JP2020164375A - チタン酸バリウム粒子を含む非水系分散体及びその製造方法 - Google Patents
チタン酸バリウム粒子を含む非水系分散体及びその製造方法 Download PDFInfo
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- barium titanate
- titanate particles
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- 239000002245 particle Substances 0.000 title claims abstract description 226
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims abstract description 184
- 229910002113 barium titanate Inorganic materials 0.000 title claims abstract description 184
- 239000006185 dispersion Substances 0.000 title claims abstract description 143
- 238000004519 manufacturing process Methods 0.000 title claims description 30
- 239000012736 aqueous medium Substances 0.000 claims abstract description 46
- 239000011164 primary particle Substances 0.000 claims abstract description 26
- 238000005481 NMR spectroscopy Methods 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims description 22
- 238000009826 distribution Methods 0.000 claims description 14
- 239000007791 liquid phase Substances 0.000 claims description 9
- 239000003125 aqueous solvent Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 30
- 239000011248 coating agent Substances 0.000 description 19
- 238000000576 coating method Methods 0.000 description 19
- 239000000463 material Substances 0.000 description 16
- 238000006243 chemical reaction Methods 0.000 description 14
- -1 propio Chemical class 0.000 description 14
- 239000007864 aqueous solution Substances 0.000 description 13
- 239000002270 dispersing agent Substances 0.000 description 13
- 239000002243 precursor Substances 0.000 description 13
- 239000010419 fine particle Substances 0.000 description 12
- 238000005259 measurement Methods 0.000 description 12
- 239000003985 ceramic capacitor Substances 0.000 description 11
- 230000008859 change Effects 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 9
- 238000001035 drying Methods 0.000 description 9
- 150000003609 titanium compounds Chemical class 0.000 description 9
- 229910052788 barium Inorganic materials 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000011010 flushing procedure Methods 0.000 description 8
- 239000002904 solvent Substances 0.000 description 8
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 7
- 150000003839 salts Chemical class 0.000 description 7
- 239000007787 solid Substances 0.000 description 7
- 238000003860 storage Methods 0.000 description 7
- 239000010936 titanium Substances 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 230000002776 aggregation Effects 0.000 description 6
- 230000018044 dehydration Effects 0.000 description 6
- 238000006297 dehydration reaction Methods 0.000 description 6
- 229910052751 metal Inorganic materials 0.000 description 6
- 239000002184 metal Substances 0.000 description 6
- 239000012299 nitrogen atmosphere Substances 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000011347 resin Substances 0.000 description 6
- 229920005989 resin Polymers 0.000 description 6
- 229910052719 titanium Inorganic materials 0.000 description 6
- 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 5
- 238000004220 aggregation Methods 0.000 description 5
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 5
- 229910001863 barium hydroxide Inorganic materials 0.000 description 5
- 159000000009 barium salts Chemical class 0.000 description 5
