WO2013153651A1 - Matériau de câblage de film mince d'oxyde supraconducteur, et procédé de production associé - Google Patents
Matériau de câblage de film mince d'oxyde supraconducteur, et procédé de production associé Download PDFInfo
- Publication number
- WO2013153651A1 WO2013153651A1 PCT/JP2012/060015 JP2012060015W WO2013153651A1 WO 2013153651 A1 WO2013153651 A1 WO 2013153651A1 JP 2012060015 W JP2012060015 W JP 2012060015W WO 2013153651 A1 WO2013153651 A1 WO 2013153651A1
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- WIPO (PCT)
- Prior art keywords
- thin film
- oxide superconducting
- superconducting thin
- heat treatment
- treatment step
- Prior art date
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- 239000010409 thin film Substances 0.000 title claims abstract description 103
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 239000002887 superconductor Substances 0.000 title abstract description 10
- 239000000463 material Substances 0.000 title abstract 3
- 239000010408 film Substances 0.000 claims abstract description 32
- 239000000758 substrate Substances 0.000 claims abstract description 31
- 238000001354 calcination Methods 0.000 claims abstract description 24
- 229910052751 metal Inorganic materials 0.000 claims abstract description 13
- 239000002184 metal Substances 0.000 claims abstract description 13
- 150000002902 organometallic compounds Chemical class 0.000 claims abstract description 13
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 6
- 239000011737 fluorine Substances 0.000 claims abstract description 6
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims abstract 2
- 238000010438 heat treatment Methods 0.000 claims description 39
- 238000000034 method Methods 0.000 claims description 27
- 239000011248 coating agent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 18
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical group [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 claims description 10
- 238000000197 pyrolysis Methods 0.000 claims description 6
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
- 230000001681 protective effect Effects 0.000 claims description 3
- 230000000630 rising effect Effects 0.000 claims 1
- 230000008021 deposition Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 14
- 229910001233 yttria-stabilized zirconia Inorganic materials 0.000 description 9
- 239000010949 copper Substances 0.000 description 8
- 239000013078 crystal Substances 0.000 description 8
- 239000007789 gas Substances 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 229910052802 copper Inorganic materials 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 238000010304 firing Methods 0.000 description 3
- -1 organic acid salt Chemical class 0.000 description 3
- 238000005325 percolation Methods 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 239000011800 void material Substances 0.000 description 3
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 229910052788 barium Inorganic materials 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011888 foil Substances 0.000 description 2
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 2
- POILWHVDKZOXJZ-ARJAWSKDSA-M (z)-4-oxopent-2-en-2-olate Chemical class C\C([O-])=C\C(C)=O POILWHVDKZOXJZ-ARJAWSKDSA-M 0.000 description 1
- 241000954177 Bangana ariza Species 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910001080 W alloy Inorganic materials 0.000 description 1
- AYJRCSIUFZENHW-DEQYMQKBSA-L barium(2+);oxomethanediolate Chemical compound [Ba+2].[O-][14C]([O-])=O AYJRCSIUFZENHW-DEQYMQKBSA-L 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000007607 die coating method Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000007735 ion beam assisted deposition Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 229940038504 oxygen 100 % Drugs 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004549 pulsed laser deposition Methods 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Images
Classifications
-
- 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
- H10N60/01—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
- H10N60/0324—Processes for depositing or forming copper oxide superconductor layers from a solution
Definitions
- the present invention relates to an oxide superconducting thin film wire and a method for producing the same, and more particularly to an oxide superconducting thin film wire excellent in superconducting properties produced by a coating pyrolysis method and a method for producing the same.
- One method of manufacturing an oxide superconducting thin film wire is a coating pyrolysis method (Metal Organic Deposition, abbreviated as MOD method) (Japanese Patent Laid-Open No. 2007-165153 (Patent Document 1)).
- a metal organic compound solution is applied to a substrate to prepare a coating film (coating film manufacturing process), and then the metal organic compound is heat-treated (calcined) at, for example, around 500 ° C. to remove the organic component of the metal organic compound.
