JPS6050359B2 - Method for manufacturing piezoelectric material - Google Patents
Method for manufacturing piezoelectric materialInfo
- Publication number
- JPS6050359B2 JPS6050359B2 JP53159787A JP15978778A JPS6050359B2 JP S6050359 B2 JPS6050359 B2 JP S6050359B2 JP 53159787 A JP53159787 A JP 53159787A JP 15978778 A JP15978778 A JP 15978778A JP S6050359 B2 JPS6050359 B2 JP S6050359B2
- Authority
- JP
- Japan
- Prior art keywords
- sheet
- piezoelectric material
- zirconium oxide
- piezoelectric
- particle size
- 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.)
- Expired
Links
- 239000000463 material Substances 0.000 title claims description 10
- 238000000034 method Methods 0.000 title claims description 7
- 238000004519 manufacturing process Methods 0.000 title claims description 6
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 claims description 12
- 229910001928 zirconium oxide Inorganic materials 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000010304 firing Methods 0.000 claims description 5
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 239000011230 binding agent Substances 0.000 claims description 2
- 239000004014 plasticizer Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 238000009826 distribution Methods 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 230000009257 reactivity Effects 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004332 silver Substances 0.000 description 2
- 229910052709 silver Inorganic materials 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- 241001391944 Commicarpus scandens Species 0.000 description 1
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 description 1
- 229910003781 PbTiO3 Inorganic materials 0.000 description 1
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical compound CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 229910010293 ceramic material Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 238000007606 doctor blade method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004927 fusion Effects 0.000 description 1
- 238000003475 lamination Methods 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 229920006267 polyester film Polymers 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Piezo-Electric Or Mechanical Vibrators, Or Delay Or Filter Circuits (AREA)
Description
【発明の詳細な説明】
本発明は、圧電体材料特に鉛系圧電体材料の製造方法
に関するもので、特に圧電体材料を積層して焼成したと
きにその剥離性がよく平滑な表面をもつた圧電体シート
を得ることを目的とするものてある。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for manufacturing a piezoelectric material, particularly a lead-based piezoelectric material, and particularly to a method for producing a piezoelectric material that has good peelability and a smooth surface when laminated and fired. There is one aimed at obtaining a piezoelectric sheet.
最近、圧電セラミックスの応用分野は多岐にわたり高
密度化、小型化が急速に進んできた。Recently, piezoelectric ceramics have been applied to a wide variety of fields, and their density and size have rapidly increased.
従来用途に応じて、焼結体もしくは単結晶のインゴット
を切断、研摩加工を施して所定形状の圧電素子を得てい
たが、加工歪みによる電気的特性の劣化、さらには加工
費用が高くつくという問題が生じている。そのために、
工程の簡略化および量産化ということから、焼成と同時
に所望形状の素子が安価に供給されることが望ましい。
この方法として、セラミックス素材を結合剤樹脂などと
ともに混練し、成形して一定の生シートを作製し、用途
に応じた所定形状に打ち抜いてから、それに高融点酸化
物を均一に塗布し積層焼成することが知られている。し
かし、積層焼成後の焼結体シート製品において、焼結体
シートと高融点酸化物との融着、焼結体シート同士の遊
着などによる歩留りの低下、さらには、剥離時の焼結体
シート割れ、銀電極のにじみ、組み立て後の電気的特性
に大きな影響を及ぼすことなどの問題点があつた。 本
発明は、このような問題点を除去した圧電体材料の製造
方法を提供するものである。すなわち、圧電体材料を積
層して焼成したときに、平滑でかつ剥離性がよくかつ安
定している圧電焼結体シートを得るために、あらかじめ
酸化ジルコニウムを1000〜1600℃の範囲で熱処
理し、その粒径を28〜140μmの粒度分布とするも
のである。 一般に酸化ジルコニウムの市販品は、セラ
ミックスなどのような一組成物として使用されることが
多いため、反応性に富んだ材料である。このため焼成時
に焼結体シートに融着する。そこで、酸化ジルコニウム
をあらかじめできるだけ高い温度で熱処理して反応性を
下げるのがよい。処理温度が1000℃より低いときに
は反応性がまだ残されているため、圧電シートと酸化ジ
ルコニウムが融着する。また、16000Cより高くな
ると酸化ジルコニウム粒子が互に反応し、粒子径が大き
くなり過ぎて剥離性が悪くなる。このようなことから、
熱処理温度は1000〜1600′Cの範囲であること
が適当である。次に、熱処理された酸化ジルコニウム粒
子径であるが、粒子径が140pmよりも大きくなると
生シートと酸化ジルコニウムとの接触面積が小さくなつ
て付着しにくくなり、28μmよりも小さい粒子径では
、逆に接触面積が大きくなり、焼成後剥離しにくくなり
