JPS63289726A - Manufacture of compound superconductive thin film - Google Patents

Manufacture of compound superconductive thin film

Info

Publication number
JPS63289726A
JPS63289726A JP62124613A JP12461387A JPS63289726A JP S63289726 A JPS63289726 A JP S63289726A JP 62124613 A JP62124613 A JP 62124613A JP 12461387 A JP12461387 A JP 12461387A JP S63289726 A JPS63289726 A JP S63289726A
Authority
JP
Japan
Prior art keywords
thin film
compound
layer
producing
substrate
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
Application number
JP62124613A
Other languages
Japanese (ja)
Inventor
Minoru Yamada
穣 山田
Shigeo Nakayama
茂雄 中山
Akira Murase
村瀬 暁
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toshiba Corp
Original Assignee
Toshiba Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Toshiba Corp filed Critical Toshiba Corp
Priority to JP62124613A priority Critical patent/JPS63289726A/en
Publication of JPS63289726A publication Critical patent/JPS63289726A/en
Pending legal-status Critical Current

Links

Classifications

    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

Abstract

PURPOSE:To secure a compound superconductive film in an L-Br-Cu-O system by stacking respective layers of metal L (Y, Er, Dy, Sm, Gd, Ho, Nd, Yb, Tm and Lu) and a single layer of Br and Cu or an oxide of Br and Cu on a substrate in order and then performing their heat treatment in oxygen. CONSTITUTION:Using an SiO2 substrate 2, a sheet of Y and BaCu is used for targets 6a-6c, by way of example, and a time ratio of each target adjoining a window 5 is properly selected, setting a timer, and sputtering takes palce in an Ar gas atmosphere, then each layer of target constituent members is stacked on the substrate in order, thus cyclic lamination is carried out at the specified frequency while holding the thickness of one layer down to less than 1mum. Next, it is applied to heat treatment at a temperature of 900 deg.C in oxygen gas flowing at 1l/min. At time of each layer formation, the thickness is controlled whereby a compound superconductive film in the desired composition of L-Br-Cu-O system is securable, thus such a thin film that is high in critical temperature can be easily produced.

Description

【発明の詳細な説明】 [発明の目的コ (産業上の利用分野) 本発明は、化合物超電導薄膜の作製方法に係り、特に、
酸化物系の化合物超電導薄膜の作製方法に関する。
[Detailed Description of the Invention] [Objective of the Invention (Industrial Application Field) The present invention relates to a method for producing a compound superconducting thin film, and in particular,
This invention relates to a method for producing an oxide-based compound superconducting thin film.

(従来の技術) 最近9組成がY−Ba−Cu−0などで表わされる酸化
物系化合物超電導体が注目されている。
(Prior Art) Recently, oxide-based compound superconductors whose composition is represented by Y--Ba--Cu-0, etc., have been attracting attention.

これら、酸化物系化合物超電導体の多くは、臨界温度が
液体窒素温度以上である。このため、冷媒として高価で
扱い難い液体ヘリウムを使用する必要がなく、また冷却
系も大幅に簡略化できるので。
Many of these oxide-based compound superconductors have a critical temperature equal to or higher than the liquid nitrogen temperature. Therefore, there is no need to use liquid helium, which is expensive and difficult to handle, as a refrigerant, and the cooling system can be significantly simplified.

超電導技術を飛躍的に発展させるものと期待されている
It is expected that this will lead to dramatic advances in superconducting technology.

ところで、酸化物系化合物超電導体を集積回路等に応用
するには、この超電導体を対象にした薄膜作製技術の確
立が不可欠である。現在、公表されている唯一の薄膜作
製方法は9組成がY−Ba−Cu−0などで表わされる
ターゲットを用いてAr−0□雰囲気中でスパッタ法で
作製する方法である。しかL、この方法では、ターゲッ
トの組成とは異なる組成の薄膜、つまり望む組成の薄膜
が得られない問題があった。
By the way, in order to apply oxide-based compound superconductors to integrated circuits and the like, it is essential to establish thin film production technology for these superconductors. Currently, the only method for producing a thin film that has been published is a method in which the thin film is produced by sputtering in an Ar-0□ atmosphere using a target whose composition is Y--Ba--Cu-0 or the like. However, this method has the problem that a thin film having a composition different from that of the target, that is, a thin film having a desired composition cannot be obtained.

