JP2013122065A - Method and apparatus for depositing functional thin film - Google Patents

Method and apparatus for depositing functional thin film Download PDF

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JP2013122065A
JP2013122065A JP2011269984A JP2011269984A JP2013122065A JP 2013122065 A JP2013122065 A JP 2013122065A JP 2011269984 A JP2011269984 A JP 2011269984A JP 2011269984 A JP2011269984 A JP 2011269984A JP 2013122065 A JP2013122065 A JP 2013122065A
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Tatsuoki Nagaishi
竜起 永石
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Sumitomo Electric Industries Ltd
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Abstract

PROBLEM TO BE SOLVED: To provide a method and apparatus for depositing a functional thin film with excellent crystallinity even if the film is thick, while fully exhibiting the characteristics as a functional thin film.SOLUTION: The method for depositing a functional thin film on a substrate by a vapor phase thin film deposition method, includes heating a film deposition side of the substrate to deposit the functional thin film. The device 1 for depositing the functional thin film on the substrate by the vapor phase thin film deposition method, includes a heating means for heating the film deposition side of the substrate. The vapor phase thin film deposition method is a laser deposition method.

Description

本発明は、膜厚が厚い場合でも、結晶性に優れた機能性薄膜を得ることができる機能性薄膜の成膜方法および成膜装置に関する。   The present invention relates to a functional thin film forming method and a film forming apparatus capable of obtaining a functional thin film having excellent crystallinity even when the film thickness is large.

酸化物超電導薄膜、磁性薄膜、圧電薄膜などの機能性薄膜の成膜に際しては、スパッタ法、ＭＯ−ＣＶＤ法、ＭＢ法、レーザ堆積法（パルスレーザデポジッション：ＰＬＤ法）などの気相薄膜合成法が広く用いられている（例えば非特許文献１、非特許文献２）。   When forming functional thin films such as oxide superconducting thin films, magnetic thin films, and piezoelectric thin films, vapor-phase thin film synthesis such as sputtering, MO-CVD, MB, and laser deposition (pulse laser deposition: PLD) is used. The method is widely used (for example, Non-Patent Document 1 and Non-Patent Document 2).

しかしながら、これらの気相薄膜合成法を用いて機能性薄膜を形成した場合、膜厚が薄い場合には十分にその特性を発揮させることができるが、膜厚が厚い場合には、その特性を十分に発揮させることができない場合があった。例えば、臨界電流値Ｉｃを向上させるために酸化物超電導薄膜の膜厚を厚くした場合、膜厚の増加と超電導特性の向上が必ずしも一致しなかった。   However, when a functional thin film is formed by using these vapor phase thin film synthesis methods, the characteristics can be sufficiently exerted when the film thickness is thin. In some cases, it was not possible to make full use. For example, when the thickness of the oxide superconducting thin film is increased in order to improve the critical current value Ic, the increase in the film thickness does not necessarily coincide with the improvement of the superconducting characteristics.

具体的な一例として、ＰＬＤ法を用いてＧｄＢＣＯ（ＧｄＢａ２Ｃｕ３Ｏ７−ｘ）酸化物超電導薄膜の形成を行った場合、図４に示すように、膜厚１．３μｍ程度までは膜厚に対して直線的だったＩｃの伸びが、その後は徐々に鈍化している。これは、膜厚が厚くなるにつれて臨界電流密度Ｊｃが低下して、膜厚の増加がＩｃの向上に寄与しなくなっていることを示している。 As a specific example, when a GdBCO (GdBa 2 Cu 3 O 7-x ) oxide superconducting thin film is formed using the PLD method, the film thickness is about 1.3 μm as shown in FIG. On the other hand, the growth of Ic, which was linear, gradually decreased after that. This indicates that the critical current density Jc decreases as the film thickness increases, and the increase in film thickness does not contribute to the improvement of Ic.

このような現象は、膜厚が厚くなるにつれて膜表面の温度が低下して、膜の表面側での結晶性を低下させていることにより発生していることが、膜の断面観察から分かっている。   It can be seen from the cross-sectional observation of the film that this phenomenon occurs because the film surface temperature decreases as the film thickness increases and the crystallinity on the surface side of the film decreases. Yes.

ＰＬＤ法では、通常、成膜される面とは反対側の面（成膜反対面）（裏面）から基材を加熱しながら成膜材料の蒸着を行い成膜している。   In the PLD method, film formation is usually performed by depositing a film forming material while heating the substrate from a surface opposite to the surface on which the film is formed (surface opposite to the film formation) (back surface).

しかし、このように成膜反対面から基材を加熱する方法の場合、膜厚が厚くなると加熱効率が低下するため、膜厚が厚くなるにつれて膜表面の温度が低下して、膜表面での結晶性が低下して、異相の析出や配向の不十分な結晶が生じ、Ｊｃの低下を招いてしまう。   However, in the case of the method of heating the substrate from the opposite side of the film formation in this way, since the heating efficiency decreases as the film thickness increases, the temperature of the film surface decreases as the film thickness increases. Crystallinity is lowered, resulting in precipitation of heterophases or crystals with insufficient orientation, resulting in a decrease in Jc.

そこで、厚膜の酸化物超電導薄膜を作製する際には、ヒータの温度を順次上昇させて、複数回に分けて成膜して厚膜化することが行われているが、ヒータの温度が高くなりすぎると、テープ線材（基材）の成膜反対面側における負荷が大きくなって、テープ線材の変形を引き起こしたり、テープ線材を構成する金属材料が拡散して、Ｊｃなどを低下させたりする等の不具合が発生していた。   Therefore, when a thick oxide superconducting thin film is manufactured, the temperature of the heater is sequentially increased, and the film is formed in multiple times to increase the thickness. If it is too high, the load on the opposite side of the tape wire (base material) will increase, causing the tape wire to deform, or the metal material constituting the tape wire will diffuse and reduce Jc, etc. There was a problem such as.

