JP3021930B2 - Method for controlling crystal orientation of ferroelectric thin film - Google Patents
Method for controlling crystal orientation of ferroelectric thin filmInfo
- Publication number
- JP3021930B2 JP3021930B2 JP4057242A JP5724292A JP3021930B2 JP 3021930 B2 JP3021930 B2 JP 3021930B2 JP 4057242 A JP4057242 A JP 4057242A JP 5724292 A JP5724292 A JP 5724292A JP 3021930 B2 JP3021930 B2 JP 3021930B2
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- Prior art keywords
- thin film
- plane
- heat treatment
- ferroelectric thin
- crystal
- Prior art date
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- Physical Or Chemical Processes And Apparatus (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemically Coating (AREA)
- Inorganic Insulating Materials (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明はチタン酸ジルコン酸鉛(P
ZT)またはランタン含有チタン酸ジルコン酸鉛(PLZT)か
らなる強誘電体薄膜の結晶配向性制御方法に関する。Ｐ
ＺＴ薄膜やＰＬＺＴ薄膜は、例えば 赤外線センサー、
圧電フィルター、振動子、レーザの変調素子、光シャッ
ター、キャパシター膜、不揮発性のメモリー等に用いら
れており、鮮明な微細パターンを形成することができる
優れた物性を具えている。本発明は、このＰＺＴ強誘電
体薄膜の結晶配向性を制御する方法に関する。This invention relates to lead zirconate titanate (P
The present invention relates to a method for controlling the crystal orientation of a ferroelectric thin film composed of ZT) or lanthanum-containing lead zirconate titanate (PLZT). P
ZT thin film and PLZT thin film are used for infrared sensors,
It is used for piezoelectric filters, vibrators, laser modulation elements, optical shutters, capacitor films, nonvolatile memories, etc., and has excellent physical properties capable of forming clear fine patterns. The present invention relates to a method for controlling the crystal orientation of the PZT ferroelectric thin film.
【０００２】[0002]
【従来技術とその課題】ＰＺＴ強誘電体薄膜やＰＬＺＴ
薄膜を基板上に形成する方法としては、(イ)粉末状複合
酸化物のペーストを基板上に塗布して乾燥焼結する方
法、(ロ)スパッタリングによる方法、(ハ)相当する金属ア
ルコキシド化合物等の複合化合物前駆体ゾルを基板上に
塗布して熱分解した後結晶化させるいわゆるゾル−ゲル
法等が知られている。強誘電体薄膜は分極反転の現象を
利用するために結晶歪による膜の疲労が問題となってお
り、その歪を抑えるために膜の単結晶化もしくは分極軸
方向への配向成長等が解決策として検討されている。こ
のうち特定の軸方向に結晶を配向させた配向膜に関して
は、スパッタリング法によって成膜したＰＺＴ薄膜につ
いての報告が比較的多く見られが、ゾル−ゲル法によっ
て薄膜を形成する場合の結晶配向性についての報告は少
ない。ゾル−ゲル法は低い温度で良好な特性を有する薄
膜が得られるので、経済性および取扱いの簡便さの面か
ら有利な方法であり最近注目されている。ところで、従
来、ゾル−ゲル法によって薄膜を形成する場合、薄膜の
結晶配向性は、基板自体の結晶軸方向に依存し、多くの
場合、薄膜の結晶は基板の結晶軸方向に一致することは
よく知られている。ところが、基板自体の結晶軸方向と
異なる配向性を示す場合もあり、薄膜の結晶配向性を信
頼性よく制御するのは必ずしも容易ではなかった。2. Description of the Related Art PZT ferroelectric thin film and PLZT
As a method of forming a thin film on a substrate, (a) a method of applying a powdery composite oxide paste on the substrate and drying and sintering it, (b) a method by sputtering, (c) a corresponding metal alkoxide compound, etc. A so-called sol-gel method or the like is known in which a composite compound precursor sol is coated on a substrate, thermally decomposed, and then crystallized. The ferroelectric thin film uses the phenomenon of polarization reversal, so the film fatigue due to crystal distortion is a problem. To suppress the distortion, solution such as single crystallization of the film or orientation growth in the direction of the polarization axis is a solution. It has been considered as. Of these, relatively many reports have been made on PZT thin films formed by the sputtering method with respect to the oriented film in which the crystals are oriented in a specific axial direction. However, the crystal orientation when forming the thin film by the sol-gel method is relatively high. There are few reports on The sol-gel method is a method that is advantageous from the viewpoint of economy and simplicity of handling because a thin film having good properties can be obtained at a low temperature, and has recently been receiving attention. By the way, conventionally, when a thin film is formed by the sol-gel method, the crystal orientation of the thin film depends on the crystal axis direction of the substrate itself, and in many cases, the crystal of the thin film does not coincide with the crystal axis direction of the substrate. well known. However, in some cases, the crystal orientation of the substrate itself is different from the crystal axis direction, and it is not always easy to control the crystal orientation of the thin film with high reliability.