(発明が解決しようとする問題点) 上述の如く、今まで公表されている方法では。(Problem that the invention attempts to solve) As mentioned above, with the methods that have been published so far.

望む組成の化合物超電導薄膜を作製することが困難であ
った。
It has been difficult to produce a compound superconducting thin film with a desired composition.

そこで本発明は、複雑な工程を伴わずに、しかも望む組
成の化合物超電導薄膜を極めて簡単に作製できる作製方
法を提供することを目的としている。
Therefore, an object of the present invention is to provide a manufacturing method that can extremely easily manufacture a compound superconducting thin film having a desired composition without involving complicated steps.

[発明の構成] (問題点を解決するための手段) 本発明では、基板上に組成が、L−バリウム−銅−酸素
(ただL、L=イットリウム、エルビウム、ジスプロシ
ウム、サマリウム、ガドリニウム、ホルミウム、ネオジ
ム、イッテルビウム、ツリウム、ルテチウムの中から選
ばれた少なくとも1種)からなる酸化物系化合物超電導
薄膜を作製するに当り、基板上に上記り、バリウム、銅
の単体の各層もしくは上記L、バリウム、銅の酸化物の
各層を順次積層形成して所望の厚みの積層体を得た後、
上記積層体を酸素ガス雰囲気中で熱処理して酸化物系化
合物超電導体に変換するようにしている。
[Structure of the Invention] (Means for Solving the Problems) In the present invention, the composition on the substrate is L-barium-copper-oxygen (only L, L=yttrium, erbium, dysprosium, samarium, gadolinium, holmium, In producing an oxide-based compound superconducting thin film consisting of at least one selected from neodymium, ytterbium, thulium, and lutetium, the above-described layers of barium and copper or the above-mentioned L, barium, After sequentially laminating each layer of copper oxide to obtain a laminate of desired thickness,
The laminate is heat-treated in an oxygen gas atmosphere to convert it into an oxide-based compound superconductor.

さらに詳しく述べると、各層の形成は、制御性の面から
スパッタ法で行なうことが望ましい。また、熱処理は、
850〜950℃で、2〜50時間が望ましい。
More specifically, each layer is preferably formed by sputtering from the viewpoint of controllability. In addition, heat treatment
Desirably, the temperature is 850-950°C for 2-50 hours.

(作用) 本発明作製方法では、酸化物系化合物超電導体を構成す
る元素の単体の層もしくはその酸化物の層を順次積層形
成して所望の厚みの積層体を形成L、この積層体を最終
的に酸化物系化合物超電導体に変換するようにしている
ので、上記各層を形成する時にその厚みを制御すること
によって所望とする組成の酸化物系化合物超電導薄膜を
作製することができる。したがって、臨界温度の高い薄
膜を容易に作製することが可能となる。
(Function) In the production method of the present invention, layers of single elements constituting an oxide-based compound superconductor or layers of their oxides are sequentially laminated to form a laminate having a desired thickness L, and this laminate is finalized. Therefore, by controlling the thickness of each of the above layers when forming them, an oxide-based compound superconducting thin film having a desired composition can be produced. Therefore, it becomes possible to easily produce a thin film with a high critical temperature.

(実施例) 第1図および第2図は1本発明作製方法の実施に使用さ
れたスパッタ装置の概略構成を示している。まず、この
スパッタ装置から説明する。
(Example) FIGS. 1 and 2 show a schematic configuration of a sputtering apparatus used to implement the manufacturing method of the present invention. First, this sputtering apparatus will be explained.

第1図中1は真空槽を示L、この真空槽1内には基板2
を支持する基板ホルダー3が配置されている。基板ホル
ダー3に対向する位置には絶縁材で形成された仕切り壁
4が配置されており、この仕切り壁4の前記基板ホルダ
ー3に対向する位置には円形の窓5が形成されている。
In Fig. 1, 1 indicates a vacuum chamber L, and inside this vacuum chamber 1 is a substrate 2.
A substrate holder 3 is arranged to support the substrate. A partition wall 4 made of an insulating material is arranged at a position facing the substrate holder 3, and a circular window 5 is formed at a position of the partition wall 4 facing the substrate holder 3.

