JPH01246143A - Sputtering target and method for producing superconducting thin film - Google Patents
Sputtering target and method for producing superconducting thin filmInfo
- Publication number
- JPH01246143A JPH01246143A JP63072469A JP7246988A JPH01246143A JP H01246143 A JPH01246143 A JP H01246143A JP 63072469 A JP63072469 A JP 63072469A JP 7246988 A JP7246988 A JP 7246988A JP H01246143 A JPH01246143 A JP H01246143A
- Authority
- JP
- Japan
- Prior art keywords
- thin film
- bismuth
- target
- sputtering target
- calcium
- 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
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
- Inorganic Compounds Of Heavy Metals (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Physical Vapour Deposition (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.
Description
【発明の詳細な説明】
産業上の利用分野
本発明は超電導体の製造に用いるスパッタリングターゲ
ットおよび薄膜の製造方法に関するものである。特に化
合物薄膜超電導体をスパッタリング蒸着により製造する
ために使用されるスパッタリングターゲットに関するも
のである。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a sputtering target used in the production of superconductors and a method for producing thin films. In particular, it relates to sputtering targets used for producing compound thin film superconductors by sputter deposition.
従来の技術
高温超電導体として、Ａ１５型２元系化合物として窒化
ニオブ（ＮｂＮ）やゲルマニウム二オブ（Ｎｂ３Ｇｅ）
などが知られていたが、これらの材料の超電導転移温度
はたかだか２４°にであった。一方、ペロブスカイト系
３元化合物は、さらに高い転移温度が期待され、Ｂａ−
Ｌａ−Ｃｕ−〇系の高温超電導体が提案された［ Ｊ、
Ｇ、 Ｂｅｎｄ。Conventional technology Niobium nitride (NbN) and germanium niobium (Nb3Ge) are used as A15 type binary compounds as high-temperature superconductors.
were known, but the superconducting transition temperature of these materials was at most 24°. On the other hand, perovskite-based ternary compounds are expected to have even higher transition temperatures, and Ba-
A La-Cu-〇-based high-temperature superconductor was proposed [J,
G. Bend.
ｒｚ ａｎｄ Ｋ、Ａ、Ｍｕｌｌｅｒ、 ツアイ
ト シコリフト フェアフィジーク（Ｚｅｔｓｈｒｉｆ
ｔ ｆ ｔｉｒｐｈｙｓｉｋ Ｂ）−Ｃｏｎｄｅｎｓｅ
ｄＭａｔｔｅｒ ６４． １８９−１９３ （１９８６
） ］。rz and K, A, Muller, Zetshrif Fair Physique
t f tirphysik B)-Condense
dMatter 64. 189-193 (1986
) ].
さらに、Ｂ ｉ −３ｒ−Ｃａ−Ｃｕ−０系の材料が１
００に以上の転移温度を示すことも発見された。Furthermore, B i -3r-Ca-Cu-0 type material is 1
It has also been discovered that it exhibits a transition temperature above 0.00.
この種の材料の超電導機構の詳細は明らかではないが、
転移温度が室温以上に高くなる可能性があり、高温超電
導体として従来の２元系化合物より、より有望な特性が
期待される。Although the details of the superconducting mechanism of this type of material are not clear,
The transition temperature can be higher than room temperature, and it is expected to have more promising properties as a high-temperature superconductor than conventional binary compounds.
発明が解決しよとする課題
しかしながら、Ｂ １−５ｒ−Ｃａ−Ｃｕ−０系の材料
は、現在の技術では焼結という過程でしか形成できない
ため、セラミックの粉末あるいはブロックの形状でしか
得られない。一方、この種の材料を実用化する場合、薄
膜状に加工することが強く要望されていが、従来の技術
では、薄膜化は非常に困難とされている。Problems to be Solved by the Invention However, with current technology, B1-5r-Ca-Cu-0-based materials can only be formed through the process of sintering, so they can only be obtained in the form of ceramic powder or blocks. do not have. On the other hand, when this type of material is to be put to practical use, there is a strong demand for processing it into a thin film, but it is considered extremely difficult to form a thin film using conventional techniques.
