JPH0369175A - Piezoelectric ceramic composition - Google Patents
Piezoelectric ceramic compositionInfo
- Publication number
- JPH0369175A JPH0369175A JP1205373A JP20537389A JPH0369175A JP H0369175 A JPH0369175 A JP H0369175A JP 1205373 A JP1205373 A JP 1205373A JP 20537389 A JP20537389 A JP 20537389A JP H0369175 A JPH0369175 A JP H0369175A
- Authority
- JP
- Japan
- Prior art keywords
- powders
- calcinated
- acquire
- composition
- lanthanoid
- 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
- 239000000203 mixture Substances 0.000 title claims abstract description 19
- 239000000919 ceramic Substances 0.000 title claims abstract description 12
- 229910052747 lanthanoid Inorganic materials 0.000 claims abstract description 5
- 150000002602 lanthanoids Chemical class 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 7
- 229910002902 BiFeO3 Inorganic materials 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 3
- 239000006104 solid solution Substances 0.000 abstract description 3
- 229910003781 PbTiO3 Inorganic materials 0.000 abstract description 2
- 239000011230 binding agent Substances 0.000 abstract description 2
- XMFOQHDPRMAJNU-UHFFFAOYSA-N lead(II,IV) oxide Inorganic materials O1[Pb]O[Pb]11O[Pb]O1 XMFOQHDPRMAJNU-UHFFFAOYSA-N 0.000 abstract description 2
- 239000007858 starting material Substances 0.000 abstract description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 abstract 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- 229910010252 TiO3 Inorganic materials 0.000 abstract 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 abstract 1
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 abstract 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 abstract 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 abstract 1
- MRELNEQAGSRDBK-UHFFFAOYSA-N lanthanum oxide Inorganic materials [O-2].[O-2].[O-2].[La+3].[La+3] MRELNEQAGSRDBK-UHFFFAOYSA-N 0.000 abstract 1
- 239000011656 manganese carbonate Substances 0.000 abstract 1
- 235000006748 manganese carbonate Nutrition 0.000 abstract 1
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 abstract 1
- PLDDOISOJJCEMH-UHFFFAOYSA-N neodymium oxide Inorganic materials [O-2].[O-2].[O-2].[Nd+3].[Nd+3] PLDDOISOJJCEMH-UHFFFAOYSA-N 0.000 abstract 1
- KTUFCUMIWABKDW-UHFFFAOYSA-N oxo(oxolanthaniooxy)lanthanum Chemical compound O=[La]O[La]=O KTUFCUMIWABKDW-UHFFFAOYSA-N 0.000 abstract 1
- 230000008878 coupling Effects 0.000 description 5
- 238000010168 coupling process Methods 0.000 description 5
- 238000005859 coupling reaction Methods 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 4
- 230000007423 decrease Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010304 firing Methods 0.000 description 4
- 238000009413 insulation Methods 0.000 description 4
- NKZSPGSOXYXWQA-UHFFFAOYSA-N dioxido(oxo)titanium;lead(2+) Chemical compound [Pb+2].[O-][Ti]([O-])=O NKZSPGSOXYXWQA-UHFFFAOYSA-N 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 229910052746 lanthanum Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 238000005476 soldering Methods 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 229910052693 Europium Inorganic materials 0.000 description 1
- 229910052688 Gadolinium Inorganic materials 0.000 description 1
- 241000255896 Galleria mellonella Species 0.000 description 1
- 229910052772 Samarium Inorganic materials 0.000 description 1
- 240000005499 Sasa Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material 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）
本発明は圧電性磁器組成物、特に、自動車の７ツキング
センサーなどのように高温下で使用される圧電素子ある
いは高周波用のフィルターや発振素子などのように誘電
率の低いことが要求される高周波用圧電素子の材料とし
て有用な、耐熱性および焼結性に優れた低誘電率の圧電
性磁器組成物に関する。Detailed Description of the Invention (Industrial Field of Application) The present invention relates to piezoelectric ceramic compositions, particularly piezoelectric elements used at high temperatures such as automobile seven-wheel sensors, high frequency filters, and oscillations. The present invention relates to a piezoelectric ceramic composition with a low dielectric constant and excellent heat resistance and sinterability, which is useful as a material for high-frequency piezoelectric elements that require a low dielectric constant, such as devices.
