JPS604133B2 - Manufacturing method of lead zirconate titanate (PZT) - Google Patents
Manufacturing method of lead zirconate titanate (PZT)Info
- Publication number
- JPS604133B2 JPS604133B2 JP55156842A JP15684280A JPS604133B2 JP S604133 B2 JPS604133 B2 JP S604133B2 JP 55156842 A JP55156842 A JP 55156842A JP 15684280 A JP15684280 A JP 15684280A JP S604133 B2 JPS604133 B2 JP S604133B2
- Authority
- JP
- Japan
- Prior art keywords
- pzt
- isopropoxide
- zirconate titanate
- lead zirconate
- manufacturing
- 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
- 229910052451 lead zirconate titanate Inorganic materials 0.000 title claims description 18
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- HFGPZNIAWCZYJU-UHFFFAOYSA-N lead zirconate titanate Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ti+4].[Zr+4].[Pb+2] HFGPZNIAWCZYJU-UHFFFAOYSA-N 0.000 title claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 12
- 238000006460 hydrolysis reaction Methods 0.000 claims description 12
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical compound [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 claims description 8
- VSFQMZYFJAOOOG-UHFFFAOYSA-N di(propan-2-yloxy)lead Chemical compound CC(C)O[Pb]OC(C)C VSFQMZYFJAOOOG-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- VXUYXOFXAQZZMF-UHFFFAOYSA-N titanium(IV) isopropoxide Chemical compound CC(C)O[Ti](OC(C)C)(OC(C)C)OC(C)C VXUYXOFXAQZZMF-UHFFFAOYSA-N 0.000 claims description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 21
- 239000000843 powder Substances 0.000 description 15
- 230000015572 biosynthetic process Effects 0.000 description 10
- 238000003786 synthesis reaction Methods 0.000 description 8
- 239000000243 solution Substances 0.000 description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 235000019441 ethanol Nutrition 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 150000004703 alkoxides Chemical class 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 238000004455 differential thermal analysis Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229910052726 zirconium Inorganic materials 0.000 description 3
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 2
- 108091006587 SLC13A5 Proteins 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 235000010650 Hyssopus officinalis Nutrition 0.000 description 1
- 240000001812 Hyssopus officinalis Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 1
- 235000019270 ammonium chloride Nutrition 0.000 description 1
- 150000008064 anhydrides Chemical class 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000004581 coalescence Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 229940046892 lead acetate Drugs 0.000 description 1
- 150000002611 lead compounds Chemical class 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- WBQTXTBONIWRGK-UHFFFAOYSA-N sodium;propan-2-olate Chemical compound [Na+].CC(C)[O-] WBQTXTBONIWRGK-UHFFFAOYSA-N 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- -1 zirconium alkoxide Chemical class 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】
本発明は、チタン酸ジルコン酸鉛（ＰＺｒ）の製造方法
に関するものである。DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing lead zirconate titanate (PZr).
更に詳しくは、本発明は、主として圧電材料に用いられ
るＰＺｒの粉末を、金属ァルコキシドから調製するＰＺ
Ｔの製造方法に関するものである。本発明の目的は、簡
単な製造プロセスによって高純度のＰＺｒを得ることの
できる新規な製造方法を提供しようとするものである。More specifically, the present invention provides PZr powder mainly used for piezoelectric materials, PZr powder prepared from metal alkoxide.
The present invention relates to a method for manufacturing T. An object of the present invention is to provide a novel manufacturing method that can obtain highly pure PZr through a simple manufacturing process.
本発明に係る製造方法は、鉛ィソプロポキシド（Ｐｂ（
ＯＲ）２）と、ジルコニウムイソプロポキシド（Ｚｒ（
ＯＲ）４）と、チタニウムイソブロボキシド（Ｔｉ（Ｏ
Ｒ）４）とを化学量論比に混合し、その溶液に水を加え
て加水分解を行い、析出物を乾燥してＰＺＴを得ること
を特徴としている。The manufacturing method according to the present invention includes lead isopropoxide (Pb(
OR)2) and zirconium isopropoxide (Zr(
OR) 4) and titanium isobroboxide (Ti(O
R) and 4) are mixed in a stoichiometric ratio, water is added to the solution to perform hydrolysis, and the precipitate is dried to obtain PZT.
以下、本発明の製造方法の一例について、第１図を参照
しながら説明してみよう。Hereinafter, an example of the manufacturing method of the present invention will be explained with reference to FIG.
本発明は、第１図イに示すように３種の金属アルコキシ
ドを出発原料に使用するものであるが、はじめに、これ
ら金属アルコキシドの合成の一例について説明する。The present invention uses three types of metal alkoxides as starting materials, as shown in FIG. 1A. First, an example of the synthesis of these metal alkoxides will be described.
