CN113646380A - 陶瓷生片用树脂组合物、陶瓷生片及层叠陶瓷电容器 - Google Patents
陶瓷生片用树脂组合物、陶瓷生片及层叠陶瓷电容器 Download PDFInfo
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- CN113646380A CN113646380A CN202080025884.XA CN202080025884A CN113646380A CN 113646380 A CN113646380 A CN 113646380A CN 202080025884 A CN202080025884 A CN 202080025884A CN 113646380 A CN113646380 A CN 113646380A
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- resin
- ceramic green
- green sheet
- resin composition
- polyvinyl acetal
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- 239000000919 ceramic Substances 0.000 title claims abstract description 114
- 239000011342 resin composition Substances 0.000 title claims abstract description 61
- 239000003985 ceramic capacitor Substances 0.000 title claims description 12
- DHKHKXVYLBGOIT-UHFFFAOYSA-N 1,1-Diethoxyethane Chemical compound CCOC(C)OCC DHKHKXVYLBGOIT-UHFFFAOYSA-N 0.000 claims abstract description 71
- 239000011354 acetal resin Substances 0.000 claims abstract description 70
- 229920006324 polyoxymethylene Polymers 0.000 claims abstract description 70
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 70
- 239000011347 resin Substances 0.000 claims description 73
- 229920005989 resin Polymers 0.000 claims description 73
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 45
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 33
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 33
- 238000006116 polymerization reaction Methods 0.000 claims description 24
- 238000007127 saponification reaction Methods 0.000 claims description 21
- 125000004036 acetal group Chemical group 0.000 claims description 13
- 239000004014 plasticizer Substances 0.000 claims description 7
- 238000005481 NMR spectroscopy Methods 0.000 claims description 3
- 238000005520 cutting process Methods 0.000 abstract description 10
- 230000007547 defect Effects 0.000 abstract description 10
- 239000000843 powder Substances 0.000 description 29
- -1 polyethylene terephthalate Polymers 0.000 description 17
- 238000000034 method Methods 0.000 description 16
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 15
- 238000002360 preparation method Methods 0.000 description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 14
- 238000001035 drying Methods 0.000 description 13
- 238000005259 measurement Methods 0.000 description 13
- 239000003960 organic solvent Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 9
- 125000002777 acetyl group Chemical group [H]C([H])([H])C(*)=O 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 150000001299 aldehydes Chemical class 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000012046 mixed solvent Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 239000004925 Acrylic resin Substances 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 3
- 229920002799 BoPET Polymers 0.000 description 3
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000006359 acetalization reaction Methods 0.000 description 3
