WO2010113628A1 - スラリー組成物の製造方法 - Google Patents
スラリー組成物の製造方法 Download PDFInfo
- Publication number
- WO2010113628A1 WO2010113628A1 PCT/JP2010/054380 JP2010054380W WO2010113628A1 WO 2010113628 A1 WO2010113628 A1 WO 2010113628A1 JP 2010054380 W JP2010054380 W JP 2010054380W WO 2010113628 A1 WO2010113628 A1 WO 2010113628A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- polyvinyl acetal
- acetal resin
- slurry composition
- resin
- inorganic
- Prior art date
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- 239000002002 slurry Substances 0.000 title claims abstract description 63
- 239000000203 mixture Substances 0.000 title claims abstract description 61
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000011354 acetal resin Substances 0.000 claims abstract description 93
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 93
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 93
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 91
- 239000000843 powder Substances 0.000 claims abstract description 75
- 239000006185 dispersion Substances 0.000 claims abstract description 43
- 239000011347 resin Substances 0.000 claims abstract description 41
- 229920005989 resin Polymers 0.000 claims abstract description 41
- 239000003960 organic solvent Substances 0.000 claims abstract description 35
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 17
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 13
- 125000000129 anionic group Chemical group 0.000 claims description 7
- 239000012046 mixed solvent Substances 0.000 claims description 7
- 238000000034 method Methods 0.000 abstract description 15
- 230000008569 process Effects 0.000 abstract description 7
- 239000000243 solution Substances 0.000 description 30
- 239000000919 ceramic Substances 0.000 description 26
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 10
- 239000004372 Polyvinyl alcohol Substances 0.000 description 10
- 229920002451 polyvinyl alcohol Polymers 0.000 description 10
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 8
- 238000006359 acetalization reaction Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000002270 dispersing agent Substances 0.000 description 8
- 238000011156 evaluation Methods 0.000 description 8
- 239000011230 binding agent Substances 0.000 description 7
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 6
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 6
- 229910002113 barium titanate Inorganic materials 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- -1 thiol compounds Chemical class 0.000 description 6
- 229920001567 vinyl ester resin Polymers 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 4
- 239000003985 ceramic capacitor Substances 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 238000000655 nuclear magnetic resonance spectrum Methods 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 230000003746 surface roughness Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 229910000859 α-Fe Inorganic materials 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 229920001577 copolymer Polymers 0.000 description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 3
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 3
- 239000010408 film Substances 0.000 description 3
- 239000000696 magnetic material Substances 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 229940116411 terpineol Drugs 0.000 description 3
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 3
- 239000004711 α-olefin Substances 0.000 description 3
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 2
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical compound OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 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
- 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
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 229910018605 Ni—Zn Inorganic materials 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-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
- 238000004220 aggregation Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- DUYAAUVXQSMXQP-UHFFFAOYSA-N ethanethioic S-acid Chemical compound CC(S)=O DUYAAUVXQSMXQP-UHFFFAOYSA-N 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
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 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
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 230000001771 impaired effect Effects 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- UODXCYZDMHPIJE-UHFFFAOYSA-N menthanol Chemical compound CC1CCC(C(C)(C)O)CC1 UODXCYZDMHPIJE-UHFFFAOYSA-N 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 125000001434 methanylylidene group Chemical group [H]C#[*] 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
- 239000000075 oxide glass Substances 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 229920000139 polyethylene terephthalate Polymers 0.000 description 2
- 239000005020 polyethylene terephthalate Substances 0.000 description 2
- 238000007127 saponification reaction Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
- HFZLSTDPRQSZCQ-UHFFFAOYSA-N 1-pyrrolidin-3-ylpyrrolidine Chemical compound C1CCCN1C1CNCC1 HFZLSTDPRQSZCQ-UHFFFAOYSA-N 0.000 description 1
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- JAHNSTQSQJOJLO-UHFFFAOYSA-N 2-(3-fluorophenyl)-1h-imidazole Chemical compound FC1=CC=CC(C=2NC=CN=2)=C1 JAHNSTQSQJOJLO-UHFFFAOYSA-N 0.000 description 1
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 description 1
- HBNHCGDYYBMKJN-UHFFFAOYSA-N 2-(4-methylcyclohexyl)propan-2-yl acetate Chemical compound CC1CCC(C(C)(C)OC(C)=O)CC1 HBNHCGDYYBMKJN-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- WOYWLLHHWAMFCB-UHFFFAOYSA-N 2-ethylhexyl acetate Chemical compound CCCCC(CC)COC(C)=O WOYWLLHHWAMFCB-UHFFFAOYSA-N 0.000 description 1
- LFEQNZNCKDNGRM-UHFFFAOYSA-N 2-ethylhexyl butanoate Chemical compound CCCCC(CC)COC(=O)CCC LFEQNZNCKDNGRM-UHFFFAOYSA-N 0.000 description 1
- QENRKQYUEGJNNZ-UHFFFAOYSA-N 2-methyl-1-(prop-2-enoylamino)propane-1-sulfonic acid Chemical compound CC(C)C(S(O)(=O)=O)NC(=O)C=C QENRKQYUEGJNNZ-UHFFFAOYSA-N 0.000 description 1
- PVFYDPMTPBPRQA-UHFFFAOYSA-N 2-methylprop-2-enenitrile;prop-2-enenitrile Chemical compound C=CC#N.CC(=C)C#N PVFYDPMTPBPRQA-UHFFFAOYSA-N 0.000 description 1
- JHUFGBSGINLPOW-UHFFFAOYSA-N 3-chloro-4-(trifluoromethoxy)benzoyl cyanide Chemical compound FC(F)(F)OC1=CC=C(C(=O)C#N)C=C1Cl JHUFGBSGINLPOW-UHFFFAOYSA-N 0.000 description 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- OKJADYKTJJGKDX-UHFFFAOYSA-N Butyl pentanoate Chemical compound CCCCOC(=O)CCCC OKJADYKTJJGKDX-UHFFFAOYSA-N 0.000 description 1
- RPRPDTXKGSIXMD-UHFFFAOYSA-N Caproic acid n-butyl ester Natural products CCCCCC(=O)OCCCC RPRPDTXKGSIXMD-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- ICMAFTSLXCXHRK-UHFFFAOYSA-N Ethyl pentanoate Chemical compound CCCCC(=O)OCC ICMAFTSLXCXHRK-UHFFFAOYSA-N 0.000 description 1
- VQTUBCCKSQIDNK-UHFFFAOYSA-N Isobutene Chemical group CC(C)=C VQTUBCCKSQIDNK-UHFFFAOYSA-N 0.000 description 1
- 229910001289 Manganese-zinc ferrite Inorganic materials 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 description 1
