WO2006011389A1 - RE-Ba-Cu-O系酸化物超電導体の作製方法 - Google Patents
RE-Ba-Cu-O系酸化物超電導体の作製方法 Download PDFInfo
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- C04B2235/6584—Oxygen containing atmosphere, e.g. with changing oxygen pressures at an oxygen percentage below that of air
Definitions
- the present invention is used for various applications such as superconducting bearings, superconducting magnetic transfer devices, superconducting permanent magnets, and magnetic shields.
- the present invention relates to a method for producing a system oxide superconductor.
- Je has a crystal orientation dependency that is maximum in an orientation parallel to the c-axis of the 1 2 3 crystal in a low magnetic field, so it is desirable to take advantage of this dependency.
- the MT G method (see S. Jin et. Al., Appl. Phys. Lett., 52 (1988), 2074), QMG method (M. Murakami et. Al., Jpn) (See J. Appl. Phys., 54 (1989), 2074.) and ⁇ C MG method (see SI Yoo et. Al .: Appl. Phys. Lett. 65 (1994), 633.) Melt growth method) is used.
- a raw material powder is molded into a predetermined shape by a uniaxial molding press apparatus and / or a cold isostatic press apparatus (CIP) using a metal mold, and this superconducting precursor (molded body) is formed.
- CIP cold isostatic press apparatus
- the RE 1 2 3 superconducting phase is once heated to the melting point or higher and then cooled to the melting point or lower for crystallization.
- the melt growth method is performed in air.
- LRE is a light rare earth element: La, Nd, Sm, Eu, Gd
- LRE ions replace Ba ions and deteriorate the superconducting properties.
- melt growth is performed under a low oxygen partial pressure to prevent the formation of a solid solution.
- a normal superconducting bulk material can be produced by partially melting a composition comprising R E 1 2 3 and R E 2 1 1 at a high temperature and then performing crystal growth.
- R E 1 2 3 a composition comprising R E 1 2 3 and R E 2 1 1 at a high temperature
- R E 1 2 3 a composition comprising R E 1 2 3 and R E 2 1 1 at a high temperature
- crystal growth a melting of R E 1 2 3
- high temperature and long-term melting may cause a reaction between the melt and the substrate material, which may deteriorate the properties of the grown superconducting crystal.
- the former R E 2 1 1 phase is mainly spherical, the latter R E 2 1 1 phase is needle-shaped, and both R E 2 1 1 phases coexist in the superconducting crystal. As a result, there is a limit in improving the performance of the superconducting bulk material.
- the present invention has developed a process that does not include the RE 1 2 3 phase pyrolysis process and does not require melting at a high temperature for a long time, and has a large size, high performance, and excellent mechanical properties.
- An object is to provide a method for producing a bulk body.
- the present inventor has earnestly studied a method for producing a RE—Ba—Cu 1 O-based oxide superconductor that does not include the RE 1 2 3 phase pyrolysis step.
- RE 2 B a 0 4 or RE 4 B a 3 0 9 (RE-B a-0 Compound, RE is one or more of rare earth elements) and B a-Cu-O-based liquid phase raw material, and the liquid phase component is melted and then crystal grown
- the superconducting crystal was found to grow according to the reaction.
- the R E 1 2 3 phase pyrolysis step can be omitted during the crystal growth process, and the R E 2 1 1 phase can be newly generated uniformly.
- U I NG method Universal Infiltration Groth Method
- the present inventor can perform the melting process at a low temperature and in a short time, thereby shortening the production time of a large superconducting bulk body, reducing characteristic deterioration due to residual oxygen, and It was found that characteristic deterioration due to reaction with the substrate material can be suppressed.
- the present invention has been made on the basis of the above findings, and the gist thereof is as follows.