- 125000000217 alkyl group Chemical group 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 239000011324 bead Substances 0.000 description 3
- 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 3
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 3
- 125000004432 carbon atom Chemical group C* 0.000 description 3
- 238000005238 degreasing Methods 0.000 description 3
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- 230000003472 neutralizing effect Effects 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000001644 13C nuclear magnetic resonance spectroscopy Methods 0.000 description 2
- HCFAJYNVAYBARA-UHFFFAOYSA-N 4-heptanone Chemical compound CCCC(=O)CCC HCFAJYNVAYBARA-UHFFFAOYSA-N 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- IMROMDMJAWUWLK-UHFFFAOYSA-N Ethenol Chemical compound OC=C IMROMDMJAWUWLK-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
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- AMIMRNSIRUDHCM-UHFFFAOYSA-N Isopropylaldehyde Chemical compound CC(C)C=O AMIMRNSIRUDHCM-UHFFFAOYSA-N 0.000 description 2
- AFVFQIVMOAPDHO-UHFFFAOYSA-N Methanesulfonic acid Chemical compound CS(O)(=O)=O AFVFQIVMOAPDHO-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 2
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 2
- XUPYJHCZDLZNFP-UHFFFAOYSA-N butyl butanoate Chemical compound CCCCOC(=O)CCC XUPYJHCZDLZNFP-UHFFFAOYSA-N 0.000 description 2
- 150000001734 carboxylic acid salts Chemical class 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 125000004122 cyclic group Chemical group 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 description 2
- 239000002270 dispersing agent Substances 0.000 description 2
- 230000000694 effects Effects 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
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000000463 material Substances 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
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- NUKZAGXMHTUAFE-UHFFFAOYSA-N methyl hexanoate Chemical compound CCCCCC(=O)OC NUKZAGXMHTUAFE-UHFFFAOYSA-N 0.000 description 2
- 125000004123 n-propyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 239000011118 polyvinyl acetate Substances 0.000 description 2
- 229920002689 polyvinyl acetate Polymers 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 239000001716 (4-methyl-1-propan-2-yl-1-cyclohex-2-enyl) acetate Substances 0.000 description 1
- 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
- VXQBJTKSVGFQOL-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethyl acetate Chemical compound CCCCOCCOCCOC(C)=O VXQBJTKSVGFQOL-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
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-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
- GCDUWJFWXVRGSM-UHFFFAOYSA-N 2-[2-(2-heptanoyloxyethoxy)ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOC(=O)CCCCCC GCDUWJFWXVRGSM-UHFFFAOYSA-N 0.000 description 1
