TWI557096B - 漿料組成物、陶瓷坯片及積層陶瓷電容器 - Google Patents
漿料組成物、陶瓷坯片及積層陶瓷電容器 Download PDFInfo
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- TWI557096B TWI557096B TW101135502A TW101135502A TWI557096B TW I557096 B TWI557096 B TW I557096B TW 101135502 A TW101135502 A TW 101135502A TW 101135502 A TW101135502 A TW 101135502A TW I557096 B TWI557096 B TW I557096B
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- slurry composition
- polyvinyl acetal
- acetal resin
- ceramic green
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- 239000000919 ceramic Substances 0.000 title claims description 97
- 239000000203 mixture Substances 0.000 title claims description 58
- 239000002002 slurry Substances 0.000 title claims description 54
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims description 79
- 229920002554 vinyl polymer Polymers 0.000 claims description 74
- 239000011354 acetal resin Substances 0.000 claims description 70
- 229920006324 polyoxymethylene Polymers 0.000 claims description 70
- 238000006359 acetalization reaction Methods 0.000 claims description 32
- 238000006116 polymerization reaction Methods 0.000 claims description 28
- 239000000843 powder Substances 0.000 claims description 23
- 239000000126 substance Substances 0.000 claims description 20
- KQNPFQTWMSNSAP-UHFFFAOYSA-N isobutyric acid Chemical compound CC(C)C(O)=O KQNPFQTWMSNSAP-UHFFFAOYSA-N 0.000 claims description 16
- 238000004519 manufacturing process Methods 0.000 claims description 15
- 239000003985 ceramic capacitor Substances 0.000 claims description 13
- 239000003960 organic solvent Substances 0.000 claims description 13
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- 125000004185 ester group Chemical group 0.000 claims 1
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 48
- 229920005989 resin Polymers 0.000 description 41
- 239000011347 resin Substances 0.000 description 41
- -1 polyethylene terephthalate Polymers 0.000 description 34
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N Butyraldehyde Chemical compound CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 32
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- 229920002451 polyvinyl alcohol Polymers 0.000 description 31
- 150000001299 aldehydes Chemical class 0.000 description 27
- IKHGUXGNUITLKF-UHFFFAOYSA-N Acetaldehyde Chemical compound CC=O IKHGUXGNUITLKF-UHFFFAOYSA-N 0.000 description 24
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical group OC=C IMROMDMJAWUWLK-UHFFFAOYSA-N 0.000 description 17
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- 238000000034 method Methods 0.000 description 15
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- 230000000052 comparative effect Effects 0.000 description 11
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- 150000003839 salts Chemical class 0.000 description 10
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- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
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- 238000003795 desorption Methods 0.000 description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
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- 239000002253 acid Chemical class 0.000 description 5
- 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 5
- 238000001035 drying Methods 0.000 description 5
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- 239000011229 interlayer Substances 0.000 description 5
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- HGBOYTHUEUWSSQ-UHFFFAOYSA-N valeric aldehyde Natural products CCCCC=O HGBOYTHUEUWSSQ-UHFFFAOYSA-N 0.000 description 5
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- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 4
