JPH0271569A - Manufacture of piezoelectric material - Google Patents
Manufacture of piezoelectric materialInfo
- Publication number
- JPH0271569A JPH0271569A JP63222943A JP22294388A JPH0271569A JP H0271569 A JPH0271569 A JP H0271569A JP 63222943 A JP63222943 A JP 63222943A JP 22294388 A JP22294388 A JP 22294388A JP H0271569 A JPH0271569 A JP H0271569A
- Authority
- JP
- Japan
- Prior art keywords
- piezoelectric material
- mixed
- pretreatment
- piezoelectric
- pretreated
- 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
Links
- 239000000463 material Substances 0.000 title claims abstract description 75
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims description 4
- 239000000843 powder Substances 0.000 abstract description 11
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000010304 firing Methods 0.000 description 8
- 238000001354 calcination Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005530 etching Methods 0.000 description 3
- 238000009694 cold isostatic pressing Methods 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910005805 NiNb Inorganic materials 0.000 description 1
- 229910020698 PbZrO3 Inorganic materials 0.000 description 1
- 241000124006 Pyrota Species 0.000 description 1
- 235000002492 Rungia klossii Nutrition 0.000 description 1
- 244000117054 Rungia klossii Species 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000020169 heat generation Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000006104 solid solution Substances 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【発明の詳細な説明】
「産業上の利用分野」
この発明は、積層圧電アクチュエータなどに使用される
圧電材料の製造方法に関するものである。DETAILED DESCRIPTION OF THE INVENTION "Field of Industrial Application" The present invention relates to a method of manufacturing a piezoelectric material used in laminated piezoelectric actuators and the like.
「従来の技術」
従来、高い圧電効果を示す圧電材料としては、Ｂ ａＴ
ｉｏ ｊ系、Ｐ ｂＴ １０３−Ｐ ｂＺ ｒｏ ３
系（ＰＺＴと略称される）などの材料が知られている。"Conventional technology" Conventionally, B aT is a piezoelectric material that exhibits a high piezoelectric effect.
io j series, P bT 103-P bZ ro 3
Materials such as PZT (abbreviated as PZT) are known.
これらの圧電材料は、圧電振動子、各種セラミックフィ
ルタ、圧電トランス、ガス器具などの着火素子、マイク
ロフォン、圧電ブザーなど種々の機器に使用されてきて
いる。These piezoelectric materials have been used in various devices such as piezoelectric vibrators, various ceramic filters, piezoelectric transformers, ignition elements for gas appliances, microphones, and piezoelectric buzzers.
また、電気−機械エネルギー変換効率の高い圧電材料と
して、Ｐ ｂ（Ｎ ｉ ’／３ Ｎ ｂ’ム）Ｏｓ−Ｐ
ｂ’ｌ’ ｉｏ ３Ｐ ｂＺ ｒｏ ３系（以下、Ｐ
ＮＮ−ＦＴ−ＰＺ系という）が知られており、各種機器
への応用が１試みられている。In addition, as a piezoelectric material with high electrical-mechanical energy conversion efficiency, Pb(N i '/3 N b' )Os-P
b'l' io 3P bZ ro 3 series (hereinafter referred to as P
(NN-FT-PZ system) is known, and one attempt has been made to apply it to various devices.
ところで、圧電材料を応用した機器Ｚ） Ｉ−）として
圧電アクチュエータがある。この圧電アクチュエータは
、消費電力、発熱、ノイズ発生などの従来より使用され
ている電磁式アクチュ」、−タＣ・）欠点をもたないば
かりでなく、小型で振動８ｉ撃に強い、位置決め分解能
が高いなどの優れた特性をらっことから実用化に向けて
研究がなされており、特に駆動性の優れた圧電アクチュ
エータとして、上記ＰＮＮ−ＰＴ−ＰＺ系などの圧電材
料からなる圧電板を多数積層した構成の積層圧電アクチ
ュエータが提案されている。By the way, there is a piezoelectric actuator as a device Z) I-) to which piezoelectric materials are applied. This piezoelectric actuator not only does not have the disadvantages of conventionally used electromagnetic actuators such as power consumption, heat generation, and noise generation, but also has a small size, high vibration resistance, and high positioning resolution. Research has been conducted toward practical application of the piezoelectric actuator, which has excellent properties such as high speed, and has been developed by laminating a large number of piezoelectric plates made of piezoelectric materials such as the PNN-PT-PZ system mentioned above. A laminated piezoelectric actuator with the following configuration has been proposed.
