WO2022168446A1 - Pâte contenant des particules inorganiques, film contenant des particules inorganiques et stratifié - Google Patents

Pâte contenant des particules inorganiques, film contenant des particules inorganiques et stratifié Download PDF

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Publication number
WO2022168446A1
WO2022168446A1 PCT/JP2021/045897 JP2021045897W WO2022168446A1 WO 2022168446 A1 WO2022168446 A1 WO 2022168446A1 JP 2021045897 W JP2021045897 W JP 2021045897W WO 2022168446 A1 WO2022168446 A1 WO 2022168446A1
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inorganic particle
chains
particles
inorganic
branched
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PCT/JP2021/045897
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English (en)
Japanese (ja)
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準 塩田
友樹 吾郷
信之 木南
明大 鶴
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株式会社村田製作所
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Priority to CN202180092230.3A priority Critical patent/CN116745872A/zh
Priority to JP2022579372A priority patent/JP7544157B2/ja
Priority to KR1020237025908A priority patent/KR20230128323A/ko
Publication of WO2022168446A1 publication Critical patent/WO2022168446A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/20—Compounding polymers with additives, e.g. colouring
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/01—Use of inorganic substances as compounding ingredients characterized by their specific function
    • C08K3/013—Fillers, pigments or reinforcing additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K7/00—Use of ingredients characterised by shape
    • C08K7/16—Solid spheres
    • C08K7/18—Solid spheres inorganic
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
    • C08L1/08—Cellulose derivatives
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
    • H01B5/16—Non-insulated conductors or conductive bodies characterised by their form comprising conductive material in insulating or poorly conductive material, e.g. conductive rubber
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
    • H01G4/00—Fixed capacitors; Processes of their manufacture
    • H01G4/30—Stacked capacitors

Definitions

  • the present invention relates to an inorganic particle-containing paste, an inorganic particle-containing film that can be formed using the inorganic particle-containing paste, and a laminate containing the inorganic particle-containing film.
  • Films containing various inorganic particles are used in various applications.
  • a method for forming such a film a method using a paste containing inorganic particles is known.
  • a film containing inorganic particles can be formed by forming a film from a paste containing inorganic particles by a method such as coating or printing, and curing or drying the formed film.
  • Laminates used to manufacture laminated ceramic electronic components such as laminated ceramic capacitors are known as typical applications of inorganic particle-containing films.
  • green sheets containing ceramic powder and precursor films of internal electrode layers containing metal particles are usually laminated.
  • a conductive paste for forming a conductive sheet that provides internal electrode layers by firing a conductive paste containing metal particles and ethyl cellulose as a binder resin has been proposed (see Patent Document 1. ).
  • Ethyl cellulose is excellent in solubility in organic solvents and decomposability during firing, and provides a conductive paste with good printing properties.
  • a laminate containing a green sheet and a conductive sheet that provides an internal electrode layer by being fired is cut into a predetermined size by a method such as pressure cutting and divided. In some cases, the divided laminate is fired.
  • a laminate containing a conductive sheet formed using a conductive paste containing ethyl cellulose as a binder resin when cutting the laminate in a direction perpendicular or substantially perpendicular to the plane direction, there is a problem that delamination easily occurs due to delamination or cohesive failure due to the action of shear force or the like.
  • the present invention has been made in view of the above problems, and when cutting a laminate obtained by laminating an inorganic particle-containing film into small pieces, the other layers due to the action of shear force etc.
  • An inorganic particle-containing paste that provides an inorganic particle-containing film that is unlikely to cause intra-layer peeling due to delamination or cohesive failure, an inorganic particle-containing film that can be formed using the inorganic particle-containing paste, and the above inorganic particle-containing film. It is an object of the present invention to provide a laminate comprising:
  • the present inventors found that in an inorganic particle-containing paste containing a binder resin, inorganic particles, and an organic solvent, a molecule having a main chain made of a cellulose polymer and a branch chain made of an aliphatic polycarbonate or an aliphatic polyester
  • a combination of a branched polymer having a chain and a dispersant having at least one selected from the group consisting of a polyether chain, a polyester chain, and a polycarbonate chain I have perfected my invention. More specifically, the present invention provides the following (1) to (3).
  • (1) comprising a branched polymer, inorganic particles, a dispersant, and an organic solvent;
  • the molecular chain of the branched polymer has a main chain made of a cellulose polymer and a branch chain made of an aliphatic polycarbonate or an aliphatic polyester,
  • the branched chain may be linear or branched, branch chains may be attached to two or more of said main chains to bridge two or more of said main chains;
  • An inorganic particle-containing paste, wherein the dispersant has at least one selected from the group consisting of polyether chains, polyester chains, and polycarbonate chains.
  • the molecular chain of the branched polymer has a main chain made of a cellulose polymer and a branch chain made of an aliphatic polycarbonate or an aliphatic polyester,
  • the branched chain may be linear or branched, branch chains may be attached to two or more of said main chains to bridge two or more of said main chains;
  • An inorganic particle-containing film, wherein the dispersant has at least one selected from the group consisting of polyether chains, polyester chains, and polycarbonate chains.
  • an inorganic particle-containing paste that provides an inorganic particle-containing film that is unlikely to cause delamination from other layers due to the action of shear force or the like when laminated, and a paste that is formed using the inorganic particle-containing paste. It is possible to provide the obtained inorganic particle-containing film and the laminate containing the inorganic particle-containing film described above.
  • the inorganic particle-containing paste contains a branched polymer, inorganic particles, a dispersant, and an organic solvent.
  • a molecular chain of a branched polymer has a main chain and a branch chain.
  • the backbone consists of a cellulosic polymer.
  • the branches consist of aliphatic polycarbonates or aliphatic polyesters. Branches may be straight or branched. A branch may be attached to two or more backbones to bridge two or more backbones.