【０００３】[0003]
【課題の解決手段：発明の構成】本発明によれば、ゾル
−ゲル法によってＰＺＴ薄膜やＰＬＺＴ薄膜を形成する
際に、原料溶液(前駆体溶液)を基板に塗布した後に施す
熱処理の温度によりこれら薄膜の結晶配向性が異なるこ
とが見出された。本発明は上記知見に基づくものであ
り、原料溶液を基板に塗布した後の熱処理温度を調整す
ることにより信頼性よくＰＺＴ薄膜およびＰＬＺＴ薄膜
の結晶配向性を制御する方法を提供する。具体的には、
結晶面が（１１１）軸方向に配向した白金基板上にチタ
ン酸ジルコン酸鉛またはランタン含有チタン酸ジルコン
酸鉛の前駆体溶液を塗布し、加熱して強誘電体薄膜を形
成する方法において、該前駆体溶液を基板上に塗布した
後、まず所望の結晶配向をもたらす１５０〜５５０℃の
温度範囲で熱処理を行い、その後５５０〜８００℃で焼
成して結晶化させることにより、薄膜の結晶面を熱処理
温度に従った特定軸方向に優先的に配向させることを特
徴とする強誘電体薄膜の結晶配向性制御方法が提供され
る。更に本発明によれば、基板上に塗布した前駆体溶液
を結晶化前に１５０〜２５０℃で熱分解させ、その後加
熱して結晶化させることにより薄膜の結晶の（１１１）
面を優先的に配向させる強誘電体薄膜の結晶配向性制御
方法が提供される。また本発明によれば、基板上に塗布
した前駆体溶液を結晶化前に２５０〜３５０℃で熱分解
させ、その後加熱して結晶化させることにより薄膜の結
晶の（１１１）面と（１００）面を優先的に配向させる
の強誘電体薄膜の結晶配向性制御方法が提供される。ま
た本発明によれば、基板上に塗布した前駆体溶液を結晶
化前に４５０〜５５０℃で熱分解させ、その後加熱して
結晶化させることにより薄膜の結晶の（１００）面と
（２００）面を優先的に配向させる強誘電体薄膜の結晶
配向性制御方法が提供される。According to the present invention, when a PZT thin film or a PLZT thin film is formed by a sol-gel method, the temperature of a heat treatment applied after a raw material solution (precursor solution) is applied to a substrate. It has been found that the crystal orientation of these thin films is different. The present invention is based on the above findings, and provides a method for controlling the crystal orientation of a PZT thin film and a PLZT thin film with high reliability by adjusting a heat treatment temperature after applying a raw material solution to a substrate. In particular,
A method for forming a ferroelectric thin film by applying a precursor solution of lead zirconate titanate or lanthanum-containing lead zirconate titanate on a platinum substrate having a crystal plane oriented in a (111) axis direction and heating the applied solution to form a ferroelectric thin film. After applying the precursor solution on the substrate, first, a heat treatment is performed in a temperature range of 150 to 550 ° C. that provides a desired crystal orientation, and then, the film is fired and crystallized at 550 to 800 ° C. A method for controlling the crystal orientation of a ferroelectric thin film, characterized by preferentially orienting in a specific axis direction according to a heat treatment temperature. Further, according to the present invention, the precursor solution applied on the substrate is thermally decomposed at 150 to 250 ° C. before crystallization, and then heated to be crystallized, whereby the (111) of the crystal of the thin film is formed.