このＰＮＮ−ＦＴ−ＰＺ系の圧電材料を作製するには、
Ｐｂ、Ｔｉ、Ｚｒ、Ｎｂ、Ｎｉの各元素の酸化物を所定
の比率で混合し、この混合材料を仮焼し、粉砕した後、
プレス成形して成形体とし、この後成形体を焼成して作
製している。To produce this PNN-FT-PZ-based piezoelectric material,
After mixing oxides of each element of Pb, Ti, Zr, Nb, and Ni in a predetermined ratio, and calcining and pulverizing this mixed material,
The molded product is produced by press molding and then firing the molded product.
「発明が解決しようとする課題」
しかしながら、上記各原料を混合して熱処理を！ｊ色−
４−と、構成元素のうちのＰｈとＮｂとが反応を起ニし
、Ｐ ｂ：＋Ｎ ｂ４０ ＋３（パイロタ〔ｌア型）な
る組成のらのが生成し、Ｐ ｂ（Ｎ ｉ’／、Ｎ １１
２／３）０３−Ｐ ｂＴ ｉｏ ＊ＰｂＺｒＯ３のペロ
ブスカイト型の相の中に上記パイロクロア相が混在した
状態にな〜てしまい、このため圧′：ｉＬ材料の性能低
下を招いてしまう問題があった。``Problem to be solved by the invention'' However, the above raw materials are mixed and heat treated! j color-
4- and the constituent elements Ph and Nb cause a reaction, and a particle with a composition of P b:+N b40 +3 (pyrota type) is generated, and P b (N i'/, N 11
2/3) 03-P bT io *There was a problem that the above pyrochlore phase was mixed in the perovskite phase of PbZrO3, leading to a decrease in the performance of the pressure':iL material. .
本発明は、上記事情に鑑みてなされたもので、上記パイ
ロクロア相の発生を抑制することによって、高性能の圧
電材料が得られる製造方法の提供を目的としている。The present invention has been made in view of the above circumstances, and aims to provide a manufacturing method capable of obtaining a high-performance piezoelectric material by suppressing the generation of the pyrochlore phase.
「課題を解決するための手段」
上記目的達成の手段として、本発明は、ＰＮＮＰＴ−Ｐ
Ｚ系圧電材料の製造方法であって、ＮｉＮｂ、Ｔｉおよ
びＺｒの各元素のうち少なくともＮｉとＮｂとを含む混
合材料に、８５０〜９５０℃で３０分〜１０時間加熱す
る前処理を施して前処理材料とし、次いでこの前処理材
料と、上記圧電材料を構成する残りの元素を含む材料と
を混合し、この後熱処理を施すことを特徴とする圧電材
料の製造方法である。"Means for Solving the Problems" As a means for achieving the above object, the present invention provides PNNPT-P
A method for manufacturing a Z-based piezoelectric material, comprising pretreating a mixed material containing at least Ni and Nb among the elements NiNb, Ti, and Zr by heating it at 850 to 950°C for 30 minutes to 10 hours. This method of manufacturing a piezoelectric material is characterized in that the pretreated material is mixed with a material containing the remaining elements constituting the piezoelectric material, and then a heat treatment is performed.
