JP7357903B2 - Method for forming microfabricated oxide films - Google Patents
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特許法第３０条第２項適用 １．「水リフトオフプロセスによるβ－Ｇａ▲２▼Ｏ▲３▼薄膜の選択成長・マイクロパターニング及び特性評価」（１９ａ－２２４Ａ－１），２０１８年 第７９回応用物理学会秋季学術講演会［講演予稿集］，発行者 公益社団法人 応用物理学会，発行日 平成３０年９月５日 ２．「水リフトオフプロセスによるβ－Ｇａ▲２▼Ｏ▲３▼薄膜の選択成長・マイクロパターニング及び特性評価」（１９ａ－２２４Ａ－１），集会名 ２０１８年第７９回 応用物理学会秋季学術講演会，開催日 平成３０年９月１９日（会期：９月１８日～９月２０日），開催場所 名古屋国際会議場 ３．第２８回日本ＭＲＳ年次大会 アブストラクト「水リフトオフ法による微細加工されたβ－Ｇａ▲２▼Ｏ▲３▼薄膜の選択成長」（Ａ１－０１９－００９），ウェブサイト掲載日 平成３０年１２月５日，ウェブサイトのアドレス ｈｔｔｐｓ：／／ｗｗｗ．ｍｒｓ－ｊ．ｏｒｇ／ｍｅｅｔｉｎｇ２０１８／ａｂｓｔｒａｃｔ／ｊｐ／ｌｏｇｉｎ．ｐｈｐ ４．「水リフトオフ法による微細加工されたβ－Ｇａ▲２▼Ｏ▲３▼薄膜の選択成長」（Ａ１－０１９－００９），開催日 平成３０年１２月１９日（会期：１２月１８日～１２月２０日），北九州国際会議場・西日本総合展示場Application of Article 30, Paragraph 2 of the Patent Act 1. “Selective growth, micropatterning and property evaluation of β-Ga▲2▼O▲3▼ thin film by water lift-off process” (19a-224A-1), 2018 79th Japan Society of Applied Physics Autumn Academic Conference [Presentation proceedings] ], Publisher: Japan Society of Applied Physics, Public Interest Incorporated Association, Publication date: September 5, 2018 2. “Selective Growth, Micropatterning and Characteristic Evaluation of β-Ga▲2▼O▲3▼ Thin Films by Water Lift-off Process” (19a-224A-1), Meeting Name 2018 79th Japan Society of Applied Physics Autumn Academic Conference, Held Sunday, September 19, 2018 (Duration: September 18 to September 20), Venue: Nagoya International Conference Center 3. 28th Japan MRS Annual Conference Abstract “Selective growth of microfabricated β-Ga▲2▼O▲3▼ thin film by water lift-off method” (A1-019-009), Website publication date December 2018 5th, website address https://www. mrs-j. org/meeting2018/abstract/jp/login. php4. “Selective Growth of Microfabricated β-Ga▲2▼O▲3▼ Thin Films by Water Lift-off Method” (A1-019-009), Date: December 19, 2018 (Duration: December 18-12 (Mon. 20), Kitakyushu International Conference Center/West Japan General Exhibition Center
本発明は、酸化物からなる膜の選択的成長技術に関し、特に水リフトオフ法により微細加工された薄膜を形成する技術に係る。 The present invention relates to a technique for selectively growing a film made of an oxide, and particularly to a technique for forming a thin film microfabricated by a water lift-off method.
パワーデバイス材料として近年、酸化ガリウムが注目されている。
酸化ガリウムには、５種類の結晶形が知られていて、コランダム構造を有するα－Ｇａ２Ｏ３，βガリア構造と称されるβ－Ｇａ２Ｏ３等が例として挙げられる。
高温超電導材料分野にても、多くの酸化物の膜が提案されている。
例えば、Ｙ－Ｂａ－Ｃｕ－Ｏ系，Ｂｉ－Ｓｒ－Ｃａ－Ｃｕ－Ｏ系の材料が報告され、具体例としてはＹＢａ２Ｃｕ３Ｏ７－Ｘ，Ｂｉ２Ｓｒ２Ｃａ２Ｃｕ３Ｏ１０等があり、いろいろな酸化物の膜が検討されている。
酸化物の膜には、強誘電特性を示すものもあり、例えばＢａＴｉＯ３（チタン酸バリウム），Ｐｂ（Ｚｒ，Ｔｉ）Ｏ３（チタン酸ジルコン酸鉛）等が例として挙げられ、これらは圧電特性を有する。
Gallium oxide has attracted attention in recent years as a power device material.
