JPH01131098A - Production of oxide superconductor crystal - Google Patents
Production of oxide superconductor crystalInfo
- Publication number
- JPH01131098A JPH01131098A JP62288117A JP28811787A JPH01131098A JP H01131098 A JPH01131098 A JP H01131098A JP 62288117 A JP62288117 A JP 62288117A JP 28811787 A JP28811787 A JP 28811787A JP H01131098 A JPH01131098 A JP H01131098A
- Authority
- JP
- Japan
- Prior art keywords
- oxide superconductor
- crystal
- oxide
- solution
- pulling
- 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
- 239000013078 crystal Substances 0.000 title claims abstract description 40
- 239000002887 superconductor Substances 0.000 title claims abstract description 24
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 230000004907 flux Effects 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 8
- XHCLAFWTIXFWPH-UHFFFAOYSA-N [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[V+5].[V+5] XHCLAFWTIXFWPH-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910001935 vanadium oxide Inorganic materials 0.000 claims abstract description 5
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910001882 dioxygen Inorganic materials 0.000 claims abstract description 4
- 239000007791 liquid phase Substances 0.000 claims abstract description 4
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 2
- 229910052691 Erbium Inorganic materials 0.000 claims description 2
- 229910052693 Europium Inorganic materials 0.000 claims description 2
- 229910052689 Holmium Inorganic materials 0.000 claims description 2
- 229910052765 Lutetium Inorganic materials 0.000 claims description 2
- 229910052775 Thulium Inorganic materials 0.000 claims description 2
- 229910052769 Ytterbium Inorganic materials 0.000 claims 2
- 229910052727 yttrium Inorganic materials 0.000 claims 2
- 230000007704 transition Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- -1 V2O5 Chemical compound 0.000 abstract 1
- 229910009203 Y-Ba-Cu-O Inorganic materials 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 8
- 239000000463 material Substances 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000010587 phase diagram Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram 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
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Landscapes
- Crystals, And After-Treatments Of Crystals (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、多元系酸化物超電導体結晶の製造方法に関す
る。DETAILED DESCRIPTION OF THE INVENTION [Object of the Invention] (Field of Industrial Application) The present invention relates to a method for producing a multi-component oxide superconductor crystal.
（従来の技術）
最近、液体窒素温度程度の高温で超電導を示す高温超電
導体材料として、ペロブスカイト構造の多元系酸化物超
電導体が注目されている。これまでに報告されている酸
化物超電導体の代表的なものは、ＹＢａ ２ Ｃｕ ３
Ｏ７−６や（Ｌａ 。(Prior Art) Recently, multi-component oxide superconductors with a perovskite structure have attracted attention as high-temperature superconductor materials that exhibit superconductivity at temperatures as high as liquid nitrogen temperatures. A typical oxide superconductor reported so far is YBa 2 Cu 3
O7-6 and (La.
Ｂａ）２ Ｃｕ Ｏ４□等である。これらの酸化物超電
導材料は、焼結法、蒸着法、スパッタ法等により得られ
ている。Ba)2CuO4□, etc. These oxide superconducting materials are obtained by sintering, vapor deposition, sputtering, or the like.
今後これらの酸化物超電導体を具体的な素子に応用する
に当たって、超電導転移温度を高く安定に保ち、また大
きい臨界電流を得、素子特性の均−件、信頼性を優れた
ものとするためには、ある程度大きい面積の単結晶基板
或いは単結晶層として実現することが強く望まれる。When applying these oxide superconductors to specific devices in the future, we will need to maintain a high and stable superconducting transition temperature, obtain a large critical current, and improve the uniformity of device characteristics and reliability. It is strongly desired to realize this as a single-crystal substrate or a single-crystal layer with a relatively large area.
（発明が解決しようとする問題点）
以上のように、多元系酸化物超電導材料の素子応用に当
たっては、均一性の優れた単結晶が望まれるが、これま
でそのような酸化物単結晶を形成する有効な方法は提案
されていない。(Problems to be Solved by the Invention) As described above, when applying multi-component oxide superconducting materials to devices, single crystals with excellent uniformity are desired, but so far it has not been possible to form such oxide single crystals. No effective method has been proposed.
