JPH0717480B2 - Method for manufacturing high temperature superconductor film - Google Patents
Method for manufacturing high temperature superconductor filmInfo
- Publication number
- JPH0717480B2 JPH0717480B2 JP62148389A JP14838987A JPH0717480B2 JP H0717480 B2 JPH0717480 B2 JP H0717480B2 JP 62148389 A JP62148389 A JP 62148389A JP 14838987 A JP14838987 A JP 14838987A JP H0717480 B2 JPH0717480 B2 JP H0717480B2
- Authority
- JP
- Japan
- Prior art keywords
- temperature superconductor
- high temperature
- film
- sputtering
- superconductor film
- 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.)
- Expired - Lifetime
Links
- 239000002887 superconductor Substances 0.000 title claims description 17
- 238000004519 manufacturing process Methods 0.000 title claims description 9
- 238000000034 method Methods 0.000 title claims description 5
- 238000004544 sputter deposition Methods 0.000 claims description 17
- 239000013077 target material Substances 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 7
- 229910002480 Cu-O Inorganic materials 0.000 claims description 4
- 229910009203 Y-Ba-Cu-O Inorganic materials 0.000 claims description 2
- 239000004020 conductor Substances 0.000 claims 1
- 239000012528 membrane Substances 0.000 claims 1
- 239000010408 film Substances 0.000 description 13
- 239000013078 crystal Substances 0.000 description 10
- 239000000758 substrate Substances 0.000 description 4
- 239000010409 thin film Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000000126 substance Substances 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
- Inorganic Compounds Of Heavy Metals (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Physical Vapour Deposition (AREA)
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、高温超伝導体膜の製造方法に関するものであ
る。TECHNICAL FIELD The present invention relates to a method for producing a high temperature superconductor film.
薄膜作製手段として一般によく用いられるスパッタリン
グ法は超伝導体薄膜の作製にも使用されている。従来の
スパッタリング装置は、図に示すように真空槽(1)、下
地基材(2)、ターゲット材(3)および電源(4)から構成さ
れている。この装置による薄膜の製造方法は、まず10-6
Torr以下に真空排気後、ArもしくはHeなどの不活性ガス
を10-3〜10-2Torrの雰囲気にコントロールしてグロー放
電を行わせ、陰極側のターゲット材を不活性ガスイオン
で衝撃し、叩き出された物質を下地基材に析出させて薄
膜を得る。必要に応じて、下地基材は加熱されることが
ある。The sputtering method, which is commonly used as a means for producing a thin film, is also used for producing a superconductor thin film. As shown in the figure, the conventional sputtering apparatus is composed of a vacuum chamber (1), a base material (2), a target material (3) and a power source (4). The thin film manufacturing method using this equipment is 10 -6
After evacuating to less than Torr, an inert gas such as Ar or He is controlled to an atmosphere of 10 -3 to 10 -2 Torr to perform glow discharge, and the target material on the cathode side is bombarded with inert gas ions, The beaten substance is deposited on the base material to obtain a thin film. If necessary, the base substrate may be heated.
然しながら前記方法においては、スパッタリングの方向
と下地基材の法線方向が常に平行であるため、スパッタ
リングによって堆積する膜の成長方向が一定に配向し、
配向性を避けたい成膜には不向きであるという問題点が
ある。また、結晶成長は核形成時の方位にも支配される
ため、従来の方法では焼結の過程で異常成長を起こしや
すく、結晶の配向成長が助長され、結晶粒の微細化を阻
害するという問題もある。However, in the above method, since the direction of sputtering and the normal direction of the base material are always parallel, the growth direction of the film deposited by sputtering is constantly oriented,
There is a problem that it is not suitable for film formation in which orientation is desired to be avoided. Further, since crystal growth is also controlled by the orientation at the time of nucleation, the conventional method tends to cause abnormal growth in the process of sintering, promotes oriented growth of crystals, and inhibits grain refinement. There is also.