そして、仕切り壁4を境にして反乱板ホルダー側には第
2図にも示すように、窓5の径より小径で円板状に形成
されたターゲット6a、6b、6cを保持するターゲッ
トホルダー7a、7b、7c (ただしターゲットホル
ダー70は図示せず。)が同一円周上に所定の開き角で
配置されている。これらターゲットホルダー7a、7b
、7cは絶縁性の支持アーム8を介して回転自在な輔9
の一端部に連結されている。軸9は、その他端側か真空
槽1の壁を気密に貫通して外部へ突出しており、また回
転中心は何れかのターゲットを選択的に窓5に臨ませ得
る位置に設定されている。軸9および支持アーム8の内
部には導体が埋め込まれており、この導体は各ターゲッ
トホルダー7a、’7b、7cに電気的に接続されてい
る。軸9の外部に突出している部分の外周には導体に接
続された導電リング10と歯車11とが装着されている
。導電リング10は摺動接触子を介して電源12に接続
されている。一方、歯車11は歯車13を介してステッ
プモータ14の回転軸に連結されている。そして。
As shown in FIG. 2, on the side of the repulsion plate holder with the partition wall 4 as a boundary, there is a target holder 7a holding disk-shaped targets 6a, 6b, and 6c with a diameter smaller than the diameter of the window 5. , 7b, and 7c (however, the target holder 70 is not shown) are arranged on the same circumference at a predetermined opening angle. These target holders 7a, 7b
, 7c is a support 9 that is rotatable via an insulating support arm 8.
is connected to one end of the The other end of the shaft 9 hermetically penetrates the wall of the vacuum chamber 1 and protrudes to the outside, and the center of rotation is set at a position that allows any target to selectively face the window 5. A conductor is embedded inside the shaft 9 and the support arm 8, and this conductor is electrically connected to each target holder 7a, '7b, 7c. A conductive ring 10 connected to a conductor and a gear 11 are attached to the outer periphery of the portion of the shaft 9 that projects outside. Conductive ring 10 is connected to a power source 12 via sliding contacts. On the other hand, the gear 11 is connected to the rotating shaft of a step motor 14 via a gear 13. and.

ステップモータ14の回転角制御および電源12のオン
、オフ制御は制御器15によって行われる。
The rotation angle control of the step motor 14 and the on/off control of the power supply 12 are performed by a controller 15.

制御器15は、タイマとモータ駆動回路とを組み合ワせ
たもので、動作指令S1が与えられると。
The controller 15 is a combination of a timer and a motor drive circuit, and when an operation command S1 is given.

指定された期間だけ電源12を投入するとともに。In addition to turning on the power supply 12 for a specified period of time.

この期間内において各ターゲット7a、7b。Each target 7a, 7b within this period.

7cが窓5に臨んでいる時間の比が指定された時間比と
なるようにステップモータ14を駆動する。
The step motor 14 is driven so that the ratio of the time that the window 7c faces the window 5 becomes the designated time ratio.

なお、第1図中16は真空槽1内を排気する排気系を示
L、17は真空槽1内に作用ガスとしてのアルゴンガス
を導入する不活性ガス供給系を示L、19は真空計を示
している。
In Fig. 1, 16 indicates an exhaust system L for evacuating the inside of the vacuum chamber 1, 17 indicates an inert gas supply system L for introducing argon gas as a working gas into the vacuum chamber 1, and 19 indicates a vacuum gauge. It shows.

このように構成されたスパッタ装置を用い1次のように
して化合物超電導薄膜を作製した。すなわち、基板2と
して5i02板を用いた。またターゲット6a、6b、
6cとしてイツトリウムの薄い板、バリウムの薄い阪お
よび銅板をそれぞれ用い、これらターゲットが窓5に臨
んでいる時間比が0.5:2:3となるようにタイマを
設定L、10’ torrのアルゴンガス雰囲気中でス
パッタリングを行なって5i02基板上に上記ターゲッ
ト構成部材の層が順次二進するまで積層された合計9層
からなる厚さ2μmの積層体を形成した。次に。
A compound superconducting thin film was produced in a first-order manner using the sputtering apparatus configured as described above. That is, a 5i02 board was used as the substrate 2. Also targets 6a, 6b,
A thin yttrium plate, a thin barium plate, and a copper plate were used as 6c, and the timer was set so that the time ratio of these targets facing window 5 was 0.5:2:3. Sputtering was performed in a gas atmosphere to form a laminate having a thickness of 2 μm and consisting of a total of 9 layers in which the layers of the target component were sequentially stacked until binary on the 5i02 substrate. next.