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- 239000003377 acid catalyst Substances 0.000 description 4
- CQEYYJKEWSMYFG-UHFFFAOYSA-N butyl acrylate Chemical compound CCCCOC(=O)C=C CQEYYJKEWSMYFG-UHFFFAOYSA-N 0.000 description 4
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- 238000000576 coating method Methods 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
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- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N Glycolaldehyde Chemical compound OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 125000003172 aldehyde group Chemical group 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
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- 230000032798 delamination Effects 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000005470 impregnation Methods 0.000 description 3
- 239000003999 initiator Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 238000007650 screen-printing Methods 0.000 description 3
- 235000011121 sodium hydroxide Nutrition 0.000 description 3
- 238000013517 stratification Methods 0.000 description 3
- 239000004711 α-olefin Substances 0.000 description 3
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- NMPVEAUIHMEAQP-UHFFFAOYSA-N 2-Bromoacetaldehyde Chemical compound BrCC=O NMPVEAUIHMEAQP-UHFFFAOYSA-N 0.000 description 2
- UNNGUFMVYQJGTD-UHFFFAOYSA-N 2-Ethylbutanal Chemical compound CCC(CC)C=O UNNGUFMVYQJGTD-UHFFFAOYSA-N 0.000 description 2
- YGHRJJRRZDOVPD-UHFFFAOYSA-N 3-methylbutanal Chemical compound CC(C)CC=O YGHRJJRRZDOVPD-UHFFFAOYSA-N 0.000 description 2
- GOUHYARYYWKXHS-UHFFFAOYSA-N 4-formylbenzoic acid Chemical compound OC(=O)C1=CC=C(C=O)C=C1 GOUHYARYYWKXHS-UHFFFAOYSA-N 0.000 description 2
- HGINCPLSRVDWNT-UHFFFAOYSA-N Acrolein Chemical compound C=CC=O HGINCPLSRVDWNT-UHFFFAOYSA-N 0.000 description 2
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-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
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 2
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- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-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
- 229960005164 acesulfame Drugs 0.000 description 2
- 239000000654 additive 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
- 230000015572 biosynthetic process Effects 0.000 description 2
- XUPYJHCZDLZNFP-UHFFFAOYSA-N butyl butanoate Chemical compound CCCCOC(=O)CCC XUPYJHCZDLZNFP-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling 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
- HFJRKMMYBMWEAD-UHFFFAOYSA-N dodecanal Chemical compound CCCCCCCCCCCC=O HFJRKMMYBMWEAD-UHFFFAOYSA-N 0.000 description 2
- FJKIXWOMBXYWOQ-UHFFFAOYSA-N ethenoxyethane Chemical compound CCOC=C FJKIXWOMBXYWOQ-UHFFFAOYSA-N 0.000 description 2
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 2
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- 239000010419 fine particle Substances 0.000 description 2
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- 125000000524 functional group Chemical group 0.000 description 2
- HHLFWLYXYJOTON-UHFFFAOYSA-N glyoxylic acid Chemical compound OC(=O)C=O HHLFWLYXYJOTON-UHFFFAOYSA-N 0.000 description 2
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- 210000001161 mammalian embryo Anatomy 0.000 description 2
- HNBDRPTVWVGKBR-UHFFFAOYSA-N methyl pentanoate Chemical compound CCCCC(=O)OC HNBDRPTVWVGKBR-UHFFFAOYSA-N 0.000 description 2
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- NUJGJRNETVAIRJ-UHFFFAOYSA-N octanal Chemical compound CCCCCCCC=O NUJGJRNETVAIRJ-UHFFFAOYSA-N 0.000 description 2
