JPH02229717A - Production of oxide superconducting thin film - Google Patents
Production of oxide superconducting thin filmInfo
- Publication number
- JPH02229717A JPH02229717A JP1072871A JP7287189A JPH02229717A JP H02229717 A JPH02229717 A JP H02229717A JP 1072871 A JP1072871 A JP 1072871A JP 7287189 A JP7287189 A JP 7287189A JP H02229717 A JPH02229717 A JP H02229717A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- superconducting thin
- substrate
- oxide
- temperature
- 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.)
- Granted
Links
- 239000010409 thin film Substances 0.000 title claims abstract description 43
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 239000000758 substrate Substances 0.000 claims abstract description 24
- 238000004544 sputter deposition Methods 0.000 claims abstract description 16
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 229910014454 Ca-Cu Inorganic materials 0.000 claims abstract description 6
- 230000001590 oxidative effect Effects 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 7
- 239000000843 powder Substances 0.000 abstract description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- 239000010408 film Substances 0.000 abstract description 6
- 238000000034 method Methods 0.000 abstract description 6
- 239000008188 pellet Substances 0.000 abstract description 4
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 abstract 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 abstract 2
- AYJRCSIUFZENHW-UHFFFAOYSA-L barium carbonate Chemical compound [Ba+2].[O-]C([O-])=O AYJRCSIUFZENHW-UHFFFAOYSA-L 0.000 abstract 2
- 239000002904 solvent Substances 0.000 abstract 2
- 229910002480 Cu-O Inorganic materials 0.000 abstract 1
- 229910008649 Tl2O3 Inorganic materials 0.000 abstract 1
- 229910000019 calcium carbonate Inorganic materials 0.000 abstract 1
- 235000010216 calcium carbonate Nutrition 0.000 abstract 1
- QTQRFJQXXUPYDI-UHFFFAOYSA-N oxo(oxothallanyloxy)thallane Chemical compound O=[Tl]O[Tl]=O QTQRFJQXXUPYDI-UHFFFAOYSA-N 0.000 abstract 1
- 238000010586 diagram Methods 0.000 description 11
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 10
- 238000002441 X-ray diffraction Methods 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 229910052786 argon Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005259 measurement Methods 0.000 description 4
- 239000013077 target material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000005292 diamagnetic effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000005245 sintering Methods 0.000 description 2
- 239000002887 superconductor Substances 0.000 description 2
- 230000018199 S phase Effects 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910001179 chromel Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229910052738 indium Inorganic materials 0.000 description 1
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000005291 magnetic effect Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 238000010671 solid-state reaction Methods 0.000 description 1
- 238000003756 stirring Methods 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
Abstract
Description
【発明の詳細な説明】
（イ）産業−Ｌの利用分野
本発明は酸化物超電導薄膜の製造法に関し、特にＴｅ−
Ｂａ−Ｃａ−Ｃｕの酸化物の超電導薄膜の製造法に関す
る。Detailed Description of the Invention (a) Field of Application of Industry-L The present invention relates to a method for manufacturing oxide superconducting thin films, particularly Te-
The present invention relates to a method for producing a superconducting thin film of Ba-Ca-Cu oxide.
（口）従来の技術
近隼、Ｔ ｌ − Ｂ ａ − Ｃ ａ − Ｃ ｕの
酸化物がＭＩ’＋窒素の沸点（７７Ｋ）より高い臨界温
度で超電導状態に入ることが見出されて脚光を浴びてい
る。(Example) Conventional technology Chikayuki discovered that the oxide of T l - B a - C a - C u enters a superconducting state at a critical temperature higher than the boiling point (77 K) of MI'+nitrogen, and it came into the spotlight. Bathing.
（ハ）発明が解決しようとする課題
ところで、現在、液体ヘリウムを用いてＭＲ＋などに実
用化されているＮｂ系の超電導体は熱的安定性あるいは
磁気的安定性のために全て薄膜化あるいは線材化して用
いられている。従って酸化物超電導体も各種分野に用い
るには同様の理由で薄膜化あるいは線材化しなければな
らない。(c) Problems to be solved by the invention By the way, Nb-based superconductors currently in practical use for MR+ etc. using liquid helium are all made into thin films or wires for thermal stability or magnetic stability. It is used as a form. Therefore, for the same reason, oxide superconductors must be made into thin films or wires in order to be used in various fields.
