JP5702311B2 - セラミックグリーンシート用スラリー組成物、セラミックグリーンシート及び積層セラミックコンデンサ - Google Patents
セラミックグリーンシート用スラリー組成物、セラミックグリーンシート及び積層セラミックコンデンサ Download PDFInfo
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- JP5702311B2 JP5702311B2 JP2011551705A JP2011551705A JP5702311B2 JP 5702311 B2 JP5702311 B2 JP 5702311B2 JP 2011551705 A JP2011551705 A JP 2011551705A JP 2011551705 A JP2011551705 A JP 2011551705A JP 5702311 B2 JP5702311 B2 JP 5702311B2
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- green sheet
- ceramic green
- slurry composition
- resin
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- 239000000919 ceramic Substances 0.000 title claims description 94
- 239000002002 slurry Substances 0.000 title claims description 44
- 239000000203 mixture Substances 0.000 title claims description 43
- 239000003985 ceramic capacitor Substances 0.000 title claims description 12
- 229920005989 resin Polymers 0.000 claims description 54
- 239000011347 resin Substances 0.000 claims description 54
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- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 46
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 35
- 239000011354 acetal resin Substances 0.000 claims description 34
- 238000006116 polymerization reaction Methods 0.000 claims description 34
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- 229920001567 vinyl ester resin Polymers 0.000 claims description 26
- 150000002148 esters Chemical group 0.000 claims description 24
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical group OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 13
- 238000006359 acetalization reaction Methods 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 125000003172 aldehyde group Chemical group 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 4
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- 238000007127 saponification reaction Methods 0.000 description 22
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
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- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 6
- 239000010409 thin film Substances 0.000 description 6
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- 239000003377 acid catalyst Substances 0.000 description 5
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 5
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- SAOKZLXYCUGLFA-UHFFFAOYSA-N bis(2-ethylhexyl) adipate Chemical compound CCCCC(CC)COC(=O)CCCCC(=O)OCC(CC)CCCC SAOKZLXYCUGLFA-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
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- 230000035882 stress Effects 0.000 description 4
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- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- 239000001431 2-methylbenzaldehyde Substances 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
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- 239000003054 catalyst Substances 0.000 description 3
- 239000012461 cellulose resin Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 230000000379 polymerizing effect Effects 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- IAVREABSGIHHMO-UHFFFAOYSA-N 3-hydroxybenzaldehyde Chemical compound OC1=CC=CC(C=O)=C1 IAVREABSGIHHMO-UHFFFAOYSA-N 0.000 description 2
- YGCZTXZTJXYWCO-UHFFFAOYSA-N 3-phenylpropanal Chemical compound O=CCCC1=CC=CC=C1 YGCZTXZTJXYWCO-UHFFFAOYSA-N 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- RGHHSNMVTDWUBI-UHFFFAOYSA-N 4-hydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1 RGHHSNMVTDWUBI-UHFFFAOYSA-N 0.000 description 2
