JPH09162680A - Piezoelectric vibrator and its manufacture - Google Patents

Piezoelectric vibrator and its manufacture

Info

Publication number
JPH09162680A
JPH09162680A JP31504895A JP31504895A JPH09162680A JP H09162680 A JPH09162680 A JP H09162680A JP 31504895 A JP31504895 A JP 31504895A JP 31504895 A JP31504895 A JP 31504895A JP H09162680 A JPH09162680 A JP H09162680A
Authority
JP
Japan
Prior art keywords
piezoelectric vibrator
temperature
pzt
heat
piezoelectric material
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.)
Pending
Application number
JP31504895A
Other languages
Japanese (ja)
Inventor
Rui Namiuchi
類 浪内
Norihiro Tani
紀広 谷
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Panasonic Holdings Corp
Original Assignee
Matsushita Electric Industrial Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Matsushita Electric Industrial Co Ltd filed Critical Matsushita Electric Industrial Co Ltd
Priority to JP31504895A priority Critical patent/JPH09162680A/en
Publication of JPH09162680A publication Critical patent/JPH09162680A/en
Pending legal-status Critical Current

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  • Compositions Of Oxide Ceramics (AREA)
  • Piezo-Electric Or Mechanical Vibrators, Or Delay Or Filter Circuits (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide the highly reliable piezoelectric vibrator and its manufacture in which production of distortion and an alterated layer due to processing after polarization and characteristic deterioration caused by dispersion in the uniformity in PZT group piezoelectric materials are not caused. SOLUTION: The piezoelectric vibrator is shaped so that an oxygen gas is penetrated inside by thermal diffusion and is made of a PZT group piezoelectric material heat-treated for 30min or over at a temperature lower than a prescribed sintering temperature by 50 to 500 deg.C in an atmosphere with 10% of oxygen concentration or over. A thick sintering body is cut to have a thickness of 2mm or below and the resulting body is heat-treated under the condition above, and a thin sintering body of 2mm or below is sintered and heat-treated under the condition above, and then the processed body is formed to be the piezoelectric vibrator after polarization, polishment, electrode vapor-deposition and cutting process.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明はテレビジョン受像
機、通信機器用のフィルター、発振子等の圧電振動子及
びその製造方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a television receiver, a filter for communication equipment, a piezoelectric vibrator such as an oscillator, and a method for manufacturing the same.

【0002】[0002]

【従来の技術】従来、チタン酸ジルコン酸鉛を主成分と
するPZT系圧電材料を圧電振動子として仕上げるに
は、厚物焼結体をそのまま分極処理をするか、スライス
したのち分極処理し、更にスライス、切断等の材料加工
をしたのち組み立てるものであった。
2. Description of the Related Art Conventionally, in order to finish a PZT type piezoelectric material containing lead zirconate titanate as a main component as a piezoelectric vibrator, a thick sintered body is polarized as it is, or sliced and then polarized. Further, it was assembled after material processing such as slicing and cutting.

【0003】[0003]

【発明が解決しようとする課題】しかしながら、このよ
うな従来の方法ではPZT系圧電材料を分極処理をして
圧電性を励起させたのち加工するため、加工歪みや加工
表面の変質層が圧電振動子の特性や信頼性を低下させる
可能性があった。
However, in such a conventional method, since the PZT-based piezoelectric material is processed by polarization to excite its piezoelectricity and then processed, processing strain and an altered layer on the processed surface cause piezoelectric vibration. There is a possibility that the characteristics and reliability of the child may deteriorate.

【0004】さらに形状の大きなPZT系圧電材料から
微小な共振子に加工していくため、焼成したPZT系圧
電材料内の均質性ばらつきが、そのまま共振子の特性ば
らつきにつながるという問題点があった。
Further, since the PZT-based piezoelectric material having a large shape is processed into a minute resonator, there is a problem that the homogeneity variation in the fired PZT-based piezoelectric material directly leads to the characteristic variation of the resonator. .