- JEYLQCXBYFQJRO-UHFFFAOYSA-N 2-[2-[2-(2-ethylbutanoyloxy)ethoxy]ethoxy]ethyl 2-ethylbutanoate Chemical compound CCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CC JEYLQCXBYFQJRO-UHFFFAOYSA-N 0.000 description 1
- SSKNCQWPZQCABD-UHFFFAOYSA-N 2-[2-[2-(2-heptanoyloxyethoxy)ethoxy]ethoxy]ethyl heptanoate Chemical compound CCCCCCC(=O)OCCOCCOCCOCCOC(=O)CCCCCC SSKNCQWPZQCABD-UHFFFAOYSA-N 0.000 description 1
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- NQBXSWAWVZHKBZ-UHFFFAOYSA-N 2-butoxyethyl acetate Chemical compound CCCCOCCOC(C)=O NQBXSWAWVZHKBZ-UHFFFAOYSA-N 0.000 description 1
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-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
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-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
- 229910019114 CoAl2O4 Inorganic materials 0.000 description 1
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 1
- ICMAFTSLXCXHRK-UHFFFAOYSA-N Ethyl pentanoate Chemical compound CCCCC(=O)OCC ICMAFTSLXCXHRK-UHFFFAOYSA-N 0.000 description 1
- 229910005451 FeTiO3 Inorganic materials 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- JGFBQFKZKSSODQ-UHFFFAOYSA-N Isothiocyanatocyclopropane Chemical compound S=C=NC1CC1 JGFBQFKZKSSODQ-UHFFFAOYSA-N 0.000 description 1
- RJUFJBKOKNCXHH-UHFFFAOYSA-N Methyl propionate Chemical compound CCC(=O)OC RJUFJBKOKNCXHH-UHFFFAOYSA-N 0.000 description 1
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 1
- 229910017676 MgTiO3 Inorganic materials 0.000 description 1
- 229910003378 NaNbO3 Inorganic materials 0.000 description 1
- 229910003303 NiAl2O4 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- 229910003781 PbTiO3 Inorganic materials 0.000 description 1
- 229910020698 PbZrO3 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- FRQDZJMEHSJOPU-UHFFFAOYSA-N Triethylene glycol bis(2-ethylhexanoate) Chemical compound CCCCC(CC)C(=O)OCCOCCOCCOC(=O)C(CC)CCCC FRQDZJMEHSJOPU-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 description 1
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- 150000001255 actinides Chemical class 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
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- IGODOXYLBBXFDW-UHFFFAOYSA-N alpha-Terpinyl acetate Chemical compound CC(=O)OC(C)(C)C1CCC(C)=CC1 IGODOXYLBBXFDW-UHFFFAOYSA-N 0.000 description 1
- WUOACPNHFRMFPN-UHFFFAOYSA-N alpha-terpineol Chemical compound CC1=CCC(C(C)(C)O)CC1 WUOACPNHFRMFPN-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
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- 150000003934 aromatic aldehydes Chemical class 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 1
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- SRSXLGNVWSONIS-UHFFFAOYSA-N benzenesulfonic acid Chemical compound OS(=O)(=O)C1=CC=CC=C1 SRSXLGNVWSONIS-UHFFFAOYSA-N 0.000 description 1
- 229940092714 benzenesulfonic acid Drugs 0.000 description 1