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- 230000000704 physical effect Effects 0.000 description 2
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- SMQUZDBALVYZAC-UHFFFAOYSA-N salicylaldehyde Chemical compound OC1=CC=CC=C1C=O SMQUZDBALVYZAC-UHFFFAOYSA-N 0.000 description 2
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- ISAZDYZOHLBJRO-UHFFFAOYSA-N (4-formylphenyl) dihydrogen phosphate Chemical compound OP(O)(=O)OC1=CC=C(C=O)C=C1 ISAZDYZOHLBJRO-UHFFFAOYSA-N 0.000 description 1
- VQROQDIDXQDQLG-UHFFFAOYSA-N (4-formylphenyl) hydrogen sulfate Chemical compound OS(=O)(=O)OC1=CC=C(C=O)C=C1 VQROQDIDXQDQLG-UHFFFAOYSA-N 0.000 description 1
- KJPRLNWUNMBNBZ-QPJJXVBHSA-N (E)-cinnamaldehyde Chemical compound O=C\C=C\C1=CC=CC=C1 KJPRLNWUNMBNBZ-QPJJXVBHSA-N 0.000 description 1
- WUOACPNHFRMFPN-SECBINFHSA-N (S)-(-)-alpha-terpineol Chemical compound CC1=CC[C@@H](C(C)(C)O)CC1 WUOACPNHFRMFPN-SECBINFHSA-N 0.000 description 1
- OWXJKYNZGFSVRC-NSCUHMNNSA-N (e)-1-chloroprop-1-ene Chemical compound C\C=C\Cl OWXJKYNZGFSVRC-NSCUHMNNSA-N 0.000 description 1
- BQCIDUSAKPWEOX-UHFFFAOYSA-N 1,1-Difluoroethene Chemical compound FC(F)=C BQCIDUSAKPWEOX-UHFFFAOYSA-N 0.000 description 1
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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
- OZCMOJQQLBXBKI-UHFFFAOYSA-N 1-ethenoxy-2-methylpropane Chemical compound CC(C)COC=C OZCMOJQQLBXBKI-UHFFFAOYSA-N 0.000 description 1
- UZKWTJUDCOPSNM-UHFFFAOYSA-N 1-ethenoxybutane Chemical compound CCCCOC=C UZKWTJUDCOPSNM-UHFFFAOYSA-N 0.000 description 1
- LAYAKLSFVAPMEL-UHFFFAOYSA-N 1-ethenoxydodecane Chemical compound CCCCCCCCCCCCOC=C LAYAKLSFVAPMEL-UHFFFAOYSA-N 0.000 description 1
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- ZUGYJALETFVYJV-UHFFFAOYSA-N 1-methylcyclopentane-1-carbaldehyde Chemical compound O=CC1(C)CCCC1 ZUGYJALETFVYJV-UHFFFAOYSA-N 0.000 description 1
- HFZLSTDPRQSZCQ-UHFFFAOYSA-N 1-pyrrolidin-3-ylpyrrolidine Chemical compound C1CCCN1C1CNCC1 HFZLSTDPRQSZCQ-UHFFFAOYSA-N 0.000 description 1
- 238000005160 1H NMR spectroscopy Methods 0.000 description 1
- WMOOOIUXYRHDEZ-UHFFFAOYSA-N 2,3,4-trichlorobenzaldehyde Chemical compound ClC1=CC=C(C=O)C(Cl)=C1Cl WMOOOIUXYRHDEZ-UHFFFAOYSA-N 0.000 description 1
- UQEDGFZRPSAHLC-UHFFFAOYSA-N 2,3,4-trifluorobenzaldehyde Chemical compound FC1=CC=C(C=O)C(F)=C1F UQEDGFZRPSAHLC-UHFFFAOYSA-N 0.000 description 1
- GEICDMWIZIQEEI-UHFFFAOYSA-N 2,3-dibromobenzaldehyde Chemical compound BrC1=CC=CC(C=O)=C1Br GEICDMWIZIQEEI-UHFFFAOYSA-N 0.000 description 1
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- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 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
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- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
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- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- YWWNNLPSZSEZNZ-UHFFFAOYSA-N n,n-dimethyldecan-1-amine Chemical compound CCCCCCCCCCN(C)C YWWNNLPSZSEZNZ-UHFFFAOYSA-N 0.000 description 1
- WXEFTOZJECWFCW-UHFFFAOYSA-N n,n-dimethylpropan-1-amine;2-methylprop-2-enoic acid Chemical class CCCN(C)C.CC(=C)C(O)=O WXEFTOZJECWFCW-UHFFFAOYSA-N 0.000 description 1
- ADTJPOBHAXXXFS-UHFFFAOYSA-N n-[3-(dimethylamino)propyl]prop-2-enamide Chemical class CN(C)CCCNC(=O)C=C ADTJPOBHAXXXFS-UHFFFAOYSA-N 0.000 description 1
- RCHKEJKUUXXBSM-UHFFFAOYSA-N n-benzyl-2-(3-formylindol-1-yl)acetamide Chemical compound C12=CC=CC=C2C(C=O)=CN1CC(=O)NCC1=CC=CC=C1 RCHKEJKUUXXBSM-UHFFFAOYSA-N 0.000 description 1
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- FSAJWMJJORKPKS-UHFFFAOYSA-N octadecyl prop-2-enoate Chemical compound CCCCCCCCCCCCCCCCCCOC(=O)C=C FSAJWMJJORKPKS-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