本発明では、高温超伝導体膜であるLa−Ba（Sr）−Cu−
Ｏ系の結晶構造は層状ペロブスカイト構造をしており、
層と平行な方向の導電性が層と直角方向の導電性よりも
良いという電気的な異方性が非常に大きく、このような
異方性は超伝導状態においても現れると考えられる。Ｙ
−Ba−Cu−Ｏ系の高温超伝導体にも結晶構造に異方性が
ありLa−Ba（Sr）−Cu−Ｏ系と同じような性質が期待さ
れる。従って多結晶膜の超伝導特性を向上させるために
は異方性を回避し、結晶粒を微細化することが重要であ
る。かかる観点から種々検討を行った結果、スパッター
方向とターゲット材および、または下地基材の公転軸お
よび、または自転軸との間に傾き角を設けることがきわ
めて有効であることを見いだし本発明を達成したもので
ある。即ち本発明方法はスパッタリング法により高温超
伝導体膜を製造するにあたり、高温超伝導体よりなるタ
ーゲット材および，または下地基材が自転および，また
は公転し、こらの自転および，または公転の軸がスパッ
タ一方向に対して傾き角を持たせてスパッタリングを行
うことを特徴とする高温超伝導体膜の製造方法である。In the present invention, the high temperature superconductor film La-Ba (Sr) -Cu-
The O-based crystal structure has a layered perovskite structure,
The electrical anisotropy that the conductivity in the direction parallel to the layer is better than the conductivity in the direction perpendicular to the layer is very large, and it is considered that such anisotropy also appears in the superconducting state. Y
The -Ba-Cu-O-based high temperature superconductor also has anisotropy in the crystal structure and is expected to have the same properties as the La-Ba (Sr) -Cu-O system. Therefore, in order to improve the superconducting properties of the polycrystalline film, it is important to avoid anisotropy and make the crystal grains finer. As a result of various studies from this viewpoint, it was found that it is extremely effective to provide a tilt angle between the sputter direction and the target material and / or the revolution axis and / or the rotation axis of the base material, and the present invention was achieved. It was done. That is, in the method of the present invention, in producing a high temperature superconductor film by the sputtering method, the target material and / or the base material made of the high temperature superconductor are rotated and / or revolved, and the axis of rotation and / or revolution is This is a method for producing a high temperature superconductor film, which is characterized in that sputtering is performed with an inclination angle with respect to one direction of sputtering.
以下に本発明の実施例について説明する。 Examples of the present invention will be described below.
（実施例１） あらかじめ、La:Sr:Cu比が1.8:0.2:1になるように調整
された直径２インチ，厚さ3mmの焼結ターゲット材を用
意し、真空槽を10-6Torrまで排気後、Ar＋O2雰囲気を５
×10-3Torrにして、結晶面（100）のMgO単結晶上にスパ
ッタリングした。その際、スパッター方向と下地基板の
軸との傾き角θ2を変えて、膜の結晶粒径（μｍ）と超
伝導特性を測定した。その結果を第１表に示す。(Example 1) A sintered target material having a diameter of 2 inches and a thickness of 3 mm, which had been adjusted so that the La: Sr: Cu ratio was 1.8: 0.2: 1, was prepared in advance, and the vacuum chamber was adjusted to 10 -6 Torr. After exhausting, Ar + O 2 atmosphere is changed to 5
It was sputtered on a MgO single crystal having a crystal face (100) at a pressure of × 10 -3 Torr. At that time, the crystal grain size (μm) and the superconducting property of the film were measured by changing the tilt angle θ 2 between the sputtering direction and the axis of the base substrate. The results are shown in Table 1.
この結果よりLa−Ba（Sr）−Cu−Ｏ系においてはスパッ
ターに対する傾き角θ2が25゜において作製された膜が
最良の超伝導特性を示すことがわかる。この結晶系では
tan-1a/cが約25゜に相当しており、ｃ軸とａ軸の比に大
きく依存して特性が変化したものと考えられる。 From these results, it can be seen that in the La-Ba (Sr) -Cu-O system, the film produced when the tilt angle θ 2 with respect to sputtering is 25 ° shows the best superconducting properties. In this crystal system
tan -1 a / c corresponds to about 25 °, and it is considered that the characteristics are largely changed depending on the ratio of the c-axis and the a-axis.
（実施例２） あらかじめ、Ba:Cu比が2:3になるように焼結された直径
２インチのターゲット材とY2O8を焼結したターゲット材
の２コのターゲット材を２極スパッタリング装置にセッ
トし、２×10-6Torrに排気後、Ar＋He＋02ガス１×10-2
Torrの雰囲気中で、Al2O3基板上にスパッタ膜を形成し
た。その際、スパッター方向とターゲット材軸との傾き
角θ1を変えて、実施例１と同様の測定を行った。その
結果を第２表に示す。Example 2 Two-pole sputtering was performed on two target materials, a target material having a diameter of 2 inches and a target material that was sintered Y 2 O 8 so that the Ba: Cu ratio was 2: 3. It was set in the apparatus, after evacuated to 2 × 10 -6 Torr, Ar + He + 0 2 gas 1 × 10 -2
A sputtered film was formed on an Al 2 O 3 substrate in a Torr atmosphere. At that time, the same measurement as in Example 1 was performed by changing the tilt angle θ 1 between the sputtering direction and the target material axis. The results are shown in Table 2.