- Crystallization is achieved by thermally decomposing (calcination heat treatment step) and heat-treating (main firing) the obtained pyrolyzate (MOD calcined film) at a higher temperature (for example, around 800 ° C.) (main heat treatment step).
- a higher temperature for example, around 800 ° C.
- main heat treatment step To produce an oxide superconducting thin film made of an oxide superconductor represented by REBa 2 Cu 3 O 7-X (RE: rare earth element), for example, and is a gas phase method mainly produced in vacuum Compared with (evaporation method, sputtering method, pulsed laser deposition method, etc.), the manufacturing facility is simple, and it is easy to cope with a large area and a complicated shape.
- REBa 2 Cu 3 O 7-X rare earth element
- the inventor of the present invention paid attention to the formation of cavities and foreign substances (hereinafter referred to as voids together) together with the superconducting phase in the production of oxide superconducting thin film wires using the MOD method.
- the volume ratio (void ratio) occupied by the voids affects the superconducting characteristics, particularly the critical current density Jc. Has a certain negative correlation, and it was confirmed that even a slight change in porosity significantly affects Jc.
- the present inventor has examined the allowable porosity for obtaining a stable and excellent superconducting characteristic, and as a result, by setting the porosity to 10% or less, a stable and excellent superconductivity It was confirmed that a characteristic oxide superconducting thin film wire can be obtained.
- the invention according to claim 1 is based on the above knowledge, An oxide superconducting thin film wire in which an oxide superconducting thin film is formed on a substrate using a coating pyrolysis method, The oxide superconducting thin film has a porosity of 10% or less.
- the porosity of the oxide superconducting thin film wire is 10% or less, an oxide superconducting thin film wire having excellent and excellent superconducting properties, particularly excellent Jc, can be provided.
- the porosity is more preferably 5% or less, and further preferably 2% or less.
- the invention described in claim 2 2.
- the oxide superconducting thin film having excellent superconducting characteristics is formed over the entire length by controlling the porosity to 10% or less, the superconducting characteristics having excellent stability can be obtained. It is possible to provide an oxide superconducting thin film wire having high yield. As described above, the present invention exhibits a particularly remarkable effect in a long oxide superconducting thin film wire.
- metal substrate for example, a biaxially oriented Ni—W alloy substrate, an IBAD wire, a clad type oriented metal substrate in which SUS, Cu, and Ni (plating) are laminated are preferably used.
- the invention according to claim 3 The oxide superconducting thin film wire according to claim 1 or 2, wherein an intermediate layer is formed between the substrate and the oxide superconducting thin film.
- an intermediate layer between the superconducting thin film By providing the intermediate layer, an oxide superconducting thin film with good crystal orientation can be formed.
- the intermediate layer include a CeO 2 (cerium oxide) layer, a Y 2 O 3 (yttrium oxide) layer, and a YSZ (yttria stabilized zirconia) layer.
- the CeO 2 layer has a crystal orientation. It has a function as a seed crystal for forming a good oxide superconducting thin film and a function of performing lattice matching with the oxide superconducting thin film.
- the Y 2 O 3 layer has a function as a seed crystal.
- the YSZ layer has a function as a buffer layer that suppresses diffusion between the substrate and the oxide superconducting thin film.
- it can also be set as the intermediate
- the invention according to claim 4 The oxide superconducting thin film wire according to any one of claims 1 to 3, wherein a periphery of the oxide superconducting thin film wire is covered with a protective / stable layer.
- the oxide superconducting thin film wire is covered with a protective / stable layer of silver, copper, etc., so that the oxide superconducting thin film is protected from direct exposure to the atmosphere, etc., and is stable for a long period of time. Characteristics can be maintained.
- the invention described in claim 5 5.
- the thickness of the oxide superconducting thin film is too thin, the superconducting characteristics cannot be sufficiently exhibited even if the porosity is low.
- the invention described in claim 6 6.
