JP2001156351A - Laminated-structure electrode, formation method therefor, and piezoelectric actuator - Google Patents
Laminated-structure electrode, formation method therefor, and piezoelectric actuatorInfo
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- JP2001156351A JP2001156351A JP33670099A JP33670099A JP2001156351A JP 2001156351 A JP2001156351 A JP 2001156351A JP 33670099 A JP33670099 A JP 33670099A JP 33670099 A JP33670099 A JP 33670099A JP 2001156351 A JP2001156351 A JP 2001156351A
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- Prior art keywords
- film
- electrode
- laminated
- substrate
- piezoelectric
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Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、積層構造電極、そ
の形成方法、及び、前記積層構造電極又は前記形成方法
によって形成された積層構造電極を用いた圧電アクチュ
エータに関し、より詳細には、セラミックス粒子をノズ
ルから基板に噴射し堆積膜を得るガスデポジション法成
膜において、圧電アクチュエータやセンサを製造するの
にふさわしい下地積層電極膜の構造及びその形成方法に
関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a laminated electrode, a method of forming the same, and a piezoelectric actuator using the laminated electrode or the laminated electrode formed by the forming method. The present invention relates to a structure of a base laminated electrode film suitable for manufacturing a piezoelectric actuator or a sensor and a method of forming the same in a gas deposition method for forming a deposited film by injecting a gas from a nozzle to a substrate.
【０００２】[0002]
【従来の技術】基板上に圧電セラミックス膜を配置し、
アクチュエータやセンサ素子に利用する試みが為されて
いる。ユニモルフ素子、バイモルフ素子として従来から
製品化されている素子は、各々の材料を接合して形成す
る為、素子の小型化にとって不向きであった。しかし、
近年、ガスデポジション法により、従来では作製が困難
であった圧電セラミックスの基板上への形成が可能にな
り、素子の小型化に有効であることが示されつつある。2. Description of the Related Art A piezoelectric ceramic film is arranged on a substrate,
Attempts have been made to use it for actuators and sensor elements. Conventionally, devices manufactured as a unimorph device and a bimorph device are not suitable for miniaturization of the device because they are formed by bonding respective materials. But,
In recent years, a gas deposition method has made it possible to form piezoelectric ceramics on a substrate, which was conventionally difficult to produce, and has been shown to be effective in miniaturizing elements.
【０００３】ガスデポジション法は、例えば、特許第１
６６０７９９号に記載されているように超微粒子を用い
た膜形成法である。真空蒸着法と同様に金属加熱源およ
び真空容器を配置させ、金属蒸気から超微粒子を形成
し、この超微粒子からなる膜を基板上に形成する。この
様なガスデポジション法による金属膜の形成は、Ｎｉ，
Ｃｕなどの配線材料で実用化され、具体的には、各種プ
リント配線基板の断線修復や半導体装置における表面実
装用パッド電極の形成などに用いられている。The gas deposition method is disclosed, for example, in Japanese Patent No.
This is a film formation method using ultrafine particles as described in Japanese Patent No. 660799. As in the case of the vacuum evaporation method, a metal heating source and a vacuum vessel are arranged, ultrafine particles are formed from metal vapor, and a film made of the ultrafine particles is formed on a substrate. Formation of a metal film by such a gas deposition method is performed by using Ni,
It is put to practical use with wiring materials such as Cu, and is specifically used for repairing disconnection of various printed wiring boards and forming pad electrodes for surface mounting in semiconductor devices.
【０００４】一方、金属材料とは異なり、酸化物セラミ
ックス材料の超微粒子を用いた膜形成も提案されてい
る。例えば、特開平３−９３６０６号公報には、Ｂｉ−
Ｐｂ−Ｓｒ−Ｃａ−Ｃｕ−Ｏからなる酸化物超伝導厚膜
の形成法が示されている。特開平４−１８８５０３号公
報には、ＢａＴｉＯ3セラミックス誘電体厚膜とその耐
圧を確保する為の高分子塗膜の複合膜に関する形成法が
示されている。特開平８−２３０１８１号公報、特開平
８−２６７７６３号公報には、ガスデポジション法によ
り鉛系圧電セラミックス素子を形成し、これを用いたイ
ンクジェット用プリンターヘッドへの展開が示されてい
る。[0004] On the other hand, unlike a metal material, a film formation using ultrafine particles of an oxide ceramic material has been proposed. For example, Japanese Patent Application Laid-Open No. 3-93606 discloses a Bi-
A method for forming an oxide superconducting thick film made of Pb-Sr-Ca-Cu-O is shown. Japanese Patent Application Laid-Open No. Hei 4-188503 discloses a method for forming a composite film of a BaTiO 3 ceramic dielectric thick film and a polymer coating film for securing the withstand voltage thereof. Japanese Patent Application Laid-Open Nos. Hei 8-230181 and Hei 8-267763 show development of a lead-based piezoelectric ceramic element formed by a gas deposition method and application to an ink jet printer head using the same.
【０００５】また、Ｊｐｎ.Ｊ.Ａｐｐｌ.Ｐｈｙｓ.Ｖｏ
ｌ.３６（１９９７）１１５９においては、Ｐｔ膜を堆
積したＳｉ基板上に、基板温度７００℃にてＰＺＴをガ
スデポジション成膜し、その後、９００℃程の高温にて
熱処理を施した例が示されているが、同文献中には、下
部電極膜を通過してＳｉとＰＺＴ膜の相互拡散が生じ、
ＰＺＴ膜特性が劣化することが示されている。[0005] Also, Jpn.J.Appl.Phys.Vo.
In 1.36 (1997) 1159, PZT is gas-deposited at a substrate temperature of 700 ° C. on a Si substrate on which a Pt film is deposited, and then heat treatment is performed at a high temperature of about 900 ° C. As shown in the document, mutual diffusion of Si and the PZT film occurs through the lower electrode film,
It is shown that the properties of the PZT film deteriorate.
