JPH0548173A - Manufacture of piezoelectric material ceramics - Google Patents
Manufacture of piezoelectric material ceramicsInfo
- Publication number
- JPH0548173A JPH0548173A JP3200697A JP20069791A JPH0548173A JP H0548173 A JPH0548173 A JP H0548173A JP 3200697 A JP3200697 A JP 3200697A JP 20069791 A JP20069791 A JP 20069791A JP H0548173 A JPH0548173 A JP H0548173A
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- JP
- Japan
- Prior art keywords
- polarization
- voltage
- time
- treatment
- applying
- 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.)
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- Compositions Of Oxide Ceramics (AREA)
- Piezo-Electric Or Mechanical Vibrators, Or Delay Or Filter Circuits (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は圧電体磁器の製造方法に
関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for manufacturing a piezoelectric ceramic.
【０００２】[0002]
【従来の技術】圧電体磁器の製造は、例えばチタン酸バ
リウム系の場合には、炭酸バリウムと酸化チタンを主原
料として、これに炭酸カルシウムや酸化鉛などを添加
し、所定のモル比になるように秤量し混合する。混合の
終わった原料は、焼成温度よりやや低い温度で仮焼して
粉砕する。この仮焼により焼成時の異常膨張や収縮が防
止される。2. Description of the Related Art In the manufacture of piezoelectric ceramics, for example, in the case of barium titanate type, barium carbonate and titanium oxide are used as main raw materials, and calcium carbonate, lead oxide, etc. are added thereto to obtain a predetermined molar ratio. And weigh and mix. The mixed raw materials are calcined at a temperature slightly lower than the firing temperature and pulverized. This calcination prevents abnormal expansion and contraction during firing.
【０００３】仮焼した粉末は可塑性がないのでポリビニ
ールアルコール水溶液などのバインダを混ぜて団粒に造
粒した後、プレス法などで成形する。成形体はふた付き
のマグネシアまたはアルミナのさやに入れて、電気炉ま
たはガス炉で所定の最適温度で所定時間焼成される。Since the calcined powder has no plasticity, a binder such as an aqueous solution of polyvinyl alcohol is mixed and granulated into granules, which are then molded by a pressing method or the like. The compact is placed in a lidded magnesia or alumina sheath and fired in an electric furnace or a gas furnace at a predetermined optimum temperature for a predetermined time.
【０００４】焼成の終わったセラミックスは所定の寸法
に加工した後、焼付けあるいは真空蒸着により銀電極を
取付け、シリコンオイル中で直流電界を印加し分極処理
が行われる。分極処理の後、セラミックスに残った残留
分極は時間の経過とともに漸減するので、初期の短時間
に生ずる変化を加速するエージング処理を行ってから使
用する。The fired ceramics are processed into a predetermined size, and then a silver electrode is attached by baking or vacuum deposition, and a direct current electric field is applied in silicon oil to perform polarization treatment. After the polarization treatment, the residual polarization remaining in the ceramics gradually decreases with the passage of time, so the aging treatment for accelerating the change occurring in the initial short time is performed before use.
【０００５】また、分極処理後の圧電磁器の熱衝撃サイ
クル（−４５℃〜８０℃）による電気的特性の劣化を防
止するために、圧電磁器のキュリー点近傍の温度で短時
間熱処理する圧電磁器の製造方法が提案されている（特
開昭６４−２３８３号公報）。Further, in order to prevent the deterioration of the electrical characteristics due to the thermal shock cycle (-45 ° C. to 80 ° C.) of the piezoelectric ceramic after the polarization treatment, the piezoelectric ceramic is heat-treated for a short time at a temperature near the Curie point of the piezoelectric ceramic. Has been proposed (Japanese Patent Laid-Open No. 64-2383).