（二）課題を解決するための下段
本発明は、Ｔ ｌ − Ｂ ａ − Ｃ ａ − Ｃ
ｕの酸化物をターゲットとし、スパッタリング法により
基板−１二にスバッタした後、酸化雰囲気中でアニール
処理する酸化物超電導薄膜の製造法にある。(2) The lower stage of the present invention for solving the problem is T l - B a - C a - C
The method of manufacturing an oxide superconducting thin film includes using an oxide of U as a target, sputtering it onto a substrate 1-2 by a sputtering method, and then annealing it in an oxidizing atmosphere.
（ホ）作 用
本発明によれば、Ｔ ｌ − Ｂ ａ − Ｃ ａ −
Ｃ ｕの酸化物からなる超電導薄膜を簡単な方法で容
易に得ることができる。(e) Effect According to the present invention, T l - B a - C a -
A superconducting thin film made of Cu oxide can be easily obtained by a simple method.
（へ）実施例
［第Ｉ実Ｍｉｔ列］
第１図は本発明超電導薄膜を得るための装置の−１’Ａ
を示し、同図において（１）はスパッタリング装置のベ
ルジャーであって、排気系（２）が連なっている。 （
３）は詠ベルジャー（１）内に放電ガスであるアルゴン
ガスを供給するアルゴンガスボンベで、 バリアブルリ
ークバルブ（４）並びにストップパルブ（５）を介して
ベルジャー（１）に連なっている（６）（７）はベルジ
ャー（１）内に可動自在のシャッター（８）を介して対
向配置された対向電極で、その陽極（６）は接地される
とともに、その表面ｔに超電導薄膜を堆積させるＳｒＴ
ｉＯ，基板（９）が置かれている。(f) Example [Ith Actual Mit Row] Figure 1 shows -1'A of the apparatus for obtaining the superconducting thin film of the present invention.
In the figure, (1) is a bell jar of a sputtering device, and an exhaust system (2) is connected thereto. (
3) is an argon gas cylinder that supplies argon gas as a discharge gas into the bell jar (1), and is connected to the bell jar (1) via a variable leak valve (4) and a stop valve (5). 7) is a counter electrode placed opposite to each other through a movable shutter (8) in the bell jar (1), the anode (6) of which is grounded, and an SrT film on which a superconducting thin film is deposited on its surface t.
iO, a substrate (9) is placed.
一方、陰極（７）は超電導材料であるＴｔ−Ｂａ−Ｃａ
−Ｃｕの酸化物（組成比は、Ｔｔ ： Ｂａ ：Ｃａ
： Ｃｕ−３ ： ２ ： ２ ： ３）の焼結体から
なるターゲット材にて構成されており、この陰極（７）
にはｔｔの高い電圧が印加されている。（１０）（１１
）は高真空計、低真空計である。On the other hand, the cathode (7) is made of superconducting material Tt-Ba-Ca.
-Cu oxide (composition ratio: Tt:Ba:Ca
: Cu-3 : 2 : 2 : 3) is made of a target material made of a sintered body, and this cathode (7)
A high voltage of tt is applied to. (10) (11)
) are high vacuum gauges and low vacuum gauges.