「作用 」
Ｎｉ Ｎｂ Ｔｉ、Ｚｒの各元素の−）ち少なくと乙Ｎ
ｉとＮｂとを含む混合材料に前処理を施すことにより、
Ｎ ｉＮ ｂｙｏ ｅのコランバイトを生成させ、この
後にｌ〕ｂｏと反応させると、次式ＣＡ）３ＰｂＯ＋Ｎ
１ＮｂｚＯｓ→３Ｐｂ（Ｎｉ’／Ｊｂ”／＋）Ｏｓ・・
・・（Ａ）のように反応が起こり、パイロクロア相の発
生が抑制されて Ｐ ｂ（Ｎ ｉ’／３Ｎ ｂ’／３）
０３−Ｐ ｂＴ ｉｏ ３Ｐ ｂＺ ｒｏ ３のペロブ
スカイト単一相が実現できる。"Action" of each element Ni Nb Ti, Zr -) at least N
By pre-treating the mixed material containing i and Nb,
When columbite of N iN byo e is generated and then reacted with l]bo, the following formula CA)3PbO+N
1NbzOs→3Pb(Ni'/Jb"/+)Os...
...The reaction occurs as shown in (A), and the generation of the pyrochlore phase is suppressed, resulting in P b (N i'/3N b'/3)
A perovskite single phase of 03-P bT io 3P bZ ro 3 can be realized.
この結果、高性能のＰＮＮ−ＰＴ−ＰＺ系圧電材料を得
ることができるとともに、低温での焼結性が向上し、焼
成時の温度範囲を広げることができることから焼成操作
を容易化でき、圧電材料の生産性を向上させることがで
きる。As a result, it is possible to obtain a high-performance PNN-PT-PZ piezoelectric material, improve sinterability at low temperatures, and expand the temperature range during firing, making the firing operation easier and piezoelectric Material productivity can be improved.
以下、本発明の詳細な説明する。The present invention will be explained in detail below.
本発明による圧電材料の製造方法において、好適に使用
される原料としては、ＰＮＮ−ＰＴ−ＰＺ系圧電材料を
構成する各元素（Ｐ ｂ、Ｔ ｉ、Ｚ ｒ、Ｎ ｂおよ
びＮｉの各元素）の酸化物粉末である。これらの酸化物
粉末は、純度が９９％以−１，の材料を用いろことか梁
上しくＩＪ
本発明方法では、まず、Ｎ ｉ、Ｎ ｂ、１’ ｉ、
７． ｒの各元素のうち少なくとらＮｉとＮｂの各元素
の酸化物粉末を、各々所定の分量だけ秤量採取して混合
し、次いてこの、混合材料に、人気中（つるい（ユ酸素
雰囲気中、８５０〜９５０℃で３０分〜１０時間加熱す
る前処理を施す。この前処理によって上記混合材料中の
ＮｉとＮｂと０とが反応してＮ１ＮｂｔＯａの組成のフ
ランバイトが生成され、前処理材料が得られる。上記前
処理温度が８５０〜９５０℃の範囲外であると上記フラ
ンバイトの生成効率が悪くなる。また、上記前処理時間
が３０分未満であると各元素間の反応が不十分となり、
１０時間以上加熱してもフランバイト生成量が増加せず
、前処理材料が粗粒化してしまう。In the method for manufacturing a piezoelectric material according to the present invention, the raw materials preferably used include each element (Pb, Ti, Zr, Nb, and Ni) constituting the PNN-PT-PZ piezoelectric material. oxide powder. These oxide powders should be made of materials with a purity of 99% or more.
7. Predetermined amounts of oxide powders of at least Ni and Nb among the elements r are weighed and mixed, and then this mixed material is mixed with powdered powder in an oxygen atmosphere. , pretreatment is performed by heating at 850 to 950°C for 30 minutes to 10 hours. Through this pretreatment, Ni, Nb, and 0 in the mixed material react to generate furanbite with a composition of N1NbtOa, and the pretreated material is obtained. If the pretreatment temperature is outside the range of 850 to 950°C, the production efficiency of furanbite will be poor. In addition, if the pretreatment time is less than 30 minutes, the reaction between each element will be insufficient. Then,
Even if heated for 10 hours or more, the amount of furanbite produced does not increase, and the pretreated material becomes coarse grained.