本発明者らは、この種の材料の薄膜がイオンプロセスに
より付着させると、薄膜状の高温超電体が形成されるこ
とを発見し、これにもとづいて薄膜超電導体を製造する
に際し、好適なスパッタリングターゲットおよびこれを
用いた製造方法を提供することを目的とする。The present inventors have discovered that when a thin film of this kind of material is deposited by an ion process, a thin film-like high-temperature superconductor is formed, and based on this, a suitable method for manufacturing a thin film superconductor has been found. An object of the present invention is to provide a sputtering target and a manufacturing method using the same.
課題を解決するための手段
本発明のスパッタリングターゲットおよび超電導薄膜の
製造方法は、主成分が少なくともビスマス、ｊｌｉｌ、
カルシウム、アルカリ土類を含む酸化物から構成される
ターゲットを用いることを特徴とするものである。ここ
でアルカリ土類は、ＩＩａ族元素のうちの少なくとも一
種あるいは二種以上の元素を示す。Means for Solving the Problems The sputtering target and the method for producing a superconducting thin film of the present invention are characterized in that the main components are at least bismuth, jlil,
This method is characterized by using a target composed of oxides containing calcium and alkaline earth metals. Here, alkaline earth refers to at least one or two or more elements of Group IIa elements.
さらに、本発明のターゲットとして、これにて作製され
る薄膜の組成よりもビスマスとカルシウムを過剰に含む
ものを用いることにより、良好な超電導特性を容易に得
ることが可能となる。Furthermore, by using a target of the present invention that contains more bismuth and calcium than the composition of the thin film produced using this target, it becomes possible to easily obtain good superconducting properties.
作用
本発明のスパッタリングターゲットを用いて形成される
薄膜超電導体の基本構成は、基体表面に主成分がビスマ
ス、鋼、カルシウム、アルカリ土類の酸化物被膜を付着
させた構造を特徴としている。本発明者らはこの種の超
電導体は、基体上に、主成分がビスマス、鋼、カルシウ
ム、アルカリ土類からなる複合酸化物被膜を本発明のス
パッタリングターゲットを用いたスパッタリング蒸着と
いうプロセスで付着させ、場合によっては熱処理するこ
とにより形成される。Function The basic structure of the thin film superconductor formed using the sputtering target of the present invention is characterized by a structure in which an oxide film containing bismuth, steel, calcium, or alkaline earth as the main components is adhered to the surface of the substrate. The present inventors have developed this type of superconductor by depositing a composite oxide film whose main components are bismuth, steel, calcium, and alkaline earth on a substrate by a process called sputtering vapor deposition using the sputtering target of the present invention. , in some cases by heat treatment.
そして、本発明者らは、作製を行う薄膜の組成よりもビ
スマスとカルシウムを過剰に含むターゲットを用いれば
、薄膜の組成を良好に所望のものに調整できるというこ
とを合わせて発見した。The present inventors also discovered that by using a target containing bismuth and calcium in excess of the composition of the thin film to be fabricated, the composition of the thin film can be favorably adjusted to a desired value.
したがって、本発明のターゲットを、１００に以上の転
移温度を持つとされるＢ１−５ｒ−Ｃａ−Ｃｕ−○系の
材料の薄膜作製に応用することにより、高品質の超電導
薄膜材料が実現され非常に有効である。Therefore, by applying the target of the present invention to the production of thin films of B1-5r-Ca-Cu-○ series materials, which are said to have a transition temperature of 100 or higher, high-quality superconducting thin film materials can be realized. It is effective for
本発明のターゲットを用いて形成される薄膜超電導体は
、薄膜化しており、薄膜化は超電導体の素材を原子状態
という極微粒子に分解してから基体上に堆積させるから
、形成された超電導体の組成は本質的に、従来の焼結体
に比べて均質である。したがって非常に高精度の超電導
体が本発明のターゲットを用いて実現される。The thin film superconductor formed using the target of the present invention is made into a thin film, and the thin film is made by decomposing the superconductor material into ultrafine particles called atomic states and then depositing them on the substrate. The composition is essentially homogeneous compared to conventional sintered bodies. Superconductors of very high precision are therefore realized using the targets of the invention.
