JPH0337103A - Production of oxide superconducting thin film and apparatus therefor - Google Patents

Production of oxide superconducting thin film and apparatus therefor

Info

Publication number
JPH0337103A
JPH0337103A JP1171303A JP17130389A JPH0337103A JP H0337103 A JPH0337103 A JP H0337103A JP 1171303 A JP1171303 A JP 1171303A JP 17130389 A JP17130389 A JP 17130389A JP H0337103 A JPH0337103 A JP H0337103A
Authority
JP
Japan
Prior art keywords
thin film
superconductor
particles
ion beam
oxide superconductor
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
JP1171303A
Other languages
Japanese (ja)
Inventor
Takeshi Morimoto
剛 森本
Toshiya Matsubara
俊哉 松原
Shinichi Ohashi
大橋 信一
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.)
AGC Inc
Original Assignee
Asahi Glass Co Ltd
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 Asahi Glass Co Ltd filed Critical Asahi Glass Co Ltd
Priority to JP1171303A priority Critical patent/JPH0337103A/en
Publication of JPH0337103A publication Critical patent/JPH0337103A/en
Pending legal-status Critical Current

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  • Physical Vapour Deposition (AREA)
  • Superconductor Devices And Manufacturing Methods Thereof (AREA)
  • Superconductors And Manufacturing Methods Therefor (AREA)
  • Oxygen, Ozone, And Oxides In General (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

PURPOSE:To enhance pin fixing effect and retain high critical current density even in state applying a magnetic field by introducing non-superconducting particles from a cluster ion beam device in a process forming an oxide superconducting thin film. CONSTITUTION:A thin film having a prescribed thickness is formed on a substrate 2 by controlling deposition rate of Y, Ba, Cu, etc., which are raw materials from Knudsen cells so as to have prescribed composition. Shutters of Knudsen cells 4 are shut and a cluster of noble metal such as gold is irradiated using a cluster ion beam device 5 to introduce non-superconducting particles into a thin film. The procedure is repeated to afford prescribed film thickness. Thereby the superconducting thin film in which non-superconducting particles are dispersed is readily obtained.

Description

【発明の詳細な説明】 [産業上の利用分野1 本発明は酸化物超電導体薄膜の製造方法および製造装置
に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application 1] The present invention relates to a method and apparatus for producing an oxide superconductor thin film.

[従来の技術] 従来、銅を含み臨界温度が液体窒素温度以上である酸化
物超電導体の薄膜は1種々の物理蒸着法(スパッタ法、
蒸着法、レーザービーム蒸着法など)や、CVD法など
で製造されてきた。方法の如何によらず、製造条件を適
正に選べば、液体窒素温度、0磁場下では100万A 
/cab”以上の臨界電流密度を有する薄膜が得られる
ようになってきている。
[Prior Art] Conventionally, thin films of oxide superconductors containing copper and having a critical temperature higher than the liquid nitrogen temperature have been produced using various physical vapor deposition methods (sputtering, sputtering, etc.).
It has been manufactured using methods such as evaporation method, laser beam evaporation method, etc.), CVD method, etc. Regardless of the method, if the manufacturing conditions are selected appropriately, it can produce up to 1 million A at liquid nitrogen temperature and zero magnetic field.
It has become possible to obtain thin films having critical current densities greater than /cab''.

【発明が解決しようとする課題] しかし、超電導マグネットなどの応用には数テスラ以上
の強い磁場下で10万A /cm”以上の電流を流せる
材料が求められており、これまで得られた薄膜は磁場下
、特に、Cu−0面に垂直に磁場を印加した場合に大き
な電流が流せないことが問題となっている。この原因は
、酸化物超電導体の単結晶を用いた実験結果から、磁場
下で電流の印加による磁束の移動を十分に抑制できてい
ないためと考えられている。
[Problems to be solved by the invention] However, for applications such as superconducting magnets, materials that can flow a current of 100,000 A/cm or more under a strong magnetic field of several Tesla or more are required, and the thin films obtained so far The problem is that a large current cannot flow under a magnetic field, especially when a magnetic field is applied perpendicular to the Cu-0 plane.The reason for this is based on experimental results using a single crystal of an oxide superconductor. This is thought to be due to the inability to sufficiently suppress the movement of magnetic flux due to the application of current under a magnetic field.

磁場下で磁束の移動を抑制するためには適切なビン止め
中心を超電導体内に導入することが必要である。ビン止
め中心としては、非超電導体の微粒子や、薄膜では電流
方向に平行な微少なりラックなどが作用すると考えられ
ているが、そのようなビン止め中心を有する薄膜を形成
する方法は未だ確立されていない。
In order to suppress the movement of magnetic flux under a magnetic field, it is necessary to introduce a suitable binning center into the superconductor. It is thought that fine particles of non-superconductors or small racks parallel to the current direction in thin films act as the binding center, but a method for forming a thin film with such a binding center has not yet been established. Not yet.

