WO2022049974A1 - Procédé de revêtement, procédé de fabrication d'une pile à combustible ou pile à combustible, procédé de fabrication d'une batterie secondaire ou batterie secondaire, et procédé de fabrication d'une batterie tout-solide ou batterie tout-solide - Google Patents

Procédé de revêtement, procédé de fabrication d'une pile à combustible ou pile à combustible, procédé de fabrication d'une batterie secondaire ou batterie secondaire, et procédé de fabrication d'une batterie tout-solide ou batterie tout-solide Download PDF

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Publication number
WO2022049974A1
WO2022049974A1 PCT/JP2021/028910 JP2021028910W WO2022049974A1 WO 2022049974 A1 WO2022049974 A1 WO 2022049974A1 JP 2021028910 W JP2021028910 W JP 2021028910W WO 2022049974 A1 WO2022049974 A1 WO 2022049974A1
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Prior art keywords
slurry
coating
gas
particles
bubbles
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PCT/JP2021/028910
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English (en)
Japanese (ja)
Inventor
正文 松永
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エムテックスマート株式会社
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Application filed by エムテックスマート株式会社 filed Critical エムテックスマート株式会社
Priority to CN202180051435.7A priority Critical patent/CN115968323A/zh
Publication of WO2022049974A1 publication Critical patent/WO2022049974A1/fr

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
    • B05D3/12—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by mechanical means
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
    • B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
    • H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
    • H01M10/0562—Solid materials
    • H—ELECTRICITY
    • 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
    • H01M10/058—Construction or manufacture
    • H01M10/0585—Construction or manufacture of accumulators having only flat construction elements, i.e. flat positive electrodes, flat negative electrodes and flat separators
    • 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
    • H01M4/04—Processes of manufacture in general
    • 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
    • H01M4/86—Inert electrodes with catalytic activity, e.g. for fuel cells
    • H01M4/88—Processes of manufacture
    • 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
    • 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
    • Y02E60/30—Hydrogen technology
    • Y02E60/50—Fuel cells
    • 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
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
    • Y02P70/50—Manufacturing or production processes characterised by the final manufactured product

Definitions

  • the present invention relates to a coating method, a method for manufacturing a fuel cell or a fuel cell, a method for manufacturing a secondary battery or a secondary battery, a method for manufacturing an all-solid-state battery or an all-solid-state battery.
  • the material to be coated in the present invention is a liquid, and the liquid contains particles and short fibers and is generally expressed as a slurry or dispersion. Binders and thickeners may or may not be contained in the slurry or the like. In addition, it is better not to contain surfactants and dispersants that adversely affect the coating film performance as much as possible.
  • a liquid containing particles having a medium diameter D50 of more than 10 micrometers tends to settle as the specific gravity of the particles increases or the particles aggregate.
  • Short fibers with a diameter on the order of nanometers such as single-walled carbon nanotubes and carbon nanofibers with generally longer fiber lengths, are effective in the film thickness direction, that is, in the vertical direction, but expand in the horizontal direction.
  • Graphene and their composite materials that contribute to their conductivity can be uniformly dispersed by adding a solvent or the like to form a dispersion or slurry, but when mixed with other liquids such as active material slurry, they tend to aggregate. Another issue arises and needs to be resolved.
  • the present invention is effective in a method of handling and applying a liquid such as a slurry or a dispersion system, and further exhibits a feature in a method for manufacturing a fuel cell or a fuel cell, a secondary battery or a manufacturing or an all-solid-state battery or a manufacturing thereof. can.
  • the present invention does not limit the electrode forming process, the electrolyte forming process such as an all-solid-state battery, or the method of applying a liquid such as a slurry.
  • the coating according to the present invention is not particularly limited, but is a roll coating, a slot nozzle (slot die) coating, a slit nozzle coating in which a slurry or the like is made into particles and ejected from an elongated slit groove, screen printing, a curtain coating, a dispenser coating, an inkjet, a spray.
  • Spraying with a nozzle atomization (including fibrousization) including rotary atomization that rotates a bell or disc at high speed to atomize by centrifugal force, and electrostatic charge and adhesion (including fibrousization) of atomized particles. It includes a method for applying particles and fibers such as these directly or indirectly to an object by using suction or the like, and also includes a micro curtain coat.
  • the object may be a powder or granular material made of a drug or chemical, an object, a film such as a long WEB, or the like, and is not limited to include the material, shape, weight, quantity, etc. of the object.
  • the micro curtain coat is a method invented by the present inventor, and uses an airless spray nozzle with a wide-angle spray pattern (for example, a cross-cut nozzle manufactured by Nordson, USA) to spray a liquid or the like at a relatively low pressure of about 0.05 to 0.7 MPa.
  • a wide-angle spray pattern for example, a cross-cut nozzle manufactured by Nordson, USA
  • it is a method of applying by moving the object and the spray nozzle relative to each other using the part of the micro liquid film (micro curtain) before it becomes a mist, and it is a method of applying 100% liquid without generating overspray particles. You can expect wearing efficiency.
  • the liquid is stretched by the liquid film from the tip of the nozzle tip to the end, and finally becomes an unstable relatively long liquid flow or large droplets from both ends of the bottom of the triangular or bell-shaped liquid film.
  • the pressure is, for example, about 3.5 MPa ⁇ s or more
  • the triangular liquid film of the above liquid film becomes smaller, and the droplets gradually become smaller due to the collision with the atmospheric pressure downstream of the liquid film, and the small flow rate wide-angle spray nozzle.