（従来の技術）
従来、自動車の／ツキングセンサーなどのように高温で
使用される圧電素子の材料、あるいは高周波用のフィル
ターや発振子の材料としては、チタン酸鉛系圧電性磁器
組成物が採用されている。(Prior art) Lead titanate-based piezoelectric ceramic compositions have conventionally been used as materials for piezoelectric elements used at high temperatures, such as in automobile/trucking sensors, or as materials for high-frequency filters and oscillators. It has been adopted.
この圧電性磁器組成物は、通常、焼結性を向上させるた
め、Ｐｂの一部をＬａやＣａなどで置換することが行わ
れている。In order to improve the sinterability of this piezoelectric ceramic composition, a portion of Pb is usually replaced with La, Ca, or the like.
（発明が解決しようとする課題）
しかしながら、チタン酸鉛のＰｂの一部をＬａ等で置換
するとキュリー点の低下を招き、使用限界温度が低下す
るという問題がある。このため、サーフェイスマウンテ
ィングする際、フローあるいはりフローハンダ付は工程
での加熱により、特性が劣化し易く、製品の特性が安定
しないという問題があった。しかも、ｐｂの一部をＬａ
やＣａで多量に置換すると、誘電率が増加し低誘電率で
あることが要求される高周波用圧電素子の材料として適
したものを得ることは困難であった。(Problems to be Solved by the Invention) However, there is a problem in that replacing a portion of Pb in lead titanate with La or the like causes a decrease in the Curie point and a decrease in the service limit temperature. For this reason, when surface mounting is performed, the properties of flow soldering tend to deteriorate due to heating during the process, and there is a problem in that the properties of the product are unstable. Moreover, some of the pb is
If a large amount is replaced with Ca or Ca, the dielectric constant increases, making it difficult to obtain a material suitable for high-frequency piezoelectric elements, which are required to have a low dielectric constant.
これを防止するためＰｂの置換量を少なくすると、十分
焼結させるための最適焼成温度範囲が狭くなり、焼成コ
ントロールが非常に困難となる。If the amount of Pb substituted is reduced in order to prevent this, the optimum firing temperature range for sufficient sintering will be narrowed, making firing control extremely difficult.
他方、チタン酸鉛に微量添加物を含有させた磁器も提案
されてはいるが、焼結が困難で、焼成後に放置しておく
と自然崩壊することがあった。On the other hand, porcelain made of lead titanate containing trace additives has been proposed, but it is difficult to sinter and may spontaneously disintegrate if left unattended after firing.
また、ｐｂ’ｒｉｏ、にＢ１Ｆｅ０．を固溶させてキュ
リー点を向上させた複合ペロブスカイト構造の強誘電体
磁器組成物が、例えば、５ｏｖｉｅｔ Ｐｈｙｓ。Also, pb'rio, B1Fe0. An example of a ferroelectric ceramic composition having a composite perovskite structure in which the Curie point is improved by incorporating solid solution is 5oviet Phys.
Ｃｒｙｓｔ、 （Ｅｎｇｌｉｓｈ Ｔｒａｎｓｌ、 ）
、７ （１９６２）６２にて提案されている。しかしな
がら、この系の磁器は絶縁抵抗が低く、圧電性を付与す
る分極処理かできないため実用化することは困難であっ
た。Cryst, (English Transl.)
, 7 (1962) 62. However, this type of porcelain has low insulation resistance and can only be subjected to polarization treatment to impart piezoelectricity, making it difficult to put it into practical use.
従って、本発明は、キュリー点が高く、耐熱性および焼
結性に優れ、低誘電率の圧電性磁器組成物を提供するこ
とを目的とするものである。Therefore, an object of the present invention is to provide a piezoelectric ceramic composition having a high Curie point, excellent heat resistance and sinterability, and a low dielectric constant.
（課題を解決するための手段）
本発明は、前記課題を解決するための手段として、基本
的には、ＰｂＴｉ０＝にＢｉＦｅＯ３を所定量固溶させ
て牛ユリー点を向上させる一方、それに起因する絶縁抵
抗の低下を、Ｍｎを所定量添加することによって防止し
、かつ、焼結性を向上させるようにしたものである。ま
た、Ｐｂをランタノイドで一部置換することにより、機
械的品質係数を向上させるようにしたものである。(Means for Solving the Problems) As a means for solving the above problems, the present invention basically improves the Urie point by dissolving a predetermined amount of BiFeO3 in PbTi0=, and at the same time A decrease in insulation resistance is prevented by adding a predetermined amount of Mn, and sinterability is improved. Furthermore, by partially replacing Pb with lanthanoid, the mechanical quality factor is improved.
