WO2011071103A1 - 希土類超電導膜形成用溶液およびその製造方法 - Google Patents

希土類超電導膜形成用溶液およびその製造方法 Download PDF

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WO2011071103A1
WO2011071103A1 PCT/JP2010/072104 JP2010072104W WO2011071103A1 WO 2011071103 A1 WO2011071103 A1 WO 2011071103A1 JP 2010072104 W JP2010072104 W JP 2010072104W WO 2011071103 A1 WO2011071103 A1 WO 2011071103A1
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film
solution
rare earth
producing
metal
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PCT/JP2010/072104
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English (en)
French (fr)
Japanese (ja)
Inventor
高明 真部
巖 山口
俊弥 熊谷
貢 相馬
近藤　和吉
謙一 塚田
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独立行政法人産業技術総合研究所
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Priority to JP2011545237A priority Critical patent/JP5445982B2/ja
Priority to US13/514,139 priority patent/US8865628B2/en
Priority to EP10836023.1A priority patent/EP2511235B1/en
Priority to CN201080056222.5A priority patent/CN102652112B/zh
Publication of WO2011071103A1 publication Critical patent/WO2011071103A1/ja

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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/006—Compounds containing, besides copper, two or more other elements, with the exception of oxygen or hydrogen
    • 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 the manufacture of a superconducting composite metal oxide film aimed at application to superconducting microwave devices, current limiters, wires, and the like.
  • a solution containing an organic compound containing an atomic species that forms a superconducting film on various supports is used as a raw material, and this is applied on a substrate and subjected to heat treatment to thermally decompose the coating film.
  • a coating pyrolysis method for forming a superconducting film.
  • an organic compound containing an atomic species is dissolved as uniformly as possible in a solvent to prepare a homogeneous mixed solution, the solution is uniformly coated on a support, and heat treatment is performed to remove an organic substance or the like.
  • this manufacturing method Compared with other methods such as vacuum deposition, this manufacturing method has the advantage that it is a low-cost film forming method because it does not require a vacuum device, and the film formation on a long, large-area substrate is possible. It has the feature of being easy. Also, from the viewpoint of the characteristics of the superconducting film produced by this method, it was highly evaluated as being better than other production methods.
  • Non-Patent Documents 1 and 2 a superconductor can be formed by applying a trifluoroacetate solution on a support and heat-treating it in a steam atmosphere.
  • Non-patent Document 3 the Superconducting Engineering Laboratory announced that the process was improved and optimized to successfully produce a superconducting film having high critical current characteristics.
  • the present invention has been made in view of the above situation, and when a rare earth superconducting composite metal oxide film (hereinafter referred to as “rare earth superconducting film”) is produced by a coating pyrolysis method, a coating / firing process is performed. Without repeating, the object is to provide a coating solution that does not cause cracks in the heat treatment step for removing organic components even when the equivalent film thickness is 500 nm or more.
  • a metal ion of a metal species containing a rare earth element, barium and copper, pyridine and / or at least one tertiary amine at least one carboxylic acid group having 1 to 8 carbon atoms, If necessary, a metal complex coordinated with an acetylacetonato group is dissolved in a solvent obtained by adding a polyhydric alcohol to a monovalent linear alcohol having 1 to 8 carbon atoms and / or water.
  • a solution for producing a rare earth superconducting film characterized in that it is a homogeneous solution.
  • a method for producing a solution for producing a rare earth superconducting film further comprising adding a polyhydric alcohol to obtain a uniform solution.
  • the polyhydric alcohol is at least one selected from divalent alcohols and trivalent alcohols.
  • the present invention in forming a rare earth superconducting film having a film thickness of 500 nm or more, the number of steps of applying a raw material solution and a heat treatment step of removing organic components is reduced, so that all steps are shortened and resource saving is achieved. , Energy saving and cost reduction are realized.
  • the solution for producing the rare earth superconducting film of the present invention comprises pyridine and / or at least one tertiary amine and at least one carbon number of 1 with respect to metal ions of the metal species containing rare earth elements, barium and copper.
  • a metal complex in which a carboxylic acid group of ⁇ 8 and a acetylacetonato group are coordinated as necessary is obtained by adding a polyhydric alcohol to a monovalent linear alcohol having 1 to 8 carbon atoms and / or water. It is characterized in that it is dissolved in a solvent to make a uniform solution.