具体的な一例として、ＳＵＳ基板、Ｃｕ箔、Ｎｉめっきで構成されるクラッド基板の場合には、加熱により、融点の低い銅がＮｉめっき層に拡散してしまう恐れがある。   As a specific example, in the case of a clad substrate composed of a SUS substrate, Cu foil, and Ni plating, copper having a low melting point may be diffused into the Ni plating layer by heating.

このように、従来の酸化物超電導薄膜の作製においては、複数回の成膜により厚膜化しようとしても、ヒータの温度を十分に上げることができないため、結晶性に優れ、十分に超電導特性を発揮させることができる酸化物超電導薄膜を得ることが困難であった。   As described above, in the production of a conventional oxide superconducting thin film, the temperature of the heater cannot be sufficiently increased even if it is attempted to increase the film thickness by multiple times of film formation. It has been difficult to obtain an oxide superconducting thin film that can be exhibited.

このような問題は、上記した酸化物超電導薄膜以外の機能性薄膜においても同様に生じており、結晶性に優れ、機能性薄膜としての特性を十分に発揮させることができる厚膜の機能性薄膜を得ることが困難であった。   Such a problem also occurs in functional thin films other than the oxide superconducting thin film described above, and is a thick functional thin film that has excellent crystallinity and can fully exhibit the characteristics as a functional thin film. It was difficult to get.

Ｓ．Ｒ．Ｆｏｌｔｙｎ他「Ｌａｒｇｅ−ａｒｅａ，ｔｗｏ−ｓｉｄｅｄ ｓｕｐｅｒｃｏｎｄｕｃｔｉｎｇ ＹＢａ２Ｃｕ３Ｏ７−ｘ ｆｉｌｍｓ ｄｅｐｏｓｉｔｅｄ ｂｙ ｐｕｌｓｅｄ ｌａｓｅｒ ｄｅｐｏｓｉｔｉｏｎ」、Ａｐｐｌ．Ｐｈｙｓ．Ｌｅｔｔ．５９（１１），９ Ｓｅｐｔｅｍｂｅｒ １９９１、１３７４−１３７６S. R. Foltyn et al. “Large-area, two-sided superconducting YBa2Cu3O7-x films deposited by pulsed laser deposition”, Appl. Phys. Lett. 59 (11), 9 September 1991, 1374-1376 Ｈ．Ｋｕｔａｍｉ他「Ｐｒｏｇｒｅｓｓ ｉｎ ｒｅｓｅａｒｃｈ ａｎｄ ｄｅｖｅｌｏｐｍｅｎｔ ｏｎ ｌｏｎｇ ｌｅｎｇｔｈ ｃｏａｔｅｄ ｃｏｎｄｕｃｔｏｒｓ ｉｎ Ｆｕｊｉｋｕｒａ」、Ｐｈｙｓｉｃａ Ｃ ４６９ （２００９）、１２９０−１２９３H. Kutama et al., "Progress in research and development on long length coated conductors in Fujikura", Physica C 469 (2009), 1290-1293.

以上のため、本発明は、膜厚が厚い場合でも、結晶性に優れ、機能性薄膜としての特性を十分に発揮させることができる機能性薄膜を得ることができる機能性薄膜の成膜方法および成膜装置を提供することを課題とする。   For the above reasons, the present invention provides a method for forming a functional thin film capable of obtaining a functional thin film that is excellent in crystallinity and can sufficiently exhibit the characteristics as a functional thin film even when the film thickness is large, and It is an object to provide a film formation apparatus.

本発明者は、鋭意検討の結果、以下に記載する発明により、上記課題が解決できることを見出し、本発明を完成させるに至った。以下、各請求項毎に説明する。   As a result of intensive studies, the present inventor has found that the above problems can be solved by the invention described below, and has completed the present invention. Hereinafter, each claim will be described.

請求項１に記載の発明は、
気相薄膜合成法を用いて、基材上に機能性薄膜を成膜する機能性薄膜の成膜方法であって、
前記基材の成膜面側から加熱して機能性薄膜の成膜を行う
ことを特徴とする機能性薄膜の成膜方法である。 The invention described in claim 1
A functional thin film forming method for forming a functional thin film on a substrate using a vapor phase thin film synthesis method,
The functional thin film is formed by heating from the film forming surface side of the substrate to form the functional thin film.

本発明者は、成膜に際しての基材（テープ線材）への加熱を、従来のように基材の成膜反対面側（裏面側）から行うのではなく、基材の成膜面側にヒータを配置して行うことに思い至った。   The inventor does not heat the base material (tape wire) during film formation from the side opposite to the film formation side (back side) of the base material as in the prior art, but on the film formation side of the base material. I came up with a heater.

基材の成膜面側から加熱することにより、厚膜の場合であっても、成膜面を十分に加熱することができる。この結果、基材上に、表面まで結晶性に優れた機能性薄膜を作製することができ、機能性薄膜としての特性を十分に発揮させることができる。   By heating from the film formation surface side of the substrate, the film formation surface can be sufficiently heated even in the case of a thick film. As a result, a functional thin film having excellent crystallinity up to the surface can be produced on the substrate, and the characteristics as the functional thin film can be sufficiently exhibited.