A method for controlling the crystal orientation of a ferroelectric thin film that preferentially orients a plane is provided. Further, according to the present invention, the precursor solution applied on the substrate is thermally decomposed at 250 to 350 ° C. before crystallization, and then heated to be crystallized, whereby the (111) plane of the crystal of the thin film and the (100) A method for controlling the crystal orientation of a ferroelectric thin film that preferentially orients a plane is provided. Further, according to the present invention, the precursor solution applied on the substrate is thermally decomposed at 450 to 550 ° C. before crystallization, and then heated to be crystallized, whereby the (100) plane of the crystal of the thin film and the (200) A method for controlling the crystal orientation of a ferroelectric thin film that preferentially orients a plane is provided.
【０００４】本発明の方法に使用される出発物質は、P
b,Zr,Ti,Laの有機酸塩、アルコキシド、β-ジケトン錯
体等で、これらは当該技術分野においてよく知られてお
り、均等的に使用できる。本発明において、ＰＺＴ薄膜
およびＰＬＺＴ薄膜を製造する基板としては結晶面が
（１１１）軸方向に配向した白金板が好適に用いられ
る。ＰＺＴ薄膜およびＰＬＺＴ薄膜の基板は、下部電極
として利用するため導電性であることが必要であり、か
つＰＺＴ薄膜およびＰＬＺＴ薄膜と反応しないことが必
要である。その点で白金は非常に好ましい下地材料であ
る。白金は板状のものに限らず、他の基板上に成膜した
白金薄膜でも同じように用いることができる。因みにシ
リコンウエハーを熱酸化させた基板上に白金を成膜する
と（１１１）軸配向膜となる。The starting material used in the process of the invention is P
b, Zr, Ti, La organic acid salts, alkoxides, β-diketone complexes and the like, which are well known in the art and can be used equally. In the present invention, as a substrate for producing a PZT thin film and a PLZT thin film, a platinum plate having a crystal plane oriented in the (111) axis direction is suitably used. The substrate of the PZT thin film and the PLZT thin film needs to be conductive to be used as a lower electrode, and must not react with the PZT thin film and the PLZT thin film. In that regard, platinum is a very preferred underlying material. Platinum is not limited to a plate-like one, and a platinum thin film formed on another substrate can be similarly used. Incidentally, when platinum is deposited on a substrate obtained by thermally oxidizing a silicon wafer, a (111) -axis oriented film is obtained.
【０００５】本発明は、ＰＺＴ薄膜ないしＰＬＺＴ薄膜
の原料溶液である有機金属化合物の複合化合物前駆体ゾ
ルを前記（１１１）軸方向に配向した白金基板上に塗布
した後、まづ１５０〜５５０℃の温度で熱分解を行い、
次いで６００℃〜８００℃に加熱焼成して結晶化させ、
この結晶化前の熱処理温度を１５０〜５５０℃の範囲内
で所定の温度範囲に調整することにより、ＰＺＴ薄膜お
よびＰＬＺＴ薄膜の結晶配向性を制御することができ
る。具体的には、結晶化前の熱処理温度を１５０℃〜２
５０℃に調整することにより（１１１）面が優先的に配
向（成長）したペロブスカイト型のＰＺＴ薄膜結晶また
はＰＬＺＴ薄膜結晶を得ることができる。１５０℃未満
の温度では熱分解が十分に進行せず、また２５０℃を超
えると（１００）軸方向の配向性が次第に強まり（１１
１）軸方向の優先性が低下する。また熱処理の温度を２
５０〜３５０℃に調整することにより（１１１）面と
（１００）面に優先的に配向したペロブスカイト型のＰ
ＺＴ薄膜結晶またはＰＬＺＴ薄膜結晶を得ることができ
る。熱処理の温度が２５０℃未満であると（１１１）面
が優先的になり、また３５０℃を越えると４５０℃まで
は（１１１）面と（１００）面を優先的に配向させるこ
とができなくなるため好ましくない。さらに熱処理温度
を４５０〜５５０℃に調整することにより（１００）面
および（２００）面を優先的に配向させたＰＺＴ薄膜を
得ることができる。結晶化させる前の熱処理の温度が４
５０℃未満であると（１００）面以外の面の配向性が出
るため、また５５０℃を超えると結晶化が始まるため何
れも好ましくない。また、結晶化温度が８００℃を超え
るとＰＺＴ薄膜と白金とが反応し始め、充分な特性の薄
膜が得られないので、結晶化温度は８００℃以下が好ま
しい。本発明の結晶配向性制御方法における結晶化前の
熱分解温度温度範囲と薄膜結晶の優先配向面を次表に纏
めて示す。According to the present invention, a sol of a precursor of a complex compound of an organometallic compound, which is a raw material solution of a PZT thin film or a PLZT thin film, is applied on the platinum substrate oriented in the (111) axis direction, and then, at 150 to 550 ° C. Pyrolysis at the temperature of
Then, heat calcination to 600 to 800 ° C to crystallize,
The crystal orientation of the PZT thin film and the PLZT thin film can be controlled by adjusting the heat treatment temperature before the crystallization to a predetermined temperature range within a range of 150 to 550 ° C. Specifically, the heat treatment temperature before crystallization is set to 150 ° C. to 2 ° C.
