JP2004155601A - Piezoelectric ceramic composition - Google Patents
Piezoelectric ceramic composition Download PDFInfo
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- JP2004155601A JP2004155601A JP2002320796A JP2002320796A JP2004155601A JP 2004155601 A JP2004155601 A JP 2004155601A JP 2002320796 A JP2002320796 A JP 2002320796A JP 2002320796 A JP2002320796 A JP 2002320796A JP 2004155601 A JP2004155601 A JP 2004155601A
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- piezoelectric ceramic
- ceramic composition
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- oxide
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- 239000000919 ceramic Substances 0.000 title claims abstract description 19
- 239000000203 mixture Substances 0.000 title claims abstract description 19
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 10
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 8
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 8
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 8
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 8
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 8
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 abstract description 8
- 230000000996 additive effect Effects 0.000 abstract description 6
- 230000008878 coupling Effects 0.000 description 8
- 238000010168 coupling process Methods 0.000 description 8
- 238000005859 coupling reaction Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 229910000464 lead oxide Inorganic materials 0.000 description 4
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- 229910052758 niobium Inorganic materials 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- -1 Li 2 CO 3 Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009774 resonance method Methods 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 229910052715 tantalum Inorganic materials 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000012856 weighed raw material Substances 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
Abstract
Description
【0001】
【発明の属する技術分野】
本発明は、センサー、アクチュエーター、フィルター等に使用される圧電素子用の圧電磁器組成物に関する。
【0002】
【従来の技術】
従来、圧電素子材料として、大きな圧電特性を示すPZT(PbTiO3−PbZrO3)系セラミックス、PMN(Pb(Mg,Nb)O3)系セラミックスなど鉛系ペロブスカイト組成物が主に用いられてきた。
【0003】
更にPZT、PMN系セラミックスは、組成の選択、様々な副成分、或いは添加物を選択することにより、センサー、アクチュエーター、フィルター等、各用途別の様々な要求に対応した特性を操作できるという特長を有している。
【0004】
【発明が解決しようとする課題】
しかし、これらの材料は、酸化鉛として60重量%以上と多量に鉛を含んでいる。酸化鉛は人体に有害であり、多量摂取は中毒を引き起こす危険性がある。また、酸化鉛は低温でも揮発性が強く、仮焼、本焼成等の製造過程で大気中に飛散してしまう。製造段階の鉛は回収することも可能であるが、市場に出された圧電製品に含有される酸化鉛については現状では回収が難しく産業廃棄物等から環境中に鉛成分が溶出することも考えられ、圧電応用分野の広がりと共に鉛成分の拡散が懸念される。従って、鉛原料を使用しない圧電磁器組成物を提供することは、環境保護の観点から、極めて重要な課題となる。
【0005】
即ち、本発明の課題は、鉛成分を含有しない安価な材料で、優れた圧電特性を有する圧電磁器組成物を提供することである。
