Classifications

• • 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
  • H01G4/002—Details
  • H01G4/018—Dielectrics
  • H01G4/06—Solid dielectrics
  • H01G4/08—Inorganic dielectrics
  • H01G4/12—Ceramic dielectrics
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
  • C04B35/26—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on ferrites
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/62218—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products obtaining ceramic films, e.g. by using temporary supports
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/62605—Treating the starting powders individually or as mixtures
  • C04B35/6261—Milling
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/62605—Treating the starting powders individually or as mixtures
  • C04B35/62625—Wet mixtures
  • C04B35/6263—Wet mixtures characterised by their solids loadings, i.e. the percentage of solids
• • C—CHEMISTRY; METALLURGY
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
  • C04B35/632—Organic additives
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
  • C04B35/632—Organic additives
  • C04B35/634—Polymers
  • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C04B35/63416—Polyvinylalcohols [PVA]; Polyvinylacetates
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  • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
  • C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
  • C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
  • C04B35/632—Organic additives
  • C04B35/634—Polymers
  • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C04B35/63424—Polyacrylates; Polymethacrylates
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  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
  • C09D129/02—Homopolymers or copolymers of unsaturated alcohols
  • C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
• • 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
• • C—CHEMISTRY; METALLURGY
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
  • C04B2235/30—Constituents and secondary phases not being of a fibrous nature
  • C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
  • C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
  • C04B2235/3272—Iron oxides or oxide forming salts thereof, e.g. hematite, magnetite
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/60—Aspects relating to the preparation, properties or mechanical treatment of green bodies or pre-forms
  • C04B2235/602—Making the green bodies or pre-forms by moulding
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/65—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes
  • C04B2235/656—Aspects relating to heat treatments of ceramic bodies such as green ceramics or pre-sintered ceramics, e.g. burning, sintering or melting processes characterised by specific heating conditions during heat treatment
  • C04B2235/6562—Heating rate
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  • C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
  • C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
  • C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
  • C04B2235/963—Surface properties, e.g. surface roughness
  • C04B2235/9638—Tolerance; Dimensional accuracy
• • 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
  • C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
  • C08K3/20—Oxides; Hydroxides
  • C08K3/22—Oxides; Hydroxides of metals
  • C08K2003/2265—Oxides; Hydroxides of metals of iron
  • C08K2003/2272—Ferric oxide (Fe2O3)
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L2205/00—Polymer mixtures characterised by other features
  • C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
  • C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L2205/00—Polymer mixtures characterised by other features
  • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
• • C—CHEMISTRY; METALLURGY
  • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
  • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
  • C08L2205/00—Polymer mixtures characterised by other features
  • C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
  • C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Definitions

• the present invention relates to a binder composition for producing a green sheet, a slurry composition for firing, a method for producing a green sheet, a method for producing a sintered body, and a method for producing a multilayer ceramic capacitor. More specifically, a binder composition for producing a green sheet, a slurry composition for firing for producing a sintered body of an inorganic powder, and a method for producing a green sheet containing a dried product of the slurry composition for firing.
• the present invention relates to a method for producing a sintered body of a slurry composition for firing, and a method for producing a multilayer ceramic capacitor containing a sintered body for green sheets.
• an organic solvent such as toluene is mainly blended as a solvent in the binder composition and the slurry composition for firing for producing a ceramic green sheet.
• the solvent to be blended in the binder composition for firing, the slurry composition, and the like is required to be converted from an organic solvent to an aqueous solvent.
• Patent Document 1 describes a hydrophobic group having a hydrocarbon having 4 or more carbon atoms, or a modified polyvinyl having both a hydrophobic group having a hydrocarbon having 4 or more carbon atoms and an ionic hydrophilic group in a side chain.
• a molding binder containing alcohol as a main component is disclosed. It is disclosed that this molding binder can mold a green sheet even if it contains an aqueous solvent.
• An object of the present invention is to impart strength and flexibility to a sheet while maintaining storage stability when producing a slurry composition in an aqueous system and maintaining high smoothness when formed on the sheet. It is an object of the present invention to provide a binder composition for producing a green sheet, and a slurry composition for firing containing the binder composition.
• Another object of the present invention is a method for producing a green sheet, a method for producing a sintered body, and a method for producing a sintered body, in which the sheet can have high strength and flexibility while maintaining high smoothness when formed on the sheet.
• a method for manufacturing a multilayer ceramic capacitor To provide a method for manufacturing a multilayer ceramic capacitor.
• the binder composition for producing a green sheet according to one aspect of the present invention is a binder composition for producing a green sheet.
• the binder composition contains a polyvinyl alcohol resin (C).
• the polyvinyl alcohol resin (C) contains at least two kinds of components having different degrees of hydrophilicity.
• the baking slurry composition according to one aspect of the present invention contains the binder composition, the inorganic powder (B), and water.
• the method for producing a green sheet according to one aspect of the present invention includes applying the slurry composition for firing and drying it.
• the method for producing a sintered body according to one aspect of the present invention includes firing the green sheet obtained by the method for producing a green sheet.
• the method for manufacturing a multilayer ceramic capacitor according to one aspect of the present invention includes firing a laminate obtained by stacking a plurality of green sheets obtained by the method for manufacturing a green sheet.