【０００６】[0006]
【発明が解決しようとする課題】しかしながら、前記の
圧電磁器の分極処理後のエージング処理は、８０〜２０
０℃の温度で１０〜１００時間保持する必要があり、エ
ージング処理時間が長く、量産効率が悪いという問題点
がある。さらに、前記特開昭６４−２３８３号公報の提
案においても、３００℃に近い温度で数十秒保持する熱
処理であるため、肉厚の圧電磁器では質量効果が問題と
なる他、高温保持により結合係数の低下が大きいという
欠点がある。However, the aging process after the polarization process of the piezoelectric ceramic is 80 to 20.
It is necessary to hold at a temperature of 0 ° C. for 10 to 100 hours, there is a problem that the aging treatment time is long and mass production efficiency is poor. Further, in the proposal of the above-mentioned Japanese Patent Laid-Open No. 64-2383, since the heat treatment is carried out at a temperature close to 300 ° C. for several tens of seconds, the mass effect becomes a problem in a thick piezoelectric ceramic, and the bonding is performed at a high temperature. There is a drawback that the coefficient is greatly reduced.
【０００７】本発明は圧電磁器の分極処理後のエージン
グ処理に長時間を要し、生産能率が悪いという前記のご
とき問題点を解決すべくなされたものであって、極めて
短時間にエージング処理ができる圧電体磁器の製造方法
を提供することを目的とする。The present invention is intended to solve the above-mentioned problem that the aging treatment after the polarization treatment of the piezoelectric ceramic requires a long time and the production efficiency is poor. It is an object of the present invention to provide a method for manufacturing a piezoelectric ceramic which can be performed.
【０００８】[0008]
【課題を解決するための手段】発明者は、残留分極の漸
減を早めるための従来のエージング処理が、専ら加熱に
よるために時間を要することに鑑み、加熱によらずに残
留分極の漸減を早める方法について鋭意検討を重ねた。
その結果、分極時とは逆方向に直流電圧を印加すれば、
エージング処理時間を著しく短縮できることを新たに知
見し本発明を完成した。In view of the fact that the conventional aging treatment for accelerating the gradual decrease of remanent polarization takes time because it is exclusively due to heating, the inventor hastens the gradual decrease of remanent polarization without depending on heating. The method was studied thoroughly.
As a result, if a DC voltage is applied in the opposite direction to that during polarization,
The present invention has been completed by newly finding that the aging treatment time can be remarkably shortened.
【０００９】本発明の圧電体磁器の製造方法は、成形焼
成後の圧電体磁器に直流電圧を印加して分極処理をする
工程と、前記圧電体磁器に分極時の電圧の１／５〜１／
５０の直流電圧を分極時と逆方向に印加する工程とから
なることを要旨とする。In the method for manufacturing a piezoelectric ceramic according to the present invention, a step of applying a DC voltage to the piezoelectric ceramic after molding and firing to perform polarization processing, and 1/5 to 1 to 1 of the voltage at the time of polarization of the piezoelectric ceramic. /
The gist is that it comprises a step of applying a DC voltage of 50 in the direction opposite to that during polarization.
【００１０】[0010]
【作用】成形焼成後の圧電体磁器に直流電圧を印加して
分極処理をする工程により、各結晶粒子内の各分域の方
向が、印加した電界に近い方向に回転または反転して電
荷が現れる。電界を取り去った後にも分極は残留し、圧
電体磁器は圧電性を示す。By the step of applying a DC voltage to the piezoelectric ceramics after molding and firing to perform polarization processing, the direction of each domain in each crystal grain rotates or reverses to a direction close to the applied electric field, and electric charges are generated. appear. The polarization remains even after the electric field is removed, and the piezoelectric ceramic exhibits piezoelectricity.
