JPH0256287B2 - - Google Patents
Info
- Publication number
- JPH0256287B2 JPH0256287B2 JP60073975A JP7397585A JPH0256287B2 JP H0256287 B2 JPH0256287 B2 JP H0256287B2 JP 60073975 A JP60073975 A JP 60073975A JP 7397585 A JP7397585 A JP 7397585A JP H0256287 B2 JPH0256287 B2 JP H0256287B2
- Authority
- JP
- Japan
- Prior art keywords
- perovskite
- powder
- compound
- titanate
- molar ratio
- 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 - Lifetime
Links
- 229910052573 porcelain Inorganic materials 0.000 claims description 16
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
- 238000000975 co-precipitation Methods 0.000 claims description 10
- 239000000203 mixture Substances 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 7
- -1 zircon compound Chemical class 0.000 claims description 7
- 150000003609 titanium compounds Chemical class 0.000 claims description 6
- 229910052845 zircon Inorganic materials 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 229910044991 metal oxide Inorganic materials 0.000 claims description 5
- 150000004706 metal oxides Chemical class 0.000 claims description 5
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims description 4
- 239000000243 solution Substances 0.000 claims description 4
- 229910052726 zirconium Inorganic materials 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000006104 solid solution Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 1
- 238000000034 method Methods 0.000 description 6
- 239000010936 titanium Substances 0.000 description 6
- 238000010304 firing Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 150000001342 alkaline earth metals Chemical class 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 229910052788 barium Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000008602 contraction Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000003989 dielectric material Substances 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 1
- 229910000464 lead oxide Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 1
- 229910052721 tungsten Inorganic materials 0.000 description 1
- 239000010937 tungsten Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Oxide Ceramics (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Description
【発明の詳細な説明】
＜産業上の利用分野＞
本発明は、チタン酸ジルコン酸系ペロブスカイ
ト型磁器粉末の製造方法に関する。DETAILED DESCRIPTION OF THE INVENTION <Industrial Field of Application> The present invention relates to a method for producing a zirconate titanate perovskite type porcelain powder.
ここでチタン酸ジルコン酸系ペロブスカイト型
磁器とは、チタン酸ジルコン酸やPbや、Ca、
Sr、Ba等のアルカリ土類金属を反応させ、ある
いはこれにタングステン等の金属の酸化物を一種
以上添加または置換の手段により変成し、または
さらに他のペロブスカイト型酸化物を固溶させて
なるものであり、例えばPb（Zr・Ti）O3、Pb
（Nb2/3・Ni1/3）O3−PbTiO3−PbZrO3、Pb
（W1/2・Ni1/2）O3−PbTiO3−PbZrO3、（Pb・
La）（Zr・Ti）O3等がある。 Here, zirconate titanate perovskite type porcelain refers to zirconate titanate, Pb, Ca,
A product made by reacting an alkaline earth metal such as Sr or Ba, or by modifying it by adding or replacing one or more oxides of a metal such as tungsten, or by dissolving another perovskite type oxide as a solid solution. For example, Pb(Zr・Ti)O 3 , Pb
(Nb 2/3・Ni 1/3 )O 3 −PbTiO 3 −PbZrO 3 , Pb
(W 1/2・Ni 1/2 )O 3 −PbTiO 3 −PbZrO 3 , (Pb・
La) (Zr・Ti)O 3 , etc.
＜従来技術＞
かかるチタン酸ジルコン酸系ペロブスカイト型
磁器は周知のように優れた圧電特性と高い誘電率
を有するため、超音波振動子を初めとする圧電応
用製品や電歪材料、誘電体材料として広く利用さ
れている。<Prior art> As is well known, this titanate zirconate perovskite type porcelain has excellent piezoelectric properties and a high dielectric constant, so it is used as piezoelectric applied products such as ultrasonic vibrators, electrostrictive materials, and dielectric materials. Widely used.
このチタン酸ジルコン酸系ペロブスカイト型磁
器の製造方法には共沈法がある。かかる共沈法
は、粒子径が２〜8μと小さく、粒度分布も一様
に揃うために、緻密かつ均質な磁器を得ることが
できる利点があることが知られている。 There is a coprecipitation method as a method for manufacturing this zirconate titanate perovskite type porcelain. It is known that this coprecipitation method has the advantage of being able to obtain dense and homogeneous porcelain because the particle size is as small as 2 to 8 microns and the particle size distribution is uniform.
