WO2021241416A1 - 正極活物質、正極材料、電池、および正極活物質の製造方法 - Google Patents

正極活物質、正極材料、電池、および正極活物質の製造方法 Download PDF

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WO2021241416A1
WO2021241416A1 PCT/JP2021/019285 JP2021019285W WO2021241416A1 WO 2021241416 A1 WO2021241416 A1 WO 2021241416A1 JP 2021019285 W JP2021019285 W JP 2021019285W WO 2021241416 A1 WO2021241416 A1 WO 2021241416A1
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positive electrode
active material
electrode active
solid electrolyte
battery
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English (en)
French (fr)
Japanese (ja)
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好政 名嘉真
勇祐 西尾
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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 JP2022526968A priority Critical patent/JP7742578B2/ja
Priority to EP21814629.8A priority patent/EP4159686B1/en
Priority to CN202180036620.9A priority patent/CN115699365B/zh
Publication of WO2021241416A1 publication Critical patent/WO2021241416A1/ja
Priority to US18/053,389 priority patent/US20230075889A1/en
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    • 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
    • H01M4/36—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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B17/00—Sulfur; Compounds thereof
    • C01B17/22—Alkali metal sulfides or polysulfides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
    • C01D15/00—Lithium compounds
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00—Compounds of rare earth metals
    • C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • C01F17/36—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 halogen being the only anion, e.g. NaYF4
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Complex oxides containing nickel and at least one other metal element
    • C01G53/42—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2
    • C01G53/44—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese
    • C01G53/50—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2
    • 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
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    • 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
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1391—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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    • 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
    • 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
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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
    • H01M4/36—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
    • H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/80—Compositional purity
    • C01P2006/82—Compositional purity water content
    • 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
    • H01M2300/0065—Solid electrolytes
    • H01M2300/0068—Solid electrolytes inorganic
    • H01M2300/008—Halides
    • 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

  • This disclosure relates to a positive electrode active material, a positive electrode material, a battery, and a method for manufacturing a positive electrode active material.
  • Patent Document 1 a composite active material particle having an active material particle and a coating layer covering at least a part of the surface of the active material particle and having a water content of a predetermined value or less and a sulfide solid electrolyte are used. Solid state batteries are disclosed.
  • lithium ion conductive oxides such as lithium niobate, lithium titanate, lithium lanthansis, lithium tantalate, and lithium tantalate are used as the coating material, and lithium niobate is particularly preferably used. It is disclosed that it will be done.
  • the present disclosure provides a battery with low internal resistance.
  • the positive electrode active material of the present disclosure is The main component is the composite oxide represented by the following formula (1), and the amount of water generated when heated at 180 ° C. by the Karl Fischer titration method is 2.9 mass ppm or more and 44.7 mass ppm or less.
  • x satisfies 0.5 ⁇ x ⁇ 1
  • Me is at least one element selected from the group consisting of Mn, Co, and Al.
  • a battery having a low internal resistance can be obtained.
  • FIG. 1 is a cross-sectional view showing a schematic configuration of the positive electrode material 1000 and the battery 2000 in the first and second embodiments.
  • FIG. 2 is a Nyquist diagram showing an example of the evaluation result of the reaction resistance by the AC impedance measurement.
  • the present inventor has diligently studied the factors that increase the battery resistance of an all-solid-state lithium-ion battery. As a result, the present inventors have found that a trace amount of water contained in the active material reacts with the halide solid electrolyte to deteriorate the halide, thereby increasing the resistance of the all-solid-state lithium-ion battery. Based on this finding, the present inventor considered that it was necessary to take measures to significantly reduce the amount of water in the active material when producing the active material, and proceeded with further research. As a result, it was found that the amount of water contained in the active material can be significantly reduced by drying the active material under predetermined conditions. When an all-solid-state lithium-ion battery was manufactured using the active material thus produced, an all-solid-state lithium-ion battery having a low battery resistance could be obtained.
  • the positive electrode active material according to the first aspect of the present disclosure is The main component is the composite oxide represented by the following formula (1), and the amount of water generated when heated at 180 ° C. by the Karl Fischer titration method is 2.9 mass ppm or more and 44.7 mass ppm or less.
