JP6032679B2 - 単一相の立方晶チタン酸バリウム微粒子、それを含有する分散体およびその製造方法 - Google Patents
単一相の立方晶チタン酸バリウム微粒子、それを含有する分散体およびその製造方法 Download PDFInfo
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- JP6032679B2 JP6032679B2 JP2013205199A JP2013205199A JP6032679B2 JP 6032679 B2 JP6032679 B2 JP 6032679B2 JP 2013205199 A JP2013205199 A JP 2013205199A JP 2013205199 A JP2013205199 A JP 2013205199A JP 6032679 B2 JP6032679 B2 JP 6032679B2
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- barium titanate
- titanate fine
- fine particles
- barium
- polyvinylpyrrolidone
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- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 title claims description 138
- 229910002113 barium titanate Inorganic materials 0.000 title claims description 138
- 239000010419 fine particle Substances 0.000 title claims description 121
- 239000006185 dispersion Substances 0.000 title claims description 25
- 238000004519 manufacturing process Methods 0.000 title claims description 12
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 60
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 60
- 239000002245 particle Substances 0.000 claims description 59
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 55
- 239000007864 aqueous solution Substances 0.000 claims description 39
- 238000010438 heat treatment Methods 0.000 claims description 27
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical group [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 19
- 229910001422 barium ion Inorganic materials 0.000 claims description 18
- 239000003002 pH adjusting agent Substances 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 claims description 12
- 239000002612 dispersion medium Substances 0.000 claims description 12
- 239000012798 spherical particle Substances 0.000 claims description 12
- 239000010936 titanium Substances 0.000 claims description 12
- 229910052719 titanium Inorganic materials 0.000 claims description 12
- -1 titanium ions Chemical class 0.000 claims description 9
- 230000002194 synthesizing effect Effects 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 description 29
- 238000006243 chemical reaction Methods 0.000 description 28
- 239000013078 crystal Substances 0.000 description 23
- 239000000843 powder Substances 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 14
- 239000012071 phase Substances 0.000 description 14
- 238000002441 X-ray diffraction Methods 0.000 description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 239000002904 solvent Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 9
- 238000003786 synthesis reaction Methods 0.000 description 9
- 150000002894 organic compounds Chemical class 0.000 description 8
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 6
- 238000010304 firing Methods 0.000 description 6
- 238000001027 hydrothermal synthesis Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 5
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 4
- 229910001626 barium chloride Inorganic materials 0.000 description 4
- 239000003989 dielectric material Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000002002 slurry Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 3
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 3
- 229910052788 barium Inorganic materials 0.000 description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 3
- 229960004106 citric acid Drugs 0.000 description 3
- 150000002500 ions Chemical class 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- HNJBEVLQSNELDL-UHFFFAOYSA-N pyrrolidin-2-one Chemical compound O=C1CCCN1 HNJBEVLQSNELDL-UHFFFAOYSA-N 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000010532 solid phase synthesis reaction Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 description 2
- 159000000009 barium salts Chemical class 0.000 description 2
- 239000003985 ceramic capacitor Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000001939 inductive effect Effects 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000002195 soluble material Substances 0.000 description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 2
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 description 2
- 239000013585 weight reducing agent Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- YASYEJJMZJALEJ-UHFFFAOYSA-N Citric acid monohydrate Chemical compound O.OC(=O)CC(O)(C(O)=O)CC(O)=O YASYEJJMZJALEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- BCKXLBQYZLBQEK-KVVVOXFISA-M Sodium oleate Chemical compound [Na+].CCCCCCCC\C=C/CCCCCCCC([O-])=O BCKXLBQYZLBQEK-KVVVOXFISA-M 0.000 description 1
- CFOBMZGYYIVJKZ-UHFFFAOYSA-N [Na].CCCCCC Chemical compound [Na].CCCCCC CFOBMZGYYIVJKZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 1
- 150000001553 barium compounds Chemical class 0.000 description 1
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 1
- 229910001863 barium hydroxide Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000007810 chemical reaction solvent Substances 0.000 description 1
- 229960002303 citric acid monohydrate Drugs 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000002050 diffraction method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002296 dynamic light scattering Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000010335 hydrothermal treatment Methods 0.000 description 1
- 230000001678 irradiating effect Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000011859 microparticle Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- BTURAGWYSMTVOW-UHFFFAOYSA-M sodium dodecanoate Chemical compound [Na+].CCCCCCCCCCCC([O-])=O BTURAGWYSMTVOW-UHFFFAOYSA-M 0.000 description 1
- 229940082004 sodium laurate Drugs 0.000 description 1
- RYYKJJJTJZKILX-UHFFFAOYSA-M sodium octadecanoate Chemical compound [Na+].CCCCCCCCCCCCCCCCCC([O-])=O RYYKJJJTJZKILX-UHFFFAOYSA-M 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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- Inorganic Compounds Of Heavy Metals (AREA)
Description
Claims (4)
- 球状の粒子形状を有し、平均粒子径が40から1500nm、その粒子径の変動係数が25.0%以下であって、4重量%以上のポリビニルピロリドンによって包まれていることを特徴とする単一相の立方晶チタン酸バリウム微粒子。
- 請求項1に記載のチタン酸バリウム微粒子が、分散媒に分散された単一相の立方晶チタン酸バリウム微粒子分散体。
- 前記分散媒が、水であることを特徴とする請求項2に記載の単一相の立方晶チタン酸バリウム微粒子分散体。
- チタンイオンとバリウムイオンとを含む水溶液に反応剤としてpH調整剤を加えて、加熱することによりチタン酸バリウム微粒子を合成するに際し、前記チタンイオンとバリウムイオンとを含む水溶液にポリビニルピロリドンが含まれ、
前記水溶液中のポリビニルピロリドンの最終濃度は、40g/l以上であり、
前記pH調整剤は、80℃以下の水酸化カリウム溶液であり、
前記pH調整剤の最終濃度は、pH調整剤濃度/チタンイオン濃度で定義される濃度比で8〜18であり、
前記加熱における加熱温度は90℃から120℃の範囲である
ことを特徴とする単一相の立方晶チタン酸バリウム微粒子の製造方法。
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IT1270828B (it) * | 1993-09-03 | 1997-05-13 | Chon Int Co Ltd | Processo per la sintesi di polveri ceramiche cristalline di composti di perovskite |
US6268054B1 (en) * | 1997-02-18 | 2001-07-31 | Cabot Corporation | Dispersible, metal oxide-coated, barium titanate materials |
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