JP4592696B2 - 超伝導酸化物を用いる有機金属蒸着用の前駆溶液の製造方法及び有機金属蒸着法による薄膜型超伝導体の製造方法 - Google Patents
超伝導酸化物を用いる有機金属蒸着用の前駆溶液の製造方法及び有機金属蒸着法による薄膜型超伝導体の製造方法 Download PDFInfo
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- JP4592696B2 JP4592696B2 JP2006520123A JP2006520123A JP4592696B2 JP 4592696 B2 JP4592696 B2 JP 4592696B2 JP 2006520123 A JP2006520123 A JP 2006520123A JP 2006520123 A JP2006520123 A JP 2006520123A JP 4592696 B2 JP4592696 B2 JP 4592696B2
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- H10N60/0268—Manufacture or treatment of devices comprising copper oxide
- H10N60/0296—Processes for depositing or forming copper oxide superconductor layers
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Description
しかしながら、これまでの化学溶液方法による高温超伝導薄膜を製造するために用いられた金属有機溶媒の中で最も優れた特性を見せるのはトリフルオロ酢酸(Trifluoracetate、TFA)溶液であった。
ここで、超伝導原料粉末-TFA前駆溶液の総陽イオン濃度は0.1ないし6モルであることが望ましい。
ここで、薄い膜を塗布する段階は、回転させるスピンコーティングや、ディップコーティングまたは、スプレー方式、転写方式を用いることが望ましい。
以下の説明において、本発明のより完全な理解を手助けするために図面による説明が追加されるが、当業者にとって、本発明は図面の詳細な説明がなくても実施可能であることは自明であろう。
場合によっては、本発明の要旨を不要に分かりにくくするような開示された特徴部または要素に対しては、その説明を省略する。これは本発明の説明を不要にあいまいにすることを回避するためである。
図2は、超伝導原料粉末-TFA溶液のか焼熱処理過程を示す図である。
図3は、超伝導薄膜の合成熱処理工程を示す図である。
図4は、超伝導合成熱処理後のX-線分析の結果を示す図である。
これにより、酸化物超伝導相が(c)軸に配列される構造を有することが分かる。
図5、6、7、8は、この試料の微細組織の観察結果であって、超伝導結晶粒が生成されることを示す図である。
図9は、これらの試料の超伝導臨界温度を測定した結果であって、89.3K以下で超伝導体の状態に転換することを示す図である。
図10は、この試料の超伝導臨界電流を測定した結果であって、薄膜の厚さが0.3μmで、幅が3mmであるので、臨界電流密度は0.85MA/cm2を有することが分かる。
粉末が完全に溶解されて溶液が透明になると、その溶液の温度を80°C未満に維持して、その溶液が粘性のゼリー状に変化するまで溶液を蒸発させる。
溶液の流動性がほぼ完全になくなると、加熱を中断し、溶液を冷やす。
常温で固まったゼリー状の化合物を20ccのメチルアルコールに溶かして、総陽イオン濃度が1〜6モルの超伝導原料粉末-TFA前駆溶液を得る。
LaAlO3単結晶基板に前駆溶液を滴下するか、ディップコーティング、スピンコーディングや、または、スプレー方式、転写方式などの方法を用いて薄い膜を塗布した後、乾燥させて前駆体薄膜を製造する。
この時、か焼熱処理過程は、20〜75°Cの飽和水蒸気を含む酸素や窒素、アルゴンまたはそれらの混合気体の雰囲気で1分当り0.5〜1°C程度の加熱速度で300〜500°Cまで加熱して金属イオンを含む前駆体を分解させる。
転換熱処理は、か焼された薄膜がエピタクシャルに成長した酸化物超伝導体薄膜に転換されるように、100〜1000ppmの酸素を含有する窒素またはアルゴンと20〜75°Cの露点を有する水蒸気の存在下で650〜850°Cの温度で、0.25〜4時間熱処理することによって行われる。
転換熱処理中に、薄膜は1分当たり5〜20°Cの加熱速度で650〜850°Cまで加熱され、酸化物と酸素フッ化物とから構成されている、か焼された薄膜がREBCO酸化物の超伝導体相に完全に転換されるまで0.25〜4時間維持される。
冷却中に400〜500°Cの温度範囲で乾燥した酸素雰囲気で1〜4時間維持して、形成された超伝導相に酸素が十分に満たされるようにする。
図2は、超伝導原料粉末-TFA溶液のか焼熱処理過程を示す図である。
図3は、超伝導薄膜の合成熱処理工程を示す図である。
図4は、製造された超伝導薄膜のX-線回折分析の結果を示す図である。
図5は、製造された超伝導薄膜の微細組織を示す図である。
図6は、製造された超伝導薄膜の微細組織を示す図である。
図7は、製造された超伝導薄膜の微細組織を示す図である。
図8は、製造された超伝導薄膜の微細組織を示す図である。
図9は、超伝導薄膜の臨界転移温度の測定結果を示す図である。
図10は、製造された超伝導薄膜の臨界電流密度の測定結果を示す図である。
Claims (12)
- 超伝導酸化物を用いる有機金属蒸着用の前駆溶液の製造方法において、
REBa2Cu3O7−x(REは希土類元素またはこれらの組合せ、0<x<0.5)系の超伝導原料粉末をトリフルオロ酢酸溶液に分散させた後に加熱して溶解させる段階と、
粉末が完全に溶解されて溶液が透明になると熱板の温度を上げて温度を80℃未満に維持して溶液を蒸発させ、粘性のあるゼリー状になるまで加熱を続ける段階と、
該溶液の流動性が完全になくなると加熱を中断して該溶液を冷却する段階と、
常温で固まったゼリー状の化合物を有機溶媒に溶かして超伝導原料粉末-トリフルオロ酢酸前駆溶液を得る段階と、を含むことを特徴とする超伝導酸化物を用いる有機金属蒸着用の前駆溶液の製造方法。 - 超伝導原料粉末-トリフルオロ酢酸前駆溶液の総陽イオン濃度が0.1ないし6モルであることを特徴とする請求項1記載の超伝導酸化物を用いる有機金属蒸着用の前駆溶液の製造方法。
- 前記超伝導原料粉末が、Y、Sm、Nd以外に他の希土類金属が含まれている123化合物 (Ya、Ybb、Smc、Lad、Nde、Hof、Gdg...)1Ba2Cu3O7−x(a+b+c+d+e+f+g+..=1、0<x<0.5)の粉末であることを特徴とする請求項1記載の超伝導酸化物を用いる有機金属蒸着用の前駆溶液の製造方法。