- 229910001053 Nickel-zinc ferrite Inorganic materials 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical group OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Propanedioic acid Natural products OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- 229910052581 Si3N4 Inorganic materials 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- WGLPBDUCMAPZCE-UHFFFAOYSA-N Trioxochromium Chemical compound O=[Cr](=O)=O WGLPBDUCMAPZCE-UHFFFAOYSA-N 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 229910001308 Zinc ferrite Inorganic materials 0.000 description 1
- LZFMACRHJXVTIV-UHFFFAOYSA-N [F].C(=C)Cl Chemical compound [F].C(=C)Cl LZFMACRHJXVTIV-UHFFFAOYSA-N 0.000 description 1
- 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
- JIYIUPFAJUGHNL-UHFFFAOYSA-N [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[O--].[Mn++].[Mn++].[Mn++].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Fe+3].[Zn++].[Zn++] JIYIUPFAJUGHNL-UHFFFAOYSA-N 0.000 description 1
- TXDRMFQQROPOKK-UHFFFAOYSA-N [Si+2]=O.[B+]=O.[O-2].[Zn+2] Chemical compound [Si+2]=O.[B+]=O.[O-2].[Zn+2] TXDRMFQQROPOKK-UHFFFAOYSA-N 0.000 description 1
- 125000004036 acetal group Chemical group 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
- 150000001241 acetals Chemical class 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 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
- 239000002216 antistatic agent Substances 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- INLLPKCGLOXCIV-UHFFFAOYSA-N bromoethene Chemical compound BrC=C INLLPKCGLOXCIV-UHFFFAOYSA-N 0.000 description 1
- 150000001656 butanoic acid esters Chemical class 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 1
- 238000001460 carbon-13 nuclear magnetic resonance spectrum Methods 0.000 description 1
- 229910000423 chromium oxide Inorganic materials 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- TVZPLCNGKSPOJA-UHFFFAOYSA-N copper zinc Chemical compound [Cu].[Zn] TVZPLCNGKSPOJA-UHFFFAOYSA-N 0.000 description 1
- 125000004956 cyclohexylene group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000005238 degreasing Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- BXKDSDJJOVIHMX-UHFFFAOYSA-N edrophonium chloride Chemical compound [Cl-].CC[N+](C)(C)C1=CC=CC(O)=C1 BXKDSDJJOVIHMX-UHFFFAOYSA-N 0.000 description 1
- YCUBDDIKWLELPD-UHFFFAOYSA-N ethenyl 2,2-dimethylpropanoate Chemical compound CC(C)(C)C(=O)OC=C YCUBDDIKWLELPD-UHFFFAOYSA-N 0.000 description 1
- GFJVXXWOPWLRNU-UHFFFAOYSA-N ethenyl formate Chemical compound C=COC=O GFJVXXWOPWLRNU-UHFFFAOYSA-N 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- LDLDYFCCDKENPD-UHFFFAOYSA-N ethenylcyclohexane Chemical group C=CC1CCCCC1 LDLDYFCCDKENPD-UHFFFAOYSA-N 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 239000011976 maleic acid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- FQPSGWSUVKBHSU-UHFFFAOYSA-N methacrylamide Chemical compound CC(=C)C(N)=O FQPSGWSUVKBHSU-UHFFFAOYSA-N 0.000 description 1
- 229940017219 methyl propionate Drugs 0.000 description 1
- LVHBHZANLOWSRM-UHFFFAOYSA-N methylenebutanedioic acid Natural products OC(=O)CC(=C)C(O)=O LVHBHZANLOWSRM-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- AJCDFVKYMIUXCR-UHFFFAOYSA-N oxobarium;oxo(oxoferriooxy)iron Chemical compound [Ba]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O.O=[Fe]O[Fe]=O AJCDFVKYMIUXCR-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- IAHIMVFWYADCJJ-UHFFFAOYSA-N prop-1-enylcyclohexane Chemical group CC=CC1CCCCC1 IAHIMVFWYADCJJ-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000011342 resin composition Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- HBMJWWWQQXIZIP-UHFFFAOYSA-N silicon carbide Chemical compound [Si+]#[C-] HBMJWWWQQXIZIP-UHFFFAOYSA-N 0.000 description 1
- 229910010271 silicon carbide Inorganic materials 0.000 description 1
- HQVNEWCFYHHQES-UHFFFAOYSA-N silicon nitride Chemical compound N12[Si]34N5[Si]62N3[Si]51N64 HQVNEWCFYHHQES-UHFFFAOYSA-N 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- BWYYYTVSBPRQCN-UHFFFAOYSA-M sodium;ethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=C BWYYYTVSBPRQCN-UHFFFAOYSA-M 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
- 125000000383 tetramethylene group Chemical group [H]C([H])([*:1])C([H])([H])C([H])([H])C([H])([H])[*:2] 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
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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
- C04B35/6342—Polyvinylacetals, e.g. polyvinylbutyral [PVB]
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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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- C04B35/26—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
- C04B35/265—Compositions containing one or more ferrites of the group comprising manganese or zinc and one or more ferrites of the group comprising nickel, copper or cobalt
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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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- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/58—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides
- C04B35/581—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on borides, nitrides, i.e. nitrides, oxynitrides, carbonitrides or oxycarbonitrides or silicides based on aluminium nitride
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- 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
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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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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
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- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/09—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in organic liquids
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/08—Metals
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- C08K3/10—Metal compounds
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of 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; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/14—Homopolymers or copolymers of acetals or ketals obtained by polymerisation of unsaturated acetals or ketals or by after-treatment of polymers of unsaturated alcohols
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/22—Conductive material dispersed in non-conductive organic material the conductive material comprising metals or alloys
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- 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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- 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
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- 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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- C04B2235/02—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
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- 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
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- C08J2329/00—Characterised by the use of 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; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
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Definitions
- the present invention relates to a method for producing a slurry composition capable of realizing excellent dispersibility in a simple process. Moreover, it is related with the slurry composition manufactured using the manufacturing method of this slurry composition.