Five types of crystal forms of gallium oxide are known, and examples thereof include α-Ga 2 O 3 having a corundum structure and β-Ga 2 O 3 called β-gallium structure.
Many oxide films have also been proposed in the field of high-temperature superconducting materials.
For example, Y-Ba-Cu-O based materials and Bi-Sr-Ca-Cu-O based materials have been reported, and specific examples include YBa 2 Cu 3 O 7-X , Bi 2 Sr 2 Ca 2 Cu 3 O 10 Various oxide films are being considered.
Some oxide films exhibit ferroelectric properties, such as BaTiO 3 (barium titanate) and Pb(Zr,Ti)O 3 (lead zirconate titanate), which are piezoelectric. have characteristics.
これらの酸化物の膜は、融点が高く、従来のレジスト材料を用いたレジストリフトオフ法を用いることができないため、微細加工された状態に成膜するのが難しいとされている。 Films of these oxides have high melting points, and resist lift-off methods using conventional resist materials cannot be used, so it is said that it is difficult to form films in a microfabricated state.
特許文献１には、基板上にフォトレジスト材料を用いたパターニングにより、基板／フォトレジスト材料表面を形成し、その上に水溶性材料を堆積した後に有機溶媒中にてフォトレジスト材料をリフトオフし、有機／無機材料を積層した後に水溶性材料をリフトオフさせるパターニング方法を開示するが、基板上に有機／無機材料をパターニングする目的であって、酸化物の膜を選択成長させるものではない。 Patent Document 1 discloses that a substrate/photoresist material surface is formed by patterning a photoresist material on a substrate, a water-soluble material is deposited thereon, and then the photoresist material is lifted off in an organic solvent. A patterning method is disclosed in which a water-soluble material is lifted off after stacking organic/inorganic materials, but the purpose is to pattern organic/inorganic materials on a substrate, and not to selectively grow an oxide film.
本発明は、所定の微細形状又はパターニングされた状態に成膜できる酸化物の膜の形成方法の提供を目的とする。 An object of the present invention is to provide a method for forming an oxide film that can be formed into a predetermined fine shape or patterned state.
本発明に係る微細加工された酸化物の膜の形成方法は、基板の表面にフォトレジスト材料を用いて所定の微細形状又はパターニングされたフォトレジスト層を形成するステップと、前記表面にａ－ＣａＯ膜（非晶質ＣａＯ膜）を形成するステップと、次に溶剤に浸漬し前記フォトレジスト層を有する部分を除去するステップと、次に前記表面に酸化物の膜を成長させるステップと、次に水に浸漬して前記ａ－ＣａＯ膜を有する部分を除去するステップとを有することを特徴とする。 The method for forming a microfabricated oxide film according to the present invention includes the steps of: forming a photoresist layer with a predetermined microshape or patterning on the surface of a substrate using a photoresist material; forming a film (amorphous CaO film), then immersing in a solvent to remove the portion having the photoresist layer, then growing an oxide film on the surface, and then The method is characterized by comprising the step of removing the portion having the a-CaO film by immersing it in water.
酸化物の膜は、各種ＰＶＤ（物理蒸着）により成膜されるが、本発明において微細加工された酸化物の膜と表現したのは、単に酸化物の膜を成膜するのではなく、例えばデバイス加工等、所定の微細形状あるいはパターニングされた状態に酸化物の膜を選択成長させることをいう。 Oxide films are formed by various types of PVD (physical vapor deposition), but what is referred to as a microfabricated oxide film in the present invention does not mean simply forming an oxide film; This refers to the selective growth of an oxide film in a predetermined fine shape or patterned state, such as in device processing.
本発明において、酸化物の膜は強誘電特性，圧電特性，高温超電導特性，半導体特性又は導電性のいずれかを有しているのが好ましい。
強誘電特性及び圧電特性を有するものとしては、ＢａＴｉＯ３，Ｐｂ（Ｚｒ，Ｔｉ）Ｏ３が挙げられ、高温超電導特性を有するものとしては、ＹＢａ２Ｃｕ３Ｏ７－Ｘ，Ｂｉ２Ｓｒ２Ｃａ２Ｃｕ３Ｏ１０等が例として挙げられる。
また、パワーデバイス材料としては、Ｇａ２Ｏ３が例として挙げられる。
導電性の酸化物としてはＳｒＲｕＯ３が例として挙げられる。
In the present invention, the oxide film preferably has ferroelectric properties, piezoelectric properties, high temperature superconducting properties, semiconductor properties, or conductivity.