- 前記有機溶媒が、メチルアルコール、エチルアルコール、メトキシエタノール(メチロールグリコールモノメチルエーテル)のうちの何れかであることを特徴とする請求項1記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
- 有機金属蒸着法を用いた薄膜型超伝導体の製造方法において、
超伝導原料粉末をトリフルオロ酢酸溶液に溶かした後に温度を加えて溶解させる段階と、
粉末が完全に溶解されて溶液が透明になると該熱板内の温度を上げて溶液を蒸発させ、粘性のあるゼリー状になるまで加熱を続ける段階と、
該溶液の流動性が完全になくなると加熱を中断して該溶液を冷却する段階と、
常温で固まったゼリー状の化合物を有機溶媒に溶かして超伝導原料粉末-トリフルオロ酢酸前駆溶液を得る段階と、
集合組織を有する金属や単結晶の金属基板に該超伝導原料粉末-トリフルオロ酢酸前駆溶液を滴下して薄い膜を塗布する段階と、
該薄い膜を塗布した後に乾燥させて薄膜を形成する段階と、
該薄膜をか焼及び焼成熱処理して薄膜が超伝導特性を有する段階と、を含むことを特徴とする有機金属蒸着法を用いた薄膜型超伝導体の製造方法。 - 前記薄い膜を塗布する段階は、回転させるスピンコーティングやディップコーティング、またはスプレー方式、転写方式を用いることを特徴とする請求項5記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
- 前記薄い膜を塗布する操作が集合組織を有する金属基板もしくは単結晶基板の上に行われ;集合組織を有する金属基板もしくは単結晶基板は、その上に塗布されたセラミック中間層を有し、金属表面上の超伝導層との反応を防止し基板の2軸配向された集合組織の結晶性を超伝導層に伝達する機能を有し;該集合組織を有する金属基板は、圧延熱処理されたNi、Ni系の合金、銀もしくは銀合金、および立方晶金属のうちの1つからなることを特徴とする請求項5記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
- 超伝導原料粉末-トリフルオロ酢酸前駆溶液の総陽イオン濃度は0.1ないし6モルであることを特徴とする請求項5記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
- 超伝導原料粉末が、REBa2Cu3O7−x(RE=Y、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Luなど希土類元素またはこれらの組合せ)の粉末であることを特徴とする請求項5記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
- 前記超伝導原料粉末が、Y、Sm、Nd以外に他の希土類金属が含まれている123化合物(Ya、Ybb、Smc、Lad、Nde、Hof、Gdg...)1Ba2Cu3O7−x(a+b+c+d+e+f+g+..=1、0<x<0.5)の粉末であることを特徴とする請求項5記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
- 前記有機溶媒が、メチルアルコール、エチルアルコール、メトキシエタノール(メチロールグリコールモノメチルエーテル)のうちの何れかであることを特徴とする請求項5記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
- 前記最終の超伝導薄膜の厚さが0.1μm以上であることを特徴とする請求項5記載の有機金属蒸着法を用いた薄膜型超伝導体の製造方法。
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US7286032B2 (en) * | 2003-07-10 | 2007-10-23 | Superpower, Inc. | Rare-earth-Ba-Cu-O superconductors and methods of making same |
US8227019B2 (en) * | 2003-12-15 | 2012-07-24 | Superpower Inc. | High-throughput ex-situ method for rare-earth-barium-copper-oxide (REBCO) film growth |
EP1655787A1 (en) * | 2004-11-03 | 2006-05-10 | Nexans | Precursor composition for YBCO-based superconductors |
JP4208806B2 (ja) * | 2004-09-16 | 2009-01-14 | 株式会社東芝 | 酸化物超電導体の製造方法 |
-
2003
- 2003-07-18 KR KR10-2003-0049157A patent/KR100529602B1/ko active IP Right Grant
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2004
- 2004-07-15 DE DE112004001309T patent/DE112004001309B4/de not_active Expired - Fee Related
- 2004-07-15 WO PCT/KR2004/001756 patent/WO2005007576A1/en active Application Filing
- 2004-07-15 JP JP2006520123A patent/JP4592696B2/ja not_active Expired - Fee Related
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2006
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Also Published As
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JP2007530398A (ja) | 2007-11-01 |
US7625843B2 (en) | 2009-12-01 |
KR100529602B1 (ko) | 2005-11-17 |
WO2005007576A1 (en) | 2005-01-27 |
US20060246216A1 (en) | 2006-11-02 |
DE112004001309B4 (de) | 2009-11-19 |
DE112004001309T5 (de) | 2006-05-11 |
KR20050010193A (ko) | 2005-01-27 |
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