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- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 1
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- HVAMZGADVCBITI-UHFFFAOYSA-M pent-4-enoate Chemical compound [O-]C(=O)CCC=C HVAMZGADVCBITI-UHFFFAOYSA-M 0.000 description 1
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- 230000000379 polymerizing effect Effects 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- BOQSSGDQNWEFSX-UHFFFAOYSA-N propan-2-yl 2-methylprop-2-enoate Chemical compound CC(C)OC(=O)C(C)=C BOQSSGDQNWEFSX-UHFFFAOYSA-N 0.000 description 1
- LYBIZMNPXTXVMV-UHFFFAOYSA-N propan-2-yl prop-2-enoate Chemical compound CC(C)OC(=O)C=C LYBIZMNPXTXVMV-UHFFFAOYSA-N 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- 238000000425 proton nuclear magnetic resonance spectrum Methods 0.000 description 1
- 125000004076 pyridyl group Chemical group 0.000 description 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- ADPUQRRLAAPXGT-UHFFFAOYSA-M sodium;2-formylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=CC=C1C=O ADPUQRRLAAPXGT-UHFFFAOYSA-M 0.000 description 1
- 125000000542 sulfonic acid group Chemical group 0.000 description 1
- 229910021653 sulphate ion Inorganic materials 0.000 description 1
- 238000010558 suspension polymerization method Methods 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
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 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
- KOZCZZVUFDCZGG-UHFFFAOYSA-N vinyl benzoate Chemical compound C=COC(=O)C1=CC=CC=C1 KOZCZZVUFDCZGG-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
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
- H01G4/1209—Ceramic dielectrics characterised by the ceramic dielectric material
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- B32B18/00—Layered products essentially comprising ceramics, e.g. refractory products
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Description
本發明係關於含有聚乙烯縮醛樹脂之漿料組成物、陶瓷胚片及積層陶瓷電容器。
在製造積層陶瓷電容器之情形中,一般係採用如下述的步驟。首先,在分散有陶瓷粉末之有機溶劑中,添加聚乙烯醇縮丁醛樹脂等的黏結劑樹脂與塑化劑,藉由利用球磨機等進行均勻地混合以調製陶瓷胚片用漿料組成物,將調製之漿料組成物流延成形於聚對苯二甲酸乙二酯薄膜等的剝離性之支持體上,利用加熱等餾除溶劑等之後,從支持體上剝離下來以製造陶瓷胚片。
接著,利用網板印刷等將由內部電極所構成之導電糊塗布於陶瓷胚片的表面而成者複數片交替重疊,並進行加熱壓接以得到積層體。然後,藉由各步驟形成積層體,切斷成規定的形狀。而且,進行將該積層體中所含有的黏結劑成分等熱分解並去除之處理,所謂的脫脂處理之後,藉由經過在燒成所得到的陶瓷燒成物之端面鍛燒外部電極之步驟,而製造積層陶瓷電容器。因此,分別對於上述漿料組成物要求調製作業的良好作業性,對於上述陶瓷胚片則要求能承受各步驟的強度。
近年來,伴隨著電子機器的多機能化或小型化,積層陶瓷電容器係要求大容量化、小型化。對應於此,做為陶瓷胚片所使用的陶瓷粉末,係使用0.5μm以下的微
細粒徑者,並嘗試在剝離性的支持體上塗敷成如5μm以下般的薄膜狀。
然而,若使用微細粒徑的陶瓷粉末,由於會為了增加填充密度或表面積,而增加使用的黏結劑樹脂量,伴隨於此,陶瓷胚片用漿料組成物的黏度也跟著增大,所以會有塗敷變得困難、或陶瓷粉末自體的分散不良產生的情形。另一方面,在陶瓷胚片製作時的各步驟中,由於負荷了拉伸或彎曲等的應力,為能承受這樣的應力,而使用高聚合度者做為黏結劑樹脂來進行。
在專利文獻1中,揭示一種機械強度優異的陶瓷胚片,其係含有聚合度超過2400且4500以下、乙烯酯單位量為1~20莫耳%、縮醛化度為55~80莫耳%之聚乙烯縮醛樹脂、陶瓷粉末、及有機溶劑之由陶瓷胚片用漿料組成物所得到之陶瓷胚片。
然而,最近係要求陶瓷胚片進一步的薄層化,用上述陶瓷漿料組成物來製作超薄層的陶瓷胚片時,若其厚度為2μm以下,則會有容易產生片材侵蝕(sheet attack)現象的問題。
此處,所謂的片材侵蝕現象,係指在所得之陶瓷胚片上印刷成為內部電極層之導電糊時,由於導電糊中的有機溶劑而使得在陶瓷胚片中所含有的黏結劑樹脂溶解,在陶瓷胚片產生破裂等的缺陷的現象,若發生該片材侵蝕現象,會降低積層陶瓷電容器的電氣性能或可靠性,且良率會顯著地降低。
在專利文獻2中,揭示一種聚乙烯縮醛樹脂組成物,其係將皂化度為80莫耳%以上且數量平均聚合度為1000~4000之聚乙烯醇樹脂予以縮醛化所得之聚乙烯縮醛樹脂,縮醛化度為60~75莫耳%,且藉由乙醛而縮醛化之部分與藉由丁醛而縮醛化之部分的比(藉由丁醛而縮醛化所消失之羥基的莫耳數/藉由乙醛而縮醛化所消失之羥基的莫耳數)為0.1~2。
然而,積層陶瓷電容器的小型化有其限度,為了能使晶片大容量化、或保持容量並小型化,除了胚片的薄層化,還要求多層化。隨著這樣的多層小型化,在保管胚片時的吸濕性係成為課題。亦即,在保管中經由黏結劑樹脂吸濕,而使得尺寸產生變化,又為了將薄膜多層地積層,當每1層的水分量較多時,則會在脫脂時產生所謂水分一口氣蒸發且進行分層作用的層間剝離。因此,胚片保管時的調濕或脫脂條件的調整變得非常重要。
例如,藉由乙醛而縮醛化之聚乙烯縮醛雖然玻璃轉移溫度較高、具有充分的機械強度,但是由於乙醛的疏水性較低,即使在與例示之丁醛的混合縮醛化物中吸濕性也較高,所以無法滿足上述課題。又,藉由丁醛而形成之縮醛化物亦為無法滿足充分的低吸濕性者。
如此一來,專利文獻1、專利文獻2中並未揭示兼具胚片保管時之尺寸變化少、在脫脂時層間剝離難以產生之性質的聚乙烯縮醛樹脂。
專利文獻1 特開2006-089354號公報
專利文獻2 特開2008-133371號公報
本發明有鑑於上述現狀,其目的係提供所得之陶瓷胚片具有充分的機械強度、保管時的尺寸變化少、且在脫脂初期難以產生層間剝離的漿料組成物。
本發明人等專心研究的結果,查明出聚合度為500以上6000以下、乙烯酯單位之含量為0.01~30莫耳%、縮醛化度為50~83莫耳%、以含2-甲基丙醛之醛予以縮醛化之聚乙烯縮醛樹脂,係顯示玻璃轉移溫度高且低吸水性,而完成了本發明。