【0006】
【課題を解決するための手段】
(Li1−x−yNaxKy)(Nb1−zSbz)O3+additiveと表わしたとき、0≦x≦0.8、0.2≦y≦1、x+y≧0.7、0≦z≦0.35の範囲であり、Ca、Sr、Zn、Cu、Ba、Mn、Mg、Cr、Fe、Co、Niのうち少なくとも1種類以上を酸化物換算で0.01〜3重量%含有することを特徴とする圧電磁器組成物を提供することにより、一般的に使用可能とされる電気機械結合係数(円板径方向振動)20%以上を達成することができる。
【0007】
【発明の実施の形態】
本発明は、(Li1−x−yNaxKy)(Nb1−zSbz)O3+additiveと表わしたとき、0≦x≦0.8、0.2≦y≦1、x+y≧0.7、0≦z≦0.35の範囲であることが必要であり、Ca、Sr、Zn、Cu、Ba、Mn、Mg、Cr、Fe、Co、Niのうち少なくとも1種種類以上を酸化物換算で0.01〜3重量%含有することを特徴とする。
【0008】
即ち、(Li1−x−yNaxKy)(Nb1−zSbz)O3と表わしたとき、0≦x≦0.8、0.2≦y≦1、x+y≧0.7、0≦z≦0.35の範囲である組成物に、Ca、Sr、Zn、Cu、Ba、Mn、Mg、Cr、Fe、Co、Niのうち少なくとも1種類以上を酸化物換算で0.01〜3重量%含有させることにより焼成密度を向上させ、電気機械結合係数(円板径方向振動)20%以上の圧電磁器を得ることができる。
【0009】
ここで、0≦x≦0.8、0.2≦y≦1、x+y≧0.7、0≦z≦0.35の範囲と限定したのは、Liが過剰に含有された場合、良好な焼結体が得られず、又それ以外の範囲では良好な特性が得られないからである。更にCa、Sr、Zn、Cu、Ba、Mn、Mg、Cr、Fe、Co、Niのうち少なくとも1種類以上を酸化物換算で0.01〜3重量%含有させるとしたのは、0.01重量%以下では効果が薄く、又3重量%以上では電気機械結合係数(円板径方向振動)の特性悪化が著しいからである。
【0010】
【実施例】
本発明の実施例を下述する。まず、出発原料としてLi2CO3、Na2CO3、K2CO3、Nb2O5、Sb2O3粉末を所定量秤量し、更にMnO2等、所望の添加物を秤量した。その際、モル比及び添加物量を表1に示す値になるように変化させた。尚、出発原料は上述されたものに限らず、熱処理後、酸化物になるものであれば良い。また添加物は、仮焼後に添加しても同様の効果が得られる。更に原料粉末不純物、工程混入不純物等として、Ca 、Si、Al、Ta、Zr、Fe等が混入する場合がある。
【0011】
次に、秤量した原料粉末は、ボールミルを使用し、有機溶媒中で1〜10時間混合した。
【0012】
乾燥後、700〜900℃で1〜10時間保持し、仮焼した。
【0013】
そして、再びボールミルを使用し、有機溶媒中で5〜24時間混合・粉砕した。
【0014】
再び乾燥した粉末に、バインダーとしてポリビニルアルコールを加えて造粒し、圧力2〜10ton/cm2で、直径12mm、厚さ1.5mmの円板にプレス成形した。
【0015】
そして、この成形試料を800〜1300℃で1〜10時間保持し、本焼成した。
【0016】
この焼結体を厚さ0.4mmまで研磨した後、その両面に銀ペーストを600〜900℃で焼き付け、電極を形成した。その後、40〜100℃のシリコンオイル中で3〜10kV/mmの直流電界を10〜40分印加して分極処理を行なった。これにより、表1の試料を得た。
【0017】
得られた試料について、インピーダンスアナライザーを用い、共振反共振法に基づき、電気機械結合係数(円板径方向振動)を測定した。又、誘電率はLCRメーターを用い、測定を行なった。
【0018】
その結果を表1に示す。
【0019】
【表1】
【0020】
表1の試料番号2〜4より、電気機械結合係数(円板径方向振動)の観点から、添加物の添加量には最適な量があることが分かる。又、試料1、2、9、15、20、21からLi、Na、Kの最適量が、そして、試料番号2、3、14、15、16、17、18からNb、Sbの最適量が分かる。
【0021】
つまり表1から、(Li1−x−yNaxKy)(Nb1−zSbz)O3と表わしたとき、0≦x≦0.8、0.2≦y≦1、x+y≧0.7、0≦z≦0.35の範囲である組成物に、Ca、Sr、Zn、Cu、Ba、Mn、Mg、Cr、Fe、Co、Niのうち少なくとも1種類を酸化物換算で0.01〜3重量%含有させることにより、電気機械結合係数(円板径方向振動)20%以上の圧電磁器を得ることができると分かる。又、電気機械結合係数(円板径方向振動)に注目すると、試料番号3、7、10の条件が好ましい。
【0022】
【発明の効果】
上述のように、本発明において、(Li1−x−yNaxKy)(Nb1−zSbz)O3と表わしたとき、0≦x≦0.8、0.2≦y≦1、x+y≧0.7、0≦z≦0.35の範囲である組成物に、Ca、Sr、Zn、Cu、Ba、Mn、Mg、Cr、Fe、Co、Niのうち少なくとも1種類を酸化物換算で0.01〜3重量%含有させることにより、電気機械結合係数(円板径方向振動)20%以上の圧電磁器を得ることができる。よって、従来、圧電素子材料として使用されてきたPZT(PbTiO3−PbZrO3)系セラミックス、PMN(Pb(Mg,Nb)O3)系セラミックスなど鉛系ペロブスカイト組成物に変わり、センサー、アクチュエーター、フィルター等に使用される圧電素子を提供できる。つまり、本発明の圧電磁器組成物は、過剰摂取すると人体に有害な鉛を一切使用してない為、鉛系ペロブスカイト組成物と違い、大気中への揮発・拡散、及び廃棄物等からの溶出など鉛成分の広がりに関する心配はない。このことは、人々の健康及び環境保護の観点から、極めて重要な効果をもたらすと期待できる。[0001]
TECHNICAL FIELD OF THE INVENTION
The present invention relates to a piezoelectric ceramic composition for a piezoelectric element used for a sensor, an actuator, a filter, and the like.