本発明は上記した点に鑑み、多元系酸化物超電導体の結
晶の製造方法を提供することを目的とする。In view of the above-mentioned points, an object of the present invention is to provide a method for producing a crystal of a multi-component oxide superconductor.
［発明の構成］
（問題点を解決するための手段）
本発明の方法は、バナジウム酸化物を含むフラックスを
用いた液相成長法（キポラス法）により多元系酸化物超
電導体結晶を製造することを特徴とする。[Structure of the Invention] (Means for Solving the Problems) The method of the present invention involves manufacturing a multi-component oxide superconductor crystal by a liquid phase growth method (Kiporas method) using a flux containing vanadium oxide. It is characterized by
例えば、ＹＢａ ２ Ｃｕ ３Ｏ７−Ｊ結晶のエピタキ
シャル成長を行うには、５０％以上のＶ２Ｏ５を含むフ
ラックスを用いることが好ましい。For example, in order to epitaxially grow a YBa 2 Cu 3O7-J crystal, it is preferable to use a flux containing 50% or more of V2O5.
（作用）
本発明によれば、キポラス法を用いることにより、低い
温度で多元系酸化物超電導体結晶の成長が可能であり、
超電導体の相転移が効果的に防止される。これにより、
超電導転移温度の均一性がよく、臨界電流が大きい所望
の酸化物超電導素子用ウェーハを再現性よく得ることが
できる。そして本発明により得られた結晶ウェーハを用
いれば、各種超電導素子を再現性よく作ることが可能に
なる。(Function) According to the present invention, multi-component oxide superconductor crystals can be grown at low temperatures by using the Kiporus method,
Phase transition of the superconductor is effectively prevented. This results in
A desired wafer for an oxide superconducting element having good uniformity of superconducting transition temperature and large critical current can be obtained with good reproducibility. By using the crystal wafer obtained according to the present invention, it becomes possible to manufacture various superconducting elements with good reproducibility.
（実施例）
以下、本発明の詳細な説明する。実施例では、ＹＢａ
２ Ｃｕ ３Ｏ７−ａ結晶に製造法を説明する二
第３図は、その結晶の引上げ装置を示す。第３図におい
て１は、アルミナシールド祠であり、この中に白金ヒー
タ２が配置され、その中心部に白金ルツボ３が支持台４
上に配置されている。支持台４は炉外部とつながる支持
棒５と一体化され、回転可能になっている。６は熱電対
である。ルツボ３内には、（１／２）Ｖ２Ｏ５が７０％
モル比のフラックスに３Ｏ％モル比の（１／２）Ｙ’２
０３ 、 ２ Ｂａ ｏ、 ３ Ｃｕ Ｏよりなる原
料を収容する。(Example) The present invention will be described in detail below. In the example, YBa
Figure 3, which explains the method for producing 2Cu3O7-a crystal, shows an apparatus for pulling the crystal. In FIG. 3, 1 is an alumina shield shrine, in which a platinum heater 2 is arranged, and a platinum crucible 3 is placed in the center of the shrine on a support stand 4.
placed above. The support stand 4 is integrated with a support rod 5 connected to the outside of the furnace, and is rotatable. 6 is a thermocouple. In crucible 3, (1/2) V2O5 is 70%
Molar ratio of flux to 30% molar ratio of (1/2) Y'2
Contains raw materials consisting of 03, 2 BaO, and 3CuO.
第４図は、Ｖ２０Ｓ Ｂａ Ｏ系の相図であり、この
系で適当なモル比を選ぶことにより、７００℃以下で液
相状態が得られる。従ってこの系をフラックスとして用
いることにより、比較的低温でＹ−Ｂａ−Ｃｕ−０系結
晶を引上げるための溶液を得ることが可能である。FIG. 4 is a phase diagram of the V20S Ba 2 O system, and by selecting an appropriate molar ratio in this system, a liquid phase state can be obtained at 700° C. or lower. Therefore, by using this system as a flux, it is possible to obtain a solution for pulling Y-Ba-Cu-0 system crystals at a relatively low temperature.