亦即,本發明係關於一種含有聚乙烯縮醛樹脂、及有機溶劑的漿料組成物,該聚乙烯縮醛樹脂係聚合度為500以上6000以下,乙烯酯單位的含量為0.01~30莫耳%,縮醛化度為50~83莫耳%,且於分子中相對於全部經縮醛化之構造單位的總莫耳量而言具有30%以上的以化學式(1)所示之構造單位者。
前述聚乙烯縮醛樹脂係以於分子中具有以化學式(2)及/或化學式(3)所示之構造單位者為佳。
本發明的漿料組成物進一步較佳者係含有陶瓷粉末。
本發明又關於一種使用前述漿料組成物所得之陶瓷胚片。
本發明又關於一種使用前述陶瓷胚片所得之積層陶瓷電容器。
根據本發明的漿料組成物,可得到具有充分的機械強度、保管時的尺寸變化少的陶瓷胚片。又,根據該陶瓷胚片,可得到在脫脂初期難以產生層間剝離的積層陶瓷電容器。
以下係詳述本發明。
本發明所使用之聚乙烯縮醛樹脂的聚合度為500以上6000以下。若聚合度未滿500,則在製作陶瓷胚片時,機械強度會變得不充分,若聚合度超過6000,則無法充分地溶解在有機溶劑中,又溶液黏度會變得過高,而塗敷性或分散性降低。較佳的下限為1000,較佳的上限為4500。進一步較佳者係下限為1500,上限為3500。
上述聚乙烯縮醛樹脂係藉由使用醛將聚合度為500以上6000以下的聚乙烯醇樹脂予以縮醛化而進行製造
此外,上述聚合度係從製造聚乙烯縮醛樹脂時所使用之聚乙烯醇樹脂的黏度平均聚合度、聚乙烯縮醛樹脂的黏度平均聚合度兩者而求得。也就是說,為了使聚合度經由縮醛化也不會產生變化,聚乙烯醇樹脂、與將該聚乙烯醇予以縮醛化所得之聚乙烯縮醛樹脂的聚合度是相同的。沒有特別地限制,聚乙烯醇樹脂的黏度平均聚合度係指依照JIS K6726所求得之平均聚合度。又,在混合2種以上的聚乙烯醇樹脂做為聚乙烯醇樹脂使用之情形,係指混合後的聚乙烯醇樹脂全體於表觀上的黏度平均聚合度。另一方面,聚乙烯縮醛樹脂的聚合度係指依照JIS K6728所記載之方法所測定的黏度平均聚合度。此處,當聚乙烯縮醛樹脂為2種以上的聚乙烯縮醛樹脂的混合物之情形,亦指混合後的聚乙烯縮醛樹脂全體於表觀上的黏度平均聚合度。
上述聚乙烯縮醛樹脂的乙烯酯單位含量之下限為0.01莫耳%、上限為30莫耳%。若未滿0.01莫耳%,聚乙烯縮醛樹脂中的羥基之分子內及分子間的氫鍵增加,且陶瓷胚片用漿料組成物的黏度會變得過高,又,於導電糊中所使用之有機溶劑的溶解性會變得過高,而容易產生片材侵蝕現象。若超過30莫耳%,由於聚乙烯縮醛樹脂的玻璃轉移溫度降低、柔軟性會變得過強,而使得陶瓷胚片的處理性、機械強度、及加熱壓接時的尺寸安定性變差。較佳的下限為0.5莫耳%,較佳的上限為23莫耳%,進一步較佳的上限為20莫耳%。此外,乙烯酯單位的含量為0.01~30莫耳%之聚乙烯縮醛樹脂,係藉由將乙烯酯單位的含量為0.01~30莫耳%之聚乙烯醇樹脂、亦即皂化度為70~99.99莫耳%之聚乙烯醇樹脂予以縮醛化而得到。聚乙烯醇樹脂的皂化度之較佳下限為77莫耳%、進一步較佳的下限為80莫耳%,較佳的上限為99.5莫耳%。
上述聚乙烯縮醛樹脂的縮醛化度的下限為50莫耳%,上限為83莫耳%。若未滿50莫耳%,則聚乙烯縮醛樹脂的親水性高,會變得難以溶於有機溶劑中,再者,在保管時會吸水且陶瓷胚片產生尺寸變化,而成為在脫脂初期之層間剝離的原因。若超過83莫耳%,殘存羥基變少,而使得聚乙烯縮醛樹脂的強靭性受損,又,從生產性、反應性之觀點而言,亦難以在工業上得到,而導致生產性降低。較佳的下限為55莫耳%、更較佳的下限為60莫耳%,較佳的上限為80莫耳%。
將上述聚乙烯縮醛樹脂的縮醛化度調整成50~83莫耳%,必須適當調整醛對於聚乙烯醇樹脂的添加量、及添加醛與酸觸媒之後的反應時間等。又,相對於聚乙烯醇100質量份而言,較佳係添加20~150質量份的醛。
聚乙烯縮醛樹脂的縮醛化度係使聚乙烯縮醛樹脂溶解於DMSO-d6(二甲亞碸)中,測定1H-NMR光譜而可算出。
本發明中所使用之聚乙烯縮醛樹脂係相對於全部經縮醛化之構造單位的總莫耳量而言,具有30%以上的於分子中以化學式(1)所示之構造單位者。
上述化學式(1)所示之構造單位由於係為在與2個氧原子鍵結之碳原子上,進一步鍵結有異丙基而成之構造,具有該構造單位規定量以上之聚乙烯縮醛樹脂係物性的平衡優異,成為塗膜之際的耐濕熱性亦為優異。另一方面,相對於聚乙烯縮醛樹脂中的全部經縮醛化之構造單位而言,若上述化學式(1)所示之構造單位的比率變得比30%還低,則吸濕性變高,而會成為胚片的尺寸變化、脫脂時的分層作用(delamination)的原因。上述化學式(1)所示之構造單位的比率係較佳為40%以上,更較佳為50%以上。關於比率的上限沒有特別地限制,亦可為100%、亦即全部經縮醛化之構造單位均為上述化學式(1)所示
之構造單位。上述聚乙烯縮醛樹脂係可藉由使用含有2-甲基丙醛之醛而將聚乙烯醇樹脂予以縮醛化而製造。
本發明中所使用之聚乙烯縮醛樹脂係較佳為進一步於分子中具有化學式(2)及/或化學式(3)所示之構造單位者。
藉由具有化學式(2)所示之構造單位,可提昇所得之聚乙烯縮醛樹脂的機械強度。又,藉由具有化學式(3)所示之構造單位,可提昇所得之聚乙烯縮醛樹脂的低吸濕性。上述化學式(2)及/或化學式(3)所示之構造單位的比率通常為70%以下,較佳為60%以下,更較佳為50%以下。關於比率的下限沒有特別地限制,較佳者為10%以上。上述聚乙烯縮醛樹脂係除了2-甲基丙醛以外,還進一步使用含有乙醛及/或正丁醛的醛將聚乙烯醇樹脂予以縮醛化而製造。
本發明中所使用之聚乙烯縮醛樹脂的玻璃轉移溫度係較佳為72~100℃,更佳為75~95℃。玻璃轉移溫度若低於72℃,則機械強度變低,過高於100℃,則熱壓接性變差,而有成為分層作用之原因的傾向。
本發明中所使用之聚乙烯縮醛樹脂通常係以聚乙烯醇樹脂做為原料而製造的。上述聚乙烯醇樹脂係能藉由以往眾所週知的手法、亦即將乙烯酯系單體聚合、將所得之聚合物皂化而可得到。做為將乙烯酯系單體聚合之方法,可應用溶液聚合法、塊狀聚合法、懸濁聚合法、乳化聚合法等、以往眾所週知的方法。做為聚合起始劑,可按照聚合方法,適當選擇偶氮基系起始劑、過氧化物系起始劑、氧化還原系起始劑等。皂化反應可應用使用以往眾所週知的鹼觸媒或酸觸媒之醇解、水解等,此等之中係以將甲醇做為溶劑且使用苛性鈉(NaOH)觸媒之皂化反應為簡便且為最佳者。
做為乙烯酯系單體,可列舉例如:甲酸乙烯酯、乙酸乙烯酯、丙酸乙烯酯、丁酸乙烯酯、異丁酸乙烯酯、三甲基乙酸乙烯酯、叔碳酸乙烯酯(Versatic vinyl)、己酸乙烯酯、辛酸乙烯酯、月桂酸乙烯酯、棕櫚酸乙烯酯、硬脂酸乙烯酯、油酸乙烯酯、苯甲酸乙烯酯等,尤其較佳者是乙酸乙烯酯。
又,將前述乙烯酯系單體聚合之際,只要在不損及本發明主旨之範圍內,亦可共聚合其他的單體。因此,本發明的聚乙烯醇樹脂亦為包括以乙烯醇單位與其他的單體單位而構成之聚合物的概念。其他的單體之例子,
可列舉例如:乙烯、丙烯、正丁烯、異丁烯等的α-烯烴;丙烯酸及其鹽;丙烯酸甲酯、丙烯酸乙酯、丙烯酸正丙酯、丙烯酸異丙酯、丙烯酸正丁酯、丙烯酸異丁酯、丙烯酸第三丁酯、丙烯酸2-乙基己酯、丙烯酸十二酯、丙烯酸十八酯等的丙烯酸酯類;甲基丙烯酸及其鹽;甲基丙烯酸甲酯、甲基丙烯酸乙酯、甲基丙烯酸正丙酯、甲基丙烯酸異丙酯、甲基丙烯酸正丁酯、甲基丙烯酸異丁酯、甲基丙烯酸第三丁酯、甲基丙烯酸2-乙基己酯、甲基丙烯酸十二酯、甲基丙烯酸十八酯等的甲基丙烯酸酯類;丙烯醯胺、N-甲基丙烯醯胺、N-乙基丙烯醯胺、N,N-二甲基丙烯醯胺、雙丙酮丙烯醯胺、丙烯醯胺丙烷磺酸及其鹽、丙烯醯胺丙基二甲基胺及其酸鹽或4級鹽、N-羥甲基丙烯醯胺及其衍生物等的丙烯醯胺衍生物;甲基丙烯酸酯、N-甲基甲基丙烯酸酯、N-乙基甲基丙烯酸酯、甲基丙烯酸酯丙烷磺酸及其鹽、甲基丙烯酸酯丙基二甲基胺及其酸鹽或4級鹽、N-羥甲基甲基丙烯酸酯及其衍生物等的甲基丙烯酸酯衍生物;甲基乙烯醚、乙基乙烯醚、正丙基乙烯醚、異丙基乙烯醚、正丁基乙烯醚、異丁基乙烯醚、第三丁基乙烯醚、十二基乙烯醚、硬酯醯烯丙基乙烯醚等的乙烯醚類;丙烯腈、甲基丙烯腈等的腈類;氯乙烯、氟化乙烯等的鹵化乙烯;偏二氯乙烯、偏二氟乙烯等的鹵化亞乙烯;乙酸烯丙酯、氯丙烯等的烯丙基化合物;馬來酸及其鹽、酯或酸酐;乙烯基三甲氧基矽烷等的乙烯基矽烷基化合物;乙酸異丙烯酯等。此等單體通常相對於乙烯酯系單體而言,係以未滿10莫耳%的比例而使用。
其他的單體單位為α-烯烴單位之情形,其含量係較佳的下限為1莫耳%,較佳的上限為20莫耳%。若未滿1莫耳%,則含有上述α-烯烴的效果變得不充分,若超過20莫耳%,則疏水性變得過強且陶瓷粉末的分散性降低,又由於聚乙烯醇樹脂的溶解性降低,所以縮醛化反應變得困難。
