JP5151477B2 - 半導体磁器組成物とその製造方法 - Google Patents
半導体磁器組成物とその製造方法 Download PDFInfo
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- JP5151477B2 JP5151477B2 JP2007514850A JP2007514850A JP5151477B2 JP 5151477 B2 JP5151477 B2 JP 5151477B2 JP 2007514850 A JP2007514850 A JP 2007514850A JP 2007514850 A JP2007514850 A JP 2007514850A JP 5151477 B2 JP5151477 B2 JP 5151477B2
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- 229910052573 porcelain Inorganic materials 0.000 title claims description 17
- 239000000843 powder Substances 0.000 claims description 150
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- 229910052758 niobium Inorganic materials 0.000 claims description 8
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- 229910052693 Europium Inorganic materials 0.000 claims description 7
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 7
- 229910052787 antimony Inorganic materials 0.000 claims description 6
- 229910052727 yttrium Inorganic materials 0.000 claims description 6
- 229910052797 bismuth Inorganic materials 0.000 claims description 5
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Description
材料学会第109回セラミックス材料部門委員会予稿集 13−14 (2003) J. Soc. Mat. Sci., Japan, Vol 52, 1155−1159 (2003)
主原料としてBaCO3、TiO2、半導体化元素としてLa2O3の原料粉末を準備し、(Ba0.994La0.006)TiO3となるように配合し、さらに、焼結助剤としてSiO2を0.3mol%、CaCO3を1.2mol%を添加し、エタノール中で混合した。得られた混合原料粉末を1000℃で4時間仮焼し、(BaLa)TiO3仮焼粉を用意した。
主原料としてBaCO3、TiO2、半導体化元素としてLa2O3、キュリー温度のシフターとしてNa2CO3、Bi2O3、TiO2を準備し、[(Bi0.5Na0.5)0.1(Ba0.994La0.006)0.9]TiO3となるように、組成物を構成する全ての元素を最初から配合し、さらに、焼結助剤としてSiO2を0.4mol%、CaCO3を1.4mol%添加し、エタノール中(湿式)で混合した。得られた混合原料粉末を、窒素中で200℃〜1200℃で4時間仮焼し、仮焼粉を得た。得られた[(Bi0.5Na0.5)0.1(Ba0.994La0.006)0.9]TiO3仮焼粉の200℃〜900℃における仮焼温度毎のX線回折パターンを図2に示す。
主原料としてBaCO3、TiO2、半導体化元素としてLa2O3の原料粉末を準備し、(Ba0.994La0.006)TiO3となるように配合し、さらに、焼結助剤としてSiO2を0.3mol%、CaCO3を1.2mol%添加し、エタノール中で混合した。得られた混合原料粉末を1000℃で4時間仮焼し、(BaLa)TiO3仮焼粉を用意した。
主原料としてBaCO3、TiO2、半導体化元素としてLa2O3、キュリー温度のシフターとしてNa2CO3、Bi2O3、TiO2を準備し、[(Bi0.5Na0.5)0.1(Ba0.994La0.006)0.9]TiO3となるように、組成物を構成する全ての元素を最初から配合し、さらに、焼結助剤としてSiO2を0.4mol%、CaCO3を1.4mol%を添加し、エタノール中で混合した後、該原料混合粉を、大気中で1000℃で4時間仮焼した。
