JP2006073236A - Manufacturing method of oxide superconductive wire rod and support tool for manufacturing the wire rod - Google Patents
Manufacturing method of oxide superconductive wire rod and support tool for manufacturing the wire rod Download PDFInfo
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- 238000004519 manufacturing process Methods 0.000 title claims abstract description 36
- 238000010438 heat treatment Methods 0.000 claims abstract description 38
- 239000002887 superconductor Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 11
- 238000009792 diffusion process Methods 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 6
- 239000000919 ceramic Substances 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 238000004804 winding Methods 0.000 claims description 6
- 239000007769 metal material Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000003779 heat-resistant material Substances 0.000 claims description 2
- 230000003647 oxidation Effects 0.000 claims 1
- 238000007254 oxidation reaction Methods 0.000 claims 1
- 239000010935 stainless steel Substances 0.000 abstract description 10
- 229910001220 stainless steel Inorganic materials 0.000 abstract description 10
- 230000006866 deterioration Effects 0.000 abstract description 3
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 8
- 238000000034 method Methods 0.000 description 8
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 229910052709 silver Inorganic materials 0.000 description 6
- 239000004332 silver Substances 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000004020 conductor Substances 0.000 description 2
- 239000000470 constituent Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 238000005482 strain hardening Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005491 wire drawing Methods 0.000 description 2
- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- 229910004247 CaCu Inorganic materials 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 229910000856 hastalloy Inorganic materials 0.000 description 1
- 229910001026 inconel Inorganic materials 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 235000012771 pancakes Nutrition 0.000 description 1
- 239000003870 refractory metal Substances 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 229910002058 ternary alloy Inorganic materials 0.000 description 1
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- 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
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- 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
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Abstract
Description
本発明は酸化物超電導線材の製造方法及びその製造用支持具の改良に関するものである。 The present invention relates to a method for manufacturing an oxide superconducting wire and an improvement of a support for manufacturing the same.
従来、酸化物超電導体として、Bi系(2212)酸化物超電導体(Bi:Sr:Ca:Cu=2:2:1:2のモル比)及びBi系(2223)酸化物超電導体(Bi:Sr:Ca:Cu=2:2:2:3のモル比)が線材化に成功しており、これらの線材は所謂銀シース法(Powder in Tube Method)によって製造されている。この方法は、銀又は銀合金シース内に超電導物質の原料粉末を充填し、これに縮径加工を施すか、あるいは更に圧延加工を施して断面丸形又はテープ状に成形した後、熱処理を施して原料粉末を超電導化するものである(例えば、非特許文献1参照。)。 Conventionally, as an oxide superconductor, a Bi-based (2212) oxide superconductor (Bi: Sr: Ca: Cu = 2: 2: 1: 2 molar ratio) and a Bi-based (2223) oxide superconductor (Bi: Sr: Ca: Cu = 2: 2: 2: 3 molar ratio) has been successfully formed into wires, and these wires are produced by a so-called silver sheath method (Powder in Tube Method). In this method, a raw material powder of a superconducting substance is filled in a silver or silver alloy sheath and subjected to diameter reduction processing or further rolling to form a round cross-section or tape, and then heat treatment. Thus, the raw material powder is superconducted (see, for example, Non-Patent Document 1).
上記の銀シース法により酸化物超電導線材を製造する場合、冷間加工後に酸化物超電導体を生成させるための熱処理が必要となる。酸化物超電導体の合成温度は適正温度範囲が狭く、例えば温度範囲を±1〜2℃に制御する必要がある。 When manufacturing an oxide superconducting wire by the above silver sheath method, a heat treatment for generating an oxide superconductor after cold working is required. The synthesis temperature of the oxide superconductor has a narrow appropriate temperature range, and it is necessary to control the temperature range to ± 1 to 2 ° C., for example.
以上の厳しい温度管理は、線材の長尺化に伴い電気炉が大型化するに従って、その困難さが著しく増大する。これに加えて、長尺の線材の重量を高温中で支えるためには、大型の線材支持具が必要となり、耐熱性の観点からこの線材支持具は耐熱ステンレス鋼、セラミックス成型体等により形成されている。 The difficulty of the above severe temperature control increases remarkably as the electric furnace becomes larger as the wire becomes longer. In addition, in order to support the weight of a long wire at a high temperature, a large wire support is required. From the viewpoint of heat resistance, this wire support is formed of heat resistant stainless steel, ceramic molded body, etc. ing.