  • the spray particle size can be made to be around 20 micrometer, for example, at a distance of about 250 mm.
  • the maximum base width changes depending on the pressure, viscosity, etc., it is common to apply with a liquid film having a width of about 5 to 20 mm and a desired flow rate.
  • the relative movement of the object and the airless nozzle may be at a medium speed of about 30 m / min.
  • the solvent evaporates slowly with a high boiling point solvent, even if the speed increases, it can be followed because it only leveles while forming a thin film.
  • the flow rate at both ends of the triangular isoliquid film is generally 10 times or more the flow rate at the center, and when the object is at room temperature, the streaks with a large flow rate such as resin solution are the solution on the object.
  • atomization is to atomize a liquid containing solid fine particles by vibrating the liquid surface with ultrasonic waves, spins such as electrospinning, and centrifugation by a rotating body. It is applied by making it into particles or fibers by force.
  • fine particles generated by spraying or other methods such as rupture of a liquid film of bubbling or colliding with another object can be carried by a carrier gas and applied as they are. Particles and the like can be charged and applied.
  • a method of stretching a group of particles at high speed with another compressed gas and applying it in an ultrafine pattern, or a melt blown method applied to a two-fluid spray is applied to a liquid to support a wide and high-speed line speed object. It also includes a method of creating the fine particles and fibers.
  • the air assist is performed with the help of compressed gas such as dry compressed air, such as argon and nitrogen, which are inert gases.
  • compressed gas such as dry compressed air, such as argon and nitrogen, which are inert gases.
  • the present invention also includes a method of adhering or applying them to an object. In the present invention, these are collectively referred to as sprays below.
  • Perovskite solar cells are the most promising organic solar cells, and prototypes such as applying a perovskite chemical solution to a wide area of 300 mm x 300 mm with a thin film by the inkjet method have been made. Further, in fuel cells, developments for reducing the amount of catalyst are progressing, and for example, the amount of metal catalyst such as platinum catalyst or platinum cobalt catalyst is required to be 0.3 mg or less per square centimeter for a cathode electrode, and an extremely small amount of 0.05 mg for an anode.
  • metal catalyst such as platinum catalyst or platinum cobalt catalyst is required to be 0.3 mg or less per square centimeter for a cathode electrode, and an extremely small amount of 0.05 mg for an anode.
  • platinums are as small as several nanometers, they have a specific gravity of 20 or more, so the carbon particles that support platinum are also primary particles of several tens of nanometers, and the solid content of electrolyte solutions such as ionomer's Nafion solution is 5 to 10. Since the total content of non-volatile content is very small, it is necessary to make the coating film an ultra-thin film in order to obtain the above-mentioned minute amount of solid-separated film. Alternatively, it was even necessary to reduce the normal solid content of 5 to 15 percent to 1 to 3 percent or less.
  • active material particles of secondary batteries, active material particles of all-solid-solid batteries, electrolyte particles, fine particles such as carbon as a conductive aid, and carbon nanotubes, especially single-walled carbon nanotubes (SWCNTs) and carbon nanofibers (CNTs) are fluorinated.
  • a binder such as vinylidene (PVDF) or a slurry composed of a solvent thereof such as normal methylpyrrolidone (NMP)
  • PVDF vinylidene
  • NMP normal methylpyrrolidone
  • Patent Document 1 is an invention by the present inventor and the like, and moves two containers mainly for preventing precipitation of a fluorescent substance slurry for the LED field.
  • a method of mixing bubbles into a slurry to prevent precipitation is disclosed.
  • a gas such as nitrogen gas is mixed as bubbles in a heat-melted thermoplastic adhesive and pressurized, sufficiently mixed with fine bubbles that cannot be seen under pressure, and then used as an object by a discharger.
  • Foam can be formed by applying and foaming by returning to atmospheric pressure, and by cooling the coated surface with the atmosphere, at least the surface quickly becomes below the softening point. Therefore, even if the inside is completely returned to room temperature, it can be made into an elastic body by mixing bubbles, so it is widely used especially for gasket purposes.
  • Patent Document 1 the application is a small device, and the method is to mix the bubbles in the slurry in the lower part of the container moving between the two small containers, and the pressure inside the container is relatively low, so the bubbles move.
  • the efficiency of foam mixing is particularly poor, and the foam-slurry mixture system is simplified without using a density sensor, etc., so the mixing ratio of foam and slurry is sometimes There was variation.
  • bubbles are mixed in a hot melt adhesive heated and melted at about 120 to 200 ° C. and discharged as a hot melt adhesive containing bubbles in an object by a discharge device to increase the bubbles, for example, for the purpose of gaskets.
  • the main purpose was to produce foam while cooling.
  • the present invention mixes in a slurry and circulates at high speed as a foam slurry mixture, prevents the precipitation of solid particles and short fibers in the slurry with the help of bubbles, improves the dispersed state, and adds particles in the slurry, if necessary.
  • the present invention has been made to solve the above-mentioned problems, and an object of the present invention is a high value-added coating method, a method for manufacturing a fuel cell in which an electrode of a fuel cell is formed, or an electrode of a fuel cell or a secondary battery.
  • Method of manufacturing the formed secondary battery or secondary battery, next-generation secondary battery, especially next-generation secondary battery manufacturing method or next-generation secondary battery in which electrodes and solid electrolytes such as all-solid-state battery and all-solid-state air battery are formed Is to provide.
  • positive electrode or negative electrode active material particles and electrolyte particles or short fibers can be independently formed into a slurry and laminated and coated in a desired order in each device. It is effective to make a thin film and make it as multi-layered as possible because ideal mixed coating can be achieved.
