JP5448514B2 - Thin film superconducting wire and manufacturing method thereof - Google Patents
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Description
本発明は、薄膜超電導線材及びその製造方法に係り、特に、基材上に酸化物超電導薄膜を形成する際の、中間層としての酸化物薄膜の製造に関する。 The present invention relates to a thin film superconducting wire and a method for producing the same, and more particularly to the production of an oxide thin film as an intermediate layer when an oxide superconducting thin film is formed on a substrate.
酸化物超電導体は、その導体としての特性が結晶方位に大きく依存するので、高い臨界電流密度（Ｊｃ）を有する超電導導体を製造するためには、超電導体の結晶配向性を向上させることが必要である。また、酸化物超電導体を導体として用いるためには、金属テープを基材として、結晶配向性の優れた超電導体の多結晶薄膜を作製する技術が必要である。 Oxide superconductors have a characteristic that their properties as a conductor greatly depend on the crystal orientation, so it is necessary to improve the crystal orientation of the superconductor in order to produce a superconductor having a high critical current density (Jc). It is. Further, in order to use an oxide superconductor as a conductor, a technique for producing a polycrystalline thin film of a superconductor excellent in crystal orientation using a metal tape as a base material is necessary.
また、酸化物超電導薄膜のＪｃを向上させるためには、超電導薄膜の製造後に酸素ガスを含む雰囲気中で加熱処理を行い、酸化物超電導薄膜層に酸素を取り込むことが有効である。 In order to improve the J c of the oxide superconducting thin film is subjected to heat treatment in an atmosphere containing oxygen gas after production of the superconducting thin film, it is effective to incorporate oxygen to the oxide superconducting thin film layer.
しかし、金属製の基材を用いる場合、加熱処理中に金属元素が超電導薄膜中へ拡散し、超電導特性を低下させるという問題がある。このため、加熱処理中の超電導薄膜中への金属元素の拡散を防ぐために、金属テープと酸化物超電導薄膜の間に金属元素の拡散係数が小さい材料からなる層を介在させた積層構造とする方法がある。 However, when a metal substrate is used, there is a problem that the metal element diffuses into the superconducting thin film during the heat treatment, thereby degrading the superconducting characteristics. Therefore, in order to prevent diffusion of the metal element into the superconducting thin film during the heat treatment, a method of forming a laminated structure in which a layer made of a material having a small diffusion coefficient of the metal element is interposed between the metal tape and the oxide superconducting thin film There is.
上記のような金属テープと、金属元素の拡散防止層を含む中間層と、超電導層の積層構造において、超電導層の結晶配向性を向上させる方法として、薄膜作成中のイオンビームアシストを利用して、中間層薄膜の結晶配向性を向上させる方法（例えば、特許文献１参照）や、結晶配向性に優れた金属基材上に配向金属基板法によって薄膜を成長させることで、２軸配向した超電導薄膜を得る方法（例えば、特許文献１参照）がある。 As a method for improving the crystal orientation of the superconducting layer in the laminated structure of the metal tape, the intermediate layer including the metal element diffusion preventing layer, and the superconducting layer, ion beam assist during thin film formation is used. Biaxially oriented superconductivity by improving the crystal orientation of the intermediate layer thin film (see, for example, Patent Document 1) or by growing the thin film on a metal substrate having excellent crystal orientation by the oriented metal substrate method There is a method for obtaining a thin film (for example, see Patent Document 1).
これらの２つの技術は共に、超電導層と中間層の薄膜積層構造を作成する必要があるが、積層薄膜の作製時に成長させる薄膜の結晶配向性は、テンプレートとする基材もしくは下層薄膜層の結晶配向性を引き継ぐホモエピタキシャル成長となるため、超電導層の結晶配向性を向上させるためには、そのテンプレートとなる中間層薄膜の結晶配向性を向上させる必要がある。 Both of these two technologies require the creation of a thin film stack structure of a superconducting layer and an intermediate layer, but the crystal orientation of the thin film grown during the preparation of the stacked thin film depends on the crystal of the substrate or lower layer thin film layer used as a template. Since the homoepitaxial growth takes over the orientation, in order to improve the crystal orientation of the superconducting layer, it is necessary to improve the crystal orientation of the intermediate layer thin film serving as the template.