- 238000004898 kneading Methods 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- FKRBAXZAJBBIAJ-UHFFFAOYSA-N 5-cyano-7-nitro-3-oxido-1,3-benzothiazol-3-ium-2-carboxamide Chemical compound C1=C(C#N)C=C2[N+]([O-])=C(C(=O)N)SC2=C1[N+]([O-])=O FKRBAXZAJBBIAJ-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 4
- 239000011230 binding agent Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 229920000259 polyoxyethylene lauryl ether Polymers 0.000 description 4
- 238000010298 pulverizing process Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- ZUDYPQRUOYEARG-UHFFFAOYSA-L barium(2+);dihydroxide;octahydrate Chemical compound O.O.O.O.O.O.O.O.[OH-].[OH-].[Ba+2] ZUDYPQRUOYEARG-UHFFFAOYSA-L 0.000 description 3
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 3
- 239000000084 colloidal system Substances 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 239000012756 surface treatment agent Substances 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- VBICKXHEKHSIBG-UHFFFAOYSA-N 1-monostearoylglycerol Chemical compound CCCCCCCCCCCCCCCCCC(=O)OCC(O)CO VBICKXHEKHSIBG-UHFFFAOYSA-N 0.000 description 2
- 238000004438 BET method Methods 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- XBDQKXXYIPTUBI-UHFFFAOYSA-M Propionate Chemical compound CCC([O-])=O XBDQKXXYIPTUBI-UHFFFAOYSA-M 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- XXROGKLTLUQVRX-UHFFFAOYSA-N allyl alcohol Chemical compound OCC=C XXROGKLTLUQVRX-UHFFFAOYSA-N 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 150000001553 barium compounds Chemical class 0.000 description 2
- 229910001422 barium ion Inorganic materials 0.000 description 2
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 238000011033 desalting Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- FLKPEMZONWLCSK-UHFFFAOYSA-N diethyl phthalate Chemical compound CCOC(=O)C1=CC=CC=C1C(=O)OCC FLKPEMZONWLCSK-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- 239000002609 medium Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 229910000077 silane Inorganic materials 0.000 description 2
- 238000010532 solid phase synthesis reaction Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
- 229910000349 titanium oxysulfate Inorganic materials 0.000 description 2
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 2
- 239000011882 ultra-fine particle Substances 0.000 description 2
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 description 1
- FFJCNSLCJOQHKM-CLFAGFIQSA-N (z)-1-[(z)-octadec-9-enoxy]octadec-9-ene Chemical compound CCCCCCCC\C=C/CCCCCCCCOCCCCCCCC\C=C/CCCCCCCC FFJCNSLCJOQHKM-CLFAGFIQSA-N 0.000 description 1
- RZRNAYUHWVFMIP-KTKRTIGZSA-N 1-oleoylglycerol Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OCC(O)CO RZRNAYUHWVFMIP-KTKRTIGZSA-N 0.000 description 1
- OAYXUHPQHDHDDZ-UHFFFAOYSA-N 2-(2-butoxyethoxy)ethanol Chemical compound CCCCOCCOCCO OAYXUHPQHDHDDZ-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
- GQTFHSAAODFMHB-UHFFFAOYSA-N 2-prop-2-enoyloxyethanesulfonic acid Chemical compound OS(=O)(=O)CCOC(=O)C=C GQTFHSAAODFMHB-UHFFFAOYSA-N 0.000 description 1
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 1
- NYUTUWAFOUJLKI-UHFFFAOYSA-N 3-prop-2-enoyloxypropane-1-sulfonic acid Chemical compound OS(=O)(=O)CCCOC(=O)C=C NYUTUWAFOUJLKI-UHFFFAOYSA-N 0.000 description 1
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 description 1
- 239000004925 Acrylic resin Substances 0.000 description 1
- 229920000178 Acrylic resin Polymers 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 239000005642 Oleic acid Substances 0.000 description 1