【0005】本発明は上記従来の問題点を解決するもの
であり、高信頼性のPZT系圧電材料を有する圧電振動
子を提供することを目的とするものである。
The present invention solves the above-mentioned conventional problems, and an object thereof is to provide a piezoelectric vibrator having a highly reliable PZT-based piezoelectric material.

【0006】[0006]

【課題を解決するための手段】この課題を解決するため
に本発明の圧電振動子は、酸素が熱拡散により内部まで
浸透し得るように2mm以下の厚みとし、酸素濃度10%
以上の雰囲気中、所定のピーク焼成温度より50〜50
0℃低い範囲内の温度で、30分以上の熱処理したPZ
T系圧電材料より構成されるものである。
In order to solve this problem, the piezoelectric vibrator of the present invention has a thickness of 2 mm or less so that oxygen can penetrate into the inside by thermal diffusion, and the oxygen concentration is 10%.
50 to 50 from the predetermined peak firing temperature in the above atmosphere
PZ heat-treated for 30 minutes or longer at a temperature within 0 ° C lower range
It is composed of a T-based piezoelectric material.

【0007】[0007]

【発明の実施の形態】本発明の請求項1記載の発明は、
形状の大きなPZT系圧電材料の焼結体を、スライス等
の厚み加工をしたのち酸素を供給しながら熱処理するこ
とにより、加工歪み、変質層の改善ができ、焼結体部位
により発生する特性ばらつきを均一化することができ
る。さらに有機系バインダー等を多く含む薄物成形体を
焼成したのち、引き続き酸素を供給しながら熱処理する
ことにより、特性が良くばらつきの小さいPZT系圧電
材料を量産性良く得ることができるものである。
BEST MODE FOR CARRYING OUT THE INVENTION The invention according to claim 1 of the present invention is
By processing a sintered body of a PZT-based piezoelectric material having a large shape by slicing or the like and then heat-treating it while supplying oxygen, it is possible to improve the processing strain and the altered layer, and the characteristic variations caused by the sintered body site Can be made uniform. Furthermore, by firing a thin molded body containing a large amount of an organic binder and the like, and subsequently subjecting it to heat treatment while supplying oxygen, it is possible to obtain a PZT-based piezoelectric material having good characteristics and small variations with good mass productivity.

