WO2021152764A1 - Procédé et dispositif de fabrication de matière d'électrode négative pour batterie secondaire au lithium-ion - Google Patents

Procédé et dispositif de fabrication de matière d'électrode négative pour batterie secondaire au lithium-ion Download PDF

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Publication number
WO2021152764A1
WO2021152764A1 PCT/JP2020/003382 JP2020003382W WO2021152764A1 WO 2021152764 A1 WO2021152764 A1 WO 2021152764A1 JP 2020003382 W JP2020003382 W JP 2020003382W WO 2021152764 A1 WO2021152764 A1 WO 2021152764A1
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WIPO (PCT)
Prior art keywords
negative electrode
electrode material
ion secondary
lithium ion
secondary battery
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PCT/JP2020/003382
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English (en)
Japanese (ja)
Inventor
高志 久保田
清志 鈴木
健志 政吉
泰裕 加藤
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昭和電工マテリアルズ株式会社
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Priority to PCT/JP2020/003382 priority Critical patent/WO2021152764A1/fr
Publication of WO2021152764A1 publication Critical patent/WO2021152764A1/fr

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—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
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • C01B32/20—Graphite
    • C01B32/205—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Definitions

  • the present invention relates to a method for manufacturing a negative electrode material for a lithium ion secondary battery and an apparatus for manufacturing a negative electrode material for a lithium ion secondary battery.
  • Lithium-ion secondary batteries have a higher energy density than other secondary batteries such as nickel-cadmium batteries, nickel-hydrogen batteries, and lead-acid batteries, so they are widely used as power sources for portable electrical appliances such as laptop computers and mobile phones. It is used. Further, it is expected that lithium ion secondary batteries will be used not only for relatively small electric appliances but also for electric vehicles, power sources for storing electricity, and the like.
  • Graphite is widely used as the negative electrode material (negative electrode material) for lithium-ion secondary batteries.
  • a method for producing a negative electrode material using graphite for example, in Patent Document 1, a mixture obtained by mixing a carbon material, a binder and the like is heated to perform graphitization treatment, and the obtained graphitized product is further pulverized. The method is described.
  • a catalyst for promoting graphitization may be added to the mixture obtained by mixing the carbon material and the binder or the like. It is considered that most of the catalyst is decomposed by heating in the graphitization step (for example, when silicon carbide is used as a catalyst, carbon atoms form a graphite skeleton and silicon atoms sublimate). However, depending on the heating state (for example, the temperature distribution inside the heating furnace), the decomposition or sublimation of the catalyst may not proceed sufficiently, and components other than carbon derived from the catalyst may remain in a part of the graphitized product obtained. .. It is desirable that the amount of the catalyst-derived component in the graphitized product is small from the viewpoint of quality assurance of the negative electrode material. On the other hand, if the graphitization step is carried out so that the catalyst is completely removed, the production cost may increase.
  • Irradiation process of irradiating an object containing carbon with electromagnetic waves A method for manufacturing a negative electrode material for a lithium ion secondary battery, comprising a detection step of determining the presence or absence of a detection target contained in the object based on the data obtained by the irradiation.
  • a method for manufacturing a negative electrode material for a lithium ion secondary battery comprising a detection step of determining the presence or absence of a detection target contained in the object based on the data obtained by the irradiation.
  • ⁇ 4> The method for producing a negative electrode material for a lithium ion secondary battery according to any one of ⁇ 1> to ⁇ 3>, wherein the dimension of the object in the irradiation direction of the electromagnetic wave is 50 mm to 180 mm.
  • ⁇ 5> The method for producing a negative electrode material for a lithium ion secondary battery according to any one of ⁇ 1> to ⁇ 4>, wherein the detection target contains silicon.
  • the negative electrode material for a lithium ion secondary battery according to ⁇ 6> for use in the method for producing a negative electrode material for a lithium ion secondary battery according to any one of ⁇ 1> to ⁇ 5>. Manufacturing equipment.