次に、先の前処理材料に、圧電材料を構成する残りの元
素の酸化物粉末を所定量混合し、好ましくは粉砕混合処
理を施す。これによって、圧電材料を構成する全ての元
素を含む圧電素材を得る。Next, a predetermined amount of oxide powder of the remaining elements constituting the piezoelectric material is mixed into the pretreated material, and preferably subjected to a pulverization and mixing treatment. As a result, a piezoelectric material containing all the elements constituting the piezoelectric material is obtained.
この後、得られた圧電素材に適宜な熱処理を施すことに
より、圧電素材中に含まれる各元素ｌよ反応を起こし、
Ｐ Ｎ Ｎ −Ｐ Ｔ −Ｐ Ｚ系（ペロブスカイト型
）の単一相からなる圧電材料が得られる。After that, by subjecting the obtained piezoelectric material to an appropriate heat treatment, each element contained in the piezoelectric material causes a reaction,
A piezoelectric material consisting of a single phase of PNN-PT-PZ system (perovskite type) is obtained.
この圧電素材に熱処理を施して圧電材料を得る方法の一
例を説明すると、まず、先の圧電素材に、大気中あるい
は酸素雰囲気中、８００〜９５０°Ｃで３０分〜数時間
加熱する仮焼を施す。To explain an example of a method for obtaining a piezoelectric material by subjecting this piezoelectric material to heat treatment, first, the piezoelectric material is calcined by heating at 800 to 950°C for 30 minutes to several hours in the air or oxygen atmosphere. give
次に、仮焼を施した材料を粉砕処理して仮焼粉末とする
。次に、仮焼粉末を造粒し、そして所望形状にプレス成
形し、ざらにＣＩＰ（冷間静水圧加圧）処理を施して成
形体とする。Next, the calcined material is pulverized into calcined powder. Next, the calcined powder is granulated, press-molded into a desired shape, and roughly subjected to CIP (cold isostatic pressing) treatment to form a compact.
次に、得られた成形体を焼成し、圧電材料を作製する。Next, the obtained molded body is fired to produce a piezoelectric material.
このときの焼成条件は、１１００〜１３００℃で３０分
〜１０時間程度が好適である。以上の各操作により、所
定の形状に焼結された圧電材料が得られる。このように
して得られた圧電材料は、使用用途に応じて研摩処理を
施しても良い。The firing conditions at this time are preferably 1100 to 1300°C for about 30 minutes to 10 hours. Through each of the above operations, a piezoelectric material sintered into a predetermined shape is obtained. The piezoelectric material thus obtained may be subjected to a polishing treatment depending on the intended use.
次に、本発明の実施例を記し、本発明による圧電材料の
製造方法の作用効果を明確化する。Next, examples of the present invention will be described to clarify the effects of the piezoelectric material manufacturing method according to the present invention.
「実施例」
Ｐ ｂ、Ｔ ｉ、 ７． ｒ、Ｘｂ、Ｎ ｉ／／）３元
素の酸化物粉末（純１炬９９％以上）を完Ｔ４として用
い、す、下に示オニＦ５：碩に、（０５０）Ｐｂ（Ｎ＋
’／３Ｎｂ’／３）０３−（０，３８）ＰｂＴ＋０３（
０，１２）ＰｂＺｒＯ，ζろ組成の圧電材木４のペレッ
トを１′］ 装 し ｆ二。"Example" P b, T i, 7. An oxide powder of three elements (r,
'/3Nb'/3)03-(0,38)PbT+03(
0,12) Loaded with pellets of piezoelectric material 4 of PbZrO, zeta composition.
（工程）
（前処理−）混合−仮焼一扮砕一造粒一プレスーｃｒｐ
→焼成
そして、前処理の有無および前処理時の混合元素、仮焼
条件、ゴミぬきの有無の各項目のいずれかが異なる８種
類の試料を作製しｆこ。前処理を行イつない４種類の試
料を比較例１ないし比較例４とし、詳細を第１表に示し
た。また前処理を行った４種類の試料を実施例１ないし
実施例４とし、詳細を第２表に示した。(Process) (Pretreatment-) Mixing - Calcination - Crushing - Granulation - Press - CRP
→Calcination Then, eight types of samples were prepared that differed in any of the following items: presence or absence of pretreatment, mixed elements during pretreatment, calcination conditions, and presence or absence of dust removal. Four types of samples subjected to pretreatment were designated as Comparative Examples 1 to 4, and details are shown in Table 1. Furthermore, the four types of samples subjected to pretreatment were designated as Examples 1 to 4, and the details are shown in Table 2.
