • H01M4/00—Electrodes
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    • 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
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    • 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
    • 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 mainly relates to positive electrodes for secondary batteries.
  • the upper limit voltage is set as a voltage (end-of-charge voltage) in a fully charged state, and corresponds to a 100% state of charge (SOC).
  • Patent Document 1 by using a positive electrode active material having a film formed of at least one selected from a specific phosphonate and a specific phosphite triester, gas generation accompanying charging and discharging can be suppressed. says it can.
  • Patent Document 2 states that the use of an electrolytic solution containing a solvent containing a specific phosphonic acid compound improves the chemical stability of the electrolytic solution, thereby suppressing the decomposition reaction of the electrolytic solution during charging and discharging. ing.
  • Patent Document 3 discloses a positive electrode containing a positive electrode active material, a negative electrode containing a lithium transition metal compound having a spinel structure as a negative electrode active material, and an electrolytic solution containing a solvent and an electrolyte salt. proposed a battery containing a phosphorus compound having a P—OH structure in at least one of
  • One aspect of the present disclosure includes a positive electrode current collector and a positive electrode active material layer supported on the positive electrode current collector, and the positive electrode active material layer includes active material particles, a binder, and and a solid organophosphorus compound, wherein the organophosphorus compound has the general formula (1):
  • R 1 and R 2 are each independently a hydrogen atom or an alkyl group having 1 to 2 carbon atoms, and R 3 is an alkyl group having 1 to 17 carbon atoms.
  • the present invention relates to a positive electrode for a secondary battery.
  • Another aspect of the present disclosure relates to a secondary battery comprising the positive electrode for a secondary battery, a negative electrode, an electrolytic solution, and a separator interposed between the positive electrode and the negative electrode.
  • Yet another aspect of the present disclosure includes a step of preparing a positive electrode slurry containing active material particles, a binder, an organic phosphorus compound that is solid at room temperature, and a liquid dispersion medium, and preparing a positive electrode current collector. applying the positive electrode slurry to the surface of the positive electrode current collector to form a coating film; drying the coating film to form an unrolled layer; and rolling the unrolled layer and forming a positive electrode active material layer, wherein the organophosphorus compound has the general formula (1):
  • R 1 and R 2 are each independently a hydrogen atom or an alkyl group having 1 to 2 carbon atoms, and R 3 is an alkyl group having 1 to 17 carbon atoms. and the dispersion medium includes an organic solvent.
  • FIG. 1 is a vertical cross-sectional view schematically showing the internal structure of a secondary battery according to an embodiment of the present disclosure
  • the present disclosure encompasses a combination of matters described in two or more claims arbitrarily selected from the multiple claims described in the attached claims. In other words, as long as there is no technical contradiction, the items described in two or more claims arbitrarily selected from the multiple claims described in the attached claims can be combined.
  • a positive electrode for a secondary battery includes a positive electrode current collector and a positive electrode active material layer supported by the positive electrode current collector.
  • the positive electrode active material layer is formed on the surface of the positive electrode current collector.
  • the positive electrode current collector is composed of a sheet-like conductive material.
  • non-porous conductive substrates metal foil, etc.
  • porous conductive substrates mesh, net, punching sheet, etc.
  • the positive electrode active material layer is carried on one or both surfaces of the positive electrode current collector.
  • the positive electrode active material layer is usually a positive electrode material mixture layer made of a positive electrode material mixture, and has a membranous or film shape.
  • the positive electrode mixture contains, as essential components, active material particles (positive electrode active material particles), a binder, and an organic phosphorus compound that is solid at room temperature.
  • the active material particles may include, for example, lithium-containing transition metal oxides.
  • the binder may contain, for example, at least one selected from the group consisting of fluororesin and hydrogenated nitrile-butadiene rubber.
  • normal temperature means a temperature of 20°C or higher and 30°C or lower.
  • Organic phosphorus compounds that are solid at room temperature have the general formula (1):
  • R 1 and R 2 are each independently a hydrogen atom or an alkyl group having 1 to 2 carbon atoms, and R 3 is an alkyl group having 1 to 17 carbon atoms. be.
  • organic phosphorus compound PR The organic phosphorus compound represented by the general formula (1) (hereinafter also referred to as "organic phosphorus compound PR”) is stable even in a high voltage environment, although it is contained in the positive electrode active material layer.