  • a method for manufacturing a negative electrode material for a lithium ion secondary battery capable of producing a negative electrode material having excellent quality with high productivity, and an apparatus for manufacturing a negative electrode material for a lithium ion secondary battery.
  • the present invention is not limited to the following embodiments.
  • the components including element steps and the like are not essential unless otherwise specified and clearly considered to be essential in principle.
  • the term "process” includes not only a process independent of other processes but also the process if the purpose of the process is achieved even if the process cannot be clearly distinguished from the other process. ..
  • the numerical range indicated by using "-" in the present disclosure includes the numerical values before and after "-" as the minimum value and the maximum value, respectively.
  • each component may contain a plurality of applicable substances.
  • the content or content of each component is the total content or content of the plurality of substances present in the composition unless otherwise specified. Means quantity.
  • a plurality of types of particles corresponding to each component may be contained.
  • the particle size of each component means a value for a mixture of the plurality of particles present in the composition unless otherwise specified.
  • the term "layer” refers to the case where the layer is formed in the entire region when the region where the layer is present is observed, and also when the layer is formed only in a part of the region. included.
  • the method for producing a negative electrode material for a lithium ion secondary battery (hereinafter, also simply referred to as a negative electrode material) of the present disclosure includes an irradiation step of irradiating an object containing carbon with an electromagnetic wave.
  • the present invention includes a detection step of determining the presence or absence of a detection target included in the object based on the data obtained by the irradiation.
  • the presence or absence of a detection target included in the object is determined based on the data obtained by irradiating the object with electromagnetic waves. Therefore, it is possible to select and remove only the object including the detection target without destroying the object, and the quality of the product as a whole can be improved. Further, by removing an object having a high hardness substance such as silicon on the surface, it can be expected to have an effect of suppressing wear of production equipment. That is, the above method may include a step of removing an object determined to include a detection target after the detection step.
  • the determination of the presence or absence of the detection target is not limited to the determination of whether or not the object does not include the detection target at all, but is the determination of whether or not the content of the detection target exceeds the value set as the allowable range. May be good.
  • the type of electromagnetic wave irradiating the object is not particularly limited as long as it can detect the detection target contained in the object.
  • the detection target contained in the object is not particularly limited as long as it is an element other than carbon. Specific examples thereof include silicon, iron, nickel, titanium and boron. In certain embodiments, the detection target comprises silicon.
  • the method of irradiating the object with electromagnetic waves is not particularly limited as long as it can detect the detection target contained in the object.
  • the object may be irradiated with electromagnetic waves from one direction or two or more directions.
  • the source of the electromagnetic wave may be fixed or mobile.
  • X-rays are used as electromagnetic waves, irradiation intensity: tube voltage 50 kV, tube current 2.0-4.0 mA, tungsten target, irradiation time per object: 0.96 seconds-2.04 seconds.
  • the irradiation step is carried out as.
  • the method of determining the presence or absence of the detection target contained in the object based on the data obtained by irradiating the electromagnetic wave is not particularly limited, and a known method can be used.
  • the criteria for determining the presence or absence of the detection target can be set according to the quality of the desired negative electrode material and the like.
  • the size or shape of the object irradiated with the electromagnetic wave is not particularly limited as long as the surface and the inside detection target can be detected by the irradiation of the electromagnetic wave.
  • the dimension in the irradiation direction of the electromagnetic wave may be 50 mm to 180 mm or 70 mm to 100 mm, the volume may be 3,000 cm 3 to 5,000 cm 3 , and a flat surface such as a rectangular parallelepiped or a cylinder is considered in consideration of handleability. It may have a shape suitable for being placed on top.
  • the carbon-containing object may be a graphite-containing object, the graphite of a mixture containing at least one selected from the group consisting of graphitizable aggregates and graphite, and a graphitizable binder. It may be a product. Details of the mixture containing at least one selected from the group consisting of graphitizable aggregate and graphitizable binder and graphitizable binder will be described later.
  • the above method may include a step of crushing an object containing carbon after a step of irradiating electromagnetic waves and determining the presence or absence of a detection target.