  • all the particles or the like may be selected and mixed to form a slurry, which may be laminated as a thin film.
  • the slurry bubbles may be mixed or mixed up to the cutting edge of the discharge device or the coating device, or more preferably, the slurry foam mixture is circulated at high speed by a pump or the like to form a uniform mixture and discharged or mixed.
  • the high speed according to the present invention is 0.3 m / s. Or more, and may be, for example, 1.5 m / s. Or higher. Further, if a static mixer, a dynamic mixer, or a collision mixing means proposed by the present inventor has been installed in the middle of the circulation circuit to promote the mixing of the slurry and the gas, the desired foam slurry mixture can be obtained in a short time. So it's even better.
  • bubbles are mixed into a slurry having a high viscosity or a high solid content to prevent particles and the like from precipitating, and the mixture is mixed with a solvent immediately before the coating device, inside the coating device, or outside the coating device to reduce the viscosity. It can be quickly applied to an object. Therefore, since the problem of precipitation, which is a weak point of the low-viscosity slurry, can be solved, it is particularly suitable for thin film coating in fine particle formation by play or the like.
  • carbon dioxide in addition to the two-fluid spray, carbon dioxide can be easily atomized by rotary atomization or by selecting carbon dioxide as a gas to make a supercritical fluid.
  • the general two-fluid spray including the air assist slot nozzle, and the slit spray nozzle that can spray wide from a narrow elongated groove, it is particularly wide and long. It can be atomized and applied to a large object at a relatively high speed. In the present invention, it is also possible to prevent the precipitation of particles with bubbles and to apply while easily eliminating the bubbles downstream of the coating device.
  • the flow rate is detected by a flow meter that can detect the flow rate of the foam slurry mixture moving in the pipe outside the pipe, and the WO2013108669 method invented by the present invention is applied to the object to be applied before being applied to the object. It is possible to combine the methods of measurement and control them for quality control.
  • a density meter may be installed instead of the flow meter.
  • a commercially available flow meter device that can control the flow rate of each slurry, or the flow rate change of the circulation line before, after, or both of the discharge devices from outside the flow path such as a pipe, etc. It can be managed by adopting such as.
  • the pulse-like spray is effective because it is easy to manage the waveform of the hydraulic pressure, it is possible to increase the drop in the hydraulic pressure, and it is easy to check the change in the flow rate. Further, the consistency with the data in the coating weight measuring device can be confirmed at a desired timing. Therefore, for example, the coating weight of each material can be controlled constantly or instantly up to the fine part of the electrode, and a high-performance, high-quality electrode or the like can be formed.
  • the present invention is a method of applying a liquid containing at least particles or particles and short fibers to an object, wherein at least the particles or at least a non-volatile component containing particles and short fibers and at least a solvent are mixed to form a slurry.
  • the foam slurry mixture is targeted by a step of mixing bubbles into the slurry to circulate the slurry circulation flow path at high speed while preventing the precipitation of at least the particles as a bubble slurry mixture, and a coating device connected to the slurry circulation flow path.
  • a coating method comprising a step of coating an object while extinguishing at least a part of the bubbles.
  • the non-volatile content of the slurry is 65% by weight or less, of which the weight ratio of solid particles or particles to short fibers is 55% or less, the binder is 10% by weight or less, and the volatile content is Provided is a coating method characterized by having a viscosity of 35% or more and a viscosity of a slurry of 3000 mPa ⁇ s or less.
  • the viscosity of the slurry of the present invention is 1000 mPa ⁇ s or less, and the viscosity is 1000 mPa ⁇ s or less.
  • At least one of the dehumidified compressed air, argon, nitrogen, and carbon dioxide gas is selected as the foam gas, and the gas is finely divided in a pulsed manner and supplied so as to be mixed in the slurry, and the object is heated.
  • a coating method characterized by.
  • the slurry of the present invention contains a binder, the solvent consists of at least two or more kinds of solvents, at least one solvent is the parent solvent of the binder, and the remaining at least one solvent has a lower boiling point than the parent solvent.
  • a coating method characterized by having a solvent having a boiling point of 120 degrees or less, which has an azeotropic effect.
  • the present invention provides a coating method characterized by extinguishing 80% or more of the gas contained in the bubbles mixed in the slurry between the coating device and the object, or on the object.
  • the coating device of the present invention is a spray device, and provides a coating method characterized by adding a solvent between the upstream and downstream of the spray device to reduce the viscosity of the slurry and applying the slurry to an object.
  • the present invention is a long base material for which the object is handled in a roll-to-roll manner
  • the coating device is a slot nozzle, a compressed gas assist slot nozzle, or a slit arranged perpendicular to or substantially perpendicular to the base material.
  • a coating method comprising selecting at least one from a spray nozzle or a head having at least a plurality of two-fluid spray nozzles.
  • the object is an electrolyte membrane for a fuel cell or a gas diffusion layer
  • the slurry is an electrode ink having a solid content of 0.5 to 15% by weight containing platinum-catalyzed nanoparticles to form a membrane electrode composite.
  • the object is an electrolyte membrane for a fuel cell or a gas diffusion layer
  • the slurry is an electrode ink having a solid content of 0.5 to 15% by weight containing platinum-catalyzed nanoparticles to form a membrane electrode composite.
  • the present invention provides an all-solid-state battery manufacturing method or an all-solid-state battery, wherein the object is selected from a current collector, an electrode layer, and a solid electrolyte layer, and the slurry is an electrode slurry or a solid electrolyte slurry. ..