- ZFMQKOWCDKKBIF-UHFFFAOYSA-N bis(3,5-difluorophenyl)phosphane Chemical compound FC1=CC(F)=CC(PC=2C=C(F)C=C(F)C=2)=C1 ZFMQKOWCDKKBIF-UHFFFAOYSA-N 0.000 description 1
- 229910052796 boron Inorganic materials 0.000 description 1
- OBNCKNCVKJNDBV-UHFFFAOYSA-N butanoic acid ethyl ester Natural products CCCC(=O)OCC OBNCKNCVKJNDBV-UHFFFAOYSA-N 0.000 description 1
- PWLNAUNEAKQYLH-UHFFFAOYSA-N butyric acid octyl ester Natural products CCCCCCCCOC(=O)CCC PWLNAUNEAKQYLH-UHFFFAOYSA-N 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
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- 239000003990 capacitor Substances 0.000 description 1
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- 229910052802 copper Inorganic materials 0.000 description 1
- PMHQVHHXPFUNSP-UHFFFAOYSA-M copper(1+);methylsulfanylmethane;bromide Chemical compound Br[Cu].CSC PMHQVHHXPFUNSP-UHFFFAOYSA-M 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- KVFDZFBHBWTVID-UHFFFAOYSA-N cyclohexanecarbaldehyde Chemical compound O=CC1CCCCC1 KVFDZFBHBWTVID-UHFFFAOYSA-N 0.000 description 1
- 125000002704 decyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- SQIFACVGCPWBQZ-UHFFFAOYSA-N delta-terpineol Natural products CC(C)(O)C1CCC(=C)CC1 SQIFACVGCPWBQZ-UHFFFAOYSA-N 0.000 description 1
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- CCIVGXIOQKPBKL-UHFFFAOYSA-M ethanesulfonate Chemical compound CCS([O-])(=O)=O CCIVGXIOQKPBKL-UHFFFAOYSA-M 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
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- 229910001676 gahnite Inorganic materials 0.000 description 1
- 229910052733 gallium Inorganic materials 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 125000005843 halogen group Chemical group 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- WNLRTRBMVRJNCN-UHFFFAOYSA-N hexanedioic acid Natural products OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 1
- 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
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- YDZQQRWRVYGNER-UHFFFAOYSA-N iron;titanium;trihydrate Chemical compound O.O.O.[Ti].[Fe] YDZQQRWRVYGNER-UHFFFAOYSA-N 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- 229910052744 lithium Inorganic materials 0.000 description 1
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- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000001247 metal acetylides Chemical class 0.000 description 1
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- 238000003756 stirring Methods 0.000 description 1
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- 229910052712 strontium Inorganic materials 0.000 description 1
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Abstract
本发明提供陶瓷生片用树脂组合物以及使用了该陶瓷生片用树脂组合物的陶瓷生片及层叠陶瓷电容器,所述陶瓷生片用树脂组合物能够制作即使在制成薄层的情况下也具有高机械强度、不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片。本发明为一种陶瓷生片用树脂组合物,其含有聚乙烯醇缩醛树脂,tanδ的峰顶为1.25以上,并且损耗模量E”为2.30×108Pa以上。
Description