、焼結体シートをはがすときに割れやすく、また剥離す
ることができても平滑性の悪焼結体シートになるので、
28〜140μmの粒度分布の範囲が適当である。この
ように選別された酸化ジルコニウム粉体を、任意に打ち
抜かれた圧電体シートの表面に、加熱振動を与えて付着
させ、積み重ねて焼成すれば、平滑でかつ剥離性の安定
した圧電焼結体シートを得ることができる。次に、本発
明の効果を明らかにするため、実施例て説明する。Conventionally, piezoelectric elements in a predetermined shape were obtained by cutting and polishing a sintered or single-crystal ingot depending on the application, but this resulted in deterioration of electrical characteristics due to processing distortion and increased processing costs. A problem has arisen. for that,
From the standpoint of process simplification and mass production, it is desirable to be able to supply elements in desired shapes at low cost simultaneously with firing.
In this method, a ceramic material is kneaded with a binder resin, etc., molded to produce a certain green sheet, punched into a predetermined shape according to the application, and then a high melting point oxide is uniformly applied to it and laminated and fired. It is known. However, in sintered sheet products after lamination firing, the yield decreases due to fusion between the sintered sheet and the high melting point oxide, adhesion between the sintered sheets, etc. Problems included sheet cracking, bleeding of silver electrodes, and a significant impact on electrical characteristics after assembly. The present invention provides a method for manufacturing a piezoelectric material that eliminates such problems. That is, in order to obtain a piezoelectric sintered sheet that is smooth, has good releasability, and is stable when piezoelectric materials are laminated and fired, zirconium oxide is heat-treated in the range of 1000 to 1600°C in advance. The particle size distribution is 28 to 140 μm. Generally, commercially available zirconium oxide products are often used as a single composition such as ceramics, and therefore are highly reactive materials. Therefore, it is fused to the sintered body sheet during firing. Therefore, it is preferable to heat-treat zirconium oxide in advance at as high a temperature as possible to lower its reactivity. When the treatment temperature is lower than 1000°C, reactivity remains, so the piezoelectric sheet and zirconium oxide are fused together. Moreover, when the temperature is higher than 16000C, the zirconium oxide particles react with each other, and the particle size becomes too large, resulting in poor releasability. From such a thing,
The heat treatment temperature is suitably in the range of 1000 to 1600'C. Next, regarding the particle size of the heat-treated zirconium oxide, when the particle size is larger than 140 pm, the contact area between the green sheet and zirconium oxide becomes smaller and it becomes difficult to adhere to the raw sheet. The contact area becomes large, making it difficult to peel off after firing, making it easy to break when peeling off the sintered sheet, and even if it can be peeled off, the sintered sheet will have poor smoothness.
A particle size distribution range of 28 to 140 μm is suitable. The zirconium oxide powder selected in this way is attached to the surface of a randomly punched piezoelectric sheet by applying heating vibrations, stacked and fired, resulting in a piezoelectric sintered body that is smooth and has stable peelability. You can get a seat. Next, in order to clarify the effects of the present invention, examples will be explained.
〔実施例1〕
粒子径0.5μmでPbTiO3:PbTrZ3:Pb
(Mgll3Nb2ノ3)03=37.5:25.0:
37.5の組成比をもつPb(Mg,Nb,Tj,Zr
)03系の仮焼原料に1.5重量%のポリビニールブチ
ラル樹脂および0.5重量%のフタル酸ジブチルと0.
5重量%のフタル酸ジオクチルを各々加え、仮焼原料に
対して銀重量%のメチルアルコールと5重量%のブチル
アルコールをさらに加え、ボールミルで川時間混合して
スラリーを作製した。[Example 1] PbTiO3:PbTrZ3:Pb with a particle size of 0.5 μm
(Mgll3Nb2ノ3)03=37.5:25.0:
Pb (Mg, Nb, Tj, Zr) with a composition ratio of 37.5
) 03 series calcined raw material, 1.5% by weight of polyvinyl butyral resin, 0.5% by weight of dibutyl phthalate and 0.03% by weight of polyvinyl butyral resin.