  • the quantity, shape, type, and specific gravity of particles and staple fibers do not matter.
  • the type of binder or solvent does not matter. Electrolyte solutions such as ionomers for fuel cells, Nafion solutions from Dupont, binders such as vinylidene fluoride (PVDF) for the positive electrode of secondary batteries and styrene butadiene rubber (SBR) for the negative electrode, and other thickeners with a high boiling point, for example. Glycerin and the like used as can be used. Glycerin can be expected to have an azeotropic effect with a low boiling point solvent such as ethanol and 2-propanol. Further, in the present invention, the volatilization of the solvent or the thickener can be promoted by heating the object, applying the slurry under vacuum, or moving the slurry under vacuum after application.
  • PVDF vinylidene fluoride
  • SBR styrene butadiene rubber
  • the type of the secondary battery does not matter.
  • a lithium ion secondary battery may be used, and a sodium ion secondary battery may be used.
  • the secondary battery of the present invention may be an all-solid-state battery of the next-generation secondary battery, and may be an all-solid-state air battery.
  • the type and shape of the active material particles for the positive electrode or the negative electrode are not limited regardless of the type of the sulfide-based or oxide-based solid electrolyte particles.
  • the porous carbon supporting platinum particles of several nanometers of the fuel cell supports platinum in the mesopores and macropores on the surface thereof, and the poisoning due to the contact with the ionomer can be reduced over time.
  • Micropores, mesopores, and macropores can be formed on the electrodes by stacking with.
  • the contact area at the interface can be increased, the battery performance can be improved.
  • a slot nozzle is used to add glycerin having a boiling point of about 400 ° C. to increase the viscosity with a solid content ink having a low solid content, for example, 7% by weight, such as an electrolyte membrane (PEM) at the outlet of the slot nozzle.
  • PEM electrolyte membrane
  • the WET application thickness is covered by bubbles, and after application, the ink viscosity can be instantaneously lowered by heating from the opposite side of application to PEM or by adsorption heating, so the final By defoaming the bubbles, it is possible to apply a thin film, a continuous film having fine irregularities with a desired distribution thickness, and a dense porous shape. Without foam, you can only apply on a coarse porous.
  • the application of the foam slurry mixture can also be applied under vacuum.
  • the number of cavities in the nozzle downstream of the on-off valve of the coating device can be reduced to the utmost. Normally, the foam slurry mixture in the cavity downstream of the open / close valve is pulled out to the outside of the nozzle or the like due to the pressure difference when the valve is closed, and the spicy of large droplets of the slurry component is generated by the explosive foaming of the foam. Then, the phenomenon can be suppressed.
  • a gas ejection means of a separate circuit is provided in the cavity and, if necessary, outside the nozzle, and collides with the spitting flow to enable pulse-like spraying, which is high-speed intermittent coating. It is also possible to heat the object at the time of application.
  • the binder and thickener of the slurry of the foam slurry mixture are heated by the object and the viscosity rapidly decreases, and at the same time, the cohesive force of the binder decreases, so that defoaming and foam bursting are promoted, and the solvent is used.
  • a desired coating film can be formed by making full use of an appropriate solvent balance and the like.
  • the surface of the coating film can be made into a dry coating film state of unevenness due to the accumulation of particles.
  • by applying the foam slurry mixture to the object under vacuum a coating film in a dry state can be obtained, and a desired speed can be achieved.
  • the method for producing a positive electrode for example, a ternary (NCM) active material, a conductive auxiliary material, PVDF, and NMP, which is a parent solvent for PVDF, are mixed to form a slurry.
  • NCM ternary
  • bubbles can be mixed and applied to the aluminum foil of the current collector, but the slurry of the active material, the foam slurry mixture of the bubbles, the carbon fine particles and carbon nanofibers of the conductive auxiliary material, and the single layer carbon mixed with the bubbles if necessary.
  • Dispersions (dispersions) of nanotubes and carbon nanofibers with a solvent can be alternately laminated and coated with thin films using separate coating devices such as sprays to form a positive electrode.
  • a small amount of binder and / and bubbles may be mixed in the conductive auxiliary agent dispersion liquid.
  • the current collector in order to promote volatilization even with a solvent having a high boiling point, the current collector is adsorbed by a heating drum, a heating table, a heating adsorption drum or a heating adsorption table to prevent the temperature from dropping due to the heat of vaporization due to solvent evaporation, and the drum or the like is used. Since it is heated from the inside, the solvent can be volatilized instantly by applying the slurry or the like.
  • the density of the electrode closer to the current collector can be inclined coating in which the density of the electrode is changed stepwise or continuously while eliminating the bubbles and leaving a desired amount of bubbles as the distance increases.
  • multiple coating devices such as slot nozzles, compressed gas assist slot nozzles, spray nozzle devices, etc. can be selected, and bubbles can be mixed into each slurry in consideration of the desired internal structure of the electrode film. Can be done.
  • the electrode formation to which the electrolyte particles of the all-solid-state battery are added and the formation of the electrolyte layer can be similarly applied to prevent precipitation by mixing bubbles with the slurry for the electrolyte layer.
  • single or multiple kinds of particles such as active material particles, single-walled carbon nanotubes (SWCNTs) and carbon nanofibers (CNF) as conductive aids, short fibers such as graphene, and a single mixture of fine particle carbon are mixed. It is also possible to laminate and coat with slurry, but it is not limited to this, and multiple slurry of different types, dispersions of multiple conductive auxiliaries, etc. are created, and a plurality of coating devices corresponding to the dispersions are used to obtain the desired distribution. Electrodes can be formed. In addition, you can choose to mix them with foam.