これらの線材支持具は熱容量が大きいため、例えば、この線材支持具を円筒状に形成し、この外周に長尺の酸化物超電導体を構成する元素を含む線材をソレノイド状に巻回して熱処理を施すと、線材の熱挙動は線材支持具の熱挙動や熱容量に大きく影響され、熱処理すべき線材の温度制御が困難になり所望の熱処理パターンを得ることが困難になるという問題があり、特に、冷却条件を厳密に制御しなければならないBi系(2212)酸化物超電導線材の製造においては、特性の優れた超電導線材を得ることは極めて困難となる。 Since these wire rod supports have a large heat capacity, for example, the wire rod support is formed in a cylindrical shape, and a wire containing an element constituting a long oxide superconductor is wound around the outer periphery in a solenoid shape to perform heat treatment. When applied, the thermal behavior of the wire is greatly influenced by the thermal behavior and heat capacity of the wire support, and there is a problem that it becomes difficult to control the temperature of the wire to be heat-treated and to obtain a desired heat treatment pattern, In the production of a Bi-based (2212) oxide superconducting wire whose cooling conditions must be strictly controlled, it is extremely difficult to obtain a superconducting wire having excellent characteristics.
また、線材支持具として耐熱ステンレス鋼を用いた場合には、線材支持具上に巻回した線材との熱膨張率の差により、熱処理時に線材に歪が加わり超電導特性が劣化するという問題がある上、線材支持具を構成する元素の線材への拡散により超電導特性が劣化するという問題がある。 In addition, when heat-resistant stainless steel is used as the wire support, there is a problem that due to the difference in coefficient of thermal expansion from the wire wound on the wire support, the wire is distorted during heat treatment and the superconducting properties deteriorate. In addition, there is a problem that the superconducting characteristics are deteriorated by diffusion of elements constituting the wire support into the wire.
本発明は、以上の問題を解決するためになされたもので、線材支持具と長尺の酸化物超電導体を構成する元素を含む線材との間に熱絶縁層を設けて線材支持具からの熱流入を防止することにより、所定の熱処理パターンで精密な熱処理制御を可能にするとともに、線材支持具からの線材支持具を構成する元素の線材への拡散を防止し、さらに、熱処理時に線材に加わる歪による劣化を防止して、超電導特性の優れた長尺の酸化物超電導線材を製造することができる酸化物超電導線材の製造方法及びその製造用支持具を提供することをその目的とする。 The present invention has been made in order to solve the above-described problems. A thermal insulating layer is provided between the wire support and the wire containing the elements constituting the long oxide superconductor, and the wire support is provided from the wire support. Preventing heat inflow enables precise heat treatment control with a predetermined heat treatment pattern, prevents diffusion of the elements constituting the wire support from the wire support to the wire, An object of the present invention is to provide an oxide superconducting wire manufacturing method and a support for manufacturing the oxide superconducting wire capable of manufacturing a long oxide superconducting wire excellent in superconducting characteristics while preventing deterioration due to applied strain.
以上の目的を達成するために、本発明による酸化物超電導線材の製造方法は、
長尺の酸化物超電導体を構成する元素を所定のモル比で含む原料粉末を収容した線材を巻回して線材支持具上に載置した後、熱処理を施して酸化物超電導線材を製造する方法において、線材支持具と線材との間に熱絶縁層を設けて熱処理を施すことを特徴としている。
In order to achieve the above object, a method for producing an oxide superconducting wire according to the present invention includes:
A method for producing an oxide superconducting wire by winding a wire containing a raw material powder containing elements constituting a long oxide superconductor in a predetermined molar ratio and placing the wire on a wire support, followed by heat treatment 1 is characterized in that a heat insulating layer is provided between the wire support and the wire to perform heat treatment.
また、本発明による他の酸化物超電導線材の製造方法は、線材支持具上に長尺の酸化物超電導体を構成する元素を所定のモル比で含む原料粉末を収容した線材をソレノイド状に巻回した後、熱処理を施して酸化物超電導線材を製造する方法において、線材支持具とソレノイド状に巻回した長尺の線材との間に熱絶縁層を設けて熱処理を施すことを特徴としている。 In addition, another oxide superconducting wire manufacturing method according to the present invention is a method in which a wire containing a raw material powder containing elements constituting a long oxide superconductor in a predetermined molar ratio is wound in a solenoid shape on a wire support. In the method of manufacturing an oxide superconducting wire by performing a heat treatment after turning, a heat insulating layer is provided between the wire support and a long wire wound in a solenoid shape, and the heat treatment is performed. .