また、基材の成膜反対面側における熱負荷が大きくなることがないため、上記した基材の変形や基材を構成する金属材料の拡散を防止することができる。   Moreover, since the thermal load on the opposite side of the film formation of the base material does not increase, it is possible to prevent the deformation of the base material and the diffusion of the metal material constituting the base material.

なお、本請求項の発明にいう「機能性薄膜」とは、薄膜化した機能性材料である。機能性材料は、材料の持つ電気的性質、誘電体特性、磁性、光学特性などの機能を発現させることを目的として製品に組み込まれるタイプの材料を称する。具体的には、酸化物超電導薄膜、ハードディスク等に適用される磁性アモルファス薄膜、薄膜太陽電池等に用いられるアモルファス半導体薄膜、圧電デバイスに用いられる圧電薄膜などの薄膜が挙げられる。   In addition, the “functional thin film” referred to in the present invention is a functional material made into a thin film. The functional material refers to a type of material that is incorporated into a product for the purpose of expressing functions such as electrical properties, dielectric properties, magnetism, and optical properties of the material. Specific examples include thin films such as oxide superconducting thin films, magnetic amorphous thin films applied to hard disks, amorphous semiconductor thin films used in thin film solar cells, and piezoelectric thin films used in piezoelectric devices.

請求項２に記載の発明は、
さらに、前記基材の成膜面と反対側の面からも加熱して機能性薄膜の成膜を行うことを特徴とする請求項１に記載の機能性薄膜の成膜方法である。 The invention described in claim 2
2. The functional thin film forming method according to claim 1, wherein the functional thin film is formed by heating also from a surface opposite to the film forming surface of the substrate.

基材の成膜面側から加熱すると共に、基材の成膜反対面側からも加熱することにより、機能性薄膜内における熱のばらつきを一層抑制することができ好ましい。また、基材の両面にヒータを配置して加熱するため、各ヒータにおける負荷を低減することができる。   Heating from the film-forming surface side of the substrate and heating from the surface opposite to the film-forming surface of the substrate is also preferable because variation in heat in the functional thin film can be further suppressed. Moreover, since a heater is arrange | positioned and heated on both surfaces of a base material, the load in each heater can be reduced.

請求項３に記載の発明は、
前記気相薄膜合成法が、レーザ堆積法であることを特徴とする請求項１または請求項２に記載の機能性薄膜の成膜方法である。 The invention according to claim 3
3. The functional thin film forming method according to claim 1, wherein the vapor phase thin film synthesis method is a laser deposition method.

レーザ堆積法は、スパッタ法などの他の気相薄膜合成法と比べて、成膜速度が速いため、より効率的に加熱する必要があるが、本発明においては基材の成膜面側から加熱しているため、より効率的な加熱が可能となり、本発明の効果を顕著に発揮させることができる。   The laser deposition method has a higher film forming speed than other vapor phase thin film synthesizing methods such as a sputtering method, and thus needs to be heated more efficiently. In the present invention, from the film forming surface side of the substrate, Since it heats, more efficient heating is attained and the effect of this invention can be exhibited notably.

請求項４に記載の発明は、
前記機能性薄膜が、酸化物薄膜であることを特徴とする請求項１ないし請求項３のいずれか１項に記載の機能性薄膜の成膜方法である。 The invention according to claim 4
The functional thin film forming method according to any one of claims 1 to 3, wherein the functional thin film is an oxide thin film.

機能性薄膜の内でも、酸化物からなる薄膜は、形成時における成長温度が高温であるため、本発明に係る成膜方法を採用することによる効果が顕著に発揮される。   Among functional thin films, a thin film made of an oxide has a high growth temperature at the time of formation, so that the effect of employing the film forming method according to the present invention is remarkably exhibited.

請求項５に記載の発明は、
前記酸化物薄膜が、酸化物超電導薄膜であることを特徴とする請求項４に記載の機能性薄膜の成膜方法である。 The invention described in claim 5
5. The method for forming a functional thin film according to claim 4, wherein the oxide thin film is an oxide superconducting thin film.

酸化物薄膜の内でも、酸化物超電導薄膜は特に高温での成長が必要である。また、酸化物超電導薄膜は黒色である。これらのため、基材の成膜反対面側からのみ加熱する従来の方法の場合には、成膜面を十分に高温とするために、大きな熱負荷を基材に加える必要があり、基材の変形や金属材料の拡散を招く恐れが高かった。   Among oxide thin films, oxide superconducting thin films need to be grown at high temperatures. The oxide superconducting thin film is black. For these reasons, in the case of the conventional method of heating only from the side opposite to the film formation side of the substrate, it is necessary to apply a large heat load to the substrate in order to make the film formation surface sufficiently hot. There was a high risk of causing deformation and diffusion of metal materials.

しかし、本発明においては、基材の成膜面側から加熱する方法を採用しているため、基材の成膜反対面側から大きな熱負荷を加える必要がなく、上記の問題の発生を回避しながら高い加熱効率で成膜を行うことができる。   However, in the present invention, since the method of heating from the film formation surface side of the substrate is adopted, it is not necessary to apply a large heat load from the film formation opposite surface side of the substrate, and the occurrence of the above problems is avoided. The film can be formed with high heating efficiency.

請求項６に記載の発明は、
気相薄膜合成法を用いて、基材上に機能性薄膜を成膜する機能性薄膜の成膜装置であって、
前記基材の成膜面側から前記基材を加熱する加熱手段を備えている
ことを特徴とする機能性薄膜の成膜装置である。 The invention described in claim 6
A functional thin film forming apparatus for forming a functional thin film on a substrate using a vapor phase thin film synthesis method,
A functional thin film forming apparatus comprising a heating means for heating the base material from the film forming surface side of the base material.

