WO2013015328A1 - 超電導薄膜用基材、超電導薄膜及び超電導薄膜の製造方法 - Google Patents
超電導薄膜用基材、超電導薄膜及び超電導薄膜の製造方法 Download PDFInfo
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- WO2013015328A1 WO2013015328A1 PCT/JP2012/068873 JP2012068873W WO2013015328A1 WO 2013015328 A1 WO2013015328 A1 WO 2013015328A1 JP 2012068873 W JP2012068873 W JP 2012068873W WO 2013015328 A1 WO2013015328 A1 WO 2013015328A1
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- 239000010409 thin film Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims description 37
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- 229910052596 spinel Inorganic materials 0.000 claims abstract description 41
- 239000011029 spinel Substances 0.000 claims abstract description 41
- 150000001875 compounds Chemical class 0.000 claims abstract description 32
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical class [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 claims abstract description 31
- 239000002184 metal Substances 0.000 claims abstract description 27
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 15
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- 239000000758 substrate Substances 0.000 claims description 38
- 238000010884 ion-beam technique Methods 0.000 claims description 9
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- 238000009792 diffusion process Methods 0.000 abstract description 14
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- 230000001629 suppression Effects 0.000 abstract description 2
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- 238000001552 radio frequency sputter deposition Methods 0.000 description 8
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- 239000000470 constituent Substances 0.000 description 7
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- 230000000694 effects Effects 0.000 description 5
- 238000011156 evaluation Methods 0.000 description 5
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- 238000007740 vapor deposition Methods 0.000 description 4
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Images
Classifications
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- 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
- H10N60/20—Permanent superconducting devices
- H10N60/203—Permanent superconducting devices comprising high-Tc ceramic materials
-
- 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
- H10N60/80—Constructional details
- H10N60/85—Superconducting active materials
- H10N60/855—Ceramic superconductors
-
- 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
-
- 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
- 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
-
- 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
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/26—Web or sheet containing structurally defined element or component, the element or component having a specified physical dimension
- Y10T428/263—Coating layer not in excess of 5 mils thick or equivalent
- Y10T428/264—Up to 3 mils
- Y10T428/265—1 mil or less
Definitions
- the present invention relates to a substrate for a superconducting thin film, a superconducting thin film, and a method for producing the superconducting thin film.
- a superconducting wire is produced in which an intermediate layer is formed on a base material and a superconducting layer made of an oxide superconductor exhibiting a superconducting phenomenon at a liquid nitrogen temperature (77 K) or higher is further formed on the intermediate layer.
- the superconducting characteristics greatly depend on the crystal orientation of the oxide superconductor, particularly the biaxial orientation. Further, in order to obtain a superconducting layer having high biaxial orientation, it is necessary to improve the crystal orientation on the surface of the intermediate layer serving as a base.
- Patent Document 1 Japanese Patent Application Laid-Open No. 2011-9106
- a lower layer called a bed layer is first formed on a metal substrate, and then MgO or the like is formed.
- IBAD method Ion Beam Assisted Deposition
- biaxial orientation the two orientations are collectively referred to as biaxial orientation.
- a cap layer made of CeO 2 or PrO 2 is formed on the forced alignment layer in order to further improve the biaxial orientation on the surface of the intermediate layer.
- a superconducting wire having good superconducting characteristics can be obtained.
- the bed layer is to have a function of suppressing the diffusion of the metal element from the metal substrate and a function of improving the orientation of the forced alignment layer formed by using the IBAD method.
- Patent Document 2 Japanese Patent No. 2641865
- a spinel compound such as MgAl 2 O 3 is formed on a silicon single crystal substrate by epitaxial growth, and a MgO film is further formed by epitaxial growth. Forming a layer is disclosed.
- Patent Document 1 discloses a method using ZrO 2 / Y 2 O 3 for a bed layer, but since there is no ability to prevent diffusion, it is necessary to form a film of a substance having an ability to prevent diffusion in the lower layer. .
- the present invention has been made in view of the above facts, and has a high effect of suppressing diffusion of a metal element from a base material, and has a configuration capable of improving the orientation of a forced orientation layer, a base material for a superconducting thin film, a superconducting thin film, and It aims at providing the manufacturing method of a superconducting thin film.
- ⁇ 1> Mainly composed of a base material containing a metal element, an unoriented spinel compound formed on the surface of the base material and comprising at least one transition metal element having a spinel crystal structure, Mg, and oxygen
- a superconducting thin film substrate comprising: a bed layer, and a forced orientation layer formed mainly on a rock salt type compound having a rock salt type crystal structure containing Mg and having biaxial orientation.
- ⁇ 2> Mainly composed of a base material containing a metal element, an unoriented spinel compound formed on the surface of the base material and comprising at least one transition metal element having a spinel crystal structure, Ba, and oxygen
- a substrate for a superconducting thin film comprising: a bed layer, and a forced orientation layer formed mainly on a rock salt type compound having a rock salt type crystal structure containing Ba and having biaxial orientation.
- the spinel compound is at least one of MgAl 2 O 4 , MgCr 2 O 4 , MgY 2 O 4 , MgLa 2 O 4, and MgGd 2 O 4. Wood.
