JPH0393685A - Surface stabilizing treatment for oxide superconductive bulk - Google Patents
Surface stabilizing treatment for oxide superconductive bulkInfo
- Publication number
- JPH0393685A JPH0393685A JP1228977A JP22897789A JPH0393685A JP H0393685 A JPH0393685 A JP H0393685A JP 1228977 A JP1228977 A JP 1228977A JP 22897789 A JP22897789 A JP 22897789A JP H0393685 A JPH0393685 A JP H0393685A
- Authority
- JP
- Japan
- Prior art keywords
- bulk
- oxide
- metal
- film
- oxide superconductive
- 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
- 230000000087 stabilizing effect Effects 0.000 title description 2
- 229910052751 metal Inorganic materials 0.000 claims abstract description 15
- 239000002184 metal Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims description 19
- 230000006641 stabilisation Effects 0.000 claims description 2
- 238000011105 stabilization Methods 0.000 claims description 2
- 229910052709 silver Inorganic materials 0.000 abstract description 12
- 239000002887 superconductor Substances 0.000 abstract description 12
- 239000000126 substance Substances 0.000 abstract description 8
- 229910052737 gold Inorganic materials 0.000 abstract description 7
- 238000004544 sputter deposition Methods 0.000 abstract description 7
- 239000011248 coating agent Substances 0.000 abstract description 6
- 238000000576 coating method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- 230000002542 deteriorative effect Effects 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 239000010408 film Substances 0.000 description 11
- 239000008188 pellet Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 239000004332 silver Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 2
- 238000000151 deposition Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000002484 inorganic compounds Chemical class 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- NDVLTYZPCACLMA-UHFFFAOYSA-N silver oxide Chemical compound [O-2].[Ag+].[Ag+] NDVLTYZPCACLMA-UHFFFAOYSA-N 0.000 description 2
- -1 A-ZO3 Chemical class 0.000 description 1
- 229910009203 Y-Ba-Cu-O Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910001923 silver oxide Inorganic materials 0.000 description 1
- 235000012976 tarts Nutrition 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000007738 vacuum evaporation Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 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
- Superconductors And Manufacturing Methods Therefor (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
Description
【発明の詳細な説明】
（イ）技術分野
本発明は、酸化物Ｍｉ電導バルクの表面安定化法に関す
るものである，
（口）従来技術
各種方法で製造した酸化物超電導体，例えばＹＢａｚＣ
ｕ３０，−ｘ等は基本的に水やＣＯ，等に弱く、化学的
安定性が小さいため、大気中に保存しておくと超電導特
性（Ｔｃ，Ｊｃ，Ｈｃ等）が劣化する．
