WO2011004684A1 - 基板および超電導線材の製造方法 - Google Patents

基板および超電導線材の製造方法 Download PDF

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Publication number
WO2011004684A1
WO2011004684A1 PCT/JP2010/060102 JP2010060102W WO2011004684A1 WO 2011004684 A1 WO2011004684 A1 WO 2011004684A1 JP 2010060102 W JP2010060102 W JP 2010060102W WO 2011004684 A1 WO2011004684 A1 WO 2011004684A1
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WIPO (PCT)
Prior art keywords
layer
substrate
heat
nickel layer
treating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2010/060102
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English (en)
French (fr)
Japanese (ja)
Inventor
肇 太田
昌也 小西
高史 山口
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sumitomo Electric Industries Ltd
Toyo Kohan Co Ltd
Original Assignee
Sumitomo Electric Industries Ltd
Toyo Kohan Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Sumitomo Electric Industries Ltd, Toyo Kohan Co Ltd filed Critical Sumitomo Electric Industries Ltd
Priority to CN201080031249.9A priority Critical patent/CN102473488B/zh
Priority to US13/381,191 priority patent/US9306147B2/en
Priority to KR1020127003395A priority patent/KR101685732B1/ko
Priority to EP10796995.8A priority patent/EP2453446A4/en
Priority to IN528DEN2012 priority patent/IN2012DN00528A/en
Publication of WO2011004684A1 publication Critical patent/WO2011004684A1/ja
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
    • H01B12/02—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
    • H01B12/06—Films or wires on bases or cores
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
    • H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
    • H01B1/026—Alloys based on copper
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
    • H—ELECTRICITY
    • H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
    • H10N60/00—Superconducting devices
    • H10N60/01—Manufacture or treatment
    • H10N60/0268—Manufacture or treatment of devices comprising copper oxide
    • H10N60/0296—Processes for depositing or forming copper oxide superconductor layers
    • H10N60/0576—Processes for depositing or forming copper oxide superconductor layers characterised by the substrate
    • H10N60/0632—Intermediate layers, e.g. for growth control
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

