WO2017029902A1 - Électrode pour éléments électrochimiques - Google Patents

Électrode pour éléments électrochimiques Download PDF

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Publication number
WO2017029902A1
WO2017029902A1 PCT/JP2016/070079 JP2016070079W WO2017029902A1 WO 2017029902 A1 WO2017029902 A1 WO 2017029902A1 JP 2016070079 W JP2016070079 W JP 2016070079W WO 2017029902 A1 WO2017029902 A1 WO 2017029902A1
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Prior art keywords
electrode
binder
active material
mass
electrode active
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PCT/JP2016/070079
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English (en)
Japanese (ja)
Inventor
寛明 三井
阿部　徹
僚治 田中
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Asahi Kasei Corp
Asahi Chemical Industry Co Ltd
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Asahi Kasei Corp
Asahi Chemical Industry Co Ltd
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Priority to CN201680047297.4A priority Critical patent/CN107925086B/zh
Priority to KR1020187001597A priority patent/KR102075897B1/ko
Priority to JP2017535290A priority patent/JP6498300B2/ja
Publication of WO2017029902A1 publication Critical patent/WO2017029902A1/fr
Anticipated expiration legal-status Critical
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/30—Electrodes characterised by their material
    • H01G11/32—Carbon-based
    • H01G11/38—Carbon pastes or blends; Binders or additives therein
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/13—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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/621—Binders
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2220/00—Batteries for particular applications
    • H01M2220/20—Batteries in motive systems, e.g. vehicle, ship, plane
    • 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 an electrode for an electrochemical element.
  • Lithium ion secondary batteries have a high energy density and are used in fields such as mobile phones and notebook personal computers. Further, with the expansion and development of applications, electrochemical devices are required to have further improved performance such as low resistance and large capacity.
  • an electrode is obtained using a binder having a core-shell structure and a specific gel content.
  • An object of the present invention is to provide an electrode for an electrochemical element having a low internal resistance and an excellent balance between cycle characteristics and peel strength when incorporated in a battery.
  • the inventors of the present invention are excellent in lithium diffusibility when rapidly charged by making the binder in the electrode for an electrochemical element into a specific shape, When incorporated in a battery, it was found that the internal resistance was low and the cycle characteristics were excellent, and the present invention was completed.
  • An electrode for an electrochemical device comprising an electrode active material layer containing an electrode active material and a binder, An electrode for an electrochemical element, wherein at least a part of the binder has a particle shape, and the roundness of the particle is 0.50 to 0.85.
  • the electrode for an electrochemical element according to [1] wherein an average particle length of the binder particles measured by cross-sectional observation is 100 to 400 nm.
  • An electrochemical device comprising the electrode for an electrochemical device according to any one of [1] to [4].
  • a lithium ion battery comprising the electrochemical element electrode according to any one of [1] to [4], a separator, and an electrolytic solution.
  • An automobile comprising the lithium ion battery according to [6].
  • an electrode for an electrochemical element that has a low internal resistance when incorporated in a battery and is excellent in balance between cycle characteristics and peel strength.
  • This embodiment is an electrode for an electrochemical device comprising an electrode active material layer containing an electrode active material and a binder, wherein at least a part of the binder has a particle shape, and the roundness of the particle is 0.00.
  • This is an electrode for an electrochemical element having a value of 50 to 0.85.
  • the electrode for an electrochemical element of the present embodiment may be an electrode used for an electrochemical element, and is not particularly limited to an electrochemical element.
  • the electrode active material layer which comprises the electrode for electrochemical elements contains an electrode active material and a binder at least.
  • the electrode active material and the binder constituting the electrode active material layer will be described.
  • the electrode active material is appropriately selected depending on the type of electrochemical element.
  • the negative electrode active material may be a low crystal such as graphitizable carbon, non-graphitizable carbon, activated carbon, or pyrolytic carbon.
  • the electrode active material illustrated above may be used independently according to a use, and may be used in mixture of multiple types.
  • the shape of the negative electrode active material for a lithium ion secondary battery is preferably a granulated particle, and if the particle shape is spherical, a higher-density electrode can be formed at the time of electrode formation.
  • the volume average particle diameter of the negative electrode active material for a lithium ion secondary battery is usually 0.1 to 100 ⁇ m, preferably 0.5 to 50 ⁇ m, more preferably 0.8 to 20 ⁇ m.
  • the tap density of the negative electrode active material for the lithium ion secondary battery is not particularly limited, but a negative electrode having a negative electrode capacity of 0.6 g / cm 3 or more is preferably used.
  • the binder used in the present invention is not particularly limited as long as it is a compound capable of binding the above-described electrode active materials to each other, but is preferably a (co) polymer having a double bond.
  • the (co) polymer having a double bond is preferably a (co) polymer obtained by polymerizing a monomer containing a conjugated diene, and more preferably contains an ethylenically unsaturated carboxylic acid as the monomer. preferable.
  • the binder is a (co) polymer obtained by polymerizing a monomer containing a conjugated diene, in addition to the conjugated diene and the ethylenically unsaturated carboxylic acid contained if necessary, other copolymerizable with these Monomers such as vinyl compounds may be included.
  • the supply form of the binder at the time of electrode manufacture is not specifically limited, For example, it is preferable to use the thing of the form of copolymer latex which the binder particle
  • the binder is a (co) polymer containing a conjugated diene as a monomer
  • the conjugated diene include 1,3-butadiene, isoprene, 2-chloro-1,3-butadiene, chloroprene, etc. Two or more types can be combined, and among these, 1,3-butadiene is preferred from the viewpoint of adhesiveness.