- IRIAEXORFWYRCZ-UHFFFAOYSA-N Butylbenzyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCC1=CC=CC=C1 IRIAEXORFWYRCZ-UHFFFAOYSA-N 0.000 description 2
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 description 2
- KCXZNSGUUQJJTR-UHFFFAOYSA-N Di-n-hexyl phthalate Chemical compound CCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCC KCXZNSGUUQJJTR-UHFFFAOYSA-N 0.000 description 2
- ZNZYKNKBJPZETN-WELNAUFTSA-N Dialdehyde 11678 Chemical compound N1C2=CC=CC=C2C2=C1[C@H](C[C@H](/C(=C/O)C(=O)OC)[C@@H](C=C)C=O)NCC2 ZNZYKNKBJPZETN-WELNAUFTSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- UUIQMZJEGPQKFD-UHFFFAOYSA-N Methyl butyrate Chemical compound CCCC(=O)OC UUIQMZJEGPQKFD-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000003963 antioxidant agent Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000004132 cross linking Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 238000005238 degreasing Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- OBNCKNCVKJNDBV-UHFFFAOYSA-N ethyl butyrate Chemical compound CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 description 2
- SHZIWNPUGXLXDT-UHFFFAOYSA-N ethyl hexanoate Chemical compound CCCCCC(=O)OCC SHZIWNPUGXLXDT-UHFFFAOYSA-N 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
- 239000010419 fine particle Substances 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- FXHGMKSSBGDXIY-UHFFFAOYSA-N heptanal Chemical compound CCCCCCC=O FXHGMKSSBGDXIY-UHFFFAOYSA-N 0.000 description 2
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 description 2
- JARKCYVAAOWBJS-UHFFFAOYSA-N hexanal Chemical compound CCCCCC=O JARKCYVAAOWBJS-UHFFFAOYSA-N 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 239000003999 initiator Substances 0.000 description 2
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 2
- NUKZAGXMHTUAFE-UHFFFAOYSA-N methyl hexanoate Chemical compound CCCCCC(=O)OC NUKZAGXMHTUAFE-UHFFFAOYSA-N 0.000 description 2
- HNBDRPTVWVGKBR-UHFFFAOYSA-N methyl pentanoate Chemical compound CCCCC(=O)OC HNBDRPTVWVGKBR-UHFFFAOYSA-N 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- BTFQKIATRPGRBS-UHFFFAOYSA-N o-tolualdehyde Chemical compound CC1=CC=CC=C1C=O BTFQKIATRPGRBS-UHFFFAOYSA-N 0.000 description 2
- FXLOVSHXALFLKQ-UHFFFAOYSA-N p-tolualdehyde Chemical compound CC1=CC=C(C=O)C=C1 FXLOVSHXALFLKQ-UHFFFAOYSA-N 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- DTUQWGWMVIHBKE-UHFFFAOYSA-N phenylacetaldehyde Chemical compound O=CCC1=CC=CC=C1 DTUQWGWMVIHBKE-UHFFFAOYSA-N 0.000 description 2
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- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
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- RUMACXVDVNRZJZ-UHFFFAOYSA-N 2-methylpropyl 2-methylprop-2-enoate Chemical compound CC(C)COC(=O)C(C)=C RUMACXVDVNRZJZ-UHFFFAOYSA-N 0.000 description 1
- CFVWNXQPGQOHRJ-UHFFFAOYSA-N 2-methylpropyl prop-2-enoate Chemical compound CC(C)COC(=O)C=C CFVWNXQPGQOHRJ-UHFFFAOYSA-N 0.000 description 1
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- 229910052581 Si3N4 Inorganic materials 0.000 description 1
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- FRQDZJMEHSJOPU-UHFFFAOYSA-N Triethylene glycol bis(2-ethylhexanoate) Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CCCC FRQDZJMEHSJOPU-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
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- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 150000003926 acrylamides Chemical class 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