さらに、本発明による酸化物超電導線材の製造用支持具は、耐熱性金属材料又はセラミックスからなる円筒状の線材支持具表面に、複数のセラミックスからなる棒状部材を線材支持具の軸方向に平行に所定の間隔を置いて配置したことを特徴としている。 Furthermore, the support for manufacturing an oxide superconducting wire according to the present invention has a cylindrical wire support made of a heat-resistant metal material or ceramic, and a rod-shaped member made of a plurality of ceramics parallel to the axial direction of the wire support. It is characterized by being arranged at a predetermined interval.
本発明における酸化物超電導体を構成する元素を所定のモル比で含む原料粉末を収容した線材としては、銀シース法により製造した単芯線、多芯線又はこれらの複数本を集合又は撚合せた集合導体を挙げることができる。 As the wire containing the raw material powder containing the element constituting the oxide superconductor in the present invention at a predetermined molar ratio, a single core wire, a multi-core wire manufactured by the silver sheath method, or a set obtained by collecting or twisting a plurality of these wires Mention may be made of conductors.
以上述べたように、本発明による酸化物超電導線材の製造方法によれば、線材支持具と長尺の線材との間に熱絶縁層を設けたことにより、線材支持具からの熱流入を防止して所定の熱処理パターンで精密な熱処理制御を可能にするとともに、線材支持具からの線材支持具を構成する元素の線材への拡散を防止し、さらに、熱処理時に線材に加わる歪による劣化を防止して、超電導特性の優れた長尺の酸化物超電導線材を製造することができる利点を有する。 As described above, according to the method for manufacturing an oxide superconducting wire according to the present invention, a heat insulating layer is provided between the wire support and the long wire, thereby preventing heat from flowing from the wire support. This enables precise heat treatment control with a predetermined heat treatment pattern, prevents diffusion of the elements constituting the wire support from the wire support to the wire, and prevents deterioration due to strain applied to the wire during heat treatment. Thus, there is an advantage that a long oxide superconducting wire excellent in superconducting characteristics can be manufactured.
本発明の酸化物超電導線材の製造方法の一実施形態においては、図3に示すように、線材支持具10の上に線材重量に耐える複数本の支柱11を立て、この上に網状の支持板12を置いて、この上にパンケーキ状に巻回した長尺の酸化物超電導体を構成する元素を含む線材13を載置した後、電気炉14内に配置して熱処理を施し酸化物超電導線材を製造する。この場合、上記の網状の支持板12により線材支持具10と線材13との間に形成される空気層によって熱絶縁層が形成される。
In one embodiment of the method for producing an oxide superconducting wire according to the present invention, as shown in FIG. 3, a plurality of
また、本発明の他の酸化物超電導線材の製造方法においては、図1に示すように、線材支持具1とソレノイド状に巻回した長尺の線材4との間に熱絶縁層が設けられるが、この熱絶縁層は、線材支持具を構成する元素の前記線材への拡散を防止する機能も有し、熱絶縁と拡散防止機能を有する材料を線材支持具上に配設することもできるが、この熱絶縁層を空気絶縁層により形成することが好ましい。
Moreover, in the manufacturing method of the other oxide superconducting wire of this invention, as shown in FIG. 1, a heat insulation layer is provided between the wire support 1 and the
上記の空気絶縁層は、線材への拡散を防止する物質からなる部材2を線材支持具1とソレノイド状に巻回した長尺の線材4との間に間欠的に配置することにより形成することができる。この場合、耐熱性材料からなる円筒状の線材支持具1表面に、複数のセラミックスからなる棒状部材2を線材支持具の軸方向に平行に所定の間隔を置いて配置して、この棒状部材の外側に長尺の酸化物超電導体を構成する元素を含む線材をソレノイド状に巻回することが好ましい。
The air insulating layer is formed by intermittently disposing the
線材支持具上に空気絶縁層を介してソレノイド状に巻回された冷間加工後の長尺の線材に、酸化物超電導体を生成させるための熱処理が施されるが、この熱処理は酸化物超電導体の合成温度で施され、Bi系(2212)酸化物超電導体の場合、酸素濃度50%以上の雰囲気中での加熱とそれに続く徐冷工程により施される。この加熱工程は、Bi系(2212)酸化物超電導体の融点以上で融点以上20℃未満の温度で施され、一方、徐冷工程は、0.1〜10℃/hの冷却速度の範囲で、少なくともBi系(2212)酸化物超電導体の凝固温度以下10℃まで施される。 A heat treatment for generating an oxide superconductor is performed on a long wire after cold working wound in a solenoid shape on a wire support through an air insulating layer. It is applied at the synthesis temperature of the superconductor, and in the case of a Bi-based (2212) oxide superconductor, it is applied by heating in an atmosphere having an oxygen concentration of 50% or more, followed by a slow cooling step. This heating step is performed at a temperature higher than the melting point of the Bi-based (2212) oxide superconductor and higher than the melting point and lower than 20 ° C., while the slow cooling step is performed at a cooling rate in the range of 0.1 to 10 ° C./h. And at least 10 ° C. below the solidification temperature of the Bi-based (2212) oxide superconductor.