本発明は、以上のような事情の下になされ、中間層薄膜の結晶配向性を向上させた薄膜超電導線材及びその製造方法を提供することを目的とする。 The present invention has been made under the circumstances as described above, and an object thereof is to provide a thin film superconducting wire having improved crystal orientation of an intermediate layer thin film and a method for producing the same.
上記課題を解決するため、本発明の第１の態様は、金属基板と、前記金属基板上に形成された、Ｃｅ、Ｚｒ、Ｙ、Ｇｄ、Ｍｇ、Ｓｒ、及びＴｉからなる群から選ばれた少なくとも１種の元素を含む複数種類の成分構成を有する複数層の金属酸化物膜を有する中間層と、前記中間層上に形成された超電導膜を有する通電層とを備える薄膜超電導線材であって、前記中間層は、ＣｅＯ ２ からなる第１の酸化物膜と、前記第１の酸化物膜上に形成された第２の酸化物膜を有し、前記第２の酸化物膜の形成後の前記第１の酸化物膜の格子定数は、前記第２の酸化物膜の形成前の格子定数よりも大きいことを特徴とする薄膜超電導線材を提供する。 In order to solve the above problems, the first aspect of the present invention is selected from the group consisting of a metal substrate and Ce, Zr, Y, Gd, Mg, Sr, and Ti formed on the metal substrate. A thin film superconducting wire comprising: an intermediate layer having a plurality of layers of metal oxide films having a plurality of types of components including at least one element; and an energization layer having a superconducting film formed on the intermediate layer. The intermediate layer has a first oxide film made of CeO 2 and a second oxide film formed on the first oxide film, and after the formation of the second oxide film The thin film superconducting wire is characterized in that the lattice constant of the first oxide film is larger than the lattice constant before the formation of the second oxide film.
本発明の第２の態様は、金属基板と、前記金属基板上に形成された、Ｃｅ、Ｚｒ、Ｙ、Ｇｄ、Ｍｇ、Ｓｒ、及びＴｉからなる群から選ばれた少なくとも１種の元素を含む複数種類の成分構成を有する複数層の金属酸化物膜を有する中間層と、前記中間層上に形成された超電導膜を有する通電層とを備える薄膜超電導線材の製造方法であって、（ａ）前記金属基板上にエレクトロンビーム蒸着法またはスパッタリング法によってＣｅＯ ２ からなる第１の酸化物膜を成膜する工程と、（ｂ）前記第１の酸化物膜の酸素量を減少させる条件で第２の酸化物膜を成膜する工程とを具備することを特徴とする薄膜超電導線材の製造方法を提供する。 The second aspect of the present invention includes a metal substrate and at least one element selected from the group consisting of Ce, Zr, Y, Gd, Mg, Sr, and Ti formed on the metal substrate. A method for producing a thin film superconducting wire comprising an intermediate layer having a plurality of layers of metal oxide films having a plurality of types of component structures, and an energizing layer having a superconducting film formed on the intermediate layer, comprising: a step of forming a first oxide film consisting of CeO 2 by electron beam evaporation or sputtering on the metal substrate, a second under a condition that reduces the amount of oxygen (b) the first oxide film A method for producing a thin film superconducting wire, comprising the step of:
このような本発明の第２の態様に係る薄膜超電導線材の製造方法において、前記工程（ｂ）を、Ａｒ雰囲気中またはＡｒおよび酸素の混合ガス雰囲気中で、前記第１の酸化物膜上に、第２の酸化物膜を成膜することにより行うことが出来る。 In the method of manufacturing a thin film superconducting wire according to the second aspect of the present invention, the step (b) is performed on the first oxide film in an Ar atmosphere or a mixed gas atmosphere of Ar and oxygen. This can be done by forming a second oxide film.
或いは、前記工程（ｂ）を、酸素を含む雰囲気中で前記第1の酸化物膜を加熱する条件で前記第２の酸化物膜を成膜することにより行うが出来る。 Alternatively, the step (b) can be performed by forming the second oxide film under a condition in which the first oxide film is heated in an atmosphere containing oxygen.