即ち、本発明の要旨は、一般式：
％式％
（但し、Ａはランタノイドのうちの少なくとも一種、０
．８≦ａ≦１．２、Ｑ＜ｘ≦０．４．０＜ｙ≦０．２、
Ｑ＜ｚ≦５である。）で表される組成を有する圧電性磁
器組成物にある。That is, the gist of the present invention is the general formula: % formula % (where A is at least one kind of lanthanoid, 0
．． 8≦a≦1.2, Q<x≦0.4.0<y≦0.2,
Q<z≦5. ) is a piezoelectric ceramic composition having a composition represented by:
代表的なランクメイドとしては、Ｌａ、Ｃｅ。Typical rank maids are La and Ce.
Ｐｒ、ＮｄＳＰｍ、Ｓｍ、Ｅｕ、Ｇｄなどが挙げられる
が、これらに限定されるものではない。Examples include, but are not limited to, Pr, NdSPm, Sm, Eu, and Gd.
（作用）
本発明における各成分の組成比を前記のように限定した
理由およびそれらの作用は次の通りである。(Function) The reasons for limiting the composition ratio of each component in the present invention as described above and their effects are as follows.
主成分であるＰ ｂａ Ｔ ＋ ０３に於けるＰｂのモ
ル分率、ａｌが０．８未満あるいは１．２を超えると、
焼結しなくなるので前記範囲とした。なお、ａが０．８
以上〜１未満の範囲では、焼成温度が高いとＴｉが析出
することがあるので、１３００℃未満の温度で焼成する
のが望ましい。When the mole fraction of Pb in the main component P ba T + 03, al is less than 0.8 or exceeds 1.2,
Since sintering does not occur, the above range was set. Note that a is 0.8
In the range from above to less than 1, Ti may precipitate if the firing temperature is high, so it is desirable to fire at a temperature of less than 1300°C.
ランクメイドは機械的品質係数を向上させるためにＰｂ
の一部と置換されるが、そのモル分率、ｙｌが０．２を
超えると、キュリー温度が著しく低下すると共に、破壊
電圧も小さくなるので分極させることができなくなり、
また、比誘電率が小さくならず、電気機械結合係数を大
きくできないので０．２以下とした。Rankmade Pb to improve mechanical quality factor
However, if its molar fraction, yl, exceeds 0.2, the Curie temperature will drop significantly and the breakdown voltage will also become small, making it impossible to polarize.
Further, since the dielectric constant cannot be reduced and the electromechanical coupling coefficient cannot be increased, it is set to 0.2 or less.
ＢｉＦｅＯ３はキュリー点を向上させるために添加され
るが、０．４を超えると、破壊電圧が著しく低下し、電
気機械結合係数も低下するので前記範囲とした。BiFeO3 is added to improve the Curie point, but if it exceeds 0.4, the breakdown voltage will drop significantly and the electromechanical coupling coefficient will also drop, so it was set in the above range.
Ｍｎは主として焼結性および絶縁抵抗を向上させるため
に添加されるが、その添加量、ｚｌが０、ＯＯ１ｍｏ１
％未満では十分な効果が得られず、また、５ｍ０１％を
超えると破壊電圧が低下し圧電特性が得られなくなるの
で前記範囲とした。Mn is added mainly to improve sinterability and insulation resistance, but its addition amount, zl is 0, OO1mol
If it is less than 5m01%, a sufficient effect cannot be obtained, and if it exceeds 5m01%, the breakdown voltage decreases and piezoelectric properties cannot be obtained, so the above range was set.
（実施例）
出発原料としてＰｂ３Ｏ４、Ｔｉｅ、、Ｂ ｚ ｔ Ｏ
ｓ、Ｆｅ＝Ｏｓ、ＭｎＣ０，、Ｌａｔｏ３、Ｎ ｄ ２
０−１ＣｅＯ。(Example) Pb3O4, Tie, BztO as starting materials
s, Fe=Os, MnC0,, Lato3, N d 2
0-1CeO.