この結果より、Ｙ−Ba−Cu−Ｏ系においてはスパッター
に対する傾き角θ1が18゜において作成された膜が最良
の超伝導特性を示すものが得られる。 From this result, in the Y-Ba-Cu-O system, the film formed with the tilt angle θ 1 with respect to sputtering of 18 ° shows the best superconducting property.
以上説明したように本発明の高温超伝導体膜の製造方法
では、高温超伝導体よりなるターゲット材および，また
は下地基材が自転および，または公転し、これらの自転
および，または公転の軸がスパッター方向に対して傾き
角を持たせてスパッタリングを行うため、得られる膜は
結晶粒が微細化し、Jcが向上したものが得られるという
優れた効果がある。As described above, in the method for producing a high temperature superconductor film of the present invention, the target material and / or the base material made of the high temperature superconductor are rotated and / or revolved, and the axis of rotation and / or revolution is Since the sputtering is performed with an inclination angle with respect to the sputter direction, the obtained film has an excellent effect that the crystal grains become finer and Jc is improved.
図面は本発明におけるスパッタリング装置の説明図であ
る。 １……真空槽,2……下地基材,3……ターゲット材,4……
電源。The drawings are illustrations of a sputtering apparatus according to the present invention. 1 ... Vacuum tank, 2 ... Base substrate, 3 ... Target material, 4 ...
Power supply.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｈ０１Ｂ 12/06 ＺＡＡ 7244−5Ｇ 13/00 ５６５ Ｄ 7244−5Ｇ Ｈ０１Ｌ 39/12 ＺＡＡ Ｃ 9276−4Ｍ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI technical display location H01B 12/06 ZAA 7244-5G 13/00 565 D 7244-5G H01L 39/12 ZAA C 9276-4M
Claims (3)
製造方法において、高温超伝導体よりなるターゲット材
および、または下地基材が自転および，または公転し、
これらの自転および，または公転の軸がスパッター方向
に対して傾き角を持たせてスパッタリングを行うことを
特徴とする高温超伝導体膜の製造方法。1. A method for producing a high temperature superconductor film by a sputtering method, wherein a target material made of a high temperature superconductor and / or a base material is rotated and / or revolved,
A method for producing a high-temperature superconductor film, characterized in that the axis of rotation and / or revolution is inclined with respect to the sputtering direction to perform sputtering.
て、傾き角が27゜以下,10゜以上であることを特徴とす
る特許請求の範囲第１項記載の高温超伝導体膜の製造方
法。2. The high temperature superconductor according to claim 1, wherein the high temperature superconductor is a La-Sr-Cu-O system and the tilt angle is 27 ° or less and 10 ° or more. Method for manufacturing conductor film.
傾き角が19゜以下,5゜以上であることを特徴とする特許
請求の範囲第１項記載の高温超伝導体膜の製造方法。3. The high-temperature superconductor according to claim 1, wherein the high-temperature superconductor is a Y-Ba-Cu-O system and the tilt angle is 19 ° or less and 5 ° or more. Body membrane manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62148389A JPH0717480B2 (en) | 1987-06-15 | 1987-06-15 | Method for manufacturing high temperature superconductor film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62148389A JPH0717480B2 (en) | 1987-06-15 | 1987-06-15 | Method for manufacturing high temperature superconductor film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63313427A JPS63313427A (en) | 1988-12-21 |
| JPH0717480B2 true JPH0717480B2 (en) | 1995-03-01 |
Family
ID=15451680
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62148389A Expired - Lifetime JPH0717480B2 (en) | 1987-06-15 | 1987-06-15 | Method for manufacturing high temperature superconductor film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0717480B2 (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2602304B2 (en) * | 1988-11-21 | 1997-04-23 | 富士電機株式会社 | Method for producing composite oxide superconducting thin film |
| KR950011339B1 (en) * | 1989-02-10 | 1995-09-30 | 미쓰비시 긴소꾸 가부시기가이샤 | Target used for formation of super conductive oxide film process of producing therfof |
| JPH02232367A (en) * | 1989-03-07 | 1990-09-14 | Canon Inc | Vacuum film forming device |
| US5180708A (en) * | 1990-06-20 | 1993-01-19 | Sumitomo Electric Industries, Ltd. | Process and apparatus for preparing superconducting thin films |
| JP4583868B2 (en) * | 2004-10-15 | 2010-11-17 | 株式会社昭和真空 | Sputtering equipment |
| JP2009235429A (en) * | 2008-03-25 | 2009-10-15 | Iwate Univ | Sputtering apparatus |
| CN104164701A (en) * | 2014-08-06 | 2014-11-26 | 上海交通大学 | Method for preparing high-temperature superconducting film by liquid-phase epitaxy |
-
1987
- 1987-06-15 JP JP62148389A patent/JPH0717480B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63313427A (en) | 1988-12-21 |
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