- ⁇ 4> The substrate for a superconducting thin film according to any one of ⁇ 1> to ⁇ 3>, wherein the bed layer has a thickness of 10 nm to 500 nm.
- ⁇ 5> The substrate for a superconducting thin film according to any one of ⁇ 1> to ⁇ 4>, wherein the metal element of the substrate is Ni or Fe.
- ⁇ 6> The superconducting thin film substrate according to any one of ⁇ 1> to ⁇ 5>, and a surface of a forced alignment layer of the superconducting thin film substrate, and is formed of an oxide superconductor. And a superconducting thin film.
- ⁇ 7> forming a bed layer having a spinel crystal structure on the surface of a base material containing a metal element and comprising a transition metal and a non-oriented spinel compound containing Mg;
- a superconducting thin film substrate having a step of forming a biaxially oriented forced alignment layer mainly using a rock salt type compound having a rock salt type crystal structure containing Mg on the surface of the layer using an ion beam assist method Manufacturing method.
- a superconducting thin film substrate comprising: a step of forming a biaxially oriented forced alignment layer mainly using a rock salt type crystal structure compound containing Ba on the surface of the layer using an ion beam assist method. Manufacturing method.
- the present invention provides a superconducting thin film substrate, a superconducting thin film, and a method of manufacturing a superconducting thin film having a configuration that has a high effect of suppressing diffusion of metal elements from the substrate and can improve the orientation of the forced alignment layer. I was able to.
- FIG. 1 is a view showing a laminated structure of superconducting thin films according to an embodiment of the present invention.
- FIG. 2 is a cross-sectional view showing a detailed configuration of the superconducting wire substrate according to the embodiment of the present invention.
- FIG. 1 is a diagram showing a laminated structure of a superconducting thin film 1 according to an embodiment of the present invention.
- the superconducting thin film 1 has a laminated structure in which an intermediate layer 20, a superconducting layer 30, and a protective layer 40 are sequentially formed on a base material 10.
- middle layer 20 in FIG. 1 comprise the base material 2 for superconducting wires which concerns on embodiment of this invention.
- the base material 10 is a base material containing a metal element that diffuses toward the diffusion suppression layer 20 side. Although other constituent elements may be contained in the base material 10, it is preferably a low magnetic non-oriented metal base material composed of only one or plural kinds of metal elements.
- a material of the base material 10 for example, metals such as Cu, Ni, Ti, Mo, Nb, Ta, W, Mn, Fe, and Ag, which are excellent in strength and heat resistance, or alloys thereof can be used.
- metals such as Cu, Ni, Ti, Mo, Nb, Ta, W, Mn, Fe, and Ag, which are excellent in strength and heat resistance, or alloys thereof can be used.
- Fe or Ni metals or alloys thereof from the viewpoint of high corrosion resistance, it is preferable to use Fe or Ni metals or alloys thereof.
- nickel alloys such as stainless steel and Hastelloy (registered trademark), which are excellent in terms of corrosion resistance and heat resistance.
- Various ceramics may be arranged on these various metal materials.
- the shape of the base material 10 is not particularly limited, and various shapes such as a plate material, a wire material, and a strip can be used.
- the superconducting thin film 1 can be applied as a superconducting wire, and by using a tape-like substrate, it can be applied as a superconducting tape.
- the intermediate layer 20 is a layer formed on the base material 10 in order to achieve high in-plane orientation in the superconducting layer 30, and has physical characteristics such as a coefficient of thermal expansion and a lattice constant that are superconducting with the base material 10.
- the intermediate value with the oxide superconductor which comprises the layer 30 is shown. A specific layer structure will be described later.
- the superconducting layer 30 is preferably formed on the intermediate layer 20 and made of an oxide superconductor, particularly a copper oxide superconductor.
- an oxide superconductor particularly a copper oxide superconductor.
- REBa 2 Cu 3 O 7- ⁇ referred to as RE-123
- Bi 2 Sr 2 CaCu 2 O 8 + ⁇ including Bi-site Pb-doped
- Bi 2 Sr 2 Ca 2 Cu 3 O 10 + ⁇ including Pb-doped Bi site
- [Ca site may be Ba]
- (Cu, Mo) Sr 2 (Ce, Y) s Cu 2 O [referred to as (Cu, Mo) -12s2, s 1, 2, 3, 4]
- Ba (Pb, Bi) O 3 or Tl 2 Ba 2 Ca n-1 Cu n O 2n + 4 (n is an is an integer of 2 or more) may be used crystal material represented by a composition formula such.
- REBa 2 Cu 3 O 7- ⁇ is preferably used because it has good superconducting characteristics and a simple crystal structure.
- the crystal material may be a polycrystalline material or a single crystal material.
- RE in REBa 2 Cu 3 O 7- ⁇ is a single rare earth element or a plurality of rare earth elements such as Y, Nd, Sm, Eu, Gd, Dy, Ho, Er, Tm, Yb, and Lu.
- Y is preferable because it does not cause substitution with the Ba site.
- ⁇ is an oxygen nonstoichiometric amount, for example, 0 or more and 1 or less, and is preferably closer to 0 from the viewpoint of a high superconducting transition temperature.