およびＰｒ、Ｏを用い、これらの粉末を第ｉ表に示す組
成になるように秤量した。この原料粉末の混合物を湿式
混合した後、７００〜９００℃で２時間仮焼し、粉砕し
て仮焼粉末を得た。この仮焼粉末にバインダーを加えて
湿式混合し、乾燥、造粒した後、２０００ ｋｇ／ ｃ
ｍ’の圧力で円板状に成形し、１０５０〜１２５０°Ｃ
で焼成し、直径１４ｍｍ、厚さ１ｍｍの磁器円板を得た
。These powders were weighed to have the compositions shown in Table i using 1, 2 and 3. This mixture of raw material powders was wet mixed, then calcined at 700 to 900°C for 2 hours and pulverized to obtain calcined powder. After adding a binder to this calcined powder, wet-mixing it, drying it, and granulating it, it weighs 2000 kg/c.
Formed into a disc shape at a pressure of m' and heated at 1050-1250°C.
A porcelain disk with a diameter of 14 mm and a thickness of 1 mm was obtained.
各円板の両面に銀ペーストを塗布し、８００’Ｃで２時
間焼き付けて銀電極を形成した後、シリコンオイル中、
１５０〜２００℃で３〜７ ｋｖ／ ｍｍの直流電圧を
印加して分極し試料を得た。Silver paste was applied to both sides of each disk and baked at 800'C for 2 hours to form silver electrodes.
A sample was obtained by polarization by applying a DC voltage of 3 to 7 kv/mm at 150 to 200°C.
各試料について、比誘電率（ε）、電気機械結合係数（
ｋｔ）、機械的品質係数（Ｑ ｍ）、破壊電圧およびキ
ュリー点を測定した。それらの結果を第１表に示す。第
１表中、＊は本発明の範囲外の組成を有する試料を示し
、それ以外のものは本発明の範囲内のものである。For each sample, the relative dielectric constant (ε), electromechanical coupling coefficient (
kt), mechanical quality factor (Q m), breakdown voltage and Curie point were measured. The results are shown in Table 1. In Table 1, * indicates a sample having a composition outside the scope of the present invention, and the other samples are within the scope of the present invention.
（以 下
余
白）
０ の
の Ｕ）
（％ＪＣ’Ｊ
−（Ｊ） ０−０〜〇−
の００００寸寸トド
ササＮＯ寸寸Ｃ４（Ｎ
Φ の
トω
ササ
Ｏ
Ｏト
０ ０ ０ ０ ０ ０ ０ ０
−＝ （：’Ｊ ｃｏ ＝ ＯＧ’） −＝−−１−−
ＣＮ −’ （Ｎ〜
（）Ｏ
Ｌ１′）ＬＯ
ＣＯ寸 の ′寸 寸 寸 ■ 寸
寸 ■−囚○ＯＯＣ’Ｊ ０００ （Ｎ Ｃ’Ｊ ０
００ＬＯ１１’） Ｅ ＬＯの の−一一〇
〇〇の一一一一一寸マ
つ Ｉ：１ つ つ つ つ つ ０
０ ω Ｏ０ω υＺ Ｚ Ｚ Ｚ
Ｚ ：Ｚ、 Ｚ Ｑ Ｑ Ｑ Ｑ Ｑ
Ｑ ＩＪ＊
蒼＋Ｎ （’Ｑ ４ ＬＯ■トの
Φ０− Ｃ’Ｊ ｃＹ） ＋ ＬＤ−一一一一一一−Ｎ
ＮＮ囚ＮＣ’１
第１表の結果から、ＰｂＴｉＯ３にＢ１Ｆｅ○、を所定
量固溶させた２成分系にＭｎを所定量添加することによ
り絶縁抵抗を大きくして分極処理が可能となると同時に
、焼結性を向上させることができ、キュリー点および電
気機械結合係数が高く、誘電率の低い圧電磁器が得られ
ることが判る。(Margins below) 0 U) (%JC'J - (J) 0-0~〇- 0000 dimension Todosasa NO dimension C4 (N Φ To ω Sasa OOto 0 0 0 0 0 0 0 0 −= (:'J co = OG') −=−−1−−
CN -' (N~ ()O L1') LO CO size ' size size size ■ size size ■-Prison○OOC'J 000 (N C'J 0
00LO11') E LO's -11000 11111 inch I: 1 tsu tsu tsu tsu 0
0 ω O0ω υZ Z Z Z Z
Z :Z, Z Q Q Q Q Q
Q IJ*
Blue+N ('Q 4 LO ■ Φ0- C'J cY) + LD-111111-N
NN Prison NC'1 From the results in Table 1, it is possible to increase the insulation resistance and perform polarization treatment by adding a predetermined amount of Mn to a two-component system in which a predetermined amount of B1Fe○ is dissolved in PbTiO3 as a solid solution. It can be seen that a piezoelectric ceramic having improved sinterability, a high Curie point and a high electromechanical coupling coefficient, and a low dielectric constant can be obtained.