以下本発明の内容をさらに深く理解されるために、さら
に具体的な実施例を示す。In order to further understand the content of the present invention, more specific examples will be shown below.
（実施例）
第２図に本発明の実施例を示す。第２図は高周波ブレナ
ーマグネトロンスパッタの実験概略図であり、２１は基
体、２２は粉末のＢ１−３ｒ−Ｃａ−Ｃｕ−０ターゲツ
ト、２３はステンレス製のターゲット粉末受皿、２４は
磁界発生用マグネットである。本実施例では１、酸化マ
グネシウム単結晶（１００）面を基体２１として用い、
ターゲットは空気中で２〜１０時間、８５０℃〜９５０
℃で焼結して、さらに粉末にしたＢ１−３ｒ−Ｃａ−Ｃ
ｕ−０ターゲツトをＡｒ、０２ガス雰囲気でスパッタリ
ング蒸着して、基体２１上に結晶性のＢ１−８ｒ−Ｃａ
−Ｃｕ−Ｏ被膜２５として付着させ層状構造を形成した
。(Example) FIG. 2 shows an example of the present invention. Figure 2 is a schematic diagram of a high-frequency Brenner magnetron sputtering experiment, in which 21 is a substrate, 22 is a powdered B1-3r-Ca-Cu-0 target, 23 is a stainless steel target powder tray, and 24 is a magnet for generating a magnetic field. be. In this example, 1, a magnesium oxide single crystal (100) plane is used as the substrate 21,
The target was heated to 850°C to 950°C for 2 to 10 hours in air.
B1-3r-Ca-C sintered at °C and further powdered
Crystalline B1-8r-Ca is deposited on the substrate 21 by sputtering a u-0 target in an Ar and O2 gas atmosphere.
-Cu-O coating 25 was deposited to form a layered structure.
この場合、スパッタガス圧力は０．５Ｐａ、スパッタリ
ング電力１５０Ｗ、スパッタリング時間１時間、被膜の
膜Ｊ！２０．５μｍ、基体温度７００ ’Ｃであった。In this case, the sputtering gas pressure was 0.5 Pa, the sputtering power was 150 W, the sputtering time was 1 hour, and the film J! The thickness was 20.5 μm, and the substrate temperature was 700′C.
形成された層状構造をさらに酸素中で８８０℃１時間熱
処理した。The formed layered structure was further heat-treated at 880° C. for 1 hour in oxygen.
Ｂ１−５ｒ−Ｃａ−Ｃｕ−０化合物の金属元素比率は、
Ｂｉ：Ｓｒ：Ｃａ：Ｃｕニー１・１：ｌ・２の近傍のと
ころが臨界温度の高い良好な超電導体となるといわれて
いる。本発明者らはターゲット組成を種々変化させて、
−１−、記の手法で薄膜作製を行った。その結果、所望
の組成よりもビスマスおよびカルシウムが過剰に入った
Ｑ、４＜−ｍ−＜１
Ｓ ｒ 」−Ｃｕ
（ここで、ＡはＢｉおよびＣａである）のターゲットを
用いた場合に、薄膜の組成は
一一一一−−□夕０．３
Ｓｒ十Ｃｕ
となり、良好な超電導特性が得られることを確認した。The metal element ratio of the B1-5r-Ca-Cu-0 compound is
It is said that the area near the Bi:Sr:Ca:Cu knee 1.1:l.2 becomes a good superconductor with a high critical temperature. The present inventors variously changed the target composition,
-1-, a thin film was prepared by the method described below. As a result, when using a target of Q,4<-m-<1 S r ''-Cu (where A is Bi and Ca) containing excess bismuth and calcium than the desired composition, The composition of the thin film was 1111--0.3 Sr+Cu, and it was confirmed that good superconducting properties were obtained.