以下余白
第１表および第２表に示す各試料を用い、各試料毎に１
１８０℃〜１３００°Ｃの間の異なる焼成温度で焼成し
て圧電材料のベレット（以下、試験品という）を作製し
、■密度、■Ｅ”／Ｅｏ（誘電率）、■ｔａｎδ（誘電
損失）、■Ｒ，（直列抵抗）、■Ｑｍ（Ｉ械的品質係数
）、■Ｋｒ（表面波結合係数）、■電歪特性、■ヒステ
リシス、■Ｘ線回折、りΦサーマルエツチングによる粒
子観察の各試験を行った。各試験の結果を以下に記す。Using each sample shown in Tables 1 and 2 in the margin below, 1
Piezoelectric material pellets (hereinafter referred to as test products) were produced by firing at different firing temperatures between 180°C and 1300°C, and the following properties were determined: ■density, ■E''/Eo (permittivity), and ■tanδ (dielectric loss). , ■R, (series resistance), ■Qm (I mechanical quality factor), ■Kr (surface wave coupling coefficient), ■electrostrictive characteristics, ■hysteresis, ■X-ray diffraction, and particle observation by thermal etching. Tests were conducted.The results of each test are described below.
以下余白
■密度
各試験品の密度を水中法で測定した。結果を第３表に示
す。The following margin is ■Density The density of each test product was measured by an underwater method. The results are shown in Table 3.
■ Ｅ”／ Ｅ ａ （誘電率）
各試験品を研摩し、電極焼付けを行い、誘電率（ポーリ
ング前の誘電率）を測定した。結果を第４表に示す。■ E"/E a (permittivity) Each test piece was polished, electrodes were baked, and the dielectric constant (permittivity before poling) was measured. The results are shown in Table 4.
また、各試験品を研摩し、？Ｉｔｌ！ｌｉｉ焼付けを行
い、さらにポーリング処理を行った後、誘電率（ポーリ
ング後の誘電率）を測定した。結果を第５表に示す。Also, each test item was polished and? Itl! After performing lii baking and further performing poling treatment, the dielectric constant (dielectric constant after poling) was measured. The results are shown in Table 5.
第５表
■ｔａｎδ（誘電損失）
各試験品を研摩し、電極焼付けを行い、誘電損失（ポー
リング前の誘電損失）を測定した。結果を第６表に示す
。Table 5 - tan δ (dielectric loss) Each test piece was polished, electrode baked, and dielectric loss (dielectric loss before poling) was measured. The results are shown in Table 6.
また、各試験品を研摩し、電極焼付けを行い、さらにポ
ーリング処理を行った後、誘電損失（ポーリング後の誘
電損失）を測定した。結果を第７表に示す。In addition, each test piece was polished, electrode baked, and further subjected to poling treatment, and then the dielectric loss (dielectric loss after poling) was measured. The results are shown in Table 7.
■ Ｒ，（直列抵抗）
各試験品を研摩し、電極焼付けを行い、直列抵抗を測定
した。結果を第８表に示す。■R, (Series Resistance) Each test piece was polished, electrodes were baked, and the series resistance was measured. The results are shown in Table 8.
■ＱＩ１１（機械的品質係数）
各試験品を＠摩し、電極焼付けを行い、機械的品質特性
を測定した。結果を第９表に示す。■QI11 (Mechanical Quality Factor) Each test product was polished, electrode baked, and mechanical quality characteristics were measured. The results are shown in Table 9.