＜発明が解決しようとする問題点＞
ところで、従来の共沈法は、チタン化合物と、
ジルコン化合物及びその余の金属酸化物を所定の
分量で混合してなる水溶液を造り、その水溶液に
沈澱形成液を加えて共沈させ、これを乾燥した後
に、焼成して製造するものであつた。このため、
この方法にあつては、夫々の化合物の溶解度の相
違から、ある成分は100％沈澱しても他の成分は
沈澱を終了していないことがあり、従つて共沈さ
せるための条件の設定が面倒で、かつ所望の組成
を得ることが困難であつた。<Problems to be solved by the invention> By the way, in the conventional coprecipitation method, a titanium compound and
It was manufactured by mixing a zircon compound and other metal oxides in predetermined amounts to create an aqueous solution, adding a precipitate-forming solution to the aqueous solution to cause coprecipitation, drying this, and then firing it. . For this reason,
In this method, due to the difference in solubility of each compound, even if one component is 100% precipitated, other components may not be completely precipitated, so it is difficult to set the conditions for coprecipitation. This was troublesome and difficult to obtain the desired composition.
本発明は、かかる従来方法の欠点のない共沈法
によるチタン酸ジルコン酸系ペロブスカイト型磁
器粉末の製造方法の提供を目的とするものであ
る。 The object of the present invention is to provide a method for producing zirconate titanate perovskite type porcelain powder by a coprecipitation method that does not have the drawbacks of the conventional methods.
＜問題点を解決するための手段＞
本発明は、チタン酸ジルコン酸系ペロブスカイ
ト型磁器粉末を、次の二工程により製造するよう
にしたものである。<Means for Solving the Problems> In the present invention, zirconate titanate-based perovskite-type porcelain powder is manufactured by the following two steps.
第一工程
チタン化合物とジルコン化合物を、所定のモル
比で混合した水溶液に、沈澱形成液を加えて共沈
させ、これを乾燥、培焼し、必要に応じて粉砕し
てチタン酸ジルコニウム粉末を作る。First step: A precipitate-forming solution is added to an aqueous solution of a titanium compound and a zircon compound mixed at a predetermined molar ratio to co-precipitate the mixture, which is then dried, calcined, and crushed as necessary to produce zirconium titanate powder. make.
第二工程
前記第一工程により形成した組成粉末に、その
余の金属酸化物を所定のモル比で混合して仮焼す
る。Second Step The remaining metal oxide is mixed with the powder composition formed in the first step at a predetermined molar ratio and calcined.
＜作用＞
チタン化合物と、ジルコン化合物の二種の共沈
は容易になし得る。<Function> Co-precipitation of the titanium compound and the zircon compound can be easily performed.
そこで第一工程として、前記チタン化合物と、
ジルコン化合物の共沈物を作つて、これを乾燥及
び培焼してチタン酸ジルコニウム（Ti・Zr）O2
を形成し、これに第二工程として酸化鉛等のその
余の金属酸化物を混合して仮焼することにより形
成する。 Therefore, as a first step, the titanium compound and
A coprecipitate of zircon compound is made, and this is dried and calcined to produce zirconium titanate (Ti・Zr)O 2
In the second step, other metal oxides such as lead oxide are mixed therewith and calcined.
＜実施例＞
Pb（Zrx・Ti1-x）O3の組成からなるチタン酸ジ
ルコン酸系ペロブスカイト型磁器粉末の具体的な
製造法を説明する。<Example> A specific method for producing a zirconate titanate perovskite type porcelain powder having a composition of Pb(Zr x Ti 1-x ) O 3 will be described.
まず試料として、ZrOClとTiOClとモル比で
ｘ：１−ｘ＝55：45の割合で混合した水溶液を沈
澱形成液であるアンモニア水中に加えて共沈さ
せ、この共沈ゾルを塩素イオンが完全に離脱する
まで蒸留水でよく水洗し、120℃で乾燥した後、
850℃で培焼して、（Zrx・Ti1-x）O2を形成し、こ
れをボールミルで粉砕した。 First, as a sample, an aqueous solution of ZrOCl and TiOCl mixed at a molar ratio of x:1-x=55:45 was added to aqueous ammonia as a precipitate forming solution to cause coprecipitation, and this coprecipitated sol was completely free of chloride ions. After washing thoroughly with distilled water until it separates and drying at 120℃,
It was calcined at 850°C to form (Zr x ·Ti 1-x )O 2 , which was ground in a ball mill.
次に、純度99.5％以上のPbOをPb（Zrx・Ti1-x）
O3の組成となるように配合し、600〜900℃で予
備焼成し、これをボールミルで粉砕して前記組成
からなるチタン酸ジルコン酸系ペロブスカイト型
磁器粉末を得た。 Next, PbO with a purity of 99.5% or more is converted into Pb(Zr x Ti 1-x )
The powder was blended to have a composition of O 3 , pre-fired at 600 to 900°C, and ground in a ball mill to obtain titanate zirconate perovskite type porcelain powder having the above composition.