技术领域
本发明涉及能够制作即使在制成薄层的情况下也具有高机械强度、不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片的陶瓷生片用树脂组合物、以及使用了该陶瓷生片用树脂组合物的陶瓷生片及层叠陶瓷电容器。
背景技术
近年来,搭载于各种电子设备的电子部件的小型化、层叠化不断发展,广泛使用多层电路基板、层叠线圈、层叠陶瓷电容器等层叠型电子部件。
其中,层叠陶瓷电容器通常经过如下工序来制造。
首先,在将聚乙烯醇缩丁醛树脂、聚(甲基)丙烯酸酯系树脂等粘结剂树脂溶解于有机溶剂而得的溶液中添加增塑剂、分散剂等后,加入陶瓷原料粉末,通过珠磨机、球磨机等混合装置更均匀地混合,脱泡后得到具有一定粘度的陶瓷浆料组合物。使用刮刀、逆转辊涂布机等将该浆料组合物流延到经脱模处理的聚对苯二甲酸乙二醇酯膜或SUS板等的支撑体面,通过加热等对其蒸馏除去溶剂等挥发成分后,从支撑体剥离而得到陶瓷生片。
接下来,在所得到的陶瓷生片上交替层叠多片通过丝网印刷而涂布有成为内部电极的导电糊的材料,进行加热压接,制作层叠体。然后,进行将层叠体中所含的粘结剂树脂成分等热分解而除去的处理、所谓的脱脂处理,经过在烧成而得到的陶瓷烧结体的端面烧结外部电极的工序,而得到层叠陶瓷电容器。
另外,随着电子设备的多功能化、小型化,对层叠陶瓷电容器要求大容量化小型化。与此对应,陶瓷生片使用更微细的粒径(例如,0.5μm以下)的陶瓷粉末,进行了以更薄膜状(例如,5μm以下)涂覆于剥离性的支撑体上的尝试。
然而,在制作陶瓷生片时的各工序中,对薄膜状的陶瓷生片施加拉伸、弯曲等应力。因此,要求具有可耐受这些应力的强度的陶瓷生片。
与此相对,在专利文献1和2中记载了通过将聚合度、乙酰基量、缩醛基量设为规定的范围,从而能够在不添加过量的有机溶剂的情况下得到涂覆性优异的浆料组合物。
现有技术文献
专利文献
专利文献1:日本专利第5462700号公报
专利文献2:日本专利第5702311号公报
发明内容
发明要解决的课题
然而,即使是专利文献1和2中记载那样的浆料组合物,也存在所得到的陶瓷生片的强度变得不充分、从支撑体剥离时发生破损的问题。
另外,在陶瓷生片制作时的切断工序中,存在切断面不均匀、产生外观不良的问题。
此外,在干燥工序中,由于尺寸发生变化,还引起产生切断后的尺寸不良的问题。
本发明鉴于上述现状,其目的在于提供:陶瓷生片用树脂组合物、以及使用了该陶瓷生片用树脂组合物的陶瓷生片及层叠陶瓷电容器,所述陶瓷生片用树脂组合物能够制作即使在制成薄层的情况下也具有高机械强度、不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片。
用于解决课题的手段
本发明为一种陶瓷生片用树脂组合物,其含有聚乙烯醇缩醛树脂,tanδ的峰顶为1.25以上,损耗模量E”为2.30×108Pa以上。
以下详细说明本发明。
本发明人等进行了深入研究,结果发现,tanδ的峰顶、损耗模量E”为规定的范围内的陶瓷生片用树脂组合物即使在制成薄层的情况下也具有高的机械强度,能够制作不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片,从而完成了本发明。
本发明的陶瓷生片用树脂组合物的tanδ的峰顶为1.25以上。由此,能够赋予适度的柔软性。上述tanδ的峰顶的优选下限为1.55,优选上限为3.00。
需要说明的是,上述tanδ的峰顶例如是:使用DMA(IT计测公司制),在温度范围30℃~150℃、升温速度6℃/分钟、频率1Hz的条件下测定时的峰温度下的tanδ的测定值。另外,上述DMA测定优选在将陶瓷生片用树脂组合物成形为片状后进行测定。
本发明的陶瓷生片用树脂组合物的损耗模量E”为2.30×108Pa以上。通过设为上述范围内,能够赋予适度的柔软性。上述损耗模量E”的优选下限为2.30×108Pa,优选上限为2.80×108Pa。
需要说明的是,上述损耗模量例如是:使用DMA(IT计测公司制)在温度范围30℃~150℃、升温速度6℃/分钟、频率1Hz的条件下测定时的峰温度下的损耗模量的测定值。另外,上述DMA测定优选在将陶瓷生片用树脂组合物成形为片状后进行测定。
本发明的陶瓷生片用树脂组合物的tanδ的峰顶温度与损耗模量E”的峰顶温度之差(峰顶温度差:[tanδ的峰顶温度]-[损耗模量E”的峰顶温度])优选为8.0~15.0℃。通过设为上述范围内,能够得到强韧的膜强度。上述峰顶温度差的更优选的下限为9.0℃,更优选的上限为14.0℃。
本发明的陶瓷生片用树脂组合物含有聚乙烯醇缩醛树脂。
上述聚乙烯醇缩醛树脂具有下述通式(1)所示的具有缩醛基的结构单元、下述通式(2)所示的具有羟基的结构单元以及下述通式(3)所示的具有乙酰基的结构单元。
[化学式1]
上述式(1)中,R1表示氢原子或碳原子数1~20的烷基。
上述式(1)中,在R1为碳原子数1~20的烷基的情况下,作为该烷基,例如可举出甲基、乙基、正丙基、异丙基、正丁基、异丁基、仲丁基、叔丁基等。另外,可举出戊基、己基、庚基、2-乙基己基、辛基、壬基、癸基、十一烷基、十二烷基、十三烷基、十四烷基、十五烷基、十八烷基等。其中,优选甲基、正丙基。
在上述聚乙烯醇缩醛树脂中,上述通式(1)所示的具有缩醛基的结构单元的含量(以下,也称为“缩醛基量”)的优选下限为45摩尔%,优选上限为83摩尔%。
如果上述缩醛基量为45摩尔%以上,则能够提高在有机溶剂中的溶解性。如果上述缩醛基量为83摩尔%以下,则能够制成强韧性优异的聚乙烯醇缩醛树脂。
上述缩醛基量的更优选的下限为60摩尔%,进一步优选的下限为62摩尔%,特别优选的下限为65摩尔%,更优选的上限为80摩尔%,进一步优选的上限为78摩尔%。
需要说明的是,在本说明书中,作为缩醛基量的计算方法,由于聚乙烯醇缩醛树脂的缩醛基是将聚乙烯醇树脂的具有2个羟基的结构单元缩醛化而得到的,因此采用对经缩醛化的具有2个羟基的结构单元进行计数的方法来计算缩醛基量。
在上述聚乙烯醇缩醛树脂中,上述通式(2)所示的具有羟基的结构单元的含量(以下,也称为“羟基量”)的优选下限为18摩尔%,优选上限为45摩尔%。
如果上述羟基量为18摩尔%以上,则能够制成强韧性优异的聚乙烯醇缩醛树脂。如果上述羟基量为45摩尔%以下,则能够充分提高在有机溶剂中的溶解性。
上述羟基量的更优选的下限为20摩尔%,进一步优选的下限为22摩尔%,更优选的上限为40摩尔%,进一步优选的上限为37摩尔%。
在上述聚乙烯醇缩醛树脂中,上述通式(3)所示的具有乙酰基的结构单元的含量(以下,也称为“乙酰基量”)的优选下限为0.5摩尔%,优选上限为20摩尔%。
如果上述乙酰基量为0.5摩尔%以上,则能够抑制聚乙烯醇缩醛树脂中的羟基的分子内和分子间的氢键所导致的高粘度化。如果上述乙酰基量为20摩尔%以下,则聚乙烯醇缩醛树脂的柔软性不会过度提高,能够提高处理性。
上述乙酰基量的更优选的下限为1.0摩尔%,更优选的上限为18摩尔%。
