JP2866416B2 - Method for producing perovskite-type composite oxide powder - Google Patents
Method for producing perovskite-type composite oxide powderInfo
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- JP2866416B2 JP2866416B2 JP34039689A JP34039689A JP2866416B2 JP 2866416 B2 JP2866416 B2 JP 2866416B2 JP 34039689 A JP34039689 A JP 34039689A JP 34039689 A JP34039689 A JP 34039689A JP 2866416 B2 JP2866416 B2 JP 2866416B2
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Description
【発明の詳細な説明】 (産業上の利用分野) この発明は、一般式ABO3で表される複合ペロブスカイ
ト型酸化物粉末、特にペロブスカイト化率が高く、粒子
が微細で焼結性に優れた粉末を製造する方法に関する。BACKGROUND OF THE INVENTION (FIELD OF THE INVENTION) This invention relates to compounds of the general formula ABO composite perovskite oxide powder represented by 3, especially perovskite rate high, particles with excellent fine sinterability The present invention relates to a method for producing a powder.
(従来の技術) 複合ペロブスカイト型酸化物は、圧電体、誘電体、半
導体、センサー材料などの機能性セラミックスとして広
範囲に利用されている。最近では、機能性の向上あるい
は新しい機能の付加が活発に進められており、原料粉末
に対して粒子の微細化、組成の均一性の向上、低温焼結
性の付与などが要望されている。(Prior Art) Composite perovskite oxides are widely used as functional ceramics such as piezoelectrics, dielectrics, semiconductors, and sensor materials. Recently, the improvement of functionality or the addition of new functions has been actively promoted, and there has been a demand for reducing the size of particles, improving the uniformity of composition, and imparting low-temperature sinterability to raw material powders.
従来、複合ペロブスカイト型酸化物粉末の製造方法と
して、固相合成法と共沈法が知られている。以下、これ
らの方法について概説する。BACKGROUND ART Conventionally, a solid phase synthesis method and a coprecipitation method have been known as methods for producing a composite perovskite oxide powder. Hereinafter, these methods will be outlined.
(a) 固相合成法 この方法は、各原料成分の化合物を秤量、混合し仮焼
する方法である。これは、最も一般的なものであるが、
高温反応であるため、鉛成分が蒸発し組成が不均一にな
りやすく、また、粒径も微細なものが得難いという欠点
がある。また、Nbを含む系では、通常の方法ではペロブ
スカイト単相のものは得難く、パイロクロア相が混在し
てしまう。パイロクロア相は焼結性を損ない、焼結体の
電気特性を著しく悪化させるので、この相を少なくする
対策もいくつか提案されている。(A) Solid-phase synthesis method This method is a method of weighing, mixing and calcining the compounds of each raw material component. This is the most common,
Since it is a high-temperature reaction, there is a disadvantage that the lead component evaporates and the composition tends to be non-uniform, and it is difficult to obtain fine particles. Further, in a system containing Nb, it is difficult to obtain a perovskite single phase by a usual method, and a pyrochlore phase is mixed. Since the pyrochlore phase impairs the sinterability and significantly deteriorates the electrical properties of the sintered body, some measures have been proposed to reduce this phase.
例えば、S.L.Swrartz、T.R.Shroutらによって、Pb(M
g1/3Nb2/3)O3の製造においては、 MgO+Nb2O5→MgNb2O6(焼成温度約1000℃) 1/3MgNb2O6+PbO→Pb(Mg1/3Nb2/3)O3 (焼成温度約900℃) という二段階焼成法によりペロブスカイト単相のものが
得られるとの報告がなされている。(Mater.Res.Bull.1
7.1245(1982)) 通常の一段焼成法でも、焼成と解砕を繰り返して行え
ば、ペロブスカイト相の割合が増加するが、この方法で
はペロブスカイト単相のものは得難い。For example, SLSwrartz, TRShrout et al.
In the production of g 1/3 Nb 2/3 ) O 3 , MgO + Nb 2 O 5 → MgNb 2 O 6 (calcination temperature about 1000 ° C.) 1 / 3MgNb 2 O 6 + PbO → Pb (Mg 1/3 Nb 2/3 It has been reported that a single-phase perovskite phase can be obtained by a two-stage calcination method of O 3 (calcination temperature of about 900 ° C.). (Mater.Res.Bull. 1
In 7.1245 (1982)) normal stage firing method, by performing repeated firing and crushing, the proportion of the perovskite phase increases, that of the perovskite single phase in this method difficult to obtain.
いずれにしても固相合成法では、粒子の微細化や組成
の均一性の点に問題がある。In any case, the solid phase synthesis method has problems in terms of finer particles and uniformity of composition.
(b) 共沈法 これは、各成分の混合溶液を作り、これをアルカリ等
の沈澱生成液と接触させて共沈物を得て、これを乾燥、
仮焼する方法である。(B) Coprecipitation method In this method, a mixed solution of each component is prepared, and the mixed solution is brought into contact with a precipitation solution such as an alkali to obtain a coprecipitate, which is dried and dried.