  • the copolymer contains an ethylenically unsaturated carboxylic acid as a monomer
  • examples of the ethylenically unsaturated carboxylic acid include fumaric acid, itaconic acid, acrylic acid, and methacrylic acid. It can be used alone or in combination of two or more. Among these, itaconic acid and acrylic acid are desirable from the viewpoint of the stability of the polymerized copolymer latex.
  • the amount of the ethylenically unsaturated carboxylic acid used is preferably 0.01 or more and 20 parts by mass or less, more preferably 0.01 or more and 15 parts by mass or less when the total of all monomers is 100 parts by mass. More preferably, it is 0.01 or more and 10 parts by mass or less.
  • vinyl compounds that can be copolymerized include aromatic vinyl compounds, (meth) acrylate compounds, vinyl cyanide compounds, and the like.
  • aromatic vinyl compound for example, styrene, ⁇ -methylstyrene, p-methylstyrene, vinyltoluene, chlorostyrene, divinylbenzene and the like can be used alone or in combination of two or more thereof. Styrene is preferred from the viewpoint of the stability of the polymerized copolymer latex.
  • the amount of the aromatic vinyl compound used is preferably 30 to 70 parts by mass, more preferably 35 to 65 parts by mass, and still more preferably 35 to 60 parts by mass.
  • Examples of the (meth) acrylate compound include methyl (meth) acrylate, ethyl (meth) acrylate, n-propyl (meth) acrylate, i-propyl (meth) acrylate, n-butyl (meth) acrylate, i-butyl (meth) ) Acrylate, n-amyl (meth) acrylate, i-amyl (meth) acrylate, hexyl (meth) acrylate, 2-hexyl (meth) acrylate, octyl (meth) acrylate, i-nonyl (meth) acrylate, decyl (meth) ) Acrylate, hydroxymethyl (meth) acrylate, hydroxyethyl (meth) acrylate, ethylene glycol (meth) acrylate, etc., can be used alone or in combination of two or more thereof.
  • the amount of the (meth) acrylate compound used is preferably 0.1 to 30 parts by mass, more preferably 0.1 to 25 parts by mass, and still more preferably 0.1 to 20 parts by mass.
  • vinyl cyanide compounds examples include acrylonitrile, methacrylonitrile, ⁇ -chloroacrylonitrile, and the like. These monomers can be used alone or in combination of two or more thereof. Then, it is desirable from the viewpoint of the stability of the copolymer latex obtained by polymerizing acrylonitrile.
  • the amount of vinyl cyanide compound used is preferably 0.1 to 30 parts by mass, more preferably 0.1 to 20 parts by mass, and still more preferably 0.1 to 15 parts by mass.
  • copolymerizable vinyl compounds include, in addition to the above, hydroxyl group-containing monomers such as 2-hydroxyethyl acrylate; aminoalkyl esters such as aminoethyl acrylate, dimethylaminoethyl acrylate, and diethylaminoethyl acrylate; Pyridines such as 2-vinylpyridine and 4-vinylpyridine; Glycidyl esters such as glycidyl acrylate and glycidyl methacrylate; acrylamide, methacrylamide, N-methylolacrylamide, glycidylmethacrylamide, N, N-butoxymethylacrylamide, etc.
  • hydroxyl group-containing monomers such as 2-hydroxyethyl acrylate
  • aminoalkyl esters such as aminoethyl acrylate, dimethylaminoethyl acrylate, and diethylaminoethyl acrylate
  • Pyridines such as 2-vinylpyridine and 4-viny
  • Carboxylic acid esters such as vinyl acetate
  • Halogenated vinyls such as vinyl chloride
  • Divinylbenzene (Poly) ethylene glycol di (meth) acrylate, Hexanediol (Meth) acrylate, 1,4-butanediol di (meth) acrylate, polyfunctional vinyl monomers such as allyl (meth) acrylate.
  • the blending amount is 0.1 to 30 parts by mass.
  • a hydroxyl group-containing monomer as another copolymerizable monomer, and among these, it is more preferable to add 2-hydroxyethyl acrylate. preferable.
  • Molecular weight modifiers include halogenated hydrocarbons such as chloroform and carbon tetrachloride; mercaptans such as n-hexyl mercaptan, n-octyl mercaptan, n-dodecyl mercaptan, t-dodecyl mercaptan, thioglycolic acid; dimethylxanthogendi All xanthogens such as sulfide and diisopropylxanthogen disulfide; those that can be used in usual emulsion polymerization such as terpinolene and ⁇ -methylstyrene dimer can be used.
  • halogenated hydrocarbons such as chloroform and carbon tetrachloride
  • mercaptans such as n-hexyl mercaptan, n-octyl mercaptan, n-dodecyl mercaptan, t-do
  • the amount of the molecular weight modifier used is preferably 0 to 5 parts by mass with respect to 100 parts by mass of the total monomers, and ⁇ -methylstyrene dimer and t-dodecyl mercaptan are preferably used.
  • the average particle diameter of the binder raw material particles in the (co) polymer latex is preferably 100 to 400 nm, more preferably 200 to 350 nm.
  • This particle size is a volume average particle size measured by a dynamic light scattering method.
  • the gel content of the binder is preferably 90 to 100%, more preferably 95 to 100%.
  • the gel content of the binder is a value that represents the molecular weight and the degree of crosslinking of the binder particles in the (co) polymer latex when the (co) polymer latex is used as the raw material of the binder, and is described in the examples. It can be measured by this method. The higher the gel content, the more the binder particles can be prevented from fusing in the electrode active material layer, that is, the binder can easily maintain the particle shape, and the roundness of the binder particles can be increased.