  • organic phosphorus compound PR contained in the positive electrode active material layer has many opportunities to come into contact with the active material particles, and at least a part of it is in a solid state. do.
  • the organic phosphorus compound PR partially dissolves in a dispersion medium (for example, N-methyl-2-pyrrolidone) in the positive electrode slurry when forming the positive electrode, coats at least part of the surface of the active material particles, and is an electrolyte. Enhances the effect of suppressing oxidative decomposition.
  • a dispersion medium for example, N-methyl-2-pyrrolidone
  • the rate of dissolution in the solvent is slow, and it tends to dissolve gradually over a long period of time. Therefore, even if the coating derived from the organophosphorus compound PR covering the surface of the active material particles in the initial stage is damaged, the coating can be repaired as needed. Therefore, even when the upper limit voltage of the secondary battery is high (for example, when it exceeds 4.3 V), a sufficient effect of suppressing the decomposition reaction of the electrolyte can be continuously obtained.
  • At least part of the organic phosphorus compound PR may exist in the positive electrode active material layer in the form of particles having a particle diameter of 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the organic phosphorus compound PR has such a particle size, it can be said that the organic phosphorus compound PR is excessively contained in the positive electrode active material layer.
  • the particulate organic phosphorus compound PR gradually dissolves over a long period of time, and the surface of the active material particles is replenished with a film derived from the organic phosphorus compound PR as needed, thereby suppressing the decomposition reaction of the electrolyte over a long period of time. will be obtained.
  • the particle size of the organic phosphorus compound PR may be 0.3 ⁇ m or more, or may be 1 ⁇ m or more. Also, the maximum particle size of the organic phosphorus compound PR may be 3 ⁇ m or less, or may be 2 ⁇ m or less. If the maximum value of the particle size is within the above range, the effect on battery performance can be sufficiently reduced.
  • particle is a concept including primary particles, secondary particles, and agglomerates of these, and in addition to general particles or particles, aggregation, agglomeration ( Also includes concepts such as agglomeration.
  • the particle size of the organic phosphorus compound PR can be measured, for example, in the following manner.
  • (1) Preparation of positive electrode cross-sectional sample First, a positive electrode to be measured is prepared. Next, the positive electrode active material layer and the positive electrode current collector are simultaneously cut along the thickness direction of the positive electrode to form a cross section. At that time, the positive electrode active material layer may be filled with a thermosetting resin and cured.
  • a cross-sectional sample of the positive electrode is obtained by a CP (cross-section polisher) method, an FIB (focused ion beam) method, or the like.
  • the positive electrode to be measured is taken out from a secondary battery with a depth of discharge (DOD) of 90% or more.
  • the depth of discharge (DOD) is the ratio of the amount of electricity discharged to the amount of electricity a battery has in a fully charged state.
  • the voltage of the fully charged battery corresponds to the end-of-charge voltage.
  • the voltage of a fully discharged battery corresponds to the end-of-discharge voltage.
  • Elemental analysis by energy dispersive X-ray spectroscopy Elemental analysis by EDX is performed using the SEM image of the cross-sectional sample.
  • a map of the organophosphorus compound PR is obtained by extracting components derived from the organophosphorus compound PR from the EDX analysis data of the cross-sectional sample. Particles of the organophosphorus compound PR are identified from the obtained map. The diameter of an equivalent circle having the same area as the specified area of the particles is taken as the particle size of the organophosphorus compound PR.
  • One or more particles of the organophosphorus compound PR having a particle diameter of 0.1 ⁇ m or more may be observed in an observation field of 400 ⁇ m 2 (for example, a rectangle of 20 ⁇ m ⁇ 20 ⁇ m), but 3 or more, further 6 or more are observed. is desirable.
  • an observation field of 400 ⁇ m 2 for example, a rectangle of 20 ⁇ m ⁇ 20 ⁇ m
  • 3 or more, further 6 or more are observed.
  • the upper limit of the number of particles of the organophosphorus compound PR having a particle diameter of 0.1 ⁇ m or more observed in the observation field is, for example, 16 or less.
  • Each of the above numbers may be an average value of the number of particles of the organophosphorus compound PR having a particle diameter of 0.1 ⁇ m or more counted in a plurality (for example, 3 or more) of observation fields. It is desirable to set the observation field near the center of the positive electrode active material layer in the cross-sectional sample.
