JP3111565B2 - Method of forming lead zirconate film - Google Patents
Method of forming lead zirconate filmInfo
- Publication number
- JP3111565B2 JP3111565B2 JP03334104A JP33410491A JP3111565B2 JP 3111565 B2 JP3111565 B2 JP 3111565B2 JP 03334104 A JP03334104 A JP 03334104A JP 33410491 A JP33410491 A JP 33410491A JP 3111565 B2 JP3111565 B2 JP 3111565B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- pbzro
- lead zirconate
- substrate
- temperature
- 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
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
Description
【０００１】[0001]
【産業上の利用分野】この発明は、基材上にジルコン酸
鉛（ＰｂＺｒＯ3）膜を容易かつ確実に形成する方法に
関する。BACKGROUND OF THE INVENTION This invention relates to a method of easily and reliably form a lead zirconate (PbZrO 3) film on the substrate.
【０００２】[0002]
【従来の技術】ジルコン酸鉛（ＰｂＺｒＯ3）は、代表
的な反強誘電体材料であり、強誘電体材料、圧電体材
料、焦電体材料として種々の用途に広く利用されている
チタン酸ジルコン酸鉛（Ｐｂ（Ｔｉ，Ｚｒ）Ｏ3）の端
成分として知られている。2. Description of the Related Art Lead zirconate (PbZrO 3 ) is a typical antiferroelectric material, and titanic acid is widely used as a ferroelectric material, a piezoelectric material and a pyroelectric material in various applications. It is known as an end component of lead zirconate (Pb (Ti, Zr) O 3 ).
【０００３】また、ＰｂＺｒＯ3は、Ｐｂ（Ｔｉ，Ｚ
ｒ）Ｏ3固溶体膜の出発材料や機能傾斜性材料の一成分
として利用できるものであり、また、大変位量を生み出
すアクチュエータとしての応用の可能性を秘めた材料と
しても注目されている。[0003] PbZrO 3 is composed of Pb (Ti, Z
r) It can be used as a starting material of an O 3 solid solution film or as a component of a functionally graded material, and is also attracting attention as a material that has the potential of being applied as an actuator that produces a large displacement.
【０００４】そして、従来のＰｂＺｒＯ3膜の形成方法
としては、主として、 例えば、スパッタリング法やイオンプレーティング法
などの物理蒸着法（ＰＶＤ法）、 薄膜材料である有機金属気体の熱分解，酸化，還元，
重合などにより、薄膜組成を基材上に沈着させて薄膜を
形成する化学蒸着法（ＣＶＤ法）、 有機金属を基材に塗布し、これを焼成して酸化物膜を
形成する、いわゆる、ゾル・ゲル法などに代表される有
機金属塗布法などが用いられている。Conventional methods for forming a PbZrO 3 film include, for example, a physical vapor deposition method (PVD method) such as a sputtering method and an ion plating method, thermal decomposition, oxidation, and the like of an organic metal gas as a thin film material. reduction,
A chemical vapor deposition method (CVD method) in which a thin film composition is deposited on a base material by polymerization or the like to form a thin film. An organic metal is applied to the base material and baked to form an oxide film. -An organic metal coating method represented by a gel method or the like is used.
【０００５】[0005]
【発明が解決しようとする課題】しかし、の物理蒸着
法においては、一般に、結晶質の膜を得るために、基板
などの基材の温度を５００℃以上にすることが必要であ
り、基材が高温にさらされるため基材の材質が著しく制
約されるとともに、基材を冷却する工程で熱歪が蓄積さ
れ、形成されたジルコン酸鉛膜にクラックや剥離が生じ
やすいという問題点がある。また、蒸着物質の蒸発は低
酸素分圧下で行われるため、生成したジルコン酸鉛膜は
酸素欠陥を有することが多く、特性の劣化やばらつきが
生じるという問題点がある。However, in the physical vapor deposition method, it is generally necessary to raise the temperature of a substrate such as a substrate to 500 ° C. or higher in order to obtain a crystalline film. Is exposed to a high temperature, so that the material of the base material is significantly restricted, and thermal strain is accumulated in the step of cooling the base material, and cracks and peeling are likely to occur in the formed lead zirconate film. In addition, since the evaporation of the deposition material is performed under a low oxygen partial pressure, the generated lead zirconate film often has oxygen vacancies, which causes a problem that characteristics are deteriorated or varied.