なお、前記第２の酸化物膜上に、第３の酸化物膜を形成することが出来る。 Note that a third oxide film can be formed over the second oxide film.
本発明によると、第1の酸化物膜を成膜した後、第1の酸化物膜中の酸素量を減少させる条件で第２の酸化物膜を形成することにより、第１の酸化物膜の格子定数を、第２の酸化物膜の形成後において、第２の酸化物膜の形成前よりも大きくすることが出来、それによって結晶配向性に優れた中間層薄膜、ひいては結晶配向性に優れた超電導膜を得ることが出来る。 According to the present invention, after the first oxide film is formed, the first oxide film is formed by forming the second oxide film under a condition that reduces the amount of oxygen in the first oxide film. The lattice constant of the intermediate layer film can be made larger after the second oxide film is formed than before the second oxide film is formed. An excellent superconducting film can be obtained.
以下、本発明の実施形態について説明する。 Hereinafter, embodiments of the present invention will be described.
図１は、本発明の一実施形態に係る薄膜超電導線材を示す断面図である。図１において、金属基板１上に中間層２及び通電層３が形成されることにより、薄膜超電導線材が構成されている。 FIG. 1 is a cross-sectional view showing a thin film superconducting wire according to an embodiment of the present invention. In FIG. 1, a thin film superconducting wire is formed by forming an intermediate layer 2 and a conductive layer 3 on a metal substrate 1.
中間層２は、Ｃｅ、Ｚｒ、Ｙ、Ｇｄ、Ｍｇ、Ｓｒ、及びＴｉからなる群から選ばれた少なくとも１種の元素を含む複数層の金属酸化物膜を有するものであり、金属基板１上に形成された第１の酸化物膜と、この第１の酸化物膜上に形成された第２の酸化物膜とを有している。この場合、第２の酸化物膜の形成後の第１の酸化物膜の格子定数は、第２の酸化物膜の形成前の格子定数よりも大きい。 The intermediate layer 2 has a plurality of metal oxide films containing at least one element selected from the group consisting of Ce, Zr, Y, Gd, Mg, Sr, and Ti. A first oxide film formed on the first oxide film, and a second oxide film formed on the first oxide film. In this case, the lattice constant of the first oxide film after the formation of the second oxide film is larger than the lattice constant before the formation of the second oxide film.
金属基板は、Ｎｉ合金からなることが望ましい。Ｎｉ合金としては、Ｗ、Ｍｏ、Ｃｒ、Ｖ、Ｆｅ、Ｃｕ、Ｎｂ、Ｔａ、Ｔｉ、Ｓｉ、Ｓｉ、Ａｌ、Ｂ、及びＣからなる群から選ばれる少なくとも１種を含むＮｉ合金を挙げることが出来る。これらの添加元素の添加量は、１〜８０原子％であることが望ましい。具体的なＮｉ合金としては、ハステロイ、インコネル、ステンレスを挙げることが出来る。 The metal substrate is preferably made of a Ni alloy. Examples of the Ni alloy include an Ni alloy containing at least one selected from the group consisting of W, Mo, Cr, V, Fe, Cu, Nb, Ta, Ti, Si, Si, Al, B, and C. I can do it. The addition amount of these additive elements is desirably 1 to 80 atomic%. Specific examples of the Ni alloy include Hastelloy, Inconel, and stainless steel.
中間層を構成する金属酸化物膜の具体例としては、ＣｅＯ２、Ｙ２Ｏ３、イットリア安定化ジルコニア（ＹＳＺ）、Ｚｒ２Ｒｅ２Ｏ７（Ｒｅは、Ｙ、Ｇｄ、Ｃｅ、ＬａおよびＮｄからなる群から選ばれた１種）、ＳｒＴｉＯ３、ＳｒＲｕＯ３が挙げられる。 Specific examples of the metal oxide film constituting the intermediate layer include CeO 2 , Y 2 O 3 , yttria-stabilized zirconia (YSZ), Zr 2 Re 2 O 7 (Re is Y, Gd, Ce, La, and Nd). 1 type selected from the group consisting of: SrTiO 3 , SrRuO 3 .