前記したように、基材の成膜面側から加熱することにより、厚膜の場合であっても、基材上に、表面まで結晶性に優れた機能性薄膜を作製することができ、優れた特性の機能性薄膜を提供することができる。   As described above, by heating from the film formation surface side of the substrate, a functional thin film having excellent crystallinity up to the surface can be produced on the substrate even in the case of a thick film. It is possible to provide a functional thin film having different characteristics.

請求項７に記載の発明は、
さらに、前記基材の成膜面と反対側の面から前記基材を加熱する加熱手段を備えていることを特徴とする請求項６に記載の機能性薄膜の成膜装置である。 The invention described in claim 7
The functional thin film deposition apparatus according to claim 6, further comprising a heating unit configured to heat the substrate from a surface opposite to the film deposition surface of the substrate.

前記したように、基材の成膜面側から加熱すると共に、基材の成膜反対面側からも加熱することにより、機能性薄膜内における熱のばらつきを一層抑制することができる。また、基材両側の各ヒータにおける負荷を低減することができる。   As described above, by heating from the film formation surface side of the base material and also from the surface opposite to the film formation side of the base material, variation in heat in the functional thin film can be further suppressed. Moreover, the load on each heater on both sides of the substrate can be reduced.

請求項８に記載の発明は、
前記気相薄膜合成法が、レーザ堆積法であることを特徴とする請求項６または請求項７に記載の機能性薄膜の成膜装置である。 The invention according to claim 8 provides:
8. The functional thin film deposition apparatus according to claim 6, wherein the vapor phase thin film synthesis method is a laser deposition method.

前記したように、レーザ堆積法は、成膜速度が速いため、本発明の装置の効果を顕著に発揮させることができる。   As described above, since the laser deposition method has a high film formation rate, the effect of the apparatus of the present invention can be remarkably exhibited.

本発明によれば、膜厚が厚い場合でも、結晶性に優れ、機能性薄膜としての特性を十分に発揮させることができる機能性薄膜を得ることができる機能性薄膜の成膜方法および成膜装置を提供することができる。   ADVANTAGE OF THE INVENTION According to this invention, even if it is thick, the functional thin film formation method and film formation which can obtain the functional thin film which is excellent in crystallinity and can fully exhibit the characteristic as a functional thin film An apparatus can be provided.

本発明の一実施の形態の気相薄膜合成法を用いた機能性薄膜の成膜装置を説明する図である。It is a figure explaining the film-forming apparatus of the functional thin film using the vapor-phase thin film synthesis method of one embodiment of this invention. 実施例および比較例で作製した酸化物超電導線材の構成を示す図である。It is a figure which shows the structure of the oxide superconducting wire produced in the Example and the comparative example. 実施例および比較例の酸化物超電導薄膜のＩｃ値と膜厚との関係を示す図である。It is a figure which shows the relationship between Ic value and film thickness of the oxide superconducting thin film of an Example and a comparative example. 従来技術によって成膜したＲＥＢＣＯ酸化物超電導薄膜のＩｃ値と膜厚の関係を示す図である。It is a figure which shows the relationship between Ic value and film thickness of the REBCO oxide superconducting thin film formed by the prior art. 従来の気相薄膜合成法を用いた機能性薄膜の成膜装置を説明する図である。It is a figure explaining the film-forming apparatus of the functional thin film using the conventional vapor-phase thin film synthesis method.

以下、酸化物超電導薄膜を作製する場合を例に挙げて、本発明の実施の形態について説明する。   Hereinafter, an embodiment of the present invention will be described with reference to an example in which an oxide superconducting thin film is manufactured.

１．成膜装置
はじめに、本実施の形態の成膜装置について説明する。図１は本実施の形態の気相薄膜合成法を用いた機能性薄膜（酸化物超電導薄膜）の成膜装置を説明する図である。図１において、１は真空チャンバ（図示省略）内に設けられた成膜装置であり、ヒータ１１、ヒータ１３、スリット１２を備えている。また、成膜装置１は、原料ターゲットＴにレーザを照射するレーザ照射装置、テープ線材Ｗ（基材）をｒｅｅｌ ｔｏ ｒｅｅｌで搬送する搬送手段、円盤状の原料ターゲットＴを保持し回転させる機構を備えている（いずれも図示省略）。なお、Ｐは、レーザ光の照射により原料ターゲットＴから放出（昇華）された成膜材料が酸素ガスと衝突して発光したレーザプルームである。 1. Film Forming Apparatus First, the film forming apparatus of the present embodiment will be described. FIG. 1 is a diagram for explaining a film forming apparatus for a functional thin film (oxide superconducting thin film) using the vapor phase thin film synthesis method of the present embodiment. In FIG. 1, reference numeral 1 denotes a film forming apparatus provided in a vacuum chamber (not shown), which includes a heater 11, a heater 13, and a slit 12. Further, the film forming apparatus 1 includes a laser irradiation apparatus that irradiates the raw material target T with a laser, a transport unit that transports the tape wire W (base material) in a reel-to-reel manner, and a mechanism that holds and rotates the disk-shaped raw material target T. Provided (both not shown). Note that P is a laser plume in which a film forming material emitted (sublimated) from the source target T by laser beam irradiation collides with oxygen gas and emits light.