【０００６】さらに、ジルコン酸鉛（ＰｂＺｒＯ3）の
ような複合酸化物の薄膜を形成する場合には、元素によ
って蒸発速度が異なるため、膜の組成を制御して目標と
する組成の複合酸化物を得ることが困難であるという問
題点がある。また、膜の成長が遅いということもこの方
法の重大な欠点である。Further, when a thin film of a composite oxide such as lead zirconate (PbZrO 3 ) is formed, the evaporation rate varies depending on the element. Is difficult to obtain. Slow film growth is also a significant drawback of this method.
【０００７】一方、の化学蒸着法においては、有機金
属の蒸発温度が比較的高く、大掛かりな設備が必要にな
るという問題点があり、また、上記の物理蒸着法の場合
と同様に、膜の組成を制御することが困難で、目標とす
る組成の膜を形成することが容易ではないという問題点
がある。さらに、原料である有機金属化合物が極めて高
価であるという欠点がある。On the other hand, in the chemical vapor deposition method, there is a problem that the evaporation temperature of the organic metal is relatively high and large-scale equipment is required. There is a problem that it is difficult to control the composition and it is not easy to form a film having a target composition. Further, there is a disadvantage that the organometallic compound as a raw material is extremely expensive.
【０００８】また、の有機金属塗布法においては、基
材に塗布された有機金属を酸化して酸化物膜を形成する
のに５００℃以上の高温で焼成を行うことが必要であ
り、基材が高温にさらされるため基材の材質が著しく制
約されるとともに、乾燥及び焼成の工程で塗布膜に大き
な収縮が生じ、形成される膜にクラックや剥離が生じや
すいという問題点がある。In addition, in the organic metal coating method, it is necessary to perform firing at a high temperature of 500 ° C. or more to oxidize the organic metal applied to the substrate to form an oxide film. Is exposed to a high temperature, so that the material of the base material is significantly restricted, and a large shrinkage occurs in the coating film in the drying and baking steps, so that the formed film is liable to crack and peel off.
【０００９】また、焼成工程中の有機物質の蒸発や燃焼
によってポーラスになり、緻密な膜を得ることが困難で
あるという問題点がある。There is also a problem that the organic substance becomes porous due to evaporation and combustion during the firing step, and it is difficult to obtain a dense film.
【００１０】この発明は、上記従来のジルコン酸鉛（Ｐ
ｂＺｒＯ3）膜の形成方法の問題点を解決するものであ
り、ジルコン酸鉛膜を低温で、かつ、後処理工程を必要
とせずに、任意の形状の基材上に形成することが可能な
ジルコン酸鉛膜の形成方法を提供することを目的とす
る。The present invention relates to the above conventional lead zirconate (P)
The present invention solves the problems of the bZrO 3 ) film forming method, and can form a lead zirconate film on a base material of an arbitrary shape at a low temperature without requiring a post-treatment step. An object of the present invention is to provide a method for forming a lead zirconate film.
【００１１】[0011]
【課題を解決するための手段】上記目的を達成するため
に、この発明のジルコン酸鉛（ＰｂＺｒＯ3）膜の形成
方法は、０．１mol／l 以上の鉛（Ｐｂ）イオンまたは
サスペンジョンと、０．１mol／l 以上のジルコニウム
（Ｚｒ）イオンまたはサスペンジョンとを含有し、か
つ、ｐＨが１４以上のアルカリ性水溶液中に基材を浸漬
し、２００℃以上の温度で水熱処理を施すことにより、
ジルコン酸鉛（ＰｂＺｒＯ3）膜を前記基材の表面に形
成することを特徴とする。In order to achieve the above object, a method for forming a lead zirconate (PbZrO 3 ) film according to the present invention comprises the steps of: forming a lead (Pb) ion or suspension of 0.1 mol / l or more; By immersing the substrate in an alkaline aqueous solution containing at least 1 mol / l zirconium (Zr) ion or suspension and having a pH of 14 or more, and performing a hydrothermal treatment at a temperature of 200 ° C. or more,
A lead zirconate (PbZrO 3 ) film is formed on the surface of the substrate.
【００１２】[0012]
【実施例】以下に、この発明の実施例を比較例とともに
示して、この発明の特徴をさらに詳しく説明する。Hereinafter, the features of the present invention will be described in more detail with reference to Examples of the present invention and Comparative Examples.