By adjusting the temperature to 50 ° C., a perovskite-type PZT thin film crystal or a PLZT thin film crystal in which the (111) plane is preferentially oriented (grown) can be obtained. At a temperature lower than 150 ° C., the thermal decomposition does not sufficiently proceed, and at a temperature higher than 250 ° C., the orientation in the (100) axis direction gradually increases (11).
1) The priority in the axial direction decreases. In addition, the heat treatment temperature is set to 2
By adjusting the temperature to 50 to 350 ° C., perovskite-type P preferentially oriented in the (111) plane and the (100) plane.
A ZT thin film crystal or a PLZT thin film crystal can be obtained. If the temperature of the heat treatment is lower than 250 ° C., the (111) plane becomes preferential, and if it exceeds 350 ° C., the (111) plane and (100) plane cannot be preferentially oriented up to 450 ° C. Not preferred. Further, by adjusting the heat treatment temperature to 450 to 550 ° C., a PZT thin film in which the (100) plane and the (200) plane are preferentially oriented can be obtained. Temperature of heat treatment before crystallization is 4
When the temperature is lower than 50 ° C., the orientation of the plane other than the (100) plane is obtained, and when the temperature is higher than 550 ° C., crystallization starts. If the crystallization temperature exceeds 800 ° C., the PZT thin film starts reacting with platinum, and a thin film having sufficient characteristics cannot be obtained. Therefore, the crystallization temperature is preferably 800 ° C. or less. The following table summarizes the temperature range of the thermal decomposition temperature before crystallization and the preferred orientation plane of the thin film crystal in the crystal orientation control method of the present invention.
【０００６】 [0006]
【０００７】実施例１ 7.59gのPb(CH3COO)3・3H2O、3.99gのZr(OBu)4、2.73gのT
i(Oi-Pr)4を55gの2-エトキシエタノールに溶解してPZT
複合化合物前駆体溶液(ゾル)からなる原料溶液を（１１
１）軸方向に配向した白金基板上に塗布し、それぞれ２
００℃、３００℃、４００℃および５００℃で１５分間
熱処理を行った後に６００℃で１時間結晶化させてPb1Z
r0.52Ti0.48O3のＰＺＴ薄膜結晶を得た。このＰＺＴ薄
膜のＸ線回折図を図１(A)〜(D)に示す。なお、(Ａ)は２
００℃、(Ｂ)は３００℃、(Ｃ)は４００℃および(Ｄ)は
５００℃の熱処理の場合をそれぞれ示す。図１の(Ａ)は
ＰＺＴ薄膜結晶の優先配向軸が（１１１）であり、(Ｂ)
は（１１１）および（１００）であることが判る。また
(Ｃ)は優先配向軸が特定されず、(Ｄ)は（１００）およ
び（２００）に優先的に配向することを示している。本
実施例において熱処理の時間をさらに長くすると（１１
１）軸方向の配列がより優先的になると考えられる。Example 1 7.59 g of Pb (CH 3 COO) 3 .3H 2 O, 3.99 g of Zr (OBu) 4 , 2.73 g of T
i (Oi-Pr) 4 is dissolved in 55 g of 2-ethoxyethanol to give PZT
The raw material solution composed of the composite compound precursor solution (sol) is
1) Coating on a platinum substrate oriented in the axial direction, 2
After heat treatment at 00 ° C., 300 ° C., 400 ° C. and 500 ° C. for 15 minutes, crystallization is performed at 600 ° C. for 1 hour to obtain Pb 1 Z
A PZT thin film crystal of r 0.52 Ti 0.48 O 3 was obtained. X-ray diffraction diagrams of this PZT thin film are shown in FIGS. (A) is 2
00C, (B) shows the case of 300 ° C, (C) shows the case of 400 ° C, and (D) shows the case of the heat treatment of 500 ° C. FIG. 1A shows that the preferred orientation axis of the PZT thin film crystal is (111), and FIG.