  • the object can be achieved by using static electricity as a single slurry or dispersion, for example, such as flocking, or by using an apparatus such as electrospinning.
  • Graphene alone or a combination of SWCNTs and the like is effective for lateral deployment of the electrode film.
  • it is important to stack independent different types of slurries, dispersions, etc. proposed by the present inventor in thin films or in trace amounts alternately in multiple layers with an independent device.
  • the ratio of the gas to the spray particles can be enriched by pulse spray or the like, and the coating can be directional while increasing the contact with the gas of fine particles or short fibers. ..
  • the solvent vapor can be volatilized by heating the dispersion, the slurry, or the like, or by heating the carrier gas or the like that moves the spray fine particles or the like. Therefore, in the present invention, the solid content of the dispersion of the conductive auxiliary agent can be suitably handled at 0.5% or less, further 0.05% or less, and pulse-like spray or static electricity is added to move electrons or the like in the electrode. Can be supported efficiently.
  • a binder having a strong adhesive effect to prevent performance deterioration due to expansion and contraction of metallic silicon particles and silicon oxide (SiOx) particles, which are effective for the negative electrode is ideally a spider web structure of fine fibers. It can partially cover silicon particles and the like so that they strongly adhere to the porous portion of porous carbon, SWCNTs, and carbon nanocups. That is, even when the silicon particles expand and contract, they can be further held by a strong adhesive or an adhesive fiber having a large surface area, which is supported on the macropores of the carbon structure or macropore carbon.
  • an electrode layer while adhering the carbon structure to the carbon structure and silicon or SiOx by forming the above into particles with separate heads and laminating them to partially form adhesive particles or non-woven fibers (cobweb-like) on the silicon surface. ..
  • a pulsed method with an impact is most suitable for spraying or moving the adhesive into fine particles and partially adhering it to the silicon surface.
  • carbon particles of a negative electrode active material to a pressure-sensitive adhesive solution or a pressure-sensitive adhesive emulsion to form a slurry, which is then applied.
  • the present invention as described above, tens to hundreds of nanometers, if necessary, several nanometers of metallic silicon or silicon oxide are supported in the pores of macroporous carbon or in the carbon structure, and further, for example, a net.
  • fine carbon in the shape of a mesh, and a pressure-sensitive adhesive that produces fine spider webs and short fibers, it is possible to prevent the silicon from falling off due to expansion and contraction during charging and discharging of the secondary battery.
  • the object can be heated.
  • the heating temperature is preferably 30 to 200 ° C., more preferably 50 to 150 ° C., as it can rapidly reduce the viscosity of the binder and cause the bubbles to expand and burst.
  • the heated adsorption drum can be heated from the inside, the temperature drop due to the heat of vaporization of the solvent can be prevented, and the evaporation of the solvent can be promoted.
  • the solvent component of the slurry that has been atomized by spraying or the like can be brought into contact with the object and wetted, and at the same time, it can be evaporated.
  • the time required to evaporate the solvent by 95% or more is preferably within 5 seconds, more ideally within 2 seconds.
  • the distance between the tip of the coating head and the object is reduced to, for example, within 50 mm.
  • the impact of the spray particles can be increased, so that high-density solid particles can be deposited.
  • the present invention it is possible to provide a high-performance coating method, a fuel cell manufacturing method or a fuel cell, a secondary battery manufacturing method or a secondary battery, an all-solid-state battery manufacturing method or an all-solid-state battery.
  • the slurry in the container according to the embodiment of the present invention is moved downstream by the first pump, and the gas that has also moved downstream of the gas cylinder is merged and mixed, and the gas slurry mixture is sucked by the pump and circulated by the circulation circuit.
  • the slurry pressurized gas in the container according to the embodiment of the present invention pressurizes and moves downstream, and the gas that has also moved downstream of the gas cylinder is merged and mixed, and the gas slurry mixture is sucked by a pump and circulated by a circulation circuit. It is a schematic cross-sectional view which arranged the coating head in a flow path.
  • Gas is mixed into the slurry in the container according to the embodiment of the present invention as bubbles from the lower part to make the structure difficult for the bubbles to rise on the slurry surface, and the mixture of bubbles and slurry is stirred and aggregated to pump the mixture.
  • It is a schematic cross-sectional view of a circulation system of a foam slurry mixture for each slurry in a container, in which a coating machine is installed in the middle of circulation by sucking and circulating the mixture, and the outlet of the circulation is made to flow into a mixture of foam and slurry.
  • Gas bubbles are mixed into the pressurized slurry in the first container according to the embodiment of the present invention, and the mixture is made into a rough mixture of the foam slurry by a stirrer and is not pressurized via the coating device or the first.
  • the foam slurry mixture in the second container is pumped to the first container at a pressure higher than the pressure in the first container, and the foam is moved to the container 1 in the second container, which is lower than the pressure inside the container.
  • It is a schematic cross-sectional view which makes a foam slurry mixture into a denser mixture as a circulation transfer system of a slurry mixture.
  • the compressed gas flows out or is ejected from the slot nozzle on the moving direction side of the object to crush the bubbles and crush the object. It is a schematic cross-sectional view which applies the slurry to.
  • the foam slurry mixture according to the embodiment of the present invention is applied to an object by a slot nozzle of a kind of coating apparatus, the compressed gas flows out or is ejected from both sides of the slot nozzle to crush the bubbles and crush the object. It is a schematic cross-sectional view which applies the slurry to.
  • the slurry 2 in the container 1 is sucked by the first pump 3 downstream and sent to the next process via the pipe 110.