- RE—B a—O compound (RE is one or more of rare earth elements) and B a—Cu—O liquid phase raw material
- RE — B a—O-based compound is RE 2 B aO 4 (RE is one or more of rare earth elements)
- the RE - B a - O-based compound and Z or B a - C u - O-based liquid phase feedstock is characterized by containing platinum (P t) or C E_ ⁇ 2 2 mass% or less
- the RE_B a —O compound and / or B a —C u —O liquid phase raw material further contains 30% by mass or less of silver (A g) as a dispersed phase.
- crystal growth can be performed at a low temperature and in a short time, characteristics can be improved by reducing residual oxygen and reaction with the substrate material, and the superconducting phase can be fine and Uniform dispersion is possible, and a large, high-performance superconducting bulk material can be produced.
- FIG. 1 is a diagram showing the structure of the superconductor of the present invention.
- Figure 2 shows the temperature dependence of the magnetic susceptibility.
- Figure 3 shows the magnetic field dependence of the critical current density.
- the present invention uses a RE_B a —O-based compound (RE is one or more of rare earth elements) and a Ba—C u —O-based liquid phase raw material as starting materials, and after melting the liquid phase components The crystal is grown.
- RE is one or more of rare earth elements
- Ba—C u —O-based liquid phase raw material as starting materials, and after melting the liquid phase components The crystal is grown.
- ⁇ System compounds and B a-Cu- ⁇ system liquid phase raw materials may be mixed in advance, and the form and production method are not particularly limited.
- the skeleton structure is preferably formed of fine particles of a RE—B a —O-based compound, but the entire space region where the Ba—Cu—O-based liquid phase raw material can permeate is used.
- the particle shape (spherical shape, needle shape, etc.), structure and manufacturing method are not particularly limited.
- the arrangement relationship between the RE-B a-O-based compound and the B a-Cu-O-based liquid phase raw material is as follows. There is no particular requirement as long as it is in a contact arrangement relationship capable of penetrating into the skin.
- the composition of the B a—Cu—O-based liquid phase raw material is selected in relation to the RE—B a—O-based compound.
- the crystallization is performed in terms of improving the critical current density (J e ) and improving the strength.
- the RE 1 2 3 phase preferably contains about 10 to 50 mol% of the RE 2 1 1 phase.
- the average composition of the composition formed from the RE—B a— ⁇ compound and the B & — 1—0 system liquid phase raw material is REB a 2 Cu 3 0 7 _ d (RE 1 2 3) + (10 to 50 mol%) RE 2 B a Cu 0 5 (RE 2 1 1) + (0 to 10 mol%) Ba 0 2 .
- RE- The B A_ ⁇ compounds, RE 2 B A_ ⁇ 4 or RE 4 B a 3 ⁇ 9 (RE is one or more of rare earth elements) is preferably a selective child is.
- the crystal of the RE-Ba-Cu-O-based oxide superconductor grows. This is a feature of the present invention.
- the RE-Ba-O compound and / or the Ba-Cu-O-based liquid phase material may be added to the second phase (RE211) and Z or RE42.2. to stabilize the fine dispersion effects of, it may be contained a P t and Roh or C E_ ⁇ 2 2 wt% or less.
- the mechanical properties of RE_B a—C u—0 oxide superconductors are improved. Therefore, the RE — B a —O-based compound and Z or B a — C u — ⁇ -based liquid phase raw material may contain 30% by mass or less of silver (A g) as a dispersed phase.
- Raw material powder of rare earth elements consisting of rare earth oxides and B A_ ⁇ 2 molar ratio of B a is 2: 1 (or 4: 3) were mixed with ⁇ to become a mixed powder of this, for example, in air, after heat treatment for 24 hours at 9 0 0 ⁇ 1 1 0 0 ° C, by mixing ground again, to produce a RE 2 B A_ ⁇ 4 or RE 4 B a 3 ⁇ 9 compound.