- the oxygen non-stoichiometric amount may be less than 0, that is, take a negative value when high-pressure oxygen annealing or the like is performed using an apparatus such as an autoclave.
- ⁇ of the crystal material other than REBa 2 Cu 3 O 7- ⁇ represents an oxygen non - stoichiometric amount, for example, 0 or more and 1 or less.
- the film thickness of the superconducting layer 30 is not particularly limited, but is, for example, not less than 500 nm and not more than 3000 nm.
- the superconducting layer 30 As a method for forming (depositing) the superconducting layer 30, for example, TFA-MOD (Metal-Organic-Deposition-using-TriFluoroAcetates) method, PLD (Pulse-Laser-Deposition) method, CVD (Chemical-Vapor-Deposition) method, MOCVD (Metal-Organic-Chemical-Vapor-Deposition) Or sputtering.
- TFA-MOD Metal-Organic-Deposition-using-TriFluoroAcetates
- PLD Pulse-Laser-Deposition
- CVD Chemical-Vapor-Deposition
- MOCVD Metal-Organic-Chemical-Vapor-Deposition
- it is preferable to use the MOCVD method because it does not require a high vacuum, can be formed on a large-area base material 10 having a complicated shape, and is excellent in mass productivity.
- a protective layer 40 made of silver is formed on the upper surface of the superconducting layer 30 as described above, for example, by sputtering. Moreover, after manufacturing the superconducting thin film 1 by forming the protective layer 40, the superconducting thin film 1 may be subjected to heat treatment.
- FIG. 2 is a cross-sectional view showing a detailed configuration of the superconducting wire substrate 2 according to the embodiment of the present invention.
- the intermediate layer 20 of the superconducting wire substrate 2 has a configuration in which a bed layer 22, a forced orientation layer 24, an LMO layer 26, and a cap layer 28 are laminated in order.
- the bed layer 22 is formed on the base material 10 (the surface of the base material 10), suppresses the diffusion of the metal element of the base material 10, and improves the biaxial orientation of the forced orientation layer 24. Is a layer.
- the bed layer 22 is characterized by the bed layer 22 comprising at least one transition metal element having a spinel crystal structure, Mg or Ba, and oxygen. This is a layer mainly composed of a non-oriented spinel compound.
- non-oriented means that the axes of spinel compounds exceeding 50% of the bed layer 22 are not oriented.
- the “main body” indicates that the content is the largest among the constituent components contained in the bed layer 22.
- the spinel compound is an oxide represented by a composition formula of AB 2 O 4 and has two sites, an A site and a B site, in the crystal.
- the A site is selected from Mg and Ba
- the B site is selected from at least one transition metal.
- “at least one kind” for the transition metal used for the B site means that the B site is substituted with another transition metal element.
- the rock salt type compound of the forced alignment layer 24 contains the same metal element as the A site of the spinel compound.
- the spinel compound include at least one of MgAl 2 O 4 , MgCr 2 O 4 , MgY 2 O 4 , MgLa 2 O 4 , MgGd 2 O 4 , and BaAl 2 O 4 .
- MgO is used for the forced alignment layer 24
- the Mg layer is the same as the A site of the spinel compound, so that the bed layer 22 and the forced alignment layer 24 hardly react and can exist stably as a compound.
- 2 O 4 , MgCr 2 O 4 , MgY 2 O 4 , MgLa 2 O 4 and MgGd 2 O 4 are preferred.
- MgAl 2 O 4 is more preferable from the viewpoint of practical use.
- the thickness of the bed layer 22 is not particularly limited, but from the viewpoint of suppressing a decrease in the function of the bed layer 22 (a function of suppressing diffusion of a metal element from the base material 10 and a function of improving the orientation of the forced alignment layer).
- the thickness is preferably 10 nm or more, and preferably 500 nm or less from the viewpoint of suppressing warpage of the substrate 10.
- the thickness is more preferably 100 nm or less from the viewpoint of reducing the thickness due to a request for cost or the like.
- Examples of the method for forming (depositing) the bed layer 22 include a TFA-MOD method, a PLD method, a CVD method, an MOCVD method, and a sputtering method. Among these, it is preferable to use a sputtering method from the viewpoint of easy manufacture.
- a sputtering method an inert gas ion (for example, Ar + ) generated by plasma discharge is caused to collide with a vapor deposition source (spinel compound), and the ejected vapor deposition particles are deposited on the film formation surface to form a film.
- the film formation conditions at this time are appropriately set depending on the constituent material and film thickness of the bed layer 22.
- the RF sputtering output is 100 W or more and 500 W or less
- the wire conveyance speed is 10 m / h or more and 100 m / h or less.
- the film temperature is set to 20 ° C. or more and 500 ° C. or less.
- the forced orientation layer 24 is a layer that is formed immediately above the bed layer 22 (the surface of the bed layer 22), mainly composed of a rock salt type compound having a rock salt type crystal structure, and having biaxial orientation.
- “having biaxial orientation” means that c-axis orientation and a-axis in-plane orientation are high, and not only the a-axis and c-axis of all rock salt type compounds are oriented, This includes the case where the a-axis and c-axis of 90% or more of the rock salt type compound of the bed layer 22 are oriented.
