TWI522402B - A method for producing a slurry composition - Google Patents
A method for producing a slurry composition Download PDFInfo
- Publication number
- TWI522402B TWI522402B TW100133587A TW100133587A TWI522402B TW I522402 B TWI522402 B TW I522402B TW 100133587 A TW100133587 A TW 100133587A TW 100133587 A TW100133587 A TW 100133587A TW I522402 B TWI522402 B TW I522402B
- Authority
- TW
- Taiwan
- Prior art keywords
- polyvinyl acetal
- acetal resin
- slurry composition
- resin
- weight
- Prior art date
Links
- 239000000203 mixture Substances 0.000 title claims description 70
- 239000002002 slurry Substances 0.000 title claims description 68
- 238000004519 manufacturing process Methods 0.000 title claims description 27
- 239000011354 acetal resin Substances 0.000 claims description 168
- 229920006324 polyoxymethylene Polymers 0.000 claims description 168
- 229920002554 vinyl polymer Polymers 0.000 claims description 165
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 164
- 239000000843 powder Substances 0.000 claims description 100
- 239000006185 dispersion Substances 0.000 claims description 60
- 239000011347 resin Substances 0.000 claims description 46
- 229920005989 resin Polymers 0.000 claims description 46
- 239000003960 organic solvent Substances 0.000 claims description 33
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 32
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 29
- 238000006116 polymerization reaction Methods 0.000 claims description 21
- 239000012046 mixed solvent Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 9
- -1 polyethylene Polymers 0.000 claims description 9
- 125000000129 anionic group Chemical group 0.000 claims description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005977 Ethylene Substances 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 239000000919 ceramic Substances 0.000 description 31
- 239000007788 liquid Substances 0.000 description 22
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 18
- 238000000034 method Methods 0.000 description 17
- 238000011156 evaluation Methods 0.000 description 15
- 239000004372 Polyvinyl alcohol Substances 0.000 description 11
- 238000006359 acetalization reaction Methods 0.000 description 11
- 239000002270 dispersing agent Substances 0.000 description 11
- 229920002451 polyvinyl alcohol Polymers 0.000 description 11
- 239000002245 particle Substances 0.000 description 10
- 230000003746 surface roughness Effects 0.000 description 10
- 239000011230 binding agent Substances 0.000 description 9
- 239000011521 glass Substances 0.000 description 8
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 7
- 229910002113 barium titanate Inorganic materials 0.000 description 7
- 239000003985 ceramic capacitor Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 238000005481 NMR spectroscopy Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000001035 drying Methods 0.000 description 6