上述聚乙烯醇缩醛树脂的平均聚合度优选为1000~10000。
通过使上述平均聚合度为1000以上,从而即使在制作厚度20μm以下这样的薄膜树脂片的情况下,也能够赋予充分的机械强度。如果上述平均聚合度为10000以下,则能够充分提高在有机溶剂中的溶解,使涂覆性、分散性优异。另外,通过设为上述范围内,能够得到具有高机械强度、不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片。
上述平均聚合度的更优选的下限为1050,进一步优选的下限为1100,更优选的上限为5000,进一步优选的上限为4900,最优选的上限为4800。
上述聚乙烯醇缩醛树脂优选的是,通过NMR测定和IR测定而定量的羟基的摩尔%换算半峰宽为0.01~0.15摩尔%/cm-1。通过设为上述范围内,能够得到具有高机械强度、不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片。另外,羟基的摩尔%换算半峰宽更优选为0.01~0.145摩尔%/cm-1。
需要说明的是,上述IR测定是指基于红外吸收分光法的吸收光谱的测定,例如可以利用IR测定计进行测定。
另外,上述羟基的摩尔%换算半峰宽可以如下算出:通过IR测定并根据在3500cm-1附近出现的峰高的1/2处的峰宽测定羟基的半峰宽后,通过NMR测定来测定羟基量,再以羟基量除以羟基的半峰宽,由此算出。
上述聚乙烯醇缩醛树脂通常可以通过将聚乙烯醇树脂缩醛化来制造。
作为上述缩醛化的方法,没有特别限定,可以使用以往公知的方法,例如可举出:在酸催化剂的存在下,在聚乙烯醇树脂的水溶液、醇溶液、水/醇混合溶液、二甲基亚砜(DMSO)溶液中添加各种醛的方法等。
作为上述醛,例如可举出碳原子数1~19的直链状、支链状、环状饱和、环状不饱和或芳香族的醛等。具体而言,例如可举出甲醛、乙醛、丙醛(日文:プロピオニルアルデヒド)、正丁醛、异丁醛、叔丁醛、苯甲醛、环己醛等。上述醛可以单独使用,也可以并用2种以上。另外,上述醛化合物可以是除甲醛以外1个以上的氢原子被卤素等取代的化合物。
作为上述聚乙烯醇树脂,可以使用例如:通过利用碱、酸、氨水等对聚乙酸乙烯酯进行皂化而制造的树脂等以往公知的聚乙烯醇树脂。
上述聚乙烯醇树脂可以被完全皂化,但只要至少在主链的1处部位存在最少1单元的、相对于内消旋位、外消旋位而具有2单元组羟基(日文:2連の水酸基)的单元,则无需被完全皂化,而可以为部分皂化聚乙烯醇系树脂。另外,作为上述聚乙烯醇树脂,也可以使用乙烯-乙烯醇共聚物树脂、部分皂化乙烯-乙烯醇共聚物树脂等能够同乙烯醇共聚的单体与乙烯醇的共聚物。
上述聚乙酸乙烯酯系树脂例如可举出乙烯-乙酸乙烯酯共聚物等。
构成本发明的陶瓷生片用树脂组合物的聚乙烯醇缩醛树脂优选为皂化度为75摩尔%以上的聚乙烯醇树脂的缩醛化物。特别是,构成本发明的陶瓷生片用树脂组合物的聚乙烯醇缩醛树脂优选为通过IR测定定量的羟基的半峰宽为300~400cm-1的聚乙烯醇树脂的缩醛化物。特别优选使用通过IR测定而定量的羟基的半峰宽为340~400cm-1的聚乙烯醇树脂的缩醛化物。由此,能够使本发明的陶瓷生片用树脂组合物的tanδ的峰顶和损耗模量E”为规定的范围内。
上述聚乙烯醇树脂通常含有皂化时产生的碱性成分即羧酸盐,因此,优选将其清洗除去或中和之后使用。通过将羧酸盐清洗除去或中和,能够有效地抑制在碱性条件下受到催化作用的醛的缩合反应,因此能够进一步抑制树脂的着色。
作为上述清洗工序中的清洗方法,例如可举出:利用溶剂提取碱性成分的方法;使树脂溶解于良溶剂后,投入劣溶剂而仅使树脂再沉淀的方法;在含有聚乙烯醇系树脂的溶液中添加吸附剂而吸附除去碱性成分的方法;等。
作为上述中和工序中使用的中和剂,例如可举出:盐酸、硫酸、硝酸、磷酸等矿物酸、碳酸等无机酸、甲酸、乙酸、丙酸、丁酸、己酸等羧酸、甲磺酸、乙磺酸等脂肪族磺酸、苯磺酸等芳香族磺酸、苯酚等酚类等。
本发明的陶瓷生片用树脂组合物可以含有增塑剂。通过添加增塑剂,能够大幅提高所得到的陶瓷生片的机械强度和柔软性。
作为上述增塑剂,例如可举出:邻苯二甲酸二辛酯(DOP)、邻苯二甲酸二丁酯(DBP)等邻苯二甲酸二酯、己二酸二辛酯等己二酸二酯等、三乙二醇-二-2-乙基己酸酯、四乙二醇-二-2-乙基己酸酯等亚烷基二醇二酯等。另外,可举出三乙二醇-二-2-乙基丁酸酯、四乙二醇-二-2-乙基丁酸酯、四乙二醇-二-庚酸酯、三乙二醇-二-庚酸酯等亚烷基二醇二酯等。
在本发明的陶瓷生片用树脂组合物中,上述增塑剂的含量相对于聚乙烯醇缩醛树脂100重量份的优选下限为7重量份,更优选的下限为8.5重量份,优选上限为25重量份,更优选的上限为15重量份,进一步优选的上限为11.5重量份。
本发明的陶瓷生片用树脂组合物可以含有有机溶剂。
作为上述有机溶剂,没有特别限定,例如,只要能够溶解上述聚乙烯醇缩醛树脂就没有特别限定,例如可举出丙酮、甲乙酮、二丙基酮、二异丁基酮等酮类。另外,可举出甲醇、乙醇、异丙醇、丁醇等醇类、甲苯、二甲苯等芳香族烃类等。此外,可举出丙酸甲酯、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-乙基己酯等酯类等。另外,可举出甲基溶纤剂、乙基溶纤剂、丁基溶纤剂、萜品醇、二氢萜品醇、丁基溶纤剂乙酸酯、丁基卡必醇乙酸酯、萜品醇乙酸酯、二氢萜品醇乙酸酯等。从涂覆性、干燥性的方面出发,特别优选醇类、酮类、芳香族烃类和它们的混合溶剂。其中,优选乙醇与甲苯的混合溶剂、甲乙酮与甲苯的混合溶剂。
本发明的陶瓷生片用树脂组合物可以在不损害本发明的效果的范围内含有:除了上述聚乙烯醇缩醛树脂以外的聚乙烯醇缩醛树脂、丙烯酸系树脂、乙基纤维素等其他树脂。这种情况下,上述聚乙烯醇缩醛树脂相对于全部粘结剂树脂的含量优选为50重量%以上。
本发明的陶瓷生片用树脂组合物中,可以根据需要适当添加无机粉末、分散剂、抗氧化剂、紫外线吸收剂、表面活性剂、填充剂等,也可以根据情况少量添加丙烯酸系树脂、氨基甲酸酯树脂等其他树脂。
作为上述无机粉末,可举出金属或非金属的氧化物或非氧化物的粉末、陶瓷粉末。另外,关于这些粉末的组成,可以将单一组成的粉末、化合物状态的粉末单独或混合地使用。需要说明的是,关于金属的氧化物或非氧化物的构成元素,阳离子或阴离子均可以由一种元素构成,也可以由多种元素构成,还可以包含为了改良氧化物或非氧化物的特性而添加的添加物。具体而言,可举出:Li、K、Mg、B、Al、Si、Cu、Ca、Sr、Ba、Zn、Cd、Ga、In、Y、镧系元素、锕系元素、Ti、Zr、Hf、Bi、V、Nb、Ta、W、Mn、Fe、Co、Ni等的氧化物、碳化物、氮化物、硼化物、硫化物等。