  • the dispersant has at least one selected from the group consisting of polyether chains, polyester chains and polycarbonate chains.
  • the inorganic particle-containing paste containing inorganic particles and an organic solvent
  • the inorganic particle-containing paste can contain inorganic particles Contains inorganic particles that do not easily cause delamination from other layers due to the action of shear force, etc., or intra-layer delamination due to cohesive failure when the laminate obtained by laminating the containing film is cut into small pieces. Give a membrane.
  • a branched polymer has a main chain and branch chains in its molecular chain.
  • the backbone consists of a cellulosic polymer.
  • the branches consist of aliphatic polycarbonates or aliphatic polyesters. Branches may be straight or branched.
  • a branch may be attached to two or more backbones to bridge two or more backbones.
  • the graft ratio which is the ratio of the mass of the branch chains to the mass of the main chain, is not particularly limited as long as the desired effects are not impaired.
  • the graft rate is preferably 10% by mass or more and 400% by mass or less, more preferably 50% by mass or more and 250% by mass or less, from the viewpoint of easily suppressing the occurrence of .
  • the graft rate can be determined by nuclear magnetic resonance spectroscopy (NMR analysis).
  • the mass average molecular weight of the branched polymer is not particularly limited.
  • the weight average molecular weight of the branched polymer is, for example, preferably 50,000 or more and 1,000,000 or less, more preferably 100,000 or more and 600,000 or less.
  • mechanical properties such as strength, elongation and toughness and moldability of the branched polymer are good.
  • Branched polymers have a backbone consisting of a cellulosic polymer.
  • the type of cellulosic polymer is not particularly limited as long as the main chain of the cellulosic polymer has functional groups to which branch chains can be bonded.
  • Preferred specific examples of cellulosic polymers include cellulose; alkylcelluloses such as methylcellulose, ethylcellulose, n-propylcellulose, isopropylcellulose, n-butylcellulose, tert-butylcellulose, and n-hexylcellulose; hydroxymethylcellulose, hydroxyethylcellulose.
  • hydroxyalkylcelluloses such as, hydroxypropylcellulose, and hydroxybutylcellulose
  • cellulose esters such as cellulose acetate, cellulose diacetate, cellulose triacetate, cellulose acetate propionate, and cellulose acetate butyrate
  • carboxymethylcellulose, carboxyethylcellulose, and carboxypropyl carboxyalkyl cellulose such as cellulose
  • cellulose derivatives such as nitrocellulose, aldehyde cellulose, dialdehyde cellulose, and sulfonated cellulose
  • a branched polymer may comprise two or more branched polymer molecules having different types of cellulosic polymer backbones.
  • Cellulose-based polymers are alkyl celluloses, alkyl celluloses, At least one selected from the group consisting of hydroxyalkyl cellulose and cellulose ester is preferred. Among the above preferred cellulosic polymers, at least one selected from the group consisting of methyl cellulose, ethyl cellulose, cellulose acetate butyrate, cellulose acetate propionate, and cellulose acetate is preferred.
  • the mass average molecular weight of the cellulose-based polymer is not particularly limited.
  • the mass average molecular weight of the cellulose-based polymer is, for example, preferably 5,000 or more, more preferably 10,000 or more, and particularly preferably 100,000 or more.
  • the mass average molecular weight of the cellulose-based polymer is preferably 1,000,000 or less, more preferably 750,000 or less, even more preferably 500,000 or less. More specifically, the molecular weight of the cellulose polymer is preferably 5,000 or more and 1,000,000 or less, more preferably 10,000 or more and 750,000 or less, and more preferably 10,000 or more and 750,000 or less.
  • the degree of substitution of the cellulosic polymer is not particularly limited as long as the desired effects are not impaired.
  • the degree of substitution of the cellulosic polymer is preferably 2 or more and 3 or less, typically 2.5.
  • the degree of substitution of a cellulosic polymer is the total number of hydroxyl groups substituted by groups other than branched chains among all hydroxyl groups in the constituent units of the cellulosic polymer.
  • branches have branches attached to a backbone composed of a cellulosic polymer.
  • the branches consist of aliphatic polycarbonates or aliphatic polyesters. Branches may be straight or branched. Typically, branches are attached to only one main chain. A branch may be attached to two or more backbones to bridge two or more backbones.
  • the aliphatic polycarbonate or aliphatic polyester that constitutes the branched chain is not particularly limited, as long as the branched chain can be formed in a state of being bound to the main chain or can be bound to the main chain.
  • Typical examples of branched chain aliphatic polycarbonates or aliphatic polyesters are given below in the description of methods for producing branched polymers.
  • the method for producing the branched polymer is not particularly limited.
  • a graft polymerization method is typically employed.
  • the graft polymerization method can be appropriately selected from various known methods depending on the type of branched chain.
  • a ring-opening polymerization method for example, a ring-opening polymerization method can be adopted.
  • a cyclic carbonate compound or a cyclic ester compound such as a lactone By subjecting a cyclic carbonate compound or a cyclic ester compound such as a lactone to ring-opening polymerization in the presence of a cellulose-based polymer, an aliphatic polycarbonate or an aliphatic polyester is formed as a graft chain on the molecular chain of the cellulose-based polymer. Generate.
  • propylene carbonate as a cyclic compound gives a branched chain made of polypropylene carbonate.
  • Butylene carbonate as a cyclic compound gives branches consisting of polybutylene carbonate.
  • Cyclohexene carbonate as a cyclic compound gives a branched chain consisting of polycyclohexene carbonate.
  • Trimethylene carbonate as a cyclic compound gives branches consisting of polytrimethylene carbonate.
  • 2,2-dimethyltrimethylene carbonate as a cyclic compound gives branches consisting of poly(2,2-dimethyltrimethylene carbonate).