この対策として、ペレット等のＹＢａ９Ｃｕ３０７−ｘ
のバルクを作製する過程で、その原料もし〈は合或粉と
共に銀又は．酸化銀を添加存在せしめ、戊型体内で熱分
解あるいは析出せしめることにより，系内の酸素を過剰
に存在させて超電導相を安定的に生成させあるいは保護
したり、超電導相の相間に存在する粒界相の影響を電気
抵抗の低い銀を析出存在せしめることで安定化させる方
法が提案されている．
また，上記のように銀を焼結体内に存在させることな＜
．ａ７ｔＬ導相の化学的安定性を向上させる方法として
、酸化物超電導体のパルク表面に化学的安定性のある被
膜を形成させて該超電導バルク表面を水やＣＯ２等から
遮断し，該酸化物超電導体の経時変化を防止する方法も
提案されている．この方法の被膜材料としては、熱硬化
型樹脂や紫外線硬化型樹脂等の有機材料，ＩＴＯ，Ｓｉ
０２ ，Ａ交ＺＯ３等の無機化合物類，あるいはＡｕ．
Ａｇ，Ｔｉ等の金属材料がある．上記の諸材料中、導電
性を有する被膜材料としては，＃化物の一部の無機化合
物とＡｕ ， Ａｇ ．Ｔｉ等の金属材料があげられる
．これらの材料による被膜を酸化物超電導体の表面に形
成させて回路形威等を行なうことも可能であるが，基本
的にこのような被膜形成により酸化物超電導バルク表面
の超電導特性を保持又は向上させることはできない．
Ｙ−Ｂａ−Ｃｕ−０系酸化物超電導体の化学的安定性向
上の対策についても上記のように諸種提案されているが
、その代表的な手法としては下記の二法があるが，いず
れも欠点があって満足されるべきものではない．即ち、
（ａ）酸化物超電導焼結体中にＡｇを存在させ，結晶粒
界に析出させて化学的安定性を向上させる方法．
この（ａ）法では．Ａｇが酸化物超電導焼結体の全体に
わたって分散存在しているので、表面の化学的安定性が
小さく、該焼結体の表面から超電導特性が劣化する．
（ｂ）酸化物超電導バルク焼結体の表面に化学的安定性
のある被膜を形威し、超電導特性の劣化を防止する方法
．
この（ｂ）法では、酸化物超電導体の表面の超電導特性
を充分に発揮させることができない．（ハ）発明の開示
木発明は、上記のような欠点を解消するもので、Ｙ−Ｂ
ａ−Ｃｕ−０系等の酸化物超電導体の低抵抗もしくは０
抵抗等の超電導特性を劣化させることなく、該酸化物超
電導体の化学的安定性を向上させる方法を提供するもの
・である．即ち、本発明は酸化物超電導バルクの表面に
金属の膜を威膜し、これを熱処理することによって該バ
ルク表面に該金属を拡散させることを特徴とする酸化物
超電導バルクの表面安定化処理法である．
この場合、上記酸化物超電導バルクがＹＢａ２Ｃｕ，０
７−ｘのペロブス力イト型結晶構造を持った結晶であっ
て、ＹやＢａを置換したものであってもよく、またバル
ク表面に或膜する金属としては、超電導特性を保持しこ
れを向上せしめ得る金属であればいかなる金属でも良い
訳であるが、好ましくはＡｇかＡｕが好適である．Ｙ−
Ｂａ−Ｃｕ−０系の酸化物超電導体の表面にＡｇ又はＡ
ｕ等をスパッタリング法（以下，スパッター法という）
により１０″″！＃ｌＯ−”ｔａｒｔ（ａｍ−Ｈｇ）
， Ａ ｒ ： ０２ ｘ １ ： １程度の酸化性雰
囲気に保持し、Ａｇ又はＡｕｌＯ．１ｐｍ〜１００Ａに
被膜形處する．その後、該被膜焼結体を約８００〜９５
０℃で焼成して、上記金属被膜を焼結体中に表面拡散さ
せるのである．上記超電導バルク表面に金属を威膜する
方法としては、スパッター法以外に真空蒸着法やイオン
クラスタービーム法等の真空装置を用いる方法のほかに
，ペーストを用いて表面被覆する方法もあるが，該法は
バルク表面にＡｕ又はＡｇ等を或膜し，これを適当な熱
処理を施してパルク表面に拡散させるのである．
次に、本発明を実施例により説明する．（二）実施例
実施例Ｉ
ＹＢａｌＣｕｌ０７−ｘ酸化物超電導体（Ｆ）１ｉｎｃ
ｈペレットの表面にスパツター装置により全圧５ＸＩＯ
−”ｔｏｒｒ（ａｍ−Ｈｇ） ，Ａｒ：０２＝１＝１
，出力１２０Ｗの条件で．４ｉｎｃｈのＡｇターゲット
により２分間スパッタリングし，Ａｇ薄膜を威膜した．
その厚さは０．１ｇｍ以下であった．これを９００℃で
３０時間熱処理して、ＹＢａ２Ｃｕ３０ｔ−ｘペレット
表面に拡散させた．このベレットのＴｃ（臨界温度）を
測定したところ、８９Ｋであった．ｙ！に、このペレッ
トを約９５℃の熱湯に１０分間浸漬させた後、再度Ｔｃ
を測定したが，その値は全く同等であり，しかも表而変
化等は全く認められず，経時変化はなかった．
実施例２
上記実施例ｌと同様にＹＢａｌＣｕ３０７−ｘ酸化物超
電導体の１ ｉｎｃｈペレットを用いて，該ペレット表
面に実施例ｌと同様のスパッター条件で４ ｉｎｃＭ）
Ａ ｕターゲットによってＡｕｇ＠を威膜した．これ
を９００℃×３０時間熱処理し．Ａｕをペレ９ト表面に
拡散させた．
このペレットのＴｃを測定したところ，８８Ｋであった
．更に、このＡｕを表面拡散させたペレットを９５℃の
熱湯にｌＯ分間浸漬させた後、表面観察とＴｃ測定を行
なったが．Ａｇの場合と同様に経時変化は全く認められ
なかった．比較例
上記実施例１と同じ酸化物超電導体を使用し、Ａｇ金属
を威膜せずかつ表面拡散処理をしなかったペレットを９
５℃の熱湯に１分間浸漬させたところ、バルク表面が白
色化し、Ｔｃも著しく低下し、経時変化が著しかった．
（ホ）発明の効果
本発明法は上述したように、Ｙ−Ｂａ−Ｃｕ−Ｏ系酸化
物超電導バルクの表面にＡｇやＡｕ等の金属を成膜し、
該バルクを熱処理して上記金属を表面拡散させることに
より、バルク表面の超電導特性を錐持し、化学的安定性
を向上させることができるのである．
なお、Ｅ記実施例ではＹ−Ｂａ−Ｃｕ−０系酸化物超電
導バルクについて説明したが，他系の酸化物超電導バル
クについても、本発明法を適用し得ることは勿論である
．
特
許
出
願
人
同和鉱業秩式会社DETAILED DESCRIPTION OF THE INVENTION (a) Technical field The present invention relates to a method for surface stabilizing a conductive bulk of oxide Mi.
