JP5526552B2 - サーミスタ用金属酸化物焼結体、サーミスタ素子及びサーミスタ温度センサ並びにサーミスタ用金属酸化物焼結体の製造方法 - Google Patents
サーミスタ用金属酸化物焼結体、サーミスタ素子及びサーミスタ温度センサ並びにサーミスタ用金属酸化物焼結体の製造方法 Download PDFInfo
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- C01G45/1264—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing rare earth, e.g. La1-xCaxMnO3, LaMnO3
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Description
自動車エンジン周りの触媒温度等を測定するには、1000℃付近の高温まで測定可能なサーミスタ素子が求められるが、このような高温用サーミスタに重要な特性として、高温での抵抗値変化が少ないことが挙げられる。しかしながら、上記従来の材料では高温保持試験において抵抗値低下がやや大きく、用途によっては使用できない場合があった。
したがって、本発明は、上記知見から得られたものであり、前記課題を解決するために以下の構成を採用した。
そこで、上記本発明のサーミスタ用金属酸化物焼結体及びその製造方法で得られた仮焼粉では、一般式:(La1−yYy)1−zAz(Cr1−xMnx)O3(ただし、A=CaとSrとの少なくとも一方、0.0≦x≦1.0、0.0<y<1.0、0.0<z≦0.7)で示される複合酸化物を含み、AサイトのLaの一部をYやCa若しくはSrで置換しているので、Laを予め少なくした状態を得ることができる。さらに、ペロブスカイト酸化物のAサイト中に100%元素を入れることができ、焼結体中に未反応のLa2O3が残ることを防ぐことができる。これにより、抵抗値変化率を2%以下に抑制することができる。Ca若しくはSrの割合を増加させると、さらに抵抗値変化率を1%以下に抑制することができる。このサーミスタ用金属酸化物焼結体は、(Y、La)とCa,Srとの比率を変化させることによって、1000〜4200KのB定数とすることが可能である。特に、B定数が2500K以下の材料については、従来のものに比べてB定数が低く、非常に広い範囲の温度(−50℃から1100℃程度)を測定することが可能である。
なお、CrとMnとの比率を変化させることによってもB定数を変えることができるが、同時に1000℃での抵抗値変化が大きくなってしまい、耐熱性が悪くなってしまう不都合がある。しかしながら、本発明では、Ca,Srを添加することで、B定数を低下させることができると同時に、1000℃での良好な耐熱性を実現することができる。
(Y、La)をCaやSrで単に置換するとB定数が低くなると共に抵抗値が小さくなり、特にCaやSrの濃度が大きい材料では、高温で抵抗値が非常に小さくなってしまい、高温域の温度検出の精度が悪くなる不都合がある。しかしながら、本発明のサーミスタ用金属酸化物焼結体では、複合酸化物に絶縁体材料が添加されているので、絶縁体材料の添加量によって抵抗値を大きくすることができる。すなわち、添加した絶縁体材料により電気伝導のパスを少なくし、抵抗値を上昇させることが可能であり、添加量を調整することで、抵抗値調整が可能になる。
なお、絶縁体材料としては、Y2O3、MgO,CeO2,ZrO2、Al2O3等が採用可能である。
また、ペロブスカイト酸化物にYが含まれていることで、Y2O3と混合焼結させた際、焼成を助成し高密度の成型体が作製できる。さらに、Y2O3膜析出を助長し高い耐熱性、高い耐還元性を実現している。
すなわち、ペロブスカイト酸化物にLaとYとCa若しくはSrの全ての元素を含ませることで、B定数が低く広範囲温度の測定ができると共に、高い耐熱性、高い耐還元性を実現している。
すなわち、このサーミスタ用金属酸化物焼結体の製造方法では、ペロブスカイト酸化物にCa若しくはSrが含まれていることで、焼成時に、焼結助剤としてCaCO3若しくはSrCO3を添加することで、さらに焼成を助成することができ、より高密度の成型体が作製できる。
