WO2011030639A1 - Bi2223酸化物超電導体及びその製造方法 - Google Patents
Bi2223酸化物超電導体及びその製造方法 Download PDFInfo
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- WO2011030639A1 WO2011030639A1 PCT/JP2010/063242 JP2010063242W WO2011030639A1 WO 2011030639 A1 WO2011030639 A1 WO 2011030639A1 JP 2010063242 W JP2010063242 W JP 2010063242W WO 2011030639 A1 WO2011030639 A1 WO 2011030639A1
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- the present invention relates to a Bi2223 oxide superconductor and a method for producing the same. More specifically, the present invention has a high critical current density in a low-temperature magnetic field and maintains the high critical current density even in a self-magnetic field at a liquid nitrogen temperature (77 K).
- the present invention relates to a Bi2223 oxide superconductor that can be manufactured and a method for manufacturing the same.
- Bi (bismuth) -based oxide superconductors are known as materials having a high critical current density.
- Bi-based oxide superconductors (Bi, Pb) 2
- Bi2223 oxide superconductor composed of —Sr 2 —Ca 2 —Cu 3 has attracted attention because a wire with a particularly high critical current density can be obtained by high orientation.
- this Bi2223 oxide superconductor has a problem that the critical current density rapidly decreases when a magnetic field is applied in the c-axis direction.
- an attempt is made to improve the critical current density in a magnetic field by performing element substitution with Ln (lanthanoid) such as La.
- Patent Document 1 a Bi2223 oxide superconductor obtained by replacing 10% or more of a rare earth element with a Bi-based oxide is disclosed, and by adopting such a configuration, The critical current density in a magnetic field is improved.
- this Bi2223 oxide superconductor has a new problem of reducing the critical current density in a 77K self-magnetic field.
- Patent Document 2 also discloses a technology of a Bi-based oxide superconductor in which Ln is substituted with an element.
- the Bi-based oxide superconductor targeted by this Patent Document 2 is a Bi2212 oxide superconductor, so that a sufficient critical current density cannot be obtained.
- the present invention provides a Bi2223 oxide superconductor that has a high critical current density in a low-temperature magnetic field and can maintain a high critical current density even in a 77 K self-magnetic field, and a method for manufacturing the same.
- the issue is to provide.
- the present inventor conducted various studies on the Bi2223 oxide superconductor in which Ln is substituted.
- the Bi2223 oxide superconductor substituted with the conventional Ln has a substitution amount as large as 10% or more, and thus tends to cause heterogeneous aggregation, which reduces the critical current density in the 77K self-magnetic field. I found out.
- the first invention of the present application is a Bi2223 oxide superconductor made of Bi, Pb, Sr, Ln, Ca, Cu, O, and the Ln is La, Ce, Pr, Nd, Pm, Sm, Eu. Bi2223 oxide characterized in that it is at least one selected from Gd, Tb, Dy, Ho, Er, Tm, Yb, and Lu, and the composition ratio of Sr and Ln is the following composition ratio: It is a superconductor.
- Sr: Ln (1-x): x (where 0.002 ⁇ x ⁇ 0.015)
- the substitution amount of Ln is smaller than the conventional amount, it is possible to suppress the aggregation of heterogeneous phases. As a result, it is possible to provide a Bi2223 oxide superconductor having a high critical current density in a low temperature magnetic field and capable of maintaining the high critical current density even in a 77K self magnetic field.
- the present inventor has further studied diligently, and as a result, as a method for producing an Ln-substituted Bi2223 oxide superconductor, a step of ionizing a material containing an element constituting the Bi2223 oxide superconductor in a solution; By injecting the solution into a high-temperature atmosphere to remove the solvent and performing a thermal decomposition reaction, the production method including the step of producing the powder containing the atoms constituting the oxide superconductor is used to completely eliminate the aggregation of the different phases.
- the present inventors have found that a Bi2223 oxide superconductor that has a high critical current density in a low temperature magnetic field and can maintain a high critical current density even in a 77 K self magnetic field can be provided.
- each element can be uniformly dispersed without separating and agglomerating, and Ln can be present in the Bi2223 oxide crystal grains produced from the calcined powder.
- Ln existing in the Bi2223 oxide crystal grains can function as a pin in the Bi2223 oxide crystal grains, it has a high critical current density in a low temperature magnetic field, and also has a high critical current even in a 77K self magnetic field. The current density can be maintained.