【0008】(実施形態1)原料を所定の組成となるよ
う秤量し、ボールミルで混合した後、最適仮焼温度にて
仮焼した。粉砕後PVA系バインダー溶液を加え造粒
し、ブロック形状に成形し、最適焼成ピーク温度120
0℃にて焼成した。このようにして得たPZT系圧電材
料のブロック型焼結体を厚み0.3mmの角板に切り出
し、前記焼成ピーク温度より100℃低い1100℃に
て、炉内の酸素濃度20%の雰囲気で1時間熱処理をし
た。その後圧電振動子として特性評価するために、この
熱処理した角板と、比較として同一焼結体の熱処理して
いない角板との両面に全面電極を設け分極し、更に両面
の電極を取り除き、代わりにスポット電極を多数蒸着し
たのち切断しエネルギー閉じ込め型圧電振動子を作製し
た。これらの圧電振動子を用いて測定したループゲイン
のばらつきから、PZT系圧電材料の均質性、特性ばら
つきを評価した。熱処理した角板から作製した圧電振動
子のループゲイン分布を図1に示す。図2は同一焼結体
の熱処理していない角板から作製した圧電振動子のルー
プゲイン分布を示す。図から明らかなように、熱処理し
ていないものに比べ熱処理したものは、ループゲインの
ばらつき巾が小さくなり、特性レベルも向上しており、
PZT系圧電材料の均質性、特性ばらつきが改善されて
いることがわかる。しかし、熱処理温度と最適焼成温度
の差が50℃より小さいか、もしくは最適焼成温度より
高いとPZT系圧電材料の主成分である一酸化鉛が角板
の表面から飛散し、均質性や特性にばらつきを生じるた
め好ましくない。また、熱処理中の炉内の酸素濃度が1
0%より小さいと、特性向上はみられるが経時変化が発
生し、信頼性の高い圧電振動子を得ることができない。
さらに、熱処理時間が30分より短いと、熱処理温度が
高くても効果は少なく、圧電振動子での評価で特性向上
もばらつき改善も確認されなかった。また、厚みが2mm
より厚くなると、熱処理をしても酸素の熱拡散による内
部への浸透が十分には行なわれず、顕著な特性向上はみ
られなかった。
(Embodiment 1) Raw materials were weighed so as to have a predetermined composition, mixed in a ball mill, and then calcined at an optimum calcining temperature. After pulverization, a PVA-based binder solution was added and granulated to form a block shape, and the optimum firing peak temperature was 120.
It was baked at 0 ° C. The block-type sintered body of the PZT-based piezoelectric material thus obtained was cut into a square plate having a thickness of 0.3 mm, and the furnace was heated at 1100 ° C., which is 100 ° C. lower than the firing peak temperature, in an atmosphere with an oxygen concentration of 20%. It heat-processed for 1 hour. After that, in order to evaluate the characteristics as a piezoelectric vibrator, this heat-treated square plate and a non-heat-treated square plate of the same sintered body were polarized by providing full-face electrodes on both sides, and then the electrodes on both sides were removed. A large number of spot electrodes were vapor-deposited on the substrate and then cut to fabricate an energy trap type piezoelectric vibrator. The homogeneity and characteristic variation of the PZT-based piezoelectric material were evaluated from the variation of loop gain measured using these piezoelectric vibrators. FIG. 1 shows the loop gain distribution of the piezoelectric vibrator manufactured from the heat-treated square plate. FIG. 2 shows a loop gain distribution of a piezoelectric vibrator manufactured from an unheated rectangular plate of the same sintered body. As is clear from the figure, the heat-treated one has a smaller loop gain variation width than the non-heat-treated one, and the characteristic level is improved.
It can be seen that the homogeneity and characteristic variation of the PZT-based piezoelectric material are improved. However, if the difference between the heat treatment temperature and the optimum firing temperature is smaller than 50 ° C or higher than the optimum firing temperature, lead monoxide, which is the main component of the PZT-based piezoelectric material, scatters from the surface of the square plate, resulting in poor homogeneity and characteristics. It is not preferable because it causes variations. Also, the oxygen concentration in the furnace during the heat treatment is 1
If it is less than 0%, the characteristics are improved, but a change over time occurs, and a highly reliable piezoelectric vibrator cannot be obtained.
Furthermore, if the heat treatment time is shorter than 30 minutes, the effect is small even if the heat treatment temperature is high, and neither the characteristic improvement nor the variation improvement was confirmed by the evaluation with the piezoelectric vibrator. Also, the thickness is 2 mm
When the thickness became thicker, even if the heat treatment was carried out, the permeation into the interior due to thermal diffusion of oxygen was not sufficiently carried out, and no remarkable improvement in the characteristics was observed.

