JPH01259583A - Synthesis of pb-ba-zr-ti uniform oxide powder - Google Patents
Synthesis of pb-ba-zr-ti uniform oxide powderInfo
- Publication number
- JPH01259583A JPH01259583A JP63087204A JP8720488A JPH01259583A JP H01259583 A JPH01259583 A JP H01259583A JP 63087204 A JP63087204 A JP 63087204A JP 8720488 A JP8720488 A JP 8720488A JP H01259583 A JPH01259583 A JP H01259583A
- Authority
- JP
- Japan
- Prior art keywords
- aqueous solution
- acid
- solution containing
- hydroxide
- oxide powder
- 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.)
- Granted
Links
- 239000000843 powder Substances 0.000 title claims abstract description 21
- 230000015572 biosynthetic process Effects 0.000 title claims description 4
- 238000003786 synthesis reaction Methods 0.000 title claims description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 33
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 229910052788 barium Inorganic materials 0.000 claims abstract description 9
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 8
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 8
- 229910052745 lead Inorganic materials 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 16
- 239000002244 precipitate Substances 0.000 claims description 11
- 230000002378 acidificating effect Effects 0.000 claims description 7
- 230000002194 synthesizing effect Effects 0.000 claims description 4
- 238000002156 mixing Methods 0.000 abstract description 7
- 239000000203 mixture Substances 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract description 5
- IVORCBKUUYGUOL-UHFFFAOYSA-N 1-ethynyl-2,4-dimethoxybenzene Chemical compound COC1=CC=C(C#C)C(OC)=C1 IVORCBKUUYGUOL-UHFFFAOYSA-N 0.000 abstract description 2
- 229910021514 lead(II) hydroxide Inorganic materials 0.000 abstract description 2
- 239000011812 mixed powder Substances 0.000 abstract description 2
- 239000013049 sediment Substances 0.000 abstract 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 abstract 1
- 239000000470 constituent Substances 0.000 abstract 1
- 239000010936 titanium Substances 0.000 description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- QDZRBIRIPNZRSG-UHFFFAOYSA-N titanium nitrate Chemical compound [O-][N+](=O)O[Ti](O[N+]([O-])=O)(O[N+]([O-])=O)O[N+]([O-])=O QDZRBIRIPNZRSG-UHFFFAOYSA-N 0.000 description 6
- IWOUKMZUPDVPGQ-UHFFFAOYSA-N barium nitrate Chemical compound [Ba+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O IWOUKMZUPDVPGQ-UHFFFAOYSA-N 0.000 description 4
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 150000004703 alkoxides Chemical class 0.000 description 3
- 238000000975 co-precipitation Methods 0.000 description 3
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 150000001242 acetic acid derivatives Chemical class 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Chemical compound [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 150000003841 chloride salts Chemical class 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 150000003891 oxalate salts Chemical class 0.000 description 2
- CPRMKOQKXYSDML-UHFFFAOYSA-M rubidium hydroxide Chemical compound [OH-].[Rb+] CPRMKOQKXYSDML-UHFFFAOYSA-M 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 1
- 238000005406 washing Methods 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、Ｐｂ−Ｂａ−Ｚｒ−Ｔｉ系均一酸化物粉末の
合成方法に関する。DETAILED DESCRIPTION OF THE INVENTION Field of the Invention The present invention relates to a method for synthesizing Pb-Ba-Zr-Ti homogeneous oxide powder.
該粉末は電歪現象が認められる。An electrostrictive phenomenon is observed in this powder.
従来の技術
従来の酸化物粉末の製造方法としては、（１）成分元素
の酸化物粉末を高温で焼成する固相反応法、
（２）水溶液中の成分元素イオンをシュウ酸塩として共
沈させる方法、
〔３）成分元素をアルカリ中へ入れ水酸化物として共沈
させる方法、
（４）成分元素のアルコキシドを加水分解して共沈させ
る方法
等が知られている。Conventional technology Conventional methods for producing oxide powder include (1) a solid-phase reaction method in which oxide powders of component elements are calcined at high temperatures; (2) ions of component elements in an aqueous solution are co-precipitated as oxalate. The following methods are known: (3) A method in which the component elements are placed in an alkali and co-precipitated as hydroxide, (4) A method in which the alkoxides of the component elements are hydrolyzed and co-precipitated.