- the c-axes and the a-axes are not only completely aligned in the same direction, but also have orientation when the c-axes and the a-axes have an angle within ⁇ 5 degrees.
- “main body” indicates that the content is the largest among the constituent components contained in the forced alignment layer 24.
- the rock salt type compound of the forced orientation layer 24 needs to select a metal element that does not cause a chemical reaction between the rock salt type compound of the forced orientation layer 24 and the spinel compound of the bed layer 22, the chemical reaction is ensured.
- Mg or Ba contained in the spinel compound of the bed layer 22 is included.
- the rock salt type compound includes at least one of MgO and BaO. From the viewpoint of practical use, MgO is more preferable. Further, for example, a part of the cation site may be replaced with another metal element such as (Mg, Ni) O.
- the film thickness of the forced alignment layer 24 is not particularly limited, but is, for example, 1 nm or more and 20 nm or less.
- a method of forming (depositing) the forced alignment layer 24 for example, a method of forming a film by the IBAD method in an atmosphere of argon, oxygen, or a mixed gas of argon and oxygen is used.
- vapor deposition particles ejected from a vapor deposition source (MgO or the like) by RF sputtering (or ion beam sputtering) are deposited on the film formation surface while irradiating an assist ion beam obliquely with respect to the film formation surface.
- the film formation conditions at this time are appropriately set depending on the constituent material and film thickness of the forced alignment layer 24.
- the assist ion beam voltage is 800 V to 1500 V
- the assist ion beam current is 80 to 350 mA
- assist ions The beam acceleration voltage may be set to 200 V
- the RF sputtering output may be set to 800 W to 1500 W
- the wire conveyance speed may be set to 40 m / h to 500 m / h
- the film formation temperature may be set to 5 ° C. to 350 ° C.
- forced alignment layer refers to a biaxially oriented layer formed by the IBAD method, and whether or not it is a forced alignment layer formed by the IBAD method is determined by X-ray diffraction measurement. Thus, it can be specified by analyzing whether the bed layer 22 is non-oriented and whether the layer to be the forced alignment layer 24 has biaxial orientation.
- the LMO layer 26 is disposed between the forced alignment layer 24 and the cap layer 28 and has a function of improving the lattice matching of the cap layer 28.
- Such an LMO layer 26 is an oxide layer made of a crystalline material whose composition formula is represented by LaMnMO 3 + ⁇ ( ⁇ is an oxygen non-stoichiometric amount). Although the value of ⁇ is not particularly limited, for example, ⁇ 1 ⁇ ⁇ 1.
- the thickness of the LMO layer 26 is not particularly limited, but is preferably 100 nm or less from the viewpoint of suppressing the surface roughness of the LMO layer 26, and is preferably 4 nm or more from the viewpoint of manufacturing. A specific value is 30 nm.
- Examples of the formation (film formation) method of the LMO layer 26 include film formation by a PLD method or an RF sputtering method performed while heating the substrate 10.
- the film forming conditions by the RF sputtering method may be appropriately set according to the M substitution amount x in La z (Mn 1 ⁇ x M x ) w O 3 + ⁇ that is a constituent material of the LMO layer 26, the film thickness of the LMO layer 26, and the like.
- the sputtering output is 100 W or more and 300 W or less
- the wire material conveyance speed is 20 m / h or more and 200 m / h or less
- the film formation temperature (base material heating temperature) is 800 ° C. or less
- the film formation atmosphere is 0.1 Pa or more and 1.5 Pa or less.
- An Ar gas atmosphere may be used.
- the cap layer 28 is formed on the LMO layer 26 and is a layer for protecting the LMO layer 26 and further improving lattice matching with the superconducting layer 30. Specifically, it is composed of a fluorite crystal structure containing a rare earth element and having self-orientation. This fluorite-type crystal structure is at least one selected from, for example, CeO 2 and PrO 2 .
- the cap layer 28 only needs to mainly include a fluorite-type crystal structure, and may further contain impurities.
- the thickness of the cap layer 28 is not particularly limited, but is preferably 50 nm or more, and more preferably 300 nm or more in order to obtain sufficient orientation. However, if it exceeds 600 nm, the film formation time increases, so it is preferably 600 nm or less.
- the film forming conditions by the RF sputtering method may be appropriately set depending on the constituent material, film thickness, etc. of the cap layer 28.
- the RF sputtering output may be 200 W to 1000 W
- the wire conveyance speed may be 2 m / h to 50 m / h
- the film formation temperature may be 450 ° C. to 800 ° C.
- At least one transition metal having a spinel crystal structure as a base of the forced alignment layer 24 composed of a rock salt type compound having a rock salt type crystal structure and having biaxial orientation. It has a bed layer 22 composed of a spinel compound composed of an element, Mg or Ba, and oxygen, and the spinel compound and the rock salt type compound contain the same metal element (Mg or Ba), so that the spinel crystal structure Since the crystal salt stability of the rock salt type compound is suppressed and the rock salt type compound of the forced orientation layer 24 and the spinel compound of the bed layer 22 do not chemically react, the orientation of the forced orientation layer 24 can be improved. . If the orientation of the forced orientation layer 24 can be increased, the orientation of the superconducting layer 30 formed as an upper layer can be enhanced, and thus the critical current characteristics of the superconducting thin film 1 can be improved.