It is a method of calcining.
この共沈法においてもペロブスカイト単相粉末は得難
く、また沈澱生成時、乾燥時または仮焼時に二次粒子を
形成し、得られた粉末は焼結性が良好でないという欠点
がある。Even in this coprecipitation method, a perovskite single-phase powder is difficult to obtain, and secondary particles are formed during precipitation, drying, or calcination, and the obtained powder has poor sinterability.
上記のように、Nbを含む鉛系複合ペロブスカイト型酸
化物の粉末で、ペロブスカイト単相で易焼結性のものを
得る製造法は確立されておらず、その開発が待たれてい
る。As described above, a method for obtaining a powder of Nb-containing lead-based composite perovskite oxide having a single phase of perovskite and easy sintering has not been established, and its development is awaited.
(発明が解決しようとする課題) 本発明の目的は、従来の製造方法ではペロブスカイト
単相のものが得難いNbを含む複合ペロブスカイト型酸化
物粉末の製造において、易焼結性、均一性を満足し、か
つペロブスカイト単相の微細な粉末を効率よく製造する
ことができ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 satisfy the sinterability and uniformity in the production of a composite perovskite-type oxide powder containing Nb, which is difficult to obtain a perovskite single phase in the conventional production method. Another object of the present invention is to provide a method for efficiently producing fine powder of single phase perovskite.
(課題を解決するための手段) 本発明は、下記からまでの工程からなる一般式AB
O3で表される複合ペロブスカイト型酸化物の製造方法を
要旨とする。(Means for Solving the Problems) The present invention provides a compound represented by the general formula AB comprising the following steps:
The gist is a method for producing a composite perovskite oxide represented by O 3 .
Nbを含む溶液と他のB成分の少なくとも一種類を含
む溶液を混合し反応させ、Nb−B成分系の均一溶液を生
成させる工程。A step of mixing and reacting a solution containing Nb and a solution containing at least one other component B to form a homogeneous solution of an Nb-B component system.
反応容器内で、PbあるいはPbと他のA成分の少なく
とも一種類を含む溶液をアルカリ金属水溶液と反応させ
て、PbあるいはPbと他のA成分の水酸化物沈殿を生成さ
せる工程。A step of causing Pb or a solution containing at least one of Pb and another A component to react with an aqueous alkali metal solution in a reaction vessel to form a hydroxide precipitate of Pb or Pb and another A component.
上記反応容器内に工程で生成させた溶液を加え
て、NbとB成分の水酸化物沈殿を生成させる工程。A step of adding the solution generated in the step to the reaction vessel to form a hydroxide precipitate of Nb and the B component.
反応容器内で水熱反応を行わせる工程。 A step of causing a hydrothermal reaction in the reaction vessel.
濾過、洗浄および乾燥する工程。 Filtration, washing and drying.
粉末を仮焼および解砕する工程。 The step of calcining and crushing the powder.
なお、上記の一般式ABO3のAおよびBは下記の各元素
であり、Oは酸素である。Note that A and B in the above general formula ABO 3 are the following elements, respectively, and O is oxygen.
A:PbまたはPbとBa、Sr、Ca、La、Liの少なくとも一種類 B:NbとZn、Mg、Zr、Ti、Ni、Fe、W、Mnの少なくとも一
種類 このABO3で表される複合ペロブスカイト型酸化物の具
体的な組成をいくつか例示すれば、前記のPb(Mg1/3Nb
2/3)O3のほかに、下記のようなものがある。A: Pb or Pb and at least one kind of Ba, Sr, Ca, La, Li B: Nb and at least one kind of Zn, Mg, Zr, Ti, Ni, Fe, W, Mn Composite represented by this ABO 3 Some examples of the specific composition of the perovskite-type oxide will be described below. The Pb (Mg 1/3 Nb
2/3) In addition to O 3, there is something like the following.
Pb(Ni1/3Nb2/3)O3、Pb(Zn1/3Nb2/3)O3 Pb(Mg1/3Nb2/3)O3−PbTiO3−PbZrO3、 Pb(Fe1/2Nb1/2)O3、Pb(Co1/3Nb2/3)O3、 Pb(Ni1/3Nb2/3)O3−PbTiO3−PbZrO3、 Pb(Mg1/3Nb2/3)O3−PbTiO3 (作用) 第1図は、本発明方法の工程を模式的に示したもので
ある。以下:この図にそって説明する。Pb (Ni 1/3 Nb 2/3 ) O 3 , Pb (Zn 1/3 Nb 2/3 ) O 3 Pb (Mg 1/3 Nb 2/3 ) O 3 -PbTiO 3 -PbZrO 3 , Pb (Fe 1/2 Nb 1/2 ) O 3 , Pb (Co 1/3 Nb 2/3 ) O 3 , Pb (Ni 1/3 Nb 2/3 ) O 3 -PbTiO 3 -PbZrO 3 , Pb (Mg 1 / 3 ( Nb 2/3 ) O 3 —PbTiO 3 (Function) FIG. 1 schematically shows the steps of the method of the present invention. The following will be described with reference to this figure.