しかしながら、（１）の面相反応によって得られる粉末
は最も焼結しにく（、該粉末を焼結するには高温もしく
は焼結促進剤の添加を必要とする。（２）のシュウ酸塩
として共沈させる方法（シュウ酸性）は、Ｚｒ、Ｔｉの
シュウ酸塩は水に対する溶解度が大きく完全に沈澱を生
じないため、希望する割合で共沈させることが困難であ
る。また、（４）のアルコキシド法は、高純度で均一性
の高いものが得られるが、各種成分イオンを一度アルコ
キシドにして合成しなければならないので、製法が煩雑
となり、経済的にも不利である等、それぞれ欠点を有し
ている。However, the powder obtained by the phase reaction in (1) is the most difficult to sinter (sintering of the powder requires high temperature or the addition of a sintering accelerator. The coprecipitation method (oxalic acidity) is difficult to coprecipitate at the desired ratio because the oxalates of Zr and Ti have high solubility in water and do not completely precipitate. Although the alkoxide method can produce products with high purity and high homogeneity, each component has its own drawbacks, such as the need to convert the various component ions into alkoxides for synthesis, which makes the manufacturing process complicated and economically disadvantageous. are doing.
Ｐｂ−Ｂａ−Ｚｒ−Ｔｉ系のような４成分系において所
定の割合で粉末を合成することは非常に難しい、共沈に
よりこの系の粉末を得ようとする場合、上記（２）のシ
ュウ酸洗ではＺｒ、Ｔｉが完全に沈澱しない、また上記
（３）の水酸化物法ではＢａの水酸化物が水に溶解する
という問題がある。It is very difficult to synthesize powder at a predetermined ratio in a four-component system such as the Pb-Ba-Zr-Ti system.When trying to obtain powder of this system by coprecipitation, it is necessary to use the oxalic acid in (2) above. Washing does not completely precipitate Zr and Ti, and the hydroxide method (3) above has the problem that Ba hydroxide dissolves in water.
発明が解決しようとする課題
本発明の目的は、Ｐｂ−Ｂａ−Ｚｒ−Ｔｉからなる４成
分系の粉末を均一に、かつ、希望の組成で合成する方法
を提供することにある。Problems to be Solved by the Invention An object of the present invention is to provide a method for uniformly synthesizing a four-component powder of Pb-Ba-Zr-Ti with a desired composition.
課題を解決゛するための手段
本発明者らは、上記目的を達成するために鋭意検討した
結果、各種金属を特定の条件下に共沈させることにより
本発明の目的が達成されることを見出し、本発明を完成
させるに至った。Means for Solving the Problems As a result of intensive studies to achieve the above object, the present inventors discovered that the object of the present invention can be achieved by co-precipitating various metals under specific conditions. , we have completed the present invention.
すなわち、本発明は、
Ｐｂ−Ｂａ−Ｚｒ−Ｔｉ系均一酸化物粉末の合成におい
て、
Ａ）Ｂａ、Ｚｒを含有した水溶液とシュウ酸水溶液とを
混合し沈澱物が溶解するまで酸を添加して得られる透明
な酸性水溶液と、
Ｂ）Ｐｂ、Ｔｉを含有した透明な酸性水溶液とを、ＰＨ
が９以上に保持されたアルカリ水溶液に同時に滴下する
ことを特徴とするＰｂ−Ｂａ−Ｚｒ−Ｔｉ系均一酸化物
粉末の合成方法である。That is, in the synthesis of a Pb-Ba-Zr-Ti homogeneous oxide powder, the present invention includes: A) mixing an aqueous solution containing Ba and Zr with an oxalic acid aqueous solution and adding acid until the precipitate is dissolved; The resulting transparent acidic aqueous solution and B) the transparent acidic aqueous solution containing Pb and Ti are
This is a method for synthesizing a Pb-Ba-Zr-Ti homogeneous oxide powder, which is characterized in that the Pb-Ba-Zr-Ti homogeneous oxide powder is simultaneously added dropwise to an alkaline aqueous solution in which Pb is maintained at 9 or more.
本発明にがかるＢａ、Ｚｒを含有した水溶液とは、例え
ば、硝酸バリウム、硝酸ジルコニウムを水に熔解させた
ものであるが、硝酸バリウム、硝酸ジルコニウム以外で
も、水に溶けるものであればなんでも良い、そのような
例としては、それぞれの酢酸塩、塩化物などがあげられ
る。また、本発明においては、Ｂａ、Ｚｒを含有した水
溶液とシュウ酸水溶液とを混合し、次に沈澱物が溶解す
るまで酸を添加する。沈澱物が完全に溶解した場合、透
明な酸性水溶液が得られる。この場合酸としては、例え
ば、硝酸、酢酸等があげられる。酸の添加後のＰＨは１
以下であることが望ましい。The aqueous solution containing Ba and Zr according to the present invention is, for example, one obtained by dissolving barium nitrate or zirconium nitrate in water, but any solution other than barium nitrate or zirconium nitrate may be used as long as it dissolves in water. Such examples include the respective acetates, chlorides, etc. Further, in the present invention, an aqueous solution containing Ba and Zr and an oxalic acid aqueous solution are mixed, and then acid is added until the precipitate is dissolved. When the precipitate is completely dissolved, a clear acidic aqueous solution is obtained. In this case, examples of the acid include nitric acid and acetic acid. pH after addition of acid is 1
The following is desirable.