  • the slurry 2 may be stirred by a stirring device (not shown).
  • a stirring device not shown
  • the compressed gas can be adjusted to a desired pressure from the cylinder 4 by the regulator 5 which is a pressure adjusting means.
  • the slurry and gas merge via check valves 6, 7, etc., which are check valves, which are check valves.
  • the mixture After merging, the mixture is mixed as a foam slurry mixture by the mixing device 8, and the second pump 4 passes through the pipe 10, the coating device 101, 102, and the return pipe 103 from the coating device, and then again via the circulation valve 104. It is sucked by the pump 9 of the above and a circulation circuit is formed.
  • the amount consumed by the coating devices 101 and 102 is automatically sent from the mixing device 8 to construct an automatic circulation system.
  • the second pump is ideally a balanced feed type plunger pump that automatically sucks in and pressurizes the consumed material.
  • a positive displacement pump may be used.
  • a volumetric pump such as a rotating electric spur gear is preferable because it is easier to adjust the volume ratio with the gas. It is better to use an ultra-precision automatic opening / closing valve that opens and closes in milliseconds or microseconds (not shown) to intermittently send fine bubbles at high speed.
  • the slurry 22 in the container 21 is pressurized and pressurized by a regulator 23 of a compressed air or an inert gas source (not shown). It is sucked by the first pump 3 downstream and sent to the next process via the pipe 110.
  • the slurry 22 may be stirred by a stirring device (not shown). In particular, when the specific gravity of the particles is heavy, it is better to stir with a stirring means or the like.
  • the compressed gas can be adjusted to a desired pressure from the cylinder 25 by the regulator 25 which is a pressure adjusting means.
  • the slurry and gas merge via the automatic opening / closing valves 26, 27 and the like.
  • the mixture After merging, the mixture is mixed as a foam slurry mixture by the mixing device 28, and is sucked by the pump 29 again via the circulation valve 204 via the pipes 200, the coating devices 201 and 202, and the return pipe 203 from the coating device.
  • a circulation circuit is formed.
  • the amount consumed by the coating devices 201 and 202 is automatically sent from the mixing device 28 side, and an automatic circulation system is constructed.
  • a mixing device or a dispersing device such as a static mixer, a dynamic mixer, or a collision mixing method invented by the present inventor can be adopted so that bubbles and slurry are densely dispersed.
  • the pump 29 is ideally a balanced feed type pressurized gas driven plunger pump that automatically sucks and pressurizes the consumed material.
  • a positive displacement pump may be used.
  • the slurry 32 in the container 31 is stirred by the stirring device 34 and can maintain a desired dispersed state.
  • the gas moves from the gas container 36 to the lower side of the container 31 via the regulator 35 that regulates the gas pressure, and then moves through the automatic opening / closing valve 37 that connects the flow path to the inside of the container 31 and enters the container.
  • the gas is finely divided by the automatic opening / closing valve 37 to form a desired foam slurry mixture with the slurry 32.
  • a hood 305 which is a three-dimensional shielding plate, is provided to prevent bubbles from moving to the upper part of the container.
  • As the gas a gas having a heavy specific density can be selected according to the specific gravity of the slurry.
  • argon and carbon dioxide have a heavier specific gravity than nitrogen and are suitable because it takes time to reach the upper surface of the slurry in the container 31.
  • a plurality of gases can be independently released into, for example, the slurry 32 in the container 31 and mixed and used.
  • the foam slurry mixture is sucked and pressurized by the pump 38, and is further passed through the pipe 39, the return pipe 302 via the coating device 301, and the shielding plate in the container 31 via the circulation valve 303 for adjusting the circulation amount. It moves below 305 and is mixed by the stirrer 34.
  • the area downstream of the circulation valve may be returned to the vicinity of the suction port of the pump 38. Since a mixing means or a dispersing means (not shown) can be provided in the circulation circuit, the foam slurry mixture can be made into a densely mixed state and applied by the coating device 301.
  • the slurry 42 of the first container 41 is pressurized by the regulator 400 of the compressed gas set to the pressure desired by the container 41.
  • the slurry in the container 41 is stirred by the stirring device 44.
  • a plurality of gases having a heavy specific density can be selected.
  • the pressurized slurry 42 flows into the second container 401 via the coating device 48 through the flow path 47 pipe communicating with the lower part of the container.
  • the slurry 402 of the second container is sucked by the pump 405 in the pipe 403 and ejected to the lower part of the first container by the pipe 406.
  • An automatic opening / closing valve 420 for supplying bubbles (gas) is installed in the middle of the pipe 403 in which the slurry 402 is sucked into the pump 405.
  • the gas in the cylinder 46 is adjusted to a desired pressure by the regulator 45.
  • the second container 401 may be pressurized to a lower pressure than the first container. Further, the slurry in the second container 401 can be stirred by the stirring device 403. Further, when the level sensor (not shown) of the slurry 402 in the second container 401 detects the lower limit, the operation of the pump 405 can be automatically stopped.
  • the slurry in the first container drops, it can be detected by a level sensor (not shown) to stop the circulation system and coating, and the slurry can be filled.
  • the slurry can be filled automatically by another automatic slurry supply system, or can be manually supplied by removing the upper lid or the like of the first container 41.
  • a second flow path 430 having a low internal resistance which is different from the flow paths 47 and 49 of the coating device 48, may be provided. can.
  • To reduce the resistance of the second flow path 430 it is possible to increase the cross-sectional area of the flow path, shorten the flow path, or adopt both.
