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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
  • C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
  • C04B35/63488—Polyethers, e.g. alkylphenol polyglycolether, polyethylene glycol [PEG], polyethylene oxide [PEO]
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  • C04B35/634—Polymers
  • C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
  • C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B32—LAYERED PRODUCTS
  • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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  • 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
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  • C04B35/111—Fine ceramics
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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
  • C04B35/46—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 titanium oxides or titanates
  • C04B35/462—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 titanium oxides or titanates based on titanates
  • C04B35/465—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates
  • C04B35/468—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates
  • C04B35/4682—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 titanium oxides or titanates based on titanates based on alkaline earth metal titanates based on barium titanates based on BaTiO3 perovskite phase
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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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  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C43/00—Ethers; Compounds having groups, groups or groups
  • C07C43/02—Ethers
  • C07C43/03—Ethers having all ether-oxygen atoms bound to acyclic carbon atoms
  • C07C43/04—Saturated ethers
  • C07C43/10—Saturated ethers of polyhydroxy compounds
• • 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
  • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
• • 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
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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
  • C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
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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
  • C04B2235/3231—Refractory metal oxides, their mixed metal oxides, or oxide-forming salts thereof
  • C04B2235/3232—Titanium oxides or titanates, e.g. rutile or anatase
  • C04B2235/3234—Titanates, not containing zirconia
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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
  • C04B2235/50—Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
  • C04B2235/54—Particle size related information
  • C04B2235/5418—Particle size related information expressed by the size of the particles or aggregates thereof
  • C04B2235/5427—Particle size related information expressed by the size of the particles or aggregates thereof millimeter or submillimeter sized, i.e. larger than 0,1 mm
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  • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
  • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
  • C04B2237/32—Ceramic
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  • C04B2237/00—Aspects relating to ceramic laminates or to joining of ceramic articles with other articles by heating
  • C04B2237/30—Composition of layers of ceramic laminates or of ceramic or metallic articles to be joined by heating, e.g. Si substrates
  • C04B2237/32—Ceramic
  • C04B2237/34—Oxidic
  • C04B2237/345—Refractory metal oxides
  • C04B2237/346—Titania or titanates
• • H—ELECTRICITY
  • H01—ELECTRIC ELEMENTS
  • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
  • H01G13/00—Apparatus specially adapted for manufacturing capacitors; Processes specially adapted for manufacturing capacitors not provided for in groups H01G4/00 - H01G11/00
• • 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
  • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
  • H01G4/1218—Ceramic dielectrics characterised by the ceramic dielectric material based on titanium oxides or titanates
• • 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
  • H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
  • H01G4/1236—Ceramic dielectrics characterised by the ceramic dielectric material based on zirconium oxides or zirconates

Definitions

• the present invention relates to a laminating aid used in a step of laminating ceramic green sheets, and a ceramic green sheet composition containing the laminating aid. More specifically, it contains a laminating aid that can suppress peeling and laminating misalignment between ceramic green sheets with a small amount of addition, as well as a decrease in sheet strength and an increase in residue during firing, and this laminating aid.
• the ceramic green sheet composition to be used.
• Electronic components such as laminated ceramic capacitors (MLCCs) and laminated chip inductors are mainly manufactured by a method of laminating green sheets made of ceramics such as barium titanate and ferrite and binder resin.
• the miniaturization and large capacity can be realized by making the ceramic green sheet and the conductive layer, which are the components thereof, thin and multi-layered.
• a binder having high strength is often selected, and for example, polyvinyl butyral is widely used.
• high-strength binders have higher hardness than conventional binders, and the adhesiveness between sheets tends to be lower than that of conventional products. If the adhesiveness is lowered, interlayer peeling may occur in the green sheet laminating step or thermocompression bonding step, resulting in defects.
• Patent Document 1 discloses a method of suppressing peeling between layers without lowering the strength of the resin by combining polyvinyl butyral and a specific plasticizer.
• an object of the present invention is to suppress peeling between ceramic green sheets and misalignment of layers without reducing sheet strength.
• the present inventors have conducted extensive studies to solve the above problems, and as a result, found that a polyether compound having a specific structure can solve the above problems.
• a ceramic green sheet laminating aid comprising a compound represented by the formula (1).
• (1) Z represents a residue having a carbon number of 1 to 22 and having 1 to 6 hydroxyl groups removed from all hydroxyl groups
• x indicates a number from 1 to 6 AO represents an oxyalkylene group having 2 to 4 carbon atoms.
• n represents a number from 5 to 500 xxn is in the range of 5 to 500
• the weight ratio of the oxyethylene group EO contained in the oxyalkylene group AO having 2 to 4 carbon atoms is 0 to 80% by weight.