- 239000000178 monomer Substances 0.000 description 6
- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 6
- 229920001567 vinyl ester resin Polymers 0.000 description 5
- DIIIISSCIXVANO-UHFFFAOYSA-N 1,2-Dimethylhydrazine Chemical compound CNNC DIIIISSCIXVANO-UHFFFAOYSA-N 0.000 description 4
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 4
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 4
- 230000002776 aggregation Effects 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229920000139 polyethylene terephthalate Polymers 0.000 description 4
- 239000005020 polyethylene terephthalate Substances 0.000 description 4
- 238000003756 stirring Methods 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
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 3
- 238000004220 aggregation Methods 0.000 description 3
- 150000001299 aldehydes Chemical class 0.000 description 3
- 150000008064 anhydrides Chemical class 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 3
- 230000006872 improvement Effects 0.000 description 3
- 239000006247 magnetic powder Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000006386 neutralization reaction Methods 0.000 description 3
- 238000007127 saponification reaction Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- 229910000859 α-Fe Inorganic materials 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
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-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
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 229910052796 boron Inorganic materials 0.000 description 2
- XUPYJHCZDLZNFP-UHFFFAOYSA-N butyl butanoate Chemical compound CCCCOC(=O)CCC XUPYJHCZDLZNFP-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 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
- 238000010438 heat treatment Methods 0.000 description 2
- 150000002430 hydrocarbons Chemical group 0.000 description 2
- 229910001867 inorganic solvent Inorganic materials 0.000 description 2
- 239000003049 inorganic solvent Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- UODXCYZDMHPIJE-UHFFFAOYSA-N menthanol Chemical compound CC1CCC(C(C)(C)O)CC1 UODXCYZDMHPIJE-UHFFFAOYSA-N 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
- 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 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 239000000049 pigment Substances 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
- 238000001556 precipitation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- KOUKXHPPRFNWPP-UHFFFAOYSA-N pyrazine-2,5-dicarboxylic acid;hydrate Chemical compound O.OC(=O)C1=CN=C(C(O)=O)C=N1 KOUKXHPPRFNWPP-UHFFFAOYSA-N 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