金属酸化物膜の膜厚は特に限定されないが、通常５０〜２００ｎｍであり、中間層全体の膜厚は、通常１５０〜６００ｎｍである。 Although the film thickness of a metal oxide film is not specifically limited, Usually, it is 50-200 nm, and the film thickness of the whole intermediate | middle layer is 150-600 nm normally.
なお、複数の酸化物膜のうち、下地の第１の酸化物膜の格子定数を、第２の酸化物膜の形成前よりも形成後で大きくするには、金属基板上に第1の酸化物膜を成膜した後、この第１の酸化物膜の酸素量を減少させる条件で第２の酸化物膜を成膜すればよい。そのための方法として、以下の２つを挙げることが出来る。 In order to increase the lattice constant of the first oxide film as a base after the formation of the second oxide film among the plurality of oxide films, the first oxidation film is formed on the metal substrate. After the physical film is formed, the second oxide film may be formed under a condition that reduces the amount of oxygen in the first oxide film. The following two methods can be cited as methods for that purpose.
１．第１の酸化物膜上に第２の酸化物膜を成膜するに際し、Ａｒ雰囲気または、Ａｒと酸素の混合ガス雰囲気で行うこと。 1. The second oxide film is formed over the first oxide film in an Ar atmosphere or a mixed gas atmosphere of Ar and oxygen.
Ａｒと酸素の混合ガス雰囲気の場合の酸素の分圧は、５．０×１０-３Ｐａ以下が望ましく、好ましくは、６．６×１０-６Ｐａ以上かつ５．０×１０-３Ｐａ以下である。 The partial pressure of oxygen in the mixed gas atmosphere of Ar and oxygen is desirably 5.0 × 10 −3 Pa or less, preferably 6.6 × 10 −6 Pa or more and 5.0 × 10 −3 Pa or less. It is.
第１の酸化物膜上に、Ａｒと酸素の混合ガス雰囲気で第２の酸化物膜を成膜することにより、第1の酸化物膜の格子定数を増加することが出来る。 By forming the second oxide film on the first oxide film in a mixed gas atmosphere of Ar and oxygen, the lattice constant of the first oxide film can be increased.
２．酸素を含む雰囲気で第１の酸化物膜を加熱する条件で前記第２の酸化物膜を成膜すること。 2. The second oxide film is formed under a condition in which the first oxide film is heated in an atmosphere containing oxygen.
酸素を含む雰囲気中の酸素の分圧は、５．０×１０-３Ｐａ以下が望ましく、好ましくは、６．６×１０-６Ｐａ以上かつ５．０×１０-３Ｐａ以下である。また、加熱温度は、３００〜７００℃が望ましく、より好ましくは、４００〜６５０℃である。 The partial pressure of oxygen in the atmosphere containing oxygen is desirably 5.0 × 10 −3 Pa or less, preferably 6.6 × 10 −6 Pa or more and 5.0 × 10 −3 Pa or less. Moreover, 300-700 degreeC is desirable for heating temperature, More preferably, it is 400-650 degreeC.
酸素を含む雰囲気で第１の酸化物膜を加熱する条件で前記第２の酸化物膜を成膜することにより、第1の酸化物膜の格子定数を増加することが出来る。 By forming the second oxide film under conditions in which the first oxide film is heated in an atmosphere containing oxygen, the lattice constant of the first oxide film can be increased.
なお、第１及び第２の酸化物膜の成膜法としては、エレクトロンビーム蒸着法、スパッタリング法等を用いることが出来る。これらの方法において、ターゲットとして、上述した酸化物を用いることが出来る。 Note that an electron beam evaporation method, a sputtering method, or the like can be used as a method for forming the first and second oxide films. In these methods, the above-described oxide can be used as a target.
以上のようにして第１及び第２の酸化物膜を成膜すると、第1の酸化物膜中の酸素量は減少し、それによって、第1の酸化物の格子定数は、第２の酸化物膜の成膜前よりも成膜後において増加し、その結果、結晶配向性に優れた中間層を形成することが出来る。 When the first and second oxide films are formed as described above, the amount of oxygen in the first oxide film is reduced, whereby the lattice constant of the first oxide is changed to the second oxidation film. It increases after film formation rather than before film formation, and as a result, an intermediate layer having excellent crystal orientation can be formed.