  • pulverizing an object containing carbon into particles having a desired particle size it can be used as a negative electrode material for a lithium ion secondary battery.
  • the method and conditions of pulverization are not particularly limited, and can be carried out by a known method.
  • the apparatus for manufacturing the negative electrode material for a lithium ion secondary battery of the present disclosure includes an irradiation apparatus that irradiates an object containing carbon with an electromagnetic wave.
  • a detection device for determining the presence / absence of a detection target included in the object based on the data obtained by the irradiation is provided.
  • the configuration of the electromagnetic wave irradiation device and the detection device in the above device is not particularly limited, and a known device may be used.
  • the details and preferred embodiments of electromagnetic wave irradiation or detection target detection using the above device are the same as the details and preferred embodiments of magnetic wave irradiation or detection target detection in the above-described negative electrode material manufacturing method.
  • the device may include a moving device that moves an object containing carbon to the irradiation device.
  • the configuration of the mobile device is not particularly limited. From the viewpoint of work efficiency, a device such as a belt conveyor capable of continuously moving an object containing a plurality of carbons is preferable.
  • the above device may include a device for removing an object determined to include a detection target among the objects for which the presence or absence of a detection target included in the object is determined based on the data obtained by irradiation with electromagnetic waves.
  • the above device may be used, for example, in the above-mentioned method for manufacturing a negative electrode material.
  • the particles may include particles (secondary particles) in which a plurality of particles are aggregated or bonded, and the plurality of flat graphite particles have the main surfaces of the graphite particles non-parallel to each other.
  • the particles may be aggregated or combined so as to be.
  • graphite secondary particles particles in which a plurality of flat graphite particles are aggregated or bonded so that the main surfaces of the graphite particles are non-parallel to each other are particularly referred to as “graphite secondary particles”.
  • the negative electrode material When the negative electrode material is in the state of graphite secondary particles, the phenomenon that the particles of the negative electrode material are oriented along the direction of the current collector when the press for increasing the density of the negative electrode is performed is suppressed, and the negative electrode material is used. There is a tendency to secure a sufficient route for lithium ions to enter and exit.
  • the effect of the pressure applied during pressing on the individual graphite particles is reduced by the voids existing between the plurality of flat graphite particles constituting the graphite secondary particles, and the destruction of the graphite particles and the generation of cracks are suppressed. Tends to be.
  • the "flat graphite particles” refer to non-spherical graphite particles having anisotropy in shape.
  • examples of the flat graphite particles include graphite particles having a shape such as scaly, scaly, and partially lumpy.
  • the aspect ratio represented by A / B of the flat graphite particles is, for example, 1.2 to 20, when the length in the major axis direction is A and the length in the minor axis direction is B. Is preferable, and 1.3 to 10 is more preferable.
  • the aspect ratio is 1.2 or more, the contact area between the particles increases, and the conductivity tends to be further improved.
  • the aspect ratio is 20 or less, the input / output characteristics such as the rapid charge / discharge characteristics of the lithium ion secondary battery tend to be further improved.
  • the aspect ratio is obtained by observing graphite particles with a microscope, arbitrarily selecting 100 graphite particles, measuring each A / B, and taking the arithmetic mean value of those measured values.
  • the length A in the major axis direction and the length B in the minor axis direction are measured as follows. That is, in the projected image of the graphite particles observed using a microscope, two parallel tangents circumscribing the outer periphery of the graphite particles, the tangent line a1 and the tangent line a2 having the maximum distance are selected, and the tangent line a1 and the tangent line a2 are selected.
  • the distance between the tangent line a1 and the tangent line a2 is defined as the length A in the major axis direction. Further, two parallel tangents circumscribing the outer periphery of the graphite particles, the tangent line b1 and the tangent line b2 having the minimum distance are selected, and the distance between the tangent line b1 and the tangent line b2 is set in the minor axis direction. Let the length be B.