• the binder composition for producing a green sheet according to the present embodiment is a binder composition (hereinafter, also referred to as a binder composition (X)) used for producing a green sheet.
• the binder composition (X) contains a polyvinyl alcohol resin (C), and the polyvinyl alcohol resin (C) contains at least two kinds of components having different degrees of hydrophilicity.
• the binder composition (X) may have a function as a binder by containing the polyvinyl alcohol resin (C).
• the slurry composition for firing hereinafter referred to as slurry composition (Y) contains the above-mentioned binder composition (X), inorganic powder (B), and water.
• the sheet formed from the slurry composition (Y) can have high strength and flexibility. Since the slurry composition (Y) contains the inorganic powder (B), the inorganic powder is obtained by firing the slurry composition (Y) or a sheet (green sheet) formed from the slurry composition (Y). The body is sintered. Thereby, a sintered body can be produced from the slurry composition (Y).
• the binder composition (X) contains the polyvinyl alcohol resin (C)
• the binder composition (X) can be easily dissolved in the slurry composition (Y).
• the components in the slurry composition (Y) can be easily dispersed.
• the polyvinyl alcohol resin (C) in the binder composition (X) contains at least two kinds of components having different degrees of hydrophilicity, the components in the slurry composition (Y) can be efficiently dispersed. Therefore, even if the slurry composition (Y) is prepared from the binder composition (X) in an aqueous solvent, aggregation and gelation are unlikely to occur, and the slurry composition (Y) has high storage stability. sell.
• the binder composition (X) and the slurry composition (Y) are formed on a sheet by containing a polyvinyl alcohol resin (C) containing two or more kinds of components having different degrees of hydrophilicity, It can contribute to the flexibility and strength of the sheet in a well-balanced manner. It is considered that this is because the interaction between the hydrophilic functional groups such as hydroxyl groups of the polyvinyl alcohol resin (C) and the surface of the inorganic powder (B) contributes to the improvement of the strength of the sheet.
• the interaction between the inorganic powder (B) and the polyvinyl alcohol resin (C) can be adjusted, and the strength and flexibility of the sheet can be easily adjusted. That is, the sheet formed from the slurry composition (X) containing the binder composition (X) can have both strength and flexibility.
• the polyvinyl alcohol resin (C) contains two or more kinds of components having different degrees of hydrophilicity, so that each component in the slurry composition (Y) can be easily dispersed uniformly. Therefore, when the slurry composition (Y) is applied by printing to form a sheet, unevenness and repelling can be less likely to occur in the coating film. Therefore, the sheet has high printability, whereby the sheet formed from the slurry composition (Y) can have high smoothness.
• the degree of hydrophilicity is different means that there is a difference in the degree of affinity with water among a plurality of components. "The degree of hydrophilicity is different” can be judged from, for example, a difference in solubility in water and a difference in water absorption. Further, it can be said that the components in the polyvinyl alcohol resin (C) having different degrees of saponification have different degrees of hydrophilicity. It can be said that the components of the polyvinyl alcohol resin (C) having different functional groups also have different degrees of hydrophilicity. Even if the components have the same functional group, if they have different functional group equivalents, it can be said that the degree of hydrophilicity is different.
• the binder composition for producing a green sheet the binder composition for producing a green sheet
• the slurry composition for firing the green sheet
• the sintered body the ceramic capacitor according to the present embodiment
• the binder composition (X) is a composition for producing a green sheet and functions as a binder.
• the binder composition (X) constitutes a slurry composition (Y) for firing together with components such as an inorganic powder (B), and the slurry composition (Y) is applied and dried if necessary.
• a green sheet can be made.
• the binder composition (X) contains the polyvinyl alcohol resin (C), and the polyvinyl alcohol resin (C) contains at least two kinds of components having different degrees of hydrophilicity. Therefore, the slurry composition (Y) containing the binder composition (X) has storage stability. In addition, the high smoothness of the sheet formed from the slurry composition (Y) can be maintained, and the sheet can have good strength and flexibility.
• the degree of hydrophilicity of the polyvinyl alcohol resin (C) depends on its molecular structure, specifically, for example, the type of hydrophilic functional group, the number of hydrophilic functional groups, the type of hydrophobic functional group, and the number of hydrophobic functional groups. , It may differ depending on the structure of the main chain and the like.
• the polyvinyl alcohol resin (C) is a polyvinyl alcohol in which polyvinyl acetate is completely saponified, a polyvinyl alcohol in which polyvinyl acetate is partially saponified, and a part of the hydroxyl groups in the structure of the polyvinyl alcohol. It contains at least one selected from the group consisting of modified products obtained by modifying a part of an acetic acid group (acetyloxy group).
• the polyvinyl alcohol resin (C) is a component capable of making the binder composition (X) function as a binder.
• the polyvinyl alcohol resin (C) contains at least two kinds of components having different degrees of hydrophilicity. Therefore, as described above, the polyvinyl alcohol resin (C) can impart storage stability to the slurry composition (Y) and can impart high smoothness and flexibility to the sheet. Further, since the polyvinyl alcohol resin (C) contains at least the above two kinds of components, the temperature range of thermal decomposition at the time of firing can be expanded when the slurry composition (Y) is fired. As a result, rapid weight loss during firing of the slurry composition (Y) can be suppressed. Therefore, cracks can be less likely to occur in the sintered body.