【００１３】所定のＰｂ濃度及びＺｒ濃度を与える量の
硝酸鉛（Ｐｂ（ＮＯ3）2）及びオキシ硝酸ジルコニウム
（ＺｒＯ（ＮＯ3）2・Ｈ2Ｏ）の水溶液をＮａＯＨでｐ
Ｈ≧１４に調整することにより処理溶液を調製する。な
お、Ｐｂ及びＺｒは、イオンとして存在している場合に
限らず、サスペンジョンとして存在していてもよい。こ
の処理溶液をオートクレーブに入れ、これに清浄で、表
面を平滑に研磨したチタン（Ｔｉ）基板（基材）を浸漬
して加熱し、処理溶液及びチタン基板を所定の温度にま
で昇温する。その後、一定時間この温度に保持し、オー
トクレーブ内の処理溶液とチタン基板を反応させて水熱
合成を行い、チタン基板の表面にジルコン酸鉛（ＰｂＺ
ｒＯ3）膜を形成させる。反応後、チタン基板を取り出
し、蒸留水中で十分に超音波洗浄し、１２０℃で６０分
間乾燥する。An aqueous solution of lead nitrate (Pb (NO 3 ) 2 ) and zirconium oxynitrate (ZrO (NO 3 ) 2 .H 2 O) in an amount giving a predetermined Pb concentration and a Zr concentration is added with NaOH.
A treatment solution is prepared by adjusting H ≧ 14. Note that Pb and Zr are not limited to being present as ions, but may also be present as suspensions. This processing solution is placed in an autoclave, and a titanium (Ti) substrate (base material) having a clean and smooth surface is immersed in the autoclave and heated to heat the processing solution and the titanium substrate to a predetermined temperature. Thereafter, the temperature is maintained at this temperature for a certain period of time, and the treatment solution in the autoclave is reacted with the titanium substrate to perform hydrothermal synthesis, and lead zirconate (PbZ
(rO 3 ) film is formed. After the reaction, the titanium substrate is taken out, sufficiently subjected to ultrasonic cleaning in distilled water, and dried at 120 ° C. for 60 minutes.
【００１４】そして、このようにして得られた実施例及
び比較例の試料について、その表面に形成された薄膜の
評価を行った。The thin films formed on the surfaces of the thus obtained samples of Examples and Comparative Examples were evaluated.
【００１５】表１に、反応温度（水熱合成温度）、反応
時間、Ｐｂイオン濃度、Ｚｒイオン濃度、ｐＨなどの反
応条件をパラメータとする種々の条件下で形成した薄膜
について測定した、ＰｂＺｒＯ3相の生成量と未知相を
含むＰｂＺｒＯ3相以外の相（異相）の生成量の関係を
示す。Table 1 shows PbZrO 3 measured for thin films formed under various conditions using reaction conditions such as reaction temperature (hydrothermal synthesis temperature), reaction time, Pb ion concentration, Zr ion concentration, and pH as parameters. The relationship between the generation amount of the phase and the generation amount of a phase (heterophase) other than the PbZrO 3 phase including the unknown phase is shown.
【００１６】[0016]
【表１】 [Table 1]
【００１７】但し、表１において、試料番号に＊印を付
したものは、この発明の範囲外の膜（比較例）を示す。However, in Table 1, samples marked with an asterisk (*) indicate a film (comparative example) outside the scope of the present invention.
【００１８】表１において、ＰｂＺｒＯ3相及び異相の
生成量の値は、ＣｕＫα線（４０ｋＶ，１００ｍＡ）を
用いたＸ線回折法により、ＰｂＺｒＯ3相及び異相によ
る回折Ｘ線の積分強度を測定し、その値をそれぞれの全
測定値の中の最大値で規格化した値である。[0018] In Table 1, the values of PbZrO 3 phase and secondary phase of production amount, CuKa ray (40 kV, 100 mA) by X-ray diffractometry using to measure the integrated intensity of diffracted X-rays by PbZrO 3 phase and secondary phase , Are values normalized by the maximum value of all the measured values.
【００１９】表１より、Ｐｂイオン濃度，Ｚｒイオン濃
度，ｐＨ，反応温度が、ＰｂＺｒＯ 3膜の生成量に関係
していることがわかる。すなわち、Ｐｂイオン濃度及び
Ｚｒイオン濃度が０．１mol／l より低い場合、ＰｂＺ
ｒＯ3膜は生成せず、また、ｐＨが１４未満の場合に
も、ＰｂＺｒＯ3膜は生成しない。As shown in Table 1, the Pb ion concentration and Zr ion concentration
Degree, pH and reaction temperature are PbZrO 3Related to film production
You can see that it is doing. That is, the Pb ion concentration and
When the Zr ion concentration is lower than 0.1 mol / l, PbZ
rOThreeIf no membrane is formed and the pH is less than 14,
Also PbZrOThreeNo film is formed.