  • x satisfies 0.5 ⁇ x ⁇ 1
  • Me is at least one element selected from the group consisting of Mn, Co, and Al.
  • the positive electrode active material according to the first aspect has a small amount of water. Therefore, it is possible to reduce the internal resistance of the battery using the positive electrode active material according to the first aspect.
  • the positive electrode active material according to the first aspect further comprises a coating material for covering the surface of the positive electrode active material, and the coating material includes a lithium element (Li) and an oxygen element ( It may contain at least one element selected from the group consisting of O), a fluorine element (F), and a chlorine element (Cl).
  • the coating material includes a lithium element (Li) and an oxygen element ( It may contain at least one element selected from the group consisting of O), a fluorine element (F), and a chlorine element (Cl).
  • the coating material is lithium niobate, lithium phosphate, lithium titanate, lithium tungstate, lithium fluoride zirconate, aluminum fluoride. It may contain at least one selected from the group consisting of lithium acid, lithium titanate fluoride, and lithium magnesium fluoride.
  • the positive electrode material according to the fourth aspect of the present disclosure includes a positive electrode active material and a solid electrolyte according to any one of the first to third aspects.
  • the solid electrolyte is represented by the following formula (2).
  • ⁇ , ⁇ , and ⁇ are independently greater than 0, respectively.
  • M comprises at least one selected from the group consisting of metallic elements other than Li and metalloid elements.
  • X comprises at least one selected from the group consisting of F, Cl, Br, and I.
  • the M may contain yttrium.
  • the X may contain at least one selected from the group consisting of Cl and Br.
  • the battery according to the ninth aspect of the present disclosure is A positive electrode containing a positive electrode material according to any one of the fourth to eighth aspects, and a positive electrode. With the negative electrode An electrolyte layer arranged between the positive electrode and the negative electrode, To prepare for.
  • the battery according to the ninth aspect can realize low internal resistance.
  • the electrolyte layer may contain the solid electrolyte.
  • the battery according to the tenth aspect can realize low internal resistance.
  • the electrolyte layer may contain a halide solid electrolyte different from the solid electrolyte.
  • the battery according to the eleventh aspect can realize low internal resistance.
  • the electrolyte layer may contain a sulfide solid electrolyte.
  • the battery according to the twelfth aspect can realize low internal resistance.
  • the method for producing a positive electrode active material according to the thirteenth aspect of the present disclosure is as follows.
  • the manufacturing method includes a drying step of drying the material constituting the positive electrode active material.
  • the drying step satisfies the following (A) or (B).
  • the drying step includes only drying the material constituting the positive electrode active material for 12 hours or more and 500 hours or less in the range of 70 ° C. or higher and lower than 120 ° C.
  • B) In the drying step the material constituting the positive electrode active material is dried in a range of 70 ° C. or higher and lower than 120 ° C.
  • the material constituting the positive electrode active material is dried at 150 ° C. It includes at least one selected from the group consisting of drying at a temperature of not more than 500 ° C. for 0.5 hours or more and drying at a temperature of 600 ° C. or more and 850 ° C. or less for 0.5 hours or more.
  • a positive electrode active material having a small amount of water can be produced. Thereby, the internal resistance of the battery can be reduced.
  • FIG. 1 is a cross-sectional view showing a schematic configuration of the positive electrode material 1000 according to the first embodiment.
  • the positive electrode material 1000 in the first embodiment includes a solid electrolyte 100 and a positive electrode active material 110. As shown in FIG. 1, the positive electrode active material 110 and the solid electrolyte 100 are, for example, in the form of particles.
  • the positive electrode active material 110 contains a composite oxide represented by the following formula (1) as a main component, and the amount of water generated when heated to 180 ° C. by the Karl Fischer titration method is 2.9 mass ppm or more and 44. It is 0.7 mass ppm or less.
  • the resistance of the battery can be reduced.
  • the “main component” is the component contained most in the mass ratio.
  • the water content of the positive electrode active material 110 is specified by measuring the water content generated when heating at 180 ° C. by the Karl Fischer titration method. It is presumed that the water generated at 180 ° C. is mainly water physically adsorbed on the positive electrode active material 110 and hydrated water bound to surface impurities and the like.