• the average degree of polymerization of the polyvinyl alcohol resin (C) is preferably 500 or more and 9000 or less. In this case, the polyvinyl alcohol resin (C) can be easily dissolved in water. Further, in this case, the polyvinyl alcohol resin (C) is more likely to adsorb the inorganic powder (B), so that the dispersibility of the inorganic powder (B) in the slurry composition (Y) is further improved. Can be done.
• the average degree of polymerization of the polyvinyl alcohol resin (C) is more preferably 500 or more and 4000 or less, and further preferably 1500 or more and 4000 or less. The average degree of polymerization can be calculated from the relative viscosity with water obtained by using an Ostwald viscometer after completely saponifying polyvinyl alcohol (C) with sodium hydroxide.
• the polyvinyl alcohol resin (C) preferably contains at least two types of components having different degrees of saponification.
• the polyvinyl alcohol resin (C) may contain at least two kinds of components having different hydrophilicity. Therefore, the polyvinyl alcohol resin (C) can efficiently disperse the components in the slurry composition (Y). Therefore, even if the slurry composition (Y) is prepared from the binder composition (X) in an aqueous solvent, aggregation and gelation are unlikely to occur, and the slurry composition (Y) has higher storage stability. Can be done.
• the degree of interaction between the polyvinyl alcohol resin (C) and the inorganic powder (B) in the slurry composition (Y) can be adjusted, and the strength and flexibility of the sheet can be more easily adjusted. Can be adjusted.
• the polyvinyl alcohol resin (C) contains two or more kinds of components having different degrees of saponification, each component in the slurry composition (Y) is easily dispersed uniformly. Therefore, when the slurry composition (Y) is applied by printing to form a sheet, unevenness and repelling can be less likely to occur in the coating film. As a result, the sheet formed from the slurry composition (Y) can have higher smoothness.
• the degree of saponification can be calculated by measuring the polyvinyl alcohol resin in accordance with, for example, JIS K6726 (1994), and it is measured that the degree of saponification of the components contained in the polyvinyl alcohol resin (C) is different. It can be judged from the result.
• the polyvinyl alcohol resin (C) preferably contains a nonionic polyvinyl alcohol resin (C1) and an anionic polyvinyl alcohol resin (C2).
• a nonionic polyvinyl alcohol resin (C1) e.g., a polyvinyl alcohol resin (C1)
• an anionic polyvinyl alcohol resin (C2) may have higher hydrophilicity than the nonionic polyvinyl alcohol resin (C1) described above.
• the anionic polyvinyl alcohol resin (C2) tends to increase the viscosity of the binder composition (X), which makes it difficult for cissing to occur on the surface of the sheet when forming the sheet.
• the polyvinyl alcohol resin (C) contains not only the nonionic polyvinyl alcohol resin (C1) but also the anionic polyvinyl alcohol resin (C2), the physical properties of the binder composition (X) and the slurry composition (Y) It is easy to adjust the balance between and pH. Therefore, it is possible to prevent agglutination and gelation when a paste is prepared from the slurry composition (Y).
• the low temperature range is, for example, a temperature in the range of 300 ° C. or higher and 500 ° C. or lower
• the high temperature range is, for example, a temperature in the range of 500 ° C. or higher and 700 ° C. or lower. However, it is not limited to these temperatures.
• the ratio of the nonionic polyvinyl alcohol resin (C1) to the total amount of the nonionic polyvinyl alcohol resin (C1) and the anionic polyvinyl alcohol resin (C2) is preferably 30% by mass or more and 90% by mass or less, preferably 40% by mass. More preferably, it is% or more and 85% by mass or less.
• the anionic polyvinyl alcohol resin (C2) preferably contains a polyvinyl alcohol resin (C21) having a carboxyl group.
• the polyvinyl alcohol resin (C21) has a carboxyl group in addition to the hydrophilic hydroxyl group. Therefore, the interaction between the carboxyl group of the polyvinyl alcohol resin (C21) and the inorganic powder (B) becomes stronger, and the strength of the sheet can be further improved. Further, in this case, it is easier to adjust the balance between the physical properties of the binder composition (X) and the slurry composition (Y) and the pH. Therefore, it is possible to prevent agglutination and gelation when a paste is produced from the slurry composition (Y), and thereby further improve the physical properties of the sheet.
• polyvinyl alcohol resin (C21) examples include KL-506, KL-318, KL-118 manufactured by Kuraray Co., Ltd .; Gosenex T-330, T-330 manufactured by Japan Synthetic Chemical Co., Ltd. 350, T-330H; Product names AP-17, AT-17, AF-17, etc. manufactured by Japan Vam & Poval Co., Ltd. can be mentioned.
• the polyvinyl alcohol resin (C) contains at least two kinds of components having different degrees of saponification
• the polyvinyl alcohol resin (C) contains a component (C3) having a degree of saponification of 85 mol% or more and 99 mol% or less and ken. It is also preferable to contain a component (C4) having a degree of conversion of 60 mol% or more and less than 85 mol%.