[課題を解決するための手段] 本発明は、薄膜内にビン止め効果を有する非超電導体の
微粒子が分散した酸化物超電導体薄膜を得ることを目的
とするものであり、酸化物超電導体薄膜を基体上に形成
する過程で、クラスターイオンビーム装置により非超電
導体粒子を該酸化物超電導体薄膜中に導入することを特
徴とする非超電導体粒子が分散した酸化物超電導体薄膜
の製造方法を提供するものである。
[Means for Solving the Problems] The present invention aims to obtain an oxide superconductor thin film in which fine particles of a non-superconductor having a bottling effect are dispersed. A method for producing an oxide superconductor thin film in which non-superconductor particles are dispersed, the method comprising: introducing non-superconductor particles into the oxide superconductor thin film using a cluster ion beam device during the process of forming the oxide superconductor thin film on a substrate. This is what we provide.

本発明においては、クラスターイオンビーム装置を用い
て非超電導体物質を酸化物超電導体薄膜中に導入する際
には、非超電導体物質を粒子状で付着させる必要がある
。高いビン止め効果を得るために、粒子の直径は100
〜500人であることが好ましい、また、非超電導体粒
子の含有量は、10〜50体積%が好ましい。含有量が
10体積%未滴の場合は、ビン止め効果が不十分になる
恐れがあるので好ましくない。含有量が50体積%を超
える場合は、超電導体の体積が少なくなり薄膜の臨界電
流密度が小さくなる恐れがあるので好ましくない。
In the present invention, when introducing a non-superconductor substance into an oxide superconductor thin film using a cluster ion beam device, it is necessary to deposit the non-superconductor substance in the form of particles. In order to obtain a high bottling effect, the diameter of the particles is 100
The number of non-superconductor particles is preferably 10 to 50% by volume. If the content is less than 10% by volume, it is not preferable because the bottle-stopping effect may become insufficient. If the content exceeds 50% by volume, it is not preferable because the volume of the superconductor may decrease and the critical current density of the thin film may decrease.

本発明においては、この非超電導体粒子を酸化物超電導
体薄膜中に均一に分散させるために以下のような方法を
採用するのが好ましい。例えば、酸化物超電導体薄膜の
形成と非超電導体粒子の導入を同時に行なって、薄膜が
成長するに従い非超電導体粒子を薄膜中に分散させる方
法は、均質な薄膜が得られやすいので好ましい。あるい
は酸化物超電導体薄膜の形成を複数回に分けて行ない、
酸化物超電導体薄膜形成の間に非超電導体粒子を導入す
る方法も採用できる。この方法では、酸化物超電導体薄
膜の成長を途中で止めて、この成長途中の薄膜上に非超
電導体を粒子状で付着させ、さらにその上に超電導体の
薄膜を形成することにより、あるいはさらにこの操作を
繰り返すことによって非超電導体粒子の分散した超電導
体薄膜を得る。この際、非超電導体が連続した膜状にな
らないように付着条件を選択する必要がある。
In the present invention, it is preferable to employ the following method in order to uniformly disperse the non-superconductor particles in the oxide superconductor thin film. For example, a method in which the formation of an oxide superconductor thin film and the introduction of non-superconductor particles are performed simultaneously, and the non-superconductor particles are dispersed in the thin film as the thin film grows, is preferred because a homogeneous thin film is likely to be obtained. Alternatively, the oxide superconductor thin film is formed in multiple steps,
A method of introducing non-superconductor particles during the formation of an oxide superconductor thin film can also be adopted. In this method, the growth of an oxide superconductor thin film is stopped midway, a non-superconductor is deposited in the form of particles on this thin film that is still growing, and a superconductor thin film is further formed on top of the non-superconductor, or By repeating this operation, a superconductor thin film in which non-superconductor particles are dispersed is obtained. At this time, it is necessary to select the deposition conditions so that the non-superconductor does not form a continuous film.

非超電導体物質としては、特に限定されず種々の物質を
用いつるが、超電導体と反応しないものであることが好
ましい0例えば、銀や、金などの貴金属が好ましく用い
られる。
The non-superconducting substance is not particularly limited and various substances can be used, but it is preferable that it does not react with the superconductor. For example, noble metals such as silver and gold are preferably used.