  • the inner diameter of the second flow path may be, for example, 6 mm or 8 mm or more.
  • mixing devices 460 and 470 such as a static mixer and a dynamic mixer using power can be installed upstream of the flow paths 47 and 49 for the coating device and the second flow path 430, for example.
  • the foam slurry mixture sucked and pressurized by the pump 405 over time is mixed by the mixing device installed in the pressure pipe 406, and ejected at a pressure higher than the pressure of the first container, and the flow paths 47 and 49 are required.
  • a circulation circuit is formed that flows into the second container 401 via the second flow path 430 and is further sucked by a pump, and the foam slurry mixture can be applied by the coating device 48 as a denser foam slurry mixture over time. ..
  • a plunger can be provided on the upper surface of the slurry 42 of the first container 41 to cut off the edge from the compressed gas.
  • FIG. 5 is a cross-sectional view of the tip of the compressed gas (air) assist slot nozzle.
  • the slot nozzle 52 downstream of the automatic opening / closing valve of the coating device (not shown) is shown. Since the clearance of the foam slurry mixture is narrow and pressure is applied in the slot nozzle 52, the bubbles of the foam slurry mixture do not expand. However, the moment the bubble leaves the nozzle, the bubble expands. Compressed gas passes through the flow path 53 toward the tip of the slot nozzle 52 and toward the foam slurry film 56 at the moment when it is applied to the object, and is ejected from the tip nozzle to form the coating film 56 while appropriately crushing the bubbles. do.
  • the viscosity of the applied foam slurry mixture decreases, the foam expands and it becomes easier to crush the foam with compressed gas, and the solvent has a high boiling point such as NMP. Also promotes evaporation.
  • FIG. 6 shows the tip of the slot nozzle 62, which is a modification of the compressed gas (air) assist slot nozzle.
  • Compressed gas is ejected from the compressed flow path from both sides of the discharge flow of the foam slurry mixture from the slot nozzle. Therefore, in addition to crushing the bubbles and applying the slurry to the object, the slurry can be applied while being sprayed into spray particles.
  • the slot nozzle length may be 100 mm, 500 mm, 1000 mm, 2000 mm or more. The slurry can be applied onto the object to the same width as the slot nozzle length.
  • the shim determines the discharge width of the slot flow, and make the length of innumerable openings (outflowing into fine stripes), for example, 50 micrometers or 200 micrometers. In addition, it can be formed to 500 micrometers or 1 mm to make the non-opening length 5 mm, 10 mm, and so on.
  • the shim thickness can also be, for example, 100 micrometers, 150 micrometers, 200 micrometers or more. Not only the slurry but also the gas outlets on both sides are processed with the same idea as the opening of the liquid, and when the opening length of the liquid is 200 micrometers, it is made slightly longer than that.
  • a large number of openings for example a 200 micrometer square opening, can be machined to the desired pitch, eg 15 mm, within a pitch of 5 to 50 mm so that the granular ejection patterns of the slurry from each opening do not interfere.
  • the desired pitch eg 15 mm
  • the ejection part is limited, but the slot nozzle is Since it is possible to perform a short traverse (for example, 7.5 mm under the above conditions) at high speed by going straight to the object, it is possible to cover the desired entire surface by pulse application even at high line speed.
  • This method can be applied not only in the field of the present invention but also in various fields such as a spray of a solution and a melt blown which is a fibrosis of a thermoplastic adhesive without mixing bubbles in the slurry.
  • a foam slurry mixture having a relatively low viscosity is sprayed from the airless spray nozzle 71 at a relatively low hydraulic pressure (about 0.15 to 0.6 MPa).
  • the liquid film 72 becomes a triangle from the tip of the airless spray nozzle 71, and the liquid film is eventually broken to generate unstable liquid mass streaks 74 at both ends and large droplets 75 downstream of the liquid film. It is generally applied to an object or the like with a liquid film near the line 73.
  • the flow rate distribution of the liquid film on the line 73 is 76,78, which is a flow with many ends, and the flow 77, which has a small flow rate, is in the center.
  • FIG. 7-b is a plan view in which the liquid film at the position of the object 700 and the line 73 is relatively moved and the liquid film of the foam slurry mixture is applied to the object 700. At the moment of application, points 76 and 78 having a high flow rate at both ends of the liquid film and places 77 having a low flow rate appear on the object.
  • points 76 and 78 having a high flow rate at both ends of the liquid film and places 77 having a low flow rate appear on the object.
  • the liquid film of the airless spray nozzle 71'and the object 700 move relative to each other to form a coating film of the foam slurry mixture on the object.
  • the coating flow rate distribution becomes a dry film having a large flow rate at both ends similar to the flow rate distribution of the liquid film of the nozzle.
  • the boiling point of the solvent of the slurry is raised and the object 700 is at room temperature or lower, the flow rate distribution at the wet ends of the liquid film is large (thick film) 76'and 78' due to surface tension. It can flow to a small (thin film) 77'location and migrate to form a relatively flat film.
  • the nozzle 71' can be pitch-feeded from the film in which the distribution at both ends is quickly set by heating or vacuuming the object, and the thick film portion can be shifted and recoated.
  • the distributions are shifted 76', 78', 77', and the liquid film is applied with fine irregularities by narrowing the angle of the triangle of the liquid film and narrowing the thin part per pattern by lowering the liquid pressure.
  • This method is also effective for slurries that do not contain bubbles.
  • the electrode formation of the fuel cell can handle more than 10 times the speed of one two-fluid spray, and the production speed is also increased. Since the coating efficiency is almost 100%, it is particularly effective for forming electrodes of an expensive platinum-catalyzed fuel cell.