上記焼結体からなるターゲットは、高純度試薬の固相反
応により形成される．すなわち純度９９９％の”ｒ ｔ
＊Ｏ ｓ （３’ｔ．３ｇ）、純度９９．９９％のＢ
ａ Ｃ Ｏ ｚ （１９．７ｇ）、純度９９．９９％
のＣａＣＯ， （Ｉ０．０ｇ）、純度９９．９９％のＣ
ｕ Ｏ （１１．９ｇ）の粉末を、仕込み組成でＴｊ
：Ｂａ：Ｃａ：Ｃｕ＝３ ： ２ ： ２ ： ３とな
るようにメタノール、工タノールなどの有機溶媒に加え
てスターラにて撹拌し，次いで有機溶媒を蒸発させた後
、乳鉢にてすりつぶして粉末状にする。この粉末をアル
ミナキャップで覆われたアルミナボートに入れて電気炉
にて９３０℃で３０分間仮焼成し、仮焼成された粉末を
成形器に入れ、成形圧力７５０ｋｇｆ／ｃ＋ｎ”でプレ
ス加工してベレット状に固める。次にこのベレットを空
気中において９２５℃で１分間焼結して直径１０ｃｍ、
厚さ０．５ｃｍのＴＪ’ｓＢａＩＣａｔｃ ｕｓｏｘの
焼結ターゲットを得る。The target made of the sintered body described above is formed by a solid-state reaction of high-purity reagents. In other words, 999% purity
*Os (3't.3g), B with purity 99.99%
a C O z (19.7 g), purity 99.99%
CaCO, (I0.0g), purity 99.99% C
U O (11.9 g) of powder was added to the preparation composition Tj
:Ba:Ca:Cu=3:2:2:3 by adding to an organic solvent such as methanol or ethanol and stirring with a stirrer, then evaporating the organic solvent, and then grinding in a mortar to form a powder. make it into a shape. This powder is placed in an alumina boat covered with an alumina cap and calcined for 30 minutes at 930°C in an electric furnace.The calcined powder is then placed in a molding machine and pressed at a molding pressure of 750kgf/c+n'' to form a pellet. This pellet is then sintered in air at 925°C for 1 minute to form a diameter of 10 cm.
A sintered target of TJ's BaICatc usox with a thickness of 0.5 cm is obtained.
而して、 アルゴンガスポンベ（３）からベルジャ−
（１）内に純度９９．９９９５％のアルゴンガスを３．
０〜３０，Ｏｍｔｏｒｒの圧力で供給すると同時に、ス
パッタ出力を１００〜２５０Ｗとしてスパッタリング処
理し、基板（９）に０．５〜５μｍの厚みの膜を形成す
る。実施例においては、スパッタ出力１ ２０Ｗ．２．
６ＫＶでターゲットに対して基板を３．５３離し、成長
速度４００人／分で、基板に１．５〜３．５μｍの厚み
の膜を形成した。Then, from the argon gas pombe (3) to the bell jar
(1) Place 99.9995% pure argon gas in 3.
At the same time, a sputtering process is carried out at a sputtering power of 100 to 250 W while supplying at a pressure of 0 to 30.0 mtorr to form a film with a thickness of 0.5 to 5 m on the substrate (9). In the example, sputtering output 1 is 20W. 2.
A film with a thickness of 1.5 to 3.5 μm was formed on the substrate at a growth rate of 400 persons/min at 6 KV, with the substrate separated by 3.53 mm with respect to the target.
その後，スパッタ装置から取り出して電気炉に入れ、流
量、２１７分の酸素雰囲気中において室温からｌ”ｃ／
秒で９４０℃まで昇温し９４０℃で１０分のアニール処
理を行い−２０℃／秒で室温まで降温して冷却した。尚
、発明者等の実験によれば、アニール温度、時間、特に
温度は上記した温度が最適であったが、雰囲気は酸化雰
囲気であれば酸素に限定されるものではなく、また冷却
条件も超電導状態を得るのに余り影響がないことが判明
している。After that, it was taken out from the sputtering equipment and placed in an electric furnace, and was heated from room temperature to 1"c/in an oxygen atmosphere for 217 minutes at a flow rate of 1"c/
The temperature was raised to 940° C. in seconds, annealing was performed at 940° C. for 10 minutes, and the temperature was lowered to room temperature at −20° C./second. According to the experiments conducted by the inventors, the annealing temperature and time, especially the temperatures mentioned above, were optimal, but the atmosphere is not limited to oxygen as long as it is an oxidizing atmosphere, and the cooling conditions are also superconducting. It has been found that it does not have much effect on obtaining the state.
