WO2025028068A1 - 電解コンデンサおよび電解コンデンサの製造方法 - Google Patents

電解コンデンサおよび電解コンデンサの製造方法 Download PDF

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Publication number
WO2025028068A1
WO2025028068A1 PCT/JP2024/022728 JP2024022728W WO2025028068A1 WO 2025028068 A1 WO2025028068 A1 WO 2025028068A1 JP 2024022728 W JP2024022728 W JP 2024022728W WO 2025028068 A1 WO2025028068 A1 WO 2025028068A1
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Prior art keywords
laminate
separator
conductive polymer
foil
anode foil
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English (en)
French (fr)
Japanese (ja)
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由起也 下山
達治 青山
瞬平 松下
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Panasonic Intellectual Property Management Co Ltd
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Panasonic Intellectual Property Management Co Ltd
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Priority to JP2025537729A priority Critical patent/JPWO2025028068A1/ja
Priority to CN202480048193.XA priority patent/CN121548872A/zh
Publication of WO2025028068A1 publication Critical patent/WO2025028068A1/ja
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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
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/02—Diaphragms; Separators
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/022—Electrolytes; Absorbents
    • H01G9/025—Solid electrolytes
    • H01G9/028—Organic semiconducting electrolytes, e.g. TCNQ
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
    • H01G9/004—Details
    • H01G9/04—Electrodes or formation of dielectric layers thereon
    • H01G9/048—Electrodes or formation of dielectric layers thereon characterised by their structure
    • H01G9/052—Sintered electrodes

Definitions

  • This disclosure relates to electrolytic capacitors and methods for manufacturing electrolytic capacitors.
  • a known electrolytic capacitor is one that includes a wound body of an anode foil, a separator, and a cathode foil.
  • One example of such an electrolytic capacitor includes a conductive polymer layer disposed in the wound body.
  • the conductive polymer layer can be formed by impregnating the wound body with a dispersion liquid that contains a conductive polymer.
  • Various proposals have been made in the past regarding electrolytic capacitors that include a conductive polymer layer.
  • Patent Document 1 (Patent No. 6911910) states in claim 1 that "an electrolytic capacitor is characterized in that a capacitor element is formed by winding an anode electrode foil and a cathode electrode foil with a separator interposed therebetween, and a solid electrolyte layer is formed using a conductive polymer compound dispersion containing conductive polymer particles and sorbitol or sorbitol and a polyhydric alcohol, the solid electrolyte layer containing 60 to 92 wt % of the sorbitol or sorbitol and a polyhydric alcohol, and the voids in the capacitor element in which the solid electrolyte layer is formed are filled with an electrolyte solution containing 10 wt % or more of ethylene glycol in a solvent.”
  • Claim 1 of Patent Document 2 JP Patent Publication No. 2019-516241 describes a "capacitor including a processing element, the processing element including: an anode including a dielectric on a surface and an anode conductive polymer layer on the surface of the dielectric; a cathode including a cathode conductive polymer layer; a conductive separator between the anode and the cathode; an anode lead in electrical contact with the anode; and a cathode lead in electrical contact with the cathode.”
  • Claim 1 of Patent Document 3 describes a hybrid electrolytic capacitor comprising: a cathode having a cathode substrate made of a valve metal, an oxide layer made of an oxide of the valve metal provided on the surface of the cathode substrate, an inorganic conductive layer containing an inorganic conductive material provided on the surface of the oxide layer, and an organic conductive layer containing a conductive polymer provided on the surface of the inorganic conductive layer; an anode having an anode substrate made of a valve metal, and a dielectric layer made of an oxide of the valve metal constituting the anode substrate provided on the surface of the anode substrate; a solid electrolyte layer provided between the organic conductive layer of the cathode and the dielectric layer of the anode and containing conductive polymer particles in contact with them, and an electrolyte filled between the conductive polymer particles in the solid electrolyte layer.
  • Patent No. 6911910 Special Publication No. 2019-516241 International Publication No. 2021/125182
  • the laminate includes an anode foil having a dielectric layer on its surface, a separator laminated to the anode foil, a cathode foil, and a conductive polymer layer formed on the surface of the dielectric layer and in the voids of the separator.
  • the anode foil and the separator are bonded together by the conductive polymer layer.
  • the manufacturing method includes a preparation step of preparing an anode foil having a dielectric layer on a surface thereof, a laminate sheet formation step of forming a laminate sheet including the anode foil, a separator bonded to the anode foil, and a conductive polymer layer, a first laminate formation step of cutting the laminate sheet to a first width to form a first laminate including the anode foil, the separator, and the conductive polymer layer, and a second laminate formation step of stacking the first laminate and a cathode foil having a second width such that the separator is disposed between the anode foil and the cathode foil to form a second laminate.
  • the laminated sheet forming process includes a coating liquid applying process in which, with the anode foil and the separator overlapped, a coating liquid containing a conductive polymer and a liquid medium is applied to the surface of the dielectric layer and into the voids of the separator, and a liquid medium removing process in which at least a portion of the liquid medium is removed from the coating liquid to form the conductive polymer layer on the surface of the dielectric layer and in the voids of the separator, and the anode foil and the separator are bonded together to form the laminated sheet.
  • an electrolytic capacitor containing a liquid component and a conductive polymer layer and having a low ESR can be obtained.
  • FIG. 1 is a side view illustrating a schematic diagram of an example of an electrolytic capacitor according to an embodiment of the present disclosure.
  • FIG. 2 is an exploded perspective view illustrating a schematic diagram of an example of a capacitor element according to an embodiment of the present disclosure.
  • FIG. 3A is a cross-sectional view that illustrates a process of an example of a method for forming a second laminate (capacitor element).
  • FIG. 3B is a cross-sectional view that illustrates an example of a step subsequent to FIG. 3A.
  • FIG. 3C is a cross-sectional view that illustrates an example of a step subsequent to FIG. 3B.
  • FIG. 4 shows a schematic diagram of a peel strength measuring device.