- the oxide superconducting thin film If the oxide superconducting thin film is too thick, the oxide superconducting thin film cracks and inhibits the current, so that the superconducting characteristics cannot be fully exhibited.
- the invention described in claim 7 The oxide superconducting thin film according to any one of claims 1 and 6, wherein the oxide superconducting thin film is formed by a coating pyrolysis method using a metal organic compound containing no fluorine. It is a wire.
- the MOD method using a metal organic compound that does not contain fluorine differs from the TFA-MOD method using an organic acid salt containing fluorine. Because it does not generate dangerous gas such as hydrogen fluoride gas, it is environmentally friendly. Moreover, since it is not necessary to provide equipment for treating the generated hydrogen fluoride gas, an increase in cost can be suppressed, and an inexpensive oxide superconducting thin film wire can be provided.
- the invention according to claim 8 provides: It is a manufacturing method of the oxide superconducting thin film wire according to any one of claims 1 to 7, A coating film production process for producing a coating film by applying a solution of a metal organic compound on a substrate; A calcining heat treatment step for producing a calcined film by thermally decomposing and removing organic components contained in the metal organic compound of the coating film; A calcination heat treatment step of crystallizing the calcined film to produce an oxide superconducting thin film, The method for producing an oxide superconducting thin film wire, wherein a temperature increase rate in the calcining heat treatment step is 2 ° C./min or less.
- the rate of temperature rise is 2 ° C./min or less, the thermal decomposition of the organic component proceeds slowly and the decomposition gas tends to escape, so that generation of voids is suppressed and a dense calcined film can be formed. It is more preferably 1 ° C./min or less, and further preferably 0.5 ° C./min or less.
- the invention according to claim 9 is: 9.
- the intermediate heat treatment step of performing thermal decomposition of barium carbonate formed in the calcining heat treatment step is provided between the calcining heat treatment step and the main baking heat treatment step. It is a manufacturing method of an oxide superconducting thin film wire.
- the oxide superconducting thin film wire in this example includes a metal substrate 1 on which a SUS foil 11, a Cu thin film layer 12, and a Ni plating layer 13 are laminated, a Y 2 O 3 layer 21, a YSZ layer 22, The intermediate layer 2 on which the CeO 2 layer 23 is laminated and the YBCO oxide superconducting thin film layer 3 are configured.
- (2) Production of oxide superconducting thin film wire The YBCO oxide superconducting thin film wire was produced by the following steps. (A) Preparation of substrate An alignment metal substrate 1 was prepared as a substrate.
- a Y 2 O 3 layer 21 having a thickness of 100 nm, a YSZ single crystal layer 22 having a thickness of 400 nm, and a CeO 2 layer 23 having a thickness of 60 nm are formed in this order on the oriented metal substrate 1.
- An intermediate layer 2 composed of three layers was provided.
- FIG. 3 is a diagram showing a temperature profile of the heat treatment in this example. However, in FIG. 3, only the last three times are described in the calcination heat treatment process. The same applies to FIGS. 4 to 6.
- (I) Calcining heat treatment step The substrate on which the coating film has been formed is placed in an atmosphere furnace, and gradually heated up to 500 ° C.
- Comparative Example 1 The oxide of Comparative Example 1 was prepared in the same manner as in Example except that the temperature was raised to 500 ° C. at a rate of temperature increase of 10 ° C./min in the calcination heat treatment, and the calcined film was formed by holding for 30 minutes. A superconducting thin film wire was obtained. The temperature profile at this time is shown in FIG.
- the oxide superconducting thin film wire of the comparative example 2 was obtained like the comparative example 1 except not having performed intermediate heat processing.
- the temperature profile at this time is shown in FIG. 4).
- Evaluation The following evaluation was performed on the oxide superconducting thin film wires of Examples and Comparative Examples 1 and 2.
- (1) Porosity In FIG. 7, the SEM photograph of the cross section of the oxide superconducting thin film wire of an Example is shown. Note that the upper and lower photographs are the same photograph only by changing the contrast. As shown in FIG. 7, in the oxide superconducting thin film of the example, black portions indicating voids are hardly seen. Actually, the obtained porosity was 2%, which was an extremely small value.