このような中間層２を形成した後、中間層２上には超電導薄膜３が形成され、図１に示すような超電導薄膜線材が得られる。この超電導薄膜線材は、結晶配向性に優れた中間層上に形成されるため、結晶配向性に優れており、高い臨界電流密度を得ることが出来る。 After such an intermediate layer 2 is formed, a superconducting thin film 3 is formed on the intermediate layer 2 to obtain a superconducting thin film wire as shown in FIG. Since this superconducting thin film wire is formed on an intermediate layer excellent in crystal orientation, it is excellent in crystal orientation and a high critical current density can be obtained.
以下、本発明の実施例を示し、本発明について具体的に説明するが、これら実施例は、本発明を限定するものではない。 EXAMPLES Hereinafter, examples of the present invention will be shown and the present invention will be described in detail, but these examples do not limit the present invention.
実施例
配向金属基板法により２軸配向組織を形成したＮｉＷテープ基板上に、ＥＢ蒸着法により厚さ１２０ｎｍのＣｅＯ２薄膜を成膜した。このときのＣｅＯ２薄膜の単位格子サイズをX線回折法により評価したところ、０．５４ｎｍであった。
Example On a NiW tape substrate on which a biaxially oriented structure was formed by the oriented metal substrate method, a CeO 2 thin film having a thickness of 120 nm was formed by the EB vapor deposition method. When the unit cell size of the CeO 2 thin film at this time was evaluated by an X-ray diffraction method, it was 0.54 nm.
このＣｅＯ２薄膜上に、イットリア安定化ジルコニア（ＹＳＺ）焼結体をターゲットとして、スパッタリング法により、到達真空度６．４×１０−４Ｐａ、酸素分圧が１．３×１０-4ＰａであるＡｒと酸素の混合ガス雰囲気下で、基板温度６５０℃、投入ＲＦパワー５００Ｗの条件で、膜厚１２０ｎｍのＹＳＺ薄膜を成膜した。 On this CeO 2 thin film, with an yttria-stabilized zirconia (YSZ) sintered body as a target, the ultimate vacuum is 6.4 × 10 −4 Pa and the oxygen partial pressure is 1.3 × 10 −4 Pa by sputtering. A YSZ thin film having a thickness of 120 nm was formed under a condition of a mixed gas of Ar and oxygen under conditions of a substrate temperature of 650 ° C. and an input RF power of 500 W.
このＹＳＺ薄膜の結晶配向性をＸ線回折法によりピーク半価幅にて評価したところ、面内（ａ軸、ｂ軸）配向度は５．７°、ＹＳＺ結晶のC軸方向への傾きは１．３５°であった。また、ＹＳＺ薄膜形成後のＣｅＯ２薄膜の単位格子サイズは０．５７ｎｍであった。 When the crystal orientation of this YSZ thin film was evaluated by the X-ray diffraction method at the peak half-value width, the in-plane (a axis, b axis) orientation degree was 5.7 °, and the inclination of the YSZ crystal in the C axis direction was 1.35 °. The unit cell size of the CeO 2 thin film after forming the YSZ thin film was 0.57 nm.
以上のように、本実施例では、ＥＢ蒸着法により厚さ１２０ｎｍのＣｅＯ２薄膜を成膜した後、Ａｒガス雰囲気でＹＳＺ薄膜を成膜することにより、ＣｅＯ２薄膜の単位格子サイズは、ＹＳＺ薄膜の成膜前が０．５４ｎｍであったところ、ＹＳＺ薄膜の成膜後には０．５７ｎｍと増加した。これにより、結晶配向性の優れた中間層を得ることが出来た。 As described above, in this example, after forming a 120 nm thick CeO 2 thin film by EB vapor deposition, the YSZ thin film is formed in an Ar gas atmosphere, whereby the unit cell size of the CeO 2 thin film is YSZ. When it was 0.54 nm before forming the thin film, it increased to 0.57 nm after forming the YSZ thin film. As a result, an intermediate layer having excellent crystal orientation could be obtained.