  • (Co) polymer latex can be obtained by emulsion polymerization of the above monomers.
  • Appropriate seed particles can be used during the polymerization, and the seed particles can also be obtained by ordinary emulsion polymerization.
  • a known method can be employed for emulsion polymerization, and the emulsion polymerization can be appropriately performed using an emulsifier, a polymerization initiator, a molecular weight regulator, a chelating agent, a PH regulator, and the like in an aqueous medium.
  • anionic surfactants nonionic surfactants, amphoteric surfactants, reactive surfactants and the like can be used alone or in combination of two or more.
  • anionic surfactants include higher alcohol sulfates, alkylbenzene sulfonates, aliphatic sulfonates, and polyethylene glycol alkyl ether sulfates.
  • alkylbenzene sulfonate sodium dodecylbenzenesulfonate is preferable.
  • an alkyl ester type, an alkyl ether type, an alkylphenyl ether type, or the like of polyethylene glycol is used.
  • amphoteric surfactants include betaines such as lauryl betaine and stearyl betaine, and amino acid types such as lauryl- ⁇ -alanine, stearyl- ⁇ -alanine and lauryl di (aminoethyl) glycine.
  • Examples of the reactive surfactant include polyoxyethylene alkylpropenyl phenyl ether, ⁇ - [1-[(allyloxy) methyl] -2- (nonylphenoxy) ethyl] - ⁇ -hydroxypolyoxyethylene, and the like.
  • the amount of the emulsifier used is preferably 0.1 to 10 parts by mass, more preferably 0.1 to 8 parts by mass, and further preferably 0.1 to 6 parts by mass with respect to 100 parts by mass of the total monomers.
  • Polymerization initiators include water-soluble polymerization initiators such as sodium persulfate, potassium persulfate, and ammonium persulfate, oil-soluble polymerization initiators such as benzoyl peroxide and lauryl peroxide, and redox polymerization initiators in combination with a reducing agent. Can be used alone or in combination.
  • the amount of the polymerization initiator used is preferably 0.1 to 3 parts by mass with respect to 100 parts by mass of all monomers.
  • the binder content in the electrode active material layer of the electrode for an electrochemical device is preferably 0.1 to 10 parts by mass, more preferably 0, based on 100 parts by mass of the electrode active material on a dry mass basis. .3 to 8 parts by mass, more preferably 0.5 to 5 parts by mass.
  • the binder content is within this range, sufficient adhesion between the electrode active material layer and the current collector can be secured, and the internal resistance can be lowered.
  • the binder content exceeds 10 parts by mass with respect to 100 parts by mass of the electrode active material, the binder particles tend to be fused together, or the roundness of the binder particles having a particle shape tends to be remarkably lowered. There is.
  • the electrode composition constituting the electrode active material layer may contain other components as necessary in addition to the binder and the electrode active material.
  • other components include conductive materials, dispersants, additives such as nonionic or anionic surfactants as stabilizers for copolymer latex, and antifoaming agents.
  • the conductive material is not particularly limited as long as it is a particulate material having conductivity.
  • conductive carbon black such as furnace black, acetylene black, and ketjen black
  • graphite such as natural graphite and artificial graphite
  • carbon fibers such as polyacrylonitrile-based carbon fibers, pitch-based carbon fibers, and vapor-grown carbon fibers.
  • acetylene black and ketjen black are preferable.
  • the average particle diameter of the conductive material is not particularly limited, but is preferably smaller than the average particle diameter of the electrode active material, usually 0.001 to 10 ⁇ m, more preferably 0.05 to 5 ⁇ m, and still more preferably 0.01. It is in the range of ⁇ 1 ⁇ m.
  • the amount of the conductive material used in the case of adding the conductive material is not particularly limited as long as the effect of the present invention is not impaired, but is preferably 0.1 to 50 with respect to 100 parts by mass of the electrode active material. Part by mass, more preferably 0.5 to 15 parts by mass, still more preferably 1 to 10 parts by mass.
  • the dispersing agent is a component having an action of uniformly dispersing each component in the solvent when the electrode active material, the binder, and optional components added as necessary are dispersed or dissolved in a solvent to form a slurry. It is.
  • the dispersant include cellulosic polymers such as carboxymethylcellulose, methylcellulose, ethylcellulose and hydroxypropylcellulose, and ammonium salts or alkali metal salts thereof, alginates such as propylene glycol alginate, and alginates such as sodium alginate.
  • Polyacrylic acid, and polyacrylic acid (or methacrylic acid) salts such as sodium polyacrylic acid (or methacrylic acid), polyvinyl alcohol, modified polyvinyl alcohol, polyethylene oxide, polyvinyl pyrrolidone, polycarboxylic acid, oxidized starch, phosphoric acid starch , Casein, various modified starches, chitin, chitosan derivatives and the like.
  • a water-soluble polymer (specific group-containing water-soluble polymer) containing one or more, preferably two or more groups such as a carboxyl group, a sulfonic acid group, a fluorine-containing group, a hydroxyl group and a phosphoric acid group is also used as a dispersant. be able to. These dispersants can be used alone or in combination of two or more.
  • a cellulose polymer is preferable, and carboxymethyl cellulose or an ammonium salt or an alkali metal salt thereof is particularly preferable.
  • the content of the dispersant is not particularly limited as long as the effect of the present invention is not impaired, but is usually 0.1 to 10 with respect to 100 parts by mass of the electrode active material. It is in the range of parts by weight, preferably 0.5 to 5 parts by weight, more preferably 0.8 to 2 parts by weight.
  • water can be used as a dispersion medium for the copolymer latex.
  • the binder particles are obtained by emulsion polymerization as described above, the water used during the polymerization is used.