  • ⁇ -caprolactone as a cyclic compound gives a branched chain composed of polycaprolactone, which is an aliphatic polyester.
  • L-lactide as a cyclic compound gives L-form polylactic acid, which is an aliphatic polyester, as a branched chain.
  • D-lactide as a cyclic compound gives D-form polylactic acid, which is an aliphatic polyester, as a branched chain.
  • Meso-lactide as a cyclic compound gives a syndiotactic polylactic acid, which is an aliphatic polyester, as a branched chain.
  • ⁇ -Propiolactone as a cyclic compound gives D-form poly(3-hydroxypropionic acid), which is an aliphatic polyester, as branched chains.
  • ⁇ -butyrolactone as a cyclic compound gives the aliphatic polyester poly(3-hydroxybutyric acid) as branched chains.
  • ⁇ -Butyrolactone as the cyclic compound gives the aliphatic polyester poly(4-hydroxybutyric acid) as branched chains.
  • ⁇ -valerolactone as a cyclic compound gives the aliphatic polyester poly(3-hydroxyvaleric acid) as branched chains.
  • P-dioxanone as a cyclic compound gives poly(p-dioxanone), an aliphatic polyester, as branched chains.
  • Ring-opening polymerization is typically carried out in the presence of a catalyst.
  • catalysts that can be used for ring-opening polymerization include alkali metals such as sodium and potassium; sodium hydroxide, potassium hydroxide, triethylaluminum, aluminum triisopropoxide, n-butyllithium, titanium tetraisopropoxy metal-containing catalysts such as sodium chloride, titanium tetrachloride, zirconium tetraisopropoxide, tin tetrachloride, sodium stannate, tin octoate, and diethylzinc dibutyltin dilaurate; pyridine, 4-N,N-dimethylaminopyridine, 1,5 ,7-triazabicyclo[4.4.0]dec-5-ene (TBD), 1,8-diazabicyclo[5.4.0]undec-7-ene (DBT) and other basic organic compounds; , acetic acid, methane
  • promoters include N-cyclohexyl-N'-phenylthiourea, N,N'-bis[3,5-bis(trifluoromethyl)phenyl]thiourea, N-[3,5-bis(tri fluoromethyl)phenyl]-N'-cyclohexylthiourea, (-)-sparteine and the like.
  • the amount of the catalyst that can be used in the ring-opening polymerization is appropriately determined in consideration of the amount of the catalyst used in conventionally known ring-opening polymerization reactions.
  • the amount of the catalyst used is preferably 0.001 mol or more, more preferably 0.005 mol or more, per 1 mol of the cyclic compound.
  • the amount of the catalyst used is preferably 0.2 mol or less, more preferably 0.1 mol or less, per 1 mol of the cyclic compound. More specifically, the amount of the catalyst used is preferably 0.001 mol or more and 0.2 mol or less, more preferably 0.005 mol or more and 0.1 mol or less, relative to 1 mol of the cyclic compound.
  • the amount of promoter used is the same as the amount of catalyst used.
  • Ring-opening polymerization is preferably carried out in the presence of a solvent.
  • the type of solvent is not particularly limited as long as it does not inhibit the ring-opening polymerization reaction.
  • Suitable specific examples of solvents include aliphatic hydrocarbon solvents such as pentane, hexane, octane, decane, and cyclohexane; aromatic hydrocarbon solvents such as benzene, toluene, and xylene; Halogenated hydrocarbon solvents such as dichloroethane, 1,2-dichloroethane, chlorobenzene, and bromobenzene; ethylene glycol dimethyl ether (monoglyme), diethylene glycol dimethyl ether (diglyme), triethylene glycol dimethyl ether (triglyme), tetrahydrofuran, 2-methyltetrahydrofuran, 1 Ether solvents such as ,4-dioxane, 1,3-dioxolane, and ani
  • the amount of solvent used is not particularly limited as long as the ring-opening polymerization reaction proceeds well.
  • the amount of the solvent used is preferably 100 parts by mass or more and 1000 parts by mass or less with respect to 100 parts by mass of the cyclic compound, for example.
  • a cellulosic resin, a cyclic compound, a catalyst, and optionally a cocatalyst and/or solvent are charged into a reaction vessel, and the mixture in the reaction vessel is stirred to carry out ring-opening polymerization. is done.
  • a preferred reaction temperature for ring-opening polymerization varies depending on the cyclic compound, the type of catalyst, the amount of catalyst used, and the like.
  • the reaction temperature for ring-opening polymerization is preferably ⁇ 80° C. or higher, more preferably ⁇ 40° C. or higher, and even more preferably 0° C. or higher.
  • the reaction temperature of the ring-opening polymerization is preferably 250° C. or lower, more preferably 200° C. or lower, and even more preferably 150° C. or lower. More specifically, the reaction temperature is preferably ⁇ 80° C. or higher and 250° C. or lower, more preferably ⁇ 40° C. or higher and 200° C. or lower, even more preferably 0° C. or higher and 150° C. or lower.
  • reaction time for ring-opening polymerization varies depending on the type of cyclic compound, the type of catalyst, the amount of catalyst used, etc. Typically, the reaction time for ring-opening polymerization is preferably 1 hour or more and 40 hours or less.
  • the amount of the cyclic compound used in the ring-opening polymerization is appropriately determined in consideration of the above-mentioned graft ratio.
  • Another preferred method for producing a branched polymer is a method of copolymerizing a cyclic ether and carbon dioxide in the presence of a cellulosic resin. Such a copolymerization reaction produces branched chains of aliphatic polycarbonate.
  • the cellulosic resin is as described above.
  • cyclic ethers the corresponding cyclic ethers of the branched aliphatic polycarbonates are suitably selected.