【０００６】[0006]
【発明が解決しようとする課題】上述の様に、Ｓｉ基板
上に形成されるＰＺＴ圧電膜を電気−機械変換素子（圧
電アクチュエータ）として使用する際、各種の熱履歴
後、電極膜を介しての相互拡散による圧電性の劣化や、
プロセス中での膜剥離等の故障が発生し、安定した素子
を供給することが困難な状態にある。その原因は、基板
と電極膜の密着性不良、電極膜とガスデポジション圧電
膜の密着力不足、電極膜の鉛拡散、Ｓｉ拡散の素子能力
の低さ、等に起因していた。As described above, when a PZT piezoelectric film formed on a Si substrate is used as an electro-mechanical transducer (piezoelectric actuator), after various heat histories, the electrode film passes through the electrode film. Degradation of piezoelectricity due to mutual diffusion of
A failure such as film peeling during the process occurs, and it is difficult to supply a stable element. The causes were caused by poor adhesion between the substrate and the electrode film, insufficient adhesion between the electrode film and the gas deposition piezoelectric film, lead diffusion of the electrode film, and low element performance of Si diffusion.
【０００７】本発明は、上述のごとき実情に鑑みてなさ
れたもので、請求項１の発明は、圧電膜／電極界面での
剥離を防ぐ為の適正化された膜厚からなる電極膜を提供
すること、請求項２の発明は、圧電膜／電極界面での剥
離を防ぐ為の良好なＰｔ膜組織を提供すること、請求項
３の発明は、圧電膜／電極界面での剥離を防ぐ為の良好
な配向成長したＰｔ膜を提供すること、請求項４の発明
は、Ｓｉ基板上に配置した電極膜の剥離を防止し、か
つ、熱履歴に対し相互拡散を防げる電極膜構成を提供す
ること、請求項５の発明は、積層電極の各種の材料の薄
膜化において良好な作製方法を提供すること、請求項６
の発明は、請求項１乃至４に記載の電極対策が施された
電極膜の上に、ガスデポジション法によって形成された
圧電膜を有する圧電アクチュエータを提供すること、を
目的としてなされたものである。SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and the invention of claim 1 provides an electrode film having an optimized film thickness for preventing separation at a piezoelectric film / electrode interface. The invention of claim 2 provides a good Pt film structure for preventing peeling at the piezoelectric film / electrode interface, and the invention of claim 3 provides for preventing peeling at the piezoelectric film / electrode interface. The invention of claim 4 provides an electrode film configuration that prevents peeling of an electrode film disposed on a Si substrate and prevents mutual diffusion against thermal history. The invention of claim 5 provides a good manufacturing method in thinning various materials of the laminated electrode.
The object of the present invention is to provide a piezoelectric actuator having a piezoelectric film formed by a gas deposition method on an electrode film provided with the electrode measures described in claims 1 to 4. is there.
【０００８】[0008]
【課題を解決するための手段】請求項１の発明は、電極
膜を配置したＳｉ基板上にガスデポジション法で圧電体
膜を形成してなる積層構造電極において、前記電極膜は
１種以上の材料膜からなり、その膜厚が０.１５μｍよ
り厚い膜厚であることを特徴としたものである。According to a first aspect of the present invention, there is provided a laminated electrode having a piezoelectric film formed by a gas deposition method on a Si substrate on which an electrode film is disposed, wherein the electrode film comprises at least one kind of electrode film. And a film thickness of more than 0.15 μm.
【０００９】請求項２の発明は、電極膜を配置したＳｉ
基板上にガスデポジション法で圧電体膜を形成してなる
積層構造電極において、前記電極膜がＰｔ材料で、か
つ、粒径が０.１μｍ以上の粒組織からなることを特徴
としたものである。According to a second aspect of the present invention, there is provided a semiconductor device in which an electrode film is disposed.
In a laminated structure electrode in which a piezoelectric film is formed on a substrate by a gas deposition method, the electrode film is made of a Pt material and has a grain structure having a grain size of 0.1 μm or more. is there.
【００１０】請求項３の発明は、請求項２の発明におい
て、前記Ｐｔの電極膜が（１１１）面に優先配向し、そ
の配向度が７５％以上であることを特徴としたものであ
る。The invention of claim 3 is characterized in that, in the invention of claim 2, the Pt electrode film is preferentially oriented to the (111) plane, and the degree of orientation is 75% or more.
【００１１】請求項４の発明は、Ｓｉ基板上に電気的な
絶縁機能を有する絶縁膜を配置し、その上に、密着機能
を有する膜を積層し、その上に、電極膜としてＩｒ又は
ＩｒＯ2、又はこれら積層体のうちの少なくとも１つを
有し、さらに、その上に、Ｐｔ膜が堆積されていること
を特徴としたものである。According to a fourth aspect of the present invention, an insulating film having an electrical insulating function is disposed on a Si substrate, a film having an adhesion function is laminated thereon, and Ir or IrO is formed thereon as an electrode film. 2 or at least one of these laminates, and further, a Pt film is deposited thereon.
【００１２】請求項５の発明は、Ｓｉ基板上に電気的な
絶縁機能を有する膜を積層し、その上に、密着機能を有
する膜を積層し、その上に、電極膜としてＩｒ又はＩｒ
Ｏ2又はこれら積層体のうちの少なくとも１つを積層
し、さらに、その上に、Ｐｔ膜を積層する積層構造電極
の形成方法において、前記各膜を成膜する時の前記基板
温度を３００℃以上とすることを特徴としたものであ
る。According to a fifth aspect of the present invention, a film having an electrical insulation function is laminated on a Si substrate, a film having an adhesion function is laminated thereon, and Ir or Ir is formed thereon as an electrode film.