（発明の効果）
以上説明したように、本発明に係る圧電性磁器組成物は
、キュリー点が高く安定した焼結性を有するため、フロ
ー若しくはリフローハンダ付は工程での加熱による劣化
がなく、かつ、自動車のノッキングセンサーなどのよう
に高温の環境下で使用しても特性劣化の少ない圧電素子
が得られる。(Effects of the Invention) As explained above, the piezoelectric ceramic composition according to the present invention has a high Curie point and stable sinterability, so flow or reflow soldering does not deteriorate due to heating in the process. In addition, a piezoelectric element whose characteristics do not deteriorate even when used in a high-temperature environment such as in an automobile knocking sensor can be obtained.
また、誘電率が低く、電気機械結合係数が大きいので高
周波フィルタや発振子などの高周波用材料としても使用
できるなど、優れた効果が得られる。Furthermore, since it has a low dielectric constant and a large electromechanical coupling coefficient, it can be used as a high-frequency material for high-frequency filters, oscillators, and other high-frequency materials, and other excellent effects can be obtained.
Claims (1)
ＴｉＯ＿３］＋ｘＢｉＦｅＯ＿３＋ｚｍｏｌ％Ｍｎ（但
し、Ａはランタノイドのうちの少なくとも一種、０．８
≦ａ≦１．２、０＜ｘ≦０．４、０＜ｙ≦０．２、０＜
ｚ≦５である。）で表される組成を有する圧電性磁器組
成物。(1) General formula: (1-x) [(Pb_a_-_3_y_/_2A_y)
TiO_3]+xBiFeO_3+zmol%Mn (However, A is at least one kind of lanthanoid, 0.8
≦a≦1.2, 0<x≦0.4, 0<y≦0.2, 0<
z≦5. ) A piezoelectric ceramic composition having a composition represented by:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1205373A JPH0369175A (en) | 1989-08-08 | 1989-08-08 | Piezoelectric ceramic composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1205373A JPH0369175A (en) | 1989-08-08 | 1989-08-08 | Piezoelectric ceramic composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0369175A true JPH0369175A (en) | 1991-03-25 |
Family
ID=16505766
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1205373A Pending JPH0369175A (en) | 1989-08-08 | 1989-08-08 | Piezoelectric ceramic composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0369175A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006032872A1 (en) * | 2004-09-22 | 2006-03-30 | Goodrich Control Systems Limited | Piezoelectric materials |
| JP2007261863A (en) * | 2006-03-28 | 2007-10-11 | Kyocera Corp | Piezoelectric ceramic composition and piezoelectric ceramic |
| JP2008050178A (en) * | 2006-08-22 | 2008-03-06 | Konica Minolta Holdings Inc | Production method of piezoelectric ceramic composition |
-
1989
- 1989-08-08 JP JP1205373A patent/JPH0369175A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2006032872A1 (en) * | 2004-09-22 | 2006-03-30 | Goodrich Control Systems Limited | Piezoelectric materials |
| JP2008513331A (en) * | 2004-09-22 | 2008-05-01 | グッドリッチ コントロール システムズ リミティド | Piezoelectric material |
| US7928637B2 (en) | 2004-09-22 | 2011-04-19 | Goodrich Control Systems | Piezoelectric materials |
| KR101369477B1 (en) * | 2004-09-22 | 2014-03-04 | 굿리치 컨트롤 시스템즈 | Piezoelectric materials |
| JP2007261863A (en) * | 2006-03-28 | 2007-10-11 | Kyocera Corp | Piezoelectric ceramic composition and piezoelectric ceramic |
| JP2008050178A (en) * | 2006-08-22 | 2008-03-06 | Konica Minolta Holdings Inc | Production method of piezoelectric ceramic composition |
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