- the second invention of the present application claims the above invention, It is a manufacturing method of Bi2223 oxide superconductor of Claim 1, Comprising: The process which ionizes the material containing the element which comprises the said Bi2223 oxide superconductor in a solution, and a solvent removal by injecting a solution to a high temperature atmosphere And a step of producing a powder containing atoms constituting the oxide superconductor by performing a thermal decomposition reaction with the Bi2223 oxide superconductor.
- Bi2223 oxide superconductor having a high critical current density in a low temperature magnetic field and capable of maintaining the high critical current density even in a 77K self magnetic field, and a method for manufacturing the same. it can.
- FIG. 1 is a diagram schematically showing the configuration of an oxide superconductor precursor powder manufacturing apparatus according to the present invention.
- FIG. 2 is a diagram showing critical current densities in a self-magnetic field and a low-temperature magnetic field of a Bi2223 oxide superconducting wire and a standard composition wire according to the present invention.
- FIG. 3 is a diagram showing the relationship between the La addition concentration and the rate of increase of the critical current value in the Bi2223 oxide superconducting wire according to the present invention.
- FIG. 4A is an X-ray diffraction diagram of an oxide superconductor precursor powder (La-added composition) according to the present invention.
- FIG. 4B is an X-ray diffraction pattern of an oxide superconductor precursor powder (without addition of La) having a standard composition.
- a material containing the elements constituting the Bi2223 oxide superconductor is prepared. That is, it contains an element contained in a lanthanoid (Ln) such as lanthanum (La) that substitutes a part of bismuth (Bi), lead (Pb), strontium (Sr), calcium (Ca), copper (Cu), and Sr.
- Ln lanthanoid
- La bismuth
- Pb lead
- Ca calcium
- Cu copper
- Sr calcium
- Sr calcium
- Sr calcium
- Cu copper
- Sr calcium
- Sr calcium
- Bi 2 O 3 , PbO, SrCO 3 , CaCO 3 , CuO, and La 2 O 3 powders may be used.
- Bi, Pb, Sr, Ca, Cu, La solid metal may be used.
- nitric acid is preferable because each material can be completely dissolved without forming a passive state of the material, and the carbon component can theoretically be zero.
- the solvent is not limited to nitric acid, and may be other inorganic acids such as sulfuric acid and hydrochloric acid, or organic acids such as oxalic acid and acetic acid. Furthermore, as long as it is a component which can dissolve not only an acid but a material, an alkaline solution may be sufficient.
- the material is dissolved in, for example, nitric acid and ionized.
- the temperature of the solution at this time is not particularly limited, and may be any temperature that can sufficiently dissolve an element serving as a material such as Bi. Furthermore, in order to obtain sufficient solubility, it is preferable to provide a stirrer and stir.
- each element (Bi, Pb, Sr, Ca, Cu, Ln) constituting the oxide superconductor is finely mixed at the ion level.
- the solution 11 is injected from the injection port 21 together with the atomizing gas.
- the injection of the solution 11 and the atomizing gas is indicated by an arrow A.
- the spray 12 is formed.
- the carrier gas is introduced from the injection port 21 in the direction indicated by the arrow B.
- the spray 12 is transferred to the electric furnace 13 by the transfer gas. And in the electric furnace 13, the solvent of the solution 11 contained in the spray 12 is heated and evaporated.
- the solution is sprayed onto the high-temperature atmosphere 14 constituted by the atomizing gas and the carrier gas, and the solvent is removed.
- the raw material powder 1a containing the atoms constituting the oxide superconductor is obtained.
- the atmosphere 15 at the outlet of the electric furnace 13 contains the removed solvent component.
- the temperature of the electric furnace 13 is not particularly limited, the temperature of the electric furnace 13 can be set to 700 ° C. or higher and 850 ° C. or lower, for example, when nitrate is thermally decomposed in the electric furnace 13.
- the length of the region having a temperature of 700 ° C. or higher and 850 ° C. or lower can be set to, for example, 300 mm.
- the powder is cooled in an atmosphere 16 introduced with a cooling gas.
- the cooling gas is introduced from the cooling gas inlet 22 in the direction indicated by the arrow C.
- This cooling gas is mixed with the atmosphere 15 to form the atmosphere 16.