レーザ照射装置は、エキシマレーザなどを用いて、回転している円盤状の原料ターゲットＴの円盤の中心の外側にレーザ光を照射する。これにより、成膜原料が放出（昇華）され、テープ線材Ｗの成膜面側（表面）に成膜される。レーザエネルギー（単位：Ｊ／パルス）および照射面積（単位：ｃｍ２）を調整することにより、成膜に適切な照射エネルギー密度（単位：Ｊ／ｃｍ２）が決定される。 The laser irradiation apparatus irradiates laser light to the outside of the center of the rotating disk-shaped raw material target T using an excimer laser or the like. Thereby, the film forming raw material is released (sublimated), and a film is formed on the film forming surface side (surface) of the tape wire W. By adjusting the laser energy (unit: J / pulse) and the irradiation area (unit: cm 2 ), an irradiation energy density (unit: J / cm 2 ) appropriate for film formation is determined.

原料ターゲットＴとテープ線材Ｗとの間隔は、通常７０ｍｍ程度が好ましい。   The distance between the raw material target T and the tape wire W is usually preferably about 70 mm.

原料ターゲットＴのレーザ照射位置から離れた場所では、昇華されてテープ線材Ｗに付着する際の元素組成比がずれてしまい、良好な超電導特性が得られなくなる恐れがある。このため、原料ターゲットＴとテープ線材Ｗの間には、開口部を有するスリット１２が設けられて、成膜領域が制限されるようになっている。   In a place away from the laser irradiation position of the raw material target T, the elemental composition ratio at the time of sublimation and adhering to the tape wire W may be shifted, and good superconducting characteristics may not be obtained. For this reason, between the raw material target T and the tape wire W, the slit 12 which has an opening part is provided, and the film-forming area | region is restrict | limited.

テープ線材Ｗの長手方向におけるスリット１２の開口部の長さＬ１は、レーザの原料ターゲットＴ上の照射形状に応じて、３０〜８０ｍｍで適宜設定される。なお、スリット１２の開口部両端では、図１に示すように、テープ線材Ｗ側に壁を設けて、昇華した成膜原料がヒータ１１に付着しないようにすることが好ましい。 The length L 1 of the opening of the slit 12 in the longitudinal direction of the tape wire W, depending on the illumination profile of the laser of raw material target T, is appropriately set in 30 to 80 mm. As shown in FIG. 1, it is preferable to provide a wall on the tape wire W side so that the sublimated film forming material does not adhere to the heater 11 at both ends of the opening of the slit 12.

また、レーザプルームＰの位置における加熱が、機能性薄膜の成長を左右するため、前記した壁とヒータ１１の端部との間隔ｄ２はできる限り小さい方が好ましく、具体的には１ｍｍ程度が好ましい。 Further, since the heating at the position of the laser plume P affects the growth of the functional thin film, the distance d 2 between the wall and the end of the heater 11 is preferably as small as possible, specifically about 1 mm. preferable.

テープ線材Ｗとスリット１２の間には、テープ線材Ｗの搬送経路の成膜ゾーンの前後にテープ線材Ｗ表面を加熱するヒータ１１が、テープ線材Ｗから３〜１０ｍｍの間隔ｄ１を隔てて設けられている。ヒータ１１としては、テープ線材Ｗと原料ターゲットＴとの距離を短縮可能であるという観点から薄いヒータが好ましく、例えば、厚みｔを１０ｍｍ程度とすることが可能な抵抗線加熱ヒータなどを用いることが好ましい。 Between the tape wire W and the slit 12, a heater 11 for heating the surface of the tape wire W before and after the film forming zone of the transport path of the tape wire W is provided at a distance d 1 of 3 to 10 mm from the tape wire W. It has been. The heater 11 is preferably a thin heater from the viewpoint that the distance between the tape wire W and the raw material target T can be shortened. For example, a resistance wire heater that can have a thickness t of about 10 mm is used. preferable.

ヒータ１１を成膜ゾーンの前後に設けて、成膜直前に基材の表面を有効に加熱するとともに、成膜直後にも加熱を行うことにより、結晶化における加熱処理を、より効率よく行うことができ好ましい。   The heater 11 is provided before and after the film formation zone to effectively heat the surface of the base material immediately before film formation and to perform heat treatment in crystallization more efficiently by heating immediately after film formation. This is preferable.

なお、ヒータ１１の大きさは、幅としてはテープ線材Ｗの幅方向の均熱を得るためにテープ線材Ｗの幅よりも両側が１０ｍｍ以上広いことが好ましく、長さ（テープ線材Ｗの長手方向の長さ）Ｌ２としてはテープ線材Ｗの移動を考慮すると５０〜１００ｍｍ程度であることが好ましい。 The width of the heater 11 is preferably 10 mm or more wider on both sides than the width of the tape wire W in order to obtain uniform heat in the width direction of the tape wire W, and the length (the longitudinal direction of the tape wire W) it is preferable as a length) L 2 is about 50~100mm considering the movement of the tape wire W.

また、本実施の形態においては、テープ線材Ｗの成膜反対面側（裏面）にも、ヒータ１３が設けられている。ヒータ１３としては、ランプヒータなどが好ましく使用される。   In the present embodiment, the heater 13 is also provided on the side opposite to the film formation (back surface) of the tape wire W. A lamp heater or the like is preferably used as the heater 13.

２．機能性薄膜の成膜方法
次に、上記の構成の成膜装置を用いた機能性薄膜の成膜方法について説明する。 2. Next, a method for forming a functional thin film using the film forming apparatus having the above-described configuration will be described.