主原料としてBaCO3、TiO2、半導体化元素としてLa2O3の原料粉末を準備し、(Ba0.994La0.006)TiO3となるように配合し、エタノール中で混合した。得られた混合原料粉末を1000℃で4時間仮焼し、(BaLa)TiO3仮焼粉を用意した。
主原料としてBaCO3、TiO2、半導体化元素としてLa2O3の原料粉末を準備し、(Ba0.994La0.006)TiO3となるように配合し、エタノール中で混合した。得られた混合原料粉末を1000℃で4時間仮焼し、(BaLa)TiO3仮焼粉を用意した。
主原料としてBaCO3、TiO2、半導体化元素としてLa2O3、キュリー温度のシフターとしてNa2CO3、Bi2O3、TiO2を準備し、[(Bi0.5Na0.5)0.1(Ba0.994La0.006)0.9]TiO3となるように、組成物を構成する全ての元素を仮焼前(原料配合段階)に混合し、エタノール中で混合した。得られた混合原料粉末を、窒素中で1000℃で4時間仮焼し、仮焼粉を得た。
実施例4により得られた(BaLa)TiO3仮焼粉と(BiNa)TiO3仮焼粉を[(Bi0.5Na0.5)0.1(Ba0.994La0.006)0.9]TiO3となるように配合し、エタノールを媒体としてポットミルにより、混合仮焼粉が0.9μmになるまで混合、粉砕した後、乾燥させた。該混合仮焼粉の粉砕粉にPVAを添加、混合した後、造粒装置によって造粒した。得られた造粒粉を一軸プレス装置で成形し、上記成形体を500℃で脱バインダー後、酸素濃度が1%未満の窒素雰囲気中において、表2に示す焼結温度、焼結時間で焼結した後、表6に示す冷却速度で冷却し、焼結体を得た。なお、表6の冷却速度におけるクエンチとは、冷却速度が550℃/hrを超える急冷によるものである。
TCR=(lnR1−lnRc)×100/(T1−Tc)
Rcは最大比抵抗、RcはTcにおける比抵抗、T1はR1を示す温度、Tcはキュリー温度である。
Claims (17)
- 組成式を[(BiNa) x (Ba 1−y R y ) 1−x ]TiO 3 (但し、RはLa、Dy、Eu、Gd、Yの少なくとも一種)を表し、前記x、yが、0<x≦0.2、0<y≦0.02を満足する半導体磁器組成物の製造方法であって、(BaR)TiO3仮焼粉(但し、RはLa、Dy、Eu、Gd、Yの少なくとも一種)を用意する工程、(BiNa)TiO3仮焼粉を用意する工程、(BaR)TiO3仮焼粉と(BiNa)TiO3仮焼粉を混合する工程、混合仮焼粉を、成形、焼結する工程とを含む半導体磁器組成物の製造方法。
- 組成式を[(BiNa) x Ba 1−x ][Ti 1−z M z ]O 3 (但し、MはNb、Ta、Sbのうち少なくとも一種)を表し、前記x、zが、0<x≦0.2、0<z≦0.005を満足する半導体磁器組成物の製造方法であって、Ba(TiM)O 3 仮焼粉(但し、MはNb、Ta、Sbのうち少なくとも一種)を用意する工程、(BiNa)TiO 3 仮焼粉を用意する工程、Ba(TiM)O 3 仮焼粉と(BiNa)TiO 3 仮焼粉を混合する工程、混合仮焼粉を、成形、焼結する工程とを含む半導体磁器組成物の製造方法。
- (BaR)TiO3仮焼粉を用意する工程において、仮焼温度が900℃〜1300℃である請求項1に記載の半導体磁器組成物の製造方法。
- Ba(TiM)O 3 仮焼粉を用意する工程において、仮焼温度が900℃〜1300℃である請求項2に記載の半導体磁器組成物の製造方法。
- (BiNa)TiO3仮焼粉を用意する工程において、仮焼温度が700℃〜950℃である請求項1または2に記載の半導体磁器組成物の製造方法。
- (BaR)TiO3仮焼粉と(BiNa)TiO3仮焼粉を混合する工程において、混合を乾式にて行う請求項1、3及び5のいずれか1項に記載の半導体磁器組成物の製造方法。
- Ba(TiM)O 3 仮焼粉と(BiNa)TiO 3 仮焼粉を混合する工程において、混合を乾式にて行う請求項2、4及び5のいずれか1項に記載の半導体磁器組成物の製造方法。
- (BaR)TiO3仮焼粉を用意する工程又は(BiNa)TiO3仮焼粉を用意する工程あるいはその両工程において、仮焼前に、Si酸化物を3.0mol%以下、Ca炭酸塩又はCa酸化物を4.0mol%以下添加する請求項1、3、5及び6のいずれか1項に記載の半導体磁器組成物の製造方法。
- Ba(TiM)O 3 仮焼粉を用意する工程又は(BiNa)TiO 3 仮焼粉を用意する工程あるいはその両工程において、仮焼前に、Si酸化物を3.0mol%以下、Ca炭酸塩又はCa酸化物を4.0mol%以下添加する請求項2、4、5及び7のいずれか1項に記載の半導体磁器組成物の製造方法。