  • the positive electrode active material 110 may contain a material that can be used as an active material for an all-solid-state lithium-ion battery, in addition to the composite oxide represented by the formula (1).
  • LiCoO 2 LiNi x Co 1-x O 2 (0 ⁇ x ⁇ 0.5), LiNi 1/3 Co 1/3 Mn 1/3. O 2 , LiMnO 2 , dissimilar element substituted Li-Mn spinels (eg LiMn 1.5 Ni 0.5 O 4 , LiMn 1.5 Al 0.5 O 4 , LiMn 1.5 Mg 0.5 O 4 , LiMn 1.5 Co 0.5 O 4 , LiMn 1.5 Fe 0.5 O 4 , Or LiMn 1.5 Zn 0.5 O 4 ), lithium titanate (eg Li 4 Ti 5 O 12 ), lithium metal phosphate (eg LiFePO 4 , LiMnPO 4 , LiCoPO 4 , or LiNiPO 4 ), transition metal oxides (eg V 2). O 5 , MoO 3 ).
  • LiCoO 2 , LiNi x Co 1-x O 2 (0 ⁇ x ⁇ 0.5), LiNi 1/3 Co 1/3 Mn 1/3 O 2 , LiMnO 2 , dissimilar element substitution Li- A lithium-containing composite oxide selected from Mn spinel, lithium metal phosphate, and the like is preferable.
  • the positive electrode active material 110 has a water content of 2.9 mass ppm or more and 44.7 mass ppm or less. By suppressing the amount of water in the positive electrode active material 110 to 44.7 mass ppm or less, the solid electrolyte 100 described later is deteriorated by the water contained in the positive electrode active material 110 when applied to an all-solid lithium-ion battery. It can be suppressed and the solid electrolyte 100 maintains high conductivity. Therefore, by using the positive electrode active material 110, a battery having a low battery resistance can be obtained.
  • the solid electrolyte 100 is oxidatively decomposed by contact with the positive electrode active material 110 as the battery is charged, and the battery resistance is low. Batteries are obtained.
  • LiNi x Me 1-x O 2 has a composition of 0.5 ⁇ x ⁇ 1 and there is a concern that it will deteriorate due to the reaction between the physically adsorbed water and the active material during high temperature drying, so the physically adsorbed water can be sufficiently removed at low temperatures. It is desirable to do.
  • the positive electrode active material 110 is dried by being heated in advance in the range of 70 ° C. or higher and lower than 120 ° C. for 12 hours or more and 500 hours or less before forming the positive electrode material.
  • the positive electrode active material 110 is, for example, preheated in a range of 70 ° C. or higher and lower than 120 ° C. for 12 hours or more and 500 hours or less before forming the positive electrode material, and at a temperature of 150 ° C. or higher and lower than 500 ° C. It is dried by at least one selected from the group consisting of heating for 5 hours or more and heating at a temperature of 600 ° C. or higher and 850 ° C. or lower for 0.5 hours or longer.
  • the atmosphere at the time of drying may be an atmosphere with a dew point of -60 ° C or less under vacuum or normal pressure. As long as the dew point is ⁇ 60 ° C. or lower, it may be in nitrogen gas or oxygen gas.
  • the dried positive electrode active material 110 is measured by a Karl Fischer moisture measuring device for the amount of moisture generated when heated at 180 ° C.
  • Heating in the range of 70 ° C. or higher and lower than 120 ° C. may be 12 hours or more and 350 hours or less, and further, 24 hours or more and 350 hours or less.
  • At least one selected from the group consisting of heating at a temperature of 150 ° C. or higher and lower than 500 ° C. and heating at a temperature of 600 ° C. or higher and 850 ° C. or lower is 0.5 hours or more and 24 hours or less, and further 1 hour or more and 12 hours. It may be as follows.
  • the positive electrode active material 110 may have a water content of 30 mass ppm or less when heated at 180 ° C. by the Karl Fischer titration method, and may be further 20 mass ppm or less. That is, the amount of water generated when heated to 180 ° C. by the Karl Fischer titration method may be 2.9 mass ppm or more and 30 mass ppm or less, or 2.9 mass ppm or more and 20 mass ppm or less.
  • the positive electrode active material 110 may be provided with a coating material 120 on the surface.