O 2 or by laminating at least one of these laminates, further thereon, the method for forming a stacked structure electrodes of laminating Pt film, 300 ° C. the substrate temperature when forming the respective films It is characterized by the above.
【００１３】請求項６の発明は、請求項１乃至４のいず
れかの電極膜の上、又は、請求項５の方法によって形成
された電極膜の上に、ガスデポジション法によりＰＺＴ
系圧電セラミックス膜を積層し、その上に、第２の電極
膜を配置してなることを特徴としたものである。According to a sixth aspect of the present invention, a PZT is formed by a gas deposition method on the electrode film of any one of the first to fourth aspects or on the electrode film formed by the method of the fifth aspect.
A piezoelectric ceramic film is laminated, and a second electrode film is disposed thereon.
【００１４】[0014]
【発明の実施の形態】（請求項１の発明）図１は、ガス
デポジション装置の一構成例を示す図で、図中、１１は
キャリアガスボンベ、１２はエアロゾルチェンバー、１
３はＰＺＴ圧電セラミックス微粒子、１４はデポジショ
ンチェンバー、１５はノズル、１６はパターンマスク、
１７は基板ホルダー、１８はＸ−Ｙ−Ｚθステージ、１
９はバキュームシステムで、成膜原理は、ＰＺＴ圧電セ
ラミックス微粒子１３をキャリアガス中に浮遊させてエ
アロゾル化し、このエアロゾルを高速で基板ホルダー１
７上の基板に噴射して膜形成するものである。ガスデポ
ジションＰＺＴ圧電セラミックスは、堆積後の６００℃
以上の熱処理による強誘電特性、ならびに、その後の分
極処理により圧電性が出現する。従って、基板材料なら
びに電極膜はこの温度以上の耐熱性や耐反応性を有する
必要がある。また、ガスデポジションＰＺＴ膜と強固な
密着力を発揮出来ることが要求される。窯業的知見に基
づき、Ｐｔ材料はＰＺＴセラミックスとの反応性が低
く、耐熱性があることから、従来から使用されている。
また、薄膜ＰＺＴの下部電極としても用いられてきた。DESCRIPTION OF THE PREFERRED EMBODIMENTS (Invention of Claim 1) FIG. 1 is a view showing an example of a configuration of a gas deposition apparatus, in which 11 is a carrier gas cylinder, 12 is an aerosol chamber, and 1 is an aerosol chamber.
3 is a PZT piezoelectric ceramic fine particle, 14 is a deposition chamber, 15 is a nozzle, 16 is a pattern mask,
17 is a substrate holder, 18 is an XYZ stage, 1
Reference numeral 9 denotes a vacuum system. The principle of film formation is that PZT piezoelectric ceramic fine particles 13 are suspended in a carrier gas to form an aerosol, and the aerosol is converted into a substrate holder 1 at high speed.
7 to form a film by spraying it on the substrate above. Gas deposited PZT piezoelectric ceramics are deposited at 600 ° C
Ferroelectric characteristics by the above heat treatment and piezoelectricity appear by the subsequent polarization treatment. Therefore, the substrate material and the electrode film need to have heat resistance and reaction resistance higher than this temperature. Further, it is required that a strong adhesion to the gas deposition PZT film can be exhibited. Based on ceramic knowledge, Pt materials have been used conventionally because of their low reactivity with PZT ceramics and heat resistance.
It has also been used as a lower electrode of a thin film PZT.
【００１５】しかし、前述のように、ＰＺＴ膜剥離など
の故障が存在し、安定した積層体を作製するのは困難で
あった。ガスデポジション膜と下地との密着力は、図２
に示すように、初期における衝突粒子が下地に食い込
む、いわゆる、アンカーリング効果にて強固な密着がな
される。従って、十分な食い込みを許容する下地電極膜
厚（０.１５μｍ以上）を提供することで、強固な密着
力が得られる。However, as described above, there was a failure such as peeling of the PZT film, and it was difficult to produce a stable laminate. Figure 2 shows the adhesion between the gas deposition film and the substrate.
As shown in (1), strong adhesion is achieved by the so-called anchoring effect, in which the collision particles in the initial stage bite into the base. Therefore, by providing a base electrode film thickness (0.15 μm or more) that allows sufficient penetration, a strong adhesion can be obtained.
【００１６】（請求項２の発明）Ｓｉ基板上にＰｔ膜を
スパッタリング法により成膜するが、その膜組織はスパ
ッタリング条件により変化する。このＰｔ膜にガスデポ
ジション法によってＰＺＴ膜を形成するが、その時、Ｐ
ＺＴ粒子がＰｔ膜に食い込むアンカーリング効果は、こ
のＰｔ膜の組織に大きく作用される。従って、成膜条件
を変化させることにより膜粒径を変化させ、その上にガ
スデポジション膜を堆積させ、その後に、膜の密着程度
を評価する。膜粒径は走査型電子顕微鏡（ＳＥＭ）にて
３００００倍の写真撮影を行い粒径を算出した。その結
果、Ｐｔ粒子の粒径が０.１μｍ以上の時に十分な密着
力が得られた。付着強度はテープ剥離試験をガスデポジ
ション成膜後の膜について実施する。(Invention of Claim 2) A Pt film is formed on a Si substrate by a sputtering method, and the structure of the film changes depending on the sputtering conditions. A PZT film is formed on this Pt film by a gas deposition method.
The anchoring effect of ZT particles digging into the Pt film is greatly affected by the structure of the Pt film. Therefore, the film diameter is changed by changing the film forming conditions, a gas deposition film is deposited thereon, and then the degree of adhesion of the film is evaluated. The particle diameter of the film was calculated by taking a photograph of 30,000 times with a scanning electron microscope (SEM). As a result, when the particle size of the Pt particles was 0.1 μm or more, sufficient adhesion was obtained. The adhesive strength is measured by performing a tape peeling test on the film after gas deposition.