• the component (C3) has a larger proportion of hydroxyl groups than the component (C4), it can contribute to improving the strength of the sheet formed from the binder composition (X) and the slurry composition (Y), while The component (C4) can contribute to the improvement of the flexibility of the sheet.
• the slurry composition (Y) prepared from the binder composition (X) tends to flow so that the film thickness becomes uniform. That is, the component (C4) can further improve the leveling property of the slurry composition (Y). Therefore, the smoothness of the sheet formed from the slurry composition (Y) can be further improved. Further, by containing the component (C4) having a relatively low degree of saponification, the temperature range of thermal decomposition when sintering the slurry composition (Y) and the sheet can be widened, so that the weight is rapidly reduced by heating.
• the degree of saponification of the component (C4) is more preferably 60 mol% or more and less than 80 mol%.
• the ratio of the component (C3) to the total amount of the component (C3) and the component (C4) is preferably 30% by mass or more and 90% by mass or less, and more preferably 40% by mass or more and 85% by mass or less. ..
• the component (C3) and the component (C4) are components that are distinguished by the degree of saponification.
• the component (C3) and the component (C4) may be either nonionic or anionic, respectively. Therefore, the component (C3) and the component (C4) can overlap with the component contained in either the nonionic polyvinyl alcohol resin (C1) or the anionic polyvinyl alcohol resin (C2).
• the nonionic polyvinyl alcohol resin (C1) includes a nonionic polyvinyl alcohol resin (C11) having a saponification degree of 85 mol% or more and 99 mol% or less, and a nonionic polyvinyl alcohol resin (C1) having a saponification degree of 60 mol% or more and less than 85 mol%. It is preferable that the anionic polyvinyl alcohol resin (C2) containing C12) contains an anionic polyvinyl alcohol resin (C21) having a carboxyl group. That is, the polyvinyl alcohol resin (C) preferably contains a nonionic polyvinyl alcohol resin (C11), a nonionic polyvinyl alcohol resin (C12), and an anionic polyvinyl alcohol resin (C21).
• the polyvinyl alcohol resin (C11) has a higher proportion of hydroxyl groups than the polyvinyl alcohol resin (C12), which contributes to improving the strength of the sheet formed from the binder composition (X) and the slurry composition (Y). it can. Further, since the polyvinyl alcohol resin (C21) has a carboxyl group, the contribution to the improvement of the strength of the sheet is further large. On the other hand, the polyvinyl alcohol resin (C12) can contribute to the improvement of the flexibility of the sheet. Therefore, higher strength and flexibility can be imparted to the sheet formed from the binder composition (X) and the slurry composition (Y).
• the leveling property of the slurry composition (Y) prepared from the binder composition (X) can be further improved. Therefore, the smoothness of the sheet formed from the slurry composition (Y) can be further improved.
• the slurry composition (Y) contains the anionic polyvinyl alcohol resin (C21), the temperature range of thermal decomposition when the slurry composition (Y) and the sheet are sintered can be widened. Sudden weight loss due to heating can be easily suppressed. As a result, when the polyvinyl alcohol resin (C21) is contained, it is easy to suppress the heat shrinkage of the sintered body in the low temperature range.
• the degree of saponification of the nonionic polyvinyl alcohol resin (C12) is more preferably 60 mol% or more and less than 80 mol%.
• the ratio of the polyvinyl alcohol resin (C21) to the total amount of the polyvinyl alcohol resin (C11), the polyvinyl alcohol resin (C12), and the polyvinyl alcohol resin (C21) is preferably 10% by mass or more and 50% by mass or less, 20%. More preferably, it is by mass% or more and 40% by mass or less.
• the polyvinyl alcohol resin (C1) contains a nonionic polyvinyl alcohol resin (C11) having a saponification degree of 85 mol% or more and 99 mol% or less, and the polyvinyl alcohol resin (C21) has a saponification degree of 60 or more and less than 85 and carboxyl. It is also preferable to contain an anionic polyvinyl alcohol resin (C211) having a group. That is, the polyvinyl alcohol resin (C) preferably contains both a nonionic polyvinyl alcohol resin (C1) and an anionic polyvinyl alcohol resin (C211).
• the polyvinyl alcohol resin (C11) since the polyvinyl alcohol resin (C11) has a larger proportion of hydroxyl groups than the polyvinyl alcohol resin (C21), it contributes to the improvement of the strength of the sheet formed from the binder composition (X) and the slurry composition (Y). it can. Further, although the polyvinyl alcohol resin (C211) has a smaller proportion of hydroxyl groups than the polyvinyl alcohol resin (C11), it has a carboxyl group, so that it contributes to the improvement of strength while maintaining the high flexibility of the sheet. Can be done. Therefore, higher strength and flexibility can be imparted to the sheet formed from the binder composition (X) and the slurry composition (Y).
• the temperature range of thermal decomposition when sintering the slurry composition (Y) and the sheet can be widened. Therefore, it becomes easy to suppress a rapid weight loss due to heating.