【００１１】分極処理はシリコンオイル中で直流電界を
印加して行われる。分極電圧は高いほど効果的である
が、圧電体磁器の耐電圧、漏洩電流の関係などによって
最適値を選択して行われる。例えばチタン酸バリウムで
は、厚さ１ｍｍ当たり２ｋｖ程度の電圧で数時間の処理
が行われる。The polarization treatment is performed by applying a DC electric field in silicon oil. The higher the polarization voltage is, the more effective it is. However, the optimum value is selected depending on the relationship between the withstand voltage and leakage current of the piezoelectric ceramics. For example, barium titanate is treated for several hours at a voltage of about 2 kv per mm of thickness.
【００１２】圧電体磁器に分極時の電圧の１／５〜１／
５０の電圧を分極時と逆方向に直流電圧を印加すること
により、残留分極の漸減が著しく早められる。印加する
電圧を分極時の電圧の１／５〜１／５０としたのは、電
圧が１／５０未満であるときは、残留分極の漸減を充分
に速めることができないからであり、電圧が１／５を越
えると結合係数が低下して電気的特性が劣化するからで
ある。1/5 to 1/1 / the voltage when polarized in the piezoelectric ceramic
By applying a DC voltage to the voltage of 50 in the direction opposite to that at the time of polarization, the gradual decrease of remanent polarization is significantly accelerated. The reason why the applied voltage is set to 1/5 to 1/50 of the voltage during polarization is that when the voltage is less than 1/50, it is not possible to sufficiently accelerate the gradual decrease of the remanent polarization. This is because if it exceeds / 5, the coupling coefficient decreases and the electrical characteristics deteriorate.
【００１３】逆電圧の印加は分極処理と同様にシリコン
オイル中で行う。逆電圧の印加時間は、圧電体磁器の厚
さ、印加する電圧、シリコンオイルの温度等により適宜
選択する。続けて行われるエージング処理は、従来から
行われている方法と何等変わりなく、８０〜２００℃の
温度に保持するものであるが、この処理により残留分極
はさらに安定化する。The reverse voltage is applied in silicone oil as in the polarization treatment. The application time of the reverse voltage is appropriately selected depending on the thickness of the piezoelectric ceramics, the applied voltage, the temperature of silicon oil, and the like. The subsequent aging treatment is the same as the conventional method, and the temperature is maintained at 80 to 200 ° C., but the residual polarization is further stabilized by this treatment.
【００１４】[0014]
【実施例】本発明の実施例を従来例および比較例と併せ
て説明し、本発明の効果を明らかにする。平均粒子径１
μｍのＰｂＯ、ＺｒＯ2、ＴｉＯ2原料粉末をＰｂ（Ｔｉ
0.48Ｚｒ 0.52）Ｏ3の組成となるように秤量後、ボール
ミルで４８時間粉砕し、９００℃で１時間焼成後、再び
ボールミルで粉砕、乾燥した。乾燥原料にバインダとし
てＰＶＡ（ポリビニールアルコール）を約５重量％加え
て造粒後、油圧プレスで圧力１ｔｏｎ／ｃｍ2で、直径
約１３ｍｍ、厚さ２ｍｍの円板に形成した。EXAMPLES Examples of the present invention are combined with conventional examples and comparative examples.
And the effect of the present invention will be clarified. Average particle size 1
μm PbO, ZrO2, TiO2The raw material powder is Pb (Ti
0.48Zr 0.52) O3After weighing to the composition
Mill for 48 hours, fire at 900 ° C for 1 hour, then
It was crushed with a ball mill and dried. As a binder for dry ingredients
Add about 5% by weight of PVA (polyvinyl alcohol)
After granulating, the pressure is 1ton / cm with a hydraulic press.2And the diameter
It was formed into a disk having a thickness of about 13 mm and a thickness of 2 mm.