  • a small amount of the organic phosphorus compound PR may be included in the positive electrode active material layer.
  • the content of the organic phosphorus compound PR contained in the positive electrode active material layer may be, for example, 0.1% by mass or more and 5% by mass or less, 0.2% by mass or more and 3% by mass or less, or 0.5% by mass or more. 2 mass % or less may be sufficient.
  • the organic phosphorus compound PR contained at the above content does not greatly affect the battery capacity.
  • the organic phosphorus compound PR contained at the above content rate can be uniformly dispersed in the positive electrode active material layer as particles having an appropriate particle size as described above.
  • the organic phosphorus compound PR desirably covers part of the surface of the active material particles. It is considered that the organophosphorus compound PR present on the surface of the active material particles effectively suppresses the contact between the active material particles and the electrolyte. It is assumed that the organophosphorus compound PR present on the surface of the active material particles includes a film (reaction product) derived from the organophosphorus compound PR. This is because a chemical reaction may proceed between the organic phosphorus compound PR and the active material particles when the organic phosphorus compound PR adheres to the surface of the active material particles.
  • R 3 may be an alkyl group having 5 to 17 carbon atoms or an alkyl group having 10 to 15 carbon atoms.
  • the organophosphorus compound PR having such an alkyl group R3 or a film derived from it has higher stability and remains in the positive electrode active material layer for a long period of time, exhibiting the effect of suppressing the decomposition reaction of the electrolyte. do.
  • the organic phosphorus compound PR having an alkyl group R 3 having 5 to 17 carbon atoms has a sufficiently slow dissolution rate in the solvent in the electrolyte, and has the effect of supplementing the surface of the active material particles with a film derived from the organic phosphorus compound PR as needed. is considered to be large.
  • the manufacturing method includes a step of preparing a positive electrode slurry containing active material particles, a binder, an organic phosphorus compound (organic phosphorus compound PR) that is solid at room temperature (20° C.
  • step (II) of preparing a positive electrode current collector step (III) of applying the positive electrode slurry on the surface of the positive electrode current collector to form a coating film, and drying the coating film , a step (IV) of forming an unrolled layer, and a step (V) of rolling the unrolled layer to form a positive electrode active material layer.
  • the positive electrode slurry is prepared by mixing a positive electrode material mixture containing active material particles, a binder and an organic phosphorus compound PR with a liquid dispersion medium and dispersing the mixture in the dispersion medium.
  • the positive electrode mixture may further contain another component (eg, a conductive material).
  • As the liquid dispersion medium an organic solvent having excellent affinity with both the binder and the organophosphorus compound PR is used.
  • NMP N-methyl-2-pyrrolidone
  • alcohols such as ethanol, ethers such as tetrahydrofuran, amides such as dimethylformamide, and ketones such as cyclohexanone may also be used.
  • the organophosphorus compound PR may be preliminarily mixed with a dispersion medium to dissolve at least a portion thereof. For example, by mixing a particulate organophosphorus compound PR having an average particle diameter D1 with a dispersion medium, a dispersion liquid of particulate organophosphorus compound PR having an average particle diameter d1 (d1 ⁇ D1 or d1 ⁇ 0.8D1) is obtained. may be prepared. This makes it easier to coat at least part of the surface of the active material particles with the organophosphorus compound PR or a coating derived therefrom.
  • the average particle diameter is the median diameter (D 50 ) at which the cumulative volume is 50% in the volume-based particle size distribution obtained by a laser diffraction particle size distribution analyzer.
  • the binder for example, at least one selected from the group consisting of fluororesin and hydrogenated nitrile-butadiene rubber can be used.
  • Fluorine resins include polyvinylidene fluoride (PVDF), polytetrafluoroethylene (PTFE), perfluoroalkoxyalkane (PFA), tetrafluoroethylene-hexafluoropropylene copolymer (FEP), ethylene-tetrafluoroethylene copolymer (ETFE), vinylidene fluoride-hexafluoropropylene copolymer, and the like.
  • a sheet-like conductive material (metal foil, mesh, net, punching sheet, etc.) is used. Among them, metal foil is preferred. Examples of materials for the positive electrode current collector include stainless steel, aluminum, aluminum alloys, and titanium. The thickness of the positive electrode current collector is not particularly limited, but is, for example, 1 to 50 ⁇ m, and may be 5 to 30 ⁇ m.
