JPS63297213A - Production of oxide superconductor - Google Patents
Production of oxide superconductorInfo
- Publication number
- JPS63297213A JPS63297213A JP62133951A JP13395187A JPS63297213A JP S63297213 A JPS63297213 A JP S63297213A JP 62133951 A JP62133951 A JP 62133951A JP 13395187 A JP13395187 A JP 13395187A JP S63297213 A JPS63297213 A JP S63297213A
- Authority
- JP
- Japan
- Prior art keywords
- oxide superconductor
- oxygen
- fluorine
- producing
- ammonium salt
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000002887 superconductor Substances 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 14
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 8
- 239000011737 fluorine Substances 0.000 claims abstract description 8
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 5
- 229910052788 barium Inorganic materials 0.000 claims abstract description 4
- 229910052727 yttrium Inorganic materials 0.000 claims abstract description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 3
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 3
- 229910052689 Holmium Inorganic materials 0.000 claims abstract description 3
- 229910052765 Lutetium Inorganic materials 0.000 claims abstract description 3
- 229910052779 Neodymium Inorganic materials 0.000 claims abstract description 3
- 229910052775 Thulium Inorganic materials 0.000 claims abstract description 3
- 229910052769 Ytterbium Inorganic materials 0.000 claims abstract description 3
- 229910052746 lanthanum Inorganic materials 0.000 claims abstract description 3
- 229910052706 scandium Inorganic materials 0.000 claims abstract description 3
- 229910052693 Europium Inorganic materials 0.000 claims abstract 2
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract 2
- 229910052772 Samarium Inorganic materials 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 8
- 230000002950 deficient Effects 0.000 claims description 4
- 230000007547 defect Effects 0.000 claims description 3
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N nitrogen Substances N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 abstract description 2
- LDDQLRUQCUTJBB-UHFFFAOYSA-N ammonium fluoride Chemical compound [NH4+].[F-] LDDQLRUQCUTJBB-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 2
- 229910019975 (NH4)2SiF6 Inorganic materials 0.000 abstract 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract 1
- 238000006467 substitution reaction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 description 4
- 238000010304 firing Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical compound [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 description 1
- 229910001632 barium fluoride Inorganic materials 0.000 description 1
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 150000002222 fluorine compounds Chemical class 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 150000002823 nitrates Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 229910052720 vanadium Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- 229940105963 yttrium fluoride Drugs 0.000 description 1
- RBORBHYCVONNJH-UHFFFAOYSA-K yttrium(iii) fluoride Chemical compound F[Y](F)F RBORBHYCVONNJH-UHFFFAOYSA-K 0.000 description 1
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
- H10N60/80—Constructional details
- H10N60/85—Superconducting active materials
- H10N60/855—Ceramic superconductors
- H10N60/857—Ceramic superconductors comprising copper oxide
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
Description
【発明の詳細な説明】 [発明の目的] (産業上の利用分野) 本発明は酸化物超電導体の製造方法に関する。[Detailed description of the invention] [Purpose of the invention] (Industrial application field) The present invention relates to a method for manufacturing an oxide superconductor.
(従来の技術)
近年、Ba−La−Cu−0系の層状ペロブスカイト型
酸化物が高い臨界温度を有する可能性のあることが発表
されて以来、各所で酸化物超電導体の研究が行なわれて
いる(Z、Phys、B Condensed Mat
te’r 84゜189−193(198B) 。その
中でもY−Ba−Cu−0系に代表される酸素欠陥を有
する欠陥ペロブスカイト型(AB CO型)の酸化物
超電導体は、Tc237−δ
が90に以上と液体窒素以上の′高い温度を示す′ため
非常に有望な材料である(P’hys、Rev、Le−
tt、vor、5’8No、9.p908−910)。(Prior art) In recent years, since it was announced that layered perovskite oxides based on Ba-La-Cu-0 may have a high critical temperature, research on oxide superconductors has been conducted in various places. There is (Z, Phys, B Condensed Mat
te'r 84°189-193 (198B). Among these, defective perovskite type (AB CO type) oxide superconductors with oxygen defects, represented by the Y-Ba-Cu-0 system, exhibit Tc237-δ of 90 or higher, which is higher than liquid nitrogen. ', it is a very promising material (P'hys, Rev, Le-
tt, vor, 5'8No, 9. p908-910).
(発明が解決しようとする間居点)
この様にペロブスカイト型の酸化物類1導□体は前述の
如く非常に有望な材料であるが、より高い臨界温度への
発展が望まれている。(The problem to be solved by the invention) Although the perovskite type oxide type 1 conductor is a very promising material as mentioned above, it is desired to develop it to a higher critical temperature.
本発病はこの様な画題点を解決するためになされたもの
であり、臨界温度の高い酸化物超電導体を得ることを目
的としてなされたものである。The present invention was made to solve this problem, and was made with the aim of obtaining an oxide superconductor with a high critical temperature.