スパッタ装置から基板を取出L、これを酸素ガスがl、
ff/minの割合で通流する雰囲気中で900 ℃で
2時間に亙って熱処理して薄膜形成工程を終了した。
Take out the substrate from the sputtering equipment, and fill it with oxygen gas.
The thin film forming process was completed by heat treatment at 900° C. for 2 hours in an atmosphere flowing at a rate of ff/min.

このようにして得られた薄膜をX線分光分析したところ
、Y1Ba2 Cu30?−Yの組成式を持つ化合物超
電導体が形成されていgことが確認された。また、上記
のようにして作製された薄膜の超電導特性を調べたとこ
ろ、臨界温度はTc、onloo K 、 Tc、en
d93にであった。一方、比較のために前述した時間比
を1  :l :lに設定して作製された薄膜について
調べたところTc、onは70K 。
X-ray spectroscopic analysis of the thin film thus obtained revealed that Y1Ba2 Cu30? It was confirmed that a compound superconductor having the composition formula -Y was formed. In addition, when the superconducting properties of the thin film produced as described above were investigated, the critical temperature was Tc, onloo K, Tc, en
It was on d93. On the other hand, for comparison, we investigated a thin film prepared by setting the above-mentioned time ratio to 1:l:l, and found that Tc,on was 70K.

Tc、end53にであった。Tc was at end53.

このように上述した作製方法であると、積層体形成時に
各層の厚みを制御でき、この結果9組成をコントロール
できるので、高い臨界温度を示す薄膜を容易に作製する
ことができる。
With the above-described manufacturing method, the thickness of each layer can be controlled during the formation of the laminate, and as a result, the composition can be controlled, so a thin film exhibiting a high critical temperature can be easily manufactured.

なお1本発明は上述した実施例に限定されるものではな
い。すなわち、イツトリウムを、エルビウム、ジスプロ
シウム、サマリウム、ガドリニウム、ホルミウム、ネオ
ジム、イッテルビウム、ツリウム、ルテチウムの中から
選ばれた少なくとも1種に置き代えてもよい。また、こ
れらの酸化物で形成されたターゲットを用いるとともに
バリウムの酸化物および酸化銅で形成されたターゲット
を用いるようにしてもよい。また、積層体を形成すると
き各層の厚みは1組成によって異なるが。
Note that the present invention is not limited to the embodiments described above. That is, yttrium may be replaced with at least one selected from erbium, dysprosium, samarium, gadolinium, holmium, neodymium, ytterbium, thulium, and lutetium. In addition to using targets made of these oxides, targets made of barium oxide and copper oxide may also be used. Furthermore, when forming a laminate, the thickness of each layer varies depending on the composition.

引き続いて行なう熱処理時の酸素の浸透性を考慮に入れ
ると一層の厚みの最大は1μm以下に抑えることが望ま
しく、また最小は20人程度とすることが望ましい。ま
た、スパッタリングを行なうときの雰囲気ガスとしては
、アルゴンガスに限らず。
Taking into account the permeability of oxygen during the subsequent heat treatment, it is desirable that the maximum thickness of each layer be kept to 1 μm or less, and the minimum thickness is preferably about 20. Furthermore, the atmospheric gas used during sputtering is not limited to argon gas.

他の不活性ガスを用いてもよい。また、積層体の形成は
、スパッタ法に限らず真空蒸若法で形成してもよいが、
膜厚制御および時間制御の面からスパッタ法か望ましい
。また、熱処理は、酸素ガス雰囲気中で850〜950
 ℃、 2〜50時間であればよい。
Other inert gases may also be used. Furthermore, the formation of the laminate is not limited to the sputtering method, but may also be formed by the vacuum evaporation method.
Sputtering is preferable from the viewpoint of film thickness control and time control. In addition, heat treatment is performed at 850 to 950 in an oxygen gas atmosphere.
℃ for 2 to 50 hours.

[発明の効果コ 以上述べたように9本発明によれば、酸化物系化合物超
電導体特有の高い臨界温度特性を持つ薄膜を容易に作製
できる化合物超電導薄膜の作製方法を提供できる。
[Effects of the Invention] As described above, according to the present invention, it is possible to provide a method for producing a compound superconducting thin film that can easily produce a thin film having high critical temperature characteristics unique to oxide-based compound superconductors.