- (BaR)TiO3仮焼粉と(BiNa)TiO3仮焼粉を混合する工程において、Si酸化物を3.0mol%以下、Ca炭酸塩又はCa酸化物を4.0mol%以下添加する請求項1、3、5及び6のいずれか1項に記載の半導体磁器組成物の製造方法。
- Ba(TiM)O 3 仮焼粉と(BiNa)TiO 3 仮焼粉を混合する工程において、Si酸化物を3.0mol%以下、Ca炭酸塩又はCa酸化物を4.0mol%以下添加する請求項2、4、5及び7のいずれか1項に記載の半導体磁器組成物の製造方法。
- 焼結工程が、酸素濃度1%未満の不活性ガス雰囲気中において実行される請求項1〜11のいずれか1項に記載の半導体磁器組成物の製造方法。
- 焼結工程が、焼結温度1290℃〜1350℃で4時間未満の焼結時間で実行される請求項1〜12のいずれか1項に記載の半導体磁器組成物の製造方法。
- 焼結工程が、焼結温度1290℃〜1350℃で下記式を満足する焼結時間で実行され、次いで、下記式を満足する冷却速度で焼結後の冷却が実行される請求項1〜12のいずれか1項に記載の半導体磁器組成物の製造方法。
式:ΔT≧25t、但し、t=焼結時間(hr)、ΔT=焼結後の冷却速度(℃/hr) - BiとNaの比が、Bi/Na=0.78〜1の関係を満足する請求項1〜14のいずれか1項に記載の半導体磁器組成物の製造方法。
- (BaR)TiO3仮焼粉(Rは半導体化元素でLa、Dy、Eu、Gd、Yの少なくとも一種)と(BiNa)TiO3仮焼粉との混合仮焼粉を成形、焼結して得られた半導体磁器組成物であり、組成式を[(BiNa)x(Ba1−yRy)1−x]TiO3と表し、x、yが、0<x≦0.2、0<y≦0.02を満足し、BiとNaの比が、Bi/Na=0.78〜1の関係を満足する半導体磁器組成物。
- Ba(TiM)O3仮焼粉(Mは半導体化元素でNb、Ta、Sbのうち少なくとも一種)と(BiNa)TiO3仮焼粉との混合仮焼粉を成形、焼結して得られた半導体磁器組成物であり、組成式を[(BiNa)xBa1−x][Ti1−zMz]O3と表し、x、zが、0<x≦0.2、0<z≦0.005を満足し、BiとNaの比が、Bi/Na=0.78〜1の関係を満足する半導体磁器組成物。
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JP5251119B2 (ja) * | 2007-12-26 | 2013-07-31 | 日立金属株式会社 | 半導体磁器組成物 |
KR100941522B1 (ko) | 2008-01-17 | 2010-02-10 | 한국세라믹기술원 | 납성분을 포함하지 않는 ptc 써미스터용 세라믹 조성물및 이에 의해 제조되는 ptc 세라믹 써미스터 |
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JPS56169301A (en) * | 1980-06-02 | 1981-12-26 | Tohoku Metal Ind Ltd | Method of producing barium titanate semiconductor porcelain |
JP2005255493A (ja) * | 2004-03-12 | 2005-09-22 | Neomax Co Ltd | 半導体磁器組成物 |
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US20080170977A1 (en) | 2008-07-17 |
TW200706511A (en) | 2007-02-16 |
US8557724B2 (en) | 2013-10-15 |
KR20120037016A (ko) | 2012-04-18 |
WO2006118274A1 (ja) | 2006-11-09 |
TWI389868B (zh) | 2013-03-21 |
KR101189293B1 (ko) | 2012-10-09 |
EP1876157A4 (en) | 2011-10-26 |
CN102674831A (zh) | 2012-09-19 |
CN101213155A (zh) | 2008-07-02 |
US20100075825A1 (en) | 2010-03-25 |
CN102674831B (zh) | 2016-01-20 |
KR20080012855A (ko) | 2008-02-12 |
US7704906B2 (en) | 2010-04-27 |
JPWO2006118274A1 (ja) | 2008-12-18 |
EP1876157A1 (en) | 2008-01-09 |
CN101213155B (zh) | 2012-11-21 |
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