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- HNAGHMKIPMKKBB-UHFFFAOYSA-N 1-benzylpyrrolidine-3-carboxamide Chemical compound C1C(C(=O)N)CCN1CC1=CC=CC=C1 HNAGHMKIPMKKBB-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
- ZSDQQJHSRVEGTJ-UHFFFAOYSA-N 2-(6-amino-1h-indol-3-yl)acetonitrile Chemical compound NC1=CC=C2C(CC#N)=CNC2=C1 ZSDQQJHSRVEGTJ-UHFFFAOYSA-N 0.000 description 1
- PTTPXKJBFFKCEK-UHFFFAOYSA-N 2-Methyl-4-heptanone Chemical compound CC(C)CC(=O)CC(C)C PTTPXKJBFFKCEK-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
- AUZRCMMVHXRSGT-UHFFFAOYSA-N 2-methylpropane-1-sulfonic acid;prop-2-enamide Chemical compound NC(=O)C=C.CC(C)CS(O)(=O)=O AUZRCMMVHXRSGT-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
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 1
- OQLZINXFSUDMHM-UHFFFAOYSA-N Acetamidine Chemical compound CC(N)=N OQLZINXFSUDMHM-UHFFFAOYSA-N 0.000 description 1
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- 229920000178 Acrylic resin Polymers 0.000 description 1
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 1
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- 239000004215 Carbon black (E152) Substances 0.000 description 1
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- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
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- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 239000000696 magnetic material 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
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- 229910052763 palladium Inorganic materials 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
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- 229910052697 platinum Inorganic materials 0.000 description 1
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- 238000002360 preparation method Methods 0.000 description 1
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- IAHIMVFWYADCJJ-UHFFFAOYSA-N prop-1-enylcyclohexane Chemical group CC=CC1CCCCC1 IAHIMVFWYADCJJ-UHFFFAOYSA-N 0.000 description 1
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- 239000004332 silver Substances 0.000 description 1
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- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 229910003468 tantalcarbide Inorganic materials 0.000 description 1
- MZLGASXMSKOWSE-UHFFFAOYSA-N tantalum nitride Chemical compound [Ta]#N MZLGASXMSKOWSE-UHFFFAOYSA-N 0.000 description 1
- 229940116411 terpineol Drugs 0.000 description 1
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 description 1
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- 239000011701 zinc Substances 0.000 description 1
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- 239000011787 zinc oxide Substances 0.000 description 1
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Description
本發明係關於一種可以簡單之方法製造可藉由簡單之步驟而實現優異之分散性,且能長期維持較高之分散性之漿料組成物的製造方法。又,係關於一種利用該漿料組成物之製造方法而製造之漿料組成物。
