JP4875703B2 - チタン酸バリウムの製造方法 - Google Patents
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Description
TiO(OH)2+Ba(OH)2・8H2O → BaTiO3+10H2O
TiO2+BaSO4+H2 → BaTiO3+SO2+H2O
メタチタン酸0.5M分散液 1.0Lを製造して、水酸化バリウム0.6Mの水溶液1.0Lを原料出発物質として使用した。この二つの水溶液を、テフロン(登録商標)ライニングされた3L内部容積のSUS反応器に投入して密閉した後、反応温度を5.0℃/minで上昇した。反応器上端の攪拌機を利用して300rpmの速度で攪拌し、反応温度が180℃に至ると2時間維持して冷却させた。反応溶液の温度が常温に至ると、反応器下端のバルブを開けて反応生成物溶液を回収し、水洗水のpH変化がないまで数回蒸留水で洗浄した後、噴霧乾燥して乾燥粉末を回収した。この粉末を雰囲気制御型高温炉に入れて、空気雰囲気で1100℃の温度で2時間焼成した。焼成後、回収された粉末を、XRDを利用してBa/Tiモル比を分析した結果、0.987であって、XRDを利用したk−factor分析結果、2.3を示した。XRFを利用した定量分析結果、S含量は、840ppmであった。BET法による比表面積は、2.6m2/gであって、FE−SEMを利用した粒子形状及び大きさ分析結果、粒子状が非定形で均一ではなく、粒子間凝集が相対的に多くて、球状当たり平均粒度は、0.42マイクロメートルであった(図3参照)。この粉末はX7R特性(EIA規格)を満足するものであった。この粉末を圧縮して直径10mm、厚さ3mmのディスクを製造し、1320℃の温度で焼結した。製造されたディスク試片の焼結密度は、5.6g/cm3であり、両面にIn/Gaペーストを塗って乾燥し、電気特性分析を行った結果、誘電率 1850、DF 0.1%、IR 1.7*1011であって、TCC分析結果、125℃で4.2%、−55℃で24.2%の誘電率変化を示した。
Claims (5)
- 誘電材料であるチタン酸バリウムの製造方法であって、
a)含水チタン酸化合物、結晶性酸化チタン、及びバリウム水酸化物を出発物質として、60〜300℃の温度、5〜50kgf/cm2の圧力下で10分〜10時間水熱反応する段階と、
b)生成物を乾燥して回収する段階と、
c)乾燥粉末を還元雰囲気下で600〜1400℃の温度で10分〜5時間 焼成する段階と、を含み、
前記バリウム水酸化物を、含水チタン酸に対し過量にして、過量分に該当する当量の結晶性酸化チタンと共に水熱反応に供することを特徴とする、チタン酸バリウムの製造方法。 - 含水チタン酸は、メタチタン酸(TiO(OH)2)、オルトチタン酸(Ti(OH)4)、チタン水酸化物(TiO2xH2O)、またはこれらの混合物から選択されることを特徴とする、請求項1に記載のチタン酸バリウムの製造方法。
- 結晶性酸化チタンは、アナターゼ酸化チタン(anatase TiO2)、ルチル酸化チタン(rutile TiO2)、ブルカイト酸化チタン(brookite TiO2)、またはこれらの混合物であることを特徴とする、請求項1又は2に記載のチタン酸バリウムの製造方法。
- 乾燥する段階は、固形分の損失無しに粉末を回収する噴霧乾燥または熱風乾燥方法を利用することを特徴とする、請求項1に記載のチタン酸バリウムの製造方法。
- 焼成する段階は、窒素、アルゴン、またはヘリウムから選択される不活性ガス99.9〜90重量%と水素0.1〜10重量%との混合ガスを利用することを特徴とする、請求項1に記載のチタン酸バリウムの製造方法。
Applications Claiming Priority (3)
Application Number | Priority Date | Filing Date | Title |
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KR10-2005-0071204 | 2005-08-04 | ||
KR1020050071204A KR100633723B1 (ko) | 2005-08-04 | 2005-08-04 | 티탄산바륨의 제조방법 |
PCT/KR2006/003025 WO2007015622A1 (en) | 2005-08-04 | 2006-08-01 | Process for preparing barium titanate |
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JP2009502725A JP2009502725A (ja) | 2009-01-29 |
JP4875703B2 true JP4875703B2 (ja) | 2012-02-15 |
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US (1) | US7854916B2 (ja) |
JP (1) | JP4875703B2 (ja) |
KR (1) | KR100633723B1 (ja) |
CN (1) | CN101238069B (ja) |
TW (1) | TWI324988B (ja) |
WO (1) | WO2007015622A1 (ja) |
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PL2358641T3 (pl) | 2008-11-04 | 2014-11-28 | Sachtleben Pigments Oy | Sposób wytwarzania tytanianów |