  • the main surfaces of the plurality of flat graphite particles are non-parallel means that the surfaces (main surfaces) having the largest cross-sectional areas of the plurality of flat graphite particles are not aligned in a certain direction. say. Whether or not the main surfaces of the plurality of flat graphite particles are non-parallel to each other can be confirmed by microscopic observation.
  • the graphite secondary particles may partially include a structure in which a plurality of flat graphite particles are assembled or bonded so that their main surfaces are parallel to each other.
  • the "state in which a plurality of flat graphite particles are aggregated or bonded” means a state in which two or more flat graphite particles are aggregated or bonded.
  • “Bond” refers to a state in which particles are chemically bonded to each other either directly or via a carbon substance.
  • the “aggregate” refers to a state in which the particles are not chemically bonded to each other, but the shape of the aggregate is maintained due to its shape or the like.
  • the flat graphite particles may be aggregated or bonded via a carbon substance. Examples of the carbon substance include graphitized binders that can be graphitized. From the viewpoint of mechanical strength, it is preferable that two or more flat graphite particles are bonded to each other via a carbon substance. Whether or not the flat graphite particles are aggregated or bonded can be confirmed by, for example, observation with a scanning electron microscope.
  • the average particle size of the flat graphite particles is preferably, for example, 1 ⁇ m to 50 ⁇ m, more preferably 1 ⁇ m to 25 ⁇ m, and 1 ⁇ m to 15 ⁇ m from the viewpoint of ease of assembly or bonding. More preferred.
  • Examples of the method for measuring the average particle size of the flat graphite particles include a method of measuring with a scanning electron microscope.
  • the flat graphite particles and their raw materials are not particularly limited, and examples thereof include artificial graphite, scaly natural graphite, scaly natural graphite, coke, resin, tar, and pitch.
  • graphite obtained from artificial graphite, natural graphite, or coke has high crystallinity and becomes soft particles, so that the density of the negative electrode tends to be easily increased.
  • the negative electrode material may contain spherical graphite particles.
  • the spherical graphite particles themselves have a high density, so that the pressing pressure required to obtain a desired electrode density tends to be reduced.
  • spherical graphite particles examples include spherical artificial graphite and spherical natural graphite.
  • the spherical graphite particles are preferably high-density graphite particles. Specifically, it is preferably spherical natural graphite that has been subjected to a particle spheroidizing treatment so that the tap density can be increased. Further, the negative electrode material layer containing spherical natural graphite has excellent peel strength and tends to be difficult to peel from the current collector even when pressed with a strong force.
  • the negative electrode material may contain the above-mentioned graphite secondary particles and spherical graphite particles.
  • the ratio of the two is not particularly limited and can be set according to a desired electrode density, pressure conditions during pressing, desired battery characteristics, and the like. ..
  • the negative electrode material contains graphite secondary particles and spherical graphite particles, a state in which the graphite secondary particles and spherical graphite particles are mixed, and a state in which the graphite secondary particles and spherical graphite particles are bonded.
  • composite particles include particles in which secondary graphite particles and spherical graphite particles are bonded via an organic carbide.
  • the average particle size of the negative electrode material produced by the above method is not particularly limited. For example, it is preferably 5 ⁇ m to 40 ⁇ m, more preferably 10 ⁇ m to 30 ⁇ m, and even more preferably 10 ⁇ m to 25 ⁇ m.
  • the average particle size may be measured with a scanning electron microscope in the same manner as the average particle size of the flat graphite particles described above, or may be a volume average particle size measured by a laser diffraction / scattering method.
  • a sample electrode is prepared, the electrode is embedded in an epoxy resin, and then mirror-polished to scan the electrode cross section with a scanning electron microscope.
  • a scanning electron microscope For example, "VE-7800” manufactured by Keyence Co., Ltd.
  • an electrode cross section is prepared using an ion milling device (for example, "E-3500” manufactured by Hitachi High-Technologies Co., Ltd.) and a scanning electron. Examples thereof include a method of measuring with a microscope (for example, “VE-7800” manufactured by Keyence Co., Ltd.).