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- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
La présente invention concerne un matériau de câblage de film mince d'oxyde supraconducteur, obtenu en formant un film mince d'oxyde supraconducteur sur un substrat en utilisant un dépôt organique métallique. La porosité du film mince d'oxyde supraconducteur n'est pas supérieure à 10 %. Le film mince d'oxyde supraconducteur est formé par dépôt organique métallique utilisant un composé organique métallique ne comprenant pas de fluor. L'invention concerne en outre un procédé de production de matériau de câblage de film mince d'oxyde supraconducteur, comprenant les étapes suivantes : une étape consistant à produire un film appliqué, dans laquelle une solution du composé organique métallique est appliquée sur un substrat afin de produire un film appliqué ; une étape consistant en une calcination préliminaire, dans laquelle les composants organiques inclus dans le composé organique métallique du film appliqué sont thermiquement décomposés et retirés afin de produire un film de calcination préliminaire ; et une étape consistant en une calcination principale, dans laquelle le film de calcination préliminaire est cristallisé afin de produire le film mince d'oxyde supraconducteur. La vitesse d'élévation de température lors de l'étape de calcination préliminaire n'est pas supérieure à 2 °C/min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2012/060015 WO2013153651A1 (fr) | 2012-04-12 | 2012-04-12 | Matériau de câblage de film mince d'oxyde supraconducteur, et procédé de production associé |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| PCT/JP2012/060015 WO2013153651A1 (fr) | 2012-04-12 | 2012-04-12 | Matériau de câblage de film mince d'oxyde supraconducteur, et procédé de production associé |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2013153651A1 true WO2013153651A1 (fr) | 2013-10-17 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/JP2012/060015 WO2013153651A1 (fr) | 2012-04-12 | 2012-04-12 | Matériau de câblage de film mince d'oxyde supraconducteur, et procédé de production associé |
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| Country | Link |
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| WO (1) | WO2013153651A1 (fr) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110544562A (zh) * | 2018-05-29 | 2019-12-06 | 北京交通大学 | 具有多孔含氟可溶聚酰亚胺绝缘涂层的钇系高温超导带材 |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010049891A (ja) * | 2008-08-20 | 2010-03-04 | Sumitomo Electric Ind Ltd | 酸化物超電導薄膜の製造方法 |
| JP2011198469A (ja) * | 2010-03-17 | 2011-10-06 | Toshiba Corp | 絶縁被覆酸化物超電導線材および樹脂含浸超電導コイル |
| JP2011230946A (ja) * | 2010-04-26 | 2011-11-17 | National Institute Of Advanced Industrial Science & Technology | 酸化物超電導薄膜の製造方法 |
| JP2012043734A (ja) * | 2010-08-23 | 2012-03-01 | Fujikura Ltd | 酸化物超電導線材およびその製造方法 |
-
2012
- 2012-04-12 WO PCT/JP2012/060015 patent/WO2013153651A1/fr active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010049891A (ja) * | 2008-08-20 | 2010-03-04 | Sumitomo Electric Ind Ltd | 酸化物超電導薄膜の製造方法 |
| JP2011198469A (ja) * | 2010-03-17 | 2011-10-06 | Toshiba Corp | 絶縁被覆酸化物超電導線材および樹脂含浸超電導コイル |
| JP2011230946A (ja) * | 2010-04-26 | 2011-11-17 | National Institute Of Advanced Industrial Science & Technology | 酸化物超電導薄膜の製造方法 |
| JP2012043734A (ja) * | 2010-08-23 | 2012-03-01 | Fujikura Ltd | 酸化物超電導線材およびその製造方法 |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110544562A (zh) * | 2018-05-29 | 2019-12-06 | 北京交通大学 | 具有多孔含氟可溶聚酰亚胺绝缘涂层的钇系高温超导带材 |
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