【図面の簡単な説明】[Brief explanation of the drawing]

第1図は本発明作製方法の一実施例に用いたスパッタ装
置の概略構成図、第2図は第1図におけるA−A線に沿
って矢印方向に見た図である。 2・・・基板、6a、6b、6c・・・ターゲット。
FIG. 1 is a schematic diagram of a sputtering apparatus used in an embodiment of the manufacturing method of the present invention, and FIG. 2 is a view taken along line A--A in FIG. 1 in the direction of the arrow. 2...Substrate, 6a, 6b, 6c...Target.

Claims (5)

【特許請求の範囲】[Claims] (1)組成がL−バリウム−銅−酸素(ただし、L=イ
ットリウム、エルビウム、ジスプロシウム、サマリウム
、ガドリニウム、ホルミウム、ネオジム、イッテルビウ
ム、ツリウム、ルテチウムの中から選ばれた少なくとも
1種)からなる酸化物系化合物超電導薄膜を作製するに
当り、基板上に上記L、バリウム、銅の単体の各層もし
くは上記L、バリウム、銅の酸化物の各層を順次積層形
成して所望の厚みの積層体を得た後、上記積層体を酸素
ガス雰囲気中で熱処理して酸化物系化合物超電導体に変
換することを特徴とする化合物超電導薄膜の作製方法。
(1) An oxide whose composition is L-barium-copper-oxygen (L = at least one selected from yttrium, erbium, dysprosium, samarium, gadolinium, holmium, neodymium, ytterbium, thulium, and lutetium) In producing a superconducting thin film based on a compound based compound, each of the single layers of L, barium, and copper or each layer of oxide of L, barium, and copper were sequentially laminated on a substrate to obtain a laminate with a desired thickness. A method for producing a compound superconducting thin film, characterized in that the laminate is then heat-treated in an oxygen gas atmosphere to convert it into an oxide-based compound superconductor.
(2)前記積層体は、前記各層を複数巡に亙って積層形
成したものであることを特徴とする特許請求の範囲第1
項記載の化合物超電導薄膜の作製方法。
(2) The laminate is formed by laminating each of the layers in multiple cycles.
A method for producing a compound superconducting thin film as described in .
(3)前記各層の厚みは、20Å〜1μmの範囲である
ことを特徴とする特許請求の範囲第1項記載の化合物超
電導薄膜の作製方法。
(3) The method for producing a compound superconducting thin film according to claim 1, wherein the thickness of each layer is in the range of 20 Å to 1 μm.
(4)前記熱処理は、850〜950℃で2時間以上行
われることを特徴とする特許請求の範囲第1項記載の化
合物超電導薄膜の作製方法。
(4) The method for producing a compound superconducting thin film according to claim 1, wherein the heat treatment is performed at 850 to 950°C for 2 hours or more.
(5)前記各層の形成は、スパッタ法で行われることを
特徴とする特許請求の範囲第1項記載の化合物超電導薄
膜の作製方法。
(5) The method for producing a compound superconducting thin film according to claim 1, wherein each layer is formed by a sputtering method.
JP62124613A 1987-05-21 1987-05-21 Manufacture of compound superconductive thin film Pending JPS63289726A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62124613A JPS63289726A (en) 1987-05-21 1987-05-21 Manufacture of compound superconductive thin film

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62124613A JPS63289726A (en) 1987-05-21 1987-05-21 Manufacture of compound superconductive thin film

Publications (1)

Publication Number Publication Date
JPS63289726A true JPS63289726A (en) 1988-11-28

Family

ID=14889757

Family Applications (1)

Application Number Title Priority Date Filing Date
JP62124613A Pending JPS63289726A (en) 1987-05-21 1987-05-21 Manufacture of compound superconductive thin film

Country Status (1)

Country Link
JP (1) JPS63289726A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01111717A (en) * 1987-10-26 1989-04-28 Nippon Telegr & Teleph Corp <Ntt> Production of oxide superconductive thin film
JPH01152772A (en) * 1987-09-25 1989-06-15 American Teleph & Telegr Co <Att> Manufacture of superconductor oxide layer on substrate
JPH0360405A (en) * 1989-07-25 1991-03-15 Sumitomo Cement Co Ltd Production of oxide superconducting thin film

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH01152772A (en) * 1987-09-25 1989-06-15 American Teleph & Telegr Co <Att> Manufacture of superconductor oxide layer on substrate
JPH01111717A (en) * 1987-10-26 1989-04-28 Nippon Telegr & Teleph Corp <Ntt> Production of oxide superconductive thin film
JPH0360405A (en) * 1989-07-25 1991-03-15 Sumitomo Cement Co Ltd Production of oxide superconducting thin film

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