- Polyvinyl acetal resin is excellent in toughness, film-forming properties, inorganic pigments, dispersibility of organic powders, adhesion to coated surfaces, etc. And conductive paste, ink, paint, baking enamel, wash primer, etc.
- a multilayer ceramic capacitor is generally manufactured through the following steps. First, a ceramic raw material powder is added to a binder resin such as a polyvinyl butyral resin and mixed uniformly to obtain a slurry composition. The obtained slurry composition is applied to the support surface subjected to the mold release treatment. This is heated to remove volatile components such as a solvent, and then peeled off from the support to obtain a ceramic green sheet. Next, on the obtained ceramic green sheet, a plurality of sheets of conductive paste containing ethyl cellulose, polyvinyl butyral resin, etc.
- a binder resin such as a polyvinyl butyral resin
- a multilayer ceramic capacitor is obtained through a step of sintering an external electrode on the end face of the fired ceramic product obtained by firing.
- Patent Document 1 As a method of dispersing ceramic powder or the like in a slurry composition, as described in Patent Document 1, an inorganic dispersion composed of an inorganic powder, an organic solvent, etc. is prepared on the one hand, and a binder resin is dissolved on the other hand. A method of mixing the inorganic dispersion and the resin solution after preparing the prepared resin solution is used. However, such a method has a problem that unless the mixed solution is stirred for a long time, the ceramic powder is not sufficiently dispersed, and stirring requires excessive energy and time. As a method for ensuring the dispersibility of the ceramic powder in the slurry composition, as described in Patent Document 2, a method of adding a dispersant is also used. However, in such a method, when the compatibility with the binder resin is poor, there is a problem that the dispersibility is deteriorated or the dispersibility is lowered during long-term storage.
- An object of this invention is to provide the manufacturing method of the slurry composition which can implement
- the present invention relates to a method for producing a slurry composition containing an inorganic powder, a polyvinyl acetal resin and an organic solvent, wherein the inorganic powder, the polyvinyl acetal resin (A) and an organic solvent for inorganic dispersion are added and mixed to form an inorganic dispersion.
- the resin (A) has a degree of polymerization of 200 to 600
- the polyvinyl acetal resin (B) has a degree of polymerization of 800 to 4000
- the polyvinyl acetal resin (A) Is added in an amount of 0.1 to 20 parts by weight per 100 parts by weight of the inorganic powder.
- the inventors prepared an inorganic dispersion composed of inorganic powder, an organic solvent for inorganic dispersion, a dispersant, etc. on the one hand, and prepared a resin solution in which the binder resin was dissolved on the other hand,
- a slurry composition in which a dispersion and a resin solution are mixed, by using a polyvinyl acetal resin as the dispersant, the dispersibility of the inorganic powder can be greatly improved, and a film-like body having high strength
- the inventors have found that a slurry composition can be produced, and have completed the present invention.
- an inorganic powder, a polyvinyl acetal resin (A) and an organic solvent for inorganic dispersion are added and mixed to prepare an inorganic dispersion, and a polyvinyl acetal resin (B) and an organic solvent for a resin solution are added and mixed.
- the polyvinyl acetal resin (A) is used as a dispersant in the step of preparing the inorganic dispersion.
- the polyvinyl acetal resin (A) adheres to the surface of the inorganic powder by using the polyvinyl acetal resin (A) as a dispersant, and as a result, the dispersibility of the inorganic powder is improved. Can be increased. Thereafter, by adding a resin solution containing the polyvinyl acetal resin (B) to the inorganic dispersion, the strength of the sheet obtained, for example, in the case of a green sheet is increased without impairing the dispersibility of the inorganic powder. be able to.
- the inorganic powder After previously mixing and dissolving the polyvinyl acetal resin (A) in the organic solvent for inorganic dispersion.
- the polyvinyl acetal resin (A) is used as a dispersant in the step of preparing the inorganic dispersion.
- the polyvinyl acetal resin (A) and the polyvinyl acetal resin (B) described later are also simply referred to as a polyvinyl acetal resin when it is not necessary to distinguish between them.
- the lower limit of the degree of polymerization of the polyvinyl acetal resin (A) is 200, and the upper limit is 600. If the degree of polymerization is less than 200, it is difficult to obtain industrially and it is not practical. When the degree of polymerization exceeds 600, the cohesive force becomes too high, and it becomes difficult to develop sufficient dispersibility.
- the preferable lower limit of the polymerization degree is 300, and the preferable upper limit is 500.
- the preferable minimum of the amount of hydroxyl groups of the said polyvinyl acetal resin (A) is 28 mol%, and a preferable upper limit is 60 mol%.