Are (111) and (100). Also
(C) shows that the preferred orientation axis is not specified, and (D) shows that the (100) and (200) are preferentially oriented. In this embodiment, if the time of the heat treatment is further increased (11)
1) It is considered that the arrangement in the axial direction becomes more preferential.
【０００８】実施例２ 結晶化前の熱処理を１時間行った以外は実施例１と同様
にしてＰＺＴ薄膜結晶を形成した。このＰＺＴ薄膜のＸ
線回折図を図２(A)〜(D)に示す。なお(Ａ)は２００℃、
(Ｂ)は３００℃、(Ｃ)は４００℃、(Ｄ)は５００℃の熱
処理の場合をそれぞれ示す。この結果は図示するように
実施例１と同様の傾向を示した。Example 2 A PZT thin film crystal was formed in the same manner as in Example 1 except that the heat treatment before crystallization was performed for 1 hour. X of this PZT thin film
The line diffraction diagrams are shown in FIGS. (A) is 200 ° C,
(B) shows the case of heat treatment at 300 ° C, (C) shows the case of heat treatment at 400 ° C, and (D) shows the case of heat treatment at 500 ° C. The result showed the same tendency as in Example 1 as shown.
【０００９】実施例３ 実施例１および２で用いたものと同じ原料溶液を１０時
間還流して用いた他は実施例２と同様にしてＰＺＴ薄膜
結晶を得た。Ｘ線回折図を実施例２と同様に図３に示し
た。Example 3 A PZT thin film crystal was obtained in the same manner as in Example 2, except that the same raw material solution as used in Examples 1 and 2 was refluxed for 10 hours. The X-ray diffraction pattern is shown in FIG.
【００１０】実施例４ 7.20gのPb(CH3COO)3・3H2O、 3.94gのZr(OBu)4、0.34gの
La(CH3COO)3・1.5H2O、2.70gのTi(Oi-Pr)4、55gの2-エト
キシエタノールを使用して実施例１と同様に実施した。
得られたＰＬＺＴはPb0.95La0.05Zr0.51Ti0.47O3であっ
た。得られたＸ線回折図を図４(A)〜(D)に示した。概ね
実施例１〜３と同様の傾向を示すが配向性の優先性はさ
らに改良されている。Example 4 7.20 g of Pb (CH 3 COO) 3 .3H 2 O, 3.94 g of Zr (OBu) 4 , 0.34 g of
La (CH 3 COO) 3 · 1.5H 2 O, 2.70g of Ti (Oi-Pr) 4, was carried out in the same manner as in Example 1 using 55g of 2-ethoxyethanol.
The obtained PLZT was Pb 0.95 La 0.05 Zr 0.51 Ti 0.47 O 3 . The obtained X-ray diffraction patterns are shown in FIGS. 4 (A) to (D). Although the same tendency as in Examples 1 to 3 is shown, the priority of the orientation is further improved.
【図１】図１（Ａ）〜（Ｄ）は実施例で得たＰＺＴ薄膜
のＸ線回折図である。FIGS. 1A to 1D are X-ray diffraction diagrams of a PZT thin film obtained in an example.
【図２】図２（Ａ）〜（Ｄ）は実施例で得たＰＺＴ薄膜
のＸ線回折図である。FIGS. 2A to 2D are X-ray diffraction diagrams of a PZT thin film obtained in an example.
【図３】図３（Ａ）〜（Ｄ）は実施例で得たＰＺＴ薄膜
のＸ線回折図である。FIGS. 3A to 3D are X-ray diffraction diagrams of a PZT thin film obtained in an example.
【図４】図４（Ａ）〜（Ｄ）は実施例で得たＰＺＴ薄膜
のＸ線回析図である。FIGS. 4A to 4D are X-ray diffraction diagrams of the PZT thin films obtained in the examples.