做為縮醛化所使用的酸觸媒係沒有特別地限制,可使用有機酸及無機酸中的任一者,可列舉例如:乙酸、對甲苯磺酸、硝酸、硫酸、鹽酸等。此等之中尤佳者係使用鹽酸、硫酸、硝酸,特佳者是使用鹽酸、硝酸。
本發明中所使用之聚乙烯縮醛樹脂係可按照下述的方法而得到。首先,在80~100℃的溫度範圍內調製濃度3~15質量%的聚乙烯醇樹脂的水溶液之後,費時10~60分鐘緩緩地冷卻。在溫度降低至-10~40℃時,添加醛及酸觸媒,將溫度保持一定,並且進行縮醛化反應10~300分鐘。然後,較佳係包括下述步驟:費時30~200分鐘將反應液升溫至15~80℃的溫度,在該溫度保持0~360分鐘之熟成步驟。接著,在將反應液適當地冷卻至室温且予以水洗之後,藉由添加鹼等的中和劑、進行洗淨、乾燥,以得到目的之聚乙烯縮醛樹脂。
本發明中,係藉由使用2-甲基丙醛做為用以使聚乙烯醇樹脂予以縮醛化所使用的醛,而可將化學式(1)所示之構造單位導入聚乙烯縮醛樹脂。但是,在不損及本發明的特性之範圍內,亦可使用以下的醛。可列舉例如:甲醛(包含多聚甲醛甲醛)、乙醛、丙醛、戊醛、異戊醛
、己醛、2-乙基丁醛、三甲基乙醛、辛醛、2-乙基己醛、壬醛、癸醛、十二醛等的脂肪族醛及其烷基縮醛;環戊烷醛、甲基環戊烷醛、二甲基環戊烷醛、環己烷醛、甲基環己烷醛、二甲基環己烷醛、環己烷乙醛等的脂環族醛及其烷基縮醛;環戊烯醛、環己烯醛等的環式不飽和醛及其烷基縮醛;苯甲醛、甲基苯甲醛、二甲基苯甲醛、甲氧基苯甲醛、苯基乙醛、苯基丙醛、對異丙苯甲醛、萘醛、蒽醛、肉桂醛、丁烯醛、丙烯醛、7-辛烯-1-醛等的芳香族或不飽和結合含有醛及其烷基縮醛;糠醛、甲基糠醛等的雜環醛及其烷基縮醛等。
又,本發明中做為具有可將聚乙烯醇樹脂予以縮醛化所使用的羥基、羧酸基、磺酸基或磷酸基等為官能基之醛,可列舉:羥基乙醛、羥基丙醛、羥基丁醛、羥基戊醛、水楊醛、二羥基苯甲醛等的羥基含有醛及其烷基縮醛;乙醛酸及其金屬鹽或銨鹽、2-甲醯乙酸及其金屬鹽或銨鹽、3-甲醯丙酸及其金屬鹽或銨鹽、5-甲醯戊烷酸及其金屬鹽或銨鹽、4-甲醯基苯氧基乙酸及其金屬鹽或銨鹽、2-羧基苯甲醛及其金屬鹽或銨鹽、4-羧基苯甲醛及其金屬鹽或銨鹽、2,4-二羧基苯甲醛及其金屬鹽或銨鹽;苯甲醛2-磺酸及其金屬鹽或銨鹽、苯甲醛-2,4-二磺酸及其金屬鹽或銨鹽、4-甲醯基苯氧基磺酸及其金屬鹽或銨鹽、3-甲醯基-1-丙烷磺酸及其金屬鹽或銨鹽、7-甲醯基-1-庚烷磺酸及其金屬鹽或銨鹽;4-甲醯基苯氧基膦酸及其金屬鹽或銨鹽等的酸含有醛及其烷基縮醛等。
然後,做為具有可將聚乙烯醇樹脂予以縮醛化所使用的胺基、氰基、硝基或4級銨鹽等為官能基之醛,可列舉:胺基乙醛、二甲基胺基乙醛、二乙基胺基乙醛、胺基丙醛、二甲基胺基丙醛、胺基丁醛、胺基戊醛、胺基苯甲醛、二甲基胺基苯甲醛、乙基甲基胺基苯甲醛、二乙基胺基苯甲醛、吡咯啶基乙醛、哌啶基乙醛、吡啶基乙醛、氰基乙醛、α-氰基丙醛、硝基苯甲醛、三甲基-p-甲醯基苯基銨碘、三乙基-p-甲醯基苯基銨碘、三甲基-2-甲醯基乙基銨碘及其烷基縮醛等。
做為具有可將聚乙烯醇樹脂予以縮醛化所使用的鹵素為官能基之醛,可列舉:氯乙醛、溴乙醛、氟基乙醛、氯丙醛、溴丙醛、氟丙醛、氯丁醛、溴丁醛、氟丁醛、氯戊醛、溴戊醛、氟戊醛、氯苯甲醛、二氯苯甲醛、三氯苯甲醛、溴苯甲醛、二溴苯甲醛、三溴苯甲醛、氟苯甲醛、二氟苯甲醛、三氟苯甲醛、三氯甲基苯甲醛、三溴甲基苯甲醛、三氟甲基苯甲醛及其烷基縮醛等。此等之中,在併用2-甲基丙醛以外之醛來進行縮醛化反應之情形,如上所述,較佳係使用乙醛及/或正丁醛。
上述聚乙烯縮醛樹脂的製造中所使用之醛係較佳為一元醛(醛基係在一分子內為1個)。在以具有2個以上的醛基之化合物進行縮醛化之情形,由於交聯部位與未交聯部位的應力緩和力不同,所以會在製膜時產生翹曲。因此,較佳係使用之醛僅為一元醛,亦可為使用2個以上醛基的化合物之情形,相對於聚乙烯醇樹脂的乙烯醇單位而言,較佳者是添加比0.005莫耳%還少的量、更佳者是添加0.003莫耳%以下的量來進行縮醛化。
本發明中所使用之聚乙烯縮醛樹脂係含有10~1000ppm的2-甲基丙酸。藉由含有少量的2-甲基丙酸,可提昇陶瓷粉末的分散性。2-甲基丙酸的含量為未滿10ppm之聚乙烯縮醛樹脂,係在製造時的洗淨條件變得嚴苛上,所得之鍛燒體的陶瓷層與導電層會產生分層作用而為不佳。另一方面,若2-甲基丙酸的含量超過1000ppm,則從本發明的漿料所得之胚片的強度降低,又會有鍛燒體產生分層作用之傾向而為不佳。
本發明的漿料組成物係除了上述聚乙烯縮醛樹脂以外,還可還有有機溶劑。做為有機溶劑沒有特別地限制,可列舉例如:丙酮、甲乙酮、二丙酮、二異丁基酮等的酮類;甲醇、乙醇、異丙醇、丁醇等的醇類;甲苯、二甲苯等的芳香族烴類;丙酸甲酯、丙酸乙酯、丙酸丁酯、丁酸甲酯、丁酸乙酯、丁酸丁酯、戊烷酸甲酯、戊烷酸乙酯、戊烷酸丁酯、己烷己酸甲酯、己烷己酸乙酯、己烷己酸丁酯、乙酸2-乙基己酯、丁酸2-乙基己酯等的酯類;甲基賽珞蘇、乙基賽珞蘇、丁基賽珞蘇、α-萜品醇、丁基賽珞蘇乙酸酯、丁基卡必醇乙酸酯等的二醇類或萜烯類。此等有機溶劑可單獨使用、亦可併用2種以上。相對於本發明的漿料組成物之全量而言,有機溶劑的含量之上限為80質量%、較佳為70質量%,下限為20質量%。若在上述範圍內,可賦予本發明的漿料組成物適度的混練性。若多於80質量%,則黏度變得過低且將片成形之際的處理性會變差,若低於20質量%,則漿料組成物的黏度變得過高且會有混練性降低之傾向。
在上述之漿料組成物中進一步含有陶瓷粉末之漿料組成物,特別是在陶瓷胚片的製造步驟中溶解於一般所使用的乙醇與甲苯的1:1混合溶劑之情形中,由於含有可賦予適度的溶液黏度之聚乙烯縮醛樹脂,所以將該漿料組成物做為原料係顯示充分的塗敷性、機械強度,且可得到具有良好的填充性之陶瓷胚片。
做為上述陶瓷粉末係沒有特別地限制,可例舉例如:氧化鋁、氧化鋯、矽酸鋁、氧化鈦、氧化鋅、鈦酸鋇、氧化鎂、氮化矽鋁氧、尖晶石(spinel)、莫來石(mullite)、碳化矽、氮化矽、氮化鋁等的粉末。此等陶瓷粉末係可單獨使用、亦可併用2種以上。相對於含有上述陶瓷粉末之漿料組成物的全量而言,陶瓷粉末的含量之上限為80質量%,下限為30質量%。若低於30質量%,則黏度變得過低且在成形陶瓷胚片之際的處理性變差,若高於80質量%,則漿料組成物的黏度變得過高且會有混練性降低的傾向。
含有上述陶瓷粉末之漿料組成物係除了做為黏結劑樹脂之上述聚乙烯縮醛樹脂以外,還可含有丙烯酸系樹脂、纖維素系樹脂。此時,上述聚乙烯縮醛樹脂佔黏結劑樹脂全體的含量之較佳下限為30質量%。若未滿30質量%,則所得之陶瓷胚片的機械強度、加熱壓接性變得不充分。
含有上述陶瓷粉末之漿料組成物可按照需要而添加塑化劑。添加之塑化劑的種類係沒有特別地限制,可列舉例如:酞酸二辛酯、酞酸苯甲基丁酯、酞酸二丁酯、
酞酸二己酯、酞酸二(2-乙基丁酯)、酞酸二(2-乙基己酯)(DOP)等的酞酸系塑化劑;己二酸二己酯、己二酸二(2-乙基己酯)(DOA)等的己二酸系塑化劑;乙二醇、二乙二醇、三乙二醇等的二醇系塑化劑;三乙二醇二丁酸酯、三乙二醇二(2-乙基丁酸酯)、三乙二醇二(2-乙基己酸酯)等的己二醇酯系塑化劑等,此等亦可組合2種以上使用。此等之中,DOP、DOA、三乙二醇2-乙基己酸酯由於揮發性低、容易保持片的柔軟性,而尤為適宜。塑化劑的使用量係沒有特別地限制,相對於漿料組成物的全量而言,較佳係使用0.1~10質量%,更適宜者為1~8質量%。
含有上述陶瓷粉末之漿料組成物係在不損及本發明的效果之範圍內,除了上述的黏結劑樹脂、塑化劑以外,亦可含有潤滑劑、分散劑、抗靜電劑、抗氧化劑等的以往眾所週知的添加劑。
做為製造含有上述陶瓷粉末之漿料組成物之方法係沒有特別地限制,可例舉例如:使用球磨機、攪拌研磨機、三輥式滾軋機等的各種混合機,將含有上述聚乙烯縮醛樹脂之黏結劑樹脂、陶瓷粉末、有機溶劑及按照需要添加之各種添加劑進行混合之方法。
含有上述陶瓷粉末之漿料組成物可製造具有充分的機械強度之薄膜陶瓷胚片。做為陶瓷胚片的製造方法係沒有特別地限制,可藉由以往眾所週知的製造方法而製造,可列舉例如:將含有上述陶瓷粉末之漿料組成物流延成形於聚對苯二甲酸乙二酯薄膜等的剝離性之支持體
上,經由加熱等將溶劑等餾去之後,從支持體上剝離下來的方法等。
可藉由在上述陶瓷胚片上塗布導電糊並進行積層,而製作積層陶瓷電容器。如此一來,使用本發明的陶瓷胚片與導電糊所得之積層陶瓷電容器亦為本發明之一者。
做為本發明的積層陶瓷電容器之製造方法係沒有特別地限制,可藉由以往眾所週知的製造方法而進行製造,可列舉例如:將藉由網板印刷等塗布由內部電極所構成之導電糊於本發明的陶瓷胚片的表面上而成者交互重疊複數片,進行加熱壓接以得到積層體,將該積層體中所含有的黏結劑成分等進行熱分解予以去除之後(脫脂處理),在進行燒成所得之陶瓷燒成物的端面鍛燒外部電極之方法等。