TWI412505B (zh) * | 2009-03-12 | 2013-10-21 | Hanwha Chemical Corp | 微細之以鈦酸鋇為基質之複合氧化物 |
JP2012523369A (ja) * | 2009-04-10 | 2012-10-04 | イーストー,インコーポレイティド | 混合金属酸化物セラミック粉体の湿式化学調製の水熱プロセス |
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TWI421882B (zh) * | 2009-06-08 | 2014-01-01 | Daiken Chemical Co Ltd | Barium titanate powder, nickel paste, preparation method and laminated ceramic capacitors |
KR101104627B1 (ko) * | 2009-06-11 | 2012-01-12 | 씨큐브 주식회사 | 나노크기를 갖는 티탄산바륨 입자 및 그의 제조 방법 |
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GB2534069B (en) * | 2013-08-23 | 2020-12-30 | Sakai Chemical Industry Co | Method for producing barium titanate powder |
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US6264912B1 (en) * | 1999-09-10 | 2001-07-24 | Ut-Battelle, Llc | Methods for producing monodispersed particles of barium titanate |
JP3780851B2 (ja) * | 2000-03-02 | 2006-05-31 | 株式会社村田製作所 | チタン酸バリウムおよびその製造方法ならびに誘電体セラミックおよびセラミック電子部品 |
US6409983B1 (en) * | 2000-07-11 | 2002-06-25 | Korea Institute Of Science And Technology | Process for preparing crystalline barium titanate powder |
JP3780405B2 (ja) * | 2000-08-11 | 2006-05-31 | 株式会社村田製作所 | 微粒チタン酸バリウム粉末、カルシウム変性微粒チタン酸バリウム粉末、ならびにその製造方法 |
US7431911B2 (en) * | 2001-07-04 | 2008-10-07 | Showa Denko K.K. | Barium titanate and production and process thereof |
JP4200427B2 (ja) * | 2001-12-28 | 2008-12-24 | 株式会社村田製作所 | 複合酸化物粉末の製造方法 |
US6692721B2 (en) * | 2002-01-15 | 2004-02-17 | Samsung Electro-Mechanics Co., Ltd. | Method for preparing barium titanate powder by oxalate synthesis |
JP4186529B2 (ja) * | 2002-07-09 | 2008-11-26 | 昭栄化学工業株式会社 | 高結晶性複酸化物粉末の製造方法 |
WO2004092070A1 (en) * | 2003-04-11 | 2004-10-28 | Showa Denko K. K. | Perovskite titanium-containing composite oxide particle, production process and uses thereof |
KR100542374B1 (ko) * | 2003-07-22 | 2006-01-11 | 한국에너지기술연구원 | 티탄산 바륨 분말의 제조 방법 |
WO2005097705A1 (en) * | 2004-04-07 | 2005-10-20 | Techpowder S.A. | Ultrafine metal oxide production |
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WO2007015622A1 (en) | 2007-02-08 |
US20090202425A1 (en) | 2009-08-13 |
TWI324988B (en) | 2010-05-21 |
US7854916B2 (en) | 2010-12-21 |
CN101238069B (zh) | 2011-04-20 |
KR100633723B1 (ko) | 2006-10-13 |
CN101238069A (zh) | 2008-08-06 |
JP2009502725A (ja) | 2009-01-29 |
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