  • the average particle size in this case is the median value of 100 particle sizes arbitrarily selected from the observed particles.
  • the sample electrode for example, a mixture of 98 parts by mass of the negative electrode material, 1 part by mass of styrene-butadiene resin as a binder, and 1 part by mass of carboxymethyl cellulose as a thickener is used as a solid content, and water is added to prepare a dispersion. Then, the dispersion liquid is coated on a copper foil having a thickness of 10 ⁇ m so as to have a thickness of about 70 ⁇ m (at the time of coating), and then dried at 105 ° C. for 1 hour to produce the dispersion.
  • the negative electrode material may have an orientation of 700 or less, or 500 or less, when it is used as a negative electrode (a negative electrode after pressing when the production of the negative electrode involves a pressing step).
  • the orientation of the negative electrode material is an index indicating the degree of orientation of the particles of the negative electrode material contained in the negative electrode.
  • the small orientation means that the particles of the negative electrode material are oriented in random directions. That is, it means that the graphite particles are suppressed from being oriented along the surface of the current collector due to the pressure at the time of pressing.
  • the method of obtaining an object containing carbon irradiated with electromagnetic waves is not particularly limited.
  • it may be obtained by a method including the following steps (a) to (c).
  • a step of obtaining a mixture containing at least one selected from the group consisting of graphitizable aggregate and graphite and a graphitizable binder (b) A step of molding the mixture to obtain a molded product (c) ) Step of graphitizing the molded product to obtain a graphitized product
  • step (a) a mixture containing at least one selected from the group consisting of graphitizable aggregate and graphite and a graphitizable binder is obtained.
  • the method for obtaining the mixture is not particularly limited, and it can be carried out using a kneader or the like.
  • the mixing is preferably carried out at a temperature at which the graphitizable binder softens.
  • the temperature may be 50 ° C. to 300 ° C.
  • the binder is a thermosetting resin
  • the temperature may be 20 ° C. to 100 ° C. ..
  • the aggregate that can be graphitized is not particularly limited as long as it is graphitized by the graphitization treatment. Specific examples thereof include coke such as fluid coke, needle coke, and mosaic coke. Examples of graphite include natural graphite and artificial graphite.
  • the graphitizable aggregate or graphite is preferably in the form of particles.
  • the binder that can be graphitized is not particularly limited as long as it is graphitized by the graphitization treatment. Specific examples thereof include coal-based, petroleum-based, artificial pitch and tar, thermoplastic resins, and thermosetting resins.
  • the compounding ratio of each material in the mixture is not particularly limited.
  • the content of the graphitizable binder may be 15 parts by mass to 150 parts by mass, or 30 parts by mass to 130 parts by mass with respect to 100 parts by mass of graphitizable aggregate or graphite. It may be 50 parts by mass to 110 parts by mass.
  • the amount of the binder is 15 parts by mass or more, the fluidity of the mixture is sufficiently ensured, and the moldability tends to be excellent.
  • the amount of the binder is 150 parts by mass or less, the amount of fixed carbon in the mixture is sufficiently secured, and the yield tends to be excellent.
  • the graphitizable aggregate, graphite and graphitizable binder contained in the mixture may be only one type or two or more types, respectively.
  • the mixture may contain components other than these.
  • components other than graphitizable aggregates, graphite and graphitizable binders include fluidity-imparting agents and graphitization catalysts.
  • the mixture contains a fluidity-imparting agent.
  • a fluidity-imparting agent when molding the mixture is performed by extrusion molding, it is preferable to include a fluidity-imparting agent in order to perform molding while flowing the mixture.
  • the inclusion of the fluidity-imparting agent in the mixture leads to a reduction in the amount of the binder that can be graphitized, and can be expected to improve the battery characteristics such as the initial charge / discharge efficiency of the negative electrode material.