  • the dispersion medium can be used as it is or after being concentrated. Further, the dispersion medium can be used by substituting with an organic solvent optimum for the active material, if necessary.
  • the organic dispersion medium is not particularly limited, and the method of substitution is not particularly limited, for example, a method of adding an organic dispersion medium to a copolymer latex obtained by emulsion polymerization and volatilizing water by vacuum distillation, Examples thereof include a method of volatilizing water from the copolymer latex and redispersing the resulting solid in an organic dispersion medium.
  • the manufacturing method of the electrode for electrochemical devices of this embodiment is demonstrated.
  • a slurry-like electrode composition is formed, the electrode composition is applied on a current collector such as a copper foil, dried, and pressure-molded to form an electrode. It is obtained by forming an active material layer.
  • the electrode active material layer is provided on the current collector, but the formation method is not limited.
  • the slurry-like electrode composition comprises an electrode active material, an essential component of a conductive material and a binder, and other dispersants and additives in water or an organic solvent such as N-methyl-2-pyrrolidone or tetrahydrofuran. It can be manufactured by kneading.
  • the solvent used for obtaining the electrode composition is not particularly limited, but when the above dispersant is used, a solvent capable of dissolving the dispersant is preferably used. Specifically, water is usually used, but an organic solvent may be used, or a mixed solvent of water and an organic solvent may be used.
  • the organic solvent examples include alkyl alcohols such as methyl alcohol, ethyl alcohol and propyl alcohol; alkyl ketones such as acetone and methyl ethyl ketone; ethers such as tetrahydrofuran, dioxane and diglyme; diethylformamide, dimethylacetamide and N-methyl- Amides such as 2-pyrrolidone and dimethylimidazolidinone; sulfur solvents such as dimethyl sulfoxide and sulfolane; and the like.
  • alcohols are preferable as the organic solvent.
  • the slurry is preferably an aqueous slurry using water as a dispersion medium from the viewpoint of ease of drying of the slurry and excellent environmental load.
  • the drying rate can be increased during spray drying. Further, the dispersibility of the binder or the solubility of the dispersant varies depending on the amount or type of the organic solvent used in combination with water. Thereby, the viscosity and fluidity
  • the amount of the solvent used when preparing the electrode composition is such that the solid content concentration is usually in the range of 1 to 90% by mass, preferably 5 to 85% by mass, more preferably 10 to 80% by mass. It is. When the solid content concentration is within this range, each component is preferably dispersed uniformly.
  • the method or procedure for dispersing or dissolving the electrode active material, the conductive material, the binder, and other dispersants and additives in the solvent is not particularly limited.
  • the electrode active material, the conductive material, the binder, the other dispersant Method of adding and mixing the additive; Dissolving the dispersant in the solvent, adding and mixing the binder dispersed in the solvent, and finally adding and mixing the electrode active material and the conductive material; Dispersing in the solvent Examples include a method in which an electrode active material and a conductive material are added to and mixed with the binder, and a dispersant dissolved in a solvent is added to and mixed with the mixture.
  • mixing means examples include mixing equipment such as a ball mill, a sand mill, a bead mill, a pigment disperser, a crusher, an ultrasonic disperser, a homogenizer, a homomixer, and a planetary mixer. Mixing is usually carried out in the range of room temperature to 80 ° C. for 10 minutes to several hours.
  • the viscosity of the electrode composition is usually in the range of 10 to 100,000 mPa ⁇ s, preferably 30 to 50,000 mPa ⁇ s, more preferably 50 to 20,000 mPa ⁇ s at room temperature. When the viscosity of the electrode composition is within this range, productivity can be increased.
  • the method for applying the electrode composition onto the current collector is not particularly limited. Examples thereof include a doctor blade method, a dip method, a reverse roll method, a direct roll method, a gravure method, an extrusion method, and a brush coating method.
  • the coating thickness of the electrode composition is appropriately set according to the thickness of the target electrode active material layer.
  • drying method examples include drying with warm air, hot air, low-humidity air, vacuum drying, and drying by irradiation with (far) infrared rays or electron beams. Among these, a drying method by irradiation with far infrared rays is preferable.
  • the drying temperature and the drying time are preferably a temperature and a time at which the solvent in the electrode composition applied to the current collector can be completely removed, and the drying temperature is 50 to 300 ° C., preferably 50 to 250 ° C.
  • the drying time is usually about 3 hours to 100 hours, preferably 5 hours to 50 hours, more preferably 10 hours to 30 hours.
  • Examples of the pressure molding method include molding methods such as roll pressing and press pressing.
  • the pressure during pressure molding is preferably 1 to 10 t / cm 2 , and the density of the electrode active material layer can be further adjusted by appropriately setting the temperature and time during pressure molding.
  • the density of the electrode active material layer (electrode density) is 0.30 to 2.0 g / cm 3 from the viewpoint of adjusting the roundness of the particles to the range defined in the present invention, where the binder has a particle shape. It is preferably 0.35 to 1.9 g / cm 3 , more preferably 0.40 to 1.8 g / cm 3 .
  • the thickness of the electrode active material layer is not particularly limited, but is usually 5 to 1000 ⁇ m, preferably 20 to 500 ⁇ m, more preferably 30 to 300 ⁇ m.
  • the electrode for an electrochemical element has at least an electrode active material layer, and the electrode active material layer may be formed on a current collector such as a copper foil.
  • the electrode active material layer includes an electrode active material and a binder, and at least a part of the binder exists in the electrode active material layer in a form having the particle shape.
  • the roundness of the particles is 0.50 to 0.85.