このようにしてルツボ３内に所望の溶液７を形成し、こ
れを１２００〜１３Ｏ０℃で約１０時間放置した後、溶
液温度を下げて約７００℃に設定する。そしてこの溶液
７に引上げ軸８の先端に取付けられたＹ−Ｂａ−Ｃｕ−
０系単結晶からなる種子結晶を浸し、十分にこの種子結
晶を馴染ませる。その後、０．１〜０．５℃／ｈという
小さい冷却速度で結晶９を引上げる。この引上げに際し
、溶液７の表面にはガス導入パイプ１２を介して酸素ガ
スを１００ｍ、ｆｆ／ｍｉｎ程度供給する。１０は内部
観察用光入射窓であり、１１は内部観察窓である。In this way, a desired solution 7 is formed in the crucible 3, and after being left at 1200-1300C for about 10 hours, the solution temperature is lowered and set at about 700C. Then, in this solution 7, a Y-Ba-Cu-
A seed crystal consisting of a 0-series single crystal is immersed in the solution, and the seed crystal is thoroughly absorbed. Thereafter, the crystal 9 is pulled up at a low cooling rate of 0.1 to 0.5°C/h. During this pulling, oxygen gas is supplied to the surface of the solution 7 through the gas introduction pipe 12 for 100 m at a rate of about ff/min. 10 is a light entrance window for internal observation, and 11 is an internal observation window.
こうして、直径１０８以上のＹＢａ２Ｃｕ３Ｏ７−６結
晶を引上げることができる。この場合、結晶引上げに際
して酸素ガスを供給することにより、溶液中および成長
結晶中の酸素欠陥の発生を防止することができる。In this way, a YBa2Cu3O7-6 crystal with a diameter of 108 or more can be pulled. In this case, by supplying oxygen gas during crystal pulling, it is possible to prevent the generation of oxygen defects in the solution and in the grown crystal.
このようにして得られたＹ−Ｂａ−Ｃｕ−０系結晶をス
ライス加工し、鏡面研磨して良質の超電導結晶基板を得
ることができた。The Y-Ba-Cu-0 crystal thus obtained was sliced and mirror-polished to obtain a high-quality superconducting crystal substrate.
上記実施例ではＹＢａ ２ Ｃｕ ３Ｏ７−１１結晶を
成長させた場合を説明したが、Ｙの代わりにＹｂ。In the above example, the case where YBa 2 Cu 3O7-11 crystal was grown was explained, but Yb was used instead of Y.
Ｈｏ、Ｄｙ、Ｅｕ、Ｅｒ、Ｔｍ、Ｌｕなど他の希土類元
素が入った酸化物超電導体結晶の場合にも本発明は有効
であり、また、Ｓｃ −Ｂａ −Ｃｕ −Ｏ系、Ｓｒ
−Ｌａ −Ｃｕ−０系、更にＳｒをＢａ。The present invention is also effective for oxide superconductor crystals containing other rare earth elements such as Ho, Dy, Eu, Er, Tm, and Lu;
-La -Cu-0 system, further Sr and Ba.
Ｃａなどで置換した系等、他のペロブスカイト構造を有
する多元系酸化物超電導体結晶を成長させる場合にも本
発明は有効である。The present invention is also effective when growing multi-component oxide superconductor crystals having other perovskite structures, such as those substituted with Ca or the like.
その池水発明はその趣旨を逸脱しない範囲で種々変形し
て実施することができる。The pond water invention can be implemented with various modifications without departing from the spirit thereof.
［発明の効果］
以上述べたように本発明によれば、酸化バナジウムをフ
ラックスとするキポラス法により、多元系酸化物超電導
体の良質の結晶を得ることができる。[Effects of the Invention] As described above, according to the present invention, high-quality crystals of a multi-component oxide superconductor can be obtained by the Kiporas method using vanadium oxide as a flux.