  • the covering material 120 may cover the entire surface of the positive electrode active material 110, or may partially cover the surface.
  • the coating material 120 may contain Li and at least one element selected from the group consisting of O, F, and Cl.
  • the coating material 120 is selected from the group consisting of lithium niobate, lithium phosphate, lithium titanate, lithium tungstate, lithium zirconium fluoride, lithium aluminium fluoride, lithium titanium fluoride, and lithium magnesium fluoride. It may contain at least one that is to be.
  • FIG. 1 schematically shows the configuration of the positive electrode material 1000.
  • the positive electrode material 1000 includes a positive electrode active material 110 and a solid electrolyte 100.
  • a halide solid electrolyte may be used as the solid electrolyte material contained in the solid electrolyte 100.
  • the solid electrolyte 100 may be a compound represented by the following formula (2).
  • ⁇ , ⁇ , and ⁇ are values larger than 0.
  • M comprises at least one selected from the group consisting of metallic elements other than Li and metalloid elements.
  • X is at least one element selected from the group consisting of F, Cl, Br, and I.
  • the metalloid element is B, Si, Ge, As, Sb, or Te.
  • Metallic elements are all elements contained in the first to twelfth groups of the periodic table except hydrogen, and the thirteenth group excluding the above-mentioned metalloid elements, C, N, P, O, S, and Se. All elements contained in Group 16 from. That is, the metal element is a group of elements that can become cations when a halogen compound and an inorganic compound are formed.
  • Li 3 YX 6 Li 2 MgX 4 , Li 2 FeX 4 , Li (Al, Ga, In) X 4 , Li 3 (Al, Ga, In) X 6 and the like can be used. ..
  • X is at least one selected from the group consisting of F, Cl, Br, and I.
  • (A, B, C) means "at least one selected from the group consisting of A, B, and C”.
  • the resistance of the battery can be reduced.
  • X may contain at least one selected from the group consisting of Cl and Br.
  • M may include yttrium (Y).
  • the solid electrolyte containing Y may be, for example, a compound represented by the composition formula of Li a M'b Y c X 6.
  • M' is at least one selected from the group consisting of metal elements and metalloid elements other than Li and Y.
  • m indicates the valence of M'.
  • X is at least one selected from the group consisting of F, Cl, Br, and I.
  • M' at least one selected from the group consisting of Mg, Ca, Sr, Ba, Zn, Sc, Al, Ga, Bi, Zr, Hf, Ti, Sn, Ta, and Nb may be used.
  • solid electrolytes containing Y Li 3 YF 6 , Li 3 YCl 6 , Li 3 YBr 6 , Li 3 YI 6 , Li 3 YBrCl 5 , Li 3 YBr 3 Cl 3 , Li 3 YBr 5 Cl, Li.
  • the resistance of the battery can be further reduced.
  • the halide solid electrolyte does not have to contain sulfur.
  • the shapes of the solid electrolyte 100 and the positive electrode active material 110 in the first embodiment are not particularly limited, and may be, for example, needle-shaped, spherical, elliptical spherical, or the like.
  • the shapes of the solid electrolyte 100 and the positive electrode active material 110 may be in the form of particles.
  • the median diameter may be 100 ⁇ m or less.
  • the positive electrode active material 110 and the solid electrolyte 100 can form a good dispersed state in the positive electrode material 1000. This improves the charge / discharge characteristics of the battery.
  • the median diameter of the solid electrolyte 100 may be 10 ⁇ m or less.
  • the positive electrode active material 110 and the solid electrolyte 100 can form a good dispersed state.
  • the median diameter of the solid electrolyte 100 may be smaller than the median diameter of the positive electrode active material 110.
  • the solid electrolyte 100 and the positive electrode active material 110 can form a better dispersed state in the positive electrode material 1000.
  • the median diameter of the positive electrode active material 110 may be 0.1 ⁇ m or more and 100 ⁇ m or less.
  • the positive electrode active material 110 When the median diameter of the positive electrode active material 110 is 0.1 ⁇ m or more, the positive electrode active material 110 and the solid electrolyte 100 can form a good dispersed state in the positive electrode material 1000. As a result, the charge / discharge characteristics of the battery are improved.