第８表
（単位
Ω）
■Ｋｒ（表面波結合係数）
各試験品を研摩し、電極焼付けを行い、表面波結合係数
を測定した。結果を第１０表に示す。Table 8 (unit: Ω) ■Kr (Surface Wave Coupling Coefficient) Each test piece was polished, electrodes were baked, and the surface wave coupling coefficient was measured. The results are shown in Table 10.
■電歪特性（０→１０ Ｋ Ｖ ／ ｃ ｍ ）各試験
品を研摩し、電極焼付けを行い、電歪特性（ポーリング
前の電歪特性）を測定した。結果を第１１表に示す。■Electrostrictive properties (0→10 KV/cm) Each test piece was polished, electrode baked, and the electrostrictive properties (electrostrictive properties before poling) were measured. The results are shown in Table 11.
また、各試験品を研摩し、電極焼付けを行い、さらにポ
ーリング処理を行った後、電歪特性（ポーリング後の電
歪特性）を測定した。結果を第１２表に示す。In addition, each test piece was polished, electrode baked, and further subjected to poling treatment, and then the electrostrictive properties (electrostrictive properties after poling) were measured. The results are shown in Table 12.
■ ヒステリシス
各試験品を研摩し、電極焼付けを行い、ヒステリシス（
ポーリング前のヒステリシス）を測定した。■ Hysteresis Each test item is polished, electrode baked, and hysteresis (
(hysteresis before polling) was measured.
結果を第１３表に示す。なお、ヒステリシス（％）は、
第１図の図中△ＵおよびＵｍａｘより、ヒステリシス（
％）＝△Ｕ／ Ｕｍａｘ （ただし、Ｖｍａｘ＝１０に
Ｖ／ｃｔａ、 １／２ＶＩＩｌａｘ＝５ＫＶ／ａｌｌ）
により求めた。The results are shown in Table 13. In addition, hysteresis (%) is
From △U and Umax in Figure 1, the hysteresis (
%)=△U/Umax (However, Vmax=10 and V/cta, 1/2VIIlax=5KV/all)
It was determined by
また、各試験品を研摩し、電極焼付けを行い、さらにポ
ーリング処理を行った後、ヒステリツス（ポーリング後
のヒステリツス）を測定した。結果を第１４表に示す。In addition, each test piece was polished, electrode baked, and further subjected to poling treatment, and then the hysteresis (hysteresis after poling) was measured. The results are shown in Table 14.
第１４表
（単位９％ ）
■Ｘ線回折
焼成館の各試料（各試料の仮焼粉末）を用い、Ｘ線回折
でそれらの結晶構造を調べた。Table 14 (Unit: 9%) ■X-ray diffraction Using each sample (calcined powder of each sample) from the calcining chamber, their crystal structures were investigated by X-ray diffraction.
その結果、比較例Ｉおよび比較例２では、まだＰＮＮ−
ＰＴ−ＰＺ系（ペロブスカイト型）まで成長しておらず
、各成分が固溶体を形成していない状態であった。また
比較例３および比較例４では、ＰＮＮ−ＰＴ−ＰＺらし
きペロブスカイト状のピークが見られろが、同時にｒ’
ｂｓＮ ！＋４０１３（パイロクロア型）のピーク６
見らメ１ｆ二。As a result, in Comparative Example I and Comparative Example 2, PNN−
It was not grown to a PT-PZ system (perovskite type), and each component did not form a solid solution. In addition, in Comparative Examples 3 and 4, a perovskite peak that seems to be PNN-PT-PZ is observed, but at the same time r'
bsN! +4013 (pyrochlore type) peak 6
Look at me 1f2.
一方、実施例また゛いし実施例４ ｙ） ｈ試料に！ｊ
いては、このＰ ｂｓ Ｎ ｂ４ｏ 、 、のピークは
見ら、４ｔなか−、た。On the other hand, Example 4 y) h sample! j
However, this peak of P bs N b4o , , was not observed at 4t.
［株］サーマルエツチングによる粒子観察サーマルエツ
チングにより、谷試験品のＴＩｒ−ｉ−状態を観察した
。[Co., Ltd.] Particle Observation by Thermal Etching The TIr-i state of the Tani test product was observed by thermal etching.