- the raw material powder 1 a is transported to the powder collector 17 by the transporting gas and stored in a container 17 a disposed at the bottom of the powder collector 17. Thereby, the raw material powder 1 is obtained.
- the carrier gas passes through the filter 18 and is discharged from the discharge port 23.
- the atomizing gas in this embodiment dry air, nitrogen, or the like can be used. Moreover, dry air etc. can be used as gas for conveyance.
- the atomizing gas and the conveying gas may be different gases or the same kind of gas. Further, the flow rate ratio between the atomizing gas and the conveying gas can be changed as appropriate.
- the cooling gas a gas capable of reducing the concentrations of carbon dioxide, nitrogen, and water vapor as compared with the atmosphere 15 and a gas having a temperature lower than that of the atmosphere 15 is used.
- a high-temperature furnace is a furnace that can be heated to a temperature necessary for completely pyrolyzing a salt such as nitrate, specifically, a decomposition temperature of all nitrates contained in a solid powder, such as 600 ° C. or higher and 850 ° C. or lower.
- a furnace that can be heated as described above, for example, an electric furnace including a heat source around it can be used.
- the inside of the high-temperature furnace is preferably maintained in an atmosphere in which an oxidation reaction is likely to occur. For example, it is preferable to maintain a low oxygen atmosphere (for example, an oxygen concentration of more than 0% by volume and 21% by volume or less).
- a precursor powder comprising a complex oxide powder containing each element in a predetermined ratio and having each element uniformly dispersed without separation and aggregation of the heterogeneous phase of the oxide of each element, particularly the Ln oxide. Can be produced.
- Bi, Pb, Sr, Ca, Cu and Ln constituting the Bi2223 oxide superconductor are finely mixed in an ion level of each element in a solution. Then, the solvent is removed from the solution to produce a solid powder mixed at the ionic level. By processing the generated solid powder in a high-temperature furnace, a precursor powder is generated instantly. For this reason, the precursor powder of Bi2223 oxide superconductor in which each element is uniformly dispersed can be produced without separation and aggregation of each element.
- a Bi2223 oxide superconducting wire is prepared using La as Ln, nitrate aqueous solution of each element constituting the oxide superconductor as a material, and precursor powder prepared by spray heat treatment after acid dissolution. This is an example.
- Table 1 The measurement results are shown in Table 1, FIG. 2 and FIG.
- the Bi2223 oxide superconductor wire obtained by the present invention has a higher up rate than the standard composition wire, that is, the critical current density Jc (20K, ⁇ 4T) in a low temperature magnetic field. You can see that it ’s big.
- the added La is uniformly dispersed at the ion level, so that La present in the Bi2223 phase crystal grains exhibits a pinning effect, and the additive concentration of La It is considered that the critical current density in a low-temperature magnetic field could be improved in this way, despite the low concentration.
- the critical current density Jc (77K, sf) in the self magnetic field of the Bi2223 oxide superconductor wire obtained by the present invention is the Jc (77K, s.f) of the standard composition wire. It can be seen that this is equivalent to f). That is, it can be seen that a decrease in critical current density in the self magnetic field due to La addition is suppressed.
- FIGS. 4A and 4B The diffraction pattern of the precursor powder prepared according to the present invention shown in FIG. 4A is substantially the same as the diffraction angle and diffraction intensity of the diffraction peak of the standard composition (without addition of La) shown in FIG. 4B.
- a diffraction peak of La different phase was not observed, and it was confirmed that no La different phase was generated.
- the i2223 oxide superconductor of the present invention is suitably used in a superconducting application field that requires a high critical current density in a low temperature magnetic field and needs to maintain a high critical current density even in a 77 K self-magnetic field. it can.
- the manufacturing method of the Bi2223 oxide superconductor of this invention can be utilized suitably for manufacture of the superconducting wire which has the said characteristic.