• the polyvinyl alcohol resin (C211) when the polyvinyl alcohol resin (C211) is contained, it is easy to suppress the heat shrinkage of the sintered body in the low temperature range. In this case, cracks can be further reduced in the sintered body.
• the degree of saponification of the anionic polyvinyl alcohol resin (C211) having a carboxyl group is more preferably 60 mol% or more and less than 80 mol%.
• the ratio of the polyvinyl alcohol resin (C211) to the total amount of the polyvinyl alcohol resin (C11) and the polyvinyl alcohol resin (C211) is preferably 10% by mass or more and 70% by mass or less, and 15% by mass or more and 60% by mass or less. Is more preferable.
• nonionic polyvinyl alcohol resin having a saponification degree of 85 or more and 99 or less
• the product names PVA-235, PVA-217, PVA-105, PVA-117 manufactured by Kuraray Co., Ltd. , PVA-124, PVA-205, PVA-224 ; Product name manufactured by Denka Co., Ltd. Denka Poval K-05, K-17C, H-17, B-20; Product name manufactured by Japan Vam & Poval Co., Ltd. JC-33 , JF-05, JM-23, JP-03 and the like.
• nonionic polyvinyl alcohol resin (C12) having a saponification degree of 60 or more and less than 85 the product names PVA-505, PVA-405, PVA-417, PVA-420 manufactured by Kuraray Co., Ltd. ; Product name Gosenol KL-05, KL-03, KH-20, KH-17, KP-08R, NK-05R manufactured by Nippon Synthetic Chemical Industry Co., Ltd .; Product name JL-05E, JL- manufactured by Japan Vam & Poval Co., Ltd. 22E, JL-25E, JR-05 and the like can be mentioned.
• the polyvinyl alcohol resin (C) may contain, for example, a cationic polyvinyl alcohol resin in addition to the nonionic polyvinyl alcohol resin (C1) and the anionic polyvinyl alcohol resin (C2) described above. Further, the polyvinyl alcohol resin (C) may contain the component having a saponification degree of less than 60 mol% as described above.
• the binder composition (X) may contain an appropriate solvent, additives and the like.
• the binder composition (X) may contain water as a solvent.
• the binder composition (X) and the slurry composition (Y) contain at least two different types of polyvinyl alcohol resin (C), and therefore, each component is contained. Highly dispersible in water. Therefore, the binder composition (X) and the slurry composition (Y) can have high storage stability. Further, since the binder composition (X) and the slurry composition (Y) have high dispersibility, the sheet formed from the binder composition (X) and the slurry composition (Y) has high smoothness.
• Additives include, for example, plasticizers.
• the plasticizer include amine compounds.
• amine compounds include, for example, diethanolamine, N-methylethanolamine, N-ethylethanolamine, Nt-butylethanolamine, N-methyldiethanolamine, Nn-butyldiethanolamine, Nt-butyldiethanolamine, N- Includes at least one aminoalcohol compound selected from the group consisting of lauryldiethanolamine, polyoxyethylene dodecylamine, polyoxyethylene laurylamine, and polyoxyethylene stearylamine.
• additives include dispersants, defoamers, rheology control agents, wetting agents, adhesion imparting agents, surfactants and the like.
• the binder composition (X) can be prepared by kneading and mixing the components described above by an appropriate method.
• the slurry composition (Y) contains the binder composition (X) described above, the inorganic powder (B), and water.
• the slurry composition (Y) contains an inorganic powder (B), water, and the polyvinyl alcohol resin (C) described above, and the polyvinyl alcohol resin (C) has at least two types of hydrophilicity.
• the component that can be contained in the slurry composition (Y) may overlap with the component that can be contained in the binder composition (X).
• the description of the components described in the components that can be contained in the binder composition (X) will be omitted as appropriate.
• the inorganic powder (B) can contain an appropriate material according to the characteristics required for the sintered body formed from the inorganic powder (B). Specifically, the inorganic powder (B) contains at least one material selected from the group consisting of, for example, metal oxides, carbides, borides, sulfides, nitrides and the like.
• the metals include, for example, Li, Pd, K, Be, Mg, B, Al, Si, Ca, Sr, Ba, Zn, Cd, Ga, In, lanthanide, actinide, Ti, Zr, Hf, Bi, V, Nb, Includes at least one selected from the group consisting of Ta, W, Mn, Fe, Ca, Ni and the like.
• the inorganic powder (B) contains a plurality of metal elements
• the inorganic powder (B) is, for example, macerite, barium titanate, silicate glass, ferrite, lead glass, CaO / Al 2 O 3 / SiO 2 system. It can contain one or more components selected from the group consisting of inorganic glass, MgO / Al 2 O 3 / SiO 2 type inorganic glass and LiO 2 / Al 2 O 3 / SiO 2 type inorganic glass. It is particularly preferable that the inorganic powder (B) contains at least one material selected from the group consisting of aluminum-containing oxides, silicon-containing nitrides, iron oxide, and barium titanate.
• Oxides containing aluminum are, for example, from CaO / Al 2 O 3 / SiO 2 inorganic glass, MgO / Al 2 O 3 / SiO 2 inorganic glass, LiO 2 / Al 2 O 3 / SiO 2 inorganic glass and the like. Includes at least one material selected from the group.