  • the dispersion liquid containing the conductive polymer has a high viscosity, even if the dispersion liquid is impregnated into the wound body, it may not be possible to form a sufficient conductive polymer layer inside the wound body. Insufficient formation of the conductive polymer layer can cause an increase in equivalent series resistance (ESR).
  • ESR equivalent series resistance
  • This disclosure provides an electrolytic capacitor that contains a liquid component and a conductive polymer layer and can reduce the ESR.
  • the manufacturing method according to this embodiment may be referred to as "manufacturing method (M)" below.
  • the manufacturing method (M) includes a preparation step, a laminated sheet forming step, a first laminate forming step, and a second laminate forming step, in this order.
  • the manufacturing method (M) may also include an impregnation step after the second laminate forming step. These steps will be described later.
  • the preparation step is a step of preparing an anode foil having a dielectric layer on its surface.
  • the anode foil having a dielectric layer on its surface may be a commercially available product, or may be formed by forming a dielectric layer on the surface of a metal foil (anode foil).
  • the dielectric layer may be formed by a known method. For example, the dielectric layer may be formed by oxidizing the surface of the metal foil (anode foil).
  • the laminate sheet forming step is a step of forming a laminate sheet including an anode foil, a separator bonded to the anode foil, and a conductive polymer layer.
  • the laminate sheet forming step includes a coating liquid application step and a liquid medium removal step.
  • the obtained laminate sheet is cut to a width to be used in a capacitor element in the next first laminate forming step. Therefore, the width of the anode foil and the separator used in the laminate sheet forming step is larger than the width of the anode foil and the separator in the capacitor element.
  • the separator is bonded to at least one side of the anode foil, for example, to both sides of the anode foil.
  • the coating liquid application process is a process in which, with the anode foil and separator superimposed, a coating liquid containing a conductive polymer and a liquid medium is applied to the surface of the dielectric layer (the dielectric layer on the surface of the anode foil) and into the voids in the separator.
  • the liquid medium removal process is a process in which at least a portion of the liquid medium is removed from the coating liquid to form a conductive polymer layer on the surface of the dielectric layer and in the voids in the separator, and the anode foil and separator are bonded together to form a laminated sheet. Examples of conductive polymers are described below.
  • the liquid medium may contain water and an organic compound that does not boil at 100°C at 1 atmosphere (101,325 Pa).
  • organic compound may be referred to as "organic compound (C).”
  • Organic compound (C) may be one type of compound or may be composed of multiple types of compounds.
  • the viscosity of the coating liquid may be, for example, 10 mPa ⁇ s or more (for example, 100 mPa ⁇ s or more) and 200 mPa ⁇ s or less.
  • the coating liquid is easy to apply to the anode foil, cathode foil, and separator, and is easy to impregnate the separator.
  • the viscosity of the coating liquid is measured at room temperature (20°C) using a vibration viscometer (e.g., VM-100A, manufactured by Sekonic Corporation).
  • Methods for applying the coating liquid to the separator include a method of impregnating the separator with the coating liquid.
  • the coating liquid applied to the separator permeates into the separator and reaches the dielectric layer on the surface of the anode foil.
  • a conductive polymer layer is formed on the surface of the dielectric layer and over the entire thickness of the separator. The formation of the conductive polymer layer greatly improves the adhesion between the anode foil (more specifically, the dielectric layer on the surface of the anode foil) and the separator.
  • the method of removing at least a part of the liquid medium from the coating liquid is not particularly limited, and can be performed by heating or the like.
  • heating may be performed so that the organic compound (C) remains in the polymer layer.
  • the coating liquid contains an organic compound (C) and water (liquid medium)
  • the heating temperature may be 100°C or higher, 120°C or higher, or 140°C or higher, and may be 200°C or lower, or 160°C or lower.
  • the heating temperature may be in the range of 100°C to 200°C. There is no particular limit to the heating time, and it may be a time that allows a part of the liquid medium to be appropriately removed. An example of the heating time is in the range of 5 to 60 minutes.
  • the organic compound (C) By leaving the organic compound (C) in the conductive polymer layer, it is possible to reduce the shrinkage of the conductive polymer layer when the liquid medium is removed from the coating liquid. As a result, in the subsequent impregnation process, the liquid component (e.g., electrolyte) can easily penetrate into the conductive polymer layer. As a result, the liquid component's function of forming a dielectric layer (oxide film) can be fully exerted, and leakage current is reduced.
  • the liquid component e.g., electrolyte
  • the first laminate formation step is a step of forming a first laminate including an anode foil, a separator, and a conductive polymer layer by cutting the laminate sheet to a first width.
  • the width W0 of the laminate sheet may be twice or more the first width W1 of the first laminate.
  • a plurality of first laminates can be formed from the laminate sheet by cutting the laminate sheet.
  • the method of cutting the laminate sheet is not limited, and a known method may be used.
  • the laminate sheet may be cut using a slitter used for cutting metal foil.
  • the width of the separator and the width of the anode foil are each substantially the same as the first width W1 of the first laminate.
  • the width means the length in a direction perpendicular to the longitudinal direction.
  • the width of the members (first laminate and cathode foil) used to form the wound body means the length in a direction parallel to the winding axis of the wound body.
  • the first width W1 is not limited and is selected according to the type and application of the electrolytic capacitor.
  • the first width W1 may be 2.0 mm or more, or 5.0 mm or more, and may be 20 mm or less, or 12 mm or less.
  • the cut surface of the anode foil is exposed. It is preferable to form a dielectric layer on the exposed cut surface by subsequent chemical conversion treatment or the like.
  • the separator is attached to one or both sides of the anode foil.
  • the second laminate forming step is a step of forming a second laminate by stacking the first laminate and a cathode foil having a second width such that a separator is disposed between the anode foil and the cathode foil.
  • the width W2 (second width W2) of the cathode foil may be smaller than the first width W1 of the first laminate. In that case, in the second laminate forming step, the first laminate and the cathode foil are stacked such that the end edge in the width direction of the cathode foil is disposed inside the end edge in the width direction of the first laminate.