  • Preferred examples of cyclic ethers include ethylene oxide, propylene oxide, trimethylene oxide (oxetane), 3,3-dimethyltrimethylene oxide (3,3-dimethyloxetane), 1,2-butylene oxide and 2,3-butylene oxide.
  • cyclic ethers there are branched polymers that have excellent polymerization reactivity and that easily suppress the occurrence of delamination due to external force when inorganic particle-containing films are laminated using inorganic particle-containing pastes.
  • Ethylene oxide, propylene oxide, trimethylene oxide, and 1,2-butylene oxide are preferred, and ethylene oxide, propylene oxide, and trimethylene oxide are more preferred, as they are available.
  • An example of an aliphatic polycarbonate produced by copolymerizing a cyclic ether and carbon dioxide is shown below.
  • Ethylene oxide gives polyethylene carbonate.
  • Propylene oxide gives polypropylene carbonate.
  • Trimethylene oxide gives polytrimethylene carbonate.
  • the copolymerization of cyclic ether and carbon dioxide is carried out in the presence of a metal catalyst.
  • metal catalysts include zinc-based catalysts, aluminum-based catalysts, chromium-based catalysts, cobalt-based catalysts, and the like. Among these, zinc-based catalysts and cobalt-based catalysts are preferred because of their high polymerization activity.
  • zinc-based catalysts include diethylzinc-water-based catalysts, diethylzinc-pyrogallol-based catalysts, bis((2,6-diphenyl)phenoxy)zinc, N-(2,6-diisopropylphenyl)- 3,5-di-tert-butyl salicylaldoiminato zinc, 2-((2,6-diisopropylphenyl)amido)-4-((2,6-diisopropylphenyl)imino)-2-pentenoic acid acetate, adipine zinc acid, zinc glutarate, and the like.
  • cobalt-based catalysts include cobalt acetate-acetic acid-based catalysts, N,N'-bis(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt acetate, N, N'-bis-(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt pentafluorobenzoate, N,N'-bis-(3,5-di-tert-butylsalicylidene) den)-1,2-cyclohexanediaminocobalt chloride, N,N'-bis-(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt nitrate, N,N'-bis -(3,5-di-tert-butylsalicylidene)-1,2-cyclohexanediaminocobalt nit
  • a cobalt-based catalyst is preferably used together with a co-catalyst.
  • promoters include pyridine, 4-N,N-dimethylaminopyridine, N-methylimidazole, tetrabutylammonium chloride, tetrabutylammonium acetate, triphenylphosphine, bis(triphenylphosphoranylidene)ammonium chloride, and bis(triphenylphosphoranylidene)ammonium acetate.
  • the amount of the catalyst that can be used in the copolymerization of the cyclic ether and carbon dioxide is appropriately determined in consideration of the amounts of conventionally known catalysts used for such copolymerization reactions.
  • the amount of the catalyst used is preferably 0.001 mol or more, more preferably 0.005 mol or more, per 1 mol of the cyclic ether.
  • the amount of the catalyst used is preferably 0.2 mol or less, more preferably 0.1 mol or less, per 1 mol of the cyclic ether. More specifically, the amount of the catalyst to be used is preferably 0.001 mol or more and 0.2 mol or less, more preferably 0.005 mol or more and 0.1 mol or less, relative to 1 mol of the cyclic ether.
  • the amount of promoter used is the same as the amount of catalyst used.
  • Copolymerization of the cyclic ether and carbon dioxide is preferably carried out in the presence of a solvent.
  • the type of solvent is not particularly limited as long as it does not inhibit the copolymerization reaction.
  • Suitable specific examples of solvents include aliphatic hydrocarbon solvents such as pentane, hexane, octane, decane, and cyclohexane; aromatic hydrocarbon solvents such as benzene, toluene, and xylene; Halogenated hydrocarbon solvents such as dichloroethane, 1,2-dichloroethane, chlorobenzene, and bromobenzene; ethylene glycol dimethyl ether (monoglyme), diethylene glycol dimethyl ether (diglyme), triethylene glycol dimethyl ether (triglyme), tetrahydrofuran, 2-methyltetrahydrofuran, 1 Ether solvents such as ,4-dioxane, 1,3-diox
  • the amount of solvent used is not particularly limited as long as the copolymerization reaction proceeds well.
  • the amount of the solvent used is preferably 100 parts by mass or more and 1000 parts by mass or less with respect to 100 parts by mass of the cyclic ether, for example.
  • a cellulose resin, a cyclic ether, a catalyst, and optionally a co-catalyst and/or solvent are charged into a reaction vessel, and then carbon dioxide is injected into the reaction vessel, followed by Copolymerization is carried out by stirring the mixture inside.
  • the amount of the cyclic ether and carbon dioxide to be used in the copolymerization is appropriately determined in consideration of the above-mentioned graft ratio.
  • the pressure of carbon dioxide in the reaction vessel during copolymerization is preferably 0.1 MPa or more, more preferably 0.2 MPa or more, more preferably 0.5 MPa as a gauge pressure at the reaction temperature, from the viewpoint of good progress of the reaction. The above is more preferable.
  • the pressure of carbon dioxide in the reaction vessel is preferably 20 MPa or less, more preferably 10 MPa or less, and 5 MPa or less from the viewpoint of work safety and that there is no need to use an expensive pressure-resistant container with high pressure resistance. It can be.
  • the gauge pressure of carbon dioxide in the reaction solution is preferably 0.1 MPa or more and 20 MPa or less, more preferably 0.2 MPa or more and 10 MPa or less, and even more preferably 0.5 MPa or more and 5 MPa or less.
  • the copolymerization reaction may be carried out under supercritical conditions of carbon dioxide.
  • a preferred reaction temperature for copolymerization varies depending on the type of cyclic ether, the type of catalyst, the amount of catalyst used, and the like.