因為聚乙烯縮醛樹脂強韌性、成膜性、顏料等無機、有機粉體等之分散性、對塗佈面之接著性等優異,故應用於例如構成積層陶瓷電容器之陶瓷生片(green sheet)或導電膏、油墨、塗料、燒繪用琺瑯、伐鏽底漆(wash primer)等之用途。
其中,積層陶瓷電容器通常係經由如下之步驟製造。
首先,藉由於聚乙烯丁醛樹脂等黏合樹脂中添加陶瓷原料粉末,均勻地混合,而獲得漿料組成物。將所獲得之漿料組成物塗敷於經脫模處理之支持體面。藉由使其加熱等而餾去溶劑等揮發成分後,自支持體剝離,獲得陶瓷生片。接著,將藉由網板印刷等於所獲得之陶瓷生片上塗佈含有乙基纖維素、聚乙烯丁醛樹脂等作為黏合樹脂之導電膏者交替堆積數片,進行加熱壓接來製作積層體,於實施脫脂處理後,經由於進行煅燒獲得之陶瓷煅燒物之端面燒結外部電極之步驟,從而獲得積層陶瓷電容器。
近年來,積層陶瓷電容器要求進一步之小型化或高電容化,對進一步之多層化、薄膜化進行研究,於該種之積層陶瓷電容器中,隨著陶瓷生片之薄膜化之發展,要求所使用之陶瓷粉末之粒徑亦較小。
通常,作為使陶瓷粉末等分散於漿料組成物中之方法,如專利文獻1所揭示,使用一方面製備由無機粉末、有機溶劑等構成之無機分散液,另一方面於製備使黏合樹脂溶解之樹脂溶液後,混合無機分散液與樹脂溶液之方法。
然而,該種之方法中,有若不長時間攪拌混合液,則陶瓷粉末無法充分地分散,有攪拌需要過多之能量或時間之問題。
又,確保漿料組成物中之陶瓷粉末之分散性之方法,如專利文獻2所揭示,亦使用添加有分散劑之方法。然而,該種之方法中,有若與黏合樹脂之相容性較差,則反而使分散性惡化之問題。
進而,於積層陶瓷電容器之製造時,於製作陶瓷漿料組成物後,有至塗敷為止設定有數天之保管期間之情形,若長期性之漿料之分散穩定性不充分,則由於分散性下降,產生陶瓷生片之強度下降、或表面之凹凸變大,而使所獲得之積層陶瓷電容器之電氣特性下降之問題。
專利文獻1:日本特開2005-139034號公報
專利文獻2:日本特開平6-325971號公報
鑒於上述現狀,本發明之目的在於提供一種可以簡單之步驟實現優異之分散性,且能長期維持較高之分散性之漿料組成物的製造方法。又,目的在於提供一種利用該漿料組成物之製造方法而製造之漿料組成物。
本發明之漿料組成物之製造方法,係製造含有無機粉末、聚乙烯縮醛樹脂及有機溶劑之漿料組成物,具有以下步驟:添加無機粉末、混合聚乙烯縮醛樹脂(A)及無機分散用有機溶劑並加以混合以製作無機分散液之步驟,添加聚乙烯縮醛樹脂(B)及樹脂溶液用有機溶劑並加以混合以製作樹脂溶液之步驟,及於上述無機分散液中添加樹脂溶液之步驟;上述混合聚乙烯縮醛樹脂(A)含有羥基量為20~40莫耳%之聚乙烯縮醛樹脂(a1)與羥基量為28~60莫耳%之聚乙烯縮醛樹脂(a2),且上述聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)具有下述(1)式之關係;
Y-X≧5 (1)
式(1)中,X表示聚乙烯縮醛樹脂(a1)之羥基量(莫耳%),Y表示聚乙烯縮醛樹脂(a2)之羥基量(莫耳%);上述聚乙烯縮醛樹脂(B)之聚合度為800~4200,於製作上述無機分散液之步驟中,相對於無機粉末100重量份,添加上述混合聚乙烯縮醛樹脂(A)0.1~20重量份。
以下詳細地對本發明進行說明。
本發明者進行潛心研究,結果發現一方面製備由無機粉末、無機分散用有機溶劑、分散劑等構成之無機分散液,另一方面於製備使黏合樹脂溶解之樹脂溶液後,混合無機分散液與樹脂溶液之漿料組成物之製造方法中,用作分散劑之聚乙烯縮醛樹脂,藉由使用羥基量不同且具有特定之關係之混合聚乙烯縮醛樹脂,可製造可大幅改善無機粉末之分散性,並能長期維持較高之分散性之漿料組成物,從而完成本發明。
於本發明中,具有:添加無機粉末、混合聚乙烯縮醛樹脂(A)及無機分散用有機溶劑並加以混合以製作無機分散液之步驟,添加聚乙烯縮醛樹脂(B)及樹脂溶液用有機溶劑並加以混合以製作樹脂溶液之步驟,及於上述無機分散液添加樹脂溶液之步驟。
於本發明中,於製作上述無機分散液之步驟中,使用混合聚乙烯縮醛樹脂(A)作為分散劑。於如此製作無機分散液之步驟中,使用混合聚乙烯縮醛樹脂(A)作為分散劑,藉此混合聚乙烯縮醛樹脂(A)附著於無機粉末之表面上,其結果,可提昇無機粉末之分散性。其後,即便於無機分散液添加含有聚乙烯縮醛樹脂(B)之樹脂溶液,亦由於之前附著之混合聚乙烯縮醛樹脂(A)之空間位阻,聚乙烯縮醛樹脂(B)不吸附於無機粉末,故而亦不會損及無機粉末之分散性,例如於製成生片時等,可提昇所獲得之片之強度。
因此,就不會抑制混合聚乙烯縮醛樹脂(A)之優異之分散性,亦表現出聚乙烯縮醛樹脂(B)所具有之高強度而言,可製作兼具無機粉末之優異之分散性、及獲得具有較高強度之膜狀體之效果的漿料組成物。
相對於此,於同時添加混合聚乙烯縮醛樹脂(A)與聚乙烯縮醛樹脂(B)之情形時,聚乙烯縮醛樹脂(B)附著於無機粉末之表面,其結果,由於引起無機粉末之凝聚,故而無機粉末之分散性大幅下降。
於製作上述無機分散液之步驟中,較佳為預先使混合聚乙烯縮醛樹脂(A)混合溶解於無機分散用有機溶劑後,添加無機粉末。
再者,上述混合聚乙烯縮醛樹脂(A)可使用預先混合者,亦可於無機粉末之添加時進行混合。
於本發明中,於製作無機分散液之步驟中,使用混合聚乙烯縮醛樹脂(A)作為分散劑。於本發明,使用與黏合樹脂同種之混合聚乙烯縮醛樹脂(A)作為分散劑,藉此無須如先前般考慮因分散劑添加而引起之不良影響。其原因在於分散劑與黏合樹脂為同種,故而相容性良好,分散劑與黏合樹脂可不分離而混雜在一起。
再者,於本說明書中,於無須特別區分混合聚乙烯縮醛樹脂(A)與下述之聚乙烯縮醛樹脂(B)之情形時,亦可僅稱作聚乙烯縮醛樹脂。
於本發明中,混合聚乙烯縮醛樹脂(A)之特徵在於具有聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)之不同性質之聚乙烯縮醛樹脂。
由於上述2種聚乙烯縮醛樹脂分別具有較易分解無機粉末之凝聚體之性質、及較易附著於無機粉末表面之性質,故而藉由該等之相乘效果,可飛躍性地改善無機粉末之分散性。
又,於本發明,就結果而言,無機分散液只要成為含有包含聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)之混合聚乙烯縮醛樹脂(A)者即可。因此,可同時添加聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)來製成混合聚乙烯縮醛樹脂(A),亦可藉由分別添加聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)來製成混合聚乙烯縮醛樹脂(A)。