【００１５】成形体をＺｒＯ2の粉末を敷いたＡｌ2Ｏ3
匣鉢に入れ、昇温速度３００℃／ｈｒで昇温して大気炉
内１２５０℃で１時間焼成した。得られた試料の表面に
Ａｇ電極ペーストを塗布し、６００℃で焼成して電極を
形成した。続いて、試料を温度８０℃に加熱したシリコ
ンオイル中で３ｋｖ／ｍｍ2の直流電圧を１時間印加し
て分極処理を施した。分極処理後の試料について、室温
で圧電特性（Ｋｐ）を測定した。The compact was Al 2 O 3 coated with ZrO 2 powder.
The mixture was placed in a sagger and heated at a temperature rising rate of 300 ° C./hr, and baked in an atmospheric furnace at 1250 ° C. for 1 hour. An Ag electrode paste was applied to the surface of the obtained sample and baked at 600 ° C. to form an electrode. Subsequently, the sample was polarized by applying a DC voltage of 3 kv / mm 2 in silicon oil heated to a temperature of 80 ° C. for 1 hour. The piezoelectric property (Kp) of the sample after the polarization treatment was measured at room temperature.
【００１６】次に分極処理後の試料について、表１に示
す温度のシリコンオイル中で、表１に示す直流電圧を分
極処理時と逆の極性にして、１時間、１０時間および１
００時間のエージング処理時の室温での圧電特性（Ｋ
ｐ）を測定した。得られた測定値は分極処理後の試料に
ついて測定した室温で圧電特性（Ｋｐ）との比（エージ
ング処理時の室温Ｋｐ値／分極処理後の室温Ｋｐ値）と
して表１にまとめて示した。Next, with respect to the sample after the polarization treatment, the direct current voltage shown in Table 1 was set in the silicone oil at the temperature shown in Table 1 with the polarity opposite to that at the time of the polarization treatment for 1 hour, 10 hours and 1 hour.
Piezoelectric properties at room temperature during aging treatment for 00 hours (K
p) was measured. The obtained measured values are collectively shown in Table 1 as a ratio (room temperature Kp value during aging treatment / room temperature Kp value after polarization treatment) to the piezoelectric characteristics (Kp) measured at room temperature after the polarization treatment.
【００１７】なお、表１において、比較例１は電圧が０
である場合、比較例２は電圧が本発明よりも高かった場
合、比較例３は電圧が本発明よりも低かった場合、比較
例４はシリコンオイルの温度が異常に低かった場合であ
る。In Table 1, Comparative Example 1 has a voltage of 0.
In Comparative Example 2, the voltage was higher than the present invention, in Comparative Example 3 the voltage was lower than the present invention, and in Comparative Example 4, the temperature of the silicone oil was abnormally low.
【００１８】[0018]
【表１】 [Table 1]
【００１９】表１から明らかなように、分極処理後に逆
電圧を印加しなかった比較例１は、残留分極の減少が大
きく、エージングによる安定化に１００時間を要した。
また、印加電圧が本発明より高かった比較例２は、エー
ジングにより残留分極の漸減はなかったものの、圧電特
性の劣化が大きかった。比較例３は印加電圧が低かった
ので、比較例１と同様に残留分極の減少が大きく、エー
ジングによる安定化に１００時間を要した。比較例４は
印加電圧は適正であったが、シリコンオイルの温度が低
かったため、同様の結果となった。As is clear from Table 1, in Comparative Example 1 in which the reverse voltage was not applied after the polarization treatment, the remanent polarization was greatly reduced and it took 100 hours to stabilize due to aging.
Further, in Comparative Example 2 in which the applied voltage was higher than that of the present invention, although the remanent polarization did not gradually decrease due to aging, the piezoelectric characteristics were significantly deteriorated. Since the applied voltage was low in Comparative Example 3, the reduction of remanent polarization was large similarly to Comparative Example 1, and it took 100 hours to stabilize due to aging. In Comparative Example 4, the applied voltage was appropriate, but the same result was obtained because the temperature of the silicone oil was low.