その結果、前処理時に添加する元素がＮｉとＮｂだけで
あった試験品（実施例２および実施例４の各試験品）の
方が、Ｎｉ、Ｎｂ、Ｔｉ、７．ｒを添加しｆ二番試験品
よりら粒径が大きくなっｆ二。（第１５表）以」二の各
試験の結果、実施例１ないし実施例４の各試験品は、前
処理を施さない比較例１ないし比較例４の各試験品に比
べ、電気特性などが良好であった。As a result, the test products in which only Ni and Nb were added at the time of pretreatment (the test products of Example 2 and Example 4) were better than those in which Ni, Nb, Ti, and 7. When r was added, the particle size became larger than that of the f2 test product. (Table 15) As a result of the following tests, the test products of Examples 1 to 4 had better electrical properties than the test products of Comparative Examples 1 to 4, which were not subjected to pretreatment. It was good.
第１５表
粒径（７１ｍ）
「発明の効果」
以上説明したように、本発明による圧電材料の製造方法
は、Ｉ） Ｎ Ｎ −Ｐ ’Ｉ’ −１） Ｚ系１１：
、電Ｍ１゛’ｌを製造するに際し、Ｎ ｉ、Ｎｂ、’ｌ
” ｉ、Ｚ ｒの６元素のうし少なくともＮｉとＮｂと
を含む混合材料に前処理を施して、Ｎ１ＮｂｔＯｓのコ
ランバイトを生成させ、この後にＰｂＯと反応させるこ
とによって、パイロクロア相の発生を抑制してＰ ｂ（
Ｎ ｉ’／３Ｎ ｂ２／３）ｏ ３Ｐ ｂＴ ＋ Ｏｓ
−Ｐ ｂＺ ｒｏ ３のペロブスカイト単一用からなる
圧電材料を製造することかでき、高性能のＰＮＮ−ＰＴ
−ＰＺ系圧電材料を得ることができる。Table 15 Particle Size (71 m) "Effects of the Invention" As explained above, the method for manufacturing a piezoelectric material according to the present invention is based on I) N N -P 'I' -1) Z system 11:
, Nb,'l when manufacturing electric M1''l
” A mixed material containing six elements i, Zr and at least Ni and Nb is pretreated to produce columbite of N1NbtOs, and then reacted with PbO to suppress the generation of the pyrochlore phase. teP b(
N i'/3N b2/3) o 3P bT + Os
- A piezoelectric material consisting of a single perovskite of P bZ ro 3 can be manufactured, and a high performance PNN-PT
- A PZ-based piezoelectric material can be obtained.
また、上記前処理を行うことによって、低温での焼結性
が向上し、焼成温度範囲を広く設定することができるこ
とから、圧電材料製造の際の焼成操作を容易化でき、圧
電材料の生産性を向上させることができる。In addition, by performing the above pretreatment, sinterability at low temperatures is improved, and the firing temperature range can be set over a wide range, making it easier to perform the firing operation when manufacturing piezoelectric materials, thereby increasing the productivity of piezoelectric materials. can be improved.
第１図はヒステリツスの求め方を説明ｔろためのグラフ
である。FIG. 1 is a graph for explaining how to obtain hysteresis.
Claims (1)
ｂＴｉＯ＿３−ＰｂＺｒＯ＿３系圧電材料の製造方法で
あって、 Ｎｉ，Ｎｂ，ＴｉおよびＺｒの各元素のうち少なくとも
ＮｉとＮｂとを含む混合材料に、８５０〜９５０℃で３
０分〜１０時間加熱する前処理を施して前処理材料とし
、次いでこの前処理材料と、上記圧電材料を構成する残
りの元素を含む材料とを混合し、この後熱処理を施すこ
とを特徴とする圧電材料の製造方法。[Claims] Pb(Ni_1_/_3Nb_2_/_3)O_3-P
bTiO_3-PbZrO_3-based piezoelectric material manufacturing method, comprising: heating a mixed material containing at least Ni and Nb among the elements Ni, Nb, Ti, and Zr at 850 to 950°C.