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- 238000007605 air drying Methods 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
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- OVKDFILSBMEKLT-UHFFFAOYSA-N alpha-Terpineol Natural products CC(=C)C1(O)CCC(C)=CC1 OVKDFILSBMEKLT-UHFFFAOYSA-N 0.000 description 1
- 229940088601 alpha-terpineol Drugs 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
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Classifications
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- 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
- C04B35/16—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 silicates other than clay
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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
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- 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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- C04B35/626—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
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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
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- 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
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- C04B35/634—Polymers
- C04B35/63404—Polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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- 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
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- 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
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/48—Isomerisation; Cyclisation
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- 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
- C04B2235/3231—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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- C04B2235/54—Particle size related information
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- General Chemical & Material Sciences (AREA)
- Compositions Of Macromolecular Compounds (AREA)
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Description
JIS K6728に記載の方法に基づき測定した。
JIS K6728に記載の方法に基づき測定した。
(ポリビニルアセタール樹脂の調製)
還流冷却器、温度計およびイカリ型攪拌翼を備えた内容積2リットルのガラス製容器に、イオン交換水1295gと、ポリビニルアルコール(PVA−1:重合度1050、けん化度99.2モル%)105gとを仕込み、全体を98℃に昇温してポリビニルアルコールを完全に溶解させ、ポリビニルアルコール水溶液(濃度7.5質量%)を形成した。形成したポリビニルアルコール水溶液を、回転速度120rpmにて攪拌し続けながら、約30分かけて5℃まで徐々に冷却した後、当該水溶液に、ブチルアルデヒド70g、および、ブチラール化触媒である酸触媒として濃度20質量%の塩酸100mlを添加して、ポリビニルアルコールのブチラール化を開始した。ブチラール化を30分間行った後、120分かけて全体を70℃まで昇温し、70℃にて180分間保持した後に、室温まで冷却した。冷却によって析出した樹脂をろ過した後、イオン交換水(樹脂に対して100倍量のイオン交換水)で複数回洗浄し、中和のために0.3質量%水酸化ナトリウム溶液を加え、70℃で5時間保持した後、遠心脱水し、さらに100倍量のイオン交換水で複数回再洗浄し、脱水したのち、40℃、減圧下で18時間乾燥し、ポリビニルブチラール樹脂(PVB−1)を得た。得られたポリビニルブチラール樹脂(PVB−1)は、ブチラール化度が71.0モル%、ビニルエステル単位の含有量が0.8モル%、ビニルアルコール単位の含有量が28.2モル%であった。
PVA−1に代わって、ポリビニルアルコール(PVA−2:重合度1700、けん化度99.6モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−2)を得た。PVB−2のブチラール化度は69.8モル%、ビニルエステル単位の含有量は0.4モル%、ビニルアルコール単位の含有量は29.8モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−3:重合度2400、けん化度99.9モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−3)を得た。PVB−3のブチラール化度は74.3モル%、ビニルエステル単位の含有量は0.1モル%、ビニルアルコール単位の含有量は25.6モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−4:重合度3500、けん化度99.8モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−4)を得た。PVB−4のブチラール化度は73.2モル%、ビニルエステル単位の含有量は0.2モル%、ビニルアルコール単位の含有量は26.6モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−5:重合度4200、けん化度99.9モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−5)を得た。PVB−5のブチラール化度は69.0モル%、ビニルエステル単位の含有量は0.1モル%、ビニルアルコール単位の含有量は30.9モル%であった。