- B A_ ⁇ 2 and C raw material powder consisting of U_ ⁇ a B a: C u of the molar ratio of 1 5:.. 3 were weighed and mixed so as to 4, the mixed powder, for example, air Then, after heat-treating at 95 ° C. for 24 hours, grinding and mixing again to prepare a Ba—Cu—O liquid phase component raw material.
- System liquid phase component raw material has an average composition of REB a 2 C u 3 0 7 _ d (RE 1 2 3) + (1 0 to 50 mol% ) RE 2 B a C u O 5 (RE 2 1 1) + (0-: L 0 mol%) B a 0 2 is mixed and uniaxial molding and CIP molding are used to form the precursor bulk molding. Make it.
- the RE — B a —O-based compound is molded and then the B a — C u — O-based liquid phase component raw material is installed.
- — B a —O-based compounds can be installed. It is also possible to disperse the B a—C u —O system liquid phase raw material in an organic solvent and apply it to the RE—B a —O system compound skeleton material. It does not limit the supply method of RE—B a—O compounds and B a—C u —O system liquid phase raw materials.
- the shape is not limited to a plate shape or a disk shape, and it is only necessary that the B a—C u— ⁇ system liquid phase component material first dissolves and reacts with the RE—B a ⁇ system compound. It can also be applied to more complex shapes such as thin-film mortars.
- RE-Ba-O compounds when using RE-Ba-O compounds as skeletal materials, it is generally used such as providing many pores in drills, adding granular polymer materials in advance, and then thermally decomposing them. It is also preferable to apply a method for producing a porous material to be a porous material.
- the above molded body is heated in an inert gas or a mixed gas of inert gas and oxygen, and Ba-Cu-O system liquid phase raw material at about 10:00 to 1100 ° C. Is dissolved and reacted with RE—B a —O compound. At this time, according to the following reaction formula, R E 2 1 1 (needle crystals) and a liquid phase are formed.
- the former R E 2 1 1 phase is mainly spherical, and the latter R E 2 1 1 phase is acicular, and both R E 2 1 1 phases coexist in the superconducting crystal. As a result, there is a limit to improving the performance of superconducting bulk materials.
- the solid phase fraction is higher when RE—B a—O system compounds are used. There is an advantage that the shape change is small.
- the raw powder consisting of G d 2 0 3 and B a 0 2 has a molar ratio of G d: B a 2: Weighed and mixed so as to be 1. After this powder was molded, it was heat-treated in air at 95 ° C. for 24 hours, and then pulverized and mixed again to obtain G d 2 B a ⁇ 4 powders were made.
- the raw material consists of B A_ ⁇ 2, and C U_ ⁇ "Powder B a: C molar ratio of u is 1.5: 3. weighed so as to 4 mixture 'was molded, this, in the air Then, after heat treatment for 24 hours at 85 ° C., pulverized and mixed again to synthesize a Ba—Cu—O-based liquid phase component raw material.
- G d 2 B a 0 4 powder and B a—C u— 0 system liquid phase component raw material have a molar ratio of G d: B a: C u in the average composition of 1.8: 2.4: 3.4 Weighed and mixed so that a 60 mm diameter mold was used, and uniaxial molding and CIP molding were performed to form a thickness of about 20 mm, followed by melt growth in an electric furnace. . At this time, 0.5% by mass of platinum and 20% by mass of silver were added.
- the temperature was raised to 10 50 ° C in an argon stream, replaced with 1% oxygen-argon gas, and after 30 minutes, the temperature was lowered to 10 20 ° C and the top of the sample
- the N d 1 2 3 seed crystal was placed on the substrate, it was cooled to 98 ° C., gradually cooled to 96 ° C. at a cooling rate of 0.5 ° C./hour, and then cooled to room temperature.
- a bulk body was obtained by cooling at ° C / hour.
- the obtained sample was annealed at 400 ° C. for 30 hours in an oxygen stream to make a superconductor. From observation of the fracture surface of the obtained sample, it was confirmed that fine acicular Gd 2 1 1 crystals were uniformly dispersed in the sample.