【００２０】また、Ｐｂイオン濃度及びＺｒイオン濃度
が０．１mol／l 以上で、かつ、ｐＨが１４以上の場合
には、特に表１には示さないが、反応温度が２００℃以
下（例えば１７５℃）でも、ある程度のＰｂＺｒＯ3膜
の生成は認められるが、ＰｂＺｒＯ3相の生成量よりも
異相の生成量のほうが多い。When the Pb ion concentration and the Zr ion concentration are 0.1 mol / l or more and the pH is 14 or more, although not shown in Table 1, the reaction temperature is 200 ° C. or less (for example, 175 ° C.). C), the formation of a PbZrO 3 film to some extent is recognized, but the amount of the hetero-phase formed is larger than the amount of the PbZrO 3 phase formed.
【００２１】一方、Ｐｂイオン濃度及びＺｒイオン濃度
が０．１mol／l 以上で、ｐＨが１４以上の処理溶液を
用いて２００℃以上の温度条件下で水熱反応を行わせた
場合は、反応時間にかかわらず、ほぼ単一層のＰｂＺｒ
Ｏ3膜を得ることができる。On the other hand, when the Pb ion concentration and the Zr ion concentration are 0.1 mol / l or more and the hydrothermal reaction is carried out at a temperature of 200 ° C. or more using a treatment solution having a pH of 14 or more, Regardless of time, almost single layer PbZr
An O 3 film can be obtained.
【００２２】なお、図１に、生成膜のＸ線回折パターン
を示す（但し、反応条件は、Ｐｂイオン濃度＝０．５mo
l／l ，Ｚｒイオン濃度＝０．５mol／l ，ｐＨ＝１４，
反応温度＝３００℃，処理時間＝３０分である）。図１
より、上記反応条件下において得られる膜は、ＰｂＺｒ
Ｏ3相以外の相（異相）の少ないほぼ単一層のＰｂＺｒ
Ｏ3であることがわかる。FIG. 1 shows an X-ray diffraction pattern of the resulting film (provided that the reaction conditions are Pb ion concentration = 0.5 mol / l).
l / l, Zr ion concentration = 0.5 mol / l, pH = 14,
Reaction temperature = 300 ° C., treatment time = 30 minutes). FIG.
Thus, the film obtained under the above reaction conditions is PbZr
Almost single layer PbZr with few phases (heterophase) other than O 3 phase
O 3 and it can be seen.
【００２３】なお、上記実施例では、基材としてチタン
基板を用い、その表面に水熱合成によりＰｂＺｒＯ3膜
を形成した場合について説明したが、基材については、
それを構成する材料の種類に特別の制約はなく、処理溶
液に対する耐食性と、水熱反応温度に対する耐熱性を有
する無機材料、金属材料、有機材料及びこれらの複合材
料などの種々の材料からなる基材を用いることが可能で
ある。In the above embodiment, a case was described in which a titanium substrate was used as a base material and a PbZrO 3 film was formed on the surface thereof by hydrothermal synthesis.
There are no particular restrictions on the types of materials that make up the material, and the base material is made of various materials such as inorganic materials, metal materials, organic materials, and composite materials having corrosion resistance to the processing solution and heat resistance to the hydrothermal reaction temperature. It is possible to use materials.
【００２４】また、基材の形状についても特に制約はな
く、バルクやフォイルなどの種々の基材を用いることが
可能であり、また、平板状の基材に限らず複雑な形状を
有する基材の表面にもＰｂＺｒＯ3膜を確実に形成する
ことができる。There is no particular limitation on the shape of the substrate, and various substrates such as bulk and foil can be used. Further, the substrate is not limited to a flat substrate and has a complicated shape. A PbZrO 3 film can also be reliably formed on the surface of.