  • a coating film is formed by applying the positive electrode slurry to the surface of the positive electrode current collector.
  • a bar coater, a gravure coater, a blade coater, a roll coater, a comma coater, a die coater, a lip coater, and the like are used as the positive electrode slurry coating apparatus, for example.
  • the organic phosphorus compound PR be in the form of particles having a particle size of 0.1 ⁇ m or more and 5 ⁇ m or less. This makes it possible to easily obtain a positive electrode active material layer containing an organic phosphorus compound PR having a particle size of 0.1 ⁇ m or more and 5 ⁇ m or less.
  • the coating film is dried to volatilize the dispersion medium to form an unrolled coating film.
  • the organic phosphorus compound PR may be migrated from the positive electrode current collector side to the outermost surface side (that is, the separator side) together with the dispersion medium.
  • the organic phosphorus compound PR is unevenly distributed on the outermost surface side of the positive electrode active material layer rather than on the positive electrode current collector side.
  • the oxidative decomposition reaction of the electrolyte progresses more easily in a region closer to the outermost surface side of the positive electrode active material layer. This is because a large amount of electrolyte flows in such a region.
  • the effect of suppressing the oxidative decomposition reaction of the electrolyte becomes more pronounced.
  • the unrolled layer is rolled to form a positive electrode active material layer.
  • the rolling conditions are not particularly limited, but the density of the active material particles (positive electrode active material) in the positive electrode active material layer after rolling is, for example, 3.3 g/cm 3 or more and 4.0 g/cm 3 or less. It may be 5 g/cm 3 or more and 4.0 g/cm 3 or less.
  • the existence probability Pt of the organophosphorus compound PR existing in the upper layer region may satisfy, for example, 1.2 ⁇ Pt/Pb.
  • Pb and Pt can be measured by analyzing a cross-sectional sample of the positive electrode obtained by the method described above with SEM and EDX. Specifically, in a map of the organophosphorus compound PR obtained from the EDX analysis data of the cross-sectional sample, the area occupied by the organophosphorus compound PR in the lower layer region and the upper layer region is measured. At this time, all organophosphorus compounds PR are counted regardless of the particle size of the organophosphorus compounds PR. Then, the ratio of the area of the organic phosphorus compound PR to the area of the lower layer region and the upper layer region is regarded as Pb and Pt, respectively.
  • Pb and Pt are measured with an observation field of view of 400 ⁇ m 2 (eg a 20 ⁇ m ⁇ 20 ⁇ m rectangle).
  • Pb and Pt may be average values of Pb and Pt obtained in a plurality of (for example, 3 or more) observation fields, respectively. It is desirable to set the observation field near the center of each of the lower layer region and the upper layer region in the cross-sectional sample.
  • a secondary battery includes the positive electrode for a secondary battery, a negative electrode, a lithium ion conductive electrolyte, and a separator interposed between the positive electrode and the negative electrode.
  • the lithium ion conductive electrolyte may be an electrolytic solution, or may be a gel electrolyte or a solid electrolyte in which the electrolytic solution is held by a matrix material.
  • the electrolyte may be a non-aqueous electrolyte or an aqueous electrolyte.
  • Secondary batteries include a lithium ion secondary battery that uses a material that reversibly absorbs and releases lithium ions as a negative electrode active material, and a lithium secondary battery that deposits lithium metal on the negative electrode during charging and dissolves lithium metal during discharging. , solid state batteries containing gel or solid electrolytes, and the like.
  • the configuration of the secondary battery will be specifically described below, taking a lithium-ion secondary battery as an example.
  • the positive electrode As the positive electrode, a positive electrode for a secondary battery having the characteristics described above is used.
  • the positive electrode active material layer is composed of a positive electrode mixture.
  • the positive electrode mixture contains active material particles (positive electrode active material particles), a binder, and an organic phosphorus compound PR as essential components, and may contain optional components.
  • Optional components may include conductive materials, thickeners, and the like.
  • the thickness of the positive electrode active material layer is not particularly limited.
  • a plurality of layers having different shapes may form one positive electrode active material layer.
  • two or more layers containing active material particles having different average particle sizes may be laminated, or two or more layers having different types or compositions of positive electrode active materials may be laminated.
  • the average particle size of the active material particles is, for example, 3 ⁇ m or more and 30 ⁇ m or less, and may be 5 ⁇ m or more and 25 ⁇ m or less.