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229920001213 Polysorbate 20 Polymers 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- 239000006087 Silane Coupling Agent Substances 0.000 description 1
- 235000021355 Stearic acid Nutrition 0.000 description 1
- ULUAUXLGCMPNKK-UHFFFAOYSA-N Sulfobutanedioic acid Chemical compound OC(=O)CC(C(O)=O)S(O)(=O)=O ULUAUXLGCMPNKK-UHFFFAOYSA-N 0.000 description 1
- XTXRWKRVRITETP-UHFFFAOYSA-N Vinyl acetate Chemical compound CC(=O)OC=C XTXRWKRVRITETP-UHFFFAOYSA-N 0.000 description 1
- AQKOHYMKBUOXEB-RYNSOKOISA-N [(2R)-2-[(2R,3R,4S)-4-hydroxy-3-(16-methylheptadecanoyloxy)oxolan-2-yl]-2-(16-methylheptadecanoyloxy)ethyl] 16-methylheptadecanoate Chemical compound CC(C)CCCCCCCCCCCCCCC(=O)OC[C@@H](OC(=O)CCCCCCCCCCCCCCC(C)C)[C@H]1OC[C@H](O)[C@H]1OC(=O)CCCCCCCCCCCCCCC(C)C AQKOHYMKBUOXEB-RYNSOKOISA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 150000003973 alkyl amines Chemical class 0.000 description 1
- 150000004996 alkyl benzenes Chemical class 0.000 description 1
- 150000005215 alkyl ethers Chemical class 0.000 description 1
- 125000005233 alkylalcohol group Chemical group 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000000149 argon plasma sintering Methods 0.000 description 1
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 1
- 229910001626 barium chloride Inorganic materials 0.000 description 1
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Inorganic materials [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
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- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- USIUVYZYUHIAEV-UHFFFAOYSA-N diphenyl ether Chemical compound C=1C=CC=CC=1OC1=CC=CC=C1 USIUVYZYUHIAEV-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000010130 dispersion processing Methods 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- YQEMORVAKMFKLG-UHFFFAOYSA-N glycerine monostearate Natural products CCCCCCCCCCCCCCCCCC(=O)OC(CO)CO YQEMORVAKMFKLG-UHFFFAOYSA-N 0.000 description 1
- RZRNAYUHWVFMIP-HXUWFJFHSA-N glycerol monolinoleate Natural products CCCCCCCCC=CCCCCCCCC(=O)OC[C@H](O)CO RZRNAYUHWVFMIP-HXUWFJFHSA-N 0.000 description 1
- SVUQHVRAGMNPLW-UHFFFAOYSA-N glycerol monostearate Natural products CCCCCCCCCCCCCCCCC(=O)OCC(O)CO SVUQHVRAGMNPLW-UHFFFAOYSA-N 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009775 high-speed stirring Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000005660 hydrophilic surface Effects 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000005394 methallyl group Chemical group 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 239000012457 nonaqueous media Substances 0.000 description 1
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 1
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 1
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000000256 polyoxyethylene sorbitan monolaurate Substances 0.000 description 1
- 235000010486 polyoxyethylene sorbitan monolaurate Nutrition 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 239000000249 polyoxyethylene sorbitan monopalmitate Substances 0.000 description 1
- 235000010483 polyoxyethylene sorbitan monopalmitate Nutrition 0.000 description 1
- 239000001818 polyoxyethylene sorbitan monostearate Substances 0.000 description 1
- 235000010989 polyoxyethylene sorbitan monostearate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- UIIIBRHUICCMAI-UHFFFAOYSA-N prop-2-ene-1-sulfonic acid Chemical compound OS(=O)(=O)CC=C UIIIBRHUICCMAI-UHFFFAOYSA-N 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