───────────────────────────────────────────────────── フロントページの続き (56)参考文献 特開 平２−6335（ＪＰ，Ａ) 特開 平３−69512（ＪＰ，Ａ) 特開 昭63−239880（ＪＰ，Ａ) 特開 昭57−82121（ＪＰ，Ａ) 特開 昭60−200403（ＪＰ，Ａ) 特開 平５−221643（ＪＰ，Ａ) 特開 平６−5948（ＪＰ，Ａ) (58)調査した分野(Int.Cl.7，ＤＢ名) C30B 29/32 C04B 35/49 C23C 18/12 H01B 3/00 B01J 19/00 ──────────────────────────────────────────────────続 き Continuation of the front page (56) References JP-A-2-6335 (JP, A) JP-A-3-69512 (JP, A) JP-A-63-239880 (JP, A) JP-A-57- 82121 (JP, A) JP-A-60-200403 (JP, A) JP-A-5-221643 (JP, A) JP-A-6-5948 (JP, A) (58) Fields investigated (Int. Cl. 7 , DB name) C30B 29/32 C04B 35/49 C23C 18/12 H01B 3/00 B01J 19/00
Claims (1)
金基板上にチタン酸ジルコン酸鉛またはランタン含有チ
タン酸ジルコン酸鉛のゾル−ゲル法前駆体溶液を塗布
し、加熱して基板上に強誘電体薄膜を形成する方法にお
いて、 前記加熱が１５０〜５５０℃の温度範囲に保持する熱処
理と、その後の５５０〜８００℃の温度範囲に保持して
結晶化させる焼成を含み、 (1) 前記熱処理を１５０〜２５０℃の温度範囲で行い、
焼成後に（１１１）面に優先的に配向した強誘電体薄膜
を生成させるか、または (2) 前記熱処理を２５０〜３５０℃の温度範囲で行い、
焼成後に（１１１）面と（１００）面に優先的に配向し
た強誘電体薄膜を生成させるか、または (3) 前記熱処理を４５０〜５５０℃の温度範囲で行い、
焼成後に（１００）面と（２００）面に優先的に配向し
た強誘電体薄膜を生成させる、 ことを特徴とする、特定軸方向に優先的に結晶配向した
強誘電体薄膜を形成する方法。1. A sol-gel method precursor solution of lead zirconate titanate or lanthanum-containing lead zirconate titanate is applied on a platinum substrate having a crystal plane oriented in the (111) axis direction, and heated to form a substrate. (1) a method of forming a ferroelectric thin film comprising: a heat treatment in which the heating is performed at a temperature in a range of 150 to 550 ° C .; Performing the heat treatment in a temperature range of 150 to 250 ° C.,
(B) generating a ferroelectric thin film preferentially oriented on the (111) plane after firing, or (2) performing the heat treatment in a temperature range of 250 to 350 ° C.
After the firing, a ferroelectric thin film preferentially oriented in the (111) plane and the (100) plane is generated, or (3) the heat treatment is performed in a temperature range of 450 to 550 ° C;
A method of forming a ferroelectric thin film preferentially oriented in a specific axis direction, which comprises producing a ferroelectric thin film preferentially oriented on the (100) plane and the (200) plane after firing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4057242A JP3021930B2 (en) | 1991-02-13 | 1992-02-12 | Method for controlling crystal orientation of ferroelectric thin film |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3-40592 | 1991-02-13 | ||
| JP3040592A JPH04259380A (en) | 1991-02-13 | 1991-02-13 | Method for controlling crystalline orientation property of pzt ferroelectric body thin film |
| JP4057242A JP3021930B2 (en) | 1991-02-13 | 1992-02-12 | Method for controlling crystal orientation of ferroelectric thin film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH06116095A JPH06116095A (en) | 1994-04-26 |
| JP3021930B2 true JP3021930B2 (en) | 2000-03-15 |
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ID=26380062
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|---|---|---|---|
| JP4057242A Expired - Lifetime JP3021930B2 (en) | 1991-02-13 | 1992-02-12 | Method for controlling crystal orientation of ferroelectric thin film |
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-
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- 1992-02-12 JP JP4057242A patent/JP3021930B2/en not_active Expired - Lifetime
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|---|---|---|---|---|
| US7530676B2 (en) | 2004-03-05 | 2009-05-12 | Panasonic Corporation | Piezoelectric element, inkjet head, angular velocity sensor, methods for manufacturing them and inkjet recording device |
| US7312558B2 (en) | 2004-04-02 | 2007-12-25 | Matsushita Electric Industrial Co., Ltd. | Piezoelectric element, ink jet head, angular velocity sensor, and ink jet recording apparatus |
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|---|---|
| JPH06116095A (en) | 1994-04-26 |
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