まず、１０〜６０Ｐａ程度の酸素ガス雰囲気に設定された真空チャンバ内に、ｒｅｅｌ ｔｏ ｒｅｅｌで数十メートルから数百メートルの長さのテープ線材Ｗを、成膜面を下側にして所定のスピードで導入する。真空チャンバ内には、予め、原料ターゲットＴが、テープ線材Ｗの成膜面に対向して設置されている。   First, in a vacuum chamber set in an oxygen gas atmosphere of about 10 to 60 Pa, a tape wire W having a length of several tens to several hundreds of meters in a reel-to-reel direction with a predetermined surface with the film-forming surface facing down. Introduced in. In the vacuum chamber, the raw material target T is previously installed facing the film-forming surface of the tape wire W.

次に、テープ線材Ｗを表面からはヒータ１１、裏面からはヒータ１３により加熱し、酸化物超電導薄膜の成膜に適した所定の温度（約６５０〜７５０℃程度）になるように各ヒータの投入パワーを調整する。   Next, the tape wire W is heated by the heater 11 from the front surface and the heater 13 from the back surface, and each heater is heated to a predetermined temperature (about 650 to 750 ° C.) suitable for forming the oxide superconducting thin film. Adjust the input power.

そして、テープ線材Ｗを所定の速度で移動させながら、原料ターゲットＴにレーザを照射して成膜材料を昇華させ、テープ線材Ｗの成膜面上に所定の厚さの酸化物超電導薄膜を成膜する。   Then, while moving the tape wire W at a predetermined speed, the raw material target T is irradiated with a laser to sublimate the film forming material, and an oxide superconducting thin film having a predetermined thickness is formed on the film forming surface of the tape wire W. Film.

本実施の形態においては、テープ線材Ｗを成膜面側から加熱しているため、膜厚が厚い場合でも、成膜面を十分に加熱することができ、基材上に、表面まで結晶性に優れた機能性薄膜を作製することができ、機能性薄膜としての特性を十分に発揮させることができる。   In the present embodiment, since the tape wire W is heated from the film formation surface side, the film formation surface can be sufficiently heated even when the film thickness is large, and the surface of the substrate is crystalline up to the surface. It is possible to produce a functional thin film having excellent characteristics and to sufficiently exhibit the characteristics as a functional thin film.

また、基材の成膜反対面側からも加熱しているため、薄膜内における熱のばらつきを一層抑制することができ、より安定した成膜が可能となる。また、表面、裏面の各ヒータにおける負荷をより低減することができる。   In addition, since the substrate is also heated from the side opposite to the film formation, the variation in heat in the thin film can be further suppressed, and more stable film formation is possible. Moreover, the load on each heater on the front surface and the back surface can be further reduced.

以上のように本実施の形態を採用することにより、厚膜であっても、基材上に、表面まで結晶性に優れた機能性薄膜（酸化物超電導薄膜）を作製することができる。   As described above, by employing this embodiment, a functional thin film (oxide superconducting thin film) having excellent crystallinity can be formed on a substrate even on a thick film.

以下、実施例により、本発明をより具体的に説明する。本実施例は、ＰＬＤ法を用いてＧｄＢＣＯ（ＧｄＢａ２Ｃｕ３Ｏ７−ｘ）酸化物超電導薄膜を成膜し、酸化物超電導線材を作製した例である。 Hereinafter, the present invention will be described more specifically by way of examples. This example is an example in which a GdBCO (GdBa 2 Cu 3 O 7-x ) oxide superconducting thin film is formed using a PLD method to produce an oxide superconducting wire.

（実施例）
図２に示す構成の酸化物超電導線材を以下の手順により作製した。 (Example)
An oxide superconducting wire having the configuration shown in FIG. 2 was produced by the following procedure.

（１）下地基材（テープ線材）の作製
まず、１００μｍ厚のステンレス基板に配向銅（Ｃｕ）を貼り合わせた後、ニッケル（Ｎｉ）めっきを施し、１２０μｍ厚の配向金属基板を作製した。次に、配向金属基板にＲＦスパッタ法を用いて、中間層を形成した。具体的には、シード層として０．１４μｍ厚のＣｅＯ２膜、Ｎｉ拡散防止層として０．３μｍ厚のＹＳＺ膜、超電導層との整合層として０．０７μｍ厚のＣｅＯ２膜を形成し、幅３０ｍｍ、長さ１５０ｍのテープ線材（基材）を作製した。 (1) Preparation of base substrate (tape wire) First, oriented copper (Cu) was bonded to a 100 μm-thick stainless steel substrate, and then nickel (Ni) plating was performed to prepare an oriented metal substrate having a thickness of 120 μm. Next, an intermediate layer was formed on the oriented metal substrate by RF sputtering. Specifically, to form a 0.14μm thick CeO 2 film, YSZ film 0.3μm thick as Ni diffusion preventing layer, 0.07 .mu.m thick CeO 2 film as a matching layer between the superconducting layer as a seed layer, the width A tape wire (base material) of 30 mm and a length of 150 m was produced.

（２）酸化物超電導薄膜の成膜
図１に示した成膜装置１を用いてＧｄＢＣＯ酸化物超電導薄膜を成膜した。レーザには２４８ｎｍの波長のエキシマレーザを使用し、レーザエネルギーを原料ターゲットＴ上で０．７５Ｊ／パルスとし、照射面積を０．２５ｃｍ２にすることで、３Ｊ／ｃｍ２程度の照射エネルギー密度とした。なお、原料ターゲットＴにはＧｄＢＣＯの焼結体を使用した。 (2) Formation of oxide superconducting thin film A GdBCO oxide superconducting thin film was formed using the film forming apparatus 1 shown in FIG. The laser is an excimer laser having a wavelength of 248 nm, the laser energy as 0.75 J / pulse on raw material target T, by the irradiation area 0.25 cm 2, and irradiation energy density of about 3J / cm 2 did. The raw material target T was a GdBCO sintered body.