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Abstract
Description
Sr:Ln=(1-x):x (但し、0.002≦x≦0.015)
請求項1に記載のBi2223酸化物超電導体の製造方法であって、前記Bi2223酸化物超電導体を構成する元素を含む材料を溶液中でイオン化する工程と、高温雰囲気に溶液を噴射して溶媒除去と熱分解反応を行うことにより、酸化物超電導体を構成する原子を含む粉末を製造する工程とを備えることを特徴とするBi2223酸化物超電導体の製造方法である。
はじめに、前駆体粉末の製造方法について説明する。
(1)材料準備
まず、Bi2223酸化物超電導体を構成する元素を含む材料を準備する。即ち、ビスマス(Bi)、鉛(Pb)、ストロンチウム(Sr)、カルシウム(Ca)、銅(Cu)およびSrの一部を置換するランタン(La)等のランタノイド(Ln)に含まれる元素を含む材料であり、具体的にはたとえばBi2O3、PbO、SrCO3、CaCO3、CuO、La2O3の各材料粉末であってもよい。また、Bi、Pb、Sr、Ca、Cu、Laの固体金属でもよい。また、Bi(NO3)3、Pb(NO3)2、Sr(NO3)2、Ca(NO3)2、Cu(NO3)2、La(NO3)3、またはこれらの水和物であってもよい。
次に、準備した材料を溶解し、溶液を作成する。溶媒としては、材料の不動態を形成せず各材料を完全に溶解することができ、理論上炭素成分をゼロにできる、硝酸が好ましい。ただし溶媒は硝酸に限られるものではなく、硫酸、塩酸などの他の無機酸でもよいし、シュウ酸、酢酸などの有機酸であってもよい。さらに、酸だけでなく、材料を溶解させることが可能な成分であれば、アルカリ溶液であってもよい。
次に、図1に示す前駆体粉末製造装置を用いて、上記溶液より前駆体粉末を作製する。具体的には、まず、溶液11を噴霧用気体と共に噴射口21から噴射する。溶液11および噴霧用気体の噴射を矢印Aで示す。これによって噴霧12が形成される。一方、噴射口21から矢印Bで示す方向に搬送用気体を導入する。この搬送用気体によって噴霧12は電気炉13へ搬送される。そして、電気炉13内において、噴霧12に含まれる溶液11の溶媒は加熱されて蒸発する。
次に、固体粉末の熱処理を行なう。具体的には、固体粉末を高温炉内に飛散させることによって酸化させ、Bi2223酸化物超電導体の前駆体粉末(仮焼粉末)を作製する。
(1)材料
(Bi、Pb)、(Sr1-x、Lax)、Ca、Cuをモル比で2:2:2:3の比率で含有し、xが異なる5種類の材料を準備した。具体的には、x=0.002、0.005、0.0075、0.01、0.01、0.015の材料を準備し、それぞれ順に実施例1、実施例2、実施例3、実施例4、実施例5、実施例6とした。なお、実施例4と実施例5は同じ組成比であるが、以降の超電導線材の作製工程において相違があるため、別の実施例とした。
上記6種類の材料をそれぞれ硝酸に溶解して、硝酸塩水溶液を調整した。この6種類の硝酸塩水溶液をそれぞれ噴霧して、固体粉末を得た。
次いで、温度800℃、酸素分圧0.008MPaの雰囲気で10時間の熱処理を行い、前駆体粉末を得た。
(1)単芯線の作製
上記のようにして得た6種類の前駆体粉末を、それぞれ銀パイプに充填し、真空中において600℃の温度で10時間の熱処理を行なってガスを抜いた。そして、金属管の端末をロウ付けすることで前駆体粉末を真空封入した後、両端を封入したまま線引き加工して単芯線を作製した。
次に、作製した6種類の単芯線をそれぞれ121本束ねて銀パイプに挿入し、再度真空中において600℃の温度で10時間の熱処理を行なってガスを抜いた。そして、銀パイプの端末をロウ付けすることで原料粉末を真空封入して多芯線を作製した。続いて、この多芯線の両端をロウ付けしたまま伸線加工および圧延加工を行ない、幅4mm、厚さ0.2mmのテープ線を作製した。
次に、作製した6種類のテープ線を820~830℃、酸素分圧0.008MPaの雰囲気で30時間の熱処理を行なった。次に、中間圧延を行なった後で、さらに810~820℃、酸素分圧0.008MPaの雰囲気で50時間の熱処理を行ない、Bi2223酸化物超電導体線材を製造した。
(1)測定方法
作製したBi2223酸化物超電導体線材の臨界電流密度(kA/cm2)を、77Kの自己磁場中、及び20Kでテープに垂直(c軸方向に垂直)に4Tの磁場を印加する2種類の条件の下で測定し、それぞれの測定値をJc(77K,s.f)、即ち自己磁場中での臨界電流密度とJc(20K,⊥4T)、即ち低温磁場中での臨界電流密度で表記した。また、それぞれの測定値に基づいてJc(20K,⊥4T)/Jc(77K,s.f)を算定し、up率とした。
測定結果を表1、図2、図3に示す。また、Laを添加していない、即ちx=0のBi2223の複数種類の標準組成線材についての測定データを併せて表1、図2、図3に示す。なお、図3では臨界電流Icで表記した。
11 溶液
12 噴霧
13 電気炉
14,15,16 雰囲気
17 粉末回収器
17a 容器
18 フィルタ
21 噴射口
22 冷却用気体導入口
23 排出口
Claims (2)
- Bi、Pb、Sr、Ln、Ca、Cu、OからなるBi2223酸化物超電導体であって、