- the LMO layer 26, the cap layer 28, and the protective layer 40 can be omitted.
- another layer can be added to the intermediate layer 20 instead of the LMO layer 26.
- the bed layer 22 is formed by forming a film using a spinel compound as a target has been described.
- MgO is mixed with Al 2 under appropriate conditions.
- the spinel compound bed layer 22 can also be formed by forming a film on O 3 .
- the spinel compound bed layer 22 can be formed by high-temperature heat treatment or ion beam irradiation.
- the superconducting thin film 1 has been described.
- the superconducting thin film 1 can be applied to various other devices.
- it can be applied to devices such as a superconducting current limiting device, SMES (Superconducting Magnetic Energy Storage), a superconducting transformer, an NMR (nuclear magnetic resonance) analyzer, a single crystal pulling device, a linear motor car, and a magnetic separation device.
- SMES Superconducting Magnetic Energy Storage
- NMR nuclear magnetic resonance
- the superconducting thin film substrate the superconducting thin film, and the method for producing the superconducting thin film according to the present invention will be described with reference to examples, but the present invention is not limited to these examples.
- a tape-shaped Hastelloy substrate was prepared as a base material, and one surface on the Hastelloy substrate was subjected to surface polishing by mechanical polishing or electric field polishing. Then, a bed layer having a thickness of 20 to 120 nm was formed on the surface-polished Hastelloy substrate by using a sputtering apparatus and changing the material for each of Examples and Comparative Examples. Then, a forced alignment layer (IBAD-MgO layer) made of MgO was formed on the bed layer by an IBAD method at a room temperature of 1 to 20 nm.
- IBAD-MgO layer forced alignment layer
- an LMO layer made of LMO was formed to a thickness of 200 nm by sputtering.
- a cap layer made of CeO 2 was formed to a thickness of 200 nm at 650 ° C. by sputtering.
- a superconducting layer made of YBCO was formed into a superconducting thin film (superconducting wire) by depositing 1 ⁇ m thick at 845 ° C. by MOCVD.
- the bed layer material is MgAl 2 O 4
- the bed layer material is MgCr 2 O 4
- the bed layer material is MgY 2 O 4
- the bed layer material was MgLa 2 O 4
- the bed layer material was MgGd 2 O 4
- Comparative Example 1 the bed layer was not prepared, and in Comparative Example 2, the material of the bed layer was GZO.
- the bed layer material was Y 2 O 3
- Comparative Example 4 the bed layer material was Al 2 O 3 .
- the bed layer has a two-layer structure of Y 2 O 3 and Al 2 O 3.
- the bed layer has a two-layer structure of Y 2 O 3 and Al 2 O 3 containing Zr—O. It was.
- the orientation ratio was calculated using a Rigaku X-ray diffractometer RINT-ULTIMAIII. Specifically, CuK ⁇ rays are used in the X-ray diffractometer, the tube voltage is 40 kV, the tube current is 40 mA, the scan speed is 2.0 deg / min, the light receiving slit is 0.15 mm, the scan range is 2 ⁇ of 5 °. Measurement was performed under a condition of ⁇ 135 ° to obtain an X-ray diffraction pattern of each superconducting wire. From the obtained diffraction pattern, the orientation ratio was determined using the following equation.
- the energizing characteristics were evaluated by measuring the critical current Ic of the obtained superconducting thin film (line width 10 mm).
- the critical current Ic was measured using a four-terminal method with the superconducting thin film immersed in liquid nitrogen.
- the voltage terminal was 1 cm, and the electric field reference was 1 ⁇ V / cm.
- Table 1 shows the results of evaluating the superconducting thin films according to the examples and comparative examples by the above evaluation methods.
- ⁇ indicates that the critical current Ic is 250 A or more
- ⁇ indicates that the critical current Ic is 180 A or more and less than 250 A
- ⁇ indicates that the critical current Ic is less than 180 A.
- ⁇ indicates that the orientation ratio is 95% or more
- ⁇ indicates that the orientation ratio is 80% or more and less than 95%
- x indicates that the orientation ratio is less than 80%.
- the material of the bed layer was a spinel compound such as MgAl 2 O 4 , so that the orientation of the superconducting layer was higher than in Comparative Examples 1 to 6. It was found that a superconducting thin film having a high critical current Ic can be obtained. This is thought to be due to the high effect of suppressing the diffusion of metal elements from the base material while suppressing the reaction with rock salt type compounds due to the crystal stability of the spinel crystal structure, and the improved orientation of the forced alignment layer. .
- Reference numeral 1 denotes a superconducting thin film.
- Reference numeral 2 denotes a substrate for a superconducting thin film.
- Reference numeral 10 denotes a base material.
- Reference numeral 22 denotes a bed layer.
- Reference numeral 24 denotes a forced alignment layer.
- Reference numeral 30 denotes a superconducting layer.