  • the reaction temperature for copolymerization is preferably 0° C. or higher, more preferably 20° C. or higher, and even more preferably 30° C. or higher.
  • the reaction temperature for copolymerization is preferably 100° C. or lower, more preferably 80° C. or lower, and even more preferably 60° C. or lower.
  • the reaction temperature for copolymerization is preferably 0° C. or higher and 100° C. or lower, more preferably 20° C. or higher and 80° C. or lower, and even more preferably 30° C. or higher and 60° C. or lower.
  • the reaction time for copolymerization varies depending on the type of cyclic ether, the type of catalyst, the amount of catalyst used, etc.
  • the reaction time for ring-opening polymerization is preferably 1 hour or more and 40 hours or less.
  • the amount of the cyclic compound used in the ring-opening polymerization is appropriately determined in consideration of the above-mentioned graft ratio.
  • the branch chain is made of an aliphatic polyester obtained by polycondensation of an aliphatic dicarboxylic acid and a glycol such as polyethylene succinate, polyethylene adipate, polybutylene succinate, polybutylene adipate, etc.
  • the fatty acid A branched polymer can also be produced by copolycondensation of an aliphatic dicarboxylic acid and glycols according to the structure of the family polyester according to a conventional method.
  • the amount of the branched polymer used in the inorganic particle-containing paste is not particularly limited as long as the desired effect is not impaired.
  • the ratio of the volume of the branched polymer to the sum of the volume of the branched polymer and the volume of the inorganic particles is preferably 17% by volume or more and 29% by volume or less, and is 19% by volume or more and 27% by volume or less. is more preferred.
  • the inorganic particle-containing paste contains inorganic particles.
  • inorganic particles inorganic particles conventionally added to various resin compositions can be used without particular limitation. Ceramic particles and/or metal particles are typically preferred as inorganic particles.
  • a suitable example of the inorganic particle-containing film formed using the inorganic particle-containing paste is a conductive sheet containing metal particles and providing an internal electrode layer, which constitutes a laminate useful as a precursor of a laminated ceramic electronic component. and green sheets containing ceramic particles.
  • Ceramic particles are used as inorganic particles when inorganic particle-containing pastes are used to form green sheets that provide dielectric layers in multilayer ceramic electronic components.
  • inorganic particles may comprise a combination of metal particles and ceramic particles.
  • the constituent material of the ceramic particles preferably contains at least one selected from the group consisting of Ba, Ti, Sr, Ca and Zr.
  • Preferred specific examples of ceramic particles include barium titanate particles, calcium titanate particles, strontium titanate particles, lead zirconate titanate particles, and the like.
  • the ceramic particles one type may be used alone, or two or more types may be used in combination.
  • ceramic particles containing barium titanate particles as a main component and a component containing Ca, Zr, or Sr as an auxiliary component may be used.
  • the particle size of the ceramic particles is not particularly limited as long as the desired effect is not impaired.
  • the average particle size of the ceramic particles is preferably 3 nm or more and 500 nm or less as an average particle size according to the BET conversion method.
  • metal particles are preferred as the inorganic particles. At least one selected from the group consisting of Ni, Cu, Ag, and Au is preferable as the metal constituting the metal particles.
  • the average particle size of the metal particles is not particularly limited as long as the desired effects are not impaired.
  • the average particle diameter of the metal particles is preferably 3000 nm or less, more preferably 30 nm or more and 1000 nm or less as an SEM diameter.
  • the metal particles may contain two or more kinds of metal particles.
  • the metal particles may be particles of an alloy containing two or more metals.
  • the mass of the ceramic particles is preferably 4% by mass or more and 25% by mass or less with respect to the mass of the metal particles.
  • the inorganic particle-containing paste contains a dispersant.
  • the dispersant has at least one selected from the group consisting of polyether chains, polyester chains and polycarbonate chains. Having a polyether chain, a polyester chain, or a polycarbonate chain makes the dispersant more compatible with branched polymers having branches made of aliphatic polycarbonates or aliphatic polyesters.
  • Polyester chains and polycarbonate chains include polyester chains and polycarbonate chains described as branches of branched polymers.
  • a polyoxyalkylene chain is preferred as the polyether chain.
  • Preferred examples of polyoxyalkylene chains include polyoxyethylene chains and polyoxypropylene chains.
  • the dispersant preferably has a hydrophobic group in terms of the dispersing effect.
  • Preferred examples of the hydrophobic group include hydrocarbon groups and fluorinated hydrocarbon groups, with aliphatic hydrocarbon groups and aliphatic fluorinated hydrocarbon groups being more preferred.
  • the dispersant preferably has an adsorptive group such as a carboxyl group, an amino group, a phosphoric acid group, or a sulfonic acid group that can bond to the surface of the inorganic particles in terms of the dispersing effect.
  • an adsorptive group such as a carboxyl group, an amino group, a phosphoric acid group, or a sulfonic acid group that can bond to the surface of the inorganic particles in terms of the dispersing effect.
  • the molecular weight of the dispersant is not particularly limited as long as the desired effects are not impaired.
  • the dispersant may be a so-called low-molecular-weight compound or a polymer-type dispersant.
  • a polymer-type dispersant is preferable as the dispersant in terms of ease of molecular design to give the dispersant the above-described various functional groups.
  • Polymer-type dispersants include, for example, (meth)acrylic monomers having hydrophobic chains such as hydrocarbon chains, and (meth)acrylic monomers having hydrophilic chains such as polyether chains, polyester chains, and polycarbonate chains.
  • a (meth)acrylic resin having a comb structure copolymerized with a monomer can be preferably used.
  • Comb-structured (meth)acrylic resins in which the above hydrophobic chains and hydrophilic chains are introduced as side chains into known (meth)acrylic resins are also preferably used as polymer-type dispersants.
