JP2012180269A - ペロブスカイト構造を有するセラミック粉末の製造方法及びこれにより製造されたペロブスカイト構造を有するセラミック粉末 - Google Patents
ペロブスカイト構造を有するセラミック粉末の製造方法及びこれにより製造されたペロブスカイト構造を有するセラミック粉末 Download PDFInfo
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- 239000000843 powder Substances 0.000 title claims abstract description 81
- 239000000919 ceramic Substances 0.000 title claims abstract description 56
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 65
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 150000001875 compounds Chemical class 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims description 25
- 239000000126 substance Substances 0.000 claims description 11
- 150000003839 salts Chemical group 0.000 claims description 6
- 229910052788 barium Inorganic materials 0.000 claims description 4
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 229910052712 strontium Inorganic materials 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 229910052726 zirconium Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 description 38
- 239000002994 raw material Substances 0.000 description 37
- 230000000052 comparative effect Effects 0.000 description 14
- 239000003985 ceramic capacitor Substances 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- 230000035484 reaction time Effects 0.000 description 5
- RQPZNWPYLFFXCP-UHFFFAOYSA-L barium dihydroxide Chemical compound [OH-].[OH-].[Ba+2] RQPZNWPYLFFXCP-UHFFFAOYSA-L 0.000 description 4
- 229910001863 barium hydroxide Inorganic materials 0.000 description 4
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 4
- 230000007547 defect Effects 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 4
- 238000001027 hydrothermal synthesis Methods 0.000 description 4
- 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
- 229910008651 TiZr Inorganic materials 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 3
- 229910002113 barium titanate Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 description 2
- 229910001626 barium chloride Inorganic materials 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000011222 crystalline ceramic Substances 0.000 description 2
- 229910002106 crystalline ceramic Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000003837 high-temperature calcination Methods 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
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- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
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- 239000007858 starting material Substances 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 238000006386 neutralization reaction Methods 0.000 description 1
- DAWBXZHBYOYVLB-UHFFFAOYSA-J oxalate;zirconium(4+) Chemical compound [Zr+4].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O DAWBXZHBYOYVLB-UHFFFAOYSA-J 0.000 description 1
- CMOAHYOGLLEOGO-UHFFFAOYSA-N oxozirconium;dihydrochloride Chemical compound Cl.Cl.[Zr]=O CMOAHYOGLLEOGO-UHFFFAOYSA-N 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000011882 ultra-fine particle Substances 0.000 description 1
- 150000003754 zirconium Chemical class 0.000 description 1
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Abstract
【解決手段】本発明によるペロブスカイト構造を有するセラミック粉末の製造方法は、ABO3のペロブスカイト構造において、上記Aサイトに該当する元素の化合物と上記Bサイトに該当する元素の化合物を超臨界水と連続式で混合してシード結晶を形成する段階と、上記シード結晶を配置式で混合して粒成長させる段階と、を含む。
【選択図】図1
Description
濃度0.1Mの水酸化バリウム水溶液とTiO2ゾルをそれぞれの供給部に貯蔵した後、ポンプを介して反応管に流入し、反応管内で超臨界水と混合させてシード結晶を生成した。上記連続式反応は、それぞれ351℃、263気圧(atm)(実施例1)及び400℃、232気圧(atm)(実施例2)で施した。その後、上記シード結晶を配置式反応器で24時間反応させ、80nmのBaTiO3の最終粉末を製造した。
濃度0.1Mの水酸化バリウム水溶液とTiO2ゾルを95℃、1気圧(atm)で蒸留水と混合させてシード結晶を生成した。その後、上記シード結晶を配置式反応器で24時間反応させ、80nmのBaTiO3の最終粉末を製造した。
140 ポンプ
160 第1ヒーター
210 配置式反応器
220 インペラ
230 第2ヒーター
Claims (15)
- ABO3のペロブスカイト構造において、上記Aサイトに該当する元素の化合物と上記Bサイトに該当する元素の化合物を超臨界水と連続式で混合してシード結晶を形成する段階と、
上記シード結晶を配置式で混合して粒成長させる段階と、
を含む、ABO3のペロブスカイト構造を有するセラミック粉末の製造方法。 - 上記シード結晶を形成する段階は5秒〜10分間行われる、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記シード結晶を形成する段階は300℃〜500℃の温度及び50〜300の気圧下で行われる、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記シード結晶は、平均粒径が3nm〜20nmであり、結晶軸比(c/a)が1.001〜1.004になるように行われる、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記粒成長させる段階は、150℃〜300℃の温度で行われる、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記粒成長させる段階は、2時間〜100時間行われる、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記粒成長したセラミック粉末は、平均粒径が50nm〜150nmであり、結晶軸比(c/a)が1.005〜1.010である、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記Aサイトに該当する元素の化合物は、塩形態の水溶性物質である、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記Bサイトに該当する元素の化合物は、塩形態の水溶性物質である、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記Bサイトに該当する元素の化合物は、ゾル形態の物質である、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記Aサイトに該当する元素は、Mg、Ca、Sr、Ba及びLaから成る群から選択される1種以上である、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- 上記Bサイトに該当する元素は、Ti及びZrから成る群から選択される1種以上である、請求項1に記載のABO3のペロブスカイト構造を有するセラミック粉末の製造方法。
- ABO3のペロブスカイト構造において、上記Aサイトに該当する元素の化合物と上記Bサイトに該当する元素の化合物を超臨界水と連続式で混合してシード結晶を形成し、上記シード結晶を配置式で混合して粒成長させた、ABO3のペロブスカイト構造を有するセラミック粉末。
- 上記シード結晶は、平均粒径が3nm〜20nmであり、結晶軸比(c/a)が1.001〜1.004である、請求項13に記載のABO3のペロブスカイト構造を有するセラミック粉末。
- 上記粒成長したセラミック粉末は、平均粒径が50nm〜150nmであり、結晶軸比(c/a)が1.005〜1.010である、請求項13に記載のABO3のペロブスカイト構造を有するセラミック粉末。
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JP2015224147A (ja) * | 2014-05-26 | 2015-12-14 | 株式会社ノリタケカンパニーリミテド | 超臨界水を用いたチタン酸バリウムのナノ粒子の製造方法 |
JP2018104230A (ja) * | 2016-12-26 | 2018-07-05 | 住友金属鉱山株式会社 | ペロブスカイト型複合酸化物の製造方法 |
KR20200053157A (ko) * | 2018-11-08 | 2020-05-18 | 고려대학교 산학협력단 | 고속 결정화가 가능한 할로겐화물 페로브스카이트 박막 및 이의 제조방법 |
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