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Abstract
Description
また、この強制配向層を得た後は、中間層表面の2軸配向性をさらに向上させるため、強制配向層上にCeO2又はPrO2などからなるキャップ層を形成している。そして、当該キャップ層上に超電導層を形成することで、良好な超電導特性を有する超電導線が得られる。
このとき、ベッド層に求められるのは、金属基材からの金属元素の拡散を抑制する機能やIBAD法を用いて形成する強制配向層の配向性を高める機能を有することである。これらの機能を実現するため、ベッド層としてAl2O3/Y2O3もしくはGZOを採用するのが一般的である。
<1>金属元素を含む基材と、前記基材の表面に形成され、スピネル型結晶構造を有した少なくとも1種の遷移金属元素と、Mgと、酸素とからなる非配向のスピネル化合物を主体とするベッド層と、前記ベッド層の表面に形成され、Mgを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層と、を備える超電導薄膜用基材。
<2>金属元素を含む基材と、前記基材の表面に形成され、スピネル型結晶構造を有した少なくとも1種の遷移金属元素と、Baと、酸素とからなる非配向のスピネル化合物を主体とするベッド層と、前記ベッド層の表面に形成され、Baを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層と、を備える超電導薄膜用基材。
<3>前記スピネル化合物は、MgAl2O4,MgCr2O4,MgY2O4,MgLa2O4及びMgGd2O4の少なくとも1種である、前記<1>に記載の超電導薄膜用基材。
<4>前記ベッド層の厚みが10nm以上500nm以下である、前記<1>~前記<3>の何れか1つに記載の超電導薄膜用基材。
<5>前記基材の金属元素は、Ni又はFeである、前記<1>~前記<4>の何れか1つに記載の超電導薄膜用基材。
<6>前記<1>~前記<5>の何れか1つに記載の超電導薄膜用基材と、前記超電導薄膜用基材の強制配向層の表面に形成され、酸化物超電導体で構成された超電導層と、を備える超電導薄膜。
<7>金属元素を含む基材の表面に、スピネル型結晶構造を有し、1種の遷移金属と、Mgを含む非配向のスピネル化合物で構成されたベッド層を形成する工程と、前記ベッド層の表面に、Mgを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層を、イオンビームアシスト法を用いて形成する工程と、を有する超電導薄膜用基材の製造方法。
<8>金属元素を含む基材の直上に、スピネル型結晶構造を有し、1種の遷移金属と、Baを含む非配向のスピネル化合物で構成されたベッド層を形成する工程と、前記ベッド層の表面に、Baを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層を、イオンビームアシスト法を用いて形成する工程と、を有する超電導薄膜用基材の製造方法。
図1は、本発明の実施形態に係る超電導薄膜1の積層構造を示す図である。
図1に示すように、超電導薄膜1は、基材10上に中間層20、超電導層30、保護層40が順に形成された積層構造を有している。そして、図1におけるテープ状の基材10と中間層20が、本発明の実施形態に係る超電導線用基材2を構成する。
基材10中には他の構成元素が含まれてもよいが、単一又は複数種の金属元素のみからなる低磁性の無配向金属基材であることが好ましい。基材10の材料としては、例えば、強度及び耐熱性に優れた、Cu,Ni,Ti,Mo,Nb,Ta,W,Mn,Fe,Ag等の金属又はこれらの合金を用いることができる。中でも、耐食性が高いという観点からFeやNiの金属又はこれらの合金を用いることが好ましい。そして、特に好ましいのは、耐食性及び耐熱性の点で優れているステンレス、ハステロイ(登録商標)などのニッケル系合金である。また、これら各種金属材料上に各種セラミックスを配してもよい。
また、REBa2Cu3O7-δ以外の結晶材料のδも酸素不定比量を表し、例えば0以上1以下である。
図2は、本発明の実施形態に係る超電導線用基材2の詳細構成を示す断面図である。
図2に示すように、超電導線用基材2の中間層20は、ベッド層22と、強制配向層24と、LMO層26と、キャップ層28と、を順に積層した構成である。
具体的にスピネル化合物としては、MgAl2O4,MgCr2O4,MgY2O4,MgLa2O4,MgGd2O4,BaAl2O4 の少なくとも1種が挙げられる。中でも、強制配向層24にMgOを用いる場合には、スピネル化合物のAサイトと同一のMgを有することでベッド層22と強制配向層24が反応しにくく、化合物として安定して存在できることから、MgAl2O4,MgCr2O4,MgY2O4,MgLa2O4及びMgGd2O4の少なくとも1種であることが好ましい。さらに、実用的という観点からMgAl2O4であることがより好ましい。
スパッタ法を用いる場合、プラズマ放電で発生した不活性ガスイオン(例えばAr+)を蒸着源(スピネル化合物)に衝突させ、はじき出された蒸着粒子を成膜面に堆積させて成膜する。このときの成膜条件は、ベッド層22の構成材料や膜厚等によって適宜設定されるが、例えば、RFスパッタ出力は100W以上500W以下、線材搬送速度は10m/h以上100m/h以下、成膜温度は20℃以上500℃以下とされる。
具体的に、岩塩型化合物としては、MgO及びBaOの少なくとも1種が挙げられる。実用的という観点からMgOであることがより好ましい。また、例えば、(Mg,Ni)O等のように、陽イオンサイトの一部を他の金属元素に置換してもよい。
本実施形態では、以上のように、岩塩型結晶構造の岩塩型化合物で構成されて2軸配向性を有する強制配向層24の下地として、スピネル型結晶構造を有し、少なくとも1種の遷移金属元素と、Mg又はBaと、酸素とからなるスピネル化合物で構成されたベッド層22を有し、スピネル化合物と岩塩型化合物は同一の金属元素(Mg又はBa)を含むことで、スピネル型結晶構造の結晶的安定性から岩塩型化合物との反応を抑制しつつ、強制配向層24の岩塩型化合物とベッド層22のスピネル化合物とが化学反応しないことから、強制配向層24の配向性を向上できる。そして、強制配向層24の配向性を高めることができれば、上層として形成される超電導層30の配向性を高められ、もって超電導薄膜1の臨界電流特性を向上することができる。