比較例
配向金属基板法により２軸配向組織を形成したＮｉＷテープ基板上に、ＥＢ蒸着法により厚さ１２０ｎｍのＣｅＯ２薄膜を成膜した。このときのＣｅＯ２薄膜の単位格子サイズをX線回折法により評価したところ、０．５４ｎｍであった。
Comparative Example A 120 nm thick CeO 2 thin film was formed by EB vapor deposition on a NiW tape substrate on which a biaxially oriented structure was formed by the oriented metal substrate method. When the unit cell size of the CeO 2 thin film at this time was evaluated by an X-ray diffraction method, it was 0.54 nm.
このＣｅＯ２薄膜上に、イットリア安定化ジルコニア（ＹＳＺ）焼結体をターゲットとして、スパッタリング法により、到達真空度６．４×１０−４Ｐａ、酸素分圧が４．５×１０-１ＰａであるＡｒと酸素の混合ガス雰囲気下で、基板温度６５０℃（、投入ＲＦパワー５００Ｗの条件で、膜厚１２０ｎｍのＹＳＺ薄膜を成膜した。 On this CeO 2 thin film, with a yttria-stabilized zirconia (YSZ) sintered body as a target, the ultimate vacuum is 6.4 × 10 −4 Pa and the oxygen partial pressure is 4.5 × 10 −1 Pa by sputtering. A YSZ thin film having a thickness of 120 nm was formed under a condition of a substrate temperature of 650 ° C. (input RF power of 500 W) in a mixed gas atmosphere of Ar and oxygen.
このＹＳＺ薄膜の結晶配向性をＸ線回折法によりピーク半価幅にて評価したところ、面内（ａ軸、ｂ軸）配向度は６．０°、ＹＳＺ結晶のC軸方向への傾きは１．７°であった。また、ＹＳＺ薄膜形成後のＣｅＯ２薄膜の単位格子サイズは０．５４ｎｍであった。 When the crystal orientation of this YSZ thin film was evaluated by the X-ray diffraction method at the peak half-value width, the in-plane (a axis, b axis) orientation degree was 6.0 °, and the inclination of the YSZ crystal in the C axis direction was It was 1.7 °. The unit cell size of the CeO 2 thin film after forming the YSZ thin film was 0.54 nm.
１・・・基板、２…中間層、３…超電導薄膜。 DESCRIPTION OF SYMBOLS 1 ... Substrate, 2 ... Intermediate layer, 3 ... Superconducting thin film.
Claims (5)
前記中間層は、ＣｅＯ ２ からなる第１の酸化物膜と、前記第１の酸化物膜上に形成された第２の酸化物膜を有し、前記第２の酸化物膜の形成後の前記第１の酸化物膜の格子定数は、前記第２の酸化物膜の形成前の格子定数よりも大きいことを特徴とする薄膜超電導線材。 A multi-layer having a metal substrate and a plurality of types of component structures formed on the metal substrate and containing at least one element selected from the group consisting of Ce, Zr, Y, Gd, Mg, Sr, and Ti A thin film superconducting wire comprising: an intermediate layer having a metal oxide film; and an energization layer having a superconducting film formed on the intermediate layer,
The intermediate layer has a first oxide film made of CeO 2 and a second oxide film formed on the first oxide film, and the intermediate layer is formed after the formation of the second oxide film. A thin film superconducting wire, wherein a lattice constant of the first oxide film is larger than a lattice constant before the formation of the second oxide film.
（ａ）前記金属基板上にエレクトロンビーム蒸着法またはスパッタリング法によってＣｅＯ ２ からなる第１の酸化物膜を成膜する工程と、
（ｂ）前記第１の酸化物膜の酸素量を減少させる条件で第２の酸化物膜を成膜する工程と
を具備することを特徴とする薄膜超電導線材の製造方法。 A multi-layer having a metal substrate and a plurality of types of component structures formed on the metal substrate and containing at least one element selected from the group consisting of Ce, Zr, Y, Gd, Mg, Sr, and Ti A method for producing a thin film superconducting wire comprising: an intermediate layer having a metal oxide film; and an energization layer having a superconducting film formed on the intermediate layer,
A step of forming a first oxide film consisting of CeO 2 (a) to the metal substrate by electron beam evaporation or sputtering,
(B) forming a second oxide film under a condition for reducing the amount of oxygen in the first oxide film, and a method for manufacturing a thin film superconducting wire.
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