  • the first laminate and the cathode foil are disposed such that both of the two end edges of the cathode foil are located between the two end edges of the first laminate in the width direction without contacting the two end edges of the first laminate.
  • a short circuit between the anode foil and the cathode foil can be suppressed.
  • the laminate may be a wound body.
  • the wound body may be formed by winding the anode foil, the cathode foil, and the separator so that the separator is disposed between the anode foil and the cathode foil.
  • the anode foil, the cathode foil, and the separator are stacked in the radial direction of the wound body.
  • the laminate may be formed by stacking flat anode foils, flat cathode foils, and flat separators in one direction.
  • a laminate may be formed by stacking multiple anode foils, multiple cathode foils, and multiple separators in one direction.
  • the anode foils and cathode foils are arranged alternately, and the separator is arranged between the anode foils and the cathode foils.
  • the difference (W1-W2) between the first width W1 of the first laminate and the second width W2 of the cathode foil may be 0.5 mm or more, or 1.0 mm or more, and may be 2.0 mm or less, 1.5 mm or less, or 1.2 mm or less.
  • the difference (W1-W2) may be in the range of 0.5 mm to 1.2 mm.
  • a capacitor element impregnated with the liquid component (LC) is obtained. Thereafter, other processes are carried out as necessary. For example, a process may be carried out in which the capacitor element impregnated with the liquid component (LC) is enclosed in an exterior body.
  • the manufacturing method (M) may include a liquid application step and a removal step in this order after the second laminate formation step and before the impregnation step.
  • the liquid application step is a step of impregnating the laminate with a liquid (hereinafter, sometimes referred to as "liquid (L)").
  • the removal step is a step of removing at least a part of the liquid (L) impregnated in the second laminate.
  • the liquid (L) may be a liquid containing water as a main component and an organic compound (C) that does not boil at 100°C under 1 atmosphere.
  • the liquid used in the liquid application step may be a liquid obtained by removing the conductive polymer component from the coating liquid used in the laminate sheet formation step.
  • the impregnation with the liquid in the liquid application step may be performed by the method exemplified for the coating liquid application step in the laminate sheet formation step.
  • the removal of the liquid in the removal step may be performed by the method exemplified for the liquid medium removal step in the laminate sheet formation step.
  • the cathode foil consists only of a metal foil (e.g., aluminum foil)
  • an oxide layer forms on the surface of the metal foil, and capacitance also occurs in the cathode foil.
  • the capacitance of the anode foil and the capacitance of the cathode foil are combined, which can cause a problem of a decrease in the capacitance of the entire capacitor.
  • an inorganic layer By covering the surface of the metal foil with an inorganic layer, etc., it is possible to prevent such a problem from occurring. In other words, by forming an inorganic layer, it is possible to draw out the capacitance of only the anode foil.
  • the ESR will be high.
  • Inorganic layers tend to repel water, so in the conventional method of forming a conductive polymer layer by impregnating a laminate (capacitor element) with an aqueous dispersion of a conductive polymer, the conductive polymer has difficulty entering between the inorganic layer of the cathode foil and the anode foil in the laminate, making it impossible to form a uniform conductive polymer layer on the separator placed between the cathode foil and anode foil, resulting in an increase in ESR.
  • manufacturing method (M) a laminate (capacitor element) is formed using a separator on which a conductive polymer layer has already been formed. This makes it possible to prevent the conductive polymer from becoming unevenly distributed within the separator.
  • the peel strength between the anode foil and the separator may be 1.0 N/cm or more, 2.0 N/cm or more, or 2.9 N/cm or more. There is no particular upper limit to the peel strength.
  • the peel strength can be measured by the method described in the examples.
  • electrolytic capacitor The electrolytic capacitor according to this embodiment may be referred to as "electrolytic capacitor (E)" below.
  • the electrolytic capacitor (E) may be manufactured by the manufacturing method (M) described above.
  • the matters described for the manufacturing method (M) may be applied to the electrolytic capacitor (E), and therefore, duplicated explanations may be omitted.
  • the matters described for the electrolytic capacitor (E) may also be applied to the manufacturing method (M).
  • the electrolytic capacitor (E) includes a laminate and a liquid component impregnated in the laminate.
  • the laminate includes an anode foil having a dielectric layer on its surface, a separator laminated on the anode foil, a cathode foil, and a conductive polymer layer formed on the surface of the dielectric layer and in the gaps of the separator.
  • the anode foil and the separator are bonded together by the conductive polymer layer.
  • the width of the cathode foil (second width W2) may be smaller than the width of the anode foil (first width W1).
  • the width of the separator is substantially the same as the first width W1 of the anode foil.
  • the electrolytic capacitor (E) provides the effects described in the manufacturing method (M).
  • the configuration of the electrolytic capacitor (E) makes it possible to reduce the ESR.
  • the surface density of the conductive polymer layer may be in the above range.
  • the surface density of the conductive polymer layer may be 0.05 mg/cm2 or more and 1.0 mg/ cm2 or less.
  • the cathode foil may have an inorganic layer on its surface. In that case, it is preferable that the conductive polymer layer is in close contact with the inorganic layer.
  • the peel strength between the anode foil and the separator may be 1.0 N/cm or more.
  • the laminate may be a wound body or a laminate other than a wound body.
  • the term "conductive polymer component" may be used.
  • the conductive polymer component is made of a conductive polymer.
  • the conductive polymer component is made of a conductive polymer and a dopant.
  • the coating liquid used in the polymer layer forming step may contain a conductive polymer and water.
  • the conductive polymer (conductive polymer component) may be contained in the coating liquid in the form of particles.
  • the coating liquid may be an aqueous dispersion of the conductive polymer (conductive polymer component).
  • the coating liquid may contain other components (e.g., organic compound (C)).
  • the organic compound (C) may contain at least one selected from the group consisting of polyhydric alcohols, sulfolane, ⁇ -butyrolactone, and boric acid esters, or may be at least one of the above.