• the lamination aid of the present invention is a polyether compound represented by the following formula (1).
• Z in the formula (1) is a residue having all the hydroxyl groups removed from an alcohol compound having 1 to 22 carbon atoms and having 1 to 6 hydroxyl groups. That is, the alcohol compound is represented by (Z(OH)x), and Z is the residue obtained by removing all (OH) from the alcohol compound.
• the alcohol compound include methanol, ethanol, n-butanol, n-octanol, 2-ethylhexanol, 3,5,5-trimethylhexanol, dodecanol, octadecanol, behenyl alcohol, ethylene glycol, propylene glycol, butylene glycol, pentane.
• the carbon number of z is preferably 2 or more, more preferably 10 or less, and particularly preferably 5 or less.
• X in the formula (1) is the number of AO chains bonded to Z, and corresponds to the number of hydroxyl groups of the alcohol (Z(OH)x).
• x is 1 to 6, preferably 1 to 5, more preferably 1 to 4, and most preferably 1 to 3.
• the lamination aid may have a high viscosity and the handling property may be deteriorated.
• AO in the formula (1) is an oxyalkylene group having 2 to 4 carbon atoms, and is specifically obtained by addition polymerization of ethylene oxide, propylene oxide, and butylene oxide.
• alkylene oxides ethylene oxide and propylene oxide are preferably used, and propylene oxide is most preferably used, from the viewpoint of suppressing stacking deviation.
• these 1 type(s) or 2 or more types can be combined.
• the order may be block-shaped or random-shaped regardless of the order, but the random-shaped is preferable from the viewpoint that the strength of the ceramic green sheet does not easily decrease.
• N indicates the average number of added moles of AO, and when there are two or more types of AO, it is the total average number of added moles of each AO, and indicates a number of 5 to 500.
• the average number of added moles [xxn] of all AOs included in the formula (1) is 5 to 500.
• the xxn is preferably 25 to 500, more preferably 10 to 450, still more preferably 25 to 450, particularly preferably 30 to 450, particularly preferably 50 to 400, and most preferably 50. ⁇ 200. If x ⁇ n is less than 5, peeling between the ceramic green sheets and misalignment may not be sufficiently suppressed, or the sheet strength may be reduced. When [xxn] exceeds 500, the viscosity of the laminating aid is high and the handleability is poor.
• the lamination aid of the present invention may contain an oxyethylene group (EO) from the viewpoint of improving the solubility with the resin, but the weight ratio of EO contained in AO [EO weight/AO weight ⁇ 100] is 80. Weight% is the upper limit.
• the weight ratio of EO contained in AO is preferably 0 to 60% by weight, more preferably 0 to 50% by weight. When the weight ratio of EO contained in AO exceeds 80% by weight, the solubility in the resin becomes high, but the strength may decrease.
• the molecular weight of the lamination aid of the present invention can be measured using a gel permeation chromatograph, and the preferred molecular weight is 500 to 35,000, more preferably 2,000 to 35,000, still more preferably 2,500 to 30. 1,000, more preferably 3,000 to 25,000, and most preferably 3,000 to 10,000.
• the molecular weight exceeds 35,000, the polyether compound represented by the formula (1) has a high viscosity, which tends to deteriorate the handleability and the solvent solubility.
• peeling between the ceramic green sheets and stacking deviation may not be sufficiently suppressed, or the sheet strength may be reduced.
• the ceramic green sheet composition of the present invention contains 0.01 to 5% by mass of a lamination aid (component (A)), 1 to 25% by mass of polyvinyl butyral (component (B)), and ceramic powder (component (C)). Contains 70 to 98% by mass. However, the total amount of the component (A), the component (B) and the component (C) is 100% by weight.
• the content of the laminating aid of the present invention is 0.01 to 5% by mass, preferably 0.05 to 3% by mass, and more preferably 0.1 to 2% by mass.
• the content of the laminating aid is less than 0.01% by mass, peeling and slippage of the green sheet cannot be sufficiently suppressed.
• the content of the laminating aid exceeds 5% by mass, the strength of the green sheet may be insufficient.
• the polyvinyl butyral (component (B)) in the ceramic green sheet composition is not limited as long as it is generally used for a green sheet, but polyvinyl butyral having a large molecular weight tends to have insufficient adhesiveness.
• the weight average molecular weight of polyvinyl butyral is preferably 500,000 or less, more preferably 300,000 or less, and particularly preferably 200,000 or less. Further, since the strength is required by thinning the green sheet, the weight average molecular weight of polyvinyl butyral is preferably 50,000 or more, and more preferably 100,000 or more.
• the content of polyvinyl butyral is 1 to 25% by mass, preferably 1 to 15% by mass, and particularly preferably 3 to 10% by mass.