もしもＰＨが１をこえる場合、Ｂａ、Ｚｒのシュウ酸塩
が再沈澱する。If the pH exceeds 1, oxalates of Ba and Zr will be reprecipitated.
本発明にかかるＰｂ、Ｔｉを含有した透明な酸性水溶液
とは、例えば、硝酸鉛、硝酸チタンを水に完全に溶解さ
せたものである。硝酸鉛、硝酸チタン以外でも、水に溶
は水溶液が酸性を示すものであればなんでも良い、その
ような例としては、それぞれの酢酸塩、塩化物などがあ
げられる。The transparent acidic aqueous solution containing Pb and Ti according to the present invention is, for example, one in which lead nitrate and titanium nitrate are completely dissolved in water. In addition to lead nitrate and titanium nitrate, any substance that dissolves in water can be used as long as the aqueous solution exhibits acidity, such as their acetates and chlorides.
前記２種の酸性水溶液には、Ｐｂ、Ｂａ、Ｚｒ、Ｔｉ以
外の金属塩を第３成分として添加しても良い。A metal salt other than Pb, Ba, Zr, and Ti may be added as a third component to the two types of acidic aqueous solutions.
本発明にかかるアルカリ水溶液は、アンモニア水で良い
、アンモニア水以外でもアルカリ性水溶液であればなん
でも良い０例えば、ＮａＯＨ。The alkaline aqueous solution according to the present invention may be ammonia water, or any alkaline aqueous solution other than ammonia water may be used. For example, NaOH.
ＫＯＨ，ＲｂＯＨおよび／またはＣｓＯＨなどの水溶液
でも良い。An aqueous solution of KOH, RbOH and/or CsOH may also be used.
本発明にかかるアルカリ水溶液は、Ｐ）ｌを９以上に保
持する。ＰＨが９に満たない場合、水酸化鉛、水酸化チ
タン、水酸化ジルコニウムの沈澱が再溶解してしまう。The alkaline aqueous solution according to the present invention maintains P)l at 9 or more. If the pH is less than 9, the precipitates of lead hydroxide, titanium hydroxide, and zirconium hydroxide will be redissolved.
本発明において水酸化物を共沈させる温度は、特に限定
されないが、通常は、１０〜６０°Ｃの範囲である。In the present invention, the temperature at which the hydroxide is coprecipitated is not particularly limited, but is usually in the range of 10 to 60°C.
本発明にかかる沈澱物の焼成条件は、通常は、５００〜
８００°Ｃでの仮焼、１１００〜１３５０°Ｃでの焼結
である。The firing conditions for the precipitate according to the present invention are usually 500~
Calcination at 800°C and sintering at 1100-1350°C.
実施例 以下実施例により本発明を更に説明する。Example The present invention will be further explained below with reference to Examples.
実施例Ｉ
Ｂ ａ （Ｎｏｗ） ｚ 、Ｚ ｒ Ｏ（ＮＣｈ） ｚ
を所定量秤量し、水に溶解させた０次にＢａ、Ｚｒの総
モル数の５倍量のシュウ酸を秤量し、水に溶解させた。Example I B a (Now) z , Z r O (NCh) z
A predetermined amount of oxalic acid was weighed, and oxalic acid in an amount five times the total number of moles of zero-order Ba and Zr dissolved in water was weighed and dissolved in water.
この２種類の水溶液を混合した。混合後に生じた沈澱物
を溶解させるために、硝酸を加え、ＰＨを１以下とした
。また、これとは別に、硝酸鉛、硝酸チタンを所定量秤
量し、水に溶解させた。These two types of aqueous solutions were mixed. In order to dissolve the precipitate formed after mixing, nitric acid was added to adjust the pH to 1 or less. Separately, predetermined amounts of lead nitrate and titanium nitrate were weighed and dissolved in water.
これら２種類の酸性水溶液を、ＰＨ１０以上のＮａＯＨ
水溶液に滴下し沈澱物を得た０滴下終了後のＰＨは １
０ であった。この沈澱物を得て４００°Ｃに加熱し、
酸化物混合粉末を作成した。These two types of acidic aqueous solutions are mixed with NaOH with a pH of 10 or more.
The pH after the 0 drop when dropping into an aqueous solution and obtaining a precipitate is 1.
It was 0. This precipitate was obtained and heated to 400°C,
An oxide mixed powder was created.