再者,藉由分別添加聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2),而變得更易明顯地表現出各自之效果。
上述混合聚乙烯縮醛樹脂(A)含有聚乙烯縮醛樹脂(a1)。藉由含有上述聚乙烯縮醛樹脂(a1),使聚乙烯縮醛樹脂(a1)更迅速地滲透至無機粉末表面,變得較易分解無機粉末之凝聚體。
上述聚乙烯縮醛樹脂(a1)之羥基量之下限為20莫耳%,上限為40莫耳%。若上述羥基量未達20莫耳%,則對無機粉末表面之親和性變得幾乎消失,不會附著於無機粉末表面上,無助於分散性之提昇,若超過40莫耳%,則對無機粉末表面之附著變得過剩,僅附著於無機粉末凝集體之表面上,變得較難分解。上述羥基量之較佳之下限為26莫耳%,較佳之上限為38莫耳%。
上述聚乙烯縮醛樹脂(a1)之聚合度之較佳之下限為20,較佳之上限為450。若上述聚合度未達20,則有於工業方面變得不易取得之情形。若上述聚合度超過450,則有由於聚乙烯縮醛樹脂(a1)本身之較大體積,變得不易滲透至無機粉末表面之情形。上述聚合度之更佳之下限為100,更佳之上限為300。
上述混合聚乙烯縮醛樹脂(A)含有聚乙烯縮醛樹脂(a2)。藉由含有上述聚乙烯縮醛樹脂(a2),使聚乙烯縮醛樹脂(a2)更強地附著於無機粉末表面,故而能夠長期保存穩定。
上述聚乙烯縮醛樹脂(a2)之羥基量之下限為28莫耳%,上限為60莫耳%。若上述羥基量未達28莫耳%,則對無機粉末表面之親和性不足,附著量不足,無助於分散性之提昇,若超過60莫耳%,則有對溶劑之溶解性變得不充分,分子無法充分地擴展,變得無法附著於無機粉末之表面之情形。上述羥基量之較佳之下限為42莫耳%,較佳之上限為55莫耳%。
上述聚乙烯縮醛樹脂(a2)之聚合度之較佳之下限為200,較佳之上限為600。若上述聚合度未達200,則有體積高度不足,變得較難適度地保持無機粉末間之距離之情形。若上述聚合度超過600,則有凝聚力變得過高,變得較難表現出充分之分散性之情形。上述聚合度之更佳之下限為320,更佳之上限為450。
較佳為上述聚乙烯縮醛樹脂(a2)具有陰離子性基。
藉由具有上述陰離子性基,使聚乙烯縮醛樹脂(a2)變得較易附著於無機粉末之表面,可提昇無機粉末之分散性。
上述陰離子性基,只要為陰離子性之改質基,則並無特別限定,例如可列舉:羧基、磺酸基、磷酸基等。
上述陰離子性基之改質度之較佳之下限為0.1莫耳%,較佳之上限為2莫耳%。
若上述陰離子性基之改質度未達0.1莫耳%,則有上述聚乙烯縮醛樹脂(a2)變得不易附著於無機粉末之表面,無助於分散性之提昇之情形,若超過2莫耳%,則有上述聚乙烯縮醛樹脂(a2)彼此發揮引力相互作用,變得不易附著於無機粉末之表面之情形。上述改質度之更佳之下限為0.2莫耳%,更佳之上限為1莫耳%。
再者,使聚乙烯縮醛樹脂(a2)溶解於DMSO-d6(二甲亞碸),測定13C-NMR光譜,可根據來自羧基鍵結之次甲基之尖峰面積、及來自經縮醛化之部分之次甲基之尖峰面積而算出上述改質度。
構成上述混合聚乙烯縮醛樹脂(A)之聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)具有下述(1)式之關係。
Y-X≧5 (1)
式(1)中,X表示聚乙烯縮醛樹脂(a1)之羥基量(莫耳%),Y表示聚乙烯縮醛樹脂(a2)之羥基量(莫耳%)。
藉由上述聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)具有上述之關係,而產生對無機粉末表面之附著力之差,不僅有效地分解無機粉末之凝聚體,亦可保持其狀態。
較佳為構成上述混合聚乙烯縮醛樹脂(A)之聚乙烯縮醛樹脂(a1)及聚乙烯縮醛樹脂(a2)之混合比(莫耳比)為2:8~8:2。藉由設為上述範圍內,可充分地發揮聚乙烯縮醛樹脂(a1)及聚乙烯縮醛樹脂(a2)之效果。
較佳為構成上述混合聚乙烯縮醛樹脂(A)之聚乙烯縮醛樹脂(a1)及聚乙烯縮醛樹脂(a2)以乙醛進行縮醛化之部分與以丁醛進行縮醛化的部分之比例為30/70~95/5。上述以乙醛進行縮醛化之部分由於起因於醛之烴基之長度變短、空間位阻下降,故而有羥基變得較易吸附於無機粉末之情形。因此,藉由將以乙醛進行縮醛化之部分設為30/70以上,而使無機粉末之分散性提昇,且可長期維持較高之分散性。更佳為以乙醛進行縮醛化之部分與以丁醛進行縮醛化之部分之比例為40/60~80/20。
上述無機粉末,並無特別限定,例如可列舉:金屬粉體、導電粉末、陶瓷粉末、玻璃粉末等。
於使用導電粉末作為上述無機粉末之情形時,可用作導電糊(paste)。
上述導電粉末,只要為表現出充分之導電性者,則並無特別限定,例如可列舉:由鎳、鈀、鉑、金、銀、銅、該等之合金等構成之粉末。該等之導電粉末可單獨使用,亦可併用2種以上。
於使用陶瓷粉末作為上述無機粉末之情形時,可用作陶瓷糊。上述陶瓷粉末,並無特別限定,例如可列舉:由氧化鋁、氧化鋯、矽酸鋁、氧化鈦、氧化鋅、鈦酸鋇、氧化鎂、賽隆(sialon)、尖晶岩(spinellite)、碳化矽、氮化矽、氮化鋁等構成之粉末。其中,較佳為由與所使用之陶瓷生片所含之陶瓷粉末相同之成分構成。該等之陶瓷粉末可單獨使用,亦可併用2種以上。
於使用玻璃粉末作為上述無機粉末之情形時,可用作玻璃糊。上述玻璃粉末,並無特別限定,例如可列舉:氧化鉛-氧化硼-氧化矽-氧化鈣系玻璃、氧化鋅-氧化硼-氧化矽系玻璃、氧化鉛-氧化鋅-氧化硼-氧化矽系玻璃等。該等之玻璃粉末可單獨使用,亦可併用2種以上。又,於不損及本發明之目的之範圍內,亦可併用氧化鋁等。
於使用磁性粉末作為上述無機粉末之情形時,可用作磁性材料糊。上述磁性粉末,並無特別限定,例如可列舉:錳鋅鐵氧體、鎳鋅鐵氧體、銅鋅鐵氧體、鋇鐵氧體、鍶鐵氧體等鐵氧體類,氧化鉻等金屬氧化物,鈷等金屬磁體,非晶磁體等。
該等之磁性粉末可單獨使用,亦可併用2種以上。
製作上述無機分散液之步驟中上述混合聚乙烯縮醛樹脂(A)的添加量之下限相對於無機粉末100重量份為0.1重量份,上限為20重量份。若上述混合聚乙烯縮醛樹脂(A)之添加量未達0.1重量份,則有例如無機粉末之分散性變得不充分之情形,若超過20重量份,則有黏度變得過高、操作性變差之情形。上述添加量之較佳之下限為0.6重量份,較佳之上限為15重量份。進而上述添加量之更佳之下限為1重量份,更佳之上限為10重量份。尤其藉由將上述添加量設為0.6重量份以上,可使混合聚乙烯縮醛樹脂(A)充分地吸附於無機粉末之表面,故而可使陶瓷漿料中之無機粉末更細微地分散。
較佳為於製作上述無機分散液之步驟中,上述無機分散液之水分量未達3重量%。若上述無機分散液之水分量為3重量%以上,則有無法長期維持較高之分散性之情形。較佳為未達1重量%。