  • the median diameter of the positive electrode active material 110 is 100 ⁇ m or less, the diffusion rate of lithium in the positive electrode active material 110 is sufficiently secured. Therefore, it is possible to operate the battery at a high output.
  • volume diameter means the particle size when the cumulative volume in the volume-based particle size distribution is equal to 50%.
  • the volume-based particle size distribution is measured, for example, by a laser diffraction measuring device or an image analysis device.
  • the particles of the solid electrolyte 100 and the particles of the positive electrode active material 110 may be in contact with each other as shown in FIG. At this time, the coating material 120 and the positive electrode active material 110 are in contact with each other.
  • the positive electrode material 1000 in the first embodiment may include particles of a plurality of solid electrolytes 100 and particles of a plurality of positive electrode active materials 110.
  • the content of the solid electrolyte 100 and the content of the positive electrode active material 110 in the positive electrode material 1000 in the first embodiment may be the same or different from each other.
  • FIG. 1 is a cross-sectional view showing a schematic configuration of the battery 2000 according to the second embodiment.
  • the battery 2000 in the second embodiment includes a positive electrode 201, an electrolyte layer 202, and a negative electrode 203.
  • the positive electrode 201 contains the positive electrode material 1000.
  • the electrolyte layer 202 is arranged between the positive electrode 201 and the negative electrode 203.
  • the discharge voltage of the battery can be improved.
  • the thickness of the positive electrode 201 may be 10 ⁇ m or more and 500 ⁇ m or less. When the thickness of the positive electrode 201 is 10 ⁇ m or more, the energy density of the battery 2000 is sufficiently secured. When the thickness of the positive electrode 201 is 500 ⁇ m or less, operation at high output is possible.
  • the electrolyte layer 202 is a layer containing an electrolyte material.
  • the electrolyte material is, for example, a solid electrolyte material. That is, the electrolyte layer 202 may be a solid electrolyte layer.
  • the material exemplified as the material of the solid electrolyte 100 in the first embodiment may be used. That is, the electrolyte layer 202 may contain a solid electrolyte having the same composition as that of the solid electrolyte 100 contained in the positive electrode material 1000.
  • the electrolyte layer 202 may contain a halide solid electrolyte having a composition different from that of the solid electrolyte contained in the positive electrode material 1000.
  • the electrolyte layer 202 may contain a sulfide solid electrolyte.
  • the electrolyte layer 202 may contain only one type of solid electrolyte selected from the above-mentioned group of solid electrolytes, or may contain two or more types of solid electrolytes selected from the above-mentioned group of solid electrolytes. .. Multiple solid electrolytes have different compositions from each other.
  • the electrolyte layer 202 may contain a halide solid electrolyte and a sulfide solid electrolyte.
  • the thickness of the electrolyte layer 202 may be 1 ⁇ m or more and 300 ⁇ m or less. When the thickness of the electrolyte layer 202 is 1 ⁇ m or more, the positive electrode 201 and the negative electrode 203 are unlikely to be short-circuited. When the thickness of the electrolyte layer 202 is 300 ⁇ m or less, operation at high output is possible.
  • the negative electrode 203 contains a material having the property of occluding and releasing metal ions (for example, lithium ions).
  • the negative electrode 203 contains, for example, a negative electrode active material.
  • a metal material, a carbon material, an oxide, a nitride, a tin compound, a silicon compound, etc. can be used as the negative electrode active material.
  • the metal material may be a single metal.
  • the metal material may be an alloy.
  • metal materials include lithium metals, lithium alloys, and the like.
  • carbon materials include natural graphite, coke, developing carbon, carbon fiber, spherical carbon, artificial graphite, amorphous carbon, and the like. From the viewpoint of capacitance density, silicon (Si), tin (Sn), a silicon compound, or a tin compound can be preferably used.
  • the negative electrode 203 may contain a solid electrolyte material. According to the above configuration, the lithium ion conductivity inside the negative electrode 203 is enhanced, and operation at high output becomes possible.
  • the solid electrolyte the material exemplified in the first embodiment may be used. That is, the negative electrode 203 may contain a solid electrolyte having the same composition as that of the solid electrolyte contained in the positive electrode material 1000.