本発明の製造方法は、超電導体の構成元素の蒸発装置と
非超電導体のクラスターイオンビーム装置とを同一真空
容器内に設置した装置を用いてこれを行なうことができ
る。超電導体の構成元素の蒸発装置は、特に限定されず
種々のものをmいることができ、例えば、クヌッセンセ
ル等が使用できる。非超電導体のクラスターイオンビー
ム装置も、特に限定されず、公知の装置を適宜使用する
ことができる・、酸化物超電導体薄膜の形成を複数回に
分けて行なう場合は、超電導体の構成元素の蒸発装置と
非超電導体のクラスターイオンビーム装置のそれぞれに
、シャッターが設けられていることが好ましい。真空容
器については、内部の雰囲気を制御できるものが好まし
い。
The manufacturing method of the present invention can be carried out using an apparatus in which an evaporator for constituent elements of a superconductor and a cluster ion beam apparatus for a non-superconductor are installed in the same vacuum vessel. The device for evaporating constituent elements of the superconductor is not particularly limited, and various devices can be used, such as a Knudsen cell. The cluster ion beam device for non-superconductors is not particularly limited, and any known device can be used as appropriate.If the oxide superconductor thin film is formed in multiple steps, the constituent elements of the superconductor may be Preferably, each of the evaporator and the non-superconductor cluster ion beam device is provided with a shutter. As for the vacuum container, one in which the internal atmosphere can be controlled is preferable.

【実施例] 真空容器内に3基のクヌッセンセル4と1基のクラスタ
ーイオンビーム装置5とを設置し、Y、Ba、Cu金属
を原料として3基のクヌッセンセル4に充填し、金をク
ラスターイオンビーム装置5の原料として用いた。クラ
スターイオンビーム装置には、加速電極6と熱電子ビー
ム発生器7が設けられており、熱電子ビーム発生器7か
らの熱電子により金のクラスターをイオン化し、これを
加速電極6により加速して基板に付着させる。基板2に
(Zoo)面を鏡面研磨したMgO単結晶を用い、基板
温度をヒーター1により700’Cに保って成膜した。
[Example] Three Knudsen cells 4 and one cluster ion beam device 5 are installed in a vacuum container, and the three Knudsen cells 4 are filled with Y, Ba, and Cu metals as raw materials, and gold is added to the cluster. It was used as a raw material for the ion beam device 5. The cluster ion beam device is provided with an accelerating electrode 6 and a thermionic beam generator 7, and gold clusters are ionized by thermionic electrons from the thermionic beam generator 7, which are then accelerated by the accelerating electrode 6. Attach it to the substrate. A MgO single crystal whose (Zoo) plane was mirror-polished was used as the substrate 2, and the substrate temperature was maintained at 700'C by the heater 1 to form a film.

Fli、膜時に、基板近傍の酸素の圧力がio−”丁o
rr程度になるよう酸素をノズル3により導入した。
During film formation, the oxygen pressure near the substrate is io-”
Oxygen was introduced through the nozzle 3 so that the temperature was about rr.

まず、クラスターイオンビーム装置5のシャッターを閉
じた状態で、クヌッセンセル4によりY:Ba:Cu=
l :2:3の組成になるよう蒸着速度を調節し、10
00人の厚さの薄膜を形成し、た。その後、クヌッセン
セル4のシャッターを閉じ、クラスターイオンビーム装
置5を用い30秒間金のクラスターを照射した。以上の
手順を繰り返し、全体の膜厚を1μmとした。X線回折
装置により、得られた薄膜はC軸が基板面に垂直である
ことが確認できた。この薄膜を、TEMにより観察した
ところ、膜中に直径約300人の粒子が約30体積%存
在し7ていた。
First, with the shutter of the cluster ion beam device 5 closed, Y:Ba:Cu=
The deposition rate was adjusted so that the composition was 1:2:3.
A thin film with a thickness of 0.000 was formed. Thereafter, the shutter of the Knudsen cell 4 was closed, and the cluster ion beam device 5 was used to irradiate the gold cluster for 30 seconds. The above procedure was repeated until the total film thickness was 1 μm. Using an X-ray diffraction apparatus, it was confirmed that the C-axis of the obtained thin film was perpendicular to the substrate surface. When this thin film was observed by TEM, it was found that about 30% by volume of particles with a diameter of about 300 particles were present in the film.

得られた薄膜を幅0.3mm、長さ50μmの大きさに
乾式エッチし、試料を液体窒素に浸漬した状態で直流4
端子法により臨界電流、密度を測定したところ、磁場を
印加しない状態で2XlO’A/Cll1t、c軸と平
行にlテスラの磁場を印加]5.た状態でI X l 
O’ Arcs2であった。
The obtained thin film was dry etched to a size of 0.3 mm in width and 50 μm in length, and the sample was immersed in liquid nitrogen and subjected to direct current
When the critical current and density were measured by the terminal method, a magnetic field of 2XlO'A/Clllt was applied parallel to the c-axis without applying a magnetic field]5. I
It was O' Arcs2.