‘１）式の反応によって合成した。 Synthesized by the reaction of formula '1).
実験では、９９．９％のＺｒＣ１４１モルに対し過剰の
ィソプロパノールとジルコニウムイソプロポキシドの溶
媒であるベンゼンを加え、この混合溶液中に乾燥アンモ
ニアガスを噴き込んで、ジルコニウムィソプロポキシド
を得た。In the experiment, excess isopropanol and benzene, a solvent for zirconium isopropoxide, were added to 141 moles of 99.9% ZrC, and dry ammonia gas was injected into this mixed solution to obtain zirconium isopropoxide. Ta.
このとき、ジルコニウムィソプロポキシドは、ベンゼン
に溶解しているので、塩化アンモニウムを炉別し、ジル
コニウムィソプロポキシドのベンゼン溶液を得た。第２
図は「ジルコニウムィソプロポキシドのベンゼン溶液を
得るまでのフローシートである。At this time, since zirconium isopropoxide was dissolved in benzene, ammonium chloride was separated in a furnace to obtain a benzene solution of zirconium isopropoxide. Second
The figure is a flow sheet for obtaining a benzene solution of zirconium isopropoxide.
〔チタニウムイソプロポキシドの合成）上記と同様な方
法によって得られる。[Synthesis of titanium isopropoxide] Obtained by the same method as above.
実験では、市販されている特級試薬を使用した。In the experiment, commercially available special grade reagents were used.
■式の反応によって合成した。 (2) Synthesized by the reaction of formula.
Ｐｂ（Ｃ２日３０２）２十２‐Ｃ３日７０Ｎａ→Ｐｂ（
ｉ‐ＯＣ３日７）２十州ａＣ２＆０３↓（２｝実験では
、はじめに、Ｐｂ（Ｃ２日３０２）２・細２０を９０℃
で１２時間以上加熱することによって「 Ｐｂ（Ｃ２日
３０２）２の無水物を得た。Pb (C2 day 302) 212-C3 day 70Na → Pb (
i-OC3day 7) 2 Jushu aC2&03↓(2} In the experiment, first, Pb (C2day 302) 2. Thin 20 was heated to 90℃
An anhydride of Pb(C2day302)2 was obtained by heating for more than 12 hours at
次に、金属ナトＩＪウム１モルに対して過剰のィソプロ
パノールを加え、還流下であって４０〜５０ｑ○で反応
させ、ナトリウムィソプロポキシドを得、これに０．６
モルの無水酢酸鉛（Ｐｂ（Ｃ２日３０２）２）を加え、
１時間還流下で反応させることにより、鈴ィソプロポキ
シドを合成した。このとき未反応のＰｂ（Ｃ２４０２）
２と、生じたＮａＣ２日３０３を除去するために、溶媒
置換を行い、過剰アルコールを除去し、続いてベンゼン
を加え、Ｐｂ（ＯＰｒｉ）２とＮａＣ２＆０３を炉列し
た。第３図は、上記の鉛ィソプロポキシドの合成のフロ
ーシートである。第１図に戻り、このようにして得られ
たジルコニウム、チタン、鉛の各々のイソプロポキシド
のベンゼン溶液を調製し、これらの溶液をＰｂ：Ｚｒ：
Ｔｉ＝１：０．５：０．５のモル比になるように混合（
第１図口）し、この混合溶液に鉛ィソプロポキシド１モ
ルに対して、５００モルの蒸留水を加え、かくはんしな
がら加水分解を行う（第１図ハ）。Next, excess isopropanol was added to 1 mole of metal sodium, and the reaction was carried out at 40 to 50 q○ under reflux to obtain sodium isopropoxide, to which 0.6
Add moles of anhydrous lead acetate (Pb(C2day302)2),
Suzu-isopropoxide was synthesized by reacting under reflux for 1 hour. At this time, unreacted Pb (C2402)
In order to remove 2 and the resulting NaC2&03, solvent replacement was performed to remove excess alcohol, followed by the addition of benzene and the addition of Pb(OPri)2 and NaC2&03. FIG. 3 is a flow sheet for the synthesis of the above lead isopropoxide. Returning to FIG. 1, benzene solutions of each of the isopropoxides of zirconium, titanium, and lead thus obtained were prepared, and these solutions were mixed into Pb:Zr:
Mixed at a molar ratio of Ti=1:0.5:0.5 (
Then, 500 mol of distilled water is added to this mixed solution per 1 mol of lead isopropoxide, and hydrolysis is carried out while stirring (Fig. 1 C).