  • the type of fluidity-imparting agent is not particularly limited. Specifically, hydrocarbons such as liquid paraffin, paraffin wax and polyethylene wax, fatty acids such as stearic acid, oleic acid, erucic acid and 12-hydroxystearic acid, zinc stearate, lead stearate, aluminum stearate, calcium stearate, Fatty metal salts such as magnesium stearate, stearic acid amide, oleic acid amide, erucic acid amide, methylene bisstearic acid amide, ethylene bisstearic acid amide and other fatty acid amides, stearic acid monoglyceride, stearyl stearate, hardened oil and other fatty acids Examples thereof include higher alcohols such as ester and stearic acid.
  • the amount thereof is not particularly limited.
  • the content of the fluidity-imparting agent in the entire mixture may be 0.1% by mass to 20% by mass, 0.5% by mass to 10% by mass, or 0.5% by mass to 5% by mass. It may be% by mass.
  • the mixture preferably contains a graphitization catalyst.
  • the type of graphitization catalyst is not particularly limited. Specific examples thereof include substances having a graphitizing catalytic action such as silicon, iron, nickel, titanium and boron, and carbides, oxides and nitrides of these substances.
  • the amount thereof is not particularly limited.
  • the content of the graphitizing catalyst in the whole mixture may be 0.1% by mass to 50% by mass, 0.5% by mass to 40% by mass, or 0.5% by mass to 30% by mass. May be%.
  • the mixture obtained in the step (a) is molded to obtain a molded product.
  • the molding of the mixture is carried out in order to increase the filling amount in the graphitizing reactor when graphitizing the mixture to improve the productivity and to improve the effect of the graphitizing catalyst.
  • the molding of the mixture is preferably carried out in a softened state of the graphitizable binder.
  • the softened state of the graphitizable binder contained in the mixture include a state in which the temperature of the mixture is equal to or higher than the temperature at which the graphitizable binder contained in the mixture softens.
  • the softened state of the graphitizable binder is not particularly limited as long as the mixture can be molded into a desired state.
  • the molding of the mixture may be carried out at a temperature of 80 ° C. or higher, or 100 ° C. or higher. From the viewpoint of suppressing the volatilization of volatile components in the mixture, the molding of the mixture may be carried out at a temperature of 200 ° C. or lower, or at 120 ° C. or lower.
  • the mixture formed in the step (b) may be one in which the graphitizable binder is maintained in a softened state after being obtained in the step (a), and once obtained in the step (a). It may be in a state where the graphitizable binder is softened (however, not crushed) by cooling and then heating or the like.
  • the method of molding the mixture is not particularly limited.
  • a molding method in which a mixture is placed in a container such as a mold and pressed in a uniaxial direction, a heavy weight is placed on the upper surface of the mixture in a container such as a mold, and vibration / impact is applied to the mold to form the mold.
  • vibration molding method for forming a mixture examples thereof include a vibration molding method for forming a mixture, and an extrusion molding method in which a mixture is extruded from a nozzle or the like with a horizontal pressing press.
  • the molded product obtained in the step (b) is preferably heat-treated before the molded product is graphitized in the step (c).
  • organic components contained in the mixture that do not contribute to graphitization are removed, and gas generation in the graphitization treatment tends to be suppressed.
  • the temperature of the heat treatment is not particularly limited, but it is preferably a temperature lower than the temperature of the heat treatment in the step (c). For example, it may be carried out in the range of 500 ° C. to 1000 ° C.
  • step (c) the molded product obtained in step (b) is graphitized.
  • the method for graphitizing the molded product is not particularly limited as long as the graphitizable component contained in the mixture can be graphitized.
  • a method of heat-treating the mixture in an atmosphere in which it is difficult to oxidize can be mentioned.
  • the atmosphere in which the mixture is difficult to oxidize is not particularly limited, and examples thereof include an inert atmosphere such as nitrogen and argon, and vacuum.
  • the temperature of the heat treatment for graphitization may be, for example, 1500 ° C. or higher, 2000 ° C. or higher, 2500 ° C. or higher, or 2800 ° C. or higher.
  • the upper limit of the heat treatment temperature is not particularly limited, but may be, for example, 3200 ° C. or lower.