【００１７】（請求項３の発明）Ｐｔ電極膜は、各種ス
パッタ条件により結晶配向が異なる。前記と同様な試験
を行い、強固な付着を得る為の膜配向を求めた。膜の配
向性はＸＲＤ測定を行い、Ｌｏｔｇｅｒｉｎｇの示した
計算法に従う。すなわち、ＸＲＤ２θ／θ測定を、２θ
が２０°〜８５°の範囲でスキャンさせ、検出される回
折ピークに対し、以下の計算を行う。無配向状態の回折
データはＪＣＰＤＳカードデータを用いる。(Invention of Claim 3) The crystal orientation of the Pt electrode film varies depending on various sputtering conditions. The same test as described above was performed, and the film orientation for obtaining strong adhesion was determined. The orientation of the film is measured by XRD and follows the calculation method shown by Lotgering. That is, the XRD2θ / θ measurement is
Is scanned in the range of 20 ° to 85 °, and the following calculation is performed on the detected diffraction peak. JCPDS card data is used as diffraction data in a non-oriented state.
【００１８】各結晶面からの反射（回折）強度をＩ（ｈ
ｋ ｌ）とし、それらの合計をΣＩ（ｈ ｋ ｌ）と
する。無配向状態における（１ １ １）反射強度の全
強度に対する割合をＰ０とすると、Ｐ０は式（１）で表
される。The reflection (diffraction) intensity from each crystal plane is represented by I (h
kl), and their sum is ΔI (hkl). Assuming that the ratio of the (11 1) reflection intensity in the non-aligned state to the total intensity is P0, P0 is represented by equation (1).
【００１９】[0019]
【数１】 (Equation 1)
【００２０】同じように、配向した膜からの反射強度に
ついても同様な計算を行い、その比をＰとすると、Ｐは
式（２）で表される。Similarly, the same calculation is performed for the reflection intensity from the oriented film, and when the ratio is P, P is expressed by equation (2).
【００２１】[0021]
【数２】 (Equation 2)
【００２２】前記式（１）、（２）で求めたＰ０とＰか
ら配向度Ｆを求めるが、その配向度Ｆは式（３）のよう
に定義される。The degree of orientation F is obtained from P0 and P obtained by the above equations (1) and (2). The degree of orientation F is defined as in equation (3).
【００２３】[0023]
【数３】 (Equation 3)
【００２４】実際の反射強度はピークの積分面積、また
は、ピーク高さより求めて良い。Ｐｔ膜の（１１１）配
向度が７５％以上の時に良好な密着力が得られる。これ
は、Ｐｔ膜強度が膜配向により変化し、結果として付着
力の向上にいたるものと考えられる。The actual reflection intensity can be obtained from the integrated area of the peak or the peak height. When the (111) orientation degree of the Pt film is 75% or more, good adhesion is obtained. This is considered to be due to the fact that the strength of the Pt film changes depending on the film orientation, and as a result, the adhesion is improved.
【００２５】（請求項４の発明）Ｐｔ電極膜は電気的に
絶縁体であるＳｉＯ2膜等の上に配置される。または、
直接Ｓｉ基板上に配置される。しかし、これら下地とＰ
ｔ膜との密着力は乏しいため、一般に、両者に相性の良
い密着膜が薄く配置される。この密着膜として、従来か
らＴｉ，Ｔａ，Ｃｒなどが用いられてきた。しかし、こ
れらの膜は６００℃以上の熱履歴により、Ｐｔ膜と反応
し、Ｐｔ膜内に取り込まれる、または、Ｐｔ膜を透過し
て来る酸素により酸化反応をし、密着膜としての機能を
低減させる。したがって、Ｐｔと密着膜との間にＩｔ系
材料からなる膜を配置することにより、このＰｔ膜の剥
離を防止する。Ｉｒ膜、または、ＩｒＯ2膜は導電性で
あり、本発明では、これら膜とＰｔ膜を電極膜として定
義している。Ｐｔ／Ｉｒ／密着膜／ＳｉＯ2／Ｓｉなる
基板に対し、ＰＺＴガスデポジション膜を形成し、熱処
理後のＰＺＴ膜の付着強度を試験する。(Invention of Claim 4) The Pt electrode film is disposed on an electrically insulating SiO 2 film or the like. Or
It is arranged directly on the Si substrate. However, these bases and P
Since the adhesion to the t film is poor, an adhesion film compatible with both is generally thinly arranged. Conventionally, Ti, Ta, Cr and the like have been used as this adhesion film. However, these films react with the Pt film due to a heat history of 600 ° C. or more, and undergo an oxidation reaction by oxygen taken in the Pt film or oxygen passing through the Pt film, thereby reducing the function as an adhesion film. Let it. Therefore, by disposing a film made of an It-based material between Pt and the adhesion film, the peeling of the Pt film is prevented. The Ir film or the IrO 2 film is conductive, and in the present invention, these films and the Pt film are defined as electrode films. A PZT gas deposition film is formed on a substrate of Pt / Ir / adhesion film / SiO 2 / Si, and the adhesion strength of the PZT film after the heat treatment is tested.
【００２６】（請求項５の発明）上述の様な密着膜を有
する積層膜を再現性よく安定して作製する為のスパッタ
リング条件のうち、基板温度を適正化する。密着膜、及
び、その上部に成膜される電極膜を基板温度３００℃以
上で成膜するのが密着膜／下地界面の剥離防止に効果的
であった。(Invention of claim 5) Among the sputtering conditions for stably producing a laminated film having the above-mentioned adhesion film with good reproducibility, the substrate temperature is optimized. Forming the adhesion film and the electrode film formed thereon at a substrate temperature of 300 ° C. or more was effective in preventing separation of the adhesion film / base interface.