  • the organic compound (C) may contain at least one selected from the group consisting of glycols, glycerins, sugar alcohols, sulfolane, ⁇ -butyrolactone, and boric acid esters, or may be at least one of the above.
  • polyhydric alcohols examples include glycols, glycerins, and sugar alcohols.
  • glycols include ethylene glycol, diethylene glycol, triethylene glycol, polyalkylene glycols (e.g., polyethylene glycol), polyoxyethylene polyoxypropylene glycol (ethylene oxide-propylene oxide copolymer), and the like.
  • glycerins include glycerin and polyglycerin.
  • sugar alcohols include mannitol, xylitol, sorbitol, erythritol, and pentaerythritol, and the like.
  • Examples of conductive polymers include polypyrrole, polythiophene, polyfuran, polyaniline, polyacetylene, and derivatives thereof.
  • the derivatives include polymers having polypyrrole, polythiophene, polyfuran, polyaniline, and polyacetylene as the basic skeleton.
  • a derivative of polythiophene includes poly(3,4-ethylenedioxythiophene).
  • These conductive polymers may be used alone or in combination.
  • the conductive polymer may also be a copolymer of two or more monomers.
  • the weight-average molecular weight of the conductive polymer is not particularly limited and may be in the range of 1,000 to 100,000, for example.
  • a preferred example of a conductive polymer is poly(3,4-ethylenedioxythiophene) (PEDOT).
  • the conductive polymer may be doped with a dopant. From the viewpoint of suppressing dedoping from the conductive polymer, it is preferable to use a polymer dopant as the dopant.
  • polymer dopants include polyvinyl sulfonic acid, polystyrene sulfonic acid, polyallyl sulfonic acid, polyacryl sulfonic acid, polymethacryl sulfonic acid, poly(2-acrylamido-2-methylpropane sulfonic acid), polyisoprene sulfonic acid, polyacrylic acid, and the like. These may be used alone or in combination of two or more. At least a portion of these may be added in the form of a salt.
  • a preferred example of a dopant is polystyrene sulfonic acid (PSS).
  • the dopant may be polystyrenesulfonic acid
  • the conductive polymer may be poly(3,4-ethylenedioxythiophene). That is, the conductive polymer component may be poly(3,4-ethylenedioxythiophene) doped with polystyrenesulfonic acid.
  • the pH of the coating liquid is preferably less than 7.0 in order to suppress dedoping of the dopant, and may be 6.0 or less or 5.0 or less.
  • the pH of the coating liquid may be 1.0 or more, or 2.0 or more.
  • the water content in the coating liquid may be 40% by mass or more, 50% by mass or more, 80% by mass or more, 90% by mass or more, or 95% by mass or more.
  • the water content may be 98% by mass or less, 95% by mass or less, 90% by mass or less, or 80% by mass or less.
  • the content of the organic compound (C) in the coating liquid may be 1.0 mass% or more, 3.0 mass% or more, 5.0 mass% or more, or 10 mass% or more. It may be 30 mass% or less, 20 mass% or less, 15 mass% or less, or 10 mass% or less.
  • the content of the conductive polymer component in the coating liquid may be 0.5 mass% or more, or 1.0 mass% or more, and may be 4.0 mass% or less, 3.0 mass% or less, or 2.0 mass% or less.
  • the content may be in the range of 0.5 to 4.0 mass% or 1.0 to 4.0 mass%. In any of these ranges, the upper limit may be 3.0 mass% or 2.0 mass%.
  • the content is preferably in the range of 1.0 to 3.0%.
  • the mass of the dopant is included in the mass of the conductive polymer component.
  • the mass of the dopant contained in the coating liquid there are no particular limitations on the mass of the dopant contained in the coating liquid, and it may be in the range of 0.1 to 5 times (e.g., 0.5 to 3 times) the mass of the conductive polymer contained in the coating liquid.
  • the water content: organic compound (C) content: conductive polymer component content may be 40-98:1.0-59.5:0.5-4.0, or the water content: organic compound (C) content: conductive polymer component content may be 69.5-98:1.0-30:0.5-4.0.
  • liquid component (LC) examples of the liquid component (LC) used in the impregnation step include a non-aqueous solvent and an electrolytic solution.
  • the electrolytic solution may be an electrolytic solution containing a non-aqueous solvent and a solute dissolved in the non-aqueous solvent.
  • the liquid component (LC) may be a component that is liquid at room temperature (25° C.) or a component that is liquid at the temperature when the electrolytic capacitor is used.
  • the non-aqueous solvent used in the liquid component (LC) may be an organic solvent, an ionic liquid, or a protic solvent.
  • non-aqueous solvents include polyhydric alcohols such as ethylene glycol and propylene glycol, cyclic sulfones such as sulfolane (SL), lactones such as ⁇ -butyrolactone ( ⁇ BL), amides such as N-methylacetamide, N,N-dimethylformamide, and N-methyl-2-pyrrolidone, esters such as methyl acetate, carbonate compounds such as propylene carbonate, ethers such as 1,4-dioxane, ketones such as methyl ethyl ketone, and formaldehyde.
  • polyhydric alcohols such as ethylene glycol and propylene glycol
  • cyclic sulfones such as sulfolane (SL)
  • lactones such as ⁇ -butyrolactone ( ⁇ BL)
  • a polymer solvent may be used as the non-aqueous solvent.
  • polymer solvents include polyalkylene glycol, derivatives of polyalkylene glycol, and compounds in which at least one hydroxyl group in a polyhydric alcohol is replaced with polyalkylene glycol (including derivatives).
  • examples of polymer solvents include polyethylene glycol (PEG), polyethylene glycol glyceryl ether, polyethylene glycol diglyceryl ether, polyethylene glycol sorbitol ether, polypropylene glycol, polypropylene glycol glyceryl ether, polypropylene glycol diglyceryl ether, polypropylene glycol sorbitol ether, and polybutylene glycol.