  • the heat treatment temperature is 1500 ° C. or higher, crystal changes occur and graphitization tends to proceed easily.
  • the calcination temperature is 2000 ° C. or higher, the development of graphite crystals tends to be better.
  • the amount of ash derived from the graphitization catalyst remaining tends to be reduced.
  • the temperature of the heat treatment for graphitization is 3200 ° C. or lower, sublimation of a part of graphite tends to be suppressed.
  • the negative electrode material obtained by the manufacturing method or manufacturing apparatus of the present disclosure is used as a material for the negative electrode of a lithium ion secondary battery.
  • the method for producing the negative electrode using the negative electrode material is not particularly limited. For example, a method of forming a negative electrode material layer on a current collector using a composition containing a negative electrode material, a binder, and a solvent, and performing heat treatment, press treatment, or the like, if necessary, can be mentioned.
  • the binder contained in the composition is not particularly limited.
  • a polymer compound containing styrene-butadiene rubber, an ethylenically unsaturated carboxylic acid ester (methyl (meth) acrylate, ethyl (meth) acrylate, butyl (meth) acrylate, hydroxyethyl (meth) acrylate, etc.) as a polymerization component Polymer compounds containing ethylenically unsaturated carboxylic acids (acrylic acid, methacrylic acid, itaconic acid, fumaric acid, maleic acid, etc.) as polymerization components, polyvinylidene fluoride, polyethylene oxide, polyepichlorohydrin, polyphosphazene, polyacrylonitrile , Polypolymeric compounds such as polyimide and polyamideimide.
  • (meth) acrylate means either or both of methacrylate and acrylate.
  • the solvent contained in the composition is not particularly limited. Specifically, organic solvents such as N-methylpyrrolidone, dimethylacetamide, dimethylformamide, and ⁇ -butyrolactone, water, and the like are used.
  • the composition may contain a thickener for adjusting the viscosity, if necessary.
  • a thickener for adjusting the viscosity
  • examples of the thickener include carboxymethyl cellulose, methyl cellulose, hydroxymethyl cellulose, ethyl cellulose, polyvinyl alcohol, polyacrylic acid and salts thereof, oxidized starch, phosphorylated starch, casein and the like.
  • the composition may be mixed with a conductive auxiliary agent, if necessary.
  • a conductive auxiliary agent include carbon black, graphite, acetylene black, oxides exhibiting conductivity, nitrides exhibiting conductivity, and the like.
  • the material and shape of the current collector used to manufacture the negative electrode are not particularly limited.
  • a material such as a band-shaped foil made of a metal or alloy such as aluminum, copper, nickel, titanium, or stainless steel, a band-shaped perforated foil, or a band-shaped mesh can be used.
  • porous materials such as porous metal (foam metal) and carbon paper can also be used.
  • the method of forming the negative electrode material layer on the current collector using the composition is not particularly limited, and is a metal mask printing method, an electrostatic coating method, a dip coating method, a spray coating method, a roll coating method, a doctor blade method, and a gravure. It can be carried out by a known method such as a coating method or a screen printing method.
  • a known method such as a roll, a press, or a combination thereof can be used.
  • heat treatment drying
  • the heat treatment may be carried out in an inert atmosphere such as helium, argon or nitrogen or in a vacuum atmosphere in order to prevent oxidation of the current collector during the treatment.
  • a press treatment may be performed.
  • the electrode density of the negative electrode can be adjusted.
  • the electrode density of the negative electrode is not particularly limited, may be 1.5g / cm 3 ⁇ 1.9g / cm 3, may be 1.6g / cm 3 ⁇ 1.8g / cm 3.
  • the press treatment is preferably performed before the heat treatment.
  • the lithium ion secondary battery manufactured by the above method may include a negative electrode, a positive electrode, and an electrolyte produced by the above method.
  • the lithium ion secondary battery can be configured such that, for example, the negative electrode and the positive electrode are arranged so as to face each other via a separator, and an electrolytic solution containing an electrolyte is injected.