- the amount of the hydroxyl group is less than 28 mol%, the polyvinyl acetal resin (A) is less likely to adhere to the surface of the inorganic powder and may not contribute to the improvement of dispersibility. Not only is the synthesis of the acetal resin (A) difficult, but the solubility in the solvent may be reduced.
- a more preferred lower limit of the hydroxyl group content is 35 mol%, and a more preferred upper limit is 55 mol%.
- the more preferable lower limit of the amount of the hydroxyl group is 40 mol%, and the more preferable upper limit is 50 mol%.
- the polyvinyl acetal resin (A) preferably has an anionic group. By having the anionic group, the polyvinyl acetal resin (A) can easily adhere to the surface of the inorganic powder, and the dispersibility of the inorganic powder can be improved.
- the anionic group is not particularly limited as long as it is an anionic modifying group, and examples thereof include a carboxyl group, a sulfonic acid group, and a phosphoric acid group.
- the preferable lower limit of the degree of modification of the anionic group is 0.1 mol%, and the preferable upper limit is 2 mol%.
- the degree of modification of the anionic group is less than 0.1 mol%, the polyvinyl acetal resin (A) is less likely to adhere to the surface of the inorganic powder, and may not contribute to improvement in dispersibility. If it exceeds 1, attractive interaction may work between the polyvinyl acetal resins (A), and it may be difficult to adhere to the surface of the inorganic powder.
- a more preferable lower limit of the degree of modification is 0.2 mol%, and a more preferable upper limit is 1 mol%.
- the degree of modification is determined by dissolving the modified polyvinyl acetal resin in DMSO-d 6 (dimethyl sulfoxide), measuring the 13 C-NMR spectrum, and determining the peak area derived from the methine group to which the carboxy group is bonded. And the peak area derived from the methine group of the acetalized portion.
- DMSO-d 6 dimethyl sulfoxide
- the ratio of the portion acetalized with acetaldehyde and the portion acetalized with butyraldehyde is preferably 20/80 to 70/30.
- the portion acetalized with the acetaldehyde the length of the hydrocarbon group due to the aldehyde is shortened and the steric hindrance is lowered, so that the hydroxyl group is easily adsorbed to the inorganic powder. Therefore, the dispersibility of inorganic powder improves by setting the part acetalized with acetaldehyde to 20/80 or more.
- the portion acetalized with acetaldehyde increases too much, the solubility in the organic solvent for inorganic dispersion decreases, or the molded and dried sheet becomes too hard and cracks are likely to occur. / 30 or less is preferable. More preferably, the ratio of the portion acetalized with acetaldehyde and the portion acetalized with butyraldehyde is 30/70 to 60/40.
- the inorganic powder is not particularly limited, and examples thereof include metal powder, conductive powder, ceramic powder, and glass powder.
- a conductive powder When a conductive powder is used as the inorganic powder, it can be used as a conductive paste.
- the conductive powder is not particularly limited as long as it exhibits sufficient conductivity, and examples thereof include powder made of nickel, palladium, platinum, gold, silver, copper, alloys thereof, and the like. These conductive powders may be used alone or in combination of two or more.
- ceramic powder When ceramic powder is used as the inorganic powder, it can be used as a ceramic paste.
- the ceramic powder is not particularly limited.
- These ceramic powders may be used alone or in combination of two or more.
- glass powder When glass powder is used as the inorganic powder, it can be used as a glass paste.
- the glass powder is not particularly limited.
- lead oxide-boron oxide-silicon oxide-calcium oxide glass zinc oxide-boron oxide-silicon oxide glass, lead oxide-zinc oxide-boron oxide-silicon oxide glass. Etc.
- These glass powders may be used alone or in combination of two or more. Moreover, you may use aluminum oxide etc. together in the range which does not impair the objective of this invention.
- magnese zinc ferrite nickel zinc ferrite, copper zinc ferrite, barium ferrite and strontium ferrite
- metal oxides such as chromium oxide
- metal magnetic materials such as cobalt, amorphous Examples include magnetic materials. These magnetic powders may be used alone or in combination of two or more.
- the lower limit of the amount of the polyvinyl acetal resin (A) added in the step of preparing the inorganic dispersion is 0.1 part by weight with respect to 100 parts by weight of the inorganic powder, and the upper limit is 20 parts by weight.
- the added amount of the polyvinyl acetal resin (A) is less than 0.1 parts by weight, for example, the dispersibility of the inorganic powder may be insufficient, and when it exceeds 20 parts by weight, the viscosity becomes too high. , Handling may be worse.
- the minimum with said preferable addition amount is 0.6 weight part, and a preferable upper limit is 15 weight part. Furthermore, the more preferable minimum of the said addition amount is 1 weight part, and a more preferable upper limit is 10 weight part.
- the polyvinyl acetal resin (A) can be sufficiently adsorbed on the surface of the inorganic powder, so that the inorganic powder in the ceramic slurry is more finely dispersed. It becomes possible.
- the minimum of the polymerization degree of the said polyvinyl acetal resin (B) is 800, and an upper limit is 4000.
- the degree of polymerization is less than 800, the sheet strength is insufficient when used for a green sheet, and when the degree of polymerization exceeds 4000, the slurry composition becomes too viscous and coating becomes difficult.
- the preferable lower limit of the polymerization degree is 1200, and the preferable upper limit is 3500.
- the minimum with the preferable amount of hydroxyl groups of the said polyvinyl acetal resin (B) is 22 mol%, and a preferable upper limit is 42 mol%.
- the amount of the hydroxyl group is less than 22 mol%, when a green sheet is produced using a slurry containing the polyvinyl acetal resin (B), the sheet strength may be insufficient, and exceeds 42 mol%. And may cause aggregation of inorganic powder particles.
- a more preferred lower limit of the hydroxyl group content is 28 mol%, and a more preferred upper limit is 40 mol%.