• the ceramic powder (component (C)) in the ceramic green sheet composition is not limited as long as it is generally used for a green sheet, and is not limited to silicate minerals, other silicic acid compounds, carbonate compounds, and sulfuric acid compounds. Powders such as, hydroxide compounds, oxide compounds, nitride compounds, carbon compounds, and titanate compounds can be used. For example, kaolin, clay, talc, mica, bentonite, dolomite, calcium silicate, aluminum silicate, magnesium silicate, calcium carbonate, magnesium carbonate, barium carbonate, calcium sulfate, barium sulfate, aluminum sulfate, aluminum hydroxide, and hydroxide.
• the ceramic powder is preferably powder of an oxide compound such as zirconium oxide, magnesium oxide, aluminum oxide, iron oxide, zinc oxide, indium tin oxide, powder of a titanate compound such as barium titanate, calcium titanate, strontium titanate.
• the body is more preferable, and powder of a titanic acid compound is more preferable, and barium titanate is particularly preferable.
• the average particle size of the ceramic powder is not particularly limited, but as the green sheet becomes thinner, the ceramic powder having a smaller average particle size tends to be used. From this viewpoint, it is preferably combined with a ceramic powder having an average particle diameter of 300 nm or less, and more preferably combined with a ceramic powder having an average particle diameter of 50 to 200 nm or less.
• the average particle size of the dispersion can be measured by an electron microscopy method using an SEM (scanning electron microscope) or a TEM (transmission electron microscope) or a microtrack method (laser diffraction / scattering method).
• the content of the ceramic powder is 70 to 98% by mass, preferably 80 to 95% by mass, more preferably 85 to 95% by mass.
• the ceramic green sheet composition may contain other ceramic additives, plasticizers, dispersants, antistatic agents, etc. as common components in addition to the above-mentioned compound.
• the plasticizer by combining the plasticizer with the laminating aid of the present invention, it is possible to effectively prevent interlayer peeling and laminating misalignment.
• the amount of the plasticizer when the total amount of the components (A), (B) and (C) is 100 parts by mass, the amount of the plasticizer is preferably 0.01 to 20 parts by mass, and 0.1 to 20 parts by mass. It is more preferably 10 parts by mass.
• the dispersant a polymer having a polar group such as a hydroxyl group, a carboxyl group, a polyether group or an amino group in a side chain can be generally used, and a polymer having both a polyether group and a carboxyl group is preferable.
• An example is a polymer of vinyl ether having a polyoxyalkylene group and maleic anhydride.
• the amount of the dispersant is preferably 0.01 to 20 parts by mass when the total amount of the components (A), (B) and (C) is 100 parts by mass. It is more preferably 0.1 to 10 parts by mass.
• a solvent can be added to the composition.
• a solvent examples include ketone-based agents such as acetone and methyl ethyl ketone, alcohol-based agents such as ethanol and isopropanol, and aromatic-based agents such as toluene and xylene. These may be used alone, or two or more kinds may be used in combination, and it is preferable to use an alcohol type and an aromatic type together.
• the amount of the solvent is preferably 20 to 500 parts by mass, and 50 to 300 parts by mass. It is more preferable to use a part.
• the lamination aids 1 to 7 and the comparative products 1 and 2 having the compositions shown in Table 1 were used as the lamination aid.
• the addition forms of EO and PO of the lamination aids 3 and 4 are random, and the addition forms of EO and PO of the lamination aids 6 and 7 are blocks in the order of EO-PO.
• the obtained slurry was applied on a PET film at a molding speed of 1.5 m/min using a doctor blade coater.
• the blade groove was 140 ⁇ m
• the PET film had a thickness of 32 ⁇ m.
• the applied slurry was dried at 40° C., 60° C., 75° C., 85° C., and 85° C. for 10 minutes each to obtain a target ceramic green sheet.
• a test piece having a width of 3 cm and a length of 10 cm was prepared using each green sheet described in the table.
• the tensile strength [N/mm 2 ] of each test piece was measured using MODEL 9502B manufactured by AIKOH. The results were evaluated based on the following criteria. ⁇ : 16.0 [N/mm 2 ] or more ⁇ : 15.0 to 16.0 [N/mm 2 ] ⁇ : Less than 15.0 [N / mm 2 ]
• Comparative Examples 1 and 5 since the weight ratio of EO contained in AO was out of the range of the present invention, a sufficient coefficient of static friction could not be obtained and the sheet strength was also lowered.
• Comparative Example 2 since the weight ratio of EO contained in AO was out of the range of the present invention, sufficient adhesive strength and static friction coefficient could not be obtained.
• Comparative Examples 3 and 4 since the laminating aid was not contained, the adhesive strength and the coefficient of static friction were insufficient.

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• 2020
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