上記の線材支持具は、熱処理中の酸化性雰囲気及び温度でその形状及び機械的強度を保持することができるものであればよく、MgO、Al2O3、Al2O3−SiO系等のセラミックス材料あるいはステンレス鋼、ハステロイ、インコネル等の耐熱金属材料を用いることができ、一方、空気絶縁層を形成するための棒状部材はセラミックスにより形成することが好ましい。 The wire support may be any material that can maintain its shape and mechanical strength in an oxidizing atmosphere and temperature during heat treatment, such as MgO, Al 2 O 3 , Al 2 O 3 —SiO series, etc. A ceramic material or a refractory metal material such as stainless steel, Hastelloy, or Inconel can be used. On the other hand, the rod-shaped member for forming the air insulating layer is preferably formed of ceramics.
以下本発明の一実施例について図面を用いて説明する。 Hereinafter, an embodiment of the present invention will be described with reference to the drawings.
実施例
外径φ18mm、内径φ15mmの純銀パイプ中に、Bi2Sr2CaCu2O8の酸化物超電導体を構成する元素を所定のモル比で含む原料粉末を充填し、これに伸線加工を施して外径φ2mmまで成形した。この61本を束ねて同一サイズの純銀パイプ中に収容し、更に外径φ4.5mmまで伸線加工を施した。
Example A pure silver pipe having an outer diameter of φ18 mm and an inner diameter of φ15 mm was filled with a raw material powder containing elements constituting the oxide superconductor of Bi 2 Sr 2 CaCu 2 O 8 at a predetermined molar ratio, and this was subjected to wire drawing. To give an outer diameter of 2 mm. The 61 pieces were bundled and accommodated in a pure silver pipe of the same size, and further drawn to an outer diameter of φ4.5 mm.
次いで、この6本を束ねてAg−Mg−Sb三元合金を用いて作製したパイプ中に収容し、これに伸線加工を施して成形し、φ1mmの線材を製造した。 Next, these 6 pieces were bundled and accommodated in a pipe produced using an Ag—Mg—Sb ternary alloy, and this was subjected to wire drawing to form a wire with a diameter of 1 mm.
一方、図2に示すように、外径φ1m、長さ0.5m、厚さ5mmの耐熱ステンレス製のドラム1の外周に、Al2O3からなる外径φ8mmのロッド2の10本を、ドラムの軸方向に平行に、かつ等間隔に配置して固定し、酸化物超電導線材の製造用支持具3を形成した。
On the other hand, as shown in FIG. 2, 10
次いで、図1に示すように、この製造用支持具3上に上記の線材4の300mをソレノイド状に巻回して、電気炉5中に入れ熱処理を施した。熱処理条件は、酸素雰囲気中で900℃、冷却速度10℃/hとした。
Next, as shown in FIG. 1, 300 m of the above-described
このようにして製造した酸化物超電導線材の臨界電流値(Ic)を4.2K、0Tで測定した結果、1050Aの値を示した。 As a result of measuring the critical current value (Ic) of the oxide superconducting wire thus manufactured at 4.2 K and 0 T, a value of 1050 A was shown.
比較例
ドラムを、外径φ1m、長さ0.5m、厚さ5mmの耐熱ステンレス製あるいはAl2O3で作製し、実施例と同様にしてこのドラム上に上記の線材の300mをソレノイド状に巻回して、電気炉中に入れ熱処理を施した。熱処理条件は、酸素雰囲気中で900℃、冷却速度10℃/hを目標とした。
Comparative Example A drum was made of heat-resistant stainless steel or Al 2 O 3 having an outer diameter of 1 m, a length of 0.5 m, and a thickness of 5 mm, and 300 m of the above-mentioned wire rod was solenoidally formed on this drum in the same manner as in the example. It was wound and placed in an electric furnace for heat treatment. The heat treatment conditions were set to 900 ° C. and a cooling rate of 10 ° C./h in an oxygen atmosphere.