  • the binder Since the binder has a particle shape in the electrode active material layer, a void portion is secured between the binders close to each other. Therefore, when an electrochemical element is obtained using such an electrode for an electrochemical element, lithium ions can easily diffuse into the electrode active material layer by passing through this void, and the internal resistance can be reduced. Can be reduced. It is preferable that 70% or more of the binder area ratio when tracing the outline of the binder particles in the cross-sectional photograph of the electrode active material layer has a particle shape, more preferably 80% or more, and still more preferably 90% or more. It is.
  • a cross-sectional photograph of the electrode active material layer is taken with an SEM, and a portion determined to be a binder is recognized as having a particle shape. It is divided into parts determined not to have a particle shape and is calculated based on the areas of both.
  • the internal resistance is reduced by ensuring the bonding area of the active material or current collector and the binder and the void portion. It is possible to improve the peel strength and cycle characteristics.
  • the roundness of the binder particles having a particle shape in the electrode active material layer is preferably 0.55 to 0.80, more preferably 0.70 to 0.80.
  • the roundness of the binder particles having a particle shape in the electrode active material layer is preferably higher in terms of securing the voids, but on the other hand, it is not too high from the viewpoint of cycle characteristics and peel strength. preferable.
  • the roundness of the binder particles in the electrode active material layer is, for example, the average particle diameter of the binder particles in the (co) polymer latex that is the binder raw material, the gel content, and the binder content in the electrode active material layer. , And the density of the electrode active material layer. Specifically, the smaller the average particle diameter is, the less rounded it can be due to the pressure during pressure molding, and the higher the roundness can be. Can be lowered. The higher the gel content, the higher the roundness of the binder particle shape in the electrode active material layer. Further, the greater the binder content, the lower the roundness, and in particular when the amount exceeds 10 parts by mass, the binders are fused together, or the roundness is significantly reduced.
  • the roundness can be lowered.
  • the binder is fused or the roundness is remarkably lowered. It becomes difficult to make the range specified in the above.
  • the roundness of the binder particles in the electrode active material layer is calculated by the following method.
  • the site determined to be the binder in the cross-sectional photograph (FIG. 1) of the electrode active material layer imaged by SEM the site exhibiting dark contrast and determining the linear and continuous connection is determined as the boundary (contour) of the particle, Trace the outline of the binder particles freehand ( Figure 2). From this trace, 100 binder particles having a particle shape are selected at random. At this time, particles having unclear outlines are not selected (not used for calculating roundness). Further, when the observation image does not have a clear dark contrast, it is determined that it does not have a particle shape.
  • contour image of each selected particle is processed by image analysis software (A image-kun, imageJ, etc.), and the roundness is calculated by the following formula from the area and circumference of the region surrounded by the contour, and its arithmetic Let the average be roundness.
  • image analysis software A image-kun, imageJ, etc.
  • the particle diameter of the binder particles in the electrode active material layer is preferably 50 to 1000 nm as an average particle long diameter measured by cross-sectional observation. When the average particle major axis is in this range, the strength and flexibility of the electrode for an electrochemical element become better.
  • the average particle major axis is more preferably 100 to 900 nm, still more preferably 200 to 800 nm.
  • the average particle major axis has a random particle shape, similar to the calculation of the roundness of the binder particles, from the trace (FIG. 2) of the cross-sectional photograph of the electrode active material layer taken by the SEM.
  • the contour image of each selected particle is processed by image analysis software (A image-kun, imageJ, etc.), and the arithmetic average of the major axis of the region surrounded by the contour is taken as the average particle major axis .
  • the electrode for an electrochemical element of the present embodiment can be used as an electrode in an electrochemical element such as a lithium ion secondary battery, an electric double layer capacitor, a lithium ion capacitor, a sodium battery, or a magnesium battery, and in particular, a lithium ion secondary battery. It can be used suitably in a battery, and can be used suitably especially for the negative electrode of a lithium ion secondary battery.
  • a lithium ion secondary battery is composed of the electrode for an electrochemical element, a separator, and an electrolytic solution.
  • a separator will not be specifically limited if it can insulate between the electrodes for electrochemical elements, and can pass a cation and an anion.
  • a porous separator having pores (a) a porous separator having pores, (b) a porous separator having a polymer coat layer formed on one or both sides, or (c) a porous resin coat layer containing an inorganic ceramic powder
  • the formed porous separator is mentioned.
  • Non-limiting examples of these include solids such as polypropylene, polyethylene, polyolefin, or aramid porous separators, polyvinylidene fluoride, polyethylene oxide, polyacrylonitrile, or polyvinylidene fluoride hexafluoropropylene copolymers.
  • a polymer film for a polymer electrolyte or a gel polymer electrolyte, a separator coated with a gelled polymer coating layer, or a separator coated with a porous membrane layer made of an inorganic filler or a dispersant for inorganic filler is used. be able to.
  • a separator is arrange
  • the thickness of the separator is appropriately selected depending on the purpose of use, but is usually 1 to 100 ⁇ m, preferably 10 to 80 ⁇ m, more preferably 20 to 60 ⁇ m.
  • the electrolytic solution is not particularly limited.
  • a solution obtained by dissolving a lithium salt as a supporting electrolyte in a non-aqueous solvent can be used.
  • the lithium salt include LiPF 6 , LiAsF 6 , LiBF 4 , LiSbF 6 , LiAlCl 4 , LiClO 4 , CF 3 SO 3 Li, C 4 F 9 SO 3 Li, CF 3 COOLi, (CF 3 CO) 2 NLi , (CF 3 SO 2 ) 2 NLi, (C 2 F 5 SO 2 ) NLi, and other lithium salts.