  • the positive electrode may be produced by forming a positive electrode layer on the surface of the current collector in the same manner as the negative electrode.
  • a material such as a band-shaped foil made of a metal or alloy such as aluminum, titanium, or stainless steel, a band-shaped perforated foil, or a band-shaped mesh can be used.
  • the separator examples include non-woven fabrics mainly composed of polyolefins such as polyethylene and polypropylene, cloths, micropore films, and combinations thereof. If the lithium ion secondary battery has a structure in which the positive electrode and the negative electrode do not come into contact with each other, it is not necessary to use a separator.
  • lithium salts such as LiClO 4 , LiPF 6 , LiAsF 6 , LiBF 4 , LiSO 3 CF 3 and the like are used, and ethylene carbonate, propylene carbonate, butylene carbonate, vinylene carbonate, fluoroethylene carbonate, cyclopentanone, sulfolane, 3 -Methyl sulfolane, 2,4-dimethyl sulfolane, 3-methyl-1,3-oxazolidine-2-one, ⁇ -butyrolactone, dimethyl carbonate, diethyl carbonate, ethyl methyl carbonate, methyl propyl carbonate, butyl methyl carbonate, ethyl propyl carbonate , Butyl ethyl carbonate, dipropyl carbonate, 1,2-dimethoxyethane, tetrahydrofuran, 2-methyl tetrahydrofuran, 1,3-dioxolane, methyl
  • organic electrolyte So-called organic electrolyte can be used.
  • the electrolytic solution containing fluoroethylene carbonate tends to form a stable SEI (solid electrolyte interface) on the surface of the negative electrode material, and is suitable because the cycle characteristics are remarkably improved.
  • the form of the lithium ion secondary battery is not particularly limited, and examples thereof include a paper type battery, a button type battery, a coin type battery, a laminated type battery, a cylindrical type battery, and a square type battery.
  • the negative electrode material for a lithium ion secondary battery can be applied to all electrochemical devices such as hybrid capacitors having a charging / discharging mechanism of inserting and removing lithium ions in addition to the lithium ion secondary battery. Is.

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

Abstract

L'invention concerne un procédé de fabrication de matière d'électrode négative pour batterie secondaire au lithium-ion qui comporte : une étape d'irradiation au cours de laquelle des ondes électromagnétiques irradient une substance contenant un carbone ; et une étape de détection au cours de laquelle il est jugé de la présence ou de l'absence d'un objet de détection contenu dans ladite substance sur la base de données obtenues au moyen de ladite irradiation.
PCT/JP2020/003382 2020-01-30 2020-01-30 Procédé et dispositif de fabrication de matière d'électrode négative pour batterie secondaire au lithium-ion WO2021152764A1 (fr)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004239776A (ja) * 2003-02-06 2004-08-26 Mitsubishi Chemicals Corp 炭素質材料の異物検出方法
JP2010267466A (ja) * 2009-05-14 2010-11-25 Hitachi Maxell Ltd 扁平形非水電池
JP2011100565A (ja) * 2009-11-04 2011-05-19 Automotive Energy Supply Corp リチウムイオン二次電池用電極の検査方法、ならびにこれを用いた製造方法および製造装置
JP2012109029A (ja) * 2010-11-15 2012-06-07 Hitachi Ltd リチウム二次電池用電極板の製造装置およびリチウム二次電池の製造方法

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2004239776A (ja) * 2003-02-06 2004-08-26 Mitsubishi Chemicals Corp 炭素質材料の異物検出方法
JP2010267466A (ja) * 2009-05-14 2010-11-25 Hitachi Maxell Ltd 扁平形非水電池
JP2011100565A (ja) * 2009-11-04 2011-05-19 Automotive Energy Supply Corp リチウムイオン二次電池用電極の検査方法、ならびにこれを用いた製造方法および製造装置
JP2012109029A (ja) * 2010-11-15 2012-06-07 Hitachi Ltd リチウム二次電池用電極板の製造装置およびリチウム二次電池の製造方法

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