於本發明中,接著實施添加聚乙烯縮醛樹脂(B)及樹脂溶液用有機溶劑並進行混合而製作樹脂溶液之步驟。
於本發明中,如此製作樹脂溶液,於後步驟中實施於無機分散液添加上述樹脂溶液之步驟,藉此防止無機粉末之凝聚,從而可使無機粉末更細微地分散。
相對於此,不使聚乙烯縮醛樹脂(B)溶解於樹脂溶液用有機溶劑中時,即,不製作上述樹脂溶液時,上述聚乙烯縮醛樹脂(B)之體積變大,並變得較易摻入複數種無機粉末,故而引起無機粉末之凝聚。
上述聚乙烯縮醛樹脂(B)之聚合度之下限為800,上限為4200。若上述聚合度未達800,則於用於生片之情形時,薄片強度變得不充分,若上述聚合度超過4200,則漿料組成物之黏度變得過高,變得較難塗敷。上述聚合度之較佳之下限為1200,較佳之上限為3500。
上述聚乙烯縮醛樹脂(B)之羥基量之較佳之下限為22莫耳%,較佳之上限為42莫耳%。若上述羥基量未達22莫耳%,則有於使用含有該聚乙烯縮醛樹脂之漿料製作生片之情形時,薄片強度變得不充分之情形,若超過42莫耳%,則有引起無機粉末粒子之凝聚之情形。上述羥基量之更佳之下限為28莫耳%,更佳之上限為40莫耳%。
製作上述樹脂溶液之步驟中之上述聚乙烯縮醛樹脂(B)的添加量之較佳之下限相對於無機粉末100重量份為5重量份,較佳之上限為20重量份。若上述聚乙烯縮醛樹脂(B)之添加量未達5重量份,則有例如無機粉末之分散性變得不充分,或乾燥後之塗膜之強度、柔軟性及接著性等變得不充分之情形,若超過20重量份,則有黏度變得過高、或塗敷性下降,而使操作性變差之情形。
於尤其要求強度之薄層之陶瓷生片中,藉由相對於聚合度較低之混合聚乙烯縮醛樹脂(A),含有聚合度較高之聚乙烯縮醛樹脂(B),可製作具有充分之分散性與薄片強度之陶瓷生片。
上述聚乙烯縮醛樹脂係以醛使聚乙烯醇縮醛化而成者。
上述聚乙烯醇例如可藉由使乙烯酯與乙烯之共聚物皂化而獲得。上述乙烯酯,例如可列舉:甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、三甲基乙酸乙烯酯等。其中,就經濟性之觀點而言,乙酸乙烯酯較為適合。
於不損及本發明之效果之範圍內,上述聚乙烯醇亦可為使乙烯性不飽和單體進行共聚合者。上述乙烯性不飽和單體,並無特別限定,例如可列舉:丙烯酸、甲基丙烯酸、鄰苯二甲酸(酐)、順丁烯二酸(酐)、衣康酸(酐)、丙烯腈、甲基丙烯腈、丙烯醯胺、甲基丙烯醯胺、三甲基-(3-丙烯醯胺-3-二甲基丙基)-氯化銨、丙烯醯胺-2-甲基丙磺酸、及其鈉鹽、乙基乙烯醚、丁基乙烯醚、N-乙烯基吡咯啶酮、氯乙烯、溴乙烯、氟乙烯、偏二氯乙烯、偏二氟乙烯、四氟乙烯、乙烯基磺酸鈉、烯丙基磺酸鈉等。又,亦可使用藉由於硫代乙酸、巰基丙酸等硫醇化合物之存在下,使乙酸乙烯酯等乙烯酯系單體與乙烯共聚合,使其皂化而獲得之末端改質聚乙烯醇。
上述聚乙烯醇亦可為使上述乙烯酯與α-烯烴共聚合之共聚物皂化者。又,亦可進而使上述乙烯性不飽和單體共聚合,製成含有來自乙烯性不飽和單體之成分之聚乙烯醇。又,亦可使用於硫代乙酸、巰基丙酸等硫醇化合物之存在下,使乙酸乙烯酯等乙烯酯系單體與α-烯烴共聚合,使其皂化而獲得之末端聚乙烯醇。上述α-烯烴,並無特別限定,例如可列舉:亞甲基、乙烯、丙烯、異丙烯、丁烯、異丁烯、戊烯、伸己基、伸環己基、環己基乙烯、環己基丙烯等。
較佳為上述聚乙烯縮醛樹脂之縮醛化度為40~80莫耳%。若上述縮醛化度未達40莫耳%,則對有機溶劑之溶解性下降,故而變得較難用於漿料組成物。若上述縮醛化度超過80莫耳%,則變得較難於工業上製造聚乙烯縮醛樹脂。較佳為50~75莫耳%。
再者,於本說明書中,所謂縮醛化度,係指於聚乙烯醇之羥基數中,以丁醛進行縮醛化之羥基數之比例,縮醛化度之計算方法,由於聚乙烯縮醛樹脂之縮醛基係由2個羥基進行縮醛化而形成,故而採用計算經縮醛化之2個羥基之方法,算出縮醛化度之莫耳%。
於本發明中,接著實施於上述無機分散液添加樹脂溶液之步驟。藉此,獲得漿料組成物。
再者,於本發明之漿料組成物之製造方法中,於不損及本發明之效果之範圍內,亦可含有上述聚乙烯縮醛樹脂以外之聚乙烯縮醛樹脂或丙烯酸系樹脂、乙基纖維素等其他樹脂。然而,於該種之情形時,上述聚乙烯縮醛樹脂相對於總黏合樹脂之含量必須為50重量%以上。
上述無機分散用有機溶劑及樹脂溶液用有機溶劑,並無特別限定,通常可使用漿料組成物中所使用之有機溶劑,例如可列舉:丙酮、甲基乙基酮、二丙基酮、二異丁基酮等酮類,甲醇、乙醇、異丙醇、丁醇等醇類,甲苯、二甲苯等芳香族烴類,丙酸甲酯、丙酸乙酯、丙酸丁酯、丁酸甲酯、丁酸乙酯、丁酸丁酯、戊酸甲酯、戊酸乙酯、戊酸丁酯、己酸甲酯、己酸乙酯、己酸丁酯、乙酸2-乙基己酯、丁酸2-乙基己酯等酯類,松脂醇(terpineol)、二氫松脂醇、松脂醇乙酸酯、二氫松脂醇乙酸酯等松脂醇及其衍生物等。該等之有機溶劑可單獨使用,亦可併用2種以上。
上述無機分散用有機溶劑及樹脂溶液用有機溶劑,尤其較佳為使用由乙醇及甲苯構成之混合溶劑。藉由使用上述混合溶劑,可大幅提昇漿料組成物之分散性。一般認為其原因在於相對於乙醇有助於防止聚乙烯縮醛樹脂(B)之凝聚,甲苯有助於混合聚乙烯縮醛樹脂(A)附著於無機粉末表面,藉由該等之相乘效果,而使漿料組成物之分散性大幅提昇。
關於使用上述混合溶劑時之上述乙醇與甲苯之混合比,較佳為設為5:5~2:8。藉由設為上述範圍內,可大幅提昇漿料組成物之分散性。
製作上述無機分散液之步驟中之上述無機分散用有機溶劑的添加量之較佳之下限相對於無機粉末100重量份為20重量份,較佳之上限為60重量份。若上述無機分散用有機溶劑之添加量未達20重量份,則有無機分散液之黏度變高、無機粉末之作用受到限制而未獲得充分之分散性之情形,若超過60重量份,則有由於無機分散液之無機粉末濃度變低、無機粉末彼此之碰撞次數減少,故而無法獲得充分之分散性之情形。
又,製作上述樹脂溶液之步驟中之上述樹脂溶液用有機溶劑的添加量之較佳之下限相對於無機粉末100重量份為70重量份,較佳之上限為130重量份。若上述樹脂溶液用有機溶劑之添加量未達70重量份,則有由於樹脂量不充足,故而生片之強度變得不充分之情形,若超過130重量份,則有生片中之樹脂量較多,於煅燒步驟中殘渣之量變多之情形。
於本發明之漿料組成物之製造方法中,於不損及本發明之效果之範圍內,亦可適當添加塑化劑、潤滑劑、抗靜電劑等。
藉由使用本發明之漿料組成物之製造方法,可製造可實現極高之分散性,且所獲得之膜狀體具有較高之強度之漿料組成物。該種之漿料組成物亦又為本發明之一態樣。
於本發明中,可提供一種可藉由簡單之方法而製造能長期維持較高之分散性之漿料組成物的漿料組成物之製造方法。又,可提供一種利用該漿料組成物之製造方法而製造之漿料組成物。