ヒータ１１には厚みが１０ｍｍの抵抗線加熱ヒータを用いた。ヒータ１１とテープ線材Ｗ（基材）との距離ｄ１は１０ｍｍとした。スリット１２の開口部の長さＬ１は６５ｍｍとした。スリット１２のテープ線材Ｗ側に設けた壁からヒータ１１の端部までの距離ｄ２は１ｍｍとした。ヒータ１１の大きさは、幅方向を５０ｍｍとし、テープ線材の長手方向の長さＬ２はテープ線材が移動するために９０ｍｍとした。また、真空チャンバ内は２０Ｐａの酸素ガスで保持した。 As the heater 11, a resistance wire heater having a thickness of 10 mm was used. The distance d 1 between the heater 11 and the tape wire W (substrate) was 10 mm. The length L 1 of the opening of the slit 12 was set to 65 mm. The distance d 2 from the walls provided on the tape wire W side of the slit 12 to the end portion of the heater 11 was set to 1 mm. The size of the heater 11, the width direction and 50 mm, longitudinal length L 2 of the tape wire was 90mm for tape wire is moved. The vacuum chamber was held with 20 Pa oxygen gas.

テープ線材Ｗをｒｅｅｌ ｔｏ ｒｅｅｌで原料ターゲットＴが設置された真空チャンバに導入し、ヒータ１１の投入パワーを３ｋＷ、ヒータ１３の投入パワーを０．４ｋＷとして、テープ線材Ｗの表裏両面から加熱することにより、酸化物超電導薄膜を成膜する表面（成膜面）側の温度が７００℃程度になるように調整した。   The tape wire W is introduced into the vacuum chamber in which the raw material target T is installed on a reel-to-reel basis, and the heating power of the heater 11 is 3 kW and the charging power of the heater 13 is 0.4 kW. Thus, the temperature on the surface (deposition surface) side on which the oxide superconducting thin film was formed was adjusted to about 700 ° C.

テープ線材Ｗを１０ｍ／時の速度で移動させながら、エキシマレーザを原料ターゲットＴに照射してターゲット材料を昇華させ、テープ線材Ｗの表面上にＧｄＢＣＯ酸化物超電導薄膜を成膜した。   While moving the tape wire W at a speed of 10 m / hour, the target material T was irradiated with an excimer laser to sublimate the target material, and a GdBCO oxide superconducting thin film was formed on the surface of the tape wire W.

（３）安定化層および保護層の形成
所定の方法を用いて、ＧｄＢＣＯ酸化物超電導薄膜上に２μｍ厚の銀（Ａｇ）安定化層を形成した後、スリッターを用いて線幅４ｍｍで６条の線材にスリットした。その後、得られた各条線材の外周に２０μｍ厚のＣｕ保護層を形成し、実施例の酸化物超電導線材を得た。 (3) Formation of stabilization layer and protective layer A predetermined method is used to form a 2 μm thick silver (Ag) stabilization layer on the GdBCO oxide superconducting thin film, and then a 6 mm strip with a slit width of 4 mm is used. Slit into the wire. Thereafter, a 20 μm-thick Cu protective layer was formed on the outer periphery of each of the obtained wire rods to obtain oxide superconducting wires of Examples.

（比較例）
図５に示したテープ線材Ｗの裏面側から加熱する従来の成膜装置２を用い、ヒータ２３の投入パワーを膜厚に応じて３．５〜４ｋＷと変化させながら、テープ線材Ｗの裏面側から加熱したこと以外は実施例と同様にしてＧｄＢＣＯ酸化物超電導薄膜を成膜し、さらに、安定化層および保護層を形成し、比較例の酸化物超電導線材を得た。 (Comparative example)
Using the conventional film forming apparatus 2 that heats from the back side of the tape wire W shown in FIG. 5, while changing the input power of the heater 23 to 3.5 to 4 kW according to the film thickness, the back side of the tape wire W A GdBCO oxide superconducting thin film was formed in the same manner as in the example except that it was heated from above, and a stabilization layer and a protective layer were further formed to obtain an oxide superconducting wire of a comparative example.

上記より、実施例の場合、比較例に比べて小さなヒータの投入パワーであるにも拘わらず、テープ線材表面を成膜に適した約７００℃程度に加熱できることが確認できた。   From the above, it was confirmed that in the case of the example, the surface of the tape wire could be heated to about 700 ° C. suitable for film formation even though the heater power was smaller than that of the comparative example.

（酸化物超電導線材の評価）
（１）評価方法
実施例および比較例の酸化物超電導線材について、７７．３Ｋの温度下、通電法によりＩｃ値を測定した。 (Evaluation of oxide superconducting wire)
(1) Evaluation method About the oxide superconducting wire of an Example and a comparative example, Ic value was measured by the electricity supply method under the temperature of 77.3K.

（２）評価結果
評価結果を図３に示す。図３において、縦軸はＩｃ値（Ａ／ｃｍ：線材幅４ｍｍでの実測値を１ｃｍ幅に換算）であり、横軸は酸化物超電導薄膜の膜厚（μｍ）である。また、実線が実施例の評価結果であり、破線が比較例の評価結果（図４と同一のデータ）である。 (2) Evaluation results The evaluation results are shown in FIG. In FIG. 3, the vertical axis is the Ic value (A / cm: the actual measurement value at the wire rod width of 4 mm is converted to 1 cm width), and the horizontal axis is the film thickness (μm) of the oxide superconducting thin film. In addition, the solid line is the evaluation result of the example, and the broken line is the evaluation result of the comparative example (the same data as FIG. 4).