このようにして製造した酸化物超電導線材の臨界電流値(Ic)を4.2K、0Tで測定した結果、耐熱ステンレス製のドラムの場合には350A、Al2O3製のドラムの場合には600Aの値を示した。 The critical current value (Ic) of the oxide superconducting wire thus manufactured was measured at 4.2 K and 0 T. As a result, in the case of a drum made of heat resistant stainless steel, 350 A, in the case of a drum made of Al 2 O 3 A value of 600A was shown.
以上の実施例及び比較例の結果から明らかなように、耐熱ステンレス製のドラムの外周にAl2O3からなる複数本のロッドを、ドラムの軸方向に平行に、かつ等間隔に配置して固定し、この上に線材をソレノイド状に巻回して線材とドラムとの間に空気絶縁層を設けて熱処理を施すことにより、高い臨界電流値を有する酸化物超電導線材を製造することができる。 As is clear from the results of the above examples and comparative examples, a plurality of rods made of Al 2 O 3 are arranged on the outer periphery of a heat-resistant stainless steel drum in parallel to the drum in the axial direction and at equal intervals. An oxide superconducting wire having a high critical current value can be produced by fixing, winding a wire in a solenoid shape on this, providing an air insulating layer between the wire and the drum, and performing heat treatment.
これに対して、耐熱ステンレス製からなるドラム上に直接線材をソレノイド状に巻回して熱処理を施した場合には、ドラムの構成元素が拡散して超電導特性が低下し、一方、Al2O3で作製したドラム上に直接線材をソレノイド状に巻回して熱処理を施した場合には、ドラムの構成元素の拡散は防止し得るものの、ドラムの熱容量が大きいために温度上昇が遅く、ドラムからの熱流入が冷却開始後も続き冷却速度を所定の範囲内に制御できず、高い臨界電流値を有する酸化物超電導線材を製造することができない。 In contrast, when a heat treatment is performed by winding a wire directly on a drum made of heat-resistant stainless steel in a solenoid shape, the constituent elements of the drum are diffused and the superconducting properties are lowered, while Al 2 O 3 When the heat treatment is performed by winding the wire directly on the drum produced in the above in the form of a solenoid, the diffusion of the constituent elements of the drum can be prevented, but the temperature rise is slow due to the large heat capacity of the drum. Heat inflow continues after the start of cooling, and the cooling rate cannot be controlled within a predetermined range, and an oxide superconducting wire having a high critical current value cannot be manufactured.
本発明は、所定の熱処理パターンで正確な熱処理制御を可能とし、特性の優れた酸化物超電導線材の製造に適用することができる。 The present invention enables accurate heat treatment control with a predetermined heat treatment pattern, and can be applied to the production of an oxide superconducting wire having excellent characteristics.
1 線材支持具(耐熱ステンレス製のドラム)
2 棒状部材(Al2O3ロッド)
3 酸化物超電導線材の製造用支持具
4、13 線材
5、14 電気炉
10 線材支持具
11 支柱
12 網状の支持板
1 Wire support (drum made of heat-resistant stainless steel)
2 Rod-shaped member (Al 2 O 3 rod)
DESCRIPTION OF
Claims (8)
Oxidation characterized in that a rod-shaped member made of a plurality of ceramics is arranged on the surface of a cylindrical wire support made of a heat-resistant metal material or ceramic at a predetermined interval in parallel to the axial direction of the wire support. Support for manufacturing superconducting wire.
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CN105529093A (en) * | 2016-02-03 | 2016-04-27 | 安徽瑞昊缆业有限公司 | Self-heating anti-cracking cable |
CN105529095A (en) * | 2016-02-03 | 2016-04-27 | 安徽瑞昊缆业有限公司 | Multi-core self heating cable |
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CN105529093A (en) * | 2016-02-03 | 2016-04-27 | 安徽瑞昊缆业有限公司 | Self-heating anti-cracking cable |
CN105529095A (en) * | 2016-02-03 | 2016-04-27 | 安徽瑞昊缆业有限公司 | Multi-core self heating cable |
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