- the preferable lower limit of the addition amount of the polyvinyl acetal resin (B) in the step of preparing the resin solution is 5 parts by weight with respect to 100 parts by weight of the inorganic powder, and the preferable upper limit is 20 parts by weight.
- the added amount of the polyvinyl acetal resin (B) is less than 5 parts by weight, for example, the dispersibility of the inorganic powder is insufficient, or the strength, flexibility, adhesiveness, etc. of the coating film after drying are insufficient.
- the amount exceeds 20 parts by weight the viscosity may become too high or the coatability may be lowered, resulting in poor handling.
- a sheet having sufficient dispersibility and a sheet can be obtained by containing a polyvinyl acetal resin (B) having a high degree of polymerization relative to a polyvinyl acetal resin (A) having a low degree of polymerization.
- a ceramic green sheet having strength can be produced.
- the polyvinyl acetal resin is obtained by acetalizing polyvinyl alcohol with an aldehyde.
- the polyvinyl alcohol can be obtained, for example, by saponifying a copolymer of vinyl ester and ethylene.
- the vinyl ester include vinyl formate, vinyl acetate, vinyl propionate, vinyl pivalate and the like. Of these, vinyl acetate is preferred from the viewpoint of economy.
- the polyvinyl alcohol may be a copolymer of an ethylenically unsaturated monomer as long as the effects of the present invention are not impaired.
- the ethylenically unsaturated monomer is not particularly limited, and examples thereof include acrylic acid, methacrylic acid, (anhydrous) phthalic acid, (anhydrous) maleic acid, (anhydrous) itaconic acid, acrylonitrile methacrylonitrile, acrylamide, and methacrylamide.
- terminal-modified polyvinyl alcohol obtained by copolymerizing vinyl ester monomer such as vinyl acetate with ethylene in the presence of thiol compounds such as thiol acetic acid and mercaptopropionic acid, and saponifying it. Can do.
- the polyvinyl alcohol may be a saponified copolymer obtained by copolymerizing the vinyl ester and an ⁇ -olefin. Furthermore, it is good also as polyvinyl alcohol which copolymerizes the said ethylenically unsaturated monomer and contains the component originating in an ethylenically unsaturated monomer. Also used is a terminal polyvinyl alcohol obtained by copolymerizing a vinyl ester monomer such as vinyl acetate with an ⁇ -olefin in the presence of a thiol compound such as thiol acetic acid or mercaptopropionic acid, and saponifying it. be able to.
- the ⁇ -olefin is not particularly limited, and examples thereof include methylene, ethylene, propylene, isopropylene, butylene, isobutylene, pentylene, hexylene, cyclohexylene, cyclohexylethylene, and cyclohexylpropylene.
- the polyvinyl acetal resin preferably has an acetalization degree of 40 to 80 mol%.
- the degree of acetalization is less than 40 mol%, the solubility in an organic solvent is lowered, and thus it is difficult to use the slurry composition.
- the degree of acetalization exceeds 80 mol%, it will be difficult to industrially produce a polyvinyl acetal resin.
- it is 50 to 80 mol%.
- the degree of acetalization is the ratio of the number of hydroxyl groups acetalized with butyraldehyde out of the number of hydroxyl groups of polyvinyl alcohol. Since the acetal group is formed by acetalization from two hydroxyl groups, a method of counting the two acetal hydroxyl groups is employed to calculate the mol% of the degree of acetalization.
- a step of adding a resin solution to the inorganic dispersion is then performed. Thereby, a slurry composition is obtained.
- the organic solvent for inorganic dispersion and the organic solvent for resin solution are not particularly limited, and organic solvents generally used in slurry compositions can be used.
- organic solvents generally used in slurry compositions can be used.
- acetone, methyl ethyl ketone, dipropyl ketone, diisobutyl ketone Ketones such as methanol, ethanol, isopropanol, butanol, aromatic hydrocarbons such as toluene, xylene, methyl propionate, ethyl propionate, butyl propionate, methyl butanoate, ethyl butanoate, butanoic acid Esters such as butyl, methyl pentanoate, ethyl pentanoate, butyl pentanoate, methyl hexanoate, ethyl hexanoate, butyl hexanoate, 2-ethylhexyl acetate,
- the organic solvent for inorganic dispersion and the organic solvent for resin solution it is particularly preferable to use a mixed solvent composed of ethanol and toluene.
- the mixed solvent By using the mixed solvent, the dispersibility of the slurry composition can be greatly improved. This is because ethanol contributes to the prevention of aggregation of the polyvinyl acetal resin (B), while toluene contributes to the adhesion of the polyvinyl acetal resin (A) to the inorganic powder surface. This is probably because the dispersibility is greatly improved.
- the mixing ratio of ethanol and toluene is preferably 5: 5 to 2: 8. By setting it within the above range, the dispersibility of the slurry composition can be greatly improved.
- the preferable lower limit of the amount of the inorganic dispersion organic solvent added in the step of preparing the inorganic dispersion is 20 parts by weight with respect to 100 parts by weight of the inorganic powder, and the preferable upper limit is 60 parts by weight.
- the added amount of the organic solvent for inorganic dispersion is less than 20 parts by weight, the viscosity of the dispersion becomes high, the movement of the ceramic powder is restricted, and sufficient dispersibility may not be obtained, and the amount exceeds 60 parts by weight.
- the ceramic powder concentration of the dispersion liquid is lowered and the number of collisions between the ceramic powders is reduced, sufficient dispersibility may not be obtained.
- the preferable minimum of the addition amount of the said organic solvent for resin solutions in the process of producing the said resin solution is 70 weight part with respect to 100 weight part of inorganic powder, and a preferable upper limit is 130 weight part.
- the addition amount of the organic solvent for the resin solution is less than 70 parts by weight, it may be difficult to adjust to a desired viscosity, and the coatability may be deteriorated. The sheet after drying may not be uniform.