以下,列舉實施例來進一步詳細說明本發明,但本發明並不因此等實施例而受到任何限制。此外,以下的實施例中,「%」及「份」只要沒有特別的解釋的話,係意味「質量%」及「質量份」。
聚乙烯縮醛樹脂的諸物性的測定係按照以下的方法來進行。
利用1H-NMR而算出。
使用精工儀器股份有限公司製EXTAR6000(RD220)做為DSC(示差掃描熱量計),將聚乙烯縮醛樹脂在氮中從30℃以升溫速度10℃/分鐘升溫至150℃之後,再冷卻至30℃,再一次以升溫速度10℃/分鐘升溫至150℃。將再升溫後的測定值當做玻璃轉移點而採用。
將厚度0.2mm、大小10cm×10cm的測定用試料在50℃、減壓下乾燥6天,接著,測定將乾燥後的試料在20℃的純水中經24小時浸漬時的質量,並依照下述式而求得吸水率。
吸水率(質量%)=[(浸漬後的質量-浸漬前的乾燥後質量)/(浸漬前的乾燥後質量)]×100
以加熱脫附GC-MS且用以下的條件,定量PVB樹脂中的2-甲基丙酸的含量。
加熱脫附條件
脫附溫度:100℃
脫附時間:10min.
捕捉溫度:-30℃
脫附溫度:260℃
脫附保持時間:30min.
烘箱溫度:從40℃升溫至240℃
載送氣體:He,1.0mL/min.
試樣量:50mg(冷凍粉碎品)
在具備迴流冷卻器、溫度計及錨式攪拌翼之內容積2公升的玻璃製容器中,飼入離子交換水1295g、聚乙烯醇(PVA-1:聚合度1700、皂化度98.8莫耳%)105g,將全體升溫至95℃將聚乙烯醇完全溶解,以得到聚乙烯醇水溶液(濃度7.5質量%)。以旋轉速度120rpm繼續攪拌所得之聚乙烯醇水溶液,並且費時約30分鐘緩緩地冷卻至13℃之後,於該水溶液中添加2-甲基丙醛60.0g,然後添加縮醛化觸媒之濃度20質量%的鹽酸100ml,開始聚乙烯醇的縮醛化。進行縮醛化15分鐘之後,費時120分鐘將反應系升溫至47℃,在47℃中保持180分鐘之後,冷卻至室温。藉由冷卻分別過濾經析出之樹脂,以相對於樹脂而言為100倍量之離子交換水洗淨10次之後,添加用以中和的0.3質量%氫氧化鈉溶液,在50℃保持5小時。再以100倍量的離子交換水重複再洗淨10次且脫水之後,在40℃、減壓下乾燥18小時,以得到聚乙烯縮醛樹脂(PVIB-1)。分析所得之聚乙烯縮醛樹脂(PVIB-1),以2-甲基丙醛而縮醛化之構造單位的含量(縮醛化度)為70.9莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為27.9莫耳%。將所得之聚乙烯縮醛樹脂10質量份加入甲苯20質量份與乙醇20質量份之混合溶劑中,而且添加做為塑化劑之DOP8質量份,進行攪拌溶解。在所得之樹脂溶液中添加做為陶瓷粉末之鈦酸鋇(堺化學工業股份有限公司製、BT-03(平均粒
徑0.3μm))100質量份,藉由以球磨機進行混合48小時,以得到陶瓷胚片用漿料組成物。
除了取代PVA-1而使用PVA-2(聚合度800、皂化度98.4莫耳%)、使用2-甲基丙醛61.5g以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVIB-2)。縮醛化度為71.7莫耳%、乙酸乙烯酯單位的含量為1.6莫耳%、乙烯醇單位的含量為26.7莫耳%。接著,使用PVIB-2且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了取代PVA-1而使用PVA-3(聚合度2400、皂化度98.8莫耳%)、使用2-甲基丙醛59.6g以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVIB-3)。縮醛化度為70.3莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為28.5莫耳%。接著,使用PVIB-3且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了取代PVA-1而使用PVA-4(聚合度4000、皂化度98.9莫耳%)、使用2-甲基丙醛65.1g以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVIB-4)。縮醛化度為75.6莫耳%、乙酸乙烯酯單位的含量為1.1莫耳%、乙烯醇單位的含量為23.3莫耳%。接著,使用PVIB-4且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了取代PVA-1而使用PVA-5(聚合度1700、皂化度88.0莫耳%)、使用2-甲基丙醛50.6g以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVIB-5)。縮醛化度為71.2莫耳%、乙酸乙烯酯單位的含量為12.0莫耳%、乙烯醇單位的含量為16.8莫耳%。接著,使用PVIB-5且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用2-甲基丙醛35.5g及正丁醛30.5g做為醛以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVIB-6)。以2-甲基丙醛而縮醛化之構造單位的含量為41.8莫耳%、以正丁醛而縮醛化之構造單位的含量為35.1莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為21.9莫耳%。接著,使用PVIB-6且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用2-甲基丙醛30.5g及乙醛20.4g做為醛以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVIB-7)。以2-甲基丙醛而縮醛化之構造單位的含量為41.6莫耳%、以乙醛而縮醛化之構造單位的含量為37.6莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為19.6莫耳%。接著,使用PVIB-7且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用正丁醛58.4g取代做為醛之2-甲基丙醛以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVB-A)。縮醛化度為68.6莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為30.2莫耳%。接著,使用PVB-A且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用正丁醛60.5g取代做為醛之2-甲基丙醛以外,與實施例2同樣地得到聚乙烯縮醛樹脂(PVB-B)。縮醛化度為71.2莫耳%、乙酸乙烯酯單位的含量為1.6莫耳%、乙烯醇單位的含量為27.2莫耳%。接著,使用PVB-B且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用正丁醛58.7g取代做為醛之2-甲基丙醛以外,與實施例3同樣地得到聚乙烯縮醛樹脂(PVB-C)。縮醛化度為68.7莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為30.1莫耳%。接著,使用PVB-C且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用正丁醛35.8g及乙醛19.5g取代做為醛之2-甲基丙醛以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVB-D)。以正丁醛而縮醛化之構造單位的含量為40.0莫耳%、以乙醛而縮醛化之構造單位的含量為36.9莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為21.9莫耳%。接著,使用PVB-D且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用2-甲基丙醛18.5g及正丁醛47.8g做為醛以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVB-E)。以2-甲基丙醛而縮醛化之構造單位的含量為21.6莫耳%、以正丁醛而縮醛化之構造單位的含量為55.3莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為21.9莫耳%。接著,使用PVB-E且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用2-甲基丙醛20.2g及乙醛29.5g做為醛以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVB-F)。以2-甲基丙醛而縮醛化之構造單位的含量為23.0莫耳%、以乙醛而縮醛化之構造單位的含量為56.2莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為19.6莫耳%。接著,使用PVB-F且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了使用2-甲基丙醛41.2g以外,與實施例1同樣地得到聚乙烯縮醛樹脂(PVB-G)。縮醛化度為48.3莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為50.5莫耳%。接著,使用PVB-G且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了取代PVA-1而使用PVA-6(聚合度400、皂化度98.8莫耳%)、使用2-甲基丙醛60.3g以外,與實施例1