- Figure 1 shows the structure of the polished surface.
- the superconducting transition temperature was 94.5 K, 7 7 ⁇ ⁇ ⁇
- the critical current density at zero magnetic field was about 800 OA / cm 2 , as measured by magnetization using S QU ID.
- the obtained sample was annealed at 400 ° C. for 30 hours in an oxygen stream to make a superconductor.
- the superconducting transition temperature was 93.5 K, 7 7 ⁇ , and the critical current density at zero magnetic field was about 400 OA / cm 2 .
- Figure 2 shows the temperature dependence of the magnetic susceptibility
- Figure 3 shows the magnetic field dependence of the critical current density
- H o 2 O 3 and B A_ ⁇ a raw material powder consisting of 2 H o: the molar ratio of B a is 4: ⁇ to be 3 were mixed, after molding the mixed powder in air, 9 5 0 ° after heat treatment for 24 hours in C, and thus to be mixed again pulverized to prepare a H o 4 B a 3 ⁇ 9 powder.
- the raw material powder consisting of B A_ ⁇ 2 and C u O B a: C u molar ratio of 1.5: 3. mixed and molded by ⁇ to be 4, this in the air , Heat treatment at 85 ° C for 24 hours, and then grind and mix again.
- a B a—Cu—O-based liquid phase component raw material was synthesized.
- H 4 B a 3 9 9 powder was dispersed in an organic solvent in which PVB binder was dissolved in diethylene glycol monoethyl ether acetate, and screen-printed on a surface-ground YSZ sintered substrate.
- the temperature was raised to ° C, held for 20 minutes, then gradually cooled from 100 ° C to 98 ° C at a cooling rate of 1 ° CZ time, and then cooled in the furnace.
- the obtained sample hardly reacted with the Y S Z substrate material.
- the obtained sample was placed in an oxygen stream at 400 ° C for 300 hours.
- the magnetic field at 300 G could be reduced to 30% or less.
- Example 2 Melt growth was performed under 1% oxygen / argon gas, and, as in Example 1, held at 100 ° C. for 30 minutes, then cooled to 10 ° 20 ° C., and N d on the top of the sample 1 2 3 Seed crystals are placed, then cooled to 9800 ° C, slowly cooled to 96 ° C at a cooling rate of 0.5 ° C / hour, and then cooled to room temperature 1 0 0 Crystal growth was performed by cooling at ° C / hour.
- the crystals obtained were polycrystalline. Also, annealing is performed for 30 hours at 400 ° C in an oxygen stream to achieve superconductivity.
- the superconducting transition temperature was 92.5 K near the surface, but it was about 80 K at the center, and the transition curve was also broad.
- crystal growth can be performed at a low temperature and in a short time, characteristics can be improved by reducing residual oxygen and reaction with the substrate material, and fine and uniform dispersion of the superconducting phase is possible.
- a large and high performance superconducting bulk material can be produced.
- the present invention can produce RE-Ba-Cu-O-based oxide superconductors used in various applications such as superconducting bearings, superconducting magnetic transfer devices, superconducting permanent magnets, and magnetic shields. It promotes industrial applications of superconductors and has great industrial applicability.