第１図は本発明の一実施例のＹ−Ｂａ−Ｃｕ−〇系結晶
の引上げ装置を示す図、第２図はＶ２０５−Ｂａ Ｏ系
の相図である。
１・・・アルミナシールド材、２・・・白金ヒータ、３
・・・白金ルツボ、４・・・支持台、５・・・支持棒、
６・・・熱電対、７・・・フラックスを含む溶液、８・
・・引上げ軸、９・・・Ｙ−Ｂａ−Ｃｕ−０系結晶、１
０・・・内部観察用光照射窓、１１・・・内部観察窓、
１２・・・ガス導入パイプ。
出願人代理人 弁理士 鈴江武彦
第１図FIG. 1 is a diagram showing a pulling device for a Y-Ba-Cu-〇-based crystal according to an embodiment of the present invention, and FIG. 2 is a phase diagram of a V205-Ba 2 O-based crystal. 1... Alumina shield material, 2... Platinum heater, 3
...Platinum crucible, 4...Support stand, 5...Support rod,
6... Thermocouple, 7... Solution containing flux, 8...
... Pulling axis, 9 ... Y-Ba-Cu-0 system crystal, 1
0... Light irradiation window for internal observation, 11... Internal observation window,
12...Gas introduction pipe. Applicant's agent Patent attorney Takehiko Suzue Figure 1
Claims (4)
成長法により多元系酸化物超電導体結晶を成長させるこ
とを特徴とする酸化物超電導体結晶の製造方法。(1) A method for producing an oxide superconductor crystal, which comprises growing a multi-component oxide superconductor crystal by a liquid phase growth method using a flux containing vanadium oxide.
Ｈｏ、Ｄｙ、Ｅｕ、Ｅｒ、Ｔｍ、Ｌｕから選ばれた一種
）であり、前記フラックスはＶ＿２Ｏ＿５である特許請
求の範囲第１項記載の酸化物超電導体結晶の製造方法。(2) The multi-component oxide superconductor is ABa_2Cu_3O_7_-_δ (A is Y, Yb,
2. The method for producing an oxide superconductor crystal according to claim 1, wherein the flux is V_2O_5.
Ｈｏ、Ｄｙ、Ｅｕ、Ｅｒ、Ｔｍ、Ｌｕから選ばれた一種
）であり、前記フラックスはＶ＿２Ｏ＿５が５０モル％
以上の溶液である特許請求の範囲第１項記載の酸化物超
電導体結晶の製造方法。(3) The multi-component oxide superconductor is ABa_2Cu_3O_7_-_δ (A is Y, Yb,
Ho, Dy, Eu, Er, Tm, Lu), and the flux contains 50 mol% of V_2O_5.
The method for producing an oxide superconductor crystal according to claim 1, which is the above solution.
する特許請求の範囲第１項記載の酸化物超電導体結晶の
製造方法。(4) The method for producing an oxide superconductor crystal according to claim 1, in which oxygen gas is supplied to the surface of the solution during the crystal growth.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62288117A JPH01131098A (en) | 1987-11-13 | 1987-11-13 | Production of oxide superconductor crystal |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62288117A JPH01131098A (en) | 1987-11-13 | 1987-11-13 | Production of oxide superconductor crystal |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01131098A true JPH01131098A (en) | 1989-05-23 |
Family
ID=17726026
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62288117A Pending JPH01131098A (en) | 1987-11-13 | 1987-11-13 | Production of oxide superconductor crystal |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01131098A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0672712A (en) * | 1990-04-13 | 1994-03-15 | Nippon Steel Corp | Oxide superconducting material containing rare-earth element and its production |
-
1987
- 1987-11-13 JP JP62288117A patent/JPH01131098A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0672712A (en) * | 1990-04-13 | 1994-03-15 | Nippon Steel Corp | Oxide superconducting material containing rare-earth element and its production |
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