  • the average particle diameter is the median diameter (D 50 ) at which the cumulative volume is 50% in the volume-based particle size distribution obtained by a laser diffraction particle size distribution analyzer.
  • the active material particles may be separated and recovered from the positive electrode.
  • "LA-750" manufactured by HORIBA, Ltd. can be used as the measuring device.
  • the average particle size of the active material particles may be measured from the above-mentioned cross-sectional sample of the positive electrode. A cross-sectional SEM image is taken so that 10 or more active material particles are observed, and the diameters of equivalent circles having the same area as the cross section of 10 or more active material particles are obtained by image processing. The value may be the average particle size.
  • the positive electrode active material that constitutes the active material particles may contain a lithium-containing transition metal oxide. From the viewpoint of increasing the capacity, it is desirable that the lithium-containing transition metal oxide contains lithium and Ni and contains a lithium nickel oxide (composite oxide N) having a layered rock salt crystal structure.
  • the ratio of the composite oxide N in the positive electrode active material is, for example, 70% by mass or more, may be 90% by mass or more, or may be 95% by mass or more.
  • the ratio of Ni to the metal elements other than Li contained in the composite oxide N may be 50 atomic % or more.
  • the composite oxide N is represented, for example, by formula (1): Li ⁇ Ni x1 M1 x2 M2 (1 ⁇ x1 ⁇ x2) O 2+ ⁇ .
  • the element M1 is at least one selected from the group consisting of V, Co and Mn.
  • Element M2 is at least one selected from the group consisting of Mg, Al, Ca, Ti, Cu, Zn and Nb.
  • formula (1) is 0.9 ⁇ ⁇ ⁇ 1.10, -0.05 ⁇ ⁇ ⁇ 0.05, 0.5 ⁇ x1 ⁇ 1, 0 ⁇ x2 ⁇ 0.5, 0 ⁇ 1-x1- satisfies x2 ⁇ 0.5. ⁇ increases and decreases due to charging and discharging.
  • the composite oxide N contains Ni and may contain at least one selected from the group consisting of Co, Mn and Al as the element M1 and the element M2. Co, Mn and Al contribute to stabilization of the crystal structure of the composite oxide N.
  • the ratio of Co in the metal elements other than Li contained in the composite oxide N is preferably 0 atomic % or more and 20 atomic % or less, and 0 atomic % or more and 15 atoms. % or less is more desirable.
  • the proportion of Mn in metal elements other than Li may be 30 atomic % or less, or may be 20 atomic % or less.
  • the ratio of Mn to the metal elements other than Li may be 1 atomic % or more, 3 atomic % or more, or 5 atomic % or more.
  • the ratio of Al to the metal elements other than Li may be 10 atomic % or less, or 5 atomic % or less.
  • the ratio of Al to the metal elements other than Li may be 1 atomic % or more, 3 atomic % or more, or 5 atomic % or more.
  • the composite oxide N can be represented, for example, by formula (2): Li ⁇ Ni (1-y1-y2-y3-z) Co y1 Mn y2 Al y3 M z O 2+ ⁇ .
  • Element M is an element other than Li, Ni, Co, Mn, Al and oxygen, and consists of Ti, Zr, Nb, Mo, W, Fe, Zn, B, Si, Mg, Ca, Sr, Sc and Y. At least one selected from the group may be used.
  • formula (2) is 0.9 ⁇ 1.10, ⁇ 0.05 ⁇ 0.05, 0 ⁇ y1 ⁇ 0.1, 0 ⁇ y2 ⁇ 0.2, 0 ⁇ y3 ⁇ 0. 1, satisfies 0 ⁇ z ⁇ 0.10.
  • v which indicates the atomic ratio of Ni
  • 0.8 or more may be 0.85 or more, or may be 0.90 or more or 0.95 or more.
  • v which indicates the atomic ratio of Ni, may be 0.98 or less, or may be 0.95 or less.
  • the ratio of Co to the metal elements other than Li may be 1.5 atomic % or less. If the Co content of the composite oxide N can be reduced and the Ni content can be increased, it is advantageous in terms of cost and can ensure a high capacity. Mn and/or Al contribute to stabilization of the crystal structure of the composite oxide N with a reduced Co content.