第２図はこのようにして得られた、ＴＩ−Ｂａ−Ｃａ−
Ｃｕ−０の超電導薄膜の温度に対する抵抗変化を示すも
のである。抵抗の温度依存性は標準的な四端子ｔ掻法に
て測定され、接続は薄膜上にインジウム電極を圧接させ
る。温度は金＋０．０７％鉄一クロメルサーモカップル
により測定する。Figure 2 shows the TI-Ba-Ca-
It shows the resistance change with respect to temperature of a Cu-0 superconducting thin film. The temperature dependence of resistance is measured using a standard four-terminal tread method, and the connection is made by pressing an indium electrode onto the thin film. Temperature is measured with a gold+0.07% iron-chromel thermocouple.
また流した電流の密度は、０．５〜５Ａ／０１１１’と
する。Further, the density of the current applied is 0.5 to 5 A/0111'.
零抵抗温度は８６Ｋ（−１８７℃）であるが、１１０Ｋ
前後で抵抗減少が観察される。このことから薄膜の一部
にＩＩＯＫ級の超電導相が含まれているものと思われる
。Zero resistance temperature is 86K (-187℃), but 110K
A decrease in resistance is observed before and after. This suggests that a portion of the thin film contains an IIOK class superconducting phase.
第３図はこのようにして得られた超電導薄膜のＸ線回折
パターンである。FIG. 3 shows the X-ray diffraction pattern of the superconducting thin film thus obtained.
一方、超電導状態を立証する他の要因であるマイスナー
効果はＩＩＯＫ付近から反磁性を示し始めた。On the other hand, the Meissner effect, which is another factor proving the superconducting state, began to exhibit diamagnetic properties around IIOK.
［第２実施例］
第２実施例は、第１実施例において使用したＳｒＴｉＯ
ｓ基板の代わりに、ＭｇＯの基板を使用したものであり
、他の条件即ち焼結ターゲット、スパッタ条件およびア
ニール条件はすべて第１実施例と同一である。[Second Example] The second example is based on the SrTiO used in the first example.
An MgO substrate was used instead of the s-substrate, and the other conditions, ie, the sintering target, sputtering conditions, and annealing conditions, were all the same as in the first example.
第４図はこのようにして得られたＴｔ−Ｂａ−Ｃａ−Ｃ
ｕ−０の超電導薄膜の温度に対する抵抗変化を示すもの
であり、この測定条件も第１実施例と同一である。第４
図から、零抵抗温度は１１６Ｋ（−１５７℃）であるこ
とがわかる。Figure 4 shows the Tt-Ba-Ca-C obtained in this way.
It shows the change in resistance of the u-0 superconducting thin film with respect to temperature, and the measurement conditions are also the same as in the first example. Fourth
From the figure, it can be seen that the zero resistance temperature is 116K (-157°C).
一方、マイスナー効果は１１５Ｋ付近から反磁性を示し
始める。On the other hand, the Meissner effect begins to exhibit diamagnetic properties around 115K.
第５図は、このようにして得られた超電導薄膜のＸ線回
折パターンで、これらの回折ピークからこの超電導薄膜
は、２２２３相と２１２２相を含むことがわかる。FIG. 5 shows the X-ray diffraction pattern of the superconducting thin film thus obtained, and it can be seen from these diffraction peaks that this superconducting thin film contains 2223 phase and 2122 phase.
［第３実施例コ
第３実施例は、第１実施例において使用したＳｒ Ｔ
ｉＯ ｓ基板の代りに、ＹＳＺ基板を使用したものであ
り、他の条件はすべて第１実施例と同一である。[Third Example] In the third example, Sr T used in the first example was used.
A YSZ substrate was used instead of the iOs substrate, and all other conditions were the same as in the first example.
第６図はこのようにして得られたＴｌ−Ｂａ７Ｃ ａ−
Ｃ ｕ−０の超電導薄膜の温度に対する抵抗変化を示す
らのであり、この測定条件もｌｔ実施例と同一である。Figure 6 shows the Tl-Ba7C a- obtained in this way.
This figure shows the resistance change with respect to temperature of the Cu-0 superconducting thin film, and the measurement conditions are the same as in the lt example.