図３より、比較例の場合、酸化物超電導薄膜の膜厚が約１．３ｍｍ以上ではＩｃ値が膜厚に比例して増加せず、Ｊｃが低下していることが分かる。これに対して、実施例の場合、Ｉｃ値が膜厚に比例して増大しており、Ｊｃが低下していないことが分かる。   From FIG. 3, it can be seen that in the comparative example, when the thickness of the oxide superconducting thin film is about 1.3 mm or more, the Ic value does not increase in proportion to the thickness, and Jc decreases. On the other hand, in the case of the example, it can be seen that the Ic value increases in proportion to the film thickness, and Jc does not decrease.

そして、５００Ａ／ｃｍのＩｃを得るためには、比較例の場合には２．８μｍの膜厚を必要とするのに対して、実施例の場合には１．８μｍの膜厚で同等のＩｃ値が得られることが分かる。また、実施例の場合には、２．２μｍの膜厚で６００Ａ／ｃｍのＩｃ値を得ることができることも分かる。   In order to obtain Ic of 500 A / cm, in the case of the comparative example, a film thickness of 2.8 μm is required, whereas in the case of the example, an equivalent Ic of 1.8 μm is obtained. It can be seen that the value is obtained. In the case of the example, it can also be seen that an Ic value of 600 A / cm can be obtained with a film thickness of 2.2 μm.

以上の結果より、本発明を採用することにより、膜厚が厚い場合でも、結晶性に優れた酸化物超電導薄膜が得られ、Ｊｃが低下せず、厚膜化により高Ｉｃ値化が可能となることが確認できた。また、同等のＩｃ値を得るために必要な膜厚を低減することができるため、成膜コストの低減が可能となることが確認できた。   From the above results, by adopting the present invention, an oxide superconducting thin film excellent in crystallinity can be obtained even when the film thickness is large, Jc does not decrease, and a high Ic value can be achieved by increasing the film thickness. It was confirmed that In addition, it was confirmed that the film formation cost can be reduced because the film thickness required to obtain an equivalent Ic value can be reduced.

以上、本発明を実施の形態に基づいて説明したが、本発明は上記の実施の形態に限定されるものではない。本発明と同一および均等の範囲内において、上記の実施の形態に対して種々の変更を加えることができる。   While the present invention has been described based on the embodiments, the present invention is not limited to the above embodiments. Various modifications can be made to the above-described embodiments within the same and equivalent scope as the present invention.

１、２ 成膜装置
１１、１３、２３ ヒータ
１２、２２ スリット
Ｐ レーザプルーム
Ｔ 原料ターゲット
Ｗ テープ線材
ｄ１ ヒータとテープ線材との間隔
ｄ２ 壁とヒータの端部との間隔
Ｌ１ スリットの開口部の長さ
Ｌ２ ヒータの長さ 1, 2, Film formation apparatus 11, 13, 23 Heater 12, 22 Slit P Laser plume T Raw material target W Tape wire d 1 Space between heater and tape wire d 2 Space between wall and end of heater L 1 Opening of slit Part length L 2 Heater length

Claims (8)

気相薄膜合成法を用いて、基材上に機能性薄膜を成膜する機能性薄膜の成膜方法であって、
前記基材の成膜面側から加熱して機能性薄膜の成膜を行う
ことを特徴とする機能性薄膜の成膜方法。 A functional thin film forming method for forming a functional thin film on a substrate using a vapor phase thin film synthesis method,
A method for forming a functional thin film, wherein the functional thin film is formed by heating from the film forming surface side of the substrate. さらに、前記基材の成膜面と反対側の面からも加熱して機能性薄膜の成膜を行うことを特徴とする請求項１に記載の機能性薄膜の成膜方法。   2. The method for forming a functional thin film according to claim 1, wherein the functional thin film is formed by heating also from a surface opposite to the film forming surface of the substrate. 前記気相薄膜合成法が、レーザ堆積法であることを特徴とする請求項１または請求項２に記載の機能性薄膜の成膜方法。   The method for forming a functional thin film according to claim 1 or 2, wherein the vapor-phase thin film synthesis method is a laser deposition method. 前記機能性薄膜が、酸化物薄膜であることを特徴とする請求項１ないし請求項３のいずれか１項に記載の機能性薄膜の成膜方法。   The method for forming a functional thin film according to any one of claims 1 to 3, wherein the functional thin film is an oxide thin film. 前記酸化物薄膜が、酸化物超電導薄膜であることを特徴とする請求項４に記載の機能性薄膜の成膜方法。   The method for forming a functional thin film according to claim 4, wherein the oxide thin film is an oxide superconducting thin film. 気相薄膜合成法を用いて、基材上に機能性薄膜を成膜する機能性薄膜の成膜装置であって、
前記基材の成膜面側から前記基材を加熱する加熱手段を備えている
ことを特徴とする機能性薄膜の成膜装置。 A functional thin film forming apparatus for forming a functional thin film on a substrate using a vapor phase thin film synthesis method,
A functional thin film deposition apparatus comprising heating means for heating the substrate from the film deposition surface side of the substrate. さらに、前記基材の成膜面と反対側の面から前記基材を加熱する加熱手段を備えていることを特徴とする請求項６に記載の機能性薄膜の成膜装置。   The functional thin film deposition apparatus according to claim 6, further comprising heating means for heating the base material from a surface opposite to the film formation surface of the base material. 前記気相薄膜合成法が、レーザ堆積法であることを特徴とする請求項６または請求項７に記載の機能性薄膜の成膜装置。   The functional thin film deposition apparatus according to claim 6 or 7, wherein the vapor phase thin film synthesis method is a laser deposition method.
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