- a plasticizer, a lubricant, an antistatic agent, and the like may be appropriately added as long as the effects of the present invention are not impaired.
- a slurry composition of the present invention By using the method for producing a slurry composition of the present invention, an extremely high dispersibility can be realized, and a slurry composition having a high strength can be produced. Such a slurry composition is also one aspect of the present invention.
- the manufacturing method of the slurry composition which can implement
- the slurry composition manufactured using the manufacturing method of this slurry composition can be provided.
- polyvinyl acetal resin (A1) The obtained polyvinyl acetal resin was dissolved in DMSO-d 6 (dimethyl sulfoxide), and the degree of butyralization was measured using 13 C-NMR (nuclear magnetic resonance spectrum). The degree of butyralization was 51 mol%. there were.
- Polyvinyl acetal resins (A2) to (A11) were synthesized in the same manner as the polyvinyl acetal resin (A1) except that the conditions shown in Table 1 were used.
- polyvinyl acetal resin (B1) was obtained through neutralization, water washing, and drying by a conventional method.
- the obtained polyvinyl acetal resin was dissolved in DMSO-d 6 (dimethyl sulfoxide), and the degree of butyralization was measured using 13 C-NMR (nuclear magnetic resonance spectrum). The degree of butyralization was 66 mol%. there were.
- Polyvinyl acetal resins (B2) to (B6) were synthesized in the same manner as the polyvinyl acetal resin (B1) except that the conditions shown in Table 2 were used.
- Example 1 Preparation of inorganic dispersion 1 part by weight of the obtained polyvinyl acetal resin (A1) was added to a mixed solvent of 20 parts by weight of toluene and 20 parts by weight of ethanol and dissolved by stirring. Next, 100 parts by weight of barium titanate powder (manufactured by Sakai Chemical Industry Co., Ltd., BT02) was added to the obtained solution, and the mixture was stirred for 180 minutes in a bead mill (IMEX ready mill), whereby the inorganic dispersion was Produced.
- barium titanate powder manufactured by Sakai Chemical Industry Co., Ltd., BT02
- Example 2 to 20 A slurry composition was obtained in the same manner as in Example 1 except that the polyvinyl acetal resin (A), the polyvinyl acetal resin (B), and the organic solvent shown in Table 3 were used.
- Example 21 In place of barium titanate as the inorganic powder, slurry was used in the same manner as in Example 1 except that aluminum nitride powder was used and the polyvinyl acetal resin (A), polyvinyl acetal resin (B) and organic solvent shown in Table 3 were used. A composition was obtained.
- Example 24 In place of barium titanate as the inorganic powder, Ni—Zn ferrite powder was used, and the same procedure as in Example 1 was used except that the polyvinyl acetal resin (A), polyvinyl acetal resin (B) and organic solvent shown in Table 3 were used. Thus, a slurry composition was obtained.
- Example 5 As shown in Table 4, a slurry composition was obtained in the same manner as in Example 1 except that the polyvinyl acetal resin (A) was not added to the inorganic dispersion but dissolved in the resin solution together with the polyvinyl acetal resin (B). It was.
- Example 6 A slurry composition was obtained in the same manner as in Example 1 except that the polyvinyl acetal resin (B) shown in Table 4 was used.
- Example 7 A slurry composition was obtained in the same manner as in Example 1 except that the addition amount of the polyvinyl acetal resin (A) was as shown in Table 4.
- Example 9 A slurry composition was obtained in the same manner as in Example 1, except that “Hypermer KD-2” (manufactured by Croda, polyamine compound having a side chain grafted with hydrocarbon) was used instead of the polyvinyl acetal resin (A). It was.
- “Hypermer KD-2” manufactured by Croda, polyamine compound having a side chain grafted with hydrocarbon
- Example 11 Example except that Ni-Zn ferrite powder was used instead of barium titanate as the inorganic powder, the polyvinyl acetal resin (B) and the organic solvent shown in Table 4 were used without adding the polyvinyl acetal resin (A). In the same manner as in No. 1, a slurry composition was obtained.
- Dispersibility evaluation Preparation of dispersibility evaluation solution
- a mixed solvent 5 parts by weight of ethanol and 5 parts by weight of toluene
- an ultrasonic disperser US-303 manufactured by SND
- a dispersion evaluation solution was prepared.
- the obtained dispersion evaluation solution was subjected to particle size distribution measurement using a laser diffraction particle size distribution analyzer (LA-910, manufactured by Horiba, Ltd.), and the position of the maximum particle size peak and the average particle size were measured.
- the manufacturing method of the slurry composition which can implement
- the slurry composition manufactured using the manufacturing method of this slurry composition can be provided.