【0009】(実施形態2)図3に本発明の第2の実施
形態の製造工程図を示す。原料を所定の組成となるよう
秤量し、ボールミルで混合した後、最適仮焼温度800
℃にて仮焼した。粉砕後PVA系バインダー溶液を加え
造粒し、厚み10mmのブロック形状に成形し、焼成温度
1220℃にて焼成した。このようにして得たPZT系
圧電材料のブロック型焼結体を厚み0.3mmの角板にス
ライス加工し、サヤ内に積層充填した状態で焼成温度よ
り100℃低い温度にて、炉内の酸素濃度20%の雰囲
気で1時間熱処理をした。次に角板の両面に全面電極を
形成し分極処理した後、厚み0.2mmまで両面研磨しス
ポット電極を多数蒸着した。そして所定の形状に切断
し、エネルギー閉じ込め型の圧電振動子を作製した。比
較として同一のPZT系圧電材料のブロック型焼結体を
スライス加工し、熱処理せずにそのまま分極処理、研
磨、電極蒸着、切断と工程をすすめ、前記と同様の圧電
振動子を作製した。このようにして得たそれぞれの圧電
振動子の特性を評価したところ、特性レベル、ばらつき
に大きな差があり、本発明の圧電振動子は熱処理したこ
とにより加工による特性劣化もみられずループゲイン値
の向上、ばらつきの巾の減少が確認された。つまり同一
のPZT系圧電材料においても、本発明の製造方法を用
いたことにより特性が改善されたうえ生産歩留まりが向
上し、信頼性の高い圧電振動子を量産性良く得ることが
できた。
(Embodiment 2) FIG. 3 shows a manufacturing process diagram of a second embodiment of the present invention. The raw materials are weighed so as to have a predetermined composition and mixed by a ball mill, and then the optimum calcination temperature is 800
It was calcined at ℃. After pulverization, a PVA-based binder solution was added and granulated to form a block shape having a thickness of 10 mm, which was then fired at a firing temperature of 1220 ° C. The block-type sintered body of the PZT-based piezoelectric material obtained in this manner was sliced into a square plate having a thickness of 0.3 mm, and stacked and packed in a sheath at a temperature 100 ° C. lower than the firing temperature in a furnace. Heat treatment was performed for 1 hour in an atmosphere with an oxygen concentration of 20%. Next, after forming electrodes on both sides of the square plate and subjecting them to polarization, both sides were polished to a thickness of 0.2 mm and a large number of spot electrodes were deposited. Then, it was cut into a predetermined shape to manufacture an energy trap type piezoelectric vibrator. For comparison, a block type sintered body of the same PZT-based piezoelectric material was sliced, and the polarization treatment, polishing, electrode deposition, and cutting were performed without heat treatment, and a piezoelectric vibrator similar to the above was manufactured. When the characteristics of the respective piezoelectric vibrators thus obtained were evaluated, there were large differences in the characteristic levels and variations, and the piezoelectric vibrators of the present invention showed no deterioration in characteristics due to heat treatment, and the loop gain value It was confirmed that the improvement and the width of variation were reduced. That is, even with the same PZT-based piezoelectric material, by using the manufacturing method of the present invention, the characteristics were improved, the production yield was improved, and a highly reliable piezoelectric vibrator could be obtained with good mass productivity.