Dioctyl phthalate was added in an amount of 5% by weight, and methyl alcohol in an amount of % by weight of silver and butyl alcohol in an amount of 5% by weight were further added to the calcined raw materials, and mixed in a ball mill for an hour to prepare a slurry.
このスラリーをポリエステルフィルム上に流し、ドクタ
ーブレード法で、シート状に成形してから40′Cで強
制乾燥させて、生シートを作製した。次に、打抜き機を
用いて直径3−の円板状に打抜いた。振動機構を有する
部品供給装置(以下、パーツフィダーと称する)内に、
下表に示す粒子径と熱処理温度を変えた酸化ジルコニウ
ムを60℃に加熱し、5分間流動させ、生シート表面に
付着させた。そして、それを8段に積層してから、13
00゜Cで焼成した。得られた圧電焼結体シートの剥離
性と平滑性を、下表に示す。このように1000〜16
00℃中で熱処理し、粒子径28〜1401J,mの粒
度分布をもつ酸化ジルコニウムにり、積層焼成しても、
平滑性に優れ、かつ安定して剥離をすることができる焼
結体シートを得ることができた。This slurry was poured onto a polyester film, formed into a sheet by a doctor blade method, and then force-dried at 40'C to produce a green sheet. Next, it was punched out into a disk shape with a diameter of 3 mm using a punching machine. Inside the parts feeder (hereinafter referred to as parts feeder) that has a vibration mechanism,
Zirconium oxides having different particle sizes and heat treatment temperatures shown in the table below were heated to 60° C., allowed to flow for 5 minutes, and adhered to the surface of the raw sheet. Then, after stacking it in 8 layers, 13
It was fired at 00°C. The peelability and smoothness of the obtained piezoelectric sintered sheet are shown in the table below. 1000-16 like this
Even if heat treated at 00℃ and laminated with zirconium oxide with a particle size distribution of 28 to 1401 J, m,
It was possible to obtain a sintered sheet that has excellent smoothness and can be peeled off stably.
以上説明したように、本発明の方法は、酸化ジルコニウ
ムをあらかじめ熱処理して、その反応性を低下せしめ、
さらに、その粒度分布を限定することによつて、剥離お
よび特性の優れた圧電体材ノ料を製造することができる
。As explained above, the method of the present invention heat-treats zirconium oxide in advance to reduce its reactivity,
Furthermore, by limiting the particle size distribution, it is possible to produce a piezoelectric material with excellent release properties and properties.
Claims (1)
媒を加えて混練し、この混練物を一定の厚みに延展して
生シートを作り、それを所定の形状に打ち抜いた後、1
000〜1600℃で熱処理した28〜140μmの粒
径を有する酸化ジルコニウムを、生シート表面に付着さ
せ、この生シートを複数枚積み合ねて焼成することを特
徴とする圧電体材料の製造方法。1 Add a binder resin, a plasticizer, and a solvent to a piezoelectric material containing lead, knead it, spread the kneaded product to a certain thickness to make a green sheet, and punch it into a predetermined shape.
A method for manufacturing a piezoelectric material, which comprises: adhering zirconium oxide having a particle size of 28 to 140 μm heat-treated at 000 to 1600° C. to the surface of a raw sheet, stacking a plurality of the raw sheets and firing the raw sheets.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP53159787A JPS6050359B2 (en) | 1978-12-22 | 1978-12-22 | Method for manufacturing piezoelectric material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP53159787A JPS6050359B2 (en) | 1978-12-22 | 1978-12-22 | Method for manufacturing piezoelectric material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5586176A JPS5586176A (en) | 1980-06-28 |
| JPS6050359B2 true JPS6050359B2 (en) | 1985-11-08 |
Family
ID=15701252
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP53159787A Expired JPS6050359B2 (en) | 1978-12-22 | 1978-12-22 | Method for manufacturing piezoelectric material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS6050359B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63136677A (en) * | 1986-11-28 | 1988-06-08 | Fuji Electric Co Ltd | Manufacture of piezoelectric ceramics thin plate |
-
1978
- 1978-12-22 JP JP53159787A patent/JPS6050359B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5586176A (en) | 1980-06-28 |
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