Definitions

  • the present invention relates to a method for manufacturing a substrate and a method for manufacturing a superconducting wire.
  • a ceramic thin film intermediate layer is formed on a metal substrate, and a superconducting layer is formed thereon.
  • a superconducting layer is formed thereon.
  • Patent Document 1 an oxide layer on the surface of an oriented metal substrate is removed, and thin films such as an intermediate layer and a superconducting layer are epitaxially grown while maintaining the biaxial orientation of the oriented metal substrate. How to do is described.
  • an object of the present invention is to provide a method for producing a substrate and a method for producing a superconducting wire capable of improving the orientation and flatness of the nickel plating layer surface.
  • the present invention provides a nickel layer after a step of preparing a substrate having a nickel layer formed on a copper layer using a plating method, a step of heat-treating the nickel layer at 800 to 1000 ° C., and a step of heat-treating the nickel layer And a step of epitaxially growing an intermediate layer thereon.
  • a substrate having improved orientation and flatness of the nickel layer surface can be obtained by heat-treating the nickel layer at 800 to 1000 ° C. Moreover, it can suppress that a copper atom diffuses from a copper layer to the nickel layer surface in the case of heat processing.
  • the step of heat-treating the nickel layer is preferably performed in a reducing atmosphere.
  • the oxide film formed on the surface of the nickel layer can be removed.
  • the step of heat-treating the nickel layer is performed under an atmosphere of a gas containing hydrogen under reduced pressure.
  • the oxide film formed on the nickel layer surface can be more effectively removed.
  • the present invention provides a nickel layer after a step of preparing a substrate having a nickel layer formed on a copper layer using a plating method, a step of heat-treating the nickel layer at 800 to 1000 ° C., and a step of heat-treating the nickel layer
  • a method of manufacturing a superconducting wire comprising a step of epitaxially growing an intermediate layer thereon and a step of forming a superconducting layer on the intermediate layer.
  • a substrate having improved nickel layer surface orientation and flatness can be obtained by heat-treating the nickel layer at 800 to 1000 ° C.
  • a superconducting wire with improved flatness can be obtained.
  • a substrate with improved orientation and flatness of the nickel layer surface and a superconducting wire with improved orientation and flatness of the superconducting layer can be obtained.
  • FIG. 1 is a cross-sectional view schematically showing a method for manufacturing a substrate 1 according to an embodiment of the present invention.
  • substrate 1 in one embodiment of this invention uses the plating method as shown in FIG.1 (b) on Cu layer 2 as shown in FIG.1 (a).
  • Step of preparing a substrate> As shown in FIG.1 (b), specifically, the base material with which the Ni layer 3 was formed on the Cu layer 2 using the plating method is prepared first.
  • the Cu layer 2 is suitable for an alignment substrate because Cu atoms are biaxially oriented.
  • the term “biaxially oriented” includes not only complete biaxial orientation but also a case where the crystal axis shift angle is 25 ° or less.
  • the orientation is preferably such that the ⁇ 100> axis is oriented in the direction perpendicular to the substrate surface and the ⁇ 010> axis is oriented in the length direction of the substrate.
  • the Cu layer 2 can be laminated on another metal or alloy.
  • the Cu layer 2 can be provided on stainless steel (hereinafter referred to as SUS), which is a high-strength material.
  • the Cu layer 2 can have a long tape-like shape.
  • the Ni layer 3 is formed on the Cu layer 2 using a plating method. Examples of the plating method include an electrolytic plating method and an electroless plating method. In consideration of efficient and continuous processing, the electrolytic plating method is preferable.
  • the Ni layer 3 is a layer for preventing oxidation when the intermediate layer 4 is formed. When the Cu layer 2 is oriented, the Ni layer 3 formed thereon is also oriented.
  • the thickness of the Ni layer 3 is preferably 1 to 10 ⁇ m, and more preferably 1 to 3 ⁇ m.
  • the thickness is 1 ⁇ m or more, Cu atoms can be prevented from diffusing to the surface of the Ni layer even when heat of about 800 to 1000 ° C. is applied in the step of heat-treating the Ni layer 3 described later. For this reason, it is possible to effectively exhibit the function of the Ni layer 3 that is not easily oxidized and has good lattice matching with the intermediate layer 4. If the thickness of the Ni layer 3 exceeds 10 ⁇ m, the orientation of the epitaxial growth of the Ni layer 3 may be greatly broken, which is not preferable.
  • the step of heat-treating the Ni layer 3 is preferably performed in a reducing atmosphere.
  • the heat treatment in a reducing atmosphere refers to heat treatment in a reducing atmosphere sufficient to remove the oxide layer formed on the surface of the oriented metal substrate.
  • Under reducing atmosphere means, for example, the presence of a reducing gas such as hydrogen (H 2 ) gas under reduced pressure.
  • Under reduced pressure is a pressure lower than atmospheric pressure, and is preferably 1 to 10 Pa, for example.
  • the H 2 gas should be 1 mol% or more. Preferably, it is 3 mol% or more.
  • the temperature for heat-treating the Ni layer 3 is preferably 800 to 1000 ° C.
  • the heat treatment temperature is less than 800 ° C.
  • the orientation and flatness of the Ni layer 3 are not sufficiently improved.
  • the temperature exceeds 1000 ° C. Ni and Cu diffuse and form a complete alloy, so that Cu diffuses on the Ni layer surface. Since Cu is easily oxidized, the orientation and flatness of the surface of the Ni layer 3 cannot be improved.
  • the time for heat-treating the Ni layer 3 is not particularly limited, but is preferably 15 minutes or more. If the heat treatment time is less than 15 minutes, the orientation and flatness of the Ni layer 3 are not sufficiently improved.