【００２０】これに対して、本発明の実施例１〜４は、
圧電特性の低下も０．８８程度と少なく、エージング処
理により１０時間位で特性が安定化し、エージング処理
時間が短縮化できることが確認された。On the other hand, Examples 1 to 4 of the present invention are
It was confirmed that the deterioration of the piezoelectric characteristics was as small as about 0.88, the characteristics were stabilized by aging treatment in about 10 hours, and the aging treatment time could be shortened.
【００２１】[0021]
【発明の効果】本発明の圧電体磁器の製造方法は以上説
明したように、成形焼成後の圧電体磁器に直流電圧を印
加して分極処理をする工程と、前記圧電体磁器に分極時
の電圧の１／５〜１／５０の電圧を分極時と逆方向の直
流電圧を印加工程とからなることを特徴とするものであ
って、分極処理後に分極時と逆方向の直流電圧が印加さ
るので、分極処理後の残留分極の漸減が速められ、エー
ジング処理時間が著しく短縮され、短時間で圧電体磁器
を安定化することができる。As described above, the method for manufacturing a piezoelectric ceramic according to the present invention includes a step of applying a DC voltage to the piezoelectric ceramic after molding and firing to perform polarization processing, and a step of performing polarization treatment on the piezoelectric ceramic. It is characterized in that it comprises a step of applying a DC voltage of 1/5 to 1/50 of the voltage in the opposite direction to that during polarization, wherein a DC voltage in the opposite direction to that during polarization is applied after the polarization treatment. Therefore, the gradual decrease of the residual polarization after the polarization treatment is accelerated, the aging treatment time is significantly shortened, and the piezoelectric ceramic can be stabilized in a short time.
Claims (1)
加して分極処理をする工程と、前記圧電体磁器に分極時
の電圧の１／５〜１／５０の直流電圧を分極時と逆方向
に印加する工程とからなることを特徴とする圧電体磁器
の製造方法。1. A step of applying a DC voltage to a piezoelectric ceramics after molding and firing for polarization, and a DC voltage of ⅕ to 1/50 of the polarization voltage applied to the piezoelectric ceramics during polarization. A method for manufacturing a piezoelectric ceramic, comprising the step of applying in the opposite direction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3200697A JPH0548173A (en) | 1991-08-09 | 1991-08-09 | Manufacture of piezoelectric material ceramics |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP3200697A JPH0548173A (en) | 1991-08-09 | 1991-08-09 | Manufacture of piezoelectric material ceramics |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0548173A true JPH0548173A (en) | 1993-02-26 |
Family
ID=16428735
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP3200697A Pending JPH0548173A (en) | 1991-08-09 | 1991-08-09 | Manufacture of piezoelectric material ceramics |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0548173A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7712878B2 (en) | 2007-03-29 | 2010-05-11 | Seiko Epson Corporation | Liquid ejecting head and method for manufacturing the same |
| JP2015536580A (en) * | 2012-12-07 | 2015-12-21 | エプコス アクチエンゲゼルシャフトＥｐｃｏｓ Ａｇ | Manufacturing method of electronic parts |
| CN105655479A (en) * | 2015-12-30 | 2016-06-08 | 中国科学院上海硅酸盐研究所 | Polarization aging treatment method for obtaining large strain effect in piezoceramics |
-
1991
- 1991-08-09 JP JP3200697A patent/JPH0548173A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7712878B2 (en) | 2007-03-29 | 2010-05-11 | Seiko Epson Corporation | Liquid ejecting head and method for manufacturing the same |
| JP2015536580A (en) * | 2012-12-07 | 2015-12-21 | エプコス アクチエンゲゼルシャフトＥｐｃｏｓ Ａｇ | Manufacturing method of electronic parts |
| US9755138B2 (en) | 2012-12-07 | 2017-09-05 | Epcos Ag | Method for producing an electronic component |
| CN105655479A (en) * | 2015-12-30 | 2016-06-08 | 中国科学院上海硅酸盐研究所 | Polarization aging treatment method for obtaining large strain effect in piezoceramics |
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