  • polymer solvents further include ethylene glycol-propylene glycol copolymers, ethylene glycol-butylene glycol copolymers, and propylene glycol-butylene glycol copolymers.
  • the non-aqueous solvent may be used alone or in a mixture of two or more.
  • the liquid component (LC) may include a non-aqueous solvent and a base component (base) dissolved in the non-aqueous solvent.
  • the liquid component (LC) may also include a non-aqueous solvent and a base component and/or an acid component (acid) dissolved in the non-aqueous solvent.
  • polycarboxylic acids and monocarboxylic acids can be used as the acid component.
  • the polycarboxylic acids include aliphatic polycarboxylic acids (saturated polycarboxylic acids such as oxalic acid, malonic acid, succinic acid, glutaric acid, adipic acid, pimelic acid, suberic acid, azelaic acid, sebacic acid, 1,6-decanedicarboxylic acid, 5,6-decanedicarboxylic acid; unsaturated polycarboxylic acids such as maleic acid, fumaric acid, itaconic acid), aromatic polycarboxylic acids (phthalic acid, isophthalic acid, terephthalic acid, trimellitic acid, pyromellitic acid), and alicyclic polycarboxylic acids (cyclohexane-1,2-dicarboxylic acid, cyclohexene-1,2-dicarboxylic acid, etc.).
  • saturated polycarboxylic acids such as ox
  • Examples of the monocarboxylic acids include aliphatic monocarboxylic acids (1 to 30 carbon atoms) ([saturated monocarboxylic acids, such as formic acid, acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, caproic acid, enanthic acid, caprylic acid, pelargonic acid, lauric acid, myristic acid, stearic acid, behenic acid]; [unsaturated monocarboxylic acids, such as acrylic acid, methacrylic acid, oleic acid]), aromatic monocarboxylic acids (such as benzoic acid, cinnamic acid, naphthoic acid), and oxycarboxylic acids (such as salicylic acid, mandelic acid, resorcylic acid).
  • saturated monocarboxylic acids such as formic acid, acetic acid, propionic acid, butyric acid, isobutyric acid, valeric acid, caproic acid
  • maleic acid, phthalic acid, benzoic acid, pyromellitic acid, and resorcylic acid are thermally stable and are preferably used.
  • Inorganic acids may be used as the acid component.
  • inorganic acids include phosphoric acid, phosphorous acid, hypophosphorous acid, alkyl phosphate esters, boric acid, boric fluoride, tetrafluoroboric acid, hexafluorophosphoric acid, benzenesulfonic acid, and naphthalenesulfonic acid.
  • composite compounds of organic acids and inorganic acids may be used as the acid component. Examples of such composite compounds include borodiglycolic acid, borodioxalic acid, and borodisalicylic acid.
  • the base component may be a compound having an alkyl-substituted amidine group, such as an imidazole compound, a benzimidazole compound, or an alicyclic amidine compound (pyrimidine compound, imidazoline compound).
  • an imidazole compound such as an imidazole compound, a benzimidazole compound, or an alicyclic amidine compound (pyrimidine compound, imidazoline compound).
  • 1,8-diazabicyclo[5,4,0]undecene-7, 1,5-diazabicyclo[4,3,0]nonene-5 1,2-dimethylimidazolinium, 1,2,4-trimethylimidazoline, 1-methyl-2-ethyl-imidazoline, 1,4-dimethyl-2-ethylimidazoline, 1-methyl-2-heptyl imidazoline, 1-methyl-2-(3'heptyl)imidazoline, 1-methyl-2-dodecyl imidazoline, 1,2-di
  • the base component may be a quaternary salt of a compound having an alkyl-substituted amidine group.
  • base components include imidazole compounds, benzimidazole compounds, and alicyclic amidine compounds (pyrimidine compounds, imidazoline compounds) that are quaternized with an alkyl group or arylalkyl group having 1 to 11 carbon atoms.
  • a tertiary amine may be used as the base component.
  • tertiary amines include trialkylamines (trimethylamine, dimethylethylamine, methyldiethylamine, triethylamine, dimethyl-n-propylamine, dimethylisopropylamine, methylethyl-n-propylamine, methylethylisopropylamine, diethyl-n-propylamine, diethylisopropylamine, tri-n-propylamine, triisopropylamine, tri-n-butylamine, tri-tert-butylamine, etc.), and phenyl group-containing amines (dimethylphenylamine, methylethylphenylamine, diethylphenylamine, etc.).
  • trialkylamines are preferred in terms of increasing electrical conductivity, and it is more preferred to include at least one selected from the group consisting of trimethylamine, dimethylethylamine, methyldiethylamine, and triethylamine.
  • secondary amines such as dialkylamines, primary amines such as monoalkylamines, and ammonia may be used as the base component.
  • the liquid component (LC) may contain a salt of an acid component and a base component.
  • the salt may be an inorganic salt and/or an organic salt.
  • An organic salt is a salt in which at least one of the anion and the cation contains an organic substance. Examples of organic salts that may be used include trimethylamine maleate, triethylamine borodisalicylate, ethyldimethylamine phthalate, mono 1,2,3,4-tetramethylimidazolinium phthalate, and mono 1,3-dimethyl-2-ethylimidazolinium phthalate.
  • the pH of the liquid component (LC) may be less than 7.0 or less than 5.0, or may be greater than 1.0, or greater than 2.0.
  • the pH may be greater than 1.0 and less than 7.0 (e.g., in the range of 2.0 to 5.0).
  • the liquid component (LC) preferably contains a protic solvent. By using a protic solvent, it is possible to particularly swell the conductive polymer layer. In addition to the protic solvent, the liquid component (LC) may contain a solvent other than the protic solvent.
  • the protic solvent may include at least one selected from the group consisting of glycols, glycerin, polyglycerin, and sugar alcohols, or may be at least one of the above.
  • the protic solvent may be composed of only one type of compound, or may include multiple types of compounds.
  • the organic compound (C) and the liquid component (LC) may contain the same compound.
  • they may contain the same polyhydric alcohol, the same glycols (such as ethylene glycol), or the same sugar alcohol.