すなわち、本発明に係るサーミスタ用金属酸化物焼結体及びそのサーミスタ用金属酸化物焼結体の製造方法によれば、一般式:(La1−yYy)1−zAz(Cr1−xMnx)O3(ただし、A=CaとSrとの少なくとも一方、0.0≦x≦1.0、0.0<y<1.0、0.0<z≦0.7)で示される複合酸化物を含むので、Aサイトの(Y、La)の一部をCa若しくはSrで置換してAサイト中に100%元素を入れることで、焼結体中に未反応のLa2O3が残ることを防ぐことができ、抵抗値変化率を2%以下に抑制することができる。Ca若しくはSrの割合を増加させると、さらに抵抗値変化率を1%以下に抑制することができる。同時に、B定数を低下させ、広範囲の温度測定が可能となる。さらに、ペロブスカイト酸化物にYを含ませることで、絶縁体材料Y2O3と混合焼結させた際、抵抗値上昇させる効果だけでなく、複合酸化物焼結体部の表面にY2O3層が形成されているので、複合酸化物焼結体部から酸素が還元によって奪われることを表面のY2O3層が抑制して、抵抗値変化を抑えて、良好な耐熱性及び耐還元性を得ることができる。
したがって、本発明のサーミスタ素子は、高温域での経時変化が小さく低温域から高温域までの広範囲で十分な測定精度が得られ、特に自動車エンジン周りの触媒温度や排気系温度を検出する高温測定用センサとして好適である。
また、このサーミスタ用金属酸化物焼結体では、複合酸化物に絶縁体材料が添加されていることが好ましい。なお、絶縁体材料としては、MgO,CeO2,ZrO2、Al2O3、Y2O3等が採用可能であるが、特に、Y2O3が好ましい。
次に、これらLa2O3、Y2O3、CaCO3及びSrCO3の少なくとも一方、Cr2O3及びMnO2の各粉末を秤量後にボールミルに入れ、Zrボールとエタノールとを適量入れて約24時間混合を行う。なお、Mn化合物については、MnCO3やMn3O4、Mn2O3を使用しても構わない。この混合したものを取り出して乾燥させた後、1300℃、5時間にて焼成し、例えば、上記一般式においてA=Ca、x=0.4、y=0.5、z=0.3、w=0.0とされた(La0.5Y0.5)0.7Ca0.3(Cr0.6Mn0.4)O3の仮焼粉を得る。
なお、仮焼粉にY2O3を添加しない場合であっても、焼結助剤CaCO3若しくはSrCO3を少量添加することが好ましい。また、Zrボールとエタノールとを用いてボールミルで混合粉砕することが好ましい。
さらに、焼成時に、焼結助剤としてCaCO3とSrCO3との少なくとも一方を添加することで、さらに焼成を助成することができ、より高密度の成型体が作製できる。
R25=25℃の抵抗値(Ω)
R50=50℃の抵抗値(Ω)
T25=25℃を絶対温度に換算した値(=298.15K)
T50=50℃を絶対温度に換算した値(=323.15K)
これらの結果より、YとLaとCa若しくはSrとの組み合わせであることが、抵抗値変化率を抑える要因となっていることがわかる。
Claims (8)
- NTCサーミスタに用いられる金属酸化物焼結体であって、
一般式:(La1−yYy)1−zAz(Cr1−xMnx)O3(ただし、A=CaとSrとの少なくとも一方、0.0≦x≦1.0、0.0<y<1.0、0.0<z≦0.7)で示される複合酸化物を含むことを特徴とするサーミスタ用金属酸化物焼結体。 - 請求項1に記載のサーミスタ用金属酸化物焼結体において、
前記複合酸化物に絶縁体材料が添加されていることを特徴とするサーミスタ用金属酸化物焼結体。 - 請求項1又は2に記載のサーミスタ用金属酸化物焼結体において、
一般式:1−w(La1−yYy)1−zAz(Cr1−xMnx)O3+wY2O3(ただし、A=CaとSrとの少なくとも一方、0.0≦x≦1.0、0.0<y<1.0、0.0<z≦0.7、0.0<w≦0.8)で示される複合酸化物を含むことを特徴とするサーミスタ用金属酸化物焼結体。 - NTCサーミスタに用いられるサーミスタ素子であって、
請求項1から3のいずれか一項に記載のサーミスタ用金属酸化物焼結体と、
前記サーミスタ用金属酸化物焼結体に一端が固定された少なくとも一対のリード線と、を有することを特徴とするサーミスタ素子。 - 請求項4に記載のサーミスタ素子を備えていることを特徴とするサーミスタ温度センサ。
- NTCサーミスタに用いられる金属酸化物焼結体の製造方法であって、