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Abstract
Description
まず、ポリビニルブチラール樹脂等のバインダー樹脂にセラミック原料粉末を加え、均一に混合することでスラリー組成物を得る。得られたスラリー組成物を、離型処理した支持体面に塗工する。これに加熱等を行うことで溶剤等の揮発分を溜去させた後、支持体から剥離してセラミックグリーンシートを得る。次いで、得られたセラミックグリーンシート上に、エチルセルロース、ポリビニルブチラール樹脂等をバインダー樹脂として含有する導電ペーストをスクリーン印刷等により塗布したものを交互に複数枚積み重ね、加熱圧着して積層体を作製し、脱脂処理を行った後、焼成して得られるセラミック焼成物の端面に外部電極を焼結する工程を経て積層セラミックコンデンサが得られる。
しかしながら、このような方法では、混合液を長時間に渡って撹拌しなければ、セラミック粉末が充分に分散せず、撹拌に過大なエネルギーや時間を要するという問題があった。
また、スラリー組成物中のセラミック粉末の分散性を確保する方法として、特許文献2に記載されているように、分散剤を添加する方法も用いられている。しかしながら、このような方法では、バインダー樹脂との相溶性が悪いと逆に分散性を悪化させたり、長期保存時に分散性が低下したりする問題があった。
以下、本発明につき詳細に説明する。
本発明では、上記無機分散液を作製する工程において、ポリビニルアセタール樹脂(A)を分散剤として用いる。このように無機分散液を作製する工程において、ポリビニルアセタール樹脂(A)を分散剤として用いることで、ポリビニルアセタール樹脂(A)が無機粉末の表面に付着し、その結果、無機粉末の分散性を高めることができる。その後、無機分散液に、ポリビニルアセタール樹脂(B)を含有する樹脂溶液を添加することで無機粉末の分散性を損なうことなく、例えば、グリーンシートにした場合等において得られるシートの強度を高くすることができる。
なお、本明細書において、ポリビニルアセタール樹脂(A)と、後述するポリビニルアセタール樹脂(B)とを特に区別する必要がない場合は、単にポリビニルアセタール樹脂ともいう。
上記アニオン性基を有することで、ポリビニルアセタール樹脂(A)が無機粉末の表面に付着しやすくなり、無機粉末の分散性を高めることができる。
上記アニオン性基の変性度が0.1モル%未満であると、無機粉末の表面に上記ポリビニルアセタール樹脂(A)が付着しにくくなり、分散性の向上に寄与しないことがあり、2モル%を超えると、上記ポリビニルアセタール樹脂(A)同士に引力相互作用が働き、無機粉末の表面に付着しにくくなることがある。上記変性度のより好ましい下限は0.2モル%であり、より好ましい上限は1モル%である。
なお、上記変性度は、変性ポリビニルアセタール樹脂をDMSO-d6(ジメチルスルホキサイド)に溶解させて、13C―NMRスペクトルを測定し、カルボキシ基が結合しているメチン基に由来するピーク面積と、アセタール化された部分のメチン基に由来するピーク面積とにより算出することができる。
上記導電粉末としては充分な導電性を示すものであれば特に限定されず、例えば、ニッケル、パラジウム、白金、金、銀、銅、これらの合金等からなる粉末が挙げられる。これらの導電粉末は、単独で用いてもよく、2種以上を併用してもよい。
特に強度の求められる薄層のセラミックグリーンシートにおいては、重合度の低いポリビニルアセタール樹脂(A)に対して、重合度の高いポリビニルアセタール樹脂(B)を含有することで、充分な分散性とシート強度を有するセラミックグリーンシートを作製することができる。
なお、本明細書において、アセタール化度とは、ポリビニルアルコールの水酸基数のうち、ブチルアルデヒドでアセタール化された水酸基数の割合のことであり、アセタール化度の計算方法としては、ポリビニルアセタール樹脂のアセタール基が2個の水酸基からアセタール化されて形成されていることから、アセタール化された2個の水酸基を数える方法を採用してアセタール化度のモル%を算出する。
これにより、スラリー組成物が得られる。
また、上記樹脂溶液を作製する工程における上記樹脂溶液用有機溶剤の添加量の好ましい下限は無機粉末100重量部に対して70重量部、好ましい上限は130重量部である。上記樹脂溶液用有機溶剤の添加量が70重量部未満であると、所望の粘度に調整することが困難になり、塗工性が低下することがあり、130重量部を超えると、セラミック粉末濃度が低くなり、乾燥後のシートが一様にならないことがある。
重合度320、ケン化度99モル%のポリビニルアルコール350重量部を純水3000重量部に加え、90℃の温度で約2時間攪拌し溶解させた。この溶液を40℃に冷却し、これに濃度35重量%の塩酸230重量部とn-ブチルアルデヒド150重量部とを添加し、液温を1℃に下げてこの温度を保持してアセタール化反応を行い、反応生成物を析出させた。その後、液温を20℃、3時間保持して反応を完了させ、常法により中和、水洗及び乾燥を経て、ポリビニルアセタール樹脂(A1)の白色粉末を得た。得られたポリビニルアセタール樹脂をDMSO-d6(ジメチルスルホキサイド)に溶解し、13C-NMR(核磁気共鳴スペクトル)を用いてブチラール化度を測定したところ、ブチラール化度は51モル%であった。
また、表1に示す条件とした以外は、ポリビニルアセタール樹脂(A1)と同様にして、ポリビニルアセタール樹脂(A2)~(A11)を合成した。
重合度1700、ケン化度99モル%のポリビニルアルコール280重量部を純水3000重量部に加え、90℃の温度で約2時間攪拌し溶解させた。この溶液を40℃に冷却し、これに濃度35重量%の塩酸200重量部とn-ブチルアルデヒド155重量部とを添加し、液温を1℃に下げてこの温度を保持してアセタール化反応を行い、反応生成物を析出させた。その後、液温を40℃、3時間保持して反応を完了させ、常法により中和、水洗及び乾燥を経て、ポリビニルアセタール樹脂(B1)の白色粉末を得た。得られたポリビニルアセタール樹脂をDMSO-d6(ジメチルスルホキサイド)に溶解し、13C-NMR(核磁気共鳴スペクトル)を用いてブチラール化度を測定したところ、ブチラール化度は66モル%であった。