  • the amount of the dispersant to be used is preferably 0.5 mg/m 2 to 5 mg/m 2 , more preferably 1.0 mg/m 2 to 2.5 mg/m 2 with respect to the surface area of the particles to be dispersed.
  • the inorganic particle-containing paste may contain components other than the above components as long as the desired effects are not impaired.
  • Other components include, for example, at least one additive selected from the group consisting of plasticizers and antistatic agents.
  • the amount of other ingredients to be used is not particularly limited as long as the desired effects are not impaired.
  • the amount of other components to be used is appropriately determined in consideration of the amounts that can be normally used according to the types of the above additives.
  • the inorganic particle-containing paste contains an organic solvent.
  • organic solvents include alkanols such as isopropanol; hydrocarbon-based solvents such as toluene, xylene, and isophorone; terpineol-based solvents such as terpineol and dihydroterpineol; Ester solvents such as pentyl, n-hexyl acetate, n-heptyl acetate, n-octyl acetate, terpineol acetate, and dihydroterpineol acetate; ethylene glycol monomethyl ether, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, methyl carbitol, Glycol ether solvents such as ethyl carbitol, butyl carbitol, propylene glycol monomethyl ether, ethylene glycol dimethyl ether, and diethylene glycol di
  • ethyl acetate, n-butyl acetate, n-pentyl acetate, n-hexyl acetate, n-heptyl acetate, and n-acetate have good affinity for branched polymers and dispersants.
  • Ester solvents such as octyl, terpineol acetate, and dihydroterpineol acetate
  • glycol ester solvents such as ethylene glycol monomethyl ether acetate, diethylene glycol monomethyl ether acetate, propylene glycol monomethyl ether acetate, and dipropylene glycol monomethyl ether acetate are preferred.
  • the amount of organic solvent used is not particularly limited as long as the desired effect is not impaired.
  • the amount of the organic solvent used is preferably 60% by volume or more and 97% by volume or less, more preferably 80% by volume or more and 94% by volume or less, relative to the total volume of the inorganic particle-containing paste.
  • the inorganic particle-containing film contains a branched polymer, inorganic particles, and a dispersant.
  • the branched polymer, inorganic particles, and dispersant are all the same as those described above for the inorganic particle-containing paste.
  • the inorganic particle-containing film can be formed by forming the inorganic particle-containing paste into a film, and then removing at least part of the organic solvent from the inorganic particle-containing paste film.
  • a method for removing the organic solvent is not particularly limited.
  • the organic solvent is removed by a method such as heating or exposure to a reduced pressure atmosphere.
  • the inorganic particle-containing film is preferably, for example, a green sheet in which inorganic particles contain ceramic particles and which, when fired, provides a dielectric layer in a multilayer ceramic electronic component.
  • a green sheet can be formed, for example, by a known method such as a die coater sheet method or a doctor blade method.
  • the thickness of the green sheet is preferably 4 ⁇ m or less, more preferably 3 ⁇ m or less.
  • the inorganic particle-containing film it is also preferable to use a conductive sheet containing inorganic particles containing metal particles and providing an internal electrode layer in a multilayer ceramic electronic component by firing.
  • the method of forming the conductive sheet is not particularly limited.
  • the conductive sheet is formed by printing an inorganic particle-containing paste on the above green sheet.
  • a printing method for example, a gravure printing method, a screen printing method, or the like can be applied.
  • the film thickness of the conductive sheet is preferably 1.5 ⁇ m or less, for example.
  • the laminate includes at least one layer made of the inorganic particle-containing film described above.
  • a green sheet that provides a dielectric layer by firing and a conductive sheet that provides an internal electrode layer by firing are stacked, Such laminates, in which the green sheet is the inorganic particle-containing film described above or the conductive sheet is the inorganic particle-containing film described above, are suitably used in the production of multilayer ceramic electronic components. After firing the laminate, the fired laminate is subjected to various known processes for manufacturing a multilayer ceramic electronic component, thereby obtaining a multilayer ceramic electronic component. Examples of laminated ceramic electronic components include laminated ceramic capacitors, inductors, piezoelectric elements, and thermistors.
  • Example 1 A conductive paste containing Ni particles as inorganic particles was produced. Ni particles with an average SEM diameter of 200 nm and barium titanate particles with a BET diameter of 20 nm were used as inorganic particles for the preparation of the conductive paste.
  • the branched polymer a resin having a main chain made of ethyl cellulose and a branch chain made of polypropylene carbonate, which is an aliphatic polycarbonate, was used.
  • the dispersant a polymer dispersant having a carboxy group as an adsorptive functional group, a chain aliphatic hydrocarbon group as a hydrophobic group, and a polyoxyethylene group (polyether chain) was used. Dihydroterpineol acetate, which is an ester solvent, was used as the organic solvent.
  • (Dielectric paste preparation) 7.2 parts by mass of polypropylene carbonate, which is an aliphatic polycarbonate, was dissolved in 26 parts by mass of n-butyl acetate and 26 parts by mass of dimethyl carbonate.
  • Polypropylene carbonate has a carboxylic acid-modified site in the repeating structure. The proportion of carboxylic acid-modified sites is 0.8 mol % in the entire structure.
  • 40 parts by mass of barium titanate particles (0.2 ⁇ m in BET equivalent diameter) as ceramic particles, 0.7 parts by mass of polyethylene glycol as a plasticizer, and 0.1 part by mass of an antistatic agent were added. added. The obtained suspension was then dispersed in a ball mill for a predetermined time to obtain a dielectric paste.
  • Green sheet preparation A dielectric paste was applied onto a PET (polyethylene terephthalate) film by a doctor blade method. After that, the coating film was dried to obtain a green sheet containing ceramic particles. The thickness of the green sheet was adjusted so that the thickness of the dielectric layer after firing was 1.7 ⁇ m.