[0002]
[Prior art]
Conventionally, as a piezoelectric element material, large show piezoelectric properties PZT (PbTiO 3 -PbZrO 3) ceramics, PMN (Pb (Mg, Nb ) O 3) based ceramics such as lead-based perovskite composition has been mainly used.
[0003]
Furthermore, PZT and PMN-based ceramics have the feature that by selecting the composition, various subcomponents, or additives, it is possible to operate the characteristics corresponding to various requirements for each application such as sensors, actuators, filters, etc. Have.
[0004]
[Problems to be solved by the invention]
However, these materials contain a large amount of lead of 60% by weight or more as lead oxide. Lead oxide is harmful to the human body and high doses can cause poisoning. Further, lead oxide has a high volatility even at a low temperature, and is scattered in the air during a manufacturing process such as calcination or main calcination. Although it is possible to recover lead in the production stage, it is difficult to recover lead oxide contained in piezoelectric products put on the market at present, and it is considered that lead components may be eluted from the industrial waste into the environment. Therefore, there is a concern that lead components may be diffused with the spread of piezoelectric application fields. Therefore, providing a piezoelectric ceramic composition that does not use a lead material is a very important issue from the viewpoint of environmental protection.
[0005]
That is, an object of the present invention is to provide a piezoelectric ceramic composition having excellent piezoelectric characteristics with an inexpensive material containing no lead component.
[0006]
[Means for Solving the Problems]
(Li 1-x-y Na x K y) (Nb 1-z Sb z) when expressed as O 3 + additive, 0 ≦ x ≦ 0.8,0.2 ≦ y ≦ 1, x + y ≧ 0.7, 0 ≦ z ≦ 0.35, and at least one of Ca, Sr, Zn, Cu, Ba, Mn, Mg, Cr, Fe, Co, and Ni is 0.01 to 3 wt. By providing a piezoelectric ceramic composition characterized by containing 0.1%, it is possible to achieve an electromechanical coupling coefficient (disc radial vibration) of 20% or more, which can be generally used.
[0007]
BEST MODE FOR CARRYING OUT THE INVENTION
The present invention, (Li 1-x-y Na x K y) (Nb 1-z Sb z) when expressed as O 3 + additive, 0 ≦ x ≦ 0.8,0.2 ≦ y ≦ 1, x + y ≧ 0.7, 0 ≦ z ≦ 0.35, and at least one of Ca, Sr, Zn, Cu, Ba, Mn, Mg, Cr, Fe, Co, and Ni It is characterized by containing 0.01 to 3% by weight in terms of oxide.
[0008]
That is, when expressed as (Li 1-x-y Na x K y) (Nb 1-z Sb z) O 3, 0 ≦ x ≦ 0.8,0.2 ≦ y ≦ 1, x + y ≧ 0.7 , 0 ≦ z ≦ 0.35, at least one of Ca, Sr, Zn, Cu, Ba, Mn, Mg, Cr, Fe, Co, and Ni in terms of oxide. By containing 0.1 to 3% by weight, the firing density can be improved and a piezoelectric ceramic having an electromechanical coupling coefficient (disc radial vibration) of 20% or more can be obtained.
[0009]
Here, the range of 0 ≦ x ≦ 0.8, 0.2 ≦ y ≦ 1, x + y ≧ 0.7, and 0 ≦ z ≦ 0.35 is limited to the case where Li is excessively contained. This is because a good sintered body cannot be obtained, and good characteristics cannot be obtained in other ranges. Further, 0.01 to 3% by weight of at least one of Ca, Sr, Zn, Cu, Ba, Mn, Mg, Cr, Fe, Co, and Ni in terms of oxide is 0.01% by weight. If the amount is less than 3% by weight, the effect is small, and if the amount is more than 3% by weight, the characteristics of the electromechanical coupling coefficient (disc radial vibration) are significantly deteriorated.