同樣地得到聚乙烯縮醛樹脂(PVB-H)。縮醛化度為70.8莫耳%、乙酸乙烯酯單位的含量為1.2莫耳%、乙烯醇單位的含量為28.0莫耳%。接著,使用PVB-H且與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了將實施例1所得之PVIB-1再以離子交換水重複再洗淨40次以外,與實施例1同樣地得到陶瓷胚片用漿料組成物。
除了實施例1所得之PVIB-1以離子交換水進行再洗淨1次以外,與實施例1同樣地得到陶瓷胚片用漿料組成物。
使用塗布棒以成為乾燥厚度為1μm的方式將實施例1~7及比較例1~10所得之陶瓷胚片用漿料組成物,塗敷於經離形處理之聚酯薄膜上,在常溫下風乾1小時之後,用熱風乾燥機於80℃乾燥3小時、接著在120℃下乾燥2小時,以得到陶瓷胚片。
將所得之陶瓷胚片從聚酯薄膜剝離下來,觀察陶瓷胚片的狀態,並用以下的3階段進行評價。將結果表示於表1。
○:於陶瓷胚片沒有觀察到小片或破裂。
△:稍微觀察到些小片或破裂。
×:明確地觀察到小片或破裂。
將30cm×30cm的陶瓷胚片靜置在23℃、65%RH的高温恒濕層,於製膜後測定10日後的尺寸變化率,並用以下的2階段進行評價。將結果表示於表1。
○:陶瓷胚片的尺寸變化率未滿0.1%且沒有觀察到翹曲。
×:陶瓷胚片的尺寸變化率為0.1%以上、或者有觀察到翹曲。
將做為導電粉末之鎳粉末(2020SS、三井金屬礦業股份有限公司製)100質量份、乙基纖維素(Dow Chemical Company公司製STD-100)5質量份、做為溶劑之萜品醇-C(日本萜烯股份有限公司製)60質量份加以混合之後,以三輥式滾軋機進行混練以得到導電糊。
利用網板印刷法將於上述所得之導電糊以乾燥後的厚度為約1.0μm的方式塗敷於上述所得之陶瓷胚片的單面上,並使其乾燥以形成導電層。將含有該導電層之陶瓷胚片切斷成5cm平方,堆疊100片,以溫度70℃、壓力150kg/cm2加熱壓接10分鐘,以得到積層體。藉由將所得之積層體在氮氣環境下、以升溫速度3℃/分鐘升溫至400℃,並保持5小時之後,繼續以升溫速度5℃/分鐘升溫至1350℃,且保持10小時,以得到陶瓷鍛燒體。
將該鍛燒體冷卻至常溫之後切割成一半,用電子顯微鏡進行觀察,觀察陶瓷層與導電層有無分層作用,並用以下的3階段進行評價。將結果表示於表1。
○:無分層作用。
△:稍微觀察到些分層作用。
×:有分層作用。
根據本發明的漿料組成物,可得到具有充分的機械強度、保管時的尺寸變化少的陶瓷胚片。又,根據該陶瓷胚片,可得到於脫脂初期難以產生層間剝離的積層陶瓷電容器。
Claims (5)
- 一種漿料組成物,其係含有聚乙烯縮醛樹脂、2-甲基丙酸及有機溶劑,其中該聚乙烯縮醛樹脂係聚合度為500以上6000以下,乙烯酯單位的含量為0.01~30莫耳%,縮醛化度為50~83莫耳%,且於分子中相對於全部經縮醛化之構造單位的總莫耳量而言具有30%以上之化學式(1)所示之構造單位者;
- 如申請專利範圍第1項之漿料組成物,其中前述聚乙烯縮醛樹脂係進一步具有於分子中具有化學式(2)及/或化學式(3)所示之構造單位者,
- 如申請專利範圍第1項之漿料組成物,其中進一步含有陶瓷粉末。
- 一種陶瓷胚片,其係使用如申請專利範圍第3項之漿料組成物而得到。
- 如申請專利範圍第4項之陶瓷胚片,其係用於積層陶瓷電容器的製造。
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WO2011102197A1 (ja) | 2010-02-16 | 2011-08-25 | 株式会社クラレ | セラミックグリーンシート用ポリビニルアセタール樹脂、およびその製造方法、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 |
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- 2012-09-28 JP JP2013536412A patent/JP5913339B2/ja active Active
- 2012-09-28 WO PCT/JP2012/075012 patent/WO2013047717A1/ja active Application Filing
- 2012-09-28 KR KR1020147011129A patent/KR101925479B1/ko active IP Right Grant
- 2012-09-28 CN CN201280047876.0A patent/CN103842313B/zh not_active Expired - Fee Related
- 2012-09-28 US US14/348,363 patent/US9355777B2/en not_active Expired - Fee Related
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Patent Citations (3)
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TW200812933A (en) * | 2006-05-10 | 2008-03-16 | Kuraray Europe Gmbh | Process for the production of ceramic green films with acetalated polyvinyl alcohols |
TW201119974A (en) * | 2009-10-16 | 2011-06-16 | Nippon Chemical Ind | Composition for forming dielectric ceramic and dielectric ceramic material |
WO2011092963A1 (ja) * | 2010-01-26 | 2011-08-04 | 株式会社クラレ | 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 |
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WO2013047717A1 (ja) | 2013-04-04 |
CN103842313B (zh) | 2015-11-25 |
JPWO2013047717A1 (ja) | 2015-03-26 |
KR101925479B1 (ko) | 2018-12-05 |
JP5913339B2 (ja) | 2016-04-27 |
EP2762463A1 (en) | 2014-08-06 |
US20140256863A1 (en) | 2014-09-11 |
EP2762463B1 (en) | 2016-05-25 |
KR20140079793A (ko) | 2014-06-27 |
US9355777B2 (en) | 2016-05-31 |
CN103842313A (zh) | 2014-06-04 |
EP2762463A4 (en) | 2015-06-17 |
TW201329018A (zh) | 2013-07-16 |
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