  • the liquid (L) may be a liquid containing the organic compound (C) and water. In this case, it is preferable to impregnate the laminate with the liquid (L) and then remove water from the laminate under conditions in which the organic compound (C) remains in the laminate.
  • the organic compound (C) may be at least one selected from the group consisting of mannitol, mannitol derivatives, xylitol, and xylitol derivatives.
  • the liquid (L) may contain at least one substance (hereinafter, sometimes referred to as "substance X") selected from the group consisting of sugar, sugar alcohol, epoxy resin, and polyvinyl alcohol.
  • substance X selected from the group consisting of sugar, sugar alcohol, epoxy resin, and polyvinyl alcohol.
  • the sugar alcohol may include at least one selected from the group consisting of mannitol, mannitol derivatives, xylitol and xylitol derivatives, or may be at least one of the above.
  • the substance X may be at least one selected from the group consisting of mannitol, mannitol derivatives, xylitol and xylitol derivatives. Mannitol, mannitol derivatives, xylitol and xylitol derivatives have the effect of an adhesive for adhering the conductive polymer layer and the cathode foil.
  • Examples of xylitol derivatives include compounds in which some of the hydroxyl groups of xylitol are esterified, compounds in which some of the hydroxyl groups of xylitol are etherified, and compounds in which some of the hydroxyl groups of xylitol are anionized to form a salt.
  • Examples of mannitol derivatives include compounds in which some of the hydroxyl groups of mannitol are esterified, compounds in which some of the hydroxyl groups of mannitol are etherified, and compounds in which some of the hydroxyl groups of mannitol are anionized to form a salt.
  • the organic solvent contained in the liquid (L) may contain at least one selected from the group consisting of ethylene glycol, diethylene glycol, triethylene glycol, and polyethylene glycol, or may be at least one of the above.
  • a preferred example of the liquid (L) is a liquid containing xylitol in at least one organic solvent selected from the group consisting of triethylene glycol and polyethylene glycol.
  • anode foil examples include metal foils containing at least one of valve metals such as titanium, tantalum, aluminum, and niobium, and may be metal foils of valve metals (e.g., aluminum foils).
  • the anode foil may contain the valve metal in the form of an alloy containing the valve metal or a compound containing the valve metal.
  • the thickness of the anode foil may be 15 ⁇ m or more and 300 ⁇ m or less.
  • the surface of the anode foil may be roughened by etching or the like.
  • a dielectric layer is formed on the surface of the anode foil.
  • the dielectric layer may be formed by subjecting the anode foil to a chemical conversion treatment.
  • the dielectric layer may contain an oxide of a valve metal (e.g., aluminum oxide).
  • the dielectric layer may be formed of any dielectric other than an oxide of a valve metal as long as it functions as a dielectric.
  • a conductive polymer layer does not need to be formed on the end surface of the anode foil.
  • a dielectric layer is formed on the end surface of the anode foil.
  • the cathode foil includes a metal foil (e.g., aluminum foil).
  • the metal constituting the metal foil may be a valve metal or an alloy containing a valve metal.
  • the surface of the metal foil may be roughened by etching or the like.
  • the thickness of the cathode foil may be 15 ⁇ m or more and 300 ⁇ m or less.
  • a conductive polymer layer may be formed on the surface of the cathode foil.
  • the conductive polymer layer may be formed by the same method as the methods described in the coating liquid application step and the liquid medium removal step.
  • the cathode foil may have an inorganic layer on its surface.
  • the cathode foil having an inorganic layer on its surface may be a commercially available product, or may be formed by forming an inorganic layer on the surface of a metal foil (cathode foil).
  • the inorganic layer may be formed by a known method.
  • the inorganic layer may be formed by a vacuum deposition method or the like.
  • the inorganic layer may be formed by applying a paste containing at least one selected from the group consisting of carbon (particularly a conductive carbon material), titanium, and nickel onto the metal foil (cathode foil) and then drying it.
  • the amount of the inorganic layer may be in the range of 50 mg/m 2 to 300 mg/m 2 (for example, in the range of 70 mg/m 2 to 200 mg/m 2 ).
  • Examples of carbon (particularly a conductive carbon material) contained in the inorganic layer include graphite, hard carbon, soft carbon, carbon black, and the like.
  • the inorganic layer may be a layer formed by depositing titanium or a layer formed by particles of titanium oxide.
  • the inorganic layer may be a carbon layer.
  • the carbon layer is a layer containing carbon, and may be a layer having a carbon content of 50 mass % or more. In this specification, the term "inorganic layer" may be replaced with the term "carbon layer".
  • the cathode foil may include a metal foil, an inorganic layer, and a titanium-containing layer disposed between the inorganic layer and the metal foil.
  • An example of the cathode foil has a laminated structure of inorganic layer/titanium-containing layer/metal foil (e.g., aluminum foil)/titanium-containing layer/inorganic layer.
  • the titanium-containing layer may contain at least one selected from the group consisting of titanium and titanium compounds. Examples of titanium compounds include titanium nitride, titanium oxide, titanium aluminum alloy, titanium carbonate, and the like.
  • the method of forming the titanium-containing layer is not limited, and the layer may be formed by a known method.
  • the titanium-containing layer may be formed by a physical vapor deposition method such as a vacuum deposition method or a sputtering method.
  • the deposition amount of the titanium-containing layer may be in the range of 200 mg/m 2 to 500 mg/m 2 (e.g., in the range of 250 mg/m 2 to 400 mg/m 2 ).
  • a porous sheet can be used for the separator.
  • the porous sheet include woven fabric, nonwoven fabric, and microporous membrane.
  • the thickness of the separator is not particularly limited and may be in the range of 10 to 300 ⁇ m.
  • the material of the separator include cellulose, polyethylene terephthalate, polybutylene terephthalate, polyphenylene sulfide, vinylon, nylon, aromatic polyamide, polyimide, polyamideimide, polyetherimide, rayon, glass, and the like.