La2O3、Y2O3、ACO3、Cr2O3及びMnO2の各粉末を混合し焼成して、一般式:(La1−yYy)1−zAz(Cr1−xMnx)O3(ただし、A=CaとSrとの少なくとも一方、0.0≦x≦1.0、0.0<y<1.0、0.0<z≦0.7)で示される複合酸化物の仮焼粉を得る工程と、
前記仮焼粉を成型して焼成する工程と、を有していることを特徴としているサーミスタ用金属酸化物焼結体の製造方法。 - 請求項6に記載のサーミスタ用金属酸化物焼結体の製造方法において、
前記仮焼粉にさらにY2O3の粉末を加えて混合し、一般式:1−w(La1−yYy)1−zAz(Cr1−xMnx)O3+wY2O3(ただし、A=CaとSrとの少なくとも一方、0.0≦x≦1.0、0.0<y<1.0、0.0<z≦0.7、0.0<w≦0.8)で示される仮焼粉を含む混合物を得る工程を有し、
前記焼成する工程が、前記混合物を成型して焼成することを特徴とするサーミスタ用金属酸化物焼結体の製造方法。 - 請求項6又は7に記載のサーミスタ用金属酸化物焼結体の製造方法において、
前記焼成する工程で、前記仮焼粉又は前記仮焼粉を含む混合物に焼結助剤としてCaCO3とSrCO3との少なくとも一方を添加することを特徴とするサーミスタ用金属酸化物焼結体の製造方法。
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GB1111351.1A GB2479293B (en) | 2009-01-30 | 2009-07-17 | Sintered metal oxide for thermistor, thermistor element, thermistor temperature sensor, and method for producing sintered metal oxide for thermistor |
PCT/JP2009/003371 WO2010086915A1 (ja) | 2009-01-30 | 2009-07-17 | サーミスタ用金属酸化物焼結体及びサーミスタ素子及びサーミスタ温度センサ並びにサーミスタ用金属酸化物焼結体の製造方法 |
DE112009004324T DE112009004324T5 (de) | 2009-01-30 | 2009-07-17 | Sintermetalloxid fiir Thermistor, Thermistorelement, Thermistortemperatursensor und Verfahren zur Erzeugung eines Sintermetalloxides fuir Thermistor |
US13/145,262 US8466771B2 (en) | 2009-01-30 | 2009-07-17 | Sintered metal oxide for thermistor, thermistor element, thermistor temperature sensor, and method for producing sintered metal oxide for thermistor |
CN200980155791.2A CN102300829B (zh) | 2009-01-30 | 2009-07-17 | 金属氧化物烧结体及其制备方法、热敏电阻元件和温度传感器 |
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KR101908775B1 (ko) | 2015-04-06 | 2018-10-16 | 니뽄 도쿠슈 도교 가부시키가이샤 | 도전성 산화물 소결체, 그것을 사용한 서미스터 소자 및 온도 센서 |
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JP6440641B2 (ja) * | 2016-01-08 | 2018-12-19 | 日本特殊陶業株式会社 | 導電性酸化物焼結体、これを用いたサーミスタ素子、および、これを用いた温度センサ |
CN105753474A (zh) * | 2016-03-31 | 2016-07-13 | 中国科学院新疆理化技术研究所 | 一种锶掺杂铬酸镧热敏电阻材料 |
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