[発明の構成]
(問題点を解決するための手段及び作用)本発明は、L
n元素(LnはY 、 La 、 Sc 、 Nd 、
5I11. Eu 、 Cd 。[Structure of the invention] (Means and effects for solving the problems) The present invention is based on L
n element (Ln is Y, La, Sc, Nd,
5I11. Eu, Cd.
Dy、Ho、Er、Tm、Yb、Luの少なくとも一種
) 、AE元素(Ba、Ca及びSrの少なくとも一種
)及びCuを含有するペロブスカイト構造の酸化物超電
導体の製造方法に於いて、原料として弗化アンモニウム
等の弗素含有のアンモニウム塩を混合し酸素の一部を弗
素で置換することを特徴とする酸化物超電導体の製造方
法である。Dy, Ho, Er, Tm, Yb, Lu), AE element (at least one of Ba, Ca and Sr) and Cu. This method of producing an oxide superconductor is characterized by mixing a fluorine-containing ammonium salt such as ammonium chloride and replacing a portion of oxygen with fluorine.
本発明でいうペロブスカイト型構造の酸化物超電導体は
La−(Ba、!3r、Ca)−Cu−0系の層状ペロ
ブスカイト型酸化物超電導体、Y−Ba−Cu−0系の
酸素欠陥を有する欠陥ペロブスカイト型酸化物超電導体
などの広義のペロブスカイト型構造の酸化物超電導体を
さす。The oxide superconductor having a perovskite structure in the present invention is a layered perovskite oxide superconductor based on La-(Ba,!3r,Ca)-Cu-0, and has oxygen defects based on Y-Ba-Cu-0. Refers to oxide superconductors with a broad perovskite structure, such as defective perovskite oxide superconductors.
本発明に用いる酸化物超電導体は、例えば以下に示す製
造方法により得ることができる。The oxide superconductor used in the present invention can be obtained, for example, by the manufacturing method shown below.
Y 、 Cu 、 Ba等の酸化物超電導体の構成元素
を含をする原料を十分混合する。混合の際にはY2O3
゜Bad、CuO等の酸化物を原料として用いることが
できる。また、これらの酸化物のほかに、焼成後酸化物
に転化する炭酸塩、硝酸塩、水酸化物また弗化イツトリ
ウム、弗化バリウム、弗化鋼等の弗化物等の化合物を用
いてもよい。さらには共沈法等で得たしゅう酸塩等を用
いても良い。Raw materials containing constituent elements of the oxide superconductor, such as Y, Cu, and Ba, are thoroughly mixed. Y2O3 when mixing
Oxides such as Bad and CuO can be used as raw materials. In addition to these oxides, compounds such as carbonates, nitrates, hydroxides, and fluorides such as yttrium fluoride, barium fluoride, and steel fluoride, which are converted into oxides after firing, may be used. Furthermore, oxalate obtained by a coprecipitation method or the like may also be used.
本発明ではこの原料にさらに弗化アンモニウム(NHF
)等を混合する。またNH4Fの代わりにNHBF、(
NH) SIF 、(NH) GcP e等を用
いても良い。In the present invention, ammonium fluoride (NHF) is added to this raw material.
) etc. Also, instead of NH4F, NHBF, (
NH) SIF, (NH) GcP e, etc. may also be used.
前述の原料を混合した後、仮焼・粉砕し所望の形状に成
形した後、930−1000℃程度で焼成する。After mixing the above raw materials, they are calcined and pulverized to form a desired shape, and then fired at about 930-1000°C.
仮焼は必ずしも必要ではない。焼成・仮焼は十分な酸素
が供給できるような酸素含有雰囲気で行なうことが好ま
しい。所望の形状に焼成した後、酸素中で加熱処理する
ことにより超電導特性を向上することができる。この加
熱処理は通常600−%0℃程度である。Calcining is not necessarily necessary. Firing and calcination are preferably carried out in an oxygen-containing atmosphere where sufficient oxygen can be supplied. After firing into a desired shape, the superconducting properties can be improved by heat treatment in oxygen. This heat treatment is usually about 600-%0°C.
この様にして得られた酸化物超電導体はLn 、 AE
。The oxide superconductor obtained in this way is Ln, AE
.
Cuを原子比で実質的にl:2:3の比率で含有する酸
素欠陥δを有するLnBa Cu O(δは2 3
7−δ
通常1以下)の酸素欠陥型ペロブスカイト構造となる。LnBa Cu O (δ is 2 3
7-δ (usually 1 or less), resulting in an oxygen-deficient perovskite structure.