このようにして得られた粉末の組成分析の結果、希望し
た組成であることが確認された。また、粉末の均一性を
評価するためにＸ線マイクロアナライザーによる分析を
行った。酸化物混合法で作成したものと比較すると、明
らかに混合の均一性が向上していることが確認できた。As a result of compositional analysis of the powder thus obtained, it was confirmed that it had the desired composition. In addition, an analysis using an X-ray microanalyzer was performed to evaluate the uniformity of the powder. When compared with those prepared using the oxide mixing method, it was confirmed that the uniformity of the mixing was clearly improved.
また、得られた粉末の電歪特性を調べるために、８００
°Ｃで仮焼し、粉砕成型して得たサンプルを１３２０
”Ｃで焼結した。焼結した試料を切断、電極付けを行っ
た。In addition, in order to investigate the electrostrictive properties of the obtained powder,
A sample obtained by calcining at °C and pulverization was heated to 1320 °C.
The sintered sample was cut and electrodes were attached.
これに１０ｋｖ／ｃｍの電圧を印加したところ、酸化物
混合法で得たものより約２倍の伸びを示した。When a voltage of 10 kv/cm was applied to this, the elongation was approximately twice that of that obtained by the oxide mixing method.
発明の効果
上記したように本発明の方法により、これまでの技術で
はなし遂げられなかった多成分系での共沈が可能になっ
た。その結果、均一性にすぐれ、かつ、希望の組成の酸
化物が得られた。このようにして得られた粉末を原料と
する焼結体の電歪特性は、酸化物混合法による焼結体と
比べて、明らかに異なる性質を示すものであり、成分元
素の均一性が電歪特性の向上に寄与していることは非常
に驚くべき結果である。Effects of the Invention As described above, the method of the present invention enables coprecipitation in a multicomponent system, which has not been possible with conventional techniques. As a result, an oxide with excellent uniformity and a desired composition was obtained. The electrostrictive properties of the sintered body made from the powder obtained in this way are clearly different from those of the sintered body made by the oxide mixing method, and the uniformity of the component elements is This is a very surprising result that it contributes to the improvement of distortion characteristics.
特許出願人 三井東圧化学株式会社Patent applicant: Mitsui Toatsu Chemical Co., Ltd.
Claims (1)
おいて、 Ａ）Ｂａ、Ｚｒを含有した水溶液とシュウ酸水溶液とを
混合し沈澱物が溶解するまで酸を添加して得られる透明
な酸性水溶液と、 Ｂ）Ｐｂ、Ｔｉを含有した透明な酸性水溶液とを、ＰＨ
が９以上に保持されたアルカリ水溶液に同時に滴下する
ことを特徴とするＰｂ−Ｂａ−Ｚｒ−Ｔｉ系均一酸化物
粉末の合成方法。[Claims] 1. In the synthesis of Pb-Ba-Zr-Ti homogeneous oxide powder, A) an aqueous solution containing Ba and Zr and an oxalic acid aqueous solution are mixed and acid is added until the precipitate is dissolved. and B) a transparent acidic aqueous solution containing Pb and Ti.
1. A method for synthesizing a Pb-Ba-Zr-Ti homogeneous oxide powder, which method comprises simultaneously dropping the Pb-Ba-Zr-Ti homogeneous oxide powder into an alkaline aqueous solution in which the
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8720488A JP2577770B2 (en) | 1988-04-11 | 1988-04-11 | Method for synthesizing Pb-Ba-Zr-Ti homogeneous oxide powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8720488A JP2577770B2 (en) | 1988-04-11 | 1988-04-11 | Method for synthesizing Pb-Ba-Zr-Ti homogeneous oxide powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01259583A true JPH01259583A (en) | 1989-10-17 |
| JP2577770B2 JP2577770B2 (en) | 1997-02-05 |
Family
ID=13908437
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8720488A Expired - Lifetime JP2577770B2 (en) | 1988-04-11 | 1988-04-11 | Method for synthesizing Pb-Ba-Zr-Ti homogeneous oxide powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2577770B2 (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6153113A (en) * | 1984-08-18 | 1986-03-17 | Natl Inst For Res In Inorg Mater | Production of powdery raw material of easily sintering perovskite and its solid solution by wet process |
| JPS61186219A (en) * | 1985-02-13 | 1986-08-19 | Natl Inst For Res In Inorg Mater | Production of lead-containing fine powder |
-
1988
- 1988-04-11 JP JP8720488A patent/JP2577770B2/en not_active Expired - Lifetime
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6153113A (en) * | 1984-08-18 | 1986-03-17 | Natl Inst For Res In Inorg Mater | Production of powdery raw material of easily sintering perovskite and its solid solution by wet process |
| JPS61186219A (en) * | 1985-02-13 | 1986-08-19 | Natl Inst For Res In Inorg Mater | Production of lead-containing fine powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2577770B2 (en) | 1997-02-05 |
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