加水分解によって得られた沈殿物を炉週、洗浄後、自然
乾燥を行い、焼成してＰＺＴの超微粉末を得る（第１図
二，ホ）。なお、加水分解を行なった後、スプレードラ
イヤーによって超微粉末を得るようにしてもよい。スプ
レードライヤーはト加水分解した溶液を、霧状にして熱
風に接触させ、水分を蒸発乾燥させるものであって、短
時間でＰＺＴの超微粉末を得ることができる利点がある
。第４図は、加水分解によって得られた白色粉末の各温
度におけるＸ線回析測定結果を示す線図であって、イは
室温、口は２００ｑｏ、ハは４００℃、二は６００℃で
の測定結果をそれぞれ示している。また、第５図は、加
水分解して得られた白色粉末を加熱していった時の加熱
温度と、白色粉末の重量とＤＴＡ（示差熱分析）曲線を
示したものである。これらの結果から、加水分解によっ
て得られた白色粉末は、室温において、完全ではないが
ＰＺＴとしての性質をもつものであって（第４図イ参照
）、加熱温度５００℃以上において、結晶性のＰＺＴが
得られることが分かった（第４図二および、第５図のＤ
ＴＡのピーク温度参照）。The precipitate obtained by hydrolysis is washed in an oven, air-dried, and then calcined to obtain an ultrafine powder of PZT (FIG. 1, 2 and 5). Incidentally, after hydrolysis, ultrafine powder may be obtained using a spray dryer. A spray dryer atomizes a hydrolyzed solution and brings it into contact with hot air to evaporate and dry the water, and has the advantage of being able to obtain ultrafine powder of PZT in a short time. Figure 4 is a diagram showing the results of X-ray diffraction measurements at various temperatures of the white powder obtained by hydrolysis, where A is room temperature, mouth is 200qo, c is 400°C, and 2 is 600°C. The measurement results are shown. Moreover, FIG. 5 shows the heating temperature when the white powder obtained by hydrolysis was heated, the weight of the white powder, and the DTA (differential thermal analysis) curve. From these results, the white powder obtained by hydrolysis has the properties of PZT at room temperature, although not completely (see Figure 4 A), and becomes crystalline at heating temperatures of 500°C or higher. It was found that PZT could be obtained (Fig. 4 2 and Fig. 5 D
(See peak temperature of TA).
また、電子顕微鏡の観察結果によれば、加水分解によっ
て得られた白色粉末の粒形は、大部分が０．１山以下の
微粒子であるが、所々に２〜３仏の大きさの六角板状の
鉛の化合物が点在していた。Furthermore, according to the results of observation using an electron microscope, the grain shape of the white powder obtained by hydrolysis is mostly fine particles of 0.1 mounds or less, but there are hexagonal plates the size of 2 to 3 Buddhas in some places. Scattered lead compounds were found.
この六角板状の粒子は、ＰＺＴの生成温度を４００℃と
した場合も認められたが、５００午０とした場合では完
全に消失し、０．１山以下の球状をした比較的均一な微
粉末となった。なお、８００００とすると、０．３ム程
度の粒子の成長が起り、粒子どうしの合体が認められた
。それ故に、５００ｑＣ付近で焼成したものが最も適当
である。このようにして得られたＰＺｒの超微粉末は、
例えばホットプレス方式によってＰＺｒ基板に構成され
る。These hexagonal plate-shaped particles were also observed when the PZT formation temperature was set to 400°C, but they completely disappeared when the PZT formation temperature was set to 500°C, and they became relatively uniform particles with a spherical shape of 0.1 peak or less. It became powder. Incidentally, when the particle size was 80,000, growth of particles of about 0.3 μm occurred, and coalescence of particles was observed. Therefore, the most suitable material is one fired at around 500qC. The PZr ultrafine powder thus obtained is
For example, it is formed into a PZr substrate using a hot press method.
なお、上記の実施例において、出発原料に使われる各金
属アルコキシドの合成に用いられるアルコールとしては
、メチルアルコール、エチルアルコ−′レ、ノルマノレ
フ。In the above examples, the alcohols used in the synthesis of each metal alkoxide used as a starting material include methyl alcohol, ethyl alcohol, and normanolev.
ロピルアルコール、ノルマ′レプチルアルコール、ター
シヤリーブチルアルコール等、各種のアルコールを用い
ることが可能である。以上説明したように、本発明によ
れば、簡単な製造プロセスによって純度の高いＰＺｒを
得ることができる。Various alcohols can be used, such as propyl alcohol, normal leptyl alcohol, and tertiary butyl alcohol. As explained above, according to the present invention, highly pure PZr can be obtained through a simple manufacturing process.