  • the intermediate layer 4 is epitaxially grown on the heat-treated Ni layer 3 to obtain the substrate 1.
  • a metal oxide having one or more metal elements having a pyrochlore type, a meteorite type, a rock salt type or a perovskite type crystal structure is preferably used.
  • the rare earth element oxide such as CeO 2, YSZ (yttria-stabilized zirconia), BZO (BaZrO 3), STO (SrTiO 3), Al 2 O 3, YAlO 3, MgO, Ln-M-O -based Compounds (Ln is one or more lanthanoid elements, M is one or more elements selected from Sr, Zr and Ga, and O is oxygen).
  • Such an oxide alleviates the difference in crystal constant and crystal orientation between the Cu layer 2 which is an oriented metal substrate and the superconducting layer 5 formed on the intermediate layer 4, and metal atoms from the Cu layer 2 to the superconducting layer. It plays a role in preventing the outflow.
  • the method for forming the oxide thin film to be the intermediate layer 4 is not particularly limited as long as it does not contradict the object of the present invention.
  • a method such as a pulse laser deposition method or a thermal evaporation method is preferably used.
  • a CeO 2 thin film is formed as an intermediate layer 4 on the Ni layer 3 that is biaxially oriented in the direction in which the ⁇ 100> axis after the heat treatment is perpendicular to the substrate surface and the ⁇ 010> axis is in the length direction of the substrate. is grown epitaxially, the ⁇ 100> axis is the direction perpendicular to the substrate surface, ⁇ 011> axes CeO 2 thin film is formed which is aligned in a lengthwise direction of the substrate, high CeO 2 thin film biaxial orientation is obtained It is done.
  • the intermediate layer 4 has good orientation and flatness, so that the superconducting layer 5 having high biaxial orientation can be obtained.
  • Superconducting layer 5 has a long tape-like shape.
  • the superconducting layer 5 is made of REBa 2 Cu 3 O y (y is 6 to 8, more preferably about 7, RE is Y (yttrium), or rare earth such as Gd (gadolinium), Sm (samarium), Ho (holmium), etc.
  • GdBCO is expressed as GdBa 2 Cu 3 O y (y is 6 to 8, more preferably approximately 7).
  • the method for forming the oxide thin film to be the superconducting layer 5 is not particularly limited as long as it does not contradict the purpose of the present invention.
  • PLD method, MOD (Metal Organic Deposition) method, MOCVD (Organic Metal Vapor Phase) A method such as growth; Metal Organic Chemical Vapor Deposition) is preferably used.
  • a protective layer (not shown) can be formed on the superconducting layer 5 as necessary.
  • the protective layer is not particularly limited as long as it has high conductivity, but Ag, Au, Pt, Al, or an alloy thereof is preferably used.
  • Methods such as a sputtering method, EBD method, PLD method, thermal evaporation method, MOD method, MOCVD method, a plating method, are used preferably.
  • Example 1 a substrate having a Cu layer with a thickness of 18 ⁇ m on a SUS substrate was prepared.
  • the substrate having the Cu layer was subjected to electrolytic nickel plating to form a Ni layer having a thickness shown in Table 1.
  • the Ni layer is formed under a pressure of 8.1 Pa atmosphere using a mixed gas of H 2 gas and Ar gas (composition: H 2 gas 3 mol%, Ar gas 97 mol%) as a reducing gas.
  • the heat treatment was performed at the heat treatment temperature shown in 1 for 16 minutes.
  • a mixed gas of H 2 gas and Ar gas composition: H 2 gas 3 mol%, Ar gas 97 mol%) was used as the reducing gas, under a pressure of 5.2 Pa atmosphere, and the substrate temperature.
  • a CeO 2 thin film having a thickness of 0.15 ⁇ m was formed on the nickel layer as a first intermediate layer.
  • a YSZ thin film having a thickness of 0.25 ⁇ m was formed as a second intermediate layer to prevent element diffusion. Further, a CeO 2 thin film having a thickness of 0.05 ⁇ m was formed as a third intermediate layer for lattice matching with the superconducting film.
  • a GdBCO film was formed as a superconducting layer on the intermediate layer consisting of the three layers by the PLD method.
  • the obtained substrate was measured for the biaxial orientation, surface roughness (Ra) and Ni—Cu diffusion of the CeO 2 thin film as the first intermediate layer. Further, the critical current value Ic was measured for the obtained superconducting wire.
  • the X-ray diffraction peak intensity from the (200) plane is the amount of crystals in which the ⁇ 100> axis is biaxially oriented in the direction perpendicular to the substrate surface and the ⁇ 011> axis is biaxially oriented in the length direction of the substrate.
  • the X-ray diffraction peak intensity from the (111) plane indicates the amount of crystals in which the ⁇ 111> axis is uniaxially oriented in the direction perpendicular to the substrate surface.
  • Ra Surface roughness
  • Ni-Cu diffusion is performed by 2A (°) of (A) copper layer (200) plane (Cu (200) plane) and (B) Ni layer (200) plane (Ni (200) plane). ), Measured by the XRD method, and evaluated by the numerical values of (B)-(A), the smaller the numerical value, the more the alloying of Ni and Cu progresses. Further, when the value is 0, it indicates that the alloy is completely alloyed.
  • the critical current value Ic was measured in a self-magnetic field at a temperature of 77 K, and was defined as an energization current value when an electric field of 10 ⁇ 6 V / cm was generated.
  • Examples 1 to 4 are substrates obtained by heat-treating the Ni layer at a temperature in the range of 850 to 950 ° C. Compared to Comparative Examples 1 and 2 in which the Ni layer was not heat-treated, the biaxial orientation of the CeO 2 thin film as the first intermediate layer could be improved. Further, the thicker the Ni layer, the higher the heat treatment temperature is required for improving the biaxial orientation of the CeO 2 thin film as the first intermediate layer. Furthermore, the surface roughness can be reduced and the surface flatness is improved as compared with Comparative Examples 1 and 2 in which the Ni layer is not heat-treated. Cu and Ni were only partially alloyed, and Cu did not diffuse on the Ni layer surface.