前記粉末は、500Kg／cm2程度の圧力で所望の形
状に加圧成形し、アルミナルツボ中で1100〜1200
℃で２時間本焼成することによりチタン酸ジルコ
ン酸系ペレブスカイト型磁器となる。 The powder is pressure-molded into a desired shape at a pressure of about 500 kg/cm 2 and heated to 1100 to 1200 kg in an aluminum crucible.
By main firing at ℃ for 2 hours, titanate zirconate perevskite type porcelain is obtained.
尚、前記実施例では、予備焼成温度を磁器生成
過程における収縮反応開始温度の600〜700℃とす
ることにより、本焼成温度は、1100〜1200℃に設
定でき、従来の温度より50〜100℃低くすること
ができ、燃焼中における鉛の蒸発量を少なくして
再現性のよい磁器を得ることができた。 In the above example, by setting the preliminary firing temperature to 600 to 700°C, which is the contraction reaction start temperature in the porcelain production process, the main firing temperature can be set to 1100 to 1200°C, which is 50 to 100°C higher than the conventional temperature. By reducing the amount of lead evaporated during combustion, we were able to obtain porcelain with good reproducibility.
＜効果＞
本発明は、上述のように、まず共沈容易な、チ
タン化合物と、ジルコン化合物とで共沈物を作つ
てから、さらにその余の全成分を混合して焼成粉
砕し、チタン酸ジルコン酸系ペロブスカイト型磁
器粉末を製造する方法であるから、共沈させるた
めの条件の設定の困難性を払拭でき、所望の組成
のチタン酸ジルコン酸系ペロブスカイト型磁器粉
末を容易に製造できる等の優れた効果がある。<Effects> As described above, the present invention first makes a coprecipitate with a titanium compound and a zircon compound, which are easy to coprecipitate, and then mixes all the remaining components and pulverizes by firing. Since this is a method for producing zirconate-based perovskite-type porcelain powder, it is possible to eliminate the difficulty of setting conditions for coprecipitation, and it is possible to easily produce zirconate-titanate-based perovskite-type porcelain powder with a desired composition. It has excellent effects.
Claims (1)
物を反応させたペロブスカイト型化合物、または
さらに他のペロブスカイト型化合物を固溶させて
なるチタン酸ジルコン酸系ペロブスカイト型磁器
粉末を、次の二工程により製造することを特徴と
するチタン酸ジルコン酸系ペロブスカイト型磁器
粉末の製造方法。 第一工程 チタン化合物とジルコン化合物を、所定のモル
比で混合した水溶液に、沈澱形成液を加えて共沈
させ、これを乾燥、培焼してチタン酸ジルコニウ
ム粉末を作る。 第二工程 前記第一工程により形成した組成粉末に、その
余の金属酸化物を所定のモル比で混合して仮焼す
る。[Scope of Claims] 1. A perovskite-type porcelain powder made of zirconium titanate and a perovskite-type compound obtained by reacting one or more metal oxides, or a solid solution of another perovskite-type compound, as follows: A method for producing a zirconate titanate perovskite type porcelain powder, which is produced by two steps. First step: A precipitate forming solution is added to an aqueous solution of a titanium compound and a zircon compound mixed at a predetermined molar ratio to cause coprecipitation, followed by drying and calcining to produce zirconium titanate powder. Second Step The remaining metal oxide is mixed with the powder composition formed in the first step at a predetermined molar ratio and calcined.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60073975A JPS60246222A (en) | 1985-04-08 | 1985-04-08 | Production of titanate zirconate-type perovskite ceramic powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60073975A JPS60246222A (en) | 1985-04-08 | 1985-04-08 | Production of titanate zirconate-type perovskite ceramic powder |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP58158382A Division JPS6051664A (en) | 1983-08-30 | 1983-08-30 | Manufacture of lead zirconate titanate ceramic |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS60246222A JPS60246222A (en) | 1985-12-05 |
| JPH0256287B2 true JPH0256287B2 (en) | 1990-11-29 |
Family
ID=13533601
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60073975A Granted JPS60246222A (en) | 1985-04-08 | 1985-04-08 | Production of titanate zirconate-type perovskite ceramic powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS60246222A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6330365A (en) * | 1986-07-23 | 1988-02-09 | 新日本製鐵株式会社 | Manufacture of plzt light-transmitting ceramics |
| JPS63235401A (en) * | 1987-03-23 | 1988-09-30 | Natl Inst For Res In Inorg Mater | Production of dielectric powder containing zirconium and lead |
| US5032559A (en) * | 1989-05-05 | 1991-07-16 | Gte Products Corporation | Method of preparing barium, titanium, zirconium oxide ferroelectric ceramic compositions |
-
1985
- 1985-04-08 JP JP60073975A patent/JPS60246222A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS60246222A (en) | 1985-12-05 |
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