  • a conductive paste was screen-printed on the green sheet.
  • the printed conductive paste was dried to obtain a conductive sheet.
  • the conductive paste was printed on the green sheet so as to form a pattern in which the planar dimension of the chip-shaped laminate cut and fired was 3.2 mm ⁇ 1.6 mm.
  • the thickness of the conductive sheet as the thickness of the metal component alone was 0.4 ⁇ m by XRF measurement.
  • the thickness of the conductive sheet immediately after drying was 0.8 ⁇ m.
  • the green sheet provided with the conductive sheet was peeled off from the PET film. 200 peeled sheets were laminated, and the 200 laminated sheets were placed in a mold. The sheets in the mold were pressed and crimped to obtain a laminate. The obtained laminate was cut into a predetermined size by press cutting to obtain a chip-shaped unfired laminate.
  • Example 2 The same test as in Example 1 was performed, except that the branched polymer was changed to a resin having a main chain made of ethyl cellulose and branch chains made of polycaprolactone, which is an aliphatic polyester. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 3 The same test as in Example 1 was performed, except that the polyoxyethylene group (polyether chain) of the dispersant was changed to a polycaprolactone group (polyester chain). Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 4 The same test as in Example 1 was conducted, except that the hydrophilic group of the dispersant was changed to a polypropylene carbonate group (polycarbonate chain). Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 5 The branched polymer is changed to a resin having a main chain made of ethyl cellulose and a branch chain made of polycaprolactone, which is an aliphatic polyester, and the polyoxyethylene group (polyether chain) of the dispersant is replaced with a polycaprolactone group ( The same test as in Example 1 was performed, except that the polyester chain was changed. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 6 A branched polymer is changed to a resin having a main chain made of ethyl cellulose and a branch chain made of polycaprolactone, which is an aliphatic polyester, and a hydrophilic group possessed by a dispersant is changed to a polypropylene carbonate group (polycarbonate chain).
  • polypropylene carbonate group polypropylene carbonate chain
  • Example 7 The same test as in Example 1 was performed, except that ceramic particles were not used in the preparation of the conductive paste. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 8 Except for changing the branched polymer to a resin having a main chain made of ethyl cellulose and branch chains made of polycaprolactone, an aliphatic polyester, and not using ceramic particles in the preparation of the conductive paste, A test similar to that of Example 1 was carried out. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 9 The same test as in Example 1 was performed except that the metal particles were changed to Cu particles having an SEM diameter of 500 nm. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 10 Except for changing the branched polymer to a resin having a main chain made of ethyl cellulose and a branch chain made of polycaprolactone, which is an aliphatic polyester, and changing the metal particles to Cu particles having an SEM diameter of 500 nm, A test similar to that of Example 1 was carried out. Table 1 shows the evaluation results of the occurrence of structural defects.
  • the binder is the ratio of the volume of the binder resin to the sum of the volume of the binder resin and the volume of the inorganic particles in the conductive paste.
  • the same test as in Example 1 was conducted except that the resin volume ratio was changed to 17% by volume. Table 1 shows the evaluation results of the occurrence of structural defects.
  • the binder is the ratio of the volume of the binder resin to the sum of the volume of the binder resin and the volume of the inorganic particles in the conductive paste.
  • the same test as in Example 1 was performed, except that the resin volume ratio was changed to 29% by volume.
  • Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 13 The branched polymer is changed to a resin having a main chain made of ethyl cellulose and a branch chain made of polycaprolactone which is an aliphatic polyester, the amount of the branched polymer used, and the amount of Ni particles and ceramic particles used are changed.
  • the binder resin volume ratio which is the ratio of the volume of the binder resin to the total of the volume of the binder resin in the conductive paste and the volume of the inorganic particles, is changed to 17% by volume. The same test as in 1 was performed. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 14 The branched polymer is changed to a resin having a main chain made of ethyl cellulose and a branch chain made of polycaprolactone which is an aliphatic polyester, the amount of the branched polymer used, and the amount of Ni particles and ceramic particles used are changed.
  • the binder resin volume ratio which is the ratio of the volume of the binder resin to the total of the volume of the binder resin in the conductive paste and the volume of the inorganic particles, is changed to 29% by volume.
  • Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 1 The same test as in Example 1 was performed, except that the branched polymer was changed to ethyl cellulose, which is a linear polymer. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 2 The branched polymer is changed to ethyl cellulose, which is a linear polymer, and the dispersant has a carboxy group, which is an adsorptive functional group, and a chain aliphatic hydrocarbon group, which is a hydrophobic group.
  • the same test as in Example 1 was performed, except that the dispersant was changed to a polymeric dispersant that did not have an ethylene group (polyether chain).
  • Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 3 The dispersant is changed to a polymeric dispersant that has a carboxy group, which is an adsorptive functional group, and a chain aliphatic hydrocarbon group, which is a hydrophobic group, but does not have a polyoxyethylene group (polyether chain). Except for this, the same test as in Example 1 was performed. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 4 The branched polymer is changed to a resin having a main chain composed of ethyl cellulose and a branch chain composed of polycaprolactone, which is an aliphatic polyester, and the dispersant is composed of a carboxy group, which is an adsorptive functional group, and a hydrophobic group.
  • the same test as in Example 1 was performed, except that the polymer dispersant was changed to a polymeric dispersant having certain linear aliphatic hydrocarbon groups but no polyoxyethylene groups (polyether chains). Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 5 The same test as in Example 1 was performed, except that the branched polymer was changed to a linear polymer, ethyl cellulose, and the hydrophilic group of the dispersant was changed to a polycaprolactone group (polyester chain). Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 6 The same test as in Example 1 was performed, except that the branched polymer was changed to a linear polymer, ethyl cellulose, and the hydrophilic group of the dispersant was changed to a polypropylene carbonate group (polycarbonate chain). Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 7 The same test as in Example 1 was performed, except that the branched polymer was changed to ethyl cellulose, which is a linear polymer, and ceramic particles were not used in the preparation of the conductive paste. Table 1 shows the evaluation results of the occurrence of structural defects.