【００２７】（請求項６の発明）上述の様な各対策を施
した電極膜の上にガスデポジション法によってＰＺＴ膜
を成膜し、熱処理を施し、その上に、上部電極を配置
し、分極処理を施す。次に、膜堆積面の裏面より、Ｓｉ
基板をエッチングして、部分的に薄層化した構造体を形
成する。電界印加に対する圧電歪みによる膜変形を計測
し、電気−機械変換素子（圧電アクチュエータ）の機能
を確認する。(Invention of claim 6) A PZT film is formed by a gas deposition method on the electrode film which has been subjected to the above-described countermeasures, and a heat treatment is performed, and an upper electrode is disposed thereon. A polarization process is performed. Next, from the back surface of the film deposition surface, Si
The substrate is etched to form a partially thinned structure. The film deformation due to the piezoelectric strain caused by the applied electric field is measured, and the function of the electromechanical transducer (piezoelectric actuator) is confirmed.
【００２８】実施例１（請求項１に対応） 表１にＰＺＴガスデポジション条件を示す。Example 1 (corresponding to claim 1) Table 1 shows PZT gas deposition conditions.
【００２９】[0029]
【表１】 [Table 1]
【００３０】図２は、Ｓｉ基板上への成膜例であるが、
ＰＺＴ粒子がＳｉ基板にめり込み、良好なアンカーリン
グ効果が得られている。この基板−膜遷移層の厚さは、
約０.１５μｍにおよんでいた。これよりアンカー効果
による密着力確保と、それを許容させる電極膜の厚さが
推定され、以下の実験を試みた。FIG. 2 shows an example of film formation on a Si substrate.
The PZT particles sink into the Si substrate, and a good anchoring effect is obtained. The thickness of this substrate-film transition layer is
It was about 0.15 μm. From this, it was estimated that the adhesion was secured by the anchor effect and the thickness of the electrode film that allowed the adhesion was estimated, and the following experiment was attempted.
【００３１】スパッタリングでＰｔ／Ｔｉ膜をＳｉＯ2
付きＳｉ基板上に成膜し、密着層Ｔｉ膜厚を５０ｎｍに
固定し、Ｐｔの膜厚をスパッタ時間を変化させることに
より、各種の膜厚を準備した。表２に、Ｐｔ膜厚とガス
デポジションＰＺＴ膜のテープ剥離試験の結果を示す。The Pt / Ti film is formed by sputtering using SiO 2
Various thicknesses were prepared by depositing a film on the Si substrate with the adhesive layer, fixing the thickness of the adhesion layer Ti to 50 nm, and changing the thickness of the Pt film by changing the sputtering time. Table 2 shows the results of the tape peeling test of the Pt film thickness and the gas deposition PZT film.
【００３２】[0032]
【表２】 [Table 2]
【００３３】実施例２（請求項２に対応） 表３に、Ｐｔ膜形成のスパッタリング条件を示す。ま
た、図３に典型的なＳＥＭ写真を示す。複数の写真撮影
を行い、無作為に直線を引き、この線に交わる粒子の径
を測定する。サンプル数は１００点以上行い、相加平均
から粒径を求めた。表４に、Ｐｔ膜粒径とガスデポジシ
ョンＰＺＴ膜のテープ剥離試験の結果を示す。Example 2 (corresponding to claim 2) Table 3 shows sputtering conditions for forming a Pt film. FIG. 3 shows a typical SEM photograph. A plurality of photographs are taken, a straight line is drawn at random, and the diameter of a particle intersecting this line is measured. The number of samples was 100 or more, and the particle size was determined from the arithmetic mean. Table 4 shows the results of the Pt film particle diameter and the tape peeling test of the gas deposition PZT film.
【００３４】[0034]
【表３】 [Table 3]
【００３５】[0035]
【表４】 [Table 4]
【００３６】実施例３（請求項３に対応） 図４に、典型的なＰｔ膜のＸＲＤパターンを示す。配向
度を極端に低下させる為に、配向度７０％以下のＰｔ膜
作製には、スパッタガスに微量のＯ2ガスを添加させ
た。Ｐｔ膜厚は０.３μｍである。表５に、Ｐｔ（１１
１）配向度とガスデポジションＰＺＴ膜のテープ剥離試
験の結果を示す。Embodiment 3 (corresponding to claim 3) FIG. 4 shows an XRD pattern of a typical Pt film. In order to extremely lower the degree of orientation, a small amount of O 2 gas was added to the sputtering gas for producing a Pt film having an degree of orientation of 70% or less. The Pt film thickness is 0.3 μm. Table 5 shows that Pt (11
1) The results of the degree of orientation and the tape peeling test of the gas deposition PZT film are shown.
【００３７】[0037]
【表５】 [Table 5]
【００３８】実施例４（請求項４に対応） 密着膜にＴａ、第１の電極にＩｒ、第２の電極にＰｔを
それぞれマグネトロンスパッタ法にて成膜した。層構成
はＰｔ（３００）／Ｉｒ（３００）／Ｔａ（１００）／
ＳｉＯ2（８００）／Ｓｉ基板である。ただし、（ ）
内の数字は厚さを示し、単位はｎｍである。ガスデポジ
ションＰＺＴ膜を成膜した後、第１のテープ剥離試験を
実施した。さらに、実プロセスに即した熱処理を行っ
た。処理温度は６００、６５０、７００℃の３水準で、
時間は２時間とした。熱処理後、テープ剥離試験を行っ
た。試料数は１０とした。比較として、次の試料：Ｐｔ
（６００）／Ｔｉ（１００）／ＳｉＯ2（８００）／Ｓ
ｉ、Ｐｔ（６００）／Ｔａ／ＳｉＯ2（８００）／Ｓｉ
について同様に行った。表６に、その結果を示す。表６
中の数字は剥離試験にて膜剥離が生じなかったものの数
を分子に、試料数を分母に示す。Example 4 (corresponding to claim 4) Ta was formed on the adhesion film, Ir was formed on the first electrode, and Pt was formed on the second electrode by magnetron sputtering. The layer structure is Pt (300) / Ir (300) / Ta (100) /
An SiO 2 (800) / Si substrate. However, ()
The numbers in parentheses indicate the thickness, and the unit is nm. After forming the gas deposition PZT film, a first tape peeling test was performed. Further, heat treatment was performed according to the actual process. The processing temperature is three levels of 600, 650 and 700 ° C.