なお、本発明を特定の実施形態について詳細に説明したが、本発明はかかる実施形態に限定されるものではなく、本発明の範囲内にて他の種々の実施形態が可能であることは当業者にとって明らかであり、例えば上述の複数の実施形態は、適宜、組み合わされて実施可能である。また、以下の変形例を、適宜、組み合わせてもよい。
なお、日本出願2011-162331の開示はその全体が参照により本明細書に取り込まれる。
本明細書に記載された全ての文献、特許出願、および技術規格は、個々の文献、特許出願、および技術規格が参照により取り込まれることが具体的かつ個々に記載された場合と同程度に、本明細書中に参照により取り込まれる。
そして、表面研磨されたハステロイ基板の上に、スパッタリング装置を用いて実施例及び比較例毎に材料を変えて厚さ20~120nmのベッド層を成膜した。そして、このベッド層の上に、MgOからなる強制配向層(IBAD-MgO層)を、IBAD法により常温で1~20nm成膜した。強制配向層の上には、LMOからなるLMO層を、スパッタ法により200nm成膜した。このLMO層には、CeO2からなるキャップ層を、スパッタ法により650℃で200nm成膜した。キャップ層の上には、YBCOからなる超電導層を、MOCVD法により845℃で厚さ1μm成膜して超電導薄膜(超電導線)とした。
各超電導薄膜の実施例において、具体的に、実施例ではベッド層の材料をMgAl2O4とし、実施例2ではベッド層の材料をMgCr2O4とし、実施例3ではベッド層の材料をMgY2O4とし、実施例4ではベッド層の材料をMgLa2O4とし、実施例5ではベッド層の材料をMgGd2O4とした。
<比較例>
各超電導薄膜の比較例において、具体的に、比較例1ではベッド層を作成しないものとし、比較例2ではベッド層の材料をGZOとした。比較例3ではベッド層の材料をY2O3とし、比較例4ではベッド層の材料をAl2O3とした。また、比較例5ではベッド層をY2O3とAl2O3の2層構造とし、比較例6ではベッド層をZr-Oを含有したY2O3とAl2O3の2層構造とした。
以下、実施例1~5、比較例1~6で作製した超電導薄膜の評価方法及び評価結果について記載する。
各実施例及び比較例に係わる超電導薄膜の超電導層について、リガク製X線回折装置RINT-ULTIMAIIIを用いて配向率の算出を行った。具体的には、上記X線回折装置にてCuKα線を用い、管電圧を40kV、管電流を40mA、スキャンスピードを2.0deg/min、受光スリットを0.15mm、スキャン範囲として2θを5°~135°とする条件下で測定を行って、各超電導線材のX線回折パターンを得た。得られた回折パターンから、配向率を以下の式を用いて求めた。
通電特性は、得られた超電導薄膜(線幅10mm)の臨界電流Icを測定することにより評価した。臨界電流Icは、超電導薄膜を液体窒素に浸漬した状態で四端子法を用いて測定した。電圧端子は1cm、電界基準は1μV/cmとした。
以上の評価方法により各実施例及び比較例に係わる超電導薄膜について評価した結果を表1に示す。
符号2は、超電導薄膜用基材である。
符号10は、基材である。
符号22は、ベッド層である。
符号24は、強制配向層である。
符号30は、超電導層である。
Claims (8)
- 金属元素を含む基材と、
前記基材の表面に形成され、スピネル型結晶構造を有した少なくとも1種の遷移金属元素と、Mgと、酸素とからなる非配向のスピネル化合物を主体とするベッド層と、
前記ベッド層の表面に形成され、Mgを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層と、
を備える超電導薄膜用基材。 - 金属元素を含む基材と、
前記基材の表面に形成され、スピネル型結晶構造を有した少なくとも1種の遷移金属元素と、Baと、酸素とからなる非配向のスピネル化合物を主体とするベッド層と、
前記ベッド層の表面に形成され、Baを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層と、
を備える超電導薄膜用基材。 - 前記スピネル化合物は、MgAl2O4,MgCr2O4,MgY2O4,MgLa2O4及びMgGd2O4の少なくとも1種である、
請求項1に記載の超電導薄膜用基材。 - 前記ベッド層の厚みが10nm以上500nm以下である、
請求項1~請求項3の何れか1項に記載の超電導薄膜用基材。 - 前記基材の金属元素は、Ni又はFeである、
請求項1~請求項4の何れか1項に記載の超電導薄膜用基材。 - 請求項1~請求項5の何れか1項に記載の超電導薄膜用基材と、
前記超電導薄膜用基材の強制配向層の表面に形成され、酸化物超電導体で構成された超電導層と、
を備える超電導薄膜。 - 金属元素を含む基材の表面に、スピネル型結晶構造を有し、1種の遷移金属と、Mgを含む非配向のスピネル化合物で構成されたベッド層を形成する工程と、
前記ベッド層の表面に、Mgを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層を、イオンビームアシスト法を用いて形成する工程と、
を有する超電導薄膜用基材の製造方法。 - 金属元素を含む基材の直上に、スピネル型結晶構造を有し、1種の遷移金属と、Baを含む非配向のスピネル化合物で構成されたベッド層を形成する工程と、
前記ベッド層の表面に、Baを含む岩塩型結晶構造の岩塩型化合物を主体とし、2軸配向性を有する強制配向層を、イオンビームアシスト法を用いて形成する工程と、
を有する超電導薄膜用基材の製造方法。
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PCT/JP2012/068873 WO2013015328A1 (ja) | 2011-07-25 | 2012-07-25 | 超電導薄膜用基材、超電導薄膜及び超電導薄膜の製造方法 |
Country Status (5)
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US (1) | US20130137580A1 (ja) |
JP (1) | JPWO2013015328A1 (ja) |
KR (1) | KR20140040248A (ja) |
CN (1) | CN103069509A (ja) |
WO (1) | WO2013015328A1 (ja) |
Families Citing this family (2)