第６図では、ＹＳＺ基板と他の基板とを比較しているが
、ＹＳＺ基板では零抵抗温度は８０Ｋ（−１９３℃）で
あり、他の基板と同様に実用上問題が無いことを示して
いる。以上第１〜第３実施例においては、 陰極
（７）のターゲット材として、超電導材料であるＴＪ！
−Ｂａ−Ｃ ａ−Ｃ ｕの酸化物の焼結体であって、そ
の酸化物の組成比が３：２：２：３のものを用いている
が、ＴＩ！−Ｂａ−Ｃａ−Ｃｕの酸化物焼結体の組成比
が１：２：２：３であるものを用いた第４〜第６実施例
を以下に示す。In Figure 6, the YSZ board is compared with other boards, and the zero resistance temperature of the YSZ board is 80K (-193°C), indicating that there is no problem in practical use like other boards. There is. In the first to third embodiments described above, the target material of the cathode (7) is TJ!, which is a superconducting material.
A sintered body of -Ba-C a-C u oxide with a composition ratio of 3:2:2:3 is used, but TI! Examples 4 to 6 using sintered oxides of -Ba-Ca-Cu having a composition ratio of 1:2:2:3 are shown below.
［第４実施例］
第４実施例は、陰極（７）のターゲット材がＴｌ−Ｂａ
−Ｃａ−Ｃｕの酸化物（組成比は、Ｔｔ：Ｂａ：Ｃａ：
Ｃｕ−１ ：２：２：３）の焼結体からなり、使用する
基板はＳ ｒ Ｔ ｉ Ｏ ｓである。[Fourth Example] In the fourth example, the target material of the cathode (7) is Tl-Ba.
-Ca-Cu oxide (composition ratio is Tt:Ba:Ca:
The substrate used is SrTiOs.
まず、仕込み組成でＴｌ：Ｂａ：Ｃａ：Ｃｕ＝１：２：
２：３の焼結ターゲットをつぎのようにして形成した。First, the preparation composition is Tl:Ba:Ca:Cu=1:2:
A 2:3 sintered target was formed as follows.
すなわち純度９９．９％のＴ！．Ｏｓ（１６．３ｇ）、
純度９９．９９％のＢ ａ Ｃ Ｏ ｓｃ２８．２ｇ）
、純度９９．９９％のＣ ａ Ｃ Ｏ ｓ （１４．
３ｇ）、純度９９．９９％のＣ ｕ Ｏ （１７．０ｇ
）の粉末を、第１実施例と同じ条件で混合、仮焼成、プ
レス成形、焼結して焼結ターゲットを得た。In other words, T with a purity of 99.9%! ．． Os (16.3g),
28.2 g of B a CO sc with a purity of 99.99%)
, 99.99% purity Ca CO s (14.
3g), 99.99% purity CuO (17.0g
) were mixed, pre-fired, press-molded and sintered under the same conditions as in the first example to obtain a sintered target.
スパッタリング装置のベルジャー（１）内の構成は、基
板（９）の構成を含め第１実施例と同じであり，アルゴ
ンガス圧力、スパッタ出力及び基板（９）上に形成する
膜厚も第１実施例と同じにした。The configuration inside the bell jar (1) of the sputtering device is the same as in the first embodiment, including the configuration of the substrate (9), and the argon gas pressure, sputtering output, and film thickness formed on the substrate (9) are also the same as in the first embodiment. I did the same as the example.
また２スパッタ装置から取り出して電気炉にいれるアニ
ール処理条件についても、第１実施例の場合と同じにし
た。Further, the annealing conditions for taking out the sample from the second sputtering apparatus and placing it in an electric furnace were also the same as in the first embodiment.
第７図はこの第４実施例で得られた超電導薄膜のＸ＃！
回折パターンであり、この薄膜がＴＪ！．Ｂａ Ｈ（：
ａ ＩＣ ｕ ｓｏ ｓ相（１２２３相）の単相であ
ることを示している。Figure 7 shows the X#! superconducting thin film obtained in this fourth example.
It is a diffraction pattern, and this thin film is TJ! ．． BaH(:
It shows that it is a single phase of a IC u so s phase (1223 phase).
第８図は第２実施例で得られた超電導薄膜の超電導特性
を示しており、１０３Ｋ（−１７０℃）で抵抗が零にな
ることがわかる。FIG. 8 shows the superconducting properties of the superconducting thin film obtained in the second example, and it can be seen that the resistance becomes zero at 103 K (-170° C.).