[0010]
【Example】
Embodiments of the present invention will be described below. First, as starting materials, Li 2 CO 3 , Na 2 CO 3 , K 2 CO 3 , Nb 2 O 5 , and Sb 2 O 3 powders were weighed in predetermined amounts, and desired additives such as MnO 2 were weighed. At that time, the molar ratio and the amount of the additive were changed so as to have the values shown in Table 1. The starting materials are not limited to those described above, and may be any as long as they become oxides after heat treatment. The same effect can be obtained by adding the additive after calcination. Further, Ca 2, Si, Al, Ta, Zr, Fe, and the like may be mixed as raw material powder impurities and process mixing impurities.
[0011]
Next, the weighed raw material powder was mixed in an organic solvent for 1 to 10 hours using a ball mill.
[0012]
After drying, it was kept at 700 to 900 ° C. for 1 to 10 hours and calcined.
[0013]
Then, using a ball mill again, the mixture was mixed and pulverized in an organic solvent for 5 to 24 hours.
[0014]
The dried powder was again granulated by adding polyvinyl alcohol as a binder, and pressed into a disc having a diameter of 12 mm and a thickness of 1.5 mm at a pressure of 2 to 10 ton / cm 2.
[0015]
Then, the molded sample was held at 800 to 1300 ° C. for 1 to 10 hours, and was fired.
[0016]
After this sintered body was polished to a thickness of 0.4 mm, silver paste was baked on both surfaces thereof at 600 to 900 ° C. to form electrodes. Thereafter, a polarization treatment was performed by applying a DC electric field of 3 to 10 kV / mm in silicon oil at 40 to 100 ° C. for 10 to 40 minutes. Thereby, the sample of Table 1 was obtained.
[0017]
With respect to the obtained sample, an electromechanical coupling coefficient (disc radial vibration) was measured based on a resonance anti-resonance method using an impedance analyzer. The dielectric constant was measured using an LCR meter.
[0018]
Table 1 shows the results.
[0019]
[Table 1]
[0020]
From the sample numbers 2 to 4 in Table 1, it can be seen that there is an optimum amount of the additive from the viewpoint of the electromechanical coupling coefficient (disc radial vibration). Further, the optimal amounts of Li, Na, and K are obtained from Samples 1, 2, 9, 15, 20, and 21, and the optimal amounts of Nb and Sb are obtained from Samples 2, 3, 14, 15, 16, 17, and 18. I understand.
[0021]
That from Table 1, when expressed as (Li 1-x-y Na x K y) (Nb 1-z Sb z) O 3, 0 ≦ x ≦ 0.8,0.2 ≦ y ≦ 1, x + y ≧ In a composition in the range of 0.7, 0 ≦ z ≦ 0.35, at least one of Ca, Sr, Zn, Cu, Ba, Mn, Mg, Cr, Fe, Co, and Ni is converted to oxide. It can be seen that by containing 0.01 to 3% by weight, a piezoelectric ceramic having an electromechanical coupling coefficient (disc radial vibration) of 20% or more can be obtained. When attention is paid to the electromechanical coupling coefficient (disc radial vibration), the conditions of sample numbers 3, 7, and 10 are preferable.
[0022]
【The invention's effect】
As described above, in the present invention, when expressed as (Li 1-x-y Na x K y) (Nb 1-z Sb z) O 3, 0 ≦ x ≦ 0.8,0.2 ≦ y ≦ 1, x + y ≧ 0.7, 0 ≦ z ≦ 0.35, at least one of Ca, Sr, Zn, Cu, Ba, Mn, Mg, Cr, Fe, Co and Ni By containing 0.01 to 3% by weight in terms of oxide, a piezoelectric ceramic having an electromechanical coupling coefficient (disc radial vibration) of 20% or more can be obtained. Therefore, instead of lead-based perovskite compositions such as PZT (PbTiO 3 -PbZrO 3 ) -based ceramics and PMN (Pb (Mg, Nb) O 3 ) -based ceramics conventionally used as piezoelectric element materials, sensors, actuators, filters And the like. In other words, the piezoelectric ceramic composition of the present invention does not use any lead that is harmful to the human body when ingested excessively.Therefore, unlike the lead-based perovskite composition, the piezoelectric ceramic composition volatilizes and diffuses into the atmosphere and elutes from wastes. There is no concern about the spread of lead components. This can be expected to have extremely important effects from the viewpoint of human health and environmental protection.
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