【００２５】また、上記実施例では、鉛（Ｐｂ）及びジ
ルコニウム（Ｚｒ）の原料として、硝酸鉛（Ｐｂ（ＮＯ
3）2）及びオキシ硝酸ジルコニウム（ＺｒＯ（ＮＯ3）2
・Ｈ 2Ｏ）を用いた場合について説明したが、鉛（Ｐ
ｂ）及びジルコニウム（Ｚｒ）の原料はこれらに限られ
るものではなく、酢酸鉛（Ｐｂ（ＣＨ3ＣＯＯＨ）4）や
オキシ酢酸ジルコニウム（ＺｒＯ（ＣＨ3ＣＯＯＨ）2）
などの他の物質を用いることも可能である。In the above embodiment, lead (Pb) and di
As a raw material of ruconium (Zr), lead nitrate (Pb (NO
Three)Two) And zirconium oxynitrate (ZrO (NOThree)Two
・ H 2O) was used, but lead (P
The raw materials for b) and zirconium (Zr) are limited to these.
Not lead acetate (Pb (CHThreeCOOH)Four) And
Zirconium oxyacetate (ZrO (CHThreeCOOH)Two)
It is also possible to use other substances such as.
【００２６】[0026]
【発明の効果】上述のように、この発明のジルコン酸鉛
（ＰｂＺｒＯ3）膜の形成方法は、鉛（Ｐｂ）イオンま
たはサスペンジョン０．１mol／l 以上と、ジルコニウ
ム（Ｚｒ）イオンまたはサスペンジョン０．１mol／l
以上とを含有し、かつ、ｐＨが１４以上のアルカリ性水
溶液中に基材を浸漬し、２００℃以上の温度で水熱処理
を施すことにより、ジルコン酸鉛（ＰｂＺｒＯ3）膜を
前記基材の表面に形成するようにしているので、低温
で、かつ、後処理工程を必要とすることなく、基材上に
均一なジルコン酸鉛（ＰｂＺｒＯ3）膜を形成すること
ができる。As described above, the method for forming a lead zirconate (PbZrO 3 ) film according to the present invention uses lead (Pb) ions or suspensions of 0.1 mol / l or more and zirconium (Zr) ions or suspensions of 0.1 mol / l or more. 1 mol / l
The lead zirconate (PbZrO 3 ) film is immersed in an alkaline aqueous solution having a pH of 14 or more and subjected to a hydrothermal treatment at a temperature of 200 ° C. or more to form a lead zirconate (PbZrO 3 ) film on the surface of the substrate. Therefore, a uniform lead zirconate (PbZrO 3 ) film can be formed on the base material at a low temperature and without the need for a post-treatment step.
【００２７】また、この発明によれば、２００℃以上の
水熱反応温度に耐える種々の材料からなる種々の形状の
基材の表面にジルコン酸鉛（ＰｂＺｒＯ3）膜を容易に
形成することができる。Further, according to the present invention, it is possible to easily form a lead zirconate (PbZrO 3 ) film on the surface of substrates of various shapes made of various materials that can withstand a hydrothermal reaction temperature of 200 ° C. or more. it can.
【００２８】さらに、金属を基材として用いる場合に
は、加工性に優れた金属基材を電極として利用すること
により、ジルコン酸鉛（ＰｂＺｒＯ3）膜の特性を利用
した各種のデバイスの形状を、その用途や特性上の必要
に応じて任意に制御することが可能になり、その用途を
さらに広げることができる。Further, when a metal is used as a substrate, the shape of various devices utilizing the characteristics of a lead zirconate (PbZrO 3 ) film is improved by using a metal substrate having excellent workability as an electrode. Thus, it is possible to arbitrarily control the use as required according to its use and characteristics, and the use can be further expanded.