［第５実施例〕
第５実施例は、第４実施例において使用したＳｒ Ｔ
＋ Ｏ ｓ基板の代りに、ＭｇＯ基板を使用したもので
あり，他の条件即ち焼結ターゲット、スパンタ条件およ
びアニール条件はすべて第４実施例と同一である。[Fifth Example] In the fifth example, the Sr T used in the fourth example
A MgO substrate was used instead of the +Os substrate, and all other conditions, ie, sintering target, spunter conditions, and annealing conditions, were the same as in the fourth embodiment.
第９図はこのようにして得られたＴｊ！＋Ｂａ＊Ｃａｔ
ｃｕｓｏｘの超電導薄膜の温度に対する抵抗変化を示す
ものであり、この測定条件も第４実施例と同一である。Figure 9 shows Tj! obtained in this way! +Ba*Cat
It shows the resistance change with respect to temperature of the superconducting thin film of CUSOX, and the measurement conditions are also the same as in the fourth example.
第９図から、零抵抗温度は１０９Ｋ（−１６４℃）であ
ることがわかる。From FIG. 9, it can be seen that the zero resistance temperature is 109K (-164°C).
第ｌＯ図は、このようにして得られた超電導薄膜のＸ線
回折パターンで、これらの回折ピークから、この超電導
薄膜は１２２３相の単相であることがわかる。Figure 10 shows the X-ray diffraction pattern of the superconducting thin film thus obtained, and from these diffraction peaks it can be seen that this superconducting thin film has a single phase of 1223 phases.
［第６実施例］
第６実施例は、第４実施例において使用したＳｒ Ｔ
＋ Ｏ ｓ基板の代りに、ＹＳＺ基板を使用したもので
あり，他の条件はすべて第４実施例と同一である。[Sixth Example] In the sixth example, the Sr T used in the fourth example
A YSZ substrate was used instead of the +Os substrate, and all other conditions were the same as in the fourth embodiment.
第１１図は、このようにして得られたＴｌ，Ｂａ ｔｃ
ａ ｔＣ ｕ ｓｏｘの超電導薄膜の温度に対する抵
抗変化を示すものであり、この測定条件も第４実施例と
同一である。第１１図では、ＹＳｚ基板と他の基板とを
比較しているが、ＹＳＺ基板では零抵抗温度はＩＯＯＫ
（−１７３℃）であり他の基板と同様に実用上問題が無
いことを示している。FIG. 11 shows Tl, Batc obtained in this way.
It shows the resistance change with respect to temperature of the superconducting thin film of a tC u sox, and the measurement conditions are also the same as in the fourth example. In Figure 11, the YSZ substrate is compared with other substrates, and the zero resistance temperature of the YSZ substrate is IOOK.
(-173°C), indicating that there is no problem in practical use as with other substrates.
第１２図は、このようにして得られた超電導薄膜のＸ線
回折パターンで、これらの回折ピークから、この超電導
薄膜は１２２３相の単相であることがノ）かる。FIG. 12 shows the X-ray diffraction pattern of the superconducting thin film thus obtained, and from these diffraction peaks it can be seen that this superconducting thin film has a single phase of 1223 phases.
（ト） 発明の効果
本発明によれば、通常のスパッタリング装置を用いる簡
単な方法でＴｌ−Ｂａ−Ｃａ−Ｃｕの酸化物の超電導薄
膜が得られ、その工業的価値は極めて大である。(G) Effects of the Invention According to the present invention, a superconducting thin film of Tl-Ba-Ca-Cu oxide can be obtained by a simple method using a normal sputtering apparatus, and its industrial value is extremely large.