• the inorganic powder (B) of the present embodiment is an aggregate (powder) of powdery particles having an average particle diameter of 10 ⁇ m or less.
• the average particle size is, for example, a volume-based median size (D 50 ) calculated from the measured value of the particle size distribution by the laser diffraction / scattering method, and can be obtained by using a commercially available laser diffraction / scattering type particle size distribution measuring device.
• the slurry composition (Y) contains water as described above. Since the slurry composition (Y) contains the binder composition (X) even when water is blended as a solvent, the dispersibility of each component in water is high. Therefore, the slurry composition (Y) can have high storage stability. Further, since the slurry composition (Y) has high dispersibility, the sheet formed from the slurry composition (Y) has high smoothness.
• the slurry composition (Y) may contain a solvent other than water.
• Solvents other than water include, for example, methanol, ethanol, propyl alcohol, isopropyl alcohol, propylene glycol monomethyl ether, ethylene glycol, ethylene glycol monoethyl ether, ethylene glycol monobutyl ether, ethylene glycol monotersial butyl ether, polyethylene glycol monomethyl ether, and 2.
• -It may contain at least one selected from the group consisting of methyl hydroxyisobutyrate and the like.
• the solvent may be a solvent constituting the slurry composition (Y).
• the slurry composition (X) may be prepared by further adding a solvent such as water according to the composition of the slurry composition (Y).
• the slurry composition (Y) may contain components such as additives other than the components described above.
• additives include dispersants, plasticizers, defoamers, rheology control agents, wetting agents, adhesion imparting agents, surfactants and the like. Specific examples of additives and the like may be the same as [Other components] in the binder composition (X).
• slurry composition (Y) for example, inorganic powder (B), water, and if necessary, additives such as a solvent and a dispersant are mixed and stirred to disperse each component.
• the slurry composition (Y) can contain an aqueous solution of the polyvinyl alcohol resin (C), that is, the slurry composition (Y) is prepared by dissolving the polyvinyl alcohol resin (C) in water in advance, and then with other components. It may be blended and adjusted.
• the amount of each component constituting the slurry composition (Y) may be appropriately set.
• the amount of (C) is preferably 1% by mass or more and 20% by mass or less, more preferably 4% by mass or more and 15% or less by mass, and further preferably 7% by mass or more and 11% by mass or less. ..
• the amount of the inorganic powder (B) with respect to the total solid content of the slurry composition (Y) is, for example, preferably 75% by mass or more and 95% by mass or less, and more preferably 80% by mass or more and 95% by mass or less. , 85% by mass or more and 95% by mass or less is more preferable.
• the amount of the polyvinyl alcohol resin (C) with respect to the inorganic powder (B) in the slurry composition (Y) is preferably, for example, 1% by mass or more and 20% by mass or less, and 5% by mass or more and 15% by mass or less. More preferably, it is more preferably 8% by mass or more and 12% by mass or less.
• the amount of the binder composition (X) is preferably 5 parts by mass or more and 20 parts by mass or less with respect to 100 parts by mass of the inorganic powder (B) in the slurry composition (Y). In this case, the smoothness and flexibility of the sheet can be maintained when forming the sheet from the slurry composition (Y).
• the amount of water with respect to the total amount of the slurry composition (Y) is preferably 6% by mass or more and 45% by mass or less, more preferably 8% by mass or more and 40% by mass or less, and 10% by mass or more and 37% by mass or less. The following is more preferable.
• total solid content of the slurry composition (Y) is the total amount of the components of the slurry composition (Y) excluding the solvent.
• the pH of the slurry composition (Y) is preferably 5 or more and less than 8. In this case, since aggregation, gelation and phase separation of the firing slurry composition are unlikely to occur, the storage stability of the firing slurry composition can be further improved. Therefore, when forming a sheet from the slurry composition for firing, a flexible sheet can be finished.
• the pH of the baking slurry composition is more preferably 6 or more and 7 or less.
• the blending amount of the amino alcohol compound (A) and the polyvinyl alcohol resin (C) (in this embodiment, the anionic polyvinyl alcohol resin (C2)) is appropriately adjusted. It is feasible by such means.
• the viscosity of the slurry composition (Y) is preferably 1000 mPa ⁇ s or more and 5000 mPa ⁇ s or less. In this case, when a coating film is formed by applying from the slurry composition (Y) by printing, uneven printing and repelling due to printing can be made particularly less likely to occur. Therefore, the sheet formed from the slurry composition (Y) can be made smoother and more uniform.
• the viscosity of the slurry composition (Y) at 25 ° C. is more preferably 1000 mPa ⁇ s or more and 4000 mPa ⁇ s or less, and further preferably 2000 mPa ⁇ s or more and 3000 mPa ⁇ s or less.
• the green sheet contains an inorganic powder (B) and at least two different polyvinyl alcohol resins (C). Therefore, the green sheet of the present embodiment has high smoothness and flexibility. Therefore, when the sheet is formed from the slurry composition (Y) containing the component of the binder composition (X), flexibility can be imparted to the sheet as described above, so that the sheet can be made less likely to warp. This makes it possible to improve the adhesion of the sheet to a base material such as a carrier film. Therefore, in the green sheet of the present embodiment, it is possible to suppress the occurrence of cracks.