[比較例] 実施例と同・じ装置を用いて、クラスターイオンビーム
装置を用いないこと以外は実施例と同様にして、酸化物
超電導体のみを蒸着して薄膜を得た。実施例ヒ同様、得
られた薄膜のC軸は基板面に垂直であった。実施例と同
様にして臨界電流密度を測定したところ、磁場を印加し
ない状態で5 X 10’ A/cl11”、lテスラ
の磁場を印加した状態で1Xlo’A/c−であった。
[Comparative Example] A thin film was obtained by depositing only an oxide superconductor in the same manner as in the example except that the cluster ion beam device was not used using the same apparatus as in the example. As in Example A, the C-axis of the obtained thin film was perpendicular to the substrate surface. When the critical current density was measured in the same manner as in the example, it was 5×10′ A/cl11” without applying a magnetic field, and 1×lo′ A/c− with a magnetic field of 1 Tesla applied.

[発明の効果〕 本発明方法によると、ビン止め効果が高く磁場を印加し
た状態においても高い臨界電流密度を有する超電導体薄
膜が得られる。
[Effects of the Invention] According to the method of the present invention, a superconductor thin film having a high bottle-stopping effect and a high critical current density even when a magnetic field is applied can be obtained.

本発明装置によると、非超電導体粒子が分散した超電導
体薄膜が容易に得られる。
According to the apparatus of the present invention, a superconductor thin film in which non-superconductor particles are dispersed can be easily obtained.

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

図1は、本発明の実施例に用いた薄膜製造装置の構成を
示す説明図である。 l:ヒーター    2:基板 3:ノズル     4:クヌッセンセル5 : クラスターイオンビーム装置 6 : 加速電極 7 : 熱電子ビーム発生器 ゝ−5 第 ! 砧
FIG. 1 is an explanatory diagram showing the configuration of a thin film manufacturing apparatus used in an example of the present invention. 1: Heater 2: Substrate 3: Nozzle 4: Knudsen cell 5: Cluster ion beam device 6: Accelerating electrode 7: Thermionic beam generator -5th! Kinuta

Claims (5)

【特許請求の範囲】[Claims] (1)酸化物超電導体薄膜を基体上に形成する過程で、
クラスターイオンビーム装置により非超電導体粒子を該
酸化物超電導体薄膜中に導入することを特徴とする非超
電導体粒子が分散した酸化物超電導体薄膜の製造方法。
(1) In the process of forming an oxide superconductor thin film on a substrate,
A method for producing an oxide superconductor thin film in which non-superconductor particles are dispersed, the method comprising introducing non-superconductor particles into the oxide superconductor thin film using a cluster ion beam device.
(2)酸化物超電導体薄膜の形成と同時に、非超電導体
粒子を導入する請求項1の製造方法。
(2) The manufacturing method according to claim 1, wherein the non-superconductor particles are introduced simultaneously with the formation of the oxide superconductor thin film.
(3)酸化物超電導体薄膜の形成を複数回に分けて行な
い、酸化物超電導体薄膜形成の間に非超電導体粒子を導
入する請求項1の製造方法。
(3) The manufacturing method according to claim 1, wherein the oxide superconductor thin film is formed in multiple steps, and the non-superconductor particles are introduced during the oxide superconductor thin film formation.
(4)非超電導体粒子が、貴金属である請求項1〜3い
ずれか一の製造方法。
(4) The manufacturing method according to any one of claims 1 to 3, wherein the non-superconducting particles are a noble metal.
(5)酸化物超電導体の構成元素の蒸発装置と非超電導
体のクラスターイオンビーム装置とを同一真空容器内に
有することを特徴とする酸化物超電導体薄膜の製造装置
(5) An apparatus for producing an oxide superconductor thin film, comprising an evaporator for constituent elements of the oxide superconductor and a cluster ion beam apparatus for a non-superconductor in the same vacuum vessel.
JP1171303A 1989-07-04 1989-07-04 Production of oxide superconducting thin film and apparatus therefor Pending JPH0337103A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1171303A JPH0337103A (en) 1989-07-04 1989-07-04 Production of oxide superconducting thin film and apparatus therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1171303A JPH0337103A (en) 1989-07-04 1989-07-04 Production of oxide superconducting thin film and apparatus therefor

Publications (1)

Publication Number Publication Date
JPH0337103A true JPH0337103A (en) 1991-02-18

Family

ID=15920783

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1171303A Pending JPH0337103A (en) 1989-07-04 1989-07-04 Production of oxide superconducting thin film and apparatus therefor

Country Status (1)

Country Link
JP (1) JPH0337103A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009051082A1 (en) * 2007-10-19 2009-04-23 Kagoshima University Superconductive material

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2009051082A1 (en) * 2007-10-19 2009-04-23 Kagoshima University Superconductive material
JP2009104813A (en) * 2007-10-19 2009-05-14 Kagoshima Univ Superconducting material

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