  • the solid content of the fuel cell electrode forming slurry can be reduced to 3% or less, and the solid content of the anode can be reduced to 1% or less to reduce the amount of platinum per unit area.
  • the electrode ink has a low solid content and a low viscosity, it is effective to circulate the foam slurry mixture at high speed in order to prevent precipitation of the catalyst.
  • a slot nozzle having a width of 200 to 2000 mm can be applied to an object at high speed. If you want to leave bubbles, just apply the slot nozzle.
  • the back roll that supports the object may be heated.
  • the object that moves relative to the slot nozzle is mixed by foam slurry by heating the back roll to, for example, 30 to 200 ° C. and heating it by heat conduction from the back roll, or by heating the object while sucking it with a heating adsorption roll. It can accelerate the defoaming of the body and the evaporation of the solvent.
  • the foam while crushing it with speed, you can apply it while ejecting the compressed gas from one side or both sides with the compressed gas assist slot nozzle.
  • the viscosity of the binder, thickener, etc. is lowered, and defoaming and evaporation of the solvent can be promoted.
  • a solvent having a boiling point of more than 200 ° C. such as NMP
  • the drying of the coating film surface of the slurry is not promoted, so that a desired film can be formed.
  • the state of containing microbubbles can also be selected by manually or automatically adjusting the strength of addition or pressurization of the press roll particularly immediately afterwards.
  • the foam slurry mixture can be prepared in advance as a foam slurry mixture in a container, pumped by a circulation device and returned to the tank via the coating device to form a circulation system and applied to an object.
  • the foam slurry in another container that is on standby in advance can be automatically guided to the circulation circuit, so there is no need to stop the line operation.
  • the present invention even if the slurry is easily settled, as a foam slurry mixture, the settling of particles and the like is prevented, and even if the slurry is a low viscosity slurry, the settling of particles is prevented, and the coating amount is the same as that of the slurry. Since the flow rate of bubbles can be reduced, it is possible to apply a thin film.

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Abstract

Lors de la formation, à partir de particules solides, d'une suspension et, à partir de la suspension, de fines particules, puis lors de stratification des fines particules résultantes sous la forme de films fins, il a jusqu'à présent été nécessaire que la suspension présente une faible viscosité et une faible cohésion. Cependant, un problème survient en ce que, lorsque la suspension présente, en particulier, une densité élevée de particules ou une faible viscosité, les particules solides comprises dans la suspension sont déposées dans un système de manipulation de suspension ou un dispositif de revêtement. L'invention concerne un procédé comprenant : la sélection d'un gaz, en particulier d'un gaz ayant une densité spécifique supérieure à celle de l'air, d'un air déshumidifié et comprimé bon marché, ou similaire, la division fine du gaz ou de l'air afin de former des bulles, le mélange des bulles dans une suspension, et la circulation à une vitesse élevée du mélange résultant de bulles et suspension dans un dispositif de circulation ou similaire, empêchant ainsi le dépôt des particules solides de la suspension même lorsque la suspension présente une faible viscosité ; le revêtement d'un objet cible au moyen du mélange en utilisant une buse telle qu'une buse à fente, une buse à fente assistée par du gaz comprimé, une buse de pulvérisation fendue et une buse de pulvérisation de deux fluides ; le revêtement de l'objet cible avec le mélange par chauffage, tel que nécessaire, l'objet cible et le freinage des bulles de gaz en projetant le gaz comprimé, ou le revêtement de l'objet cible avec le mélange tout en retirant les bulles à l'aide d'un flux d'assistance comprimé à partir de la buse à fente à accompagnement par du gaz comprimé ; et l'élimination d'au moins 80 % du gaz obtenu par expansion ou élimination, selon les besoins, des bulles de gaz du mélange de bulles et suspension sur l'objet cible.
PCT/JP2021/028910 2020-09-01 2021-08-04 Procédé de revêtement, procédé de fabrication d'une pile à combustible ou pile à combustible, procédé de fabrication d'une batterie secondaire ou batterie secondaire, et procédé de fabrication d'une batterie tout-solide ou batterie tout-solide WO2022049974A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000256666A (ja) * 1999-03-09 2000-09-19 Toshiba Corp 蛍光体の再生方法および蛍光体の再生装置
JP2010232073A (ja) * 2009-03-27 2010-10-14 Sanyo Electric Co Ltd 非水電解質二次電池用の電極の製造方法
JP2018107355A (ja) * 2016-12-27 2018-07-05 日亜化学工業株式会社 発光装置の製造方法

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Publication number Priority date Publication date Assignee Title
JP5202838B2 (ja) * 2006-12-12 2013-06-05 東京応化工業株式会社 スリットノズル
JP5386408B2 (ja) * 2010-03-03 2014-01-15 三菱重工業株式会社 電極製造装置
WO2015045533A1 (fr) * 2013-09-27 2015-04-02 株式会社日立ハイテクノロジーズ Procédé de fabrication de batterie secondaire au lithium-ion, dispositif de fabrication de batterie secondaire au lithium-ion et batterie secondaire au lithium-ion

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2000256666A (ja) * 1999-03-09 2000-09-19 Toshiba Corp 蛍光体の再生方法および蛍光体の再生装置
JP2010232073A (ja) * 2009-03-27 2010-10-14 Sanyo Electric Co Ltd 非水電解質二次電池用の電極の製造方法
JP2018107355A (ja) * 2016-12-27 2018-07-05 日亜化学工業株式会社 発光装置の製造方法

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