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- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- 150000003608 titanium Chemical class 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- NLVXSWCKKBEXTG-UHFFFAOYSA-N vinylsulfonic acid Chemical compound OS(=O)(=O)C=C NLVXSWCKKBEXTG-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A90/00—Technologies having an indirect contribution to adaptation to climate change
- Y02A90/30—Assessment of water resources
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Ceramic Capacitors (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
Description
本発明に係る非水系分散体は、非水系媒体中のチタン酸バリウム粒子の比表面積A1を高度に制御、即ち、チタン酸バリウム粒子の非水系媒体への濡れ性を高めたものである。親水性の表面を有するチタン酸バリウムに対し、互いに強い粒子間凝集をさせることなく非水系の分散媒に分散させることによって、分散性及び保存安定性を向上させたものである。得られる非水系分散体は、積層セラミックコンデンサーの内部電極層用共材に用いるチタン酸バリウム粒子を含む非水系分散体として好適である。
[測定条件]
パルスNMR:Xigo nanotools社製Acorn Area
測定温度:25℃
測定試料A:チタン酸バリウム粒子を含む非水系分散体
測定試料B:測定試料Aの遠心分離上澄み液(10,000rpm、60分)
<数1>
A1={[(Rav/Rb)−1]×Rb}/(0.0016×Ψp)
<数1>中、A1はチタン酸バリウム粒子を含む非水系分散体のチタン酸バリウム粒子の比表面積(m2/g)を示す。Ravは測定試料Aを用いて得られたパルスNMRの緩和時間の逆数を示す。Rbは測定試料Bを用いて得られたパルスNMRの緩和時間の逆数を示す。Ψpは下記<数2>によって算出される。
<数2>
Ψp=(Sc/Sd)/[(1−Sc)/Td]
<数2>中、Scは、測定試料Aの固形分濃度(重量%)を示す。Sdは測定試料Aの密度(g/cm3)を示す。Tdは測定試料Bの上澄み液の密度(g/cm3)を示す。
A2=6/(P50×d)
<数3>中、P50はチタン酸バリウム粒子の一次粒径(μm=103nm)を示す。dはチタン酸バリウム粒子の真比重の6.02g/cm3を示す。
<数4>
D=(D90−D10)/D50
分散度DはD10からD90までの分布の広がりをD50で割ったもので、粒度分布の広がりの指標となり、Dが1.0以下になると、単分散に近いと云われる。
粘度変化率(%)=(V2−V1)/V1×100
△:粘度変化率が±10%を超えて、±30%以下
×:粘度変化率が30%を超える
◎:L*が30.0以下のもの
○:L*が30.0を超えて35.0以下のもの
△:L*が35.0を超えて40.0以下のもの
×:L*が40.0を超えたもの
<チタン酸バリウム粒子含水ケーキの製造:第一及び第二工程>
水酸化バリウム八水塩1120重量部を純水に溶解、精製したものを塩化チタン水溶液688重量部に滴下・中和して水酸化チタンコロイドを得た。次に、水酸化バリウム八水塩1280重量部を水に溶解、精製したものを温度70℃、pH12.5で窒素雰囲気の反応容器中に保持した。次に、前記水酸化チタンコロイドを前記水酸化バリウム水溶液に8分間かけて投入した。該混合溶液を反応温度70℃で2時間かけてチタン酸バリウム前駆体粒子を生成した。得られたチタン酸バリウム前駆体粒子をチタン酸バリウム粒子とみなし、室温まで冷却して第一工程を終了した後、次に示す第二工程へ移った。ヌッチェで窒素雰囲気下にてろ液にBaイオンが認められなくなるまで水洗し、ろ過、圧縮を行って、固形分濃度50重量%のチタン酸バリウム粒子含水ケーキを得た。(チタン酸バリウム粒子含水ケーキ名:BTO−1)
得られたチタン酸バリウム粒子含水ケーキBTO−1、600重量部(即ち、チタン酸バリウム粒子300重量部)を窒素雰囲気下、40℃にて2軸ニーダーにて、60rpmにて3時間混練し、水系スラリーとし、第三工程を終了した。これに、ジヒドロターピニルアセテート200重量部、ポリオキシエチレンラウリルエーテルカルボン酸9重量部を加え(第四工程)、窒素雰囲気下で40℃にて2時間混練すると、チタン酸バリウム粒子がジヒドロタービニルアセテート相にフラッシングされ、水が分離されていることを確認した。その後、2軸ニーダーを傾け、水を200重量部排出した(第五工程)。続いて、ジヒドロターピニルアセテートを100重量部加えて、40℃にて3時間、0.05mmHgにて、混練しながら、真空脱水した。残った水分を1重量%以下にして、チタン酸バリウム粒子を含む非水系スラリーとした(第六工程)。これに、さらにポリオキシエチレンラウリルエーテルカルボン酸9重量部と、ジヒドロターピニルアセテート132重量部を加え、ダルトン製超音波ホモジナイザーにて分散操作を10分間行い、本発明に係るチタン酸バリウム粒子を含む非水系分散体を得た(第七工程)。
実施例1のチタン酸バリウム粒子の合成条件において反応温度70℃で1時間と変化させた以外は、前記チタン酸バリウム粒子含水ケーキ1と同様にして、チタン酸バリウム粒子含水ケーキを得た。(チタン酸バリウム粒子含水ケーキ名:BTO−2)
チタン酸バリウム粒子含水ケーキBTO−1、600重量部を窒素雰囲気下80℃で乾燥し、チタン酸バリウム粒子300重量部を得た。これにポリオキシエチレンラウリルエーテルカルボン酸18重量部、ジヒドロターピニルアセテート432重量部を加えて、ダルトン製超音波ホモジナイザーにて分散操作を行い、チタン酸バリウム粒子を含む非水系分散体を得た。
チタン酸バリウム粒子の種類、並びに非水系媒体及び分散剤の量を変化させた以外は前記比較例1と同様にして、チタン酸バリウム粒子を含む非水系分散体とそれを用いた塗膜塗膜を得た。
Claims (4)
- 一次粒径100nm以下のチタン酸バリウム粒子を含む非水系分散体であって、パルスNMR測定から算出されたチタン酸バリウム粒子の比表面積A1と、一次粒径から算出されたチタン酸バリウム粒子の比表面積A2との比であるA1/A2が0.5〜1.0であることを特徴とする非水系分散体。
- 一次粒径100nm以下のチタン酸バリウム粒子を含む非水系分散体であって、パルスNMR測定から算出されたチタン酸バリウム粒子の比表面積A1が10〜100m2/gであることを特徴とする非水系分散体。
- チタン酸バリウム粒子を含む非水系分散体の散乱強度分布において、n%の分散粒径をDnとするとき、D50が100nm以下であって、分散度(D90−D10)/D50の値が1.0以下である請求項1又は2記載の非水系分散体。
- 請求項1〜3のいずれかに記載のチタン酸バリウム粒子を含む非水系分散体の製造方法であって、水溶媒の液相法により合成されたチタン酸バリウム粒子を含む水系スラリーをフラッシングにより非水系媒体に転相することで調製される非水系分散体の製造方法。
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