另外,如果根据晶体结构对通常被称为复合氧化物的包含多种金属元素的氧化物粉末的具体物质进行分类,则作为具有钙钛矿型结构的物质,可举出NaNbO3、SrZrO3、PbZrO3、SrTiO3、BaZrO3、PbTiO3、BaTiO3等。作为具有尖晶石型结构的物质,可举出MgAl2O4、ZnAl2O4、CoAl2O4、NiAl2O4、MgFe2O4等。作为具有钛铁矿型结构的物质,可举出MgTiO3、MnTiO3、FeTiO3等。作为具有石榴石型结构的物质,可举出GdGa5O12、Y6Fe5O12等。其中,本申请的改性聚乙烯醇缩醛树脂相对于与BaTiO3的粉末混合而成的陶瓷生片显示出高特性。
上述无机粉末的平均粒径没有特别限定,例如,作为薄层陶瓷生片(厚度5μm以下)的制作用途,优选为0.05~0.5μm以下。
在本发明的陶瓷生片用树脂组合物含有无机粉末的情况下,上述聚乙烯醇缩醛树脂的含量的优选下限相对于无机粉末100重量份为0.1重量份,优选上限为20重量份。通过将上述聚乙烯醇缩醛树脂的含量设为0.1重量份以上,无机粉末的分散性变得充分,通过设为20重量份以下,粘度能够成为适度的范围,能够提高处理性。上述含量的更优选的下限为0.6重量份,进一步优选的上限为15重量份。特别是,通过将上述含量设为0.6重量份以上,能够使聚乙烯醇缩醛树脂充分地吸附于无机粉末的表面,因此能够使无机粉末更微细地分散。
在本发明的陶瓷生片用树脂组合物含有无机粉末的情况下,上述有机溶剂的含量的优选下限相对于无机粉末100重量份为20重量份,优选上限为60重量份。通过将上述有机溶剂的含量设为20重量份以上,能够使粘度为适度范围,不会限制无机粉末的活动而得到充分的分散性,通过设为60重量份以下,从而无机粉末浓度不会过度降低,能够减少无机粉末彼此的碰撞次数而得到充分的分散性。
作为制造本发明的陶瓷生片用树脂组合物的方法,没有特别限定,例如可举出:使用球磨机、混合磨机、三辊磨机等各种混合机将上述聚乙烯醇缩醛树脂、有机溶剂和根据需要添加的各种添加剂无机粉末混合的方法等。需要说明的是,上述无机粉末可以在制备无机分散液后另行添加。
涂覆本发明的陶瓷生片用树脂组合物后,通过加热使其干燥而得到树脂片。
作为涂覆本发明的陶瓷生片用树脂组合物时的方法,没有特别限定,例如可举出辊涂机、模涂机、帘涂机等方法。需要说明的是,关于其他具体的方法,可以使用以往公知的方法。
包含陶瓷粉末的树脂片可以用作陶瓷生片。这样的陶瓷生片也是本发明之一。
使用上述陶瓷生片,能够制造陶瓷电子部件。例如,通过进行在陶瓷生片的表面涂覆电极层用糊的工序、将形成有电极层的陶瓷生片层叠并进行加热压接而得到层叠体,对所得到的层叠体进行脱脂、烧成的工序,从而能够制造陶瓷电子部件。
作为上述陶瓷电子部件,没有特别限定,例如可举出层叠陶瓷电容器、层叠陶瓷电感器、电容器、压电致动器、层叠压敏电阻、层叠热敏电阻、EMI滤波器、氮化铝多层基板、氧化铝多层基板等。这样的陶瓷电子部件也是本发明之一。
在上述陶瓷电子部件的制造方法中,进行在上述陶瓷生片的表面涂覆电极层用糊的工序。
作为电极层用糊,例如可以通过将聚乙烯醇缩醛树脂、乙基纤维素、丙烯酸系树脂等作为粘结剂树脂溶解于有机溶剂,使导电粉末等分散而得到。这些树脂可以单独使用,也可以混合使用2种以上。含有聚乙烯醇缩醛树脂的电极层用糊在加热压接工序中对陶瓷生片显示优异的粘接性,因此优选。
在上述陶瓷电子部件的制造方法中,在制作出上述的形成有电极层的陶瓷生片后,将同样地操作而制作出的形成有电极层的陶瓷生片层叠并进行加热压接而得到层叠体,对所得到的层叠体进行脱脂、烧成,由此得到解决了片材侵蚀(日文:シートアタック)、裂纹等问题的层叠陶瓷电子部件。
需要说明的是,对于上述加热压接工序、对层叠体进行脱脂、烧成的工序没有特别限定,可以使用以往公知的方法。
发明的效果
根据本发明,能够提供陶瓷生片用树脂组合物以及使用了该陶瓷生片用树脂组合物的陶瓷生片及层叠陶瓷电容器,所述陶瓷生片用树脂组合物能够制作即使在制成薄层的情况下也具有高机械强度、不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片。
具体实施方式
以下,列举实施例更详细地说明本发明,但本发明并不仅限定于这些实施例。
(实施例1)
(聚乙烯醇缩醛树脂的制作)
在平均聚合度1000、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g中加入纯水2700g,在90℃下搅拌约2小时使其溶解。将溶液冷却至40℃,向其中添加浓度35重量%的盐酸100g和正丁醛115g,进行缩醛化反应,使反应产物析出。然后,在40℃下完成缩醛化反应,通过常规方法进行中和、水洗和干燥,得到聚乙烯醇缩醛树脂的白色粉末。
将所得到的聚乙烯醇缩醛树脂以10重量%的浓度溶解于DMSO-d6中,使用13C-NMR测定缩醛基量、羟基量、乙酰基量。需要说明的是,聚乙烯醇树脂的羟基的半峰宽使用HORIBA FT-720(堀场制作所公司制)进行测定。
(陶瓷生片用树脂组合物的制作)
加入所得到的聚乙烯醇缩醛树脂10.0重量份以及作为增塑剂的1.0重量份的DOP,加入乙醇/甲苯混合溶剂(重量比1:1)45.0重量份,搅拌溶解,得到陶瓷生片用树脂组合物。
(树脂片的制作)
使用涂布机将所得到的陶瓷生片用树脂组合物以干燥后的厚度成为15μm的方式涂覆于经脱模处理的PET膜后,在70℃下加热干燥120分钟,由此制作树脂片。
(实施例2)
(聚乙烯醇缩醛树脂的制作)
使用聚合度1700、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例3)
(聚乙烯醇缩醛树脂的制作)
使用聚合度3300、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例4)
(聚乙烯醇缩醛树脂的制作)
使用聚合度4900、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例5)
(聚乙烯醇缩醛树脂的制作)
使用聚合度1700、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例6)
(聚乙烯醇缩醛树脂的制作)
使用聚合度1700、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例7)
(聚乙烯醇缩醛树脂的制作)
使用聚合度1700、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例8)
(聚乙烯醇缩醛树脂的制作)
使用聚合度5000、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例9)
(聚乙烯醇缩醛树脂的制作)
使用聚合度9200、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例10)
(聚乙烯醇缩醛树脂的制作)
使用聚合度8000、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(实施例11)