以下列舉實施例更詳細地對本發明進行說明,但本發明並非僅限定於該等實施例。
(聚乙烯縮醛樹脂(a1)[(a1-1)~(a1-9)]之合成)
於純水3000重量份添加聚合度250、皂化度99莫耳%之聚乙烯醇350重量份,於90℃之溫度攪拌約2小時使其溶解。將該溶液冷卻至40℃,於其中添加濃度35重量%之鹽酸230重量份後,將液溫降低至0℃,添加正丁醛205重量份,保持該溫度進行縮醛化反應,析出反應生成物。其後,將液溫設為20℃,保持3小時使反應結束,藉由常用方法經由中和、水洗及乾燥而獲得聚乙烯縮醛樹脂(a1-1)之白色粉末。使所獲得之聚乙烯縮醛樹脂溶解於DMSO-d6(二甲亞碸)中,使用13C-NMR(核磁共振光譜)測定丁醛化度、羥基量及乙醯基量,結果丁醛化度為69莫耳%,羥基量為30莫耳%,乙醯基量為1莫耳%。
又,除設為表1所示之條件以外,以與聚乙烯縮醛樹脂(a1-1)相同之方式合成聚乙烯縮醛樹脂(a1-2)~(a1-9)。
(聚乙烯縮醛樹脂(a2)[(a2-1)~(a2-10)]之合成)
於純水3000重量份添加聚合度320、皂化度99莫耳%之聚乙烯醇350重量份,於90℃之溫度攪拌約2小時使其溶解。將該溶液冷卻至40℃,於其中添加濃度35重量%之鹽酸230重量份後,將液溫降低至1℃,添加正丁醛150重量份,保持該溫度進行縮醛化反應,析出反應生成物。其後,將液溫設為20℃,保持3小時使反應結束,藉由常用方法經由中和、水洗及乾燥而獲得聚乙烯縮醛樹脂(a2-1)之白色粉末。使所獲得之聚乙烯縮醛樹脂溶解於DMSO-d6(二甲亞碸)中,使用13C-NMR(核磁共振光譜)測定丁醛化度、羥基量及乙醯基量,結果丁醛化度為51莫耳%,羥基量為48莫耳%,乙醯基量為1莫耳%。
又,除設為表2所示之條件以外,以與聚乙烯縮醛樹脂(a2-1)相同之方式合成聚乙烯縮醛樹脂(a2-2)~(a2-10)。
(聚乙烯縮醛樹脂(B)[(B1)~(B12)]之合成)
於純水3000重量份添加聚合度1700、皂化度99莫耳%之聚乙烯醇280重量份,於90℃之溫度攪拌約2小時使其溶解。將該溶液冷卻至10℃,於其中添加濃度35重量%之鹽酸200重量份與正丁醛155重量份,將液溫降低至1℃,保持該溫度進行縮醛化反應,析出反應生成物。其後,將液溫設為40℃,保持3小時使反應結束,藉由常用方法經由中和、水洗及乾燥而獲得聚乙烯縮醛樹脂(B1)之白色粉末。使所獲得之聚乙烯縮醛樹脂(B1)溶解於DMSO-d6(二甲亞碸)中,使用13C-NMR(核磁共振光譜)測定丁醛化度、羥基量及乙醯基量,結果丁醛化度為66莫耳%,羥基量為33莫耳%,乙醯基量為1莫耳%。
又,除設為表3所示之條件以外,以與聚乙烯縮醛樹脂(B1)相同之方式合成聚乙烯縮醛樹脂(B2)~(B12)。
(實施例1)
(無機分散液之製作)
於甲苯25重量份與乙醇25重量份之混合溶劑添加表4所示之聚乙烯縮醛樹脂(a1)0.5重量份及聚乙烯縮醛樹脂(a2)0.5重量份,進行攪拌溶解。接著,於所獲得之溶液中添加100重量份之鈦酸鋇之粉末(Sakai化學工業股份有限公司製造,BT01),添加直徑2mm之陶瓷球80ml,使用球磨機(Seiwa技研工業股份有限公司製造,BM-10),於旋轉數60rpm之條件下攪拌300分鐘,藉此製作無機分散液。
(樹脂溶液之製作)
於乙醇45重量份與甲苯45重量份之混合溶劑添加所獲得之聚乙烯縮醛樹脂(B1)8重量份、DOP2重量份,進行攪拌溶解,藉此製作樹脂溶液。
(漿料組成物之製作)
於所獲得之無機分散液添加樹脂溶液,利用球磨機於旋轉數60rpm之條件下攪拌180分鐘,藉此獲得漿料組成物。
(實施例2~27)
除使用表4所示之聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2)、聚乙烯縮醛樹脂(B)及有機溶劑以外,以與實施例1相同之方式而獲得漿料組成物。
(實施例28~30)
(無機分散液之製作)
於甲苯25重量份與乙醇25重量份之混合溶劑添加表4所示之聚乙烯縮醛樹脂(a1)0.5重量份,進行攪拌溶解。接著,於所獲得之溶液中添加100重量份之鈦酸鋇之粉末(Sakai化學工業股份有限公司製造,BT01),添加直徑2mm之陶瓷球80ml,使用球磨機(Seiwa技研工業股份有限公司製造,BM-10),於旋轉數60rpm之條件下攪拌180分鐘。
其後,進而添加表4所示之聚乙烯縮醛樹脂(a2)0.5重量份,利用球磨機於旋轉數60rpm之條件下攪拌120分鐘,藉此製作無機分散液,除此以外以與實施例1相同之方式而獲得漿料組成物。
(比較例1)
不將聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2)添加至無機分散液,而使用表5所示之聚乙烯縮醛樹脂(B)及有機溶劑,除此以外以與實施例1相同之方式而獲得漿料組成物。
(比較例2~4)
不將聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2)添加至無機分散液,而與表5所示之聚乙烯縮醛樹脂(B)一同溶解於樹脂溶液,除此以外以與實施例1相同之方式而獲得漿料組成物。
(比較例5~7)
不將聚乙烯縮醛樹脂(B)溶解於有機溶劑而添加至無機分散液,除此以外以與實施例1相同之方式而獲得漿料組成物。
(比較例8~21)
使用表4所示之聚乙烯縮醛樹脂樹脂(a1)、聚乙烯縮醛樹脂(a2)、聚乙烯縮醛樹脂(B)、及有機溶劑,除此以外以與實施例1相同之方式而獲得漿料組成物。
(比較例22)
使用於分散劑側鏈上接枝有烴之聚胺化合物(Croda公司製造,「Hypermer KD-2」)代替聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2),除此以外以與實施例1相同之方式而獲得漿料組成物。
(評價)
對於所獲得之漿料組成物進行以下之評價。
(1)生片之評價
(生片之製作)
於經脫模處理之聚對苯二甲酸乙二酯(PET)膜上,以乾燥後之膜厚成為20μm之方式塗敷漿料組成物,進行乾燥而製作陶瓷生片。
(1-1)表面粗糙度
對於上述所獲得之陶瓷生片,基於JIS B 0601(1994)測定表面粗糙度Ra,對陶瓷漿料之表面粗糙度進行評價。又,亦測定於23℃放置一週後之表面粗糙度Ra。
通常,漿料組成物之分散性越高,陶瓷生片之表面粗糙度變得越小。
◎ 未達0.025μm
○ 0.025μm以上、未達0.035μm
△ 0.035μm以上、未達0.045μm
× 0.045μm以上
(一週後)
◎ 未達0.030μm
○ 0.030μm以上、未達0.040μm
△ 0.040μm以上、未達0.050μm
× 0.050μm以上
(1-2)拉伸彈性率