  • LiPF 6 , LiClO 4 , and CF 3 SO 3 Li that are easily soluble in a solvent and exhibit a high degree of dissociation are preferably used. These can be used alone or in admixture of two or more.
  • the amount of the supporting electrolyte is usually 1% by mass or more, preferably 5% by mass or more, and usually 30% by mass or less, preferably 20% by mass or less, with respect to the electrolytic solution. If the amount of the supporting electrolyte is too small or too large, the ionic conductivity is lowered, and the charging characteristics and discharging characteristics of the battery are degraded.
  • the solvent used in the electrolytic solution is not particularly limited as long as it can dissolve the supporting electrolyte.
  • Alkyl carbonates such as carbonate (BC) and methyl ethyl carbonate (MEC); esters such as ⁇ -butyrolactone and methyl formate; ethers such as 1,2-dimethoxyethane; tetrahydrofuran; sulfolane and dimethyl sulfoxide Sulfur-containing compounds are used.
  • dimethyl carbonate, ethylene carbonate, propylene carbonate, diethyl carbonate, and methyl ethyl carbonate are preferable because high ion conductivity is easily obtained and the use temperature range is wide. These can be used alone or in admixture of two or more. Moreover, it is also possible to use an electrolyte containing an additive.
  • the additive is preferably a carbonate compound such as vinylene carbonate (VC).
  • electrolyte other than the above examples include gel polymer electrolytes in which a polymer electrolyte such as polyethylene oxide and polyacrylonitrile is impregnated with the electrolyte, and inorganic solid electrolytes such as lithium sulfide, LiI, and Li3N.
  • a secondary battery is obtained by stacking a negative electrode and a positive electrode through a separator, winding this in accordance with the shape of the battery, folding it into a battery container, injecting an electrolyte into the battery container, and sealing. Further, if necessary, an expanded metal, an overcurrent prevention element such as a fuse or a PTC element, a lead plate and the like can be inserted to prevent an increase in pressure inside the battery and overcharge / discharge.
  • the shape of the battery may be any of a laminated cell type, a coin type, a button type, a sheet type, a cylindrical type, a square type, a flat type, and the like.
  • the lithium ion secondary battery in the present embodiment includes, for example, a mobile phone, a portable computer, a smartphone, a tablet PC, a smart pad, a netbook, a LEV (Light Electronic Vehicle), a UAV (Unmanned Aerial Vehicle), an automobile, and a power storage. It can use suitably for an apparatus etc.
  • Examples of the automobile include an electric vehicle, a hybrid electric vehicle, and a plug-in hybrid electric vehicle.
  • Copolymer latex is applied to a glass plate at a thickness of 0.5 mm, and 0.5 g is weighed from a coating film (dried coating film of the copolymer before immersion) obtained by drying by heating at 130 ° C. for 30 minutes. After that, it was immersed in 40 ml of toluene and shaken for 3 hours. The copolymer coating film after shaking was filtered through a 325 mesh stainless steel wire mesh and dried at 130 ° C. for 1 hour to obtain a dried coating film of the copolymer after immersion, which was weighed. The gel content was calculated from the mass of the coating film before and after immersion (dried coating film) by the following formula.
  • the cross section of the negative electrode active material layer was prepared by first disassembling a laminated laminate cell-shaped lithium secondary battery in an Ar glove box, washing the collected negative electrode with dimethyl carbonate, and then drying in air.
  • the dried negative electrode was cut into a 2 mm square, subjected to OsO4 dyeing treatment, and then a cross section was made perpendicular to the electrode surface using a cross section polisher (product name “SM-09010”, manufactured by JEOL Ltd.). .
  • a cross-sectional photograph taken by the above method 100 binder particles are selected at random, and from a portion judged to be a binder, dark contrast is observed in an observation image, and a portion showing a linear and continuous connection is represented by a particle. The boundary (contour) was judged, and the contour of the binder particles was traced freehand. Particles with unclear outlines were not used for calculating roundness.
  • ⁇ Average particle long diameter of binder particles> The 100 contour images obtained by the above ⁇ Binder particle roundness> were processed by image analysis software (imageJ), and the arithmetic average of the major axis of the region surrounded by the outline was defined as the average particle major axis.
  • ⁇ Peel strength> The negative electrodes obtained in the examples and comparative examples were cut into rectangular pieces each having a width of 1 cm and a length of 10 cm to form test pieces, which were fixed with the negative electrode active material layer face up, and cellophane tape was applied to the surface of the negative electrode active material layer. After pasting, the stress when the cellophane tape was peeled off from one end of the test piece in the 180 ° direction at a speed of 50 mm / min was measured. And this measurement was performed 10 times, the average value was calculated
  • the internal resistance was determined according to the following criteria. A: Internal resistance is less than 3.0 ⁇ B: Internal resistance is 3.0 ⁇ or more and less than 3.5 ⁇ C: Internal resistance is 3.5 ⁇ or more and less than 4.0 ⁇ D: Internal resistance is 4.0 ⁇ or more, 4.5 ⁇ Less than E: Internal resistance is 4.5 ⁇ or more
  • Capacity maintenance rate is 90% or more
  • Example 1 Manufacture of binder for negative electrode>
  • Initial water 75 parts by mass of ion exchange water, 3.0 parts by mass of itaconic acid, seed (polystyrene latex having a particle size of 35 nm), emulsifier (0.3 parts by mass of sodium dodecylbenzenesulfonate)
  • seed polystyrene latex having a particle size of 35 nm
  • emulsifier 0.3 parts by mass of sodium dodecylbenzenesulfonate
  • Monomer blended here (40 parts by mass of 1,3-butadiene, 49 parts by mass of styrene, 3.0 parts by mass of methyl methacrylate, 3.0 parts by mass of acrylonitrile, 1.0 part by mass of 2-hydroxyethyl acrylate, acrylic acid 1.0 part by mass, 0.1 part by mass of ⁇ -methylstyrene dimer, 0.1 part by mass of t-dodecyl mercaptan) were added over 6.5 hours.