  • the laminate and the liquid component (LC) are housed in an exterior body.
  • the exterior body includes a case and/or a sealing resin.
  • the sealing resin may include a thermosetting resin.
  • the thermosetting resin include an epoxy resin, a phenolic resin, a silicone resin, a melamine resin, a urea resin, an alkyd resin, a polyurethane, a polyimide, an unsaturated polyester, and the like.
  • the sealing resin may include a filler, a curing agent, a polymerization initiator, and/or a catalyst, and the like.
  • FIG. 1 is a cross-sectional view showing an example of an electrolytic capacitor 100 according to this embodiment.
  • FIG. 2 is a schematic diagram showing an exploded view of a portion of a capacitor element 10 included in the electrolytic capacitor 100.
  • the electrolytic capacitor 100 comprises a capacitor element 10, a bottomed case 101 that houses the capacitor element 10, a sealing member 102 that closes the opening of the bottomed case 101, a seat plate 103 that covers the sealing member 102, lead wires 104A, 104B that extend from the sealing member 102 and pass through the seat plate 103, and lead tabs 105A, 105B that connect the lead wires to the electrodes of the capacitor element 10.
  • the area near the open end of the bottomed case 101 is drawn inward, and the open end is curled so as to be crimped to the sealing member 102.
  • Capacitor element 10 is, for example, a wound body as shown in FIG. 1.
  • the wound body includes an anode foil connected to lead tab 105A, a cathode foil 12 connected to lead tab 105B, and a separator 13.
  • Capacitor element 10 (wound body) includes a conductive polymer layer (not shown).
  • the conductive polymer layer may include an organic compound (C).
  • Electrolytic capacitor 100 includes a liquid component (LC) (e.g., an electrolyte) impregnated in capacitor element 10.
  • LC liquid component
  • the capacitor element 10 is formed by winding a strip-shaped first laminate 11y having a first width W1 and a strip-shaped cathode foil 12 having a second width W2.
  • the first laminate 11y includes an anode foil, a separator bonded to the anode foil, and a conductive polymer layer.
  • the first laminate 11y and the cathode foil 12 are wound such that the separator 13 is disposed between the anode foil and the cathode foil 12.
  • the outermost periphery of the wound body is fixed by a stop tape 14. Note that FIG. 2 shows the wound body in a partially unfolded state before the outermost periphery is stopped.
  • An electrolytic capacitor may have at least one capacitor element, but may also have multiple capacitor elements.
  • the number of capacitor elements included in an electrolytic capacitor may be determined according to the application.
  • FIG. 3A An example of a method for forming the second laminate (capacitor element) is shown in the cross-sectional views of Figures 3A to 3C.
  • the anode foil 11a and the separator 13a are superimposed.
  • a dielectric layer (not shown) is formed on the surfaces (both sides) of the anode foil 11a.
  • the above-mentioned coating liquid application process and liquid medium removal process are performed to form the laminate sheet 11x shown in Figure 3B.
  • the laminate sheet 11x includes the anode foil 11a and the separator 13b in which a conductive polymer layer is formed in the voids.
  • the conductive polymer layer is integrally formed on the surface of the dielectric layer and in the voids of the separator.
  • the anode foil 11a and the separator 13b are bonded together.
  • the above-mentioned coating liquid application process and liquid medium removal process are performed on the surface opposite to the surface of the anode foil 11a to which the separator 13b is bonded, so that the anode foil 11a and the separator 13b are bonded together.
  • a laminate sheet 11x in which separators 13b are bonded to both sides of an anode foil 11a is cut to a first width W1 to form a first laminate 11y including an anode foil 11, a conductive polymer layer, and a separator 13 (13b).
  • a second laminate is obtained by laminating the first laminate 11y and a cathode foil 12 having a second width W2.
  • the first laminate 11y and the cathode foil 12 may be rolled up as shown in FIG. 2.
  • An electrolytic capacitor comprising a laminate and a liquid component impregnated in the laminate,
  • the laminate comprises: an anode foil having a dielectric layer on a surface thereof; A separator laminated on the anode foil; A cathode foil; a conductive polymer layer formed on a surface of the dielectric layer and in the voids of the separator; the anode foil and the separator are bonded together by the conductive polymer layer.
  • the cathode foil has an inorganic layer on a surface thereof,
  • a method for manufacturing an electrolytic capacitor comprising the steps of: A preparation step of preparing an anode foil having a dielectric layer on a surface thereof; a laminated sheet forming step of forming a laminated sheet including the anode foil, a separator bonded to the anode foil, and a conductive polymer layer; a first laminate formation step of cutting the laminate sheet to a first width to form a first laminate including the anode foil, the separator, and the conductive polymer layer; a second laminate formation step of forming a second laminate by laminating the first laminate and a cathode foil having a second width such that the separator is disposed between the anode foil and the cathode foil,
  • the laminate sheet forming step includes: a coating liquid applying step of applying a coating liquid containing a conductive polymer and a liquid medium onto a surface of the dielectric layer and into voids in the separator in a state in which the anode foil and the separator are superimposed;
  • the cathode foil has an inorganic layer on a surface thereof, The method for producing an electrolytic capacitor according to any one of Techniques 8 to 10, wherein the conductive polymer layer is in close contact with the inorganic layer.
  • Capacitor A1 An electrolytic capacitor (capacitor A1) was produced by the following method.
  • a nonwoven fabric (thickness 50 ⁇ m) was prepared as a separator.
  • the nonwoven fabric used was made of polyester fiber, aramid fiber, and cellulose.
  • a dispersion liquid (commercially available product) in which particles of polyethylenedioxythiophene (PEDOT) doped with polystyrene sulfonic acid (PSS) were dispersed in water was prepared.
  • PEDOT polyethylenedioxythiophene
  • PSS polystyrene sulfonic acid
  • a coating liquid was applied to the separator, thereby applying the coating liquid to the surface of the dielectric layer of the anode foil and into the gaps in the separator.