The time was 2 hours. After the heat treatment, a tape peeling test was performed. The number of samples was 10. For comparison, the following sample: Pt
(600) / Ti (100) / SiO 2 (800) / S
i, Pt (600) / Ta / SiO 2 (800) / Si
Was performed similarly. Table 6 shows the results. Table 6
The numbers in the table indicate the number of samples that did not undergo film peeling in the peeling test as the numerator and the number of samples as the denominator.
【００３９】[0039]
【表６】 [Table 6]
【００４０】Ｔｉ密着層は熱処理中に酸化され、密着膜
としての機能を消失させる。Ｔａ膜も同様に好ましくな
い結果を示す。ただし、６５０℃以上ではＴｉより優位
である。Ｉｒ膜を配置することにより、密着膜の機能は
保持される。The Ti adhesion layer is oxidized during the heat treatment and loses its function as an adhesion film. Ta films also show undesirable results. However, it is superior to Ti at 650 ° C. or higher. By arranging the Ir film, the function of the adhesion film is maintained.
【００４１】実施例５（請求項５に対応） 表３に示した条件でスパッタリング成膜をした場合、ス
パッタ粒子のエネルギが各条件により変化し、膜質も変
化する。しかし、スパッタ圧力、ターゲット投入パワー
に対する膜質依存は少なく、主に、基板温度が膜質を決
定的に支配することがわかった。実施例４のＰｔ／Ｉｒ
／Ｔａ膜を各温度でスパッタ成膜し、６００℃熱処理後
のガスデポジションＰＺＴ膜剥離試験を行った。剥離し
た試料は全て密着膜／ＳｉＯ2界面で発生した。表７
に、その結果を示すが、全ての膜を３００℃以上で成膜
することで不良は発生しない。Example 5 (corresponding to claim 5) When a film is formed by sputtering under the conditions shown in Table 3, the energy of sputtered particles changes according to each condition, and the film quality also changes. However, it has been found that the film quality is less dependent on the sputtering pressure and the target input power, and the substrate temperature mainly determines the film quality. Pt / Ir of Example 4
A / Ta film was formed by sputtering at each temperature, and a gas deposition PZT film peeling test after heat treatment at 600 ° C. was performed. All of the peeled samples were generated at the interface between the adhesion film and SiO 2 . Table 7
The results are shown below, but no defect occurs when all the films are formed at 300 ° C. or higher.
【００４２】[0042]
【表７】 [Table 7]
【００４３】実施例６（請求項６に対応） 図５に示す構成のアクチュエータを作製した。図５にお
いて、上層から、上部電極（Ａｕ）２１，ガスデポジシ
ョンＰＺＴ（５０μｍ）２２，Ｐｔ／Ｉｒ／Ｔａ／Ｓｉ
Ｏ2２３，Ｓｉ基板（６５０μｍ）２４である。電極膜
等は前述の実施例４と同じである。また、裏面より堀加
工Ａを施した部位のＳｉ基板２４の厚さは１７０μｍで
ある。なお、図中、Ｄは６×６ｍｍ、ＰＺＴの幅ｄは５
×５ｍｍである。Example 6 (corresponding to claim 6) An actuator having the structure shown in FIG. 5 was manufactured. In FIG. 5, an upper electrode (Au) 21, a gas deposition PZT (50 μm) 22, Pt / Ir / Ta / Si,
O 2 23 and a Si substrate (650 μm) 24. The electrode film and the like are the same as those in the fourth embodiment. Further, the thickness of the Si substrate 24 at the portion where the moat processing A was performed from the back surface is 170 μm. In the drawing, D is 6 × 6 mm, and the width d of PZT is 5
× 5 mm.
【００４４】Ｓｉ基板２４上に各膜を成膜した（前述ま
での実施例と同じ条件）。次に、６００℃熱処理を行っ
た。ＰＺＴ面積とほぼ等しい面積で、上部電極２１をス
パッタリングにて成膜した。下地電極２３と上部電極２
１に電界を印加し、分極処理を行い、最後に、堀加工部
ＡをＫＯＨアルカリ溶液にてエッチング処理を行った。
０−１００Ｖのパルス信号を印加し、振動変位をレーザ
ー変位計で測定した。図６に、その結果を示す。図６に
示すように、試料は周辺固定端平板歪みに対応した理想
的な振動変位を示す。また、周波数帯域も広く１０ｋＨ
ｚ以上においても変位は一定であり、１００Ｖ印加時の
最大変位は１.６μｍであった。Each film was formed on the Si substrate 24 (under the same conditions as in the above-described embodiments). Next, a heat treatment at 600 ° C. was performed. The upper electrode 21 was formed by sputtering with an area approximately equal to the PZT area. Base electrode 23 and upper electrode 2
An electric field was applied to No. 1 to perform a polarization process. Finally, the trench A was etched with a KOH alkaline solution.
A pulse signal of 0 to 100 V was applied, and the vibration displacement was measured with a laser displacement meter. FIG. 6 shows the results. As shown in FIG. 6, the sample shows an ideal vibration displacement corresponding to the peripheral fixed end plate distortion. In addition, the frequency band is wide and 10 kHz
The displacement was constant even at z or more, and the maximum displacement when 100 V was applied was 1.6 μm.