【0010】(実施形態3)図4に本発明の第3の実施
形態の製造工程図を示す。原料を所定の組成となるよう
秤量し、ボールミルで混合した後、最適仮焼温度にて仮
焼した。粉砕後PVA系バインダー溶液、分散剤を加え
混練し0.6mmの厚みに押し出し成形した。次に所定の
シート形状に切断しサヤ内に積層充填し最適焼成温度で
大気雰囲気中で1150℃で焼成した。さらに引き続き
前記焼成温度より100℃低い温度にて、炉内の酸素濃
度を30%の雰囲気とし1時間熱処理をした。このよう
にして得たPZT系圧電材料のシート型焼結体と、熱処
理していないPZT系圧電材料のシート型焼結体を実施
形態2と同様にして圧電振動子を作製し比較評価したと
ころ、熱処理したことにより特性が向上、安定化し、分
極処理後の加工による特性劣化やバインダー残留等によ
る特性ばらつきが改善されていることが確認された。な
お、本発明に関わる圧電振動子は、実施形態1に限定さ
れるものではなく、主旨の範囲内で変更できるものであ
る。さらに、本発明に関わる圧電振動子の製造方法は、
実施形態2,3に限定されるものではなく、特にPZT
系圧電材料の混合方法、造粒方法、成形方法、加工法、
サヤ内充填方法、電極形成方法は実施形態での説明以外
に任意であり、本発明の効果が有効であることは言うま
でもない。
(Embodiment 3) FIG. 4 shows a manufacturing process diagram of a third embodiment of the present invention. The raw materials were weighed so as to have a predetermined composition, mixed by a ball mill, and then calcined at an optimum calcining temperature. After pulverization, a PVA-based binder solution and a dispersant were added and kneaded, followed by extrusion molding to a thickness of 0.6 mm. Next, it was cut into a predetermined sheet shape, stacked and filled in the sheath, and fired at 1150 ° C. in the air atmosphere at the optimum firing temperature. Further, subsequently, a heat treatment was performed at a temperature lower than the firing temperature by 100 ° C. in an atmosphere having an oxygen concentration of 30% in the furnace for 1 hour. A sheet-type sintered body of the PZT-based piezoelectric material thus obtained and a sheet-type sintered body of the PZT-based piezoelectric material that has not been heat-treated were manufactured in the same manner as in Embodiment 2 and a comparative evaluation was conducted. It was confirmed that the characteristics were improved and stabilized by the heat treatment, and the characteristic deterioration due to the processing after the polarization treatment and the characteristic variation due to the residual binder were improved. The piezoelectric vibrator according to the present invention is not limited to the first embodiment, and can be changed within the scope of the gist. Furthermore, the method for manufacturing a piezoelectric vibrator according to the present invention is
The present invention is not limited to Embodiments 2 and 3, and in particular PZT
-Based piezoelectric material mixing method, granulation method, molding method, processing method,
Needless to say, the method of filling the sheath and the method of forming the electrodes are arbitrary except the description in the embodiment, and the effects of the present invention are effective.

【0011】[0011]

【発明の効果】以上のように本発明は、圧電振動子を、
酸素が熱拡散により内部まで浸透し得るように2mm以下
の厚みにして、酸素濃度10%以上の雰囲気中、所定の
焼成ピーク温度より50〜500℃低い範囲内の温度
で、30分以上の熱処理したPZT系圧電材料より構成
することにより特性ばらつきの少ない高信頼性の圧電振
動子を歩留まり良く得ることができるものである。さら
に形状の大きなPZT系圧電材料の焼結体を、スライス
等の厚み加工をしたのち酸素を供給しながら熱処理する
ことにより、加工歪み、変質層の改善ができ、焼結体部
位により発生する特性ばらつきを均一化することができ
る。さらに有機系バインダー等を多く含む薄物成形体を
焼成したのち、引き続き酸素を供給しながら熱処理する
ことにより、高特性でばらつきの小さいPZT系圧電材
料を量産性良く得ることができ、高信頼性の圧電振動子
を歩留まり良く得ることができるものである。
As described above, the present invention provides a piezoelectric vibrator,
Heat treatment for 30 minutes or more at a temperature of 50 to 500 ° C. lower than a predetermined firing peak temperature in an atmosphere having an oxygen concentration of 10% or more so that oxygen can penetrate into the inside by thermal diffusion. By using the PZT-based piezoelectric material described above, it is possible to obtain a highly reliable piezoelectric vibrator with a small variation in characteristics at a high yield. Further, by subjecting a sintered body of a PZT-based piezoelectric material having a larger shape to thickness processing such as slicing and then heat-treating it while supplying oxygen, it is possible to improve processing strain and an altered layer, and characteristics generated by the sintered body site. The variation can be made uniform. Further, by firing a thin molded body containing a large amount of an organic binder and the like, and subsequently performing heat treatment while supplying oxygen, a PZT-based piezoelectric material having high characteristics and small variations can be obtained with good mass productivity, and high reliability can be obtained. The piezoelectric vibrator can be obtained with high yield.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明の実施形態1の圧電振動子のループゲイ
ン特性の分布を示す図
FIG. 1 is a diagram showing a distribution of loop gain characteristics of a piezoelectric vibrator according to a first embodiment of the present invention.