Those with ferroelectric properties and piezoelectric properties include BaTiO 3 and Pb(Zr,Ti)O 3 , and those with high temperature superconducting properties include YBa 2 Cu 3 O 7-X and Bi 2 Sr 2 Ca. 2Cu3O10 etc. are mentioned as an example.
Moreover, as a power device material, Ga2O3 is mentioned as an example.
An example of the conductive oxide is SrRuO 3 .
本発明においては、所定の微細形状にあるいは微細にパターニングされた酸化物の成膜に対して融点が高く、水による潮解性に優れたａ－ＣａＯの堆積膜を水リフトオフ法の犠牲層に用いたので、精密に制御された選択成長膜を形成することができる。
例えば、ａ－ＣａＯはａ－ＭｇＯに比較して、約２９０倍の潮解レート（２１０ｎｍ／ｍｉｎ）を有する。
In the present invention, a deposited film of a-CaO, which has a high melting point and is excellent in deliquescence with water, is used as a sacrificial layer in the water lift-off method compared to the formation of an oxide film formed into a predetermined fine shape or finely patterned. Therefore, it is possible to form a selectively grown film that is precisely controlled.
For example, a-CaO has a deliquescence rate (210 nm/min) about 290 times higher than a-MgO.
本発明に係る微細加工された酸化物の膜の形成方法の例を以下、図に基づいて説明するが、本発明はこれに限定されない。 An example of the method for forming a microfabricated oxide film according to the present invention will be described below based on the drawings, but the present invention is not limited thereto.
図１に、評価したプロセスの流れを模式的に示す。
まず、ｃ面サファイア基板の表面にフォトリソグラフィによりレジスト材料を用いて、レジスト層をパターニングする（図１ａ）。
次に、図１（ｂ）に示すようにPulsed Laser Deposition（ＰＬＤ）法を用いて、ａ－ＣａＯの膜を堆積した。
次に、図１（ｃ）に示すようにアセントに浸漬し、レジスト層を有する部分を除去することで、ａ－ＣａＯ犠牲層がパターニングされる。
ａ－ＣａＯ層がパターニングされた基板の表面にＰＬＤ法を用い、６００℃の高温にて減圧下、β－Ｇａ２Ｏ３の膜を成膜した（図１ｄ）。
次に、ａ－ＣａＯ層を有する部分を純水に浸漬し、潮解させることでリフトオフさせた。
Figure 1 schematically shows the flow of the evaluated process.
First, a resist layer is patterned using a resist material on the surface of a c-plane sapphire substrate by photolithography (FIG. 1a).
Next, as shown in FIG. 1(b), an a-CaO film was deposited using the Pulsed Laser Deposition (PLD) method.
Next, as shown in FIG. 1C, the a-CaO sacrificial layer is patterned by immersing it in Ascent and removing the portion having the resist layer.
A β-Ga 2 O 3 film was formed on the surface of the substrate on which the a-CaO layer was patterned using the PLD method at a high temperature of 600° C. under reduced pressure (FIG. 1d).
Next, the part having the a-CaO layer was immersed in pure water to deliquesce and lift off.
上記のプロセスにて作製した試料（サンプル）の表面の電子顕微鏡画像を図２，図３に示す。
図２は、サファイア基板上にａ－ＣａＯの残渣がないか確認したものであり、パターニングされた以外の部位には、ａ－ＣａＯが認められなかった。
図３は、いろいろな微細形状の選択成長例を示す。
図４は、上記サンプルのＸＲＤの分析結果を示す。
β－Ｇａ２Ｏ３が配向成長されているのが分かる。
図５にＥＢＳＤによる解析結果を示し、図６のＡＦＭ像を示す。
これらの情報から、パターニング部における表面形状の変化や結晶性の劣化が見られないがことが確認できた。
Electron microscope images of the surface of the sample produced by the above process are shown in FIGS. 2 and 3.
In FIG. 2, it was confirmed that there was no a-CaO residue on the sapphire substrate, and no a-CaO was observed in areas other than the patterned areas.
FIG. 3 shows examples of selective growth of various fine features.