The piezoelectric material is characterized by performing a pretreatment of heating for 0 minutes to 10 hours to obtain a pretreatment material, then mixing this pretreatment material with a material containing the remaining elements constituting the piezoelectric material, and then subjecting the piezoelectric material to a heat treatment. A method for manufacturing a piezoelectric material.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63222943A JPH0271569A (en) | 1988-09-06 | 1988-09-06 | Manufacture of piezoelectric material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63222943A JPH0271569A (en) | 1988-09-06 | 1988-09-06 | Manufacture of piezoelectric material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0271569A true JPH0271569A (en) | 1990-03-12 |
Family
ID=16790301
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63222943A Pending JPH0271569A (en) | 1988-09-06 | 1988-09-06 | Manufacture of piezoelectric material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0271569A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07133152A (en) * | 1993-11-04 | 1995-05-23 | Nec Corp | Production of piezoelectric porcelain composition |
-
1988
- 1988-09-06 JP JP63222943A patent/JPH0271569A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07133152A (en) * | 1993-11-04 | 1995-05-23 | Nec Corp | Production of piezoelectric porcelain composition |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4541985B2 (en) | Method for producing polycrystal | |
| US8269402B2 (en) | BNT-BKT-BT piezoelectric composition, element and methods of manufacturing | |
| CN100509703C (en) | Method for preparing ferrite bismuth lanthanum-titanate lead solid solution ceramic under strong magnetic field action | |
| JP2518703B2 (en) | Laminated composite piezoelectric body and manufacturing method thereof | |
| JP4450636B2 (en) | Method for manufacturing piezoelectric ceramics | |
| Kim et al. | Fabrication of fine-grain piezoelectric ceramics using reactive calcination | |
| CN109553413B (en) | Textured piezoelectric ceramic and preparation method and application thereof | |
| CN106518070B (en) | A kind of polynary system high-voltage electricity active piezoelectric ceramic material and preparation method thereof | |
| CN111269009A (en) | Bismuth zirconate manganate-bismuth scandate-lead titanate series piezoelectric ceramic material and preparation method thereof | |
| JP3666182B2 (en) | Method for producing crystal-oriented ceramics | |
| JPH10139552A (en) | Crystal oriented ceramics and its production | |
| JP5937774B1 (en) | Piezoelectric ceramic and manufacturing method thereof, and electronic component | |
| US5788876A (en) | Complex substituted lanthanum-lead-zirconium-titanium perovskite, ceramic composition and actuator | |
| EP1358137A2 (en) | Method for making lead zirconate titanate-based ceramic powder, piezoelectric ceramic and method for making same | |
| Pang et al. | A lead-reduced ferrolectric solid solution with high curie temperature: BiScO3–Pb (Zn1/3Nb2/3) O3–PbTiO3 | |
| GB2550887A (en) | Temperature stable lead-free piezoelectric/electrostrictive materials with enhanced fatigue resistance | |
| CN115894020B (en) | PMNZT-based piezoelectric ceramic with high piezoelectric coefficient and preparation method and application thereof | |
| JPH0271569A (en) | Manufacture of piezoelectric material | |
| CN114213121A (en) | High-voltage, high-dielectric and high-curie piezoelectric ceramic piece | |
| CN102351535B (en) | Low-loss sodium potassium niobate-based lead-free piezoelectric ceramic material and preparation method thereof | |
| JP2010222185A (en) | Anisotropic-shape powder and method for manufacturing of crystal-oriented ceramic | |
| JP6627440B2 (en) | Piezoelectric ceramic, piezoelectric ceramic electronic component, and method of manufacturing piezoelectric ceramic | |
| Tunkasiri | Properties of PZT ceramics prepared from aqueous solutions | |
| CN114804874B (en) | Quaternary piezoelectric ceramic and preparation method and application thereof | |
| CN117326866B (en) | Cerium-manganese co-doped lead zirconate titanate-based piezoelectric ceramic material and preparation method thereof |