  • catalyst water 24 parts by mass of ion exchange water, 1.2 parts by mass of sodium persulfate, 0.3 parts by mass of caustic soda, 0.15 parts by mass of an emulsifier (sodium dodecylbenzenesulfonate)
  • emulsifier sodium dodecylbenzenesulfonate
  • ⁇ Preparation of positive electrode> 100 parts of lithium cobaltate having a volume average particle size of 8 ⁇ m as the electrode active material of the positive electrode and 1.5% aqueous solution of carboxymethylcellulose ammonium (DN-800Hl Daicel Chemical Industries, Ltd.) as the dispersing agent in a solid content equivalent of 2. 0 parts, 5 parts of acetylene black (Denka black powder: manufactured by Denki Kagaku Kogyo Co., Ltd.) as the conductive material, and acrylate having a glass transition temperature of ⁇ 28 ° C.
  • carboxymethylcellulose ammonium DN-800Hl Daicel Chemical Industries, Ltd.
  • a positive electrode composition by mixing a 40% aqueous dispersion of a polymer with a planetary mixer so that the solid content is 3.0 parts and the total solid content is 35%. did.
  • the positive electrode composition was applied to a current collector made of an aluminum foil having a thickness of 20 ⁇ m on both the front and back surfaces of the current collector at an electrode forming speed of 20 m / min, dried at 120 ° C. for 5 minutes, and then punched into a 5 cm square.
  • a positive electrode having an electrode active material layer with a thickness of 100 ⁇ m on one side was obtained.
  • Electrode active material for the negative electrode 100 parts of graphite (KS-6: manufactured by Timcal) having a volume average particle diameter of 3.7 ⁇ m and a 1.5% aqueous solution of carboxymethyl cellulose ammonium as a dispersant (DN-800H: Daicel Chemical) (Made by Kogyo Co., Ltd.) 2.0 parts in terms of solid content, 5 parts of acetylene black (Denka Black powder: made by Denki Kagaku Kogyo Co., Ltd.) as the conductive material, and the above-described copolymer latex as the binder for the electrode composition 3.0 parts by weight and ion-exchanged water were mixed so that the total solid content concentration was 35% to prepare a slurry-like negative electrode composition.
  • KS-6 manufactured by Timcal
  • the negative electrode composition was applied to one side of a current collector made of a copper foil having a thickness of 18 ⁇ m so that the film thickness after drying was about 100 ⁇ m, and dried at 60 ° C. for 20 hours. Thus, a negative electrode active material layer was formed. Subsequently, it was rolled using a roll press so that the pressing pressure was 2 t / cm 2 with respect to the electrode, to obtain a negative electrode having a thickness of 50 ⁇ m.
  • ⁇ Manufacture of batteries> Using the polyethylene microporous film (film thickness: 25 ⁇ m) (Hypore manufactured by Asahi Kasei E-Materials Co., Ltd.) as the positive electrode, the negative electrode, and the separator, a laminated laminate cell-shaped lithium ion battery was produced.
  • the electrolytic solution a solution obtained by dissolving LiPF 6 at a concentration of 1.0 mol / liter in a mixed solvent of ethylene carbonate and diethyl carbonate in a mass ratio of 1: 2 was used.
  • Example 2 When forming the negative electrode active material layer, a negative electrode was obtained in the same manner as in Example 1 except that the drying temperature was 100 ° C. and the drying time was 14 hours. A secondary battery was manufactured and evaluated in the same manner. The results are shown in Table 1.
  • Example 3 When forming the negative electrode active material layer, a negative electrode was obtained in the same manner as in Example 1 except that the drying temperature was 150 ° C. and the drying time was 10 hours. A secondary battery was manufactured and evaluated in the same manner. The results are shown in Table 1.
  • Example 1 In rolling using a roll press, a negative electrode was obtained in the same manner as in Example 1 except that the pressing pressure was 6 t / cm 2 with respect to the electrode, and a lithium ion secondary battery was obtained using the obtained negative electrode. Were manufactured and evaluated in the same manner. The results are shown in Table 1.
  • Monomer blended here (40 parts by mass of 1,3-butadiene, 49 parts by mass of styrene, 3.0 parts by mass of methyl methacrylate, 3.0 parts by mass of acrylonitrile, 1.0 part by mass of 2-hydroxyethyl acrylate, acrylic acid 1.0 part by mass, 0.1 part by mass of ⁇ -methylstyrene dimer, 0.8 part by mass of t-dodecyl mercaptan) were added over 6.5 hours.
  • catalyst water 24 parts by mass of ion exchange water, 1.2 parts by mass of sodium persulfate, 0.3 parts by mass of caustic soda, 0.15 parts by mass of an emulsifier (sodium dodecylbenzenesulfonate)
  • emulsifier sodium dodecylbenzenesulfonate
  • a slurry-like negative electrode composition was prepared in the same manner as in Example 1 except that the above-described copolymer latex was used as a binder for an electrode composition, and the same negative electrode composition as in Example 1 was prepared using the obtained negative electrode composition. Thus, a negative electrode was obtained.
  • a laminated laminate cell-shaped lithium ion battery was prepared in the same manner as in Example 1 except that the above negative electrode was used as the negative electrode, and evaluated in the same manner as in Example 1.
  • the binder did not have a particle shape. The results are shown in Table 1.