Cu元元素Ba元素の置換元素はそれぞれのサイトに置
換した形で入る。なおF元素はO元素を置換する形で入
る。弗素の置換量は超電導特性を低下しない範囲で適宜
設定でき、るが、実用上は90原子%以下、好ましくば
50原子%以下程度である。また少量の置換量で臨界温
度の上昇の効果を得ることができるが0.01原子%以
上の置換量で顕著である。Substituting elements for the Cu element and the Ba element enter the respective sites in a substituted form. Note that the F element replaces the O element. The amount of fluorine substitution can be appropriately set within a range that does not deteriorate the superconducting properties, but in practice it is about 90 atomic % or less, preferably about 50 atomic % or less. Further, the effect of increasing the critical temperature can be obtained with a small amount of substitution, but it becomes noticeable when the amount of substitution is 0.01 atomic % or more.
ペロブスカイト型酸化物超電導体を構成する元素は、基
本的に化学量論比の組成となるように混合するが、多少
製造条件等との関係等でずれていても構わない。例えば
Y−Ba−Cu−Q系ではYlmolに対しB a 2
l101% Cu 3 molが、標準組成であ
るが、実用上はY1a+olに対し、Ba2±0.6
mol 。The elements constituting the perovskite-type oxide superconductor are basically mixed so as to have a stoichiometric composition, but there may be a slight deviation depending on the manufacturing conditions, etc. For example, in the Y-Ba-Cu-Q system, B a 2 for Ylmol
The standard composition is 101% Cu 3 mol, but in practice Ba2 ± 0.6 for Y1a + ol.
mol.
Cu3±0.21101程度のずれは問題ない。A deviation of approximately Cu3±0.21101 is not a problem.
また上述の粉末焼結に限らず、蒸着法、スパッタリング
法、CVD法などの方法による膜状の酸化物超電導体を
形成することもできる。更に酸化物超電導体ペーストを
用いたスクリーン印刷法、ゾル・ゲル法等を用いての製
造もできる。更に金属管等のシース材を用いての線材化
、溶湯急冷法を用いての線材化等も可能である。In addition to the powder sintering described above, a film-like oxide superconductor can also be formed by a method such as a vapor deposition method, a sputtering method, or a CVD method. Furthermore, it can also be manufactured using a screen printing method using an oxide superconductor paste, a sol-gel method, or the like. Furthermore, it is also possible to make a wire using a sheath material such as a metal tube, or to make a wire using a molten metal quenching method.
なお本発明に用いる酸化物超電導体ではBa元素をSr
、Caの少なくとも一種で置換することができる。この
様な置換量よっても臨界電流密度を向上することかで・
きる。置換は少量でその効果を発揮するが、0.01m
ol、%以上の添加でその効果が顕著となる。置換量は
超電導特性を低下させない程度の範囲で適宜設定可能で
あるが1、あまり多量の置換は超電導特性を低下してし
まうため80mo1%以下、さらに実用上は一20mo
1%以下程度の添加含有量が好ましい。さらにCuの一
部をTi、V、Cr、Mn、Fa、Co、Ni。In addition, in the oxide superconductor used in the present invention, Ba element is replaced with Sr.
, Ca. Is it possible to improve the critical current density by such a substitution amount?
Wear. Replacement is effective in small amounts, but 0.01 m
The effect becomes remarkable when it is added in an amount of 1% or more. The amount of substitution can be set as appropriate within a range that does not reduce the superconducting properties1, but too much substitution will reduce the superconducting properties, so it should be less than 80 mo1%, and more practically -20 mo.
The added content is preferably about 1% or less. Furthermore, a part of Cu is Ti, V, Cr, Mn, Fa, Co, and Ni.
Zn等で置換して臨界電流密度を向上することもできる
。置換は少量でその効果を発揮するが、0.01so1
%以上の添加でその効果が顕著となる。置換量は超電導
特性を低下させない程度の範囲で適宜設定可能であるが
、あまり多量の置換は超電導特性を低下してしまうため
80io1%以下、さらに実用上は20mo1%以下程
度の添加量を量が好ましい。The critical current density can also be improved by substituting with Zn or the like. Substitution exhibits its effect in small amounts, but 0.01so1
The effect becomes remarkable when the addition amount is more than %. The amount of substitution can be set as appropriate within a range that does not reduce the superconducting properties, but too much substitution will reduce the superconducting properties, so the addition amount should be 80io1% or less, and more practically 20mo1% or less. preferable.
(実施例) 以下に本発明の詳細な説明する。(Example) The present invention will be explained in detail below.
実施例−1
原子比でY:Ba:Cu=1 : 2 : 3となるよ
うに、Y O、BaC0、CuOを秤量し、さらに弗
化アンモニウムを前記原料全体に対し30重量%添加し
た原料を十分混合した後900℃で仮焼した後、粉砕し
た。この混合原料を%0℃、12H1酸素中の条件で焼
成した。次いで860℃、 IOHの条件で加熱処理を
施した。Example-1 A raw material was prepared in which Y2O, BaC0, and CuO were weighed so that the atomic ratio was Y:Ba:Cu=1:2:3, and 30% by weight of ammonium fluoride was added to the total raw material. After thorough mixing, the mixture was calcined at 900°C and then pulverized. This mixed raw material was fired under conditions of 0° C. and 12H1 oxygen. Next, heat treatment was performed under the conditions of 860°C and IOH.