根據JIS K 7113,使用AUTOGRAPH(島津製作所股份有限公司製造,「AGS-J」),於拉伸速度20mm/min之條件下進行拉伸彈性率(MPa)之測定。又,亦測定於23℃放置一週後之拉伸彈性率(MPa)。
◎ 1600MPa以上
○ 1400MPa以上、未達1600MPa
△ 1200MPa以上、未達1400MPa
× 未達1200MPa
(一週後)
◎ 1500MPa以上
○ 1300MPa以上、未達1500MPa
△ 1100MPa以上、未達1300MPa
× 未達1100MPa
(2)分散性評價
(分散性評價溶液之製作)
於乙醇5重量份與甲苯5重量份之混合溶劑添加所獲得之漿料組成物0.1重量份,利用超音波分散機(SND股份有限公司製造,「US-303」)攪拌10分鐘,藉此製作分散評價用溶液。
(分散性評價)
使用雷射繞射式粒度分佈儀(堀場製作所股份有限公司製造,LA-910)對所獲得之分散評價用溶液進行粒度分佈測定,測定最大粒徑尖峰值之位置、及平均分散徑。又,亦測定於23℃放置一週後之最大粒徑尖峰值之位置、及平均分散徑。
◎ 未達0.4μm
○ 0.4μm以上、未達0.5μm
△ 0.5μm以上、未達0.6μm
× 0.6μm以上
(一週後)
◎ 未達0.5μm
○ 0.5μm以上、未達0.6μm
△ 0.6μm以上、未達0.7μm
× 0.7μm以上
(實施例31~32)
使用氮化鋁粉代替鈦酸鋇作為無機粉末,使用表8所示之聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2)、聚乙烯縮醛樹脂(B)及有機溶劑,除此以外以與實施例1相同之方式而獲得漿料組成物。
(實施例33~34)
使用Ni-Zn系鐵氧體粉代替鈦酸鋇作為無機粉末,使用表8所示之聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2)、聚乙烯縮醛樹脂(B)及有機溶劑,除此以外以與實施例1相同之方式而獲得漿料組成物。
(比較例23)
使用氮化鋁粉代替鈦酸鋇作為無機粉末,不添加聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2)而使用表8所示之聚乙烯縮醛樹脂(B)及有機溶劑,除此以外以與實施例1相同之方式而獲得漿料組成物。
(比較例24)
使用Ni-Zn系鐵氧體粉代替鈦酸鋇作為無機粉末,不添加聚乙烯縮醛樹脂(a1)、聚乙烯縮醛樹脂(a2)而使用表8所示之聚乙烯縮醛樹脂(B)及有機溶劑,除此以外以與實施例1相同之方式而獲得漿料組成物。
對於所獲得之漿料組成物進行以下之評價。
(1)生片之評價
(生片之製作)
於經脫模處理之聚對苯二甲酸乙二酯(PET)膜上,以乾燥後之膜厚成為20μm之方式塗敷漿料組成物,進行乾燥而製作陶瓷生片。
(1-1)表面粗糙度
關於上述所獲得之陶瓷生片,基於JIS B 0601(1994)測定表面粗糙度Ra,對陶瓷漿料之表面粗糙度進行評價。又,亦測定於23℃放置一週後之表面粗糙度Ra。
通常,漿料組成物之分散性越高,則陶瓷生片之表面粗糙度變得越小。
◎ 未達0.2μm
○ 0.2μm以上、未達0.3μm
△ 0.33μm以上、未達0.4μm
× 0.4μm以上
(一週後)
◎ 未達0.25μm
○ 0.25μm以上、未達0.35μm
△ 0.35μm以上、未達0.45μm
× 0.45μm以上
(1-2)拉伸彈性率
根據JIS K 7113,使用AUTOGRAPH(島津製作所股份有限公司製造,「AGS-J」),於拉伸速度20mm/min之條件下進行拉伸彈性率(MPa)之測定。又,亦測定於23℃放置一週後之拉伸彈性率(MPa)。
◎ 1500MPa以上
○ 1200MPa以上、未達1500MPa
△ 900MPa以上、未達1200MPa
× 未達900MPa
(一週後)
◎ 1450MPa以上
○ 1150MPa以上、未達1450MPa
△ 850MPa以上、未達1150MPa
× 未達850MPa
(2)分散性評價
(分散性評價溶液之製作)
於乙醇5重量份與甲苯5重量份之混合溶劑添加所獲得之漿料組成物0.1重量份,利用超音波分散機(SND股份有限公司製造,「US-303」)攪拌10分鐘,藉此製作分散性評價用溶液。
(分散性評價)
使用雷射繞射式粒度分佈儀(堀場製作所股份有限公司製造,LA-910)對所獲得之分散性評價用溶液-進行粒度分佈測定,測定最大粒徑尖峰值之位置、及平均分散徑。又,亦測定於23℃放置一週後之最大粒徑尖峰值之位置、及平均分散徑。
◎ 未達2μm
○ 2μm以上、未達3μm
△ 3μm以上、未達4μm
× 4μm以上
(一週後)
◎ 未達2.5μm
○ 2.5μm以上、未達3.5μm
△ 3.5μm以上、未達4.5μm
× 4.5μm以上
根據本發明,可提供一種可藉由簡單之步驟而實現優異之分散性,且能長期維持較高之分散性之漿料組成物的製造方法。又,可提供一種利用該漿料組成物之製造方法而製造之漿料組成物。
Claims (5)
- 一種漿料組成物之製造方法,係製造含有無機粉末、聚乙烯縮醛樹脂及有機溶劑之漿料組成物,具有以下步驟:添加無機粉末、混合聚乙烯縮醛樹脂(A)及無機分散用有機溶劑並加以混合以製作無機分散液之步驟,添加聚乙烯縮醛樹脂(B)及樹脂溶液用有機溶劑並加以混合以製作樹脂溶液之步驟,及於該無機分散液添加樹脂溶液之步驟;其中,該混合聚乙烯縮醛樹脂(A)含有羥基量為20~40莫耳%之聚乙烯縮醛樹脂(a1)與羥基量為28~60莫耳%,聚合度為200~600之聚乙烯縮醛樹脂(a2),且該聚乙烯縮醛樹脂(a1)與聚乙烯縮醛樹脂(a2)具有下述(1)式之關係:Y-X≧5 (1)式(1)中,X表示聚乙烯縮醛樹脂(a1)之羥基量(莫耳%),Y表示聚乙烯縮醛樹脂(a2)之羥基量(莫耳%);該聚乙烯縮醛樹脂(B)之聚合度為800~4200;於製作該無機分散液之步驟中,相對於無機粉末100重量份,添加該混合聚乙烯縮醛樹脂(A)0.1~20重量份,相對於無機粉末100重量份,添加聚乙烯縮醛樹脂(B)5~20重量份。
- 如申請專利範圍第1項之漿料組成物之製造方法,其中,聚乙烯縮醛樹脂(a1)之聚合度為20~450。
- 如申請專利範圍第1項之漿料組成物之製造方法,其 中,聚乙烯縮醛樹脂(a2)具有陰離子性基。
- 如申請專利範圍第1項之漿料組成物之製造方法,其中,聚乙烯縮醛樹脂(B)之羥基量為22~42莫耳%。
- 如申請專利範圍第1、2、3、4項中任一項之漿料組成物之製造方法,其中,無機分散用有機溶劑及樹脂溶液用有機溶劑係由乙醇及甲苯構成之混合溶劑。
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