【図2】従来の圧電振動子のループゲイン特性の分布を
示す図
FIG. 2 is a diagram showing a distribution of loop gain characteristics of a conventional piezoelectric vibrator.

【図3】本発明の実施形態2の圧電振動子の製造工程の
フローチャート
FIG. 3 is a flowchart of manufacturing steps of the piezoelectric vibrator according to the second embodiment of the present invention.

【図4】本発明の実施形態3の圧電振動子の製造工程の
フローチャート
FIG. 4 is a flowchart of a manufacturing process of the piezoelectric vibrator according to the third embodiment of the present invention.

───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 FI 技術表示箇所 H03H 3/02 H01L 41/22 Z ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Office reference number FI technical display location H03H 3/02 H01L 41/22 Z

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 厚み2mm以下の形状で、所定のピーク温
度で焼成した後、酸素濃度10%以上の雰囲気中、前記
所定のピーク焼成温度より50乃至500℃低い範囲内
の温度で、30分以上の熱処理をしたPZT系の圧電材
料より構成される圧電振動子。
1. A shape having a thickness of 2 mm or less, after firing at a predetermined peak temperature, and then in an atmosphere having an oxygen concentration of 10% or more at a temperature within a range of 50 to 500 ° C. lower than the predetermined peak firing temperature for 30 minutes. A piezoelectric vibrator composed of a PZT-based piezoelectric material that has been subjected to the above heat treatment.
【請求項2】 所定のピーク温度で焼成したPZT系の
圧電材料を、厚み2mm以下にスライス加工した後、酸素
濃度10%以上の雰囲気中で、前記所定のピーク焼成温
度より50乃至500℃低い範囲内の温度で、30分以
上の熱処理して形成する圧電振動子の製造方法。
2. A PZT-based piezoelectric material fired at a predetermined peak temperature is sliced to a thickness of 2 mm or less, and then 50 to 500 ° C. lower than the predetermined peak firing temperature in an atmosphere having an oxygen concentration of 10% or more. A method for manufacturing a piezoelectric vibrator, which is formed by performing heat treatment for 30 minutes or more at a temperature within the range.
【請求項3】 厚み2mm以下にシート成形したPZT系
の圧電材料を、所定のピーク温度で焼成したのち、酸素
濃度10%以上の雰囲気中で、所定の焼成温度より50
乃至500℃低い範囲内の温度で、30分以上の熱処理
して形成する圧電振動子の製造方法。
3. A PZT-based piezoelectric material formed into a sheet having a thickness of 2 mm or less is fired at a predetermined peak temperature, and then 50% from a predetermined firing temperature in an atmosphere having an oxygen concentration of 10% or more.
A method for manufacturing a piezoelectric vibrator, which is formed by performing heat treatment for 30 minutes or more at a temperature within a range of lower by 500 ° C to 500 ° C.
JP31504895A 1995-12-04 1995-12-04 Piezoelectric vibrator and its manufacture Pending JPH09162680A (en)

Priority Applications (1)

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JP31504895A JPH09162680A (en) 1995-12-04 1995-12-04 Piezoelectric vibrator and its manufacture

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JP31504895A JPH09162680A (en) 1995-12-04 1995-12-04 Piezoelectric vibrator and its manufacture

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JPH09162680A true JPH09162680A (en) 1997-06-20

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6129886A (en) * 1997-03-31 2000-10-10 Tdk Corporation Method of preparation of piezoelectric ceramics
CN110041082A (en) * 2018-01-15 2019-07-23 日本碍子株式会社 The manufacturing method of ceramic firing body and the process for calcining of ceramic mouldings

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6129886A (en) * 1997-03-31 2000-10-10 Tdk Corporation Method of preparation of piezoelectric ceramics
CN110041082A (en) * 2018-01-15 2019-07-23 日本碍子株式会社 The manufacturing method of ceramic firing body and the process for calcining of ceramic mouldings

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