• the green sheet can be produced, for example, as follows.
• a green sheet can be obtained by preparing the slurry composition (Y) described above, applying it on a substrate, and drying it if necessary.
• a method for applying the slurry composition (Y) to the substrate an appropriate method can be adopted, and examples thereof include a doctor blade method, a screen printing method, and a dispensing method.
• the base material for applying the slurry composition (Y) an appropriate base material can be adopted, and for example, a carrier film such as a polyethylene terephthalate (PET) film may be used.
• PET polyethylene terephthalate
• the green sheet of this embodiment can be suitably used for the purpose of a ceramic green sheet for manufacturing a multilayer ceramic capacitor or the like.
• components such as the polyvinyl alcohol resin (C) are thermally decomposed and removed, and the inorganic powder (B) is sintered.
• a sintered body of the inorganic powder (B) is formed, and this sintered body can form appropriate elements such as electrodes and conductor wiring.
• an appropriate element such as a conductor layer, a dielectric layer, an insulating layer, etc. can be produced from the green sheet.
• the green sheet is contained in a dielectric layer in a multilayer ceramic capacitor and a ceramic circuit board.
• the green sheet of the present embodiment has high strength and flexibility, it is possible to easily make a thin film even if it is laminated in multiple layers when manufacturing a multilayer ceramic capacitor from the green sheet.
• a multilayer ceramic capacitor can be manufactured from a green sheet, for example, as follows.
• the pressure at which the green sheets are laminated and pressurized is not particularly limited and may be appropriately set according to the number of laminated sheets or the like, but can be, for example, 10 MPa or more and 100 MPa or less.
• the conditions for firing may be appropriately set according to the sintering temperature of the inorganic powder (B), but the heating temperature is, for example, 500 ° C. or higher and 1500 ° C. or lower, and the heating time is, for example, 1 hour or longer. It can be 24 hours or less.
• a single layer ceramic capacitor may be manufactured from one green sheet having appropriate dimensions.
• -PVA-217 aqueous solution (manufactured by Kuraray Co., Ltd .: concentration 20%, saponification degree 88 mol%, average degree of polymerization 1700).
• -Gosenol KL-05 aqueous solution (manufactured by Nippon Synthetic Chemical Co., Ltd .: concentration 30%, saponification degree 80 mol%, average degree of polymerization 500).
• -PVA-505 aqueous solution (manufactured by Kuraray Co., Ltd .: concentration 30%, saponification degree 74 mol%, polymerization degree 500).
• -KL-118 aqueous solution (manufactured by Kuraray Co., Ltd .: concentration 30%, saponification degree 98 mol%, carboxyl group content, average degree of polymerization 1800).
• -PVA-205 aqueous solution (manufactured by Kuraray Co., Ltd .: concentration 30%, saponification degree 88 mol%, average degree of polymerization 500).
• -PVA-105 aqueous solution (manufactured by Kuraray Co., Ltd .: concentration 30%, saponification degree 98 mol%, average degree of polymerization 500).
• -PVA-117 aqueous solution (manufactured by Kuraray Co., Ltd .: concentration 30%, saponification degree 98 mol%, average degree of polymerization 1700).
• the [polyvinyl alcohol resin] shown above was mixed by adjusting an aqueous solution dissolved in water so as to have the concentration shown in parentheses.
• the values in the table indicate the amount of the aqueous solution of each aqueous solution of the polyvinyl alcohol resin at each of the above concentrations.
• the weight loss rate of the baking slurry composition at 550 ° C. was 99% by mass or more, but a small amount of baking residue was observed.
• C The weight loss rate of the baking slurry composition at 550 ° C. was 95% by mass or more and less than 99% by mass.
• D The weight loss rate of the baking slurry composition at 550 ° C. was less than 95% by mass, and after the measurement was completed, residues such as carbides were visually observed.
• B The film can be peeled off from the PET film and can withstand pulling, but the strength decreases after 2 weeks or more.
• C The film can be peeled off from the PET film, but it is easily torn by pulling.
• D The film cannot be peeled off from the PET film, or is torn when peeled off.
• the firing slurry composition prepared in (1) has a film thickness of about 100 ⁇ m on a release PET film (dimensions 100 mm ⁇ 100 mm) using a four-sided applicator (manufactured by Taiyu Kikai Co., Ltd., model number No. 112).
• a film was formed by applying the above.
• the coating unevenness of the obtained film was observed and evaluated according to the following criteria.
• B The film has slight coating unevenness, but the surface of the film is almost smooth and uniform.
• C Coating unevenness is observed in the range of less than 50% of the film, and the surface of the film is neither smooth nor uniform.
• D Coating unevenness is observed in the range of 50% or more of the film, and the surface of the film is neither smooth nor uniform.
• the firing slurry composition prepared in (1) has a film thickness of about 100 ⁇ m on a release PET film (dimensions 100 mm ⁇ 100 mm) using a four-sided applicator (manufactured by Taiyu Kikai Co., Ltd., model number No. 112).
• a film was formed by applying the above.
• the repellency of the obtained film on the PET substrate was observed and evaluated according to the following criteria.