第1工程 Nbを含む溶液とNb以外のB成分を含む溶液とを混合し
て、反応させる。このときの反応温度は40〜80℃が望ま
しい。温度が低すぎると反応が遅く、高すぎると溶媒
(水、アルコールなど)の蒸発が多くなってよくない。First Step A solution containing Nb and a solution containing a component B other than Nb are mixed and reacted. The reaction temperature at this time is preferably from 40 to 80 ° C. If the temperature is too low, the reaction is slow, and if it is too high, the evaporation of the solvent (water, alcohol, etc.) increases, which is not good.
この反応に用いられる原料は、溶解性のものならば特
に制限はなく、例えば、塩化物、オキシ塩化物、硝酸
塩、炭酸塩、水酸化物および酢酸塩、シュウ酸塩、アル
コキシド等から選択される。通常は、水溶液として使用
されるが、水に難溶性の場合は、酸または適当な溶媒を
用いて可溶させればよく、不溶性原料の場合には、懸濁
溶液として使用することも可能である。The raw material used in this reaction is not particularly limited as long as it is soluble, and is selected from, for example, chlorides, oxychlorides, nitrates, carbonates, hydroxides and acetates, oxalates, alkoxides and the like. . Usually, it is used as an aqueous solution.If it is hardly soluble in water, it may be dissolved using an acid or a suitable solvent.In the case of an insoluble raw material, it can be used as a suspension solution. is there.
望ましい原料化合物としては、Nb2O、NbCl5、Pb(N
O3)2、PbO、Mg(NO3)2、MgCl2、TiCl4、TiO2、NiCl
2、Ni(NO3)2、Fe(NO3)3、FeCl3、CoCl2、Co(N
O3)2がある。Desirable starting compounds include Nb 2 O, NbCl 5 , Pb (N
O 3 ) 2 , PbO, Mg (NO 3 ) 2 , MgCl 2 , TiCl 4 , TiO 2 , NiCl
2 , Ni (NO 3 ) 2 , Fe (NO 3 ) 3 , FeCl 3 , CoCl 2 , Co (N
O 3 ) 2 .
この第1工程において、一般式ABO3のB成分を予め反
応させることが本発明方法の特徴のひとつである。即
ち、パイロクロア相の原因となるPbとNbの反応を抑制す
る目的で、NbがPbと接触する以前にNbと他のB成分の化
合物を生成させておくのである。In the first step, it is one of the features of the method of the present invention that the component B of the general formula ABO 3 is reacted in advance. That is, for the purpose of suppressing the reaction between Pb and Nb that causes the pyrochlore phase, compounds of Nb and other B components are generated before Nb comes into contact with Pb.
第2工程 この工程では、PbまたはPbと他のA成分の混合溶液
と、アルカリ金属水溶液、例えばKOH水溶液を反応させ
て水酸化物沈澱を生成させる。Second Step In this step, hydroxide precipitate is formed by reacting Pb or a mixed solution of Pb and another A component with an aqueous alkali metal solution, for example, an aqueous KOH solution.
第3工程 この工程では、第1工程で生成したNb−B成分系の均
一溶液を、第2工程で生成したPb−A成分系の水酸化物
沈澱およびアルカリ金属水溶液に添加し、つぎのような
反応によってNb−B成分系の水酸化物沈澱を生成させ
る。Third Step In this step, the homogeneous solution of the Nb-B component system produced in the first step is added to the hydroxide precipitate of the Pb-A component system produced in the second step and the aqueous alkali metal solution. The reaction produces a hydroxide precipitate of the Nb-B component system.
前記第1工程で、予めNb−B成分系化合物を生成させ
ているので、PbとNbの直接反応が抑制され、従って、パ
イロクロア相の生成がなくなりペロブスカイト単相の粉
末が得られる。In the first step, since the Nb-B component-based compound is generated in advance, the direct reaction between Pb and Nb is suppressed, and therefore, the generation of the pyrochlore phase is eliminated, and a perovskite single phase powder is obtained.
なお、第2工程と第3工程で使用するアルカリ金属水
溶液は、1〜15mol/の範囲の濃度の液であるのが好ま
しい。この濃度が高すぎると最終的に得られる粉末にア
ルカリ金属が残留して焼結性の悪化等の悪い影響を及ぼ
すことがある。The aqueous alkali metal solution used in the second and third steps is preferably a liquid having a concentration in the range of 1 to 15 mol /. If the concentration is too high, the alkali metal remains in the powder finally obtained, which may have adverse effects such as deterioration of sinterability.
第4工程 この工程は、水熱反応を起こさせる工程である。この
反応は、100〜200℃の温度と大気圧から15atm程度まで
の圧力の下で行わせるのがよい。Fourth step This step is a step for causing a hydrothermal reaction. This reaction is preferably carried out at a temperature of 100 to 200 ° C. and a pressure from atmospheric pressure to about 15 atm.