第１図は本発明による酸化物超電導薄膜を得るためのス
パッタリング装置の概略図、第２図は本発明の第１実施
例によって得られた超電導薄膜の抵抗一温度特性図２第
３図は同じく第１実施例によって得られた超電導薄膜の
Ｘ線回折パターン図、第４図は第２実施例によって得ら
れた超電導薄膜の抵抗一温度特性図、第５図は同じく第
２実施例によって得られた超電導薄膜のＸ線回折パター
ン図、第６図は第３実施例によって得られた超電導薄膜
の抵抗一温度特性比較図、第７図は同じく第３実施例に
よって得られた超電導薄膜の抵抗一温度特性図、第８図
は第４実施例によって得られた超電導薄膜の抵抗一温度
特性図、第９図は第５実施例によって得られた超電導薄
膜の抵抗一温度特性図、第ｌＯ図は同じく第５実施例に
よって得られた超電導薄膜のＸ線回折パターン図、第１
１図は第６実施例によって得られた超電導薄膜の抵抗一
温度特性比較図、第１２図は同じく第６実施例によって
得られた超電導薄膜のＸ線回折パターン図である。（１
）・・・ベルジャー、（６）（７）・・・対向電極、（
９）・・・基板。Fig. 1 is a schematic diagram of a sputtering apparatus for obtaining an oxide superconducting thin film according to the present invention, Fig. 2 is a diagram showing the resistance-temperature characteristics of a superconducting thin film obtained according to the first embodiment of the present invention, and Fig. 3 is the same. FIG. 4 is an X-ray diffraction pattern diagram of the superconducting thin film obtained in the first embodiment, FIG. 4 is a resistance-temperature characteristic diagram of the superconducting thin film obtained in the second embodiment, and FIG. FIG. 6 is a comparison diagram of the resistance-temperature characteristics of the superconducting thin film obtained in the third embodiment, and FIG. 7 is the resistance-temperature characteristic diagram of the superconducting thin film obtained in the third embodiment. FIG. 8 is a resistance-temperature characteristic diagram of the superconducting thin film obtained in the fourth embodiment, FIG. 9 is a resistance-temperature characteristic diagram of the superconducting thin film obtained in the fifth embodiment, and FIG. Similarly, X-ray diffraction pattern diagram of the superconducting thin film obtained in the fifth example, 1st
FIG. 1 is a comparison diagram of the resistance-temperature characteristics of the superconducting thin film obtained in the sixth embodiment, and FIG. 12 is an X-ray diffraction pattern diagram of the superconducting thin film also obtained in the sixth embodiment. (1
)...Bell jar, (6) (7)...Counter electrode, (
9)...Substrate.
Claims (1)
し、スパッタリング法により基板上にスパッタした後、
酸化雰囲気中でアニール処理することを特徴とした酸化
物超電導薄膜の製造法。(1) After sputtering onto a substrate using a sputtering method using Tl-Ba-Ca-Cu oxide as a target,
A method for producing an oxide superconducting thin film characterized by annealing in an oxidizing atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1072871A JP2523013B2 (en) | 1988-03-25 | 1989-03-24 | Manufacturing method of oxide superconducting thin film |
Applications Claiming Priority (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63-72390 | 1988-03-25 | ||
| JP7239088 | 1988-03-25 | ||
| JP29143688 | 1988-11-17 | ||
| JP63-291436 | 1988-11-17 | ||
| JP1072871A JP2523013B2 (en) | 1988-03-25 | 1989-03-24 | Manufacturing method of oxide superconducting thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02229717A true JPH02229717A (en) | 1990-09-12 |
| JP2523013B2 JP2523013B2 (en) | 1996-08-07 |
Family
ID=27300939
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1072871A Expired - Lifetime JP2523013B2 (en) | 1988-03-25 | 1989-03-24 | Manufacturing method of oxide superconducting thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2523013B2 (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01236663A (en) * | 1988-03-17 | 1989-09-21 | Matsushita Electric Ind Co Ltd | Manufacture of superconducting wiring |
| JPH0244014A (en) * | 1987-11-25 | 1990-02-14 | Kawatetsu Mining Co Ltd | Production of electroconductive or superconducting thin film |
-
1989
- 1989-03-24 JP JP1072871A patent/JP2523013B2/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0244014A (en) * | 1987-11-25 | 1990-02-14 | Kawatetsu Mining Co Ltd | Production of electroconductive or superconducting thin film |
| JPH01236663A (en) * | 1988-03-17 | 1989-09-21 | Matsushita Electric Ind Co Ltd | Manufacture of superconducting wiring |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2523013B2 (en) | 1996-08-07 |
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