Since u30, -x, etc. are basically weak to water, CO, etc. and have low chemical stability, their superconducting properties (Tc, Jc, Hc, etc.) deteriorate if they are stored in the atmosphere. As a countermeasure for this, YBa9Cu307-x such as pellets
In the process of making the bulk, if the raw materials are combined with silver or powder. By adding silver oxide and causing it to thermally decompose or precipitate within the hollow body, it is possible to create an excess of oxygen in the system, stably generate or protect the superconducting phase, and reduce the amount of grains existing between the superconducting phases. A method has been proposed to stabilize the effect of the interfacial phase by precipitating silver with low electrical resistance. In addition, as mentioned above, silver should not be present in the sintered body.
．． As a method to improve the chemical stability of the a7tL conductive phase, a chemically stable film is formed on the bulk surface of the oxide superconductor to shield the superconducting bulk surface from water, CO2, etc. Methods have also been proposed to prevent changes in the body over time. Coating materials used in this method include organic materials such as thermosetting resins and ultraviolet curable resins, ITO, and Si.
02, inorganic compounds such as A-ZO3, or Au.
There are metal materials such as Ag and Ti. Among the above-mentioned materials, examples of conductive coating materials include some inorganic compounds of oxides, Au, Ag. Examples include metal materials such as Ti. Although it is possible to form a film made of these materials on the surface of an oxide superconductor to form a circuit, etc., it is basically possible to maintain or improve the superconducting properties of the bulk surface of an oxide superconductor by forming such a film. I can't do it. As mentioned above, various measures have been proposed to improve the chemical stability of Y-Ba-Cu-0 based oxide superconductors. It has its flaws and should not be satisfied. That is, (a) A method in which Ag is present in an oxide superconducting sintered body and precipitated at grain boundaries to improve chemical stability. In this law (a). Since Ag is dispersed throughout the oxide superconducting sintered body, the chemical stability of the surface is low, and the superconducting properties deteriorate from the surface of the sintered body. (b) A method of forming a chemically stable film on the surface of an oxide superconducting bulk sintered body to prevent deterioration of superconducting properties. In this method (b), the superconducting properties of the surface of the oxide superconductor cannot be fully exhibited. (c) Disclosure of the Invention The invention solves the above-mentioned drawbacks, and Y-B
Low or zero resistance of oxide superconductors such as a-Cu-0 series
The present invention provides a method for improving the chemical stability of oxide superconductors without deteriorating superconducting properties such as resistance. That is, the present invention provides a surface stabilization treatment method for an oxide superconducting bulk, which is characterized by depositing a metal film on the surface of the oxide superconducting bulk and heat-treating the film to diffuse the metal onto the surface of the bulk. It is. In this case, the oxide superconducting bulk is YBa2Cu,0
It is a crystal with a 7-x perovusite crystal structure, and may be one in which Y or Ba is substituted.Also, as a metal film on the bulk surface, it maintains and improves superconducting properties. Any metal may be used as long as it can be used, but Ag or Au is preferable. Y-
Ag or A on the surface of Ba-Cu-0 based oxide superconductor
sputtering method (hereinafter referred to as sputtering method)
10″″! #lO-”tart(am-Hg)
, A r : 02 x 1 : 1 or so in an oxidizing atmosphere, and Ag or AlO. Form a film at 1 pm to 100 A. Thereafter, the coated sintered body was
By firing at 0°C, the metal coating is diffused into the sintered body. Methods for depositing a metal film on the surface of the superconducting bulk include, in addition to the sputtering method, methods using vacuum equipment such as vacuum evaporation and ion cluster beam methods, as well as methods of surface coating using paste. The method involves forming a film of Au or Ag on the surface of the bulk, subjecting it to appropriate heat treatment, and diffusing it onto the surface of the bulk. Next, the present invention will be explained using examples. (2) Examples Example I YBalCul07-x oxide superconductor (F) 1 inc
A total pressure of 5XIO is applied to the surface of the pellet using a sputtering device.