前記Lnは、La、Ce、Pr、Nd、Pm、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb、Luから選ばれた1種以上であり、
前記Srと前記Lnとの組成比が以下の組成比であることを特徴とするBi2223酸化物超電導体。
Sr:Ln=(1-x):x (但し、0.002≦x≦0.015) - 請求項1に記載のBi2223酸化物超電導体の製造方法であって、
前記Bi2223酸化物超電導体を構成する元素を含む材料を溶液中でイオン化する工程と、
高温雰囲気に溶液を噴射して溶媒除去と熱分解反応を行うことにより、酸化物超電導体を構成する原子を含む粉末を製造する工程と
を備えることを特徴とするBi2223酸化物超電導体の製造方法。
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DE112010003576T DE112010003576T8 (de) | 2009-09-08 | 2010-08-05 | BI2223-Oxidsupraleiter und Verfahren zu seiner Herstellung |
US13/394,617 US20120172230A1 (en) | 2009-09-08 | 2010-08-05 | Bi2223 OXIDE SUPERCONDUCTOR AND METHOD FOR PRODUCING SAME |
CN2010800398184A CN102482112A (zh) | 2009-09-08 | 2010-08-05 | Bi2223氧化物超导体及其制造方法 |
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CN102701728A (zh) * | 2012-05-15 | 2012-10-03 | 西南交通大学 | 一种高温超导涂层导体缓冲层Gd1-xPbxBiO3及其制备方法 |
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US8637433B2 (en) * | 2010-10-04 | 2014-01-28 | Florida State University Technology Transfer Office | Method for making a composite high-temperature superconductor |
CN104129985B (zh) * | 2014-07-08 | 2016-04-06 | 西南交通大学 | 表面具有纳米颗粒析出相的高温超导涂层导体Eu0.6Sr0.4BiO3缓冲层及其制备方法 |
CN105575545A (zh) * | 2015-12-29 | 2016-05-11 | 北京英纳超导技术有限公司 | 一种Bi2223氧化物薄膜及其工业化制备方法 |
CN107935041A (zh) * | 2017-12-14 | 2018-04-20 | 西北有色金属研究院 | 一种铋系超导前驱粉末的制备方法 |
CN109942290A (zh) * | 2019-03-12 | 2019-06-28 | 西北工业大学 | 拓扑发光体异质相掺杂的Bi(Pb)-Sr-Ca-Cu-O系超构超导体及其制备方法 |
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2010
- 2010-08-05 DE DE112010003576T patent/DE112010003576T8/de not_active Withdrawn - After Issue
- 2010-08-05 US US13/394,617 patent/US20120172230A1/en not_active Abandoned
- 2010-08-05 WO PCT/JP2010/063242 patent/WO2011030639A1/ja active Application Filing
- 2010-08-05 CN CN2010800398184A patent/CN102482112A/zh active Pending
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Cited By (1)
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CN102701728A (zh) * | 2012-05-15 | 2012-10-03 | 西南交通大学 | 一种高温超导涂层导体缓冲层Gd1-xPbxBiO3及其制备方法 |
Also Published As
Publication number | Publication date |
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DE112010003576T8 (de) | 2012-11-08 |
JP2011057484A (ja) | 2011-03-24 |
CN102482112A (zh) | 2012-05-30 |
DE112010003576T5 (de) | 2012-09-06 |
US20120172230A1 (en) | 2012-07-05 |
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