  • Examples of conductive materials that can be included as optional components in the positive electrode active material layer include carbon nanotubes (CNT), carbon fibers other than CNT, and conductive particles (eg, carbon black and graphite).
  • CNT carbon nanotubes
  • carbon fibers other than CNT carbon fibers other than CNT
  • conductive particles eg, carbon black and graphite
  • the negative electrode includes at least a negative electrode current collector, for example, a negative electrode current collector and a negative electrode active material layer.
  • the negative electrode active material layer is carried on one or both surfaces of the negative electrode current collector.
  • the negative electrode active material layer may be a negative electrode mixture layer composed of a negative electrode mixture.
  • the negative electrode mixture layer is membranous or film-like.
  • the negative electrode mixture contains particles of a negative electrode active material as an essential component, and may contain a binder, a conductive agent, a thickener, and the like as optional components. Also, a lithium metal foil or a lithium alloy foil may be attached to the negative electrode current collector as the negative electrode active material layer.
  • the negative electrode mixture layer can be formed, for example, by applying a negative electrode slurry in which a negative electrode mixture containing particles of a negative electrode active material, a binder, etc. is dispersed in a dispersion medium on the surface of the negative electrode current collector and drying the slurry. .
  • the dried coating film may be rolled if necessary.
  • Negative electrode active materials include materials that electrochemically absorb and release lithium ions, lithium metal, and lithium alloys. Carbon materials, alloy materials, and the like are used as materials that electrochemically occlude and release lithium ions. Examples of carbon materials include graphite, graphitizable carbon (soft carbon), and non-graphitizable carbon (hard carbon). Among them, graphite is preferable because it has excellent charging/discharging stability and low irreversible capacity. Examples of alloy-based materials include those containing at least one metal capable of forming an alloy with lithium, and specific examples include silicon, tin, silicon alloys, tin alloys, and silicon compounds. Silicon oxide, tin oxide, etc. may also be used.
  • a lithium ion conductive phase and a composite material in which silicon particles are dispersed in the lithium ion conductive phase can be used.
  • the lithium ion conductive phase for example, a silicon oxide phase, a silicate phase, a carbon phase, or the like can be used.
  • a major component (eg, 95-100% by weight) of the silicon oxide phase can be silicon dioxide.
  • a composite material composed of a silicate phase and silicon particles dispersed in the silicate phase is preferable in terms of high capacity and low irreversible capacity.
  • a lithium silicate phase (a silicate phase containing lithium) having a small irreversible capacity and a high initial charge-discharge efficiency is preferable.
  • the lithium silicate phase may be an oxide phase containing lithium (Li), silicon (Si), and oxygen (O), and may contain other elements.
  • the atomic ratio of O to Si: O/Si in the lithium silicate phase is greater than 2 and less than 4, for example.
  • O/Si is greater than 2 and less than 3.
  • the atomic ratio of Li to Si in the lithium silicate phase: Li/Si is greater than 0 and less than 4, for example.
  • Elements other than Li, Si and O that can be contained in the lithium silicate phase include, for example, iron (Fe), chromium (Cr), nickel (Ni), manganese (Mn), copper (Cu), molybdenum (Mo), Examples include zinc (Zn) and aluminum (Al).
  • the carbon phase can be composed of, for example, amorphous carbon with low crystallinity (that is, amorphous carbon).
  • Amorphous carbon may be, for example, hard carbon, soft carbon, or otherwise.
  • a nonporous conductive substrate metal foil, etc.
  • a porous conductive substrate mesh, net, punching sheet, etc.
  • materials for the negative electrode current collector include stainless steel, nickel, nickel alloys, copper, and copper alloys.
  • Binder for example, a resin material is used.
  • binders include polyacrylic acid, polyacrylic acid salts and derivatives thereof, fluororesins, polyolefin resins, polyamide resins, polyimide resins, acrylic resins, vinyl resins, rubber particles and the like.
  • the binder may be used alone or in combination of two or more.
  • Examples of conductive materials include carbon nanotubes (CNT), carbon fibers other than CNT, and conductive particles (eg, carbon black, graphite).
  • CNT carbon nanotubes
  • carbon fibers other than CNT carbon fibers other than CNT
  • conductive particles eg, carbon black, graphite
  • thickeners examples include carboxymethyl cellulose (CMC) and modified products thereof (including salts such as Na salts), cellulose derivatives such as methyl cellulose (cellulose ethers, etc.); polymer cellulose having a vinyl acetate unit such as polyvinyl alcohol; compound; polyether (polyalkylene oxide such as polyethylene oxide, etc.), and the like.