  • Monomers here (40 parts by weight of butadiene, 49 parts by weight of styrene, 3.0 parts by weight of methyl methacrylate, 3.0 parts by weight of acrylonitrile, 1.0 part by weight of 2-hydroxyethyl acrylate, 1.0 part by weight of acrylic acid) Part, ⁇ -methylstyrene dimer 0.1 part by mass, t-dodecyl mercaptan 0.05 part by mass) was added over 6.5 hours.
  • catalyst water 24 parts by mass of ion exchange water, 1.2 parts by mass of sodium persulfate, 0.3 parts by mass of caustic soda, 0.15 parts by mass of an emulsifier (sodium dodecylbenzenesulfonate)
  • emulsifier sodium dodecylbenzenesulfonate
  • a slurry-like negative electrode composition was prepared in the same manner as in Example 1 except that the above-described copolymer latex was used as a binder for an electrode composition, and Example 1 was obtained using the obtained negative electrode composition.
  • a negative electrode was obtained in the same manner.
  • a laminated laminate cell-shaped lithium ion battery was prepared in the same manner as in Example 1 except that the above negative electrode was used as the negative electrode, and evaluated in the same manner as in Example 1. The results are shown in Table 1.
  • the electrode for an electrochemical element of the present invention can be used as an electrode (positive electrode / negative electrode) of various electrochemical elements, and can be particularly preferably used as a negative electrode of a lithium ion secondary battery.

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Abstract

Cette invention concerne une électrode pour éléments électrochimiques, comprenant une couche de matériau actif d'électrode contenant un matériau actif d'électrode et un liant, au moins une partie du liant présentant une forme particulaire et la circularité de la particule allant de 0,50 à 0,85.
PCT/JP2016/070079 2015-08-14 2016-07-07 Électrode pour éléments électrochimiques Ceased WO2017029902A1 (fr)

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WO2019017480A1 (fr) * 2017-07-20 2019-01-24 株式会社大阪ソーダ Électrode et dispositif de stockage d'électricité
JP2020004627A (ja) * 2018-06-28 2020-01-09 于 暁玲 ナトリウムイオン電池用負極材料及びこれを用いたナトリウムイオン電池
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WO2021187366A1 (fr) * 2020-03-16 2021-09-23 株式会社クラレ Liant pour électrodes de dispositif de stockage d'électricité, solution de liant, bouillie pour électrode de dispositif de stockage d'électricité, électrode de dispositif de stockage d'électricité et dispositif de stockage d'électricité
JP2021190545A (ja) * 2020-05-29 2021-12-13 パナソニックＩｐマネジメント株式会社 電気化学デバイス
JPWO2022249933A1 (fr) * 2021-05-27 2022-12-01
US12148949B2 (en) * 2021-07-28 2024-11-19 Contemporary Amperex Technology (Hong Kong) Limited Battery, battery module, battery pack and electric device
EP4528842A4 (fr) * 2022-06-13 2025-10-15 Gs Yuasa Int Ltd Électrode négative pour élément de stockage d'énergie et élément de stockage d'énergie

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JP2019008961A (ja) * 2017-06-23 2019-01-17 Fdk株式会社 電極板および電池
JP7180595B2 (ja) 2017-07-20 2022-11-30 株式会社大阪ソーダ 電極及び蓄電デバイス
JPWO2019017480A1 (ja) * 2017-07-20 2020-07-16 株式会社大阪ソーダ 電極及び蓄電デバイス
WO2019017480A1 (fr) * 2017-07-20 2019-01-24 株式会社大阪ソーダ Électrode et dispositif de stockage d'électricité
JP2020004627A (ja) * 2018-06-28 2020-01-09 于 暁玲 ナトリウムイオン電池用負極材料及びこれを用いたナトリウムイオン電池
WO2021029411A1 (fr) * 2019-08-13 2021-02-18 Jsr株式会社 Composition pour dispositifs de stockage d'électricité, suspension pour électrodes de dispositif de stockage d'électricité, électrode de dispositif de stockage d'électricité et dispositif de stockage d'électricité
CN115210914A (zh) * 2020-03-16 2022-10-18 株式会社可乐丽 适合于蓄电设备电极的粘接剂、粘接剂溶液、蓄电设备电极浆料、蓄电设备电极和蓄电设备
JPWO2021187366A1 (fr) * 2020-03-16 2021-09-23
WO2021187366A1 (fr) * 2020-03-16 2021-09-23 株式会社クラレ Liant pour électrodes de dispositif de stockage d'électricité, solution de liant, bouillie pour électrode de dispositif de stockage d'électricité, électrode de dispositif de stockage d'électricité et dispositif de stockage d'électricité
JP7708738B2 (ja) 2020-03-16 2025-07-15 株式会社クラレ 蓄電デバイス電極に適したバインダー、バインダー溶液、蓄電デバイス電極スラリー、蓄電デバイス電極および蓄電デバイス
JP2021190545A (ja) * 2020-05-29 2021-12-13 パナソニックＩｐマネジメント株式会社 電気化学デバイス
JP7542213B2 (ja) 2020-05-29 2024-08-30 パナソニックＩｐマネジメント株式会社 電気化学デバイス
JPWO2022249933A1 (fr) * 2021-05-27 2022-12-01
US12148949B2 (en) * 2021-07-28 2024-11-19 Contemporary Amperex Technology (Hong Kong) Limited Battery, battery module, battery pack and electric device
EP4528842A4 (fr) * 2022-06-13 2025-10-15 Gs Yuasa Int Ltd Électrode négative pour élément de stockage d'énergie et élément de stockage d'énergie

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