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EP2728590B9 (en) * | 2012-04-16 | 2018-09-05 | Furukawa Electric Co., Ltd. | Substrate for superconducting film, superconducting wire, and superconducting wire fabrication method |
EP3367394A4 (en) | 2015-11-06 | 2019-08-07 | Fujikura Ltd. | SUPERCONDUCTING OXIDE WIRE |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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JPH01185980A (ja) * | 1988-01-20 | 1989-07-25 | Sanyo Electric Co Ltd | 超電導積層体 |
JPH01241876A (ja) * | 1988-03-23 | 1989-09-26 | Nec Corp | 電子デバイス用基板 |
WO2010058823A1 (ja) * | 2008-11-21 | 2010-05-27 | 財団法人 国際超電導産業技術研究センター | 超電導膜成膜用基板、超電導線材及びそれらの製造方法 |
Family Cites Families (9)
Publication number | Priority date | Publication date | Assignee | Title |
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JP2641865B2 (ja) * | 1987-05-29 | 1997-08-20 | 日本電気株式会社 | 電子デバイス用基板 |
US5084438A (en) * | 1988-03-23 | 1992-01-28 | Nec Corporation | Electronic device substrate using silicon semiconductor substrate |
JPH03232723A (ja) * | 1990-02-09 | 1991-10-16 | Ricoh Co Ltd | 超伝導体 |
US6849580B2 (en) * | 2003-06-09 | 2005-02-01 | University Of Florida | Method of producing biaxially textured buffer layers and related articles, devices and systems |
US7718574B2 (en) * | 2004-04-08 | 2010-05-18 | Superpower, Inc. | Biaxially-textured film deposition for superconductor coated tapes |
JP4359649B2 (ja) * | 2007-03-29 | 2009-11-04 | 株式会社フジクラ | 多結晶薄膜とその製造方法及び酸化物超電導導体 |
JP2011009106A (ja) * | 2009-06-26 | 2011-01-13 | Fujikura Ltd | 酸化物超電導導体用基材及び酸化物超電導導体 |
JP5427553B2 (ja) * | 2009-10-30 | 2014-02-26 | 公益財団法人国際超電導産業技術研究センター | 酸化物超電導導体用基材及びその製造方法と酸化物超電導導体及びその製造方法 |
US8486864B2 (en) * | 2009-12-29 | 2013-07-16 | Ut-Battelle, Llc | Method for producing microstructured templates and their use in providing pinning enhancements in superconducting films deposited thereon |
-
2012
- 2012-07-25 CN CN2012800023500A patent/CN103069509A/zh active Pending
- 2012-07-25 WO PCT/JP2012/068873 patent/WO2013015328A1/ja active Application Filing
- 2012-07-25 US US13/814,580 patent/US20130137580A1/en not_active Abandoned
- 2012-07-25 KR KR1020147001676A patent/KR20140040248A/ko not_active Application Discontinuation
- 2012-07-25 JP JP2012552184A patent/JPWO2013015328A1/ja active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH01185980A (ja) * | 1988-01-20 | 1989-07-25 | Sanyo Electric Co Ltd | 超電導積層体 |
JPH01241876A (ja) * | 1988-03-23 | 1989-09-26 | Nec Corp | 電子デバイス用基板 |
WO2010058823A1 (ja) * | 2008-11-21 | 2010-05-27 | 財団法人 国際超電導産業技術研究センター | 超電導膜成膜用基板、超電導線材及びそれらの製造方法 |
Also Published As
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CN103069509A (zh) | 2013-04-24 |
KR20140040248A (ko) | 2014-04-02 |
US20130137580A1 (en) | 2013-05-30 |
JPWO2013015328A1 (ja) | 2015-02-23 |
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