  • CMC carboxymethyl cellulose
  • modified products thereof including salts such as Na salts
  • cellulose derivatives such as methyl cellulose (cellulose ethers, etc.)
  • polymer cellulose having a vinyl acetate unit such as polyvinyl alcohol
  • compound compound
  • polyether polyalkylene oxide such as polyethylene oxide, etc.
  • a separator is interposed between a positive electrode and a negative electrode.
  • the separator has high ion permeability and moderate mechanical strength and insulation. Examples of separators include microporous thin films, woven fabrics, non-woven fabrics, and the like.
  • Polyolefin such as polypropylene or polyethylene is used as the material of the separator.
  • the separator may have a heat-resistant insulating layer on at least one surface layer.
  • the heat-resistant insulating layer may contain an inorganic oxide filler as a main component (for example, 80% by mass or more), or may contain a heat-resistant resin as a main component (for example, 40% by mass or more).
  • a polyamide resin such as an aromatic polyamide (aramid), a polyimide resin, a polyamideimide resin, or the like may be used as the heat-resistant resin.
  • the lithium ion conductive electrolyte may be a liquid electrolyte (electrolytic solution), a gel electrolyte, or a solid electrolyte.
  • the liquid electrolyte is, for example, an electrolytic solution containing a non-aqueous solvent and a lithium salt dissolved in the non-aqueous solvent.
  • the lithium salt concentration in the electrolytic solution is, for example, 0.5 mol/L or more and 2 mol/L or less.
  • the electrolytic solution may contain known additives.
  • a gel electrolyte contains a lithium salt and a matrix polymer, or contains a lithium salt, a non-aqueous solvent and a matrix polymer.
  • the matrix polymer for example, a polymer material that gels by absorbing a non-aqueous solvent is used. Examples of polymer materials include fluorine resins, acrylic resins, polyether resins, polyethylene oxide, and the like.
  • the solid electrolyte may be an inorganic solid electrolyte.
  • the inorganic solid electrolyte for example, a known material (for example, an oxide-based solid electrolyte, a sulfide-based solid electrolyte, a halide-based solid electrolyte, etc.) is used for all-solid-state lithium ion secondary batteries and the like.
  • non-aqueous solvent for example, cyclic carbonate, chain carbonate, cyclic carboxylate, and the like are used.
  • Cyclic carbonates include propylene carbonate (PC) and ethylene carbonate (EC).
  • Chain carbonates include diethyl carbonate (DEC), ethyl methyl carbonate (EMC), dimethyl carbonate (DMC) and the like.
  • Cyclic carboxylic acid esters include ⁇ -butyrolactone (GBL) and ⁇ -valerolactone (GVL).
  • the non-aqueous solvent may be used singly or in combination of two or more.
  • Lithium salts include, for example, lithium salts of chlorine-containing acids ( LiClO4 , LiAlCl4 , LiB10Cl10 , etc.), lithium salts of fluorine-containing acids ( LiPF6 , LiBF4 , LiSbF6 , LiAsF6 , LiCF3SO3 ) . , LiCF3CO2 , etc.
  • LiN( SO2F ) 2 lithium salts of fluorine - containing acid imides (LiN( SO2F ) 2 , LiN ( CF3SO2 ) 2 , LiN( CF3SO2 ) ( C4F9SO2 ) , LiN ( C2F5SO2 ) 2 , etc.), lithium halides (LiCl, LiBr, LiI, etc.).
  • Lithium salts may be used singly or in combination of two or more.
  • a secondary battery there is a structure in which an electrode group, in which a positive electrode and a negative electrode are wound with a separator interposed therebetween, is housed in an outer package together with an electrolytic solution.
  • an electrode group in which a positive electrode and a negative electrode are wound with a separator interposed therebetween
  • an electrolytic solution e.g., aqueous solution
  • a laminated electrode group in which a positive electrode and a negative electrode are laminated with a separator interposed therebetween may be used.
  • the form of the secondary battery is also not limited, and may be, for example, cylindrical, square, coin, button, laminate, or the like.
  • FIG. 1 is a vertical cross-sectional view of a cylindrical non-aqueous secondary battery 10 that is an example of the present embodiment.