また、表2に示す条件とした以外は、ポリビニルアセタール樹脂(B1)と同様にして、ポリビニルアセタール樹脂(B2)~(B6)を合成した。
(無機分散液の作製)
得られたポリビニルアセタール樹脂(A1)1重量部を、トルエン20重量部とエタノール20重量部との混合溶剤に加え、攪拌溶解した。次いで、100重量部のチタン酸バリウムの粉末(堺化学工業社製、BT02)を得られた溶液に添加し、ビーズミル(アイメックス社製 レディーミル)にて180分間撹拌することにより、無機分散液を作製した。
得られたポリビニルアセタール樹脂(B1)8重量部、DOP2重量部を、エタノール45重量部とトルエン45重量部との混合溶剤に加え、攪拌溶解することにより、樹脂溶液を作製した。
得られた無機分散液に樹脂溶液を添加しビーズミルにて90分間攪拌することにより、スラリー組成物を得た。
表3に示すポリビニルアセタール樹脂(A)、ポリビニルアセタール樹脂(B)、及び、有機溶剤を用いた以外は実施例1と同様にして、スラリー組成物を得た。
無機粉末としてチタン酸バリウムに代えて、窒化アルミニウム粉を用い、表3に示すポリビニルアセタール樹脂(A)、ポリビニルアセタール樹脂(B)及び有機溶剤を用いた以外は実施例1と同様にして、スラリー組成物を得た。
無機粉末としてチタン酸バリウムに代えて、Ni-Zn系フェライト粉を用い、表3に示すポリビニルアセタール樹脂(A)、ポリビニルアセタール樹脂(B)及び有機溶剤を用いた以外は実施例1と同様にして、スラリー組成物を得た。
ポリビニルアセタール樹脂(A)を添加せず、表4に示すポリビニルアセタール樹脂(B)及び有機溶剤を用いた以外は実施例1と同様にして、スラリー組成物を得た。
表4に示すように、ポリビニルアセタール樹脂(A)を無機分散液に添加せず、ポリビニルアセタール樹脂(B)とともに樹脂溶液に溶解させた以外は実施例1と同様にして、スラリー組成物を得た。
表4に示すポリビニルアセタール樹脂(B)を用いた以外は実施例1と同様にして、スラリー組成物を得た。
ポリビニルアセタール樹脂(A)の添加量を表4に示す通りにした以外は実施例1と同様にして、スラリー組成物を得た。
ポリビニルアセタール樹脂(A)を表4に示す通りにした以外は実施例1と同様にして、スラリー組成物を得た。
ポリビニルアセタール樹脂(A)に代えて、「Hypermer KD-2」(クローダ社製、側鎖に炭化水素をグラフトしたポリアミン化合物)を用いた以外は実施例1と同様にして、スラリー組成物を得た。
無機粉末としてチタン酸バリウムに代えて、窒化アルミニウム粉を用い、ポリビニルアセタール樹脂(A)を添加せず、表4に示すポリビニルアセタール樹脂(B)及び有機溶剤を用いた以外は実施例1と同様にして、スラリー組成物を得た。
無機粉末としてチタン酸バリウムに代えて、Ni-Zn系フェライト粉を用い、ポリビニルアセタール樹脂(A)を添加せず、表4に示すポリビニルアセタール樹脂(B)及び有機溶剤を用いた以外は実施例1と同様にして、スラリー組成物を得た。
得られたスラリー組成物について、以下の評価を行った。
(グリーンシートの作製)
離型処理されたポリエチレンテレフタレート(PET)フィルム上に、得られたスラリー組成物を乾燥後の膜厚が20μmとなるように塗工、乾燥してセラミックグリーンシートを作製した。
得られたセラミックグリーンシートについて、JIS B 0601(1994)に基づいて表面粗さRaを測定し、セラミックスラリーの表面粗さを評価した。一般に、スラリー組成物の分散性が高いほど、セラミックグリーンシートの表面粗さは小さくなる。
JIS K 7113に準拠して、TENSILON(島津製作所社製、AUTOGRAPH AGS-J)を用い、引張速度20mm/分の条件にて引張弾性率(MPa)の測定を行った。
(分散性評価溶液の作製)
得られたスラリー組成物0.1重量部を、エタノール5重量部とトルエン5重量部の混合溶剤に添加し、超音波分散機(エスエヌディ社製 US-303)にて10分間撹拌することにより、分散評価用溶液を作製した。
(分散性評価)
得られた分散評価用溶液について、レーザー回折式粒度分布計(堀場製作所社製、LA-910)を用いて粒度分布測定を行い、最大粒子径ピークの位置、及び、平均粒子径を測定した。
Claims (6)
- 無機粉末、ポリビニルアセタール樹脂及び有機溶剤を含有するスラリー組成物の製造方法であって、
無機粉末、ポリビニルアセタール樹脂(A)及び無機分散用有機溶剤を添加、混合して無機分散液を作製する工程、ポリビニルアセタール樹脂(B)及び樹脂溶液用有機溶剤を添加、混合して樹脂溶液を作製する工程、及び、前記無機分散液に樹脂溶液を添加する工程を有し、
前記ポリビニルアセタール樹脂(A)は、重合度が200~600、
前記ポリビニルアセタール樹脂(B)は、重合度が800~4000であり、かつ、
前記無機分散液を作製する工程において、前記ポリビニルアセタール樹脂(A)を無機粉末100重量部に対して0.1~20重量部添加する
ことを特徴とするスラリー組成物の製造方法。 - ポリビニルアセタール樹脂(A)は、アニオン性基を有することを特徴とする請求項1記載のスラリー組成物の製造方法。
- ポリビニルアセタール樹脂(A)は、水酸基量が28~60モル%であることを特徴とする請求項1又は2記載のスラリー組成物の製造方法。
- ポリビニルアセタール樹脂(B)は、水酸基量が22~42モル%であることを特徴とする請求項1記載のスラリー組成物の製造方法。
- 無機分散用有機溶剤及び樹脂溶液用有機溶剤は、エタノール及びトルエンからなる混合溶媒であることを特徴とする請求項1、2、3又は4記載のスラリー組成物の製造方法。
- 請求項1、2、3、4又は5記載のスラリー組成物の製造方法を用いて製造されることを特徴とするスラリー組成物。
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EP10758404.7A EP2415731B1 (en) | 2009-03-31 | 2010-03-16 | Method for producing slurry composition |
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