-”torr(am-Hg), Ar:02=1=1
, under the condition of output 120W. Sputtering was performed using a 4-inch Ag target for 2 minutes to form an Ag thin film.
Its thickness was less than 0.1 gm. This was heat treated at 900°C for 30 hours and diffused onto the surface of the YBa2Cu30t-x pellet. The Tc (critical temperature) of this pellet was measured and found to be 89K. Y! After immersing the pellets in boiling water at about 95°C for 10 minutes, Tc
were measured, and the values were exactly the same, and no changes in appearance were observed, and there was no change over time. Example 2 A 1 inch pellet of YBalCu307-x oxide superconductor was used in the same manner as in Example 1 above, and 4 inM) was applied to the surface of the pellet under the same sputtering conditions as in Example 1).
Aug@ was attacked by A u target. This was heat treated at 900°C for 30 hours. Au was diffused onto the surface of the pellet. When the Tc of this pellet was measured, it was 88K. Furthermore, the pellets with Au diffused on their surfaces were immersed in hot water at 95°C for 10 minutes, and then surface observation and Tc measurements were performed. As in the case of Ag, no changes over time were observed. Comparative Example Using the same oxide superconductor as in Example 1 above, 9 pellets were prepared without coating Ag metal and without surface diffusion treatment.
When immersed in hot water at 5°C for 1 minute, the bulk surface turned white, Tc decreased significantly, and changes over time were significant. (e) Effects of the invention As described above, the method of the present invention forms a film of metal such as Ag or Au on the surface of a Y-Ba-Cu-O based oxide superconducting bulk,
By heat-treating the bulk and diffusing the metal on the surface, the superconducting properties of the bulk surface can be maintained and the chemical stability can be improved. Although the Y-Ba-Cu-0 based oxide superconducting bulk was explained in Example E, it goes without saying that the method of the present invention can also be applied to other types of oxide superconducting bulks. Patent applicant Dowa Mining Chichishiki Company
Claims (1)
を熱処理することによって該バルク表面に上記金属を拡
散させることを特徴とする酸化物超電導バルクの表面安
定化処理法。1. A method for surface stabilization of an oxide superconducting bulk, comprising forming a metal film on the surface of the oxide superconducting bulk and heat-treating the metal to diffuse the metal onto the surface of the bulk.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1228977A JP2969273B2 (en) | 1989-09-04 | 1989-09-04 | Surface stabilization method for oxide superconducting bulk |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1228977A JP2969273B2 (en) | 1989-09-04 | 1989-09-04 | Surface stabilization method for oxide superconducting bulk |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0393685A true JPH0393685A (en) | 1991-04-18 |
| JP2969273B2 JP2969273B2 (en) | 1999-11-02 |
Family
ID=16884838
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1228977A Expired - Lifetime JP2969273B2 (en) | 1989-09-04 | 1989-09-04 | Surface stabilization method for oxide superconducting bulk |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2969273B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012089455A (en) * | 2010-10-22 | 2012-05-10 | Fujikura Ltd | Manufacturing method of superconducting wire rod and superconducting wire rod |
| CN111272533A (en) * | 2020-03-07 | 2020-06-12 | 北京工业大学 | Sample preparation method for researching oxygen element diffusion mechanism of high-temperature superconducting material |
-
1989
- 1989-09-04 JP JP1228977A patent/JP2969273B2/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012089455A (en) * | 2010-10-22 | 2012-05-10 | Fujikura Ltd | Manufacturing method of superconducting wire rod and superconducting wire rod |
| CN111272533A (en) * | 2020-03-07 | 2020-06-12 | 北京工业大学 | Sample preparation method for researching oxygen element diffusion mechanism of high-temperature superconducting material |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2969273B2 (en) | 1999-11-02 |
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