  • the present disclosure is not limited to the following configurations.
  • the secondary battery 10 includes an electrode group 18, an electrolytic solution (not shown), and a bottomed cylindrical battery can 22 that accommodates them.
  • a sealing member 11 is crimped and fixed to the opening of the battery can 22 via a gasket 21 . The inside of the battery is thereby sealed.
  • the sealing body 11 includes a valve body 12 , a metal plate 13 , and an annular insulating member 14 interposed between the valve body 12 and the metal plate 13 .
  • the valve body 12 and the metal plate 13 are connected to each other at their respective centers.
  • a positive electrode lead 15 a led out from the positive electrode plate 15 is connected to the metal plate 13 . Therefore, the valve body 12 functions as a positive external terminal.
  • a negative lead 16 a led out from the negative plate 16 is connected to the inner surface of the bottom of the battery can 22 .
  • An annular groove 22 a is formed near the open end of the battery can 22 .
  • a first insulating plate 23 is arranged between one end surface of the electrode group 18 and the annular groove portion 22a.
  • a second insulating plate 24 is arranged between the other end surface of the electrode group 18 and the bottom of the battery can 22 .
  • the electrode group 18 is formed by winding the positive electrode plate 15 and the negative electrode plate 16 with the separator 17 interposed therebetween.
  • I Preparation of positive electrode (I) Slurry preparation process Active material particles (LiNi 0.8 Mn 0.2 O 2 ) 95 parts by mass, polyvinylidene fluoride (PVDF) 2.5 parts by mass as a binder, acetylene black as a conductive material 2.5 parts by weight, and a given amount of the following formula:
  • PR decylphosphonic acid
  • the content of the organic phosphorus compound PR (decylphosphonic acid) in the positive electrode mixture was 0.1% by mass in Example 1, and 0.1% by mass in Example 1. 2 was set to 1.0% by mass.
  • the organic phosphorus compound PR in the positive electrode slurry was not completely dissolved, but was partially present in the positive electrode slurry in the form of particles having a particle size of 0.1 ⁇ m or more and 5 ⁇ m or less (average particle size d1 ⁇ 3 ⁇ m).
  • the positive electrode was cut into a predetermined shape, and the positive electrode active material layer was partially peeled off to obtain a positive electrode for evaluation.
  • the positive electrode was shaped to have a power generation region of 60 mm ⁇ 40 mm with a positive electrode active material layer and a connection region of 10 mm ⁇ 10 mm without a positive electrode active material layer.
  • a positive tab lead was connected to the connection area.
  • a negative electrode was produced by attaching a lithium metal foil to one side of an electrolytic copper foil (collector). The negative electrode was cut into the same shape as the positive electrode, the lithium metal foil on the connection area was peeled off, and the negative electrode tab lead was connected to the connection area.
  • An electrolyte was prepared by dissolving LiPF 6 at a concentration of 1 mol/L in a mixed solvent of fluoroethylene carbonate (FEC) and dimethyl carbonate (DMC) at a volume ratio of 20:80. .
  • FEC fluoroethylene carbonate
  • DMC dimethyl carbonate
  • a cell having a design capacity of 114 mAh, which is regulated for the negative electrode was prepared.
  • An electrode plate group was obtained by stacking the positive electrode and the negative electrode with a polyethylene separator (thickness: 15 ⁇ m) interposed between the positive electrode active material layer and the lithium metal foil.
  • the electrode group was housed in an envelope-shaped case made of a laminate film with both ends opened together with 1.2 cm 3 of electrolyte, and each tab lead was led out from one opening and the opening was sealed.
  • the positive electrode active material layer was impregnated with the electrolytic solution by allowing it to stand under a reduced pressure of 0.02 MPa for 3 minutes and then returning to atmospheric pressure twice. Finally, the other opening was sealed, and evaluation cells A1 and A2 of Examples 1 and 2 were obtained.
  • the evaluation cell was produced in a dry air atmosphere with a dew point of -60°C or less.
  • Table 1 shows the discharge capacity and the amount of gas generated.
  • Table 1 shows relative values when the discharge capacity and gas generation amount of cell B1 of Comparative Example 1, which will be described later, are assumed to be 100%.
  • a positive electrode for a secondary battery according to the present disclosure and a secondary battery including the same are useful as main power sources for mobile communication devices, portable electronic devices, electric vehicles, and the like.

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