得られた酸化物超電導体の超電導特性を調べたところ、
臨界温度Tcは一50℃と優れたものであった。When we investigated the superconducting properties of the obtained oxide superconductor, we found that
The critical temperature Tc was excellent at -50°C.
実施例−2
YをYbに変え、実施例−1と同様にして酸化物超電導
体を製造した。Example 2 An oxide superconductor was produced in the same manner as in Example 1 except that Y was replaced with Yb.
この酸化物超電導体の超電導特性を調べたところ、Tc
−−50℃と非常に優れたものであった。When we investigated the superconducting properties of this oxide superconductor, we found that Tc
--50°C, which was very excellent.
実施例−3
弗化アンモニウムの添加量を40%に変え、実施例−1
と同様にして酸化物超電導体を製造した。Example-3 The amount of ammonium fluoride added was changed to 40%, and Example-1
An oxide superconductor was produced in the same manner.
この酸化物超電導体の超電導特性を調べたところ、Tc
−−60℃と非常に優れたものであった。When we investigated the superconducting properties of this oxide superconductor, we found that Tc
--60°C, which was very excellent.
比較例−1
弗化アンモニウムを添加することなく、実施例−1と同
様にして酸化物超電導体を製造した。Comparative Example-1 An oxide superconductor was produced in the same manner as in Example-1 without adding ammonium fluoride.
得られた酸化物超電導体の超電導特性を調べたところ、
臨界温度はTc−−180℃と低いものであった。When we investigated the superconducting properties of the obtained oxide superconductor, we found that
The critical temperature was as low as Tc--180°C.
[発明の効果]
以上説明したように本発明によれば臨界温度の高い酸化
物超電導体を得ることができる。従って工業上寄与する
こと大である。[Effects of the Invention] As explained above, according to the present invention, an oxide superconductor with a high critical temperature can be obtained. Therefore, it will make a great contribution to industry.
Claims (4)
Eu、Gd、Dy、Ho、Er、Tm、Yb、Luの少
なくとも一種)、AE元素(Ba、Ca及びSrの少な
くとも一種)及びCuを含有するペロブスカイト構造の
酸化物超電導体の製造方法に於いて、原料として弗素含
有のアンモニウム塩を混合し酸素の一部を弗素で置換す
ることを特徴とする酸化物超電導体の製造方法。(1) Ln element (Ln is Y, La, Sc, Nd, Sm,
In a method for producing an oxide superconductor with a perovskite structure containing at least one of Eu, Gd, Dy, Ho, Er, Tm, Yb, and Lu), an AE element (at least one of Ba, Ca, and Sr), and Cu. A method for producing an oxide superconductor, which comprises mixing a fluorine-containing ammonium salt as a raw material and replacing a portion of oxygen with fluorine.
質的に1:2:3の比率で含有することを特徴とする特
許請求の範囲第1項記載の酸化物超電導体の製造方法。(2) Production of an oxide superconductor according to claim 1, wherein the oxide superconductor contains Ln, AE, and Cu in an atomic ratio of substantially 1:2:3. Method.
−_δ(δは酸素欠陥を表わす)で表わされる酸素欠陥
型ペロブスカイト構造を有することを特徴とする特許請
求の範囲第1項記載の酸化物超電導体の製造方法。(3) The oxide superconductor is LnBa_2Cu_3O_7_
2. The method for producing an oxide superconductor according to claim 1, wherein the oxide superconductor has an oxygen-deficient perovskite structure represented by -_δ (δ represents an oxygen defect).
を特徴とする特許請求の範囲第1項記載の酸化物超電導
体の製造方法。(4) The method for producing an oxide superconductor according to claim 1, wherein the amount of fluorine substituted is 90 atomic % or less of oxygen.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62133951A JPS63297213A (en) | 1987-05-29 | 1987-05-29 | Production of oxide superconductor |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
JP62133951A JPS63297213A (en) | 1987-05-29 | 1987-05-29 | Production of oxide superconductor |
Publications (1)
Publication Number | Publication Date |
---|---|
JPS63297213A true JPS63297213A (en) | 1988-12-05 |
Family
ID=15116886
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
JP62133951A Pending JPS63297213A (en) | 1987-05-29 | 1987-05-29 | Production of oxide superconductor |
Country Status (1)
Country | Link |
---|---|
JP (1) | JPS63297213A (en) |
-
1987
- 1987-05-29 JP JP62133951A patent/JPS63297213A/en active Pending
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