第１図は本発明の製造方法の一例について示す説明図、
第２図はジルコニウムイソプ。
ポキシドのベンゼン溶液を得るまでのフローシ−ト、第
３図は鉛イソプロポキシドの合成のフローシート、第４
図は加水分解によって得られた白色粉末の各温度におけ
るＸ線回析測定結果を示す線図、第５図は加水分解して
得られた白色粉末を加熱していったときの加熱温度と白
色粉末の重量、ＤＴＡを示した線図である。第１図
第２図
第３図
第５図
緒ム図FIG. 1 is an explanatory diagram showing an example of the manufacturing method of the present invention,
Figure 2 shows zirconium isop. Flow sheet for obtaining a benzene solution of poxide. Figure 3 is a flow sheet for synthesis of lead isopropoxide. Figure 4 is a flow sheet for the synthesis of lead isopropoxide.
The figure is a diagram showing the results of X-ray diffraction measurements at various temperatures of the white powder obtained by hydrolysis. Figure 5 shows the heating temperature and white color when the white powder obtained by hydrolysis is heated. It is a diagram showing the weight of powder and DTA. Figure 1 Figure 2 Figure 3 Figure 5 Diagram
Claims (1)
シドと、チタニウムイソプロポキシドとを化学量論比に
混合し、その溶液に水を加えて加水分解を行い、折出物
を乾燥してＰＺＴを得るようにしたチタン酸ジルコン酸
鉛（ＰＺＴ）の製造方法。 ２ 鉛イソプロポキシドを次式の反応によつて合成した
特許請求の範囲第１項記載のチタン酸ジルコン酸鉛（Ｐ
ＺＴ）の製造方法。 Ｐｂ（Ｃ＿２Ｈ＿３Ｏ＿２）＿２＋２ｉ−Ｃ＿３Ｈ＿７
ＯＮａ→Ｐｂ（ｉ−ＯＣ＿３Ｈ＿７）＿２＋２ＮａＣ＿
２Ｈ＿３Ｏ＿３↓３ ジルコニウムイソプロポキシドを
次式の反応によつて合成した特許請求の範囲第１項記載
のチタン酸ジルコン酸鉛（ＰＺＴ）の製造方法。 ▲数式、化学式、表等があります▼４ 加水分解して得
られた析出物を５００℃付近で焼成するようにした特許
請求の範囲第１項記載のチタン酸ジルコン酸鉛（ＰＺＴ
）の製造方法。[Claims] 1. Mix lead isopropoxide, zirconium isopropoxide, and titanium isopropoxide in a stoichiometric ratio, add water to the solution to perform hydrolysis, and dry the precipitate. A method for producing lead zirconate titanate (PZT) in which PZT is obtained by 2. Lead zirconate titanate (P
ZT) manufacturing method. Pb(C_2H_3O_2)_2+2i-C_3H_7
ONa→Pb(i-OC_3H_7)_2+2NaC_
2H_3O_3↓3 The method for producing lead zirconate titanate (PZT) according to claim 1, wherein zirconium isopropoxide is synthesized by the reaction of the following formula. ▲There are mathematical formulas, chemical formulas, tables, etc.▼4 Lead zirconate titanate (PZT) according to claim 1, in which the precipitate obtained by hydrolysis is calcined at around 500°C.
) manufacturing method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55156842A JPS604133B2 (en) | 1980-11-07 | 1980-11-07 | Manufacturing method of lead zirconate titanate (PZT) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP55156842A JPS604133B2 (en) | 1980-11-07 | 1980-11-07 | Manufacturing method of lead zirconate titanate (PZT) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS5782121A JPS5782121A (en) | 1982-05-22 |
| JPS604133B2 true JPS604133B2 (en) | 1985-02-01 |
Family
ID=15636558
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP55156842A Expired JPS604133B2 (en) | 1980-11-07 | 1980-11-07 | Manufacturing method of lead zirconate titanate (PZT) |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS604133B2 (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6086026A (en) * | 1983-10-17 | 1985-05-15 | Mitsubishi Mining & Cement Co Ltd | Production of composite perovskite compound |
| JPS6090826A (en) * | 1983-10-20 | 1985-05-22 | Mitsubishi Mining & Cement Co Ltd | Manufacture of tungstate |
| JPS624340U (en) * | 1985-06-24 | 1987-01-12 | ||
| JPS62162670A (en) * | 1986-01-09 | 1987-07-18 | 住友金属鉱山株式会社 | Manufacturing method of lead zirconate titanate sintered body |
-
1980
- 1980-11-07 JP JP55156842A patent/JPS604133B2/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| JPS5782121A (en) | 1982-05-22 |
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