  • the homogeneous solution containing the metal complex of the present invention contains each metal component composed of rare earth metal, barium (Ba), and copper (Cu) as an essential component.
  • This solution is used to form an oxide superconducting film, and can be used to synthesize an inorganic compound containing these metal components by performing a heat treatment.
  • the essential rare earth metal elements include yttrium (Y) and lanthanoid elements, lanthanum (La), neodymium (Nd), samarium (Sm), europium (Eu), gadolinium (Gd), dysprosium (Dy). , Holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb), and lutetium (Lu). These rare earth metals can also use a plurality of metals selected from these.
  • rare earth metal barium and copper essential metal components
  • other rare earth metals such as cerium (Ce) and praseodymium (Pr), calcium
  • strontium the electrical characteristics of the resulting superconducting film can be changed.
  • any metal species that can be used as a metal species that can be used when forming a superconducting film can be used as appropriate.
  • the ratio of rare earth metal, barium, and copper is a rare earth 123 system having a ratio of 1: 2: 3 (hereinafter, for example, when the rare earth metal is yttrium, A superconducting film having a ratio of 1: 2: 4 (hereinafter referred to as Y124 when the rare earth metal is yttrium, for example).
  • the mixing ratio of the element species in the raw material solution is preferably a molar ratio of 1: 2: 3 to 1: 2: 4, but a preferable result can be obtained even with, for example, a composition lacking barium. , This ratio is not something that can be tied.
  • monovalent metals such as silver, divalent metals such as calcium and strontium, trivalent metals such as rare earth metals other than the essential rare earth metals constituting the superconducting phase, and tetravalent metals such as zirconium and hafnium are added to the above solution.
  • a superconductor containing an additive element or a compound thereof superconductors containing additive elements such as calcium and strontium or their compounds have different electrical characteristics from superconductors that do not contain them, so by controlling the ratio of metals in the solution, It is possible to control various characteristics such as critical temperature and critical current density.
  • these metal ions contain pyridine and / or at least one tertiary amine, at least one carboxylic acid group having 1 to 8 carbon atoms, and, if necessary, an acetylacetonate group.
  • the coordinated metal complex is uniformly dissolved.
  • tertiary amine which is one of the ligands in the metal complex, for example, trimethylamine, triethylamine, tripropylamine, tributylamine and the like are used, and “carboxylic acid group having 1 to 8 carbon atoms” is used.
  • carboxylic acid examples include 2-ethylhexanoic acid, caprylic acid, butyric acid, propionic acid, acetic acid, oxalic acid, citric acid, lactic acid, benzoic acid, and salicylic acid.
  • a metal species containing a rare earth element, barium and copper, a metal carboxylate having 1 to 8 carbon atoms and / or a metal acetylacetonate powder mixture, pyridine and / or It is prepared by adding at least one tertiary amine and at least one carboxylic acid having 1 to 8 carbon atoms.
  • the metal complex is dissolved in a solvent obtained by adding a polyhydric alcohol to a monovalent linear alcohol having 1 to 8 carbon atoms and / or water, It is a homogeneous solution. That is, the solution for producing a rare earth superconducting film of the present invention is obtained by adding pyridine and / or at least one tertiary amine and at least one carboxylic acid having 1 to 8 carbon atoms to the powder mixture. After the excess solvent is volatilized, the product is dissolved in a monovalent linear alcohol having 1 to 8 carbon atoms and / or water, and a polyhydric alcohol is added to obtain a uniform solution. Manufactured.
  • Examples of the monovalent linear alcohol having 1 to 8 carbon atoms include methanol, ethanol, n-propanol, n-butanol, n-pentanol, n-hexanol and the like, and a mixture thereof can also be used.
  • water can be used to dissolve the metal complex, and a mixture of one or more of the aforementioned monovalent linear alcohols having 1 to 8 carbon atoms and water can also be used.
  • the present invention by using a solvent in which a polyhydric alcohol is added to the linear alcohol having 1 to 8 carbon atoms and / or water, an effect that cracks do not occur in temporary firing can be obtained.
  • the polyhydric alcohol in the present invention include ethylene glycol, hexylene glycol, octylene glycol, glycerin, diethylene glycol, triethylene glycol, tetraethylene glycol, and propylene glycol.
  • the solution is applied onto a substrate to form a solution thin film of a metal-containing compound.
  • the solution coating method conventionally known methods, for example, various methods such as a dipping method, a spin coating method, a spray method, and a brush coating method can be used.