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Abstract
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AT05762065T ATE545720T1 (de) | 2004-07-26 | 2005-07-12 | Verfahren zur herstellung eines re-ba-cu-o supraleiters |
US10/580,368 US20070128735A1 (en) | 2004-07-26 | 2005-07-12 | Method of fabrication of re-ba-cu-o-based oxide superconductor |
EP05762065A EP1770190B1 (en) | 2004-07-26 | 2005-07-12 | METHOD OF FABRICATING RE-Ba-Cu-O SUPERCONDUCTOR |
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JP2004217594A JP4794145B2 (ja) | 2004-07-26 | 2004-07-26 | RE−Ba−Cu−O酸化物超電導体の作製方法 |
JP2004-217594 | 2004-07-26 |
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EP (1) | EP1770190B1 (ja) |
JP (1) | JP4794145B2 (ja) |
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US7964532B2 (en) * | 2005-03-31 | 2011-06-21 | International Superconductivity Technology Center, The Juridical Foundation | RE123-based oxide superconductor and method of production of same |
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CN101665981B (zh) * | 2009-09-25 | 2012-01-11 | 陕西师范大学 | 单畴钆钡铜氧超导块材的制备方法 |
CN101665980B (zh) * | 2009-09-25 | 2012-01-11 | 陕西师范大学 | 用熔渗法制备单畴钆钡铜氧超导块材的方法 |
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JP2004107178A (ja) * | 2002-09-20 | 2004-04-08 | Aisin Seiki Co Ltd | 酸化物超電導体、その製造方法およびその熱処理炉 |
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US4857504A (en) * | 1987-08-25 | 1989-08-15 | University Of Arkansas | Melt-produced high temperature rare earth barium copper oxide superconductor and processes for making same |
DE59002238D1 (de) * | 1989-03-15 | 1993-09-16 | Asea Brown Boveri | Verfahren zur herstellung einer kristallorientierten oberflaechenschicht aus einem keramischen hochtemperatur-supraleiter. |
US5300483A (en) * | 1992-01-16 | 1994-04-05 | Sinha Shome N | Process for preparing shaped superconductor materials via nonequilibrium precursors |
JP3725197B2 (ja) * | 1995-03-24 | 2005-12-07 | 石川島播磨重工業株式会社 | 超電導酸化物結晶の製造方法 |
JP2003020225A (ja) * | 2001-07-06 | 2003-01-24 | Internatl Superconductivity Technology Center | 酸化物超電導体の製造方法及び酸化物超電導体 |
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2004
- 2004-07-26 JP JP2004217594A patent/JP4794145B2/ja not_active Expired - Fee Related
-
2005
- 2005-07-12 WO PCT/JP2005/013213 patent/WO2006011389A1/ja active Application Filing
- 2005-07-12 EP EP05762065A patent/EP1770190B1/en not_active Not-in-force
- 2005-07-12 CN CNB2005800249691A patent/CN100538918C/zh not_active Expired - Fee Related
- 2005-07-12 AT AT05762065T patent/ATE545720T1/de active
- 2005-07-12 US US10/580,368 patent/US20070128735A1/en not_active Abandoned
Patent Citations (3)
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JPH09255334A (ja) * | 1996-03-22 | 1997-09-30 | International Superconductivity Technology Center | バルク酸化物超電導体の作製方法 |
JPH1121126A (ja) * | 1997-07-04 | 1999-01-26 | Sumitomo Electric Ind Ltd | 酸化物超電導バルクの製造方法 |
JP2004107178A (ja) * | 2002-09-20 | 2004-04-08 | Aisin Seiki Co Ltd | 酸化物超電導体、その製造方法およびその熱処理炉 |
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J.P.SINGH ET AL., J. APPL. PHYS., vol. 66, no. 7, 1989, pages 3154 |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US7964532B2 (en) * | 2005-03-31 | 2011-06-21 | International Superconductivity Technology Center, The Juridical Foundation | RE123-based oxide superconductor and method of production of same |
Also Published As
Publication number | Publication date |
---|---|
CN100538918C (zh) | 2009-09-09 |
CN1989277A (zh) | 2007-06-27 |
US20070128735A1 (en) | 2007-06-07 |
EP1770190A1 (en) | 2007-04-04 |
EP1770190A4 (en) | 2010-11-24 |
JP4794145B2 (ja) | 2011-10-19 |
JP2006036574A (ja) | 2006-02-09 |
EP1770190B1 (en) | 2012-02-15 |
ATE545720T1 (de) | 2012-03-15 |
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