FIG. 4 shows the results of XRD analysis of the sample.
It can be seen that β-Ga 2 O 3 is grown in an oriented manner.
FIG. 5 shows the analysis results by EBSD, and the AFM image in FIG. 6 is shown.
From this information, it was confirmed that no change in surface shape or deterioration of crystallinity was observed in the patterned portion.
次に、ＰＺＴ：Ｐｂ（Ｚｒ，Ｔｉ）Ｏ３の膜を成膜した例を図７に示す。
基板上にＰＬＤ法により、ＳＲＯ（ＳｒＲｕＯ３）膜を成膜し、その上、本発明に係るプロセスを用いて、ＰＺＴの膜をパターニングした。
図７では、犠牲層にａ－ＣａＯを用いたものの他に、比較例としてａ－ＭｇＯを用いたもの及びＰＺＴを一様堆積させたサンプルを作製し、そのＰ－Ｅヒステリシスループを計測した。
図７中、ＣａＯで示したループは、犠牲層にａ－ＣａＯを用いたものを示し、ＭｇＯで示したループは犠牲層にａ－ＭｇＯを用いたものを示す。
また、ｃｆで示したループは、ＰＺＴを一様堆積させたものを示す。
このことから、ａ－ＣａＯの方がａ－ＭｇＯよりも電気特性の劣化が抑えられていることが分かる。
これは、ａ－ＣａＯの方がａ－ＭｇＯよりも水による潮解性に優れているためと推定される。
Next, FIG. 7 shows an example in which a PZT:Pb(Zr,Ti)O 3 film is formed.
An SRO (SrRuO 3 ) film was formed on the substrate by the PLD method, and then a PZT film was patterned using the process according to the present invention.
In FIG. 7, in addition to the sacrificial layer using a-CaO, samples using a-MgO and uniformly deposited PZT were prepared as comparative examples, and their PE hysteresis loops were measured.
In FIG. 7, loops indicated by CaO indicate those using a-CaO for the sacrificial layer, and loops indicated by MgO indicate those using a-MgO for the sacrificial layer.
Further, a loop indicated by cf indicates a uniformly deposited PZT.
From this, it can be seen that deterioration of electrical properties is suppressed more in a-CaO than in a-MgO.
This is presumed to be because a-CaO has better deliquescence with water than a-MgO.
Claims (2)
前記表面にａ－ＣａＯ膜を形成するステップと、
次に溶剤に浸漬し前記フォトレジスト層を有する部分を除去するステップと、
次に前記表面に酸化物の膜を成長させるステップと、
次に水に浸漬して前記ａ－ＣａＯ膜を有する部分を潮解レート２１０ｎｍ／ｍｉｎ以上で除去するステップとを有し、
前記酸化物の膜はβ－Ｇａ ２ Ｏ ３ であることを特徴とする微細加工された酸化物の膜の形成方法。 forming a photoresist layer with a predetermined fine shape or pattern using a photoresist material on the surface of the substrate;
forming an a-CaO film on the surface;
then immersing in a solvent to remove the portion having the photoresist layer;
then growing an oxide film on the surface;
Next, immersing in water to remove the part having the a-CaO film at a deliquescent rate of 210 nm/min or more ,
A method for forming a microfabricated oxide film, characterized in that the oxide film is β-Ga 2 O 3 .
前記表面にａ－ＣａＯ膜を形成するステップと、
次に溶剤に浸漬し前記フォトレジスト層を有する部分を除去するステップと、
次に前記表面に酸化物の膜を成長させるステップと、
次に水に浸漬して前記ａ－ＣａＯ膜を有する部分を潮解レート２１０ｎｍ／ｍｉｎ以上で除去するステップとを有し、
前記酸化物の膜はＰｂ（Ｚｒ，Ｔｉ）Ｏ ３ であることを特徴とする微細加工された酸化物の膜の形成方法。 forming a SrRuO 3 film on the surface of the substrate , and forming a photoresist layer with a predetermined fine shape or pattern using a photoresist material on the surface;
forming an a-CaO film on the surface;
then immersing in a solvent to remove the portion having the photoresist layer;
then growing an oxide film on the surface;
Next, immersing in water to remove the part having the a-CaO film at a deliquescent rate of 210 nm/min or more,
A method for forming a microfabricated oxide film, characterized in that the oxide film is Pb(Zr,Ti)O 3 .
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