  • the median diameter of the negative electrode active material may be 0.1 ⁇ m or more and 100 ⁇ m or less.
  • the median diameter of the negative electrode active material is 0.1 ⁇ m or more, the negative electrode active material and the solid electrolyte material can form a good dispersed state. As a result, the charge / discharge characteristics of the battery are improved.
  • the median diameter of the negative electrode active material is 100 ⁇ m or less, the diffusion rate of lithium in the negative electrode active material is sufficiently secured. Therefore, it is possible to operate the battery at a high output.
  • 30 ⁇ v2 ⁇ 95 may be satisfied with respect to the volume ratio “v2: 100-v2” of the negative electrode active material and the solid electrolyte material contained in the negative electrode 203.
  • the energy density of the battery 2000 is sufficiently secured.
  • v2 ⁇ 95 is satisfied, operation at high output becomes possible.
  • the thickness of the negative electrode 203 may be 10 ⁇ m or more and 500 ⁇ m or less. When the thickness of the negative electrode 203 is 10 ⁇ m or more, the energy density of the battery 2000 is sufficiently secured. When the thickness of the negative electrode 203 is 500 ⁇ m or less, operation at high output is possible.
  • At least one selected from the group consisting of the positive electrode 201, the electrolyte layer 202, and the negative electrode 203 may contain a binder for the purpose of improving the adhesion between the particles.
  • the binder is used to improve the binding property of the material constituting the electrode.
  • polyvinylidene fluoride polytetrafluoroethylene, polyethylene, polypropylene, aramid resin, polyamide, polyimide, polyamideimide, polyacrylic nitrile, polyacrylic acid, polyacrylic acid methyl ester, polyacrylic acid ethyl ester, poly Acrylic acid hexyl ester, polymethacrylic acid, polymethacrylic acid methyl ester, polymethacrylic acid ethyl ester, polymethacrylic acid hexyl ester, polyvinylidene acetate, polyvinylpyrrolidone, polyether, polyether sulfone, hexafluoropolypropylene, styrene butadiene rubber, Carboxymethyl cellulose, etc.
  • the binders include tetrafluoroethylene, hexafluoroethylene, hexafluoropropylene, perfluoroalkyl vinyl ether, vinylidene fluoride, chlorotrifluoroethylene, ethylene, propylene, pentafluoropropylene, fluoromethyl vinyl ether, acrylic acid, and hexadiene. Copolymers of two or more materials selected from the above can be used. Further, two or more kinds selected from these may be mixed and used as a binder.
  • At least one selected from the group consisting of the positive electrode 201 and the negative electrode 203 may contain a conductive auxiliary agent for the purpose of enhancing electronic conductivity.
  • the conductive auxiliary agent include graphites of natural graphite or artificial graphite, carbon blacks such as acetylene black and ketjen black, conductive fibers such as carbon fibers or metal fibers, and metal powders such as carbon fluoride and aluminum.
  • conductive whiskers such as zinc oxide or potassium titanate, conductive metal oxides such as titanium oxide, conductive polymer compounds such as polyaniline, polypyrrole, polythiophene, and the like can be used.
  • the cost can be reduced.
  • the battery according to the second embodiment can be configured as a battery having various shapes such as a coin type, a cylindrical type, a square type, a sheet type, a button type, a flat type, and a laminated type.
  • Example 1 [Preparation of positive electrode active material]
  • the positive electrode active material LiNi 0.8 (Co, Mn) 0.2 O 2 was vacuum dried at 100 ° C. for 2 weeks and then taken out in a dry atmosphere with a dew point of ⁇ 20 ° C. or lower.
  • LiNi 0.8 (Co, Mn) 0.2 O 2 is referred to as NCM. In this way, the positive electrode active material of Example 1 was obtained.
  • the positive electrode active material could sufficiently remove the physically adsorbed water by vacuum drying at 100 ° C. for 2 weeks. Specifically, it was confirmed that the water content of the positive electrode active material according to this example measured by the Karl Fischer titration method at 120 ° C. was 1 ppm or less.
  • the water content of the prepared positive electrode active material of Example 1 was measured with a Karl Fischer water content measuring device (CA-310 manufactured by Mitsubishi Chemical Analytech). The heating temperature of the measurement sample was set to 180 ° C. The water content of the positive electrode active material of Example 1 was 44.7 mass ppm.