次いで、ポリビニルブチラール樹脂を8質量部、可塑剤であるDOAを8質量部添加した以外は参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−6:重合度1700、けん化度99.95モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−6)を得た。PVB−6のブチラール化度は74.25モル%、ビニルエステル単位の含有量は0.05モル%、ビニルアルコール単位の含有量は25.70モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−7:重合度1700、けん化度99.9モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−7)を得た。PVB−7のブチラール化度は80.6モル%、ビニルエステル単位の含有量は0.1モル%、ビニルアルコール単位の含有量は19.3モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−8:重合度1700、けん化度99.8モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−8)を得た。PVB−8のブチラール化度は65.2モル%、ビニルエステル単位の含有量は0.2モル%、ビニルアルコール単位の含有量は34.6モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−A:重合度850、けん化度99.2モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−A)を得た。PVB−Aのブチラール化度は71.0モル%、ビニルエステル単位の含有量は0.8モル%、ビニルアルコール単位の含有量は28.2モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−B:重合度1700、けん化度99モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−B)を得た。PVB−Bのブチラール化度は70モル%、ビニルエステル単位の含有量は1モル%、ビニルアルコール単位の含有量は29モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−C:重合度3500、けん化度98.5モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−C)を得た。PVB−Cのブチラール化度は71.5モル%、ビニルエステル単位の含有量は1.5モル%、ビニルアルコール単位の含有量は27モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−D:重合度4800、けん化度99.9モル%)を用いた以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−D)を得た。PVB−Dのブチラール化度は71.9モル%、ビニルエステル単位の含有量は0.1モル%、ビニルアルコール単位の含有量は28モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得たが、スラリー粘度が高く、塗工性が悪くグリーンシート中の粒子分散性に斑が見られた。
PVA−1に代わって、ポリビニルアルコール(PVA−E:重合度2400、けん化度99.9モル%)を用い、ブチルアルデヒドと同時にグルタルアルデヒド0.08g添加した以外は参考例1と同様にして、ポリビニルブチラール樹脂(PVB−E)を得た。PVB−Eのブチラール化度は71.9モル%、ビニルエステル単位の含有量は0.1モル%、ビニルアルコール単位の含有量は28モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
PVA−1に代わって、ポリビニルアルコール(PVA−F:重合度1700、けん化度99.5モル%)を用いた以外は比較例5と同様にして、ポリビニルブチラール樹脂(PVB−F)を得た。PVB−Fのブチラール化度は71.0モル%、ビニルエステル単位の含有量は0.5モル%、ビニルアルコール単位の含有量は28.5モル%であった。次いで、参考例1と同様にしてセラミックグリーンシート用スラリー組成物を得た。
(機械的強度の評価)
得られたセラミックグリーンシートをポリエステルフィルムから剥離し、セラミックグリーンシートの状態を観察した。
○:セラミックグリーンシートに切れや破れが観察されなかったもの
×:切れや破れがわずかでも観察されたもの
の2段階で評価した。
ポリエチレンテレフタレートからセラミックグリーンシートを60mm×50mmのサイズで切り出し、20℃で3分放置後、シートの側面を光学顕微鏡で観測した。
○:セラミックスシートの反りが認められないもの
×:セラミックスシートにわずかでも反りが認められるもの
の2段階で評価した。
Claims (3)
- 重合度が1000を超え4500以下であり、ビニルエステル単位の含有量が0.2モル%以下であるポリビニルアルコール樹脂をモノアルデヒドでアセタール化して得られ、2つ以上のアルデヒド基を有する化合物を併用する場合は、ポリビニルアルコール樹脂のビニルアルコール単位に対して0.005モル%より少ない量の2つ以上のアルデヒド基を有する化合物を添加してアセタール化して得られ、アセタール化度が60〜83モル%であるポリビニルアセタール樹脂、セラミック粉末、及び、有機溶剤を含有するセラミックグリーンシート用スラリー組成物。
- 請求項1記載のセラミックグリーンシート用スラリー組成物を用いて得られるセラミックグリーンシートであって、厚さが2μm以下であることを特徴とするセラミックグリーンシート。
- 請求項2記載のセラミックグリーンシートと導電ペーストとを用いて得られることを特徴とする積層セラミックコンデンサ。
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TWI557096B (zh) * | 2011-09-28 | 2016-11-11 | 可樂麗股份有限公司 | 漿料組成物、陶瓷坯片及積層陶瓷電容器 |
JP2014141394A (ja) * | 2012-12-26 | 2014-08-07 | Murata Mfg Co Ltd | セラミックグリーンシートおよびその製造方法 |
JP5900706B2 (ja) * | 2014-02-17 | 2016-04-06 | 株式会社クラレ | セラミック成形用又は導電ペースト用のバインダー、及びそれらの用途 |
WO2017014295A1 (ja) * | 2015-07-22 | 2017-01-26 | 昭栄化学工業株式会社 | 無機粒子分散ペースト用のバインダー樹脂及び無機粒子分散ペースト |
CN109563001A (zh) * | 2016-07-28 | 2019-04-02 | 株式会社可乐丽 | 陶瓷生片和涂覆片 |
JP7498896B2 (ja) * | 2018-12-25 | 2024-06-13 | 住友金属鉱山株式会社 | 導電性ペースト、電子部品、及び積層セラミックコンデンサ |
JP7493946B2 (ja) * | 2019-01-29 | 2024-06-03 | 花王株式会社 | セラミック成形体からの有機物成分の除去方法 |
CN112028625A (zh) * | 2020-07-31 | 2020-12-04 | 深圳陶陶科技有限公司 | 氧化锆陶瓷材料及其制备方法和用途 |
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KR20210148088A (ko) | 2019-03-29 | 2021-12-07 | 세키스이가가쿠 고교가부시키가이샤 | 세라믹 그린 시트용 수지 조성물, 세라믹 그린 시트 및 적층 세라믹 콘덴서 |
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