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
PCT/JP2010/060102 2009-07-10 2010-06-15 基板および超電導線材の製造方法 Ceased WO2011004684A1 (ja)

Priority Applications (5)

Application Number Priority Date Filing Date Title
CN201080031249.9A CN102473488B (zh) 2009-07-10 2010-06-15 制造衬底和超导线材的方法
US13/381,191 US9306147B2 (en) 2009-07-10 2010-06-15 Method of producing substrate and superconducting wire
KR1020127003395A KR101685732B1 (ko) 2009-07-10 2010-06-15 기판 및 초전도 선재의 제조 방법
EP10796995.8A EP2453446A4 (en) 2009-07-10 2010-06-15 METHOD FOR PRODUCING A SUBSTRATE AND SUPERCONDUCTING WIRE
IN528DEN2012 IN2012DN00528A (enExample) 2009-07-10 2010-10-07

Applications Claiming Priority (2)

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JP2009163513A JP5096422B2 (ja) 2009-07-10 2009-07-10 基板および超電導線材の製造方法
JP2009-163513 2009-07-10

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WO2011004684A1 true WO2011004684A1 (ja) 2011-01-13

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US (1) US9306147B2 (enExample)
EP (1) EP2453446A4 (enExample)
JP (1) JP5096422B2 (enExample)
KR (1) KR101685732B1 (enExample)
CN (1) CN102473488B (enExample)
IN (1) IN2012DN00528A (enExample)
WO (1) WO2011004684A1 (enExample)

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Publication number Priority date Publication date Assignee Title
WO2012132128A1 (ja) * 2011-03-28 2012-10-04 株式会社村田製作所 検出デバイスおよびその製造方法、センサ電極、ならびに、空隙配置構造体およびそれを用いた検出方法
JP2013089354A (ja) * 2011-10-14 2013-05-13 Sumitomo Electric Ind Ltd 超電導薄膜線材用の中間層付基材とその製造方法、および超電導薄膜線材
US10174420B2 (en) 2013-09-04 2019-01-08 Toyo Kohan Co., Ltd. Method for forming oxide layer, laminated substrate for epitaxial growth, and method for producing the same

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JP2005001935A (ja) 2003-06-11 2005-01-06 Sumitomo Electric Ind Ltd 酸化物薄膜の製造方法
JP2006127847A (ja) * 2004-10-27 2006-05-18 Sumitomo Electric Ind Ltd 膜形成用配向基板および超電導線材
JP2007165153A (ja) * 2005-12-14 2007-06-28 Internatl Superconductivity Technology Center 厚膜テープ状ｒｅ系（１２３）超電導体の製造方法。
JP2007188756A (ja) * 2006-01-13 2007-07-26 Internatl Superconductivity Technology Center 希土類系テープ状酸化物超電導体
JP2010192349A (ja) * 2009-02-20 2010-09-02 Chubu Electric Power Co Inc 超電導線材

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JP2006127847A (ja) * 2004-10-27 2006-05-18 Sumitomo Electric Ind Ltd 膜形成用配向基板および超電導線材
JP2007165153A (ja) * 2005-12-14 2007-06-28 Internatl Superconductivity Technology Center 厚膜テープ状ｒｅ系（１２３）超電導体の製造方法。
JP2007188756A (ja) * 2006-01-13 2007-07-26 Internatl Superconductivity Technology Center 希土類系テープ状酸化物超電導体
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See also references of EP2453446A4

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Publication number Publication date
CN102473488B (zh) 2015-05-06
US20120108439A1 (en) 2012-05-03
KR20120051010A (ko) 2012-05-21
US9306147B2 (en) 2016-04-05
JP2011018598A (ja) 2011-01-27
EP2453446A4 (en) 2015-04-22
KR101685732B1 (ko) 2016-12-12
EP2453446A1 (en) 2012-05-16
IN2012DN00528A (enExample) 2015-08-21
JP5096422B2 (ja) 2012-12-12
CN102473488A (zh) 2012-05-23

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