  • Li 3 YBr 2 Cl 4 and the positive electrode active material of Example 1 were weighed in a mass ratio of 20:80 in an argon glove box having a dew point of ⁇ 60 ° C. or lower. By mixing these in an agate mortar, the positive electrode material of Example 1 was prepared.
  • metal Li thickness 200 ⁇ m
  • metal Li thickness 200 ⁇ m
  • Example 1 was produced by sealing the inside of the insulating outer cylinder from the outside air atmosphere by sealing the insulating outer cylinder using an insulating ferrule.
  • the battery was placed in a constant temperature bath at 25 ° C and connected to a potentiostat (manufactured by Solartron) equipped with a frequency response analyzer.
  • Constant current charging was performed at a current value of 96 ⁇ A, which is a 0.05 C rate (20 hour rate) with respect to the theoretical capacity of the battery, and charging was completed at a voltage of 4.3 V.
  • reaction resistance of the battery at room temperature was measured by the electrochemical AC impedance measurement method.
  • FIG. 2 is a Nyquist diagram showing an example of the evaluation result of the reaction resistance by the AC impedance measurement.
  • the waveform of the semi-circular arc appearing in the obtained Nyquist diagram is assigned to the resistance between the positive electrode resistance and the negative electrode In, and the value of the positive electrode resistance is calculated by performing a fitting analysis.
  • the reaction resistance of the positive electrode of the battery was 49 ⁇ .
  • Example 3 After vacuum drying the NCM at 100 ° C. for 2 weeks, it was calcined at 400 ° C. for 1 hour in a nitrogen gas atmosphere. Then, it was taken out in a dry atmosphere with a dew point of ⁇ 20 ° C. or lower. In this way, the positive electrode active material of Example 3 was obtained.
  • Example 4 After vacuum drying the NCM at 100 ° C. for 2 weeks, it was calcined at 800 ° C. for 1 hour in a nitrogen gas atmosphere. Then, it was taken out in a dry atmosphere with a dew point of ⁇ 20 ° C. or lower. In this way, the positive electrode active material of Example 4 was obtained.
  • the positive electrode active material of Example 6 was obtained in the same manner as in Example 3.
  • Example 7 After vacuum drying the NCM at 100 ° C. for 2 weeks, it was calcined at 450 ° C. for 1 hour in a nitrogen gas atmosphere. Then, it was taken out in a dry atmosphere with a dew point of ⁇ 20 ° C. or lower. In this way, the positive electrode active material of Example 7 was obtained.
  • the positive electrode active material of Example 8 was obtained in the same manner as in Example 4.
  • the positive electrode materials of Examples 6 to 8 were prepared in the same manner as in Example 5.
  • the batteries of Examples 6 to 8 were produced in the same manner as in Example 5.
  • the water content of the positive electrode active material of Comparative Example 1 was measured in the same manner as in Example 1.
  • the water content of the positive electrode active material of Comparative Example 1 was 274.8 mass ppm.
  • Li 3 YBr 2 Cl 4 and the positive electrode active material of Comparative Example 1 were weighed in a weight ratio of 20:80 in an argon glove box having a dew point of ⁇ 60 ° C. or lower. By mixing these in an agate mortar, the positive electrode material of Comparative Example 1 was prepared.
  • the water content of the prepared positive electrode active material of Comparative Example 2 was measured in the same manner as in Example 1.
  • the heating temperature of the measurement sample was set to 180 ° C.
  • the water content of the positive electrode active material of Comparative Example 2 was 2.5 mass ppm.
  • Li 3 YBr 2 Cl 4 and the positive electrode active material of Comparative Example 2 were weighed in a weight ratio of 20:80 in an argon glove box having a dew point of ⁇ 60 ° C. or lower. By mixing these in an agate mortar, the positive electrode material of Comparative Example 2 was prepared.
  • Example 1 shows, when the amount of water generated when heating at 180 ° C. by the Karl Fischer titration method of the positive electrode active material is 2.9 mass ppm or more and 44.7 mass ppm or less, the reaction resistance of the battery is high. It turns out to be low. This is to suppress the hydration and hydrolysis of the halide solid electrolyte Li 3 YBr 2 Cl 4 by reducing the water content of the positive electrode active material.