  • the substrate various materials and shapes can be used.
  • examples of materials include metals and alloys such as nickel, copper, gold, silver, stainless steel, and hastelloy, and metal oxides such as alumina, zirconia, titania, strontium titanate, lanthanum aluminate, neodymium gallate, and yttrium aluminate. Ceramics such as materials and silicon carbide are used, and the shape thereof is adopted regardless of the curved surface or flat surface. For example, any shape such as a plate shape, a linear shape, a coil shape, a fiber shape, a woven fabric shape, and a tubular shape can be used. Adopted.
  • the support may be porous.
  • a metal film or a metal oxide film such as zirconia or ceria is previously formed on the surface of the base material as an intermediate layer. Can be formed.
  • This step is a step of heating and baking the metal-containing compound film formed on the substrate as described above, and converting the film into a film made of barium carbonate, rare earth metal oxide and copper oxide. .
  • a temperature of 400 to 650 ° C., preferably 450 to 550 ° C. is adopted.
  • the equivalent film thickness is preferably 500 nm or more. Hold for 150-300 minutes and then cool down.
  • the firing atmosphere an atmosphere of air, oxygen, nitrogen, argon or the like is employed.
  • This step is a step of reacting barium carbonate, rare earth metal oxide, and copper oxide while baking the film formed in the preliminary baking step to remove carbon dioxide from the barium carbonate.
  • this firing step is performed under the condition that the oxygen partial pressure in the atmosphere is 0.01 to 100 Pa, preferably 1 to 20 Pa.
  • the condition where the oxygen partial pressure is 0.01 to 100 Pa can be formed by using an inert gas.
  • this firing step can be performed under a reduced pressure such that the oxygen partial pressure is 0.01 to 100 Pa, preferably 1 to 20 Pa.
  • the decomposition of barium carbonate can be carried out smoothly at a reduced temperature, so that the base material and / or the intermediate layer and Reaction between the composite metal oxides can be substantially avoided.
  • the general firing temperature in this step is 650 to 900 ° C. According to the firing conditions as described above in the present invention, it is possible to substantially prevent the reaction between the base material and / or the intermediate layer and the composite metal oxide as conventionally observed.
  • the composite metal oxide film formed in the main baking step is oxidized using molecular oxygen to form a composite metal oxide film having superconductivity.
  • the oxygen partial pressure in the atmosphere is maintained to be 0.01 to 100 Pa. Therefore, the superconducting properties of the obtained composite metal oxide film are unsatisfactory. It can be converted into an excellent composite metal oxide film.
  • the oxidation step for absorbing oxygen is preferably performed at an oxygen partial pressure of 0.2 to 1.2 atm.
  • the molecular oxygen pure oxygen or air is used.
  • the superconducting properties of the film are adversely affected by the carbon dioxide contained therein, so the carbon dioxide partial pressure in the air is reduced to 1 Pa or less, preferably 0.5 Pa or less by decarboxylation. It is good to adjust.
  • This oxidation step is performed at a medium to high temperature, and the reaction between the substrate and / or the intermediate layer and the composite metal oxide can be substantially avoided.
  • the temperature of this oxidation step is generally 400 to 900 ° C.
  • a superconducting composite metal oxide film having a film thickness of 500 nm or more can be formed on the substrate surface by performing each of the above steps once.
  • Example 1 Preparation of temporary fired film
  • a commercially available product manufactured by Nippon Kagaku Sangyo Co., Ltd.
  • acetylacetonate powder of yttrium, barium and copper is weighed so that the molar ratio of metal components is 1: 2: 3, and these are mixed to obtain a powder mixture. Obtained.
  • pyridine and propionic acid were added in amounts until the powder mixture was completely dissolved.
  • the concentration of the solution was set to an amount containing 0.2 to 0.3 mmol of rare earth metal species per 1 g of the solution.
  • 0.02 to 0.04 ml of ethylene glycol, hexylene glycol, octylene glycol, glycerin, diethylene glycol, triethylene glycol, tetraethylene glycol, or propylene glycol is added as an additive and uniformly added.
  • a coating solution was prepared. This solution was applied by spin coating on a sapphire substrate on which cerium oxide was previously deposited. This coating film was pre-baked to remove organic components by raising the temperature to 500 ° C. in an air stream containing water vapor with an oxygen partial pressure of 0.6 atm and a dew point of 24 ° C. Each additive used is shown in Table 1 below.
  • Comparative Example 1 Preparation of pre-baked film