  • Example 8 The same test as in Example 1 was performed, except that the branched polymer was changed to ethyl cellulose, which is a linear polymer, and the metal particles were changed to Cu particles having an SEM diameter of 500 nm. Table 1 shows the evaluation results of the occurrence of structural defects.
  • the specific functional groups in Table 1 below are types of functional groups corresponding to any of polyether chains, polyester chains, and polycarbonate chains.
  • the binder resin volume ratio is the ratio of the volume of the binder resin to the sum of the volume of the binder resin and the volume of the inorganic particles in the conductive paste.
  • the abbreviations in the table below are as follows.
  • EC ethyl cellulose
  • PCL polycaprolactone (aliphatic polyester)
  • PPC polypropylene carbonate (aliphatic polycarbonate)
  • a branched polymer having a main chain composed of a cellulosic polymer and branch chains composed of an aliphatic polycarbonate or an aliphatic polyester, and a dispersant having hydrophilic chains such as polyether chains are combined.
  • the binder resin contained in the conductive paste consists only of a main chain made of a cellulose polymer, or when the dispersant does not have a specific hydrophilic chain, when cutting the laminate It can be seen that delamination is likely to occur as a structural defect.

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Power Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

L'invention concerne une pâte contenant des particules inorganiques qui produit un film contenant des particules inorganiques qui, lorsqu'il est stratifié, résiste à la génération, en raison de l'action, par exemple, d'une force de cisaillement, d'une séparation intercouche d'une autre couche ; un film contenant des particules inorganiques qui peut être formé à l'aide de la pâte contenant des particules inorganiques ; et un stratifié qui contient le film contenant des particules inorganiques.　La combinaison d'un polymère ramifié et d'un agent dispersant est utilisée dans une pâte contenant des particules inorganiques comprenant une résine liante, particules inorganiques, et un solvant organique, le polymère ramifié ayant une chaîne moléculaire qui a une chaîne principale qui comprend un polymère cellulosique et une chaîne ramifiée comprenant un polycarbonate aliphatique ou un polyester aliphatique, et l'agent de dispersion a au moins un élément sélectionné dans le groupe constitué par les chaînes de polyéther, les chaînes de polyester et les chaînes de polycarbonate.
PCT/JP2021/045897 2021-02-02 2021-12-13 Pâte contenant des particules inorganiques, film contenant des particules inorganiques et stratifié WO2022168446A1 (fr)

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CN202180092230.3A CN116745872A (zh) 2021-02-02 2021-12-13 含无机粒子的糊剂、含无机粒子的膜、及层叠体
JP2022579372A JP7544157B2 (ja) 2021-02-02 2021-12-13 無機粒子含有ペースト、無機粒子含有膜、及び積層体
KR1020237025908A KR20230128323A (ko) 2021-02-02 2021-12-13 무기 입자 함유 페이스트, 무기 입자 함유 막, 및 적층체

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JP2009182128A (ja) * 2008-01-30 2009-08-13 Sekisui Chem Co Ltd 積層セラミックコンデンサ内部電極用導電ペースト
JP2014005192A (ja) * 2012-05-29 2014-01-16 Sekisui Chem Co Ltd 無機質焼結体製造用バインダー
JP2014070002A (ja) * 2012-09-28 2014-04-21 Sekisui Chem Co Ltd スラリー組成物の製造方法
WO2015040924A1 (fr) * 2013-09-18 2015-03-26 株式会社村田製作所 Corps moulé en céramique et procédé pour la production de composant électronique céramique empilé
JP2019140372A (ja) * 2018-02-08 2019-08-22 サムソン エレクトロ−メカニックス カンパニーリミテッド． キャパシタ部品及びその製造方法
JP2020088389A (ja) * 2018-11-19 2020-06-04 積水化学工業株式会社 導電ペースト
WO2020137289A1 (fr) * 2018-12-25 2020-07-02 住友金属鉱山株式会社 Pâte conductrice, composant électronique et condensateur céramique stratifié

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6939015B2 (ja) 2017-03-29 2021-09-22 住友金属鉱山株式会社 積層セラミックコンデンサ内部電極用のグラビア印刷用導電性ペースト

Patent Citations (8)

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Publication number Priority date Publication date Assignee Title
JP2007261941A (ja) * 2007-05-14 2007-10-11 Tdk Corp 水系セラミックグリーンシート用塗料組成物、セラミックグリーンシートの製造方法およびセラミック電子部品の製造方法
JP2009182128A (ja) * 2008-01-30 2009-08-13 Sekisui Chem Co Ltd 積層セラミックコンデンサ内部電極用導電ペースト
JP2014005192A (ja) * 2012-05-29 2014-01-16 Sekisui Chem Co Ltd 無機質焼結体製造用バインダー
JP2014070002A (ja) * 2012-09-28 2014-04-21 Sekisui Chem Co Ltd スラリー組成物の製造方法
WO2015040924A1 (fr) * 2013-09-18 2015-03-26 株式会社村田製作所 Corps moulé en céramique et procédé pour la production de composant électronique céramique empilé
JP2019140372A (ja) * 2018-02-08 2019-08-22 サムソン エレクトロ−メカニックス カンパニーリミテッド． キャパシタ部品及びその製造方法
JP2020088389A (ja) * 2018-11-19 2020-06-04 積水化学工業株式会社 導電ペースト
WO2020137289A1 (fr) * 2018-12-25 2020-07-02 住友金属鉱山株式会社 Pâte conductrice, composant électronique et condensateur céramique stratifié

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