  • Comparative Example 2 shows, when the amount of water generated when heating at 180 ° C. is less than 2.9 mass ppm by the Karl Fischer titration method of the positive electrode active material, it can be seen that the reaction resistance of the battery is large. This is because the hydration and hydrolysis of the halide solid electrolyte Li 3 YBr 2 Cl 4 were suppressed too much, so that the positive electrode active material powder and the halide solid electrolyte Li 3 YBr 2 Cl 4 came into contact with each other, and the battery was charged. This is because it is oxidatively decomposed.
  • the reaction resistance of the battery is large when the temperature of the positive electrode active material at the time of drying is 500 ° C. This is because the temperature affects the surface condition of the active material. For example, when the drying temperature reaches 500 ° C., it is considered that the surface of the active material becomes in a state where the reaction resistance increases. Further, when the temperature at the time of drying becomes 600 ° C. or higher, which is a higher temperature, it is considered that the surface of the active material is in a state where the reaction resistance is lowered.
  • the internal resistance of the battery during charging can be reduced.
  • Positive electrode material 100 Solid electrolyte 110 Positive electrode active material 120 Coating material 2000 Battery 201 Positive electrode 202 Electrolyte layer 203 Negative electrode

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PCT/JP2021/019285 2020-05-27 2021-05-21 正極活物質、正極材料、電池、および正極活物質の製造方法 Ceased WO2021241416A1 (ja)

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WO2024096107A1 (ja) * 2022-11-04 2024-05-10 住友化学株式会社 電池
EP4362135A4 (en) * 2021-06-24 2024-11-13 Panasonic Intellectual Property Management Co., Ltd. POSITIVE ELECTRODE ACTIVE SUBSTANCE, COATED POSITIVE ELECTRODE ACTIVE SUBSTANCE, POSITIVE ELECTRODE MATERIAL AND BATTERY
WO2024262182A1 (ja) * 2023-06-21 2024-12-26 パナソニックホールディングス株式会社 被覆活物質、正極材料、および電池
WO2024262183A1 (ja) * 2023-06-21 2024-12-26 パナソニックホールディングス株式会社 被覆活物質、正極材料、および電池
EP4404303A4 (en) * 2021-09-13 2025-07-30 Panasonic Ip Man Co Ltd COATED ACTIVE MATERIAL, METHOD FOR PRODUCING COATED ACTIVE MATERIAL, POSITIVE ELECTRODE MATERIAL, AND BATTERY
EP4459695A4 (en) * 2021-12-28 2025-11-19 Panasonic Ip Man Co Ltd POSITIVE ELECTRODE FOR RECHARGEABLE BATTERIES AND PROCESS FOR PRODUCING ACTIVE MATERIAL FOR POSITIVE ELECTRODE FOR RECHARGEABLE BATTERIES

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EP4362135A4 (en) * 2021-06-24 2024-11-13 Panasonic Intellectual Property Management Co., Ltd. POSITIVE ELECTRODE ACTIVE SUBSTANCE, COATED POSITIVE ELECTRODE ACTIVE SUBSTANCE, POSITIVE ELECTRODE MATERIAL AND BATTERY
EP4404303A4 (en) * 2021-09-13 2025-07-30 Panasonic Ip Man Co Ltd COATED ACTIVE MATERIAL, METHOD FOR PRODUCING COATED ACTIVE MATERIAL, POSITIVE ELECTRODE MATERIAL, AND BATTERY
EP4459695A4 (en) * 2021-12-28 2025-11-19 Panasonic Ip Man Co Ltd POSITIVE ELECTRODE FOR RECHARGEABLE BATTERIES AND PROCESS FOR PRODUCING ACTIVE MATERIAL FOR POSITIVE ELECTRODE FOR RECHARGEABLE BATTERIES
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WO2024262183A1 (ja) * 2023-06-21 2024-12-26 パナソニックホールディングス株式会社 被覆活物質、正極材料、および電池

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CN115699365A (zh) 2023-02-03
CN115699365B (zh) 2026-03-20
US20230075889A1 (en) 2023-03-09
EP4159686A1 (en) 2023-04-05

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