第１図に薄膜の抵抗の温度依存性を示す。上記範囲のビ
スマスおよびカルシウム量を持つターゲットを用いて薄
膜を作製した場合、特性曲線１１のように零抵抗温度が
８０に以上という良好な超電導特性の薄膜が得られた。Figure 1 shows the temperature dependence of the resistance of the thin film. When a thin film was produced using a target having bismuth and calcium contents in the above ranges, a thin film with good superconducting properties with a zero resistance temperature of 80 or higher was obtained as shown in characteristic curve 11.
また特に０．５≦□−≦０．６
Ｓｒ＋Ｃｕ
というターゲットを用いた場合においては、一部が超電
導状態になっていると考えられるオンセット温度１２０
Ｋを持つ特性１２が観測された。In addition, especially when using a target of 0.5□-≦0.6 Sr+Cu, the onset temperature is 120, which is considered to be partially in a superconducting state.
Characteristic 12 with K was observed.
さらに、
Ｃａ
というターゲットを用いた場合、オンセット温度１２０
Ｋ、オンセット温度１００に以上の特性１３が観測され
、より高い温度で超電導を示す薄膜材料の作製に非常に
有効であると考えられる。Furthermore, when a target of Ca is used, the onset temperature is 120
The above characteristic 13 was observed at K and onset temperature of 100, and it is considered to be very effective for producing thin film materials that exhibit superconductivity at higher temperatures.
この場合、ターゲットの構成は焼結体例えば円板、円筒
などが有用である。しかし、必ずしも成型品である必要
はな（、例えば、粉末又は粒状あるいはチャック状であ
ってもよい。In this case, it is useful for the target to have a sintered body such as a disk or a cylinder. However, it does not necessarily have to be a molded product (for example, it may be in the form of powder, granules, or zipper).
特に本発明にかかる粉末ターゲットは成型の必要がない
上、スパッタ中に連続的に供給できる特長があり、この
種の超電導体の製造に一層有効である。In particular, the powder target according to the present invention does not require molding and can be continuously supplied during sputtering, making it more effective for producing this type of superconductor.
発明の効果
本発明のスパッタリング用ターゲットを用いて超電導薄
膜を形成するに際し、ターゲットを粉末あるいは粒状等
にすることが可能で、超電導薄膜形成に特に要求される
組成の調整が容易でかつ均一な材料組成のターゲットを
作成することが出来、信頼性の高い安定な超電導体を再
現性良く得ることが可能となる。したがって、本発明に
かかるターゲットにより作製される超電導体は、超電導
体を安定な薄膜として形成することが可能となる。すな
わち、均質で組成が最適に制御されたターゲットを用い
、超電導体の素材を原子状態という極微粒子に分解して
から、基体１−に堆積させるため、形成された超電導体
の組成は本質的に、従来の焼結体に比べて均質である。Effects of the Invention When forming a superconducting thin film using the sputtering target of the present invention, the target can be made into powder or granules, and the composition can be easily adjusted and the material is uniform, which is particularly required for forming a superconducting thin film. It is possible to create a target composition, and it becomes possible to obtain a highly reliable and stable superconductor with good reproducibility. Therefore, the superconductor produced using the target according to the present invention can be formed as a stable thin film. In other words, using a homogeneous target with an optimally controlled composition, the superconductor material is decomposed into ultrafine particles in the atomic state and then deposited on the substrate 1-, so the composition of the formed superconductor is essentially , more homogeneous than conventional sintered bodies.
したがって、非常に高精度の超電導体が本発明で実現さ
れる。Therefore, a superconductor with very high precision is realized with the present invention.