(聚乙烯醇缩醛树脂的制作)
使用聚合度1700、皂化度98.5摩尔%、羟基半峰宽350cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(比较例1)
使用聚合度600、皂化度98.5摩尔%、羟基半峰宽335cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(比较例2)
使用聚合度4900、皂化度98.5摩尔%、羟基半峰宽335cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(比较例3)
使用聚合度1700、皂化度98.5摩尔%、羟基半峰宽335cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(比较例4)
使用聚合度3300、皂化度98.5摩尔%、羟基半峰宽335cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(比较例5)
使用聚合度4900、皂化度98.5摩尔%、羟基半峰宽335cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(比较例6)
使用聚合度9000、皂化度98.5摩尔%、羟基半峰宽335cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(比较例7)
使用聚合度9000、皂化度98.5摩尔%、羟基半峰宽335cm-1的聚乙烯醇树脂250g,除此以外,与实施例1同样地操作,制作聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物、树脂片。
(评价)
对于实施例和比较例中得到的聚乙烯醇缩醛树脂、陶瓷生片用树脂组合物和树脂片,进行以下的评价。将结果示于表1。
(1)摩尔%换算半峰宽的确认
对于实施例和比较例中得到的聚乙烯醇缩醛树脂,使用HORIBA FT-720(堀场制作所公司制),通过IR测定来测定羟基的半峰宽。根据通过IR测定测得的羟基的半峰宽和通过13C-NMR测得的羟基量,对聚乙烯醇缩醛树脂求出羟基的摩尔%换算半峰宽。
(2)tanδ和损耗模量E”
将所得到的树脂片切割成0.5cm×2.0cm而制作试验片后,使用DMA(IT计测公司制),在下述条件下测定动态粘弹性。
需要说明的是,tanδ(损耗角正切)使用峰顶温度时的数值。另外,对于储能模量E’和损耗模量E”,也同样地测定峰顶温度时的数值。另外,算出tanδ的峰顶温度与损耗模量E”的峰顶温度之差(峰顶温度差:[tanδ的峰顶温度]-[损耗模量E”的峰顶温度])。
(测定条件)
测定模式:拉伸模式
强制振动频率:1Hz
温度范围:30℃~150℃
升温速度:6℃/分钟
(3)拉伸弹性模量、断裂点伸长率和断裂点应力
(陶瓷生片的制作)
将聚乙烯醇缩醛树脂(积水化学工业公司制,BL-1)1重量份加入到甲苯20重量份与乙醇20重量份的混合溶剂中,搅拌溶解。接下来,将100重量份的钛酸钡的粉末(堺化学工业公司制,BT01,平均粒径0.1μm)添加到所得到的溶液中,利用珠磨机(AIMEX公司制ReadyMill)搅拌180分钟,由此制作无机分散液。
在所得到的无机分散液中添加陶瓷生片用树脂组合物,利用珠磨机搅拌90分钟后,使用涂布机以干燥后的厚度成为20μm的方式涂覆于经脱模处理的PET膜上。然后,在40℃下加热干燥30分钟,剥离PET膜,由此制作出陶瓷生片。
对于所得到的陶瓷生片,按照JIS K 7113,使用拉伸试验机(岛津制作所公司制,AUTOGRAPH AGS-J),在拉伸速度20mm/分钟的条件下进行拉伸弹性模量(MPa)、断裂点伸长率(%)和断裂点应力(MPa)的测定。
(4)切断截面状态
利用SEM观察“(3)拉伸弹性模量、断裂点伸长率和断裂点应力”测定后的断裂面,按照下述评价基准进行判定。
◎:断裂面无缺口、裂纹、伤痕
○:断裂面无缺口、裂纹,但有伤痕
△:断裂面无缺口,但有裂纹
×:断裂面有缺口
(5)尺寸变化率
利用与“(3)拉伸弹性模量、断裂点伸长率和断裂点应力”相同的方法制作陶瓷生片。使所得到的陶瓷生片在70℃下干燥3小时,算出70℃干燥前后的尺寸变化率,按照以下基准进行评价。
◎:2%以下
○:超过2%且为3%以下
△:超过3%且为4%以下
×:超过4%
[表1]
产业上的可利用性
根据本发明,能够提供陶瓷生片用树脂组合物以及使用了该陶瓷生片用树脂组合物的陶瓷生片及层叠陶瓷电容器,所述陶瓷生片用树脂组合物能够制作即使在制成薄层的情况下也具有高机械强度、不易产生切断后的外观不良、干燥后的尺寸变化的陶瓷生片。
Claims (8)
1.一种陶瓷生片用树脂组合物,其含有聚乙烯醇缩醛树脂,
tanδ的峰顶为1.25以上,并且损耗模量E”为2.30×108Pa以上。
2.根据权利要求1所述的陶瓷生片用树脂组合物,其中,聚乙烯醇缩醛树脂的通过NMR测定和IR测定而定量的羟基的摩尔%换算半峰宽为0.01摩尔%/cm-1~0.15摩尔%/cm-1。
3.根据权利要求1或2所述的陶瓷生片用树脂组合物,其中,相对于聚乙烯醇缩醛树脂100重量份,增塑剂的含量为25重量份以下。
4.根据权利要求1、2或3所述的陶瓷生片用树脂组合物,其中,聚乙烯醇缩醛树脂是皂化度为75摩尔%以上的聚乙烯醇系树脂的缩醛基量。
5.根据权利要求1、2、3或4所述的陶瓷生片用树脂组合物,其中,聚乙烯醇缩醛树脂的缩醛基量为45摩尔%~83摩尔%。
6.根据权利要求1、2、3、4或5所述的陶瓷生片用树脂组合物,其中,聚乙烯醇缩醛树脂的平均聚合度为1000~10000。
7.一种陶瓷生片,其是使用权利要求1、2、3、4、5或6所述的陶瓷生片用树脂组合物而成的。
8.一种层叠陶瓷电容器,其具有权利要求7所述的陶瓷生片。
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CN116057080A (zh) * | 2020-09-30 | 2023-05-02 | 积水化学工业株式会社 | 聚乙烯醇缩醛树脂 |
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US20220186017A1 (en) | 2022-06-16 |
JP6821094B1 (ja) | 2021-01-27 |
EP3950829A4 (en) | 2023-01-11 |
MY189297A (en) | 2022-02-03 |
WO2020203786A1 (ja) | 2020-10-08 |
SG11202110780QA (en) | 2021-10-28 |
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