【００４５】[0045]
【発明の効果】請求項１の発明は、電極膜を配置したＳ
ｉ基板上にガスデポジション法で圧電体膜を形成してな
る積層構造電極において、前記電極膜を１種以上の材料
膜とし、その膜厚を０.１５μｍより厚くすることによ
り、圧電膜／電極膜界面での剥離防止が出来た。According to the first aspect of the present invention, an S electrode having an electrode film is provided.
In a laminated electrode in which a piezoelectric film is formed on an i-substrate by a gas deposition method, the electrode film is made of one or more kinds of material films, and the film thickness is made larger than 0.15 μm. The separation at the electrode film interface was prevented.
【００４６】請求項２の発明は、電極膜を配置したＳｉ
基板上にガスデポジション法で圧電体膜を形成してなる
積層構造電極において、前記電極膜をＰｔ材料とし、か
つ、粒径を０.１μｍ以上の粒組織とすることにより、
圧電膜／電極膜界面での剥離防止が出来た。According to a second aspect of the present invention, there is provided a semiconductor device in which an electrode film is disposed.
In a laminated structure electrode in which a piezoelectric film is formed on a substrate by a gas deposition method, the electrode film is made of a Pt material and has a grain structure of 0.1 μm or more.
The separation at the piezoelectric film / electrode film interface was prevented.
【００４７】請求項３の発明は、請求項２の発明におい
て、前記Ｐｔの電極膜を（１１１）面に優先配向し、そ
の配向度を７５％以上とすることにより、圧電膜／電極
膜界面での剥離防止が出来た。According to a third aspect of the present invention, in the second aspect of the present invention, the Pt electrode film is preferentially oriented to the (111) plane, and the degree of orientation is set to 75% or more, whereby the piezoelectric film / electrode film interface is improved. Was able to prevent peeling.
【００４８】請求項４の発明は、Ｓｉ基板上に電気的な
絶縁機能を有する膜、その上に、密着機能を有する膜、
その上に、電極膜としてＩｒ又はＩｒＯ2又はこれら積
層体のうちの少なくとも１つを有し、さらに、その上
に、Ｐｔ膜が堆積されているようにしたので、密着膜機
能の低減が防止され、密着膜／下地界面剥離が防止でき
た。According to a fourth aspect of the present invention, there is provided a film having an electrical insulation function on a Si substrate, a film having an adhesion function thereon,
Further, Ir or IrO 2 or at least one of these laminates is provided as an electrode film, and a Pt film is further deposited thereon, so that the function of the adhesion film is prevented from being reduced. As a result, peeling of the adhesion film / base interface was prevented.
【００４９】請求項５の発明は、Ｓｉ基板上に電気的な
絶縁機能を有する膜を積層し、その上に、密着機能を有
する膜を積層し、その上に、電極膜としてＩｒ又はＩｒ
Ｏ2又はこれら積層体のうちの少なくとも１つを積層
し、さらに、その上に、Ｐｔ膜を積層する積層構造電極
の形成方法において、前記各膜を成膜する時の前記Ｓｉ
基板の温度を３００℃以上としたので、密着膜機能の低
減が防止され、密着膜／下地界面剥離が防止できる、電
気−機械変換素子が出来た。According to a fifth aspect of the present invention, a film having an electrical insulation function is laminated on a Si substrate, a film having an adhesion function is laminated thereon, and Ir or Ir is formed thereon as an electrode film.
O 2 or at least one of these laminates is laminated, and a Pt film is further laminated thereon to form a laminated electrode.
Since the temperature of the substrate was set to 300 ° C. or higher, an electromechanical conversion element capable of preventing a decrease in the function of the adhesive film and preventing peeling of the interface between the adhesive film and the underlayer was obtained.
【００５０】請求項６の発明は、請求項１乃至４のいず
れかに記載の電極膜の上、又は、請求項５記載の電極膜
形成方法により形成されるＳｉ基板上の電極層の上に、
ガスデポジション法によりＰＺＴ系圧電セラミックス膜
が積層され、その上に、第２の電極膜が配置されるよう
にしたので、密着膜機能の低減が防止され、密着膜／下
地界面剥離が防止できる、電気−機械変換素子が出来
た。According to a sixth aspect of the present invention, there is provided an electrode film according to any one of the first to fourth aspects, or an electrode layer on a Si substrate formed by the electrode film forming method according to the fifth aspect. ,
Since the PZT-based piezoelectric ceramic film is laminated by the gas deposition method, and the second electrode film is disposed thereon, reduction in the function of the adhesive film is prevented, and peeling of the interface between the adhesive film and the base can be prevented. Thus, an electro-mechanical conversion element was completed.
【図１】 ガスデポジション装置の一構成例を示す図で
ある。FIG. 1 is a diagram showing an example of a configuration of a gas deposition device.
【図２】 Ｓｉ基板上への成膜例を示す図である。FIG. 2 is a view showing an example of film formation on a Si substrate.
【図３】 典型的なＳＥＭ写真を示す図である。FIG. 3 is a view showing a typical SEM photograph.
【図４】 典型的なＰｔ膜のＸＲＤパターンを示す図で
ある。FIG. 4 is a view showing an XRD pattern of a typical Pt film.
【図５】 本発明による圧電アクチュエータの一例を示
す図である。FIG. 5 is a diagram showing an example of a piezoelectric actuator according to the present invention.
【図６】 本発明による圧電アクチュエータの振動変位
を示す図である。FIG. 6 is a diagram showing a vibration displacement of a piezoelectric actuator according to the present invention.