【図１】この発明のジルコン酸鉛（ＰｂＺｒＯ3）膜の
形成方法により形成した膜のＸ線回折パターンを示す図
である。FIG. 1 is a view showing an X-ray diffraction pattern of a film formed by a method for forming a lead zirconate (PbZrO 3 ) film of the present invention.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平２−6334（ＪＰ，Ａ) 特開 平３−24279（ＪＰ，Ａ) 特開 平４−21785（ＪＰ，Ａ) 特開 平１−108164（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C01G 25/00 H01B 3/00 C23C 18/12 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-2-6334 (JP, A) JP-A-3-24279 (JP, A) JP-A-4-21785 (JP, A) JP-A-1- 108164 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C01G 25/00 H01B 3/00 C23C 18/12
Claims (1)
またはサスペンジョンと、０．１mol／l 以上のジルコ
ニウム（Ｚｒ）イオンまたはサスペンジョンとを含有
し、かつ、ｐＨが１４以上のアルカリ性水溶液中に基材
を浸漬し、２００℃以上の温度で水熱処理を施すことに
より、ジルコン酸鉛（ＰｂＺｒＯ3）膜を前記基材の表
面に形成することを特徴とするジルコン酸鉛膜の形成方
法。An alkaline aqueous solution containing at least 0.1 mol / l of lead (Pb) ions or suspensions and at least 0.1 mol / l of zirconium (Zr) ions or suspensions and having a pH of 14 or more. A lead zirconate (PbZrO 3 ) film is formed on a surface of the substrate by immersing the substrate in a substrate and performing a hydrothermal treatment at a temperature of 200 ° C. or higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03334104A JP3111565B2 (en) | 1991-11-21 | 1991-11-21 | Method of forming lead zirconate film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP03334104A JP3111565B2 (en) | 1991-11-21 | 1991-11-21 | Method of forming lead zirconate film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH05139749A JPH05139749A (en) | 1993-06-08 |
| JP3111565B2 true JP3111565B2 (en) | 2000-11-27 |
Family
ID=18273575
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP03334104A Expired - Lifetime JP3111565B2 (en) | 1991-11-21 | 1991-11-21 | Method of forming lead zirconate film |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3111565B2 (en) |
-
1991
- 1991-11-21 JP JP03334104A patent/JP3111565B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH05139749A (en) | 1993-06-08 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Tu et al. | Processing and characterization of Pb (Zr, Ti) O3 films, up to 10 μm thick, produced from a diol sol-gel route | |
| JP2003163176A (en) | Substrate for electronic device, method for manufacturing the same, and electronic device | |
| KR100229608B1 (en) | Method for fabricating dielectric device | |
| JP4122430B2 (en) | Ferroelectric film | |
| CN114342099A (en) | Piezoelectric assembly and method of forming a piezoelectric assembly | |
| JP3111565B2 (en) | Method of forming lead zirconate film | |
| KR20090063541A (en) | Room temperature conducting dense thick film prepared by aerosol deposition and preparation method thereof | |
| Yoon et al. | Dielectric and piezoelectric properties of (x) Pb (Mg 1/3 Nb 2/3) O 3–(1− x) Pb (Zr 1/2 Ti 1/2) O 3 thin films prepared by the sol–gel method | |
| JP2001223403A (en) | Ferroelectric substance thin film, its forming method and ferroelectric substance thin film element using the thin film | |
| JP3224905B2 (en) | Composite oxide thin film and method for producing the same | |
| JPH04133369A (en) | Dielectric thin-film, thin-film device and manufacture thereof | |
| JP2000173349A (en) | Dielectric thin film and manufacture thereof, and capacitor | |
| JP3937538B2 (en) | Method for producing PZT fine particles and PZT thin film | |
| US6838117B2 (en) | Film production method and film-element production method | |
| JPH06211523A (en) | Production of composite body containing film of titanium metal and lead titanate zirconate and composite body | |
| JP4528950B2 (en) | Method for manufacturing ferroelectric film structure | |
| JPH0558634A (en) | Formation of lead titanate film and composite obtained by forming the same on metallic titanium base | |
| Hendrickson et al. | Processing of PZT piezoelectric thin films for microelectromechanical systems | |
| KR100975283B1 (en) | high-performance piezoelectric thick film containing room temperature conducting film and prepartion method thereof | |
| JP3951359B2 (en) | Piezoelectric crystal film | |
| Lakeman et al. | Crystallization behavior and improved properties for sol-gel derived PZT and PLZT thin layers processed with a lead oxide cover coating | |
| JP4066518B2 (en) | Piezoelectric crystal thin film, method for manufacturing the same, and piezoelectric element | |
| JP7168079B2 (en) | Piezoelectric film and piezoelectric element | |
| JPH10291885A (en) | Production of thin oxide ceramic film | |
| JP2001146421A (en) | Method for producing crystallized ceramic film and the ceramic film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A01 | Written decision to grant a patent or to grant a registration (utility model) |
Free format text: JAPANESE INTERMEDIATE CODE: A01 Effective date: 20000822 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080922 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080922 Year of fee payment: 8 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090922 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20090922 Year of fee payment: 9 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100922 Year of fee payment: 10 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20100922 Year of fee payment: 10 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20110922 Year of fee payment: 11 |
|
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120922 Year of fee payment: 12 |
|
| EXPY | Cancellation because of completion of term | ||
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20120922 Year of fee payment: 12 |