  • the anode foil and separator to which the coating liquid had been applied were heated at 125°C for 5 minutes to remove the liquid medium in the applied coating liquid. This heating formed a conductive polymer layer on the surface of the dielectric layer and in the gaps in the separator, and also bonded the anode foil and separator together.
  • separators were bonded to both sides of the anode foil. In this way, a laminated sheet was obtained.
  • an anode lead wire and a cathode lead wire were connected to the ends of each lead tab protruding from the wound body.
  • the resulting wound body was again subjected to chemical conversion treatment to form a dielectric layer on the end surface of the anode foil. In this way, a capacitor element was obtained.
  • Capacitor A1 Sealing of Capacitor Element
  • the capacitor element impregnated with the electrolytic solution was sealed to produce an electrolytic capacitor as shown in Fig. 1. Then, aging was performed for 90 minutes at 95°C while applying a voltage. In this manner, an electrolytic capacitor (capacitor A1) was produced.
  • Capacitor C1 An electrolytic capacitor (capacitor C1) was produced in the same manner and under the same conditions as those for producing capacitor A1, except that the method for forming the conductive polymer layer and the method for forming the wound body were different.
  • the conductive polymer layer formed on the dielectric layer on the surface of the anode foil was formed by applying the coating liquid used in capacitor A1 to the dielectric layer and then drying it.
  • the conductive polymer layer formed in the gaps of the separator was formed by applying the coating liquid used in capacitor A1 to the separator and then drying it. That is, in producing capacitor C1, the conductive polymer layer on the dielectric layer and the conductive polymer layer in the separator were formed separately, and the anode foil and the separator were not bonded together.
  • the wound body was formed by winding an anode foil with a conductive polymer layer formed thereon, a cathode foil with a conductive polymer layer formed thereon, and a separator, with the separator positioned between the anode foil and the cathode foil.
  • the sizes of these components were the same as those used in capacitor A1.
  • capacitor C1 was made using the same method and conditions as capacitor A1.
  • ESR equivalent series resistance
  • the schematic configuration of the measuring device 20 used to measure the peel strength is shown in FIG. 4.
  • the measuring device is preferably designed to perform tests conforming to JIS C0806-3:2014.
  • the measuring device 20 includes a feed sheet 21, feed rollers 22, and a recovery device 23.
  • the outer peripheral surface of the peeled anode foil 11 is fixed to the feed sheet 21 by a fixing jig 24.
  • the feed sheet 21 is fed in a first direction by the feed rollers 22.
  • the recovery device 23 recovers the cathode foil 12 and separator 13 from which the anode foil 11 has been peeled off while pulling them in a second direction opposite to the first direction.
  • the recovery device 23 has a winding roller that winds up the cathode foil 12 and separator 13.
  • the feed speed of the anode foil 11 by the feed rollers 22 and the winding speed of the cathode foil 12 and separator 13 by the recovery device 23 are controlled so that the position of the capacitor element 10 does not move during measurement.
  • the peeled-off portion of the anode foil 11 was fixed to a feed sheet, and the cathode foil 12 and separator 13 from which the anode foil 11 had been peeled off were set in the recovery device 23.
  • the measurement device used was an embossed tape high-speed peel strength tester (PTS-5000K) manufactured by EPI Co., Ltd.
  • the anode foil 11, cathode foil 12, and separator 13 were pulled in the measuring device 20 so that the angle between the direction in which the anode foil 11 fixed to the feed sheet 21 was pulled and the direction in which the cathode foil 12 and separator 13 were pulled by the recovery device 23 was approximately 175°.
  • the anode foil 11 and separator 13 were pulled for 60 seconds so that the anode foil 11 and separator 13 were continuously peeled off at a constant speed (160 mm/min).
  • the force pulling the cathode foil 12 at this time was measured at sampling intervals of 0.01 seconds.
  • the average value of the measured forces pulling the cathode foil 12 was taken as the peel strength.
  • Capacitor A1 is an electrolytic capacitor (E) according to the present disclosure manufactured by manufacturing method (M).
  • Capacitor C1 is a comparative example. As shown in Table 1, capacitor A1 had a high peel strength between the anode foil and the separator and a low ESR.
  • This disclosure can be used in electrolytic capacitors.

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Publication number Priority date Publication date Assignee Title
US20250095923A1 (en) * 2022-01-28 2025-03-20 Panasonic Intellectual Property Management Co., Ltd. Electrolytic capacitor and method for manufacturing electrolytic capacitor

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JP2008047783A (ja) * 2006-08-18 2008-02-28 Nichicon Corp 固体電解コンデンサおよび固体電解コンデンサの製造方法
WO2020158780A1 (ja) * 2019-01-31 2020-08-06 パナソニックＩｐマネジメント株式会社 電解コンデンサおよびその製造方法
JP2022035309A (ja) * 2020-08-20 2022-03-04 ニッポン高度紙工業株式会社 アルミニウム電解コンデンサ用セパレータ及びアルミニウム電解コンデンサ
JP2023034887A (ja) * 2021-08-31 2023-03-13 株式会社東芝 電解コンデンサの製造方法、電解コンデンサ及び電解コンデンサの製造装置

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JP2008047783A (ja) * 2006-08-18 2008-02-28 Nichicon Corp 固体電解コンデンサおよび固体電解コンデンサの製造方法
WO2020158780A1 (ja) * 2019-01-31 2020-08-06 パナソニックＩｐマネジメント株式会社 電解コンデンサおよびその製造方法
JP2022035309A (ja) * 2020-08-20 2022-03-04 ニッポン高度紙工業株式会社 アルミニウム電解コンデンサ用セパレータ及びアルミニウム電解コンデンサ
JP2023034887A (ja) * 2021-08-31 2023-03-13 株式会社東芝 電解コンデンサの製造方法、電解コンデンサ及び電解コンデンサの製造装置

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US20250095923A1 (en) * 2022-01-28 2025-03-20 Panasonic Intellectual Property Management Co., Ltd. Electrolytic capacitor and method for manufacturing electrolytic capacitor

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