特に高臨界温度の期待の高いＢ１−５ｒ−Ｃａ−Ｃｕ
−０系の超電導薄膜作製に際し、良好な特性を持つ薄膜
製造に適したものであり、本発明の工業的価値は高い。B1-5r-Ca-Cu, which is expected to have a particularly high critical temperature
The present invention is suitable for producing a thin film with good characteristics when producing a -0-based superconducting thin film, and the industrial value of the present invention is high.
第１図は本発明を用いて形成された薄膜超電導体の基本
特性図、第２図は本発明の薄膜超電導体作製の実験概略
図である。
２１・・・基体、２２・・・粉末ターゲット、２３・・
・ターゲット受皿、２４・・・磁界発生用マグネット、
２５ ・・・Ｂ ｉ −３ｒ−Ｃａ−Ｃｕ−ＯＷＪｍ。FIG. 1 is a basic characteristic diagram of a thin film superconductor formed using the present invention, and FIG. 2 is a schematic diagram of an experiment for producing the thin film superconductor of the present invention. 21...Base body, 22...Powder target, 23...
・Target saucer, 24... Magnet for magnetic field generation,
25...B i -3r-Ca-Cu-OWJm.
Claims (5)
ｕ）カルシウム（Ｃａ）およびアルカリ土類（IIａ族）
を含む酸化物から構成され、作製を行う薄膜の組成より
ビスマスとカルシウムを過剰に含んだことを特徴とする
スパッタリング用ターゲット。ここでアルカリ土類は、
IIａ族元素のうちのすくなくとも一種あるいは二種以上
の元素を示す。(1) The main components are at least bismuth (Bi) and copper (C).
u) Calcium (Ca) and alkaline earths (group IIa)
1. A sputtering target characterized in that it is composed of an oxide containing , and contains bismuth and calcium in excess compared to the composition of the thin film to be fabricated. Here, the alkaline earth is
Indicates at least one or more elements of group IIa elements.
囲第１項記載のスパッタリング用ターゲット。(2) The sputtering target according to claim 1, characterized in that it is made of a sintered body.
徴とする特許請求の範囲第１項記載のスパッタリング用
ターゲット。(3) The sputtering target according to claim 1, wherein the sintered body is in the form of powder or particles.
ことを特徴とする特許請求の範囲第１項記載のスパッタ
リング用ターゲット。(4) The sputtering target according to claim 1, wherein the alkaline earth metal is strontium (Sr).
アルカリ土類を含む酸化物からなるターゲットを用い、
基体上にスパッタリング法にて少なくともビスマス、銅
、アルカリ土類を含む酸化物薄膜を形成する際し、前記
ターゲットのビスマスとカルシウムの組成比を、前記薄
膜中のビスマスの組成比よりも大きくすることを特徴と
する超電導薄膜の製造方法。(5) The main components are at least bismuth, copper, calcium,
Using a target made of oxides containing alkaline earth elements,
When forming an oxide thin film containing at least bismuth, copper, and alkaline earth metals on a substrate by sputtering, the composition ratio of bismuth to calcium in the target is made larger than the composition ratio of bismuth in the thin film. A method for producing a superconducting thin film characterized by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63072469A JPH01246143A (en) | 1988-03-25 | 1988-03-25 | Sputtering target and method for producing superconducting thin film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63072469A JPH01246143A (en) | 1988-03-25 | 1988-03-25 | Sputtering target and method for producing superconducting thin film |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01246143A true JPH01246143A (en) | 1989-10-02 |
Family
ID=13490202
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63072469A Pending JPH01246143A (en) | 1988-03-25 | 1988-03-25 | Sputtering target and method for producing superconducting thin film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01246143A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02129009A (en) * | 1988-11-04 | 1990-05-17 | Mitsubishi Metal Corp | Production of oxide superconductor |
-
1988
- 1988-03-25 JP JP63072469A patent/JPH01246143A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02129009A (en) * | 1988-11-04 | 1990-05-17 | Mitsubishi Metal Corp | Production of oxide superconductor |
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