  • a pre-fired film was prepared in the same manner as in Example 1 except that 0.02 ml of polyethylene glycol (400 manufactured by Wako Pure Chemical Industries, Ltd.) was added as an additive. There were thin cracks. The result confirmed with the optical microscope about the comparative example 1 is shown in FIG.
  • Example 2 Production of superconductor film
  • the substrate was a yttria-stabilized zirconia single crystal substrate on which cerium oxide was vapor-deposited in advance and the additive was any one of hexylene glycol, octylene glycol, and tetraethylene glycol.
  • a fired film was produced.
  • membrane after performing this baking process at 760 degreeC in the airflow of oxygen partial pressure 10Pa for 2 hours, oxygen was absorbed at atmospheric pressure and the Y123 superconductor film
  • the Y123 film thus prepared was examined with the naked eye and observed with an optical microscope at 40 to 1000 times, no cracks were generated. The results are shown in Table 3 below.
  • FIG. 3 shows the results of X-ray diffraction of a film prepared using hexylene glycol as an additive.
  • the criteria for determining the state of the film are the naked eye and the optical microscope VH7000 manufactured by Keyence, Inc., 40 to 100 times the entire surface of the film, and further 100 to 1000 times, several points of the film are observed, and cracks are observed. What was not done was defined as “no crack”.
  • Example 3 Production of superconductor film
  • a Y123 film having an equivalent film thickness of 550 nm was prepared in the same manner as in Example 2 except that the molar ratio of the metal components of yttrium, barium and copper was 1: 2: 3.7. It was found that no cracks were observed by observation with an optical microscope and that a c-axis oriented Y123 film was grown by X-ray diffraction.
  • Example 4 Production of superconductor film
  • a Y123 film having an equivalent film thickness of 550 nm was prepared in the same manner as in Example 2 except that the molar ratio of the metal components of yttrium, barium and copper was 1: 1.6: 3. It was found that no cracks were observed by observation with an optical microscope and that a c-axis oriented Y123 film was grown by X-ray diffraction.
  • Example 5 Production of superconductor film
  • a Y123 film having an equivalent film thickness of 550 nm was prepared in the same manner as in Example 2 except that the solvent for dissolving the dried complex was changed to a mixed solvent of n-pentanol and water. It was found that cracks were not observed by optical microscope observation, and that a c123-oriented Y123 film was grown by X-ray diffraction.
  • Example 6 Production of superconductor film
  • the equivalent film thickness is 550 nm in the same manner as in Example 2 except that the starting material is a commercial product (manufactured by Wako Pure Chemical Industries, Ltd.), yttrium, barium and copper acetate powder, and the solvent is trimethylamine and propionic acid.
  • the Y123 film was prepared, it was found that cracks were not observed with the naked eye and optical microscope observation at 40 to 1000 times, and that the c123-oriented Y123 film was grown by X-ray diffraction.
  • Example 7 Production of superconductor film
  • a Y123 superconductor film having a thickness of 680 nm was prepared in the same manner as in Example 2 except that the substrate was a strontium titanate single crystal substrate on which cerium oxide was vapor-deposited in advance.
  • the substrate was a strontium titanate single crystal substrate on which cerium oxide was vapor-deposited in advance.
  • the Y123 film thus prepared was examined with the naked eye and observed with an optical microscope at 40 to 1000 times, no cracks were generated. Further, it was found by X-ray diffraction using an X-ray diffractometer that a c-axis oriented film was grown. Further, when the critical current density of the obtained Y123 film was measured by an induction method at a liquid nitrogen temperature, it was 2.1 MA / cm 2 .

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PCT/JP2010/072104 2009-12-09 2010-12-09 希土類超電導膜形成用溶液およびその製造方法 WO2011071103A1 (ja)

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JP2011545237A JP5445982B2 (ja) 2009-12-09 2010-12-09 希土類超電導膜形成用溶液およびその製造方法
US13/514,139 US8865628B2 (en) 2009-12-09 2010-12-09 Solution for forming rare-earth superconductive film and production method thereof
EP10836023.1A EP2511235B1 (en) 2009-12-09 2010-12-09 Solution for forming rare-earth superconductive film, and method for producing same
CN201080056222.5A CN102652112B (zh) 2009-12-09 2010-12-09 稀土类超导膜形成用溶液及其制造方法

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CN102807372A (zh) * 2012-08-28 2012-12-05 西北有色金属研究院 一种钆钡铜氧致密膜的制备方法
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US11765908B1 (en) 2023-02-10 2023-09-19 Kepler Computing Inc. Memory device fabrication through wafer bonding

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EP2511235B1 (en) 2019-07-10
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CN102652112B (zh) 2014-09-03
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