１１…キャリアガスボンベ、１２…エアロゾルチェンバ
ー、１３…ＰＺＴ圧電セラミックス微粒子、１４…デポ
ジションチェンバー、１５…ノズル、１６…パターンマ
スク、１７…基板ホルダー、１８…Ｘ−Ｙ−Ｚθステー
ジ、１９…バキュームシステム、２１…上部電極、２２
…ガスデポジションＰＺＴ、２３…Ｐｔ／Ｉｒ／Ｔａ／
ＳｉＯ2膜、２４…Ｓｉ基板。11 ... Carrier gas cylinder, 12 ... Aerosol chamber, 13 ... PZT piezoelectric ceramic fine particles, 14 ... Deposition chamber, 15 ... Nozzle, 16 ... Pattern mask, 17 ... Substrate holder, 18 ... XYZZ stage, 19 ... Vacuum system , 21 ... upper electrode, 22
... Gas deposition PZT, 23 ... Pt / Ir / Ta /
SiO 2 film, 24 ... Si substrate.
Claims (6)
ジション法で圧電体膜を形成してなる積層構造電極にお
いて、前記電極膜は１種以上の材料からなり、膜厚が
０.１５μｍより厚いことを特徴とする積層構造電極。1. A laminated structure electrode in which a piezoelectric film is formed by a gas deposition method on a Si substrate on which an electrode film is disposed, wherein the electrode film is made of at least one material and has a thickness of 0.15 μm. A laminated electrode characterized by being thicker.
ジション法で圧電体膜を形成してなる積層構造電極にお
いて、前記電極膜がＰｔ材料で、かつ、粒径が０.１μ
ｍ以上の粒組織からなることを特徴とする積層構造電
極。2. A laminated electrode comprising a piezoelectric film formed by a gas deposition method on a Si substrate on which an electrode film is disposed, wherein the electrode film is made of a Pt material and has a particle size of 0.1 μm.
A laminated electrode comprising a grain structure of m or more.
配向し、その配向度が７５％以上であることを特徴とす
る請求項２記載の積層構造電極。3. The laminated structure electrode according to claim 2, wherein the Pt electrode film is preferentially oriented to the (111) plane, and the degree of orientation is 75% or more.
絶縁膜、その上に、密着機能を有する密着機能膜、その
上に、電極膜としてＩｒ又はＩｒＯ2又はこれら積層体
のうちの少なくとも１つを有し、さらに、その上に、Ｐ
ｔ膜が堆積されていることを特徴とする積層構造電極。4. An insulating film having an electrical insulating function on a Si substrate, an adhesive function film having an adhesive function on the insulating film, and an electrode film made of Ir or IrO 2 or at least one of these laminates. Have one, and additionally, P
A laminated structure electrode having a t film deposited thereon.
膜を積層し、その上に、密着機能を有する膜を積層し、
その上に、電極膜としてＩｒ又はＩｒＯ2又はこれら積
層体のうちの少なくとも１つを積層し、さらに、その上
にＰｔ膜を積層する積層構造電極の形成方法であって、
前記各膜を成膜する時の前記基板温度を３００℃以上と
することを特徴とする積層構造電極の形成方法。5. A film having an electrical insulating function is laminated on a Si substrate, and a film having an adhesion function is laminated thereon.
A method for forming a laminated electrode, on which Ir or IrO 2 or at least one of these laminates is laminated as an electrode film, and further, a Pt film is laminated thereon.
A method of forming a laminated structure electrode, wherein the substrate temperature at which each of the films is formed is 300 ° C. or higher.
膜の上、又は、請求項５記載の形成方法により形成され
たＳｉ基板上の電極層の上に、ガスデポジション法によ
りＰＺＴ系圧電セラミックス膜が積層され、その上に第
２の電極膜が配置されていることを特徴とする圧電アク
チュエータ。6. PZT by gas deposition on the electrode film according to claim 1 or on the electrode layer on the Si substrate formed by the method according to claim 5. A piezoelectric actuator, wherein a system piezoelectric ceramic film is laminated, and a second electrode film is disposed thereon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33670099A JP2001156351A (en) | 1999-11-26 | 1999-11-26 | Laminated-structure electrode, formation method therefor, and piezoelectric actuator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP33670099A JP2001156351A (en) | 1999-11-26 | 1999-11-26 | Laminated-structure electrode, formation method therefor, and piezoelectric actuator |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2001156351A true JP2001156351A (en) | 2001-06-08 |
Family
ID=18301906
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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| JP2004014933A (en) * | 2002-06-10 | 2004-01-15 | Matsushita Electric Ind Co Ltd | Piezo-electric element and method of manufacturing the same |
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| JP2005101577A (en) * | 2003-09-01 | 2005-04-14 | Fuji Photo Film Co Ltd | Laminate structure, piezoelectric actuator, and manufacturing method thereof |
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| JP2004014933A (en) * | 2002-06-10 | 2004-01-15 | Matsushita Electric Ind Co Ltd | Piezo-electric element and method of manufacturing the same |
| JP2004120320A (en) * | 2002-09-26 | 2004-04-15 | Fuji Photo Film Co Ltd | Ultrasonic transducer array and its manufacturing method |
| JP2004207692A (en) * | 2002-12-09 | 2004-07-22 | Seiko Epson Corp | Piezoelectric device, liquid discharge head, ferroelectric device, electronic device, and method for manufacturing them |
| JP4507564B2 (en) * | 2002-12-09 | 2010-07-21 | セイコーエプソン株式会社 | Method for manufacturing piezoelectric device, method for manufacturing liquid discharge head, and method for manufacturing liquid discharge apparatus |
| US7579251B2 (en) | 2003-05-15 | 2009-08-25 | Fujitsu Limited | Aerosol deposition process |
| JP2005101577A (en) * | 2003-09-01 | 2005-04-14 | Fuji Photo Film Co Ltd | Laminate structure, piezoelectric actuator, and manufacturing method thereof |
| US7673385B2 (en) | 2003-09-01 | 2010-03-09 | Fujifilm Corporation | Laminated structure method |
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| US10374140B2 (en) | 2015-12-17 | 2019-08-06 | Seiko Epson Corporation | Piezoelectric device for ultrasonic sensor |
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