• C Repellent from the base material is observed in the range of less than 50% of the film, and the surface of the film is neither smooth nor uniform.
• D Repellent from the base material is observed in the range of 50% or more of the film, and the surface of the film is neither smooth nor uniform.
• the binder composition for producing a green sheet according to the first aspect of the present invention is a binder composition for producing a green sheet.
• the binder composition contains a polyvinyl alcohol resin (C), and the polyvinyl alcohol resin (C) contains at least two kinds of components having different hydrophilicities.
• the sheet is imparted with strength and flexibility while having storage stability when the slurry composition is prepared in an aqueous system and maintaining high smoothness when formed on the sheet. be able to.
• the polyvinyl alcohol resin (C) contains at least two kinds of components having different degrees of saponification.
• the binder composition for producing a green sheet according to the third aspect has, in any one of the first to second aspects, a component (C3) having a saponification degree of 85 mol% or more and 99 mol% or less, and a saponification degree of 60 mol%. It contains a component (C4) which is more than 85 mol% or more.
• the component (C3) has a higher proportion of hydroxyl groups than the component (C4), the strength of the sheet produced from the binder composition (X) and the slurry composition (Y) can be improved.
• the component (C4) can contribute to the improvement of the flexibility of the sheet. Therefore, better strength and flexibility can be imparted to the sheets prepared from the binder composition (X) and the slurry composition (Y).
• the binder composition for producing a green sheet according to the fourth aspect contains a nonionic polyvinyl alcohol resin (C1) and an anionic polyvinyl alcohol resin (C2) in any one of the first to third aspects.
• the strength of the sheet produced from the baking slurry composition can be further improved.
• the binder composition for producing a green sheet in the fifth aspect contains the polyvinyl alcohol resin (C2) containing a carboxyl group as the anionic polyvinyl alcohol resin (C2).
• the storage stability of the slurry composition can be further improved. Further, when formed on a sheet, good strength and flexibility can be imparted while maintaining higher smoothness.
• the binder composition for producing a green sheet according to the sixth aspect is the polyvinyl alcohol resin (C1) with a nonionic polyvinyl alcohol resin (C11) having a saponification degree of 85 mol% or more and 99 mol% or less.
• the polyvinyl alcohol resin (C11) since the polyvinyl alcohol resin (C11) has a larger proportion of hydroxyl groups than the polyvinyl alcohol resin (C12), it can contribute to the improvement of the strength of the sheet produced from the slurry composition for firing. Further, since the polyvinyl alcohol resin (C21) has a carboxyl group, the contribution to the improvement of the strength of the sheet is further large. On the other hand, the polyvinyl alcohol resin (C12) can contribute to the improvement of the flexibility of the sheet. Therefore, it is possible to impart even better strength and flexibility to the sheets produced from the binder composition (X) and the slurry composition (Y).
• the binder composition for producing a green sheet according to the seventh aspect is a nonionic polyvinyl alcohol resin (C12) having a saponification degree of 85 mol% or more and 99 mol% or less as the polyvinyl alcohol resin (C1) in the fifth aspect.
• the polyvinyl alcohol resin (C12) contains an anionic polyvinyl alcohol resin (C211) having a saponification degree of 60 mol% or more and less than 85 mol% and having a carboxyl group.
• the sheet prepared from the binder composition (X) and the slurry composition (Y) It can contribute to the improvement of strength.
• the polyvinyl alcohol resin (C21) has a smaller proportion of hydroxyl groups than the polyvinyl alcohol resin (C5), it has a carboxyl group, so that it contributes to the improvement of strength while maintaining the high flexibility of the sheet. Can be done. Therefore, it is possible to impart even better strength and flexibility to the sheet produced from the binder composition and the slurry composition for firing.
• the baking slurry composition of the eighth aspect contains the binder composition according to any one of the first to eighth aspects, the inorganic powder (B), and water.
• the baking slurry composition has high storage stability.
• the amount of the binder composition of the baking slurry composition in the ninth aspect is 5 parts by mass or more and 20 parts by mass or less with respect to 100 parts by mass of the inorganic powder (B).
• the ninth aspect in producing the sheet, it is possible to impart good strength and flexibility to the sheet while maintaining the higher smoothness of the sheet.
• the method for producing the tenth green sheet includes applying the baking slurry composition of the ninth or tenth aspect and drying it.
• a green sheet having high smoothness and good strength and flexibility can be obtained.
• the method for producing a sintered body according to the eleventh aspect includes firing the green sheet obtained by the method for producing a green sheet according to the tenth aspect.
• the eleventh aspect since the above-mentioned green sheet has high smoothness and flexibility, it is possible to easily make a thin film even if it is laminated in multiple layers when manufacturing a multilayer ceramic capacitor from the green sheet. ..
• the tenth method of manufacturing a multilayer ceramic capacitor includes firing a laminated body in which a plurality of green sheets obtained by the method of manufacturing a green sheet of the tenth aspect are stacked.
• the thin film can be easily thinned even if it is laminated in multiple layers.

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• 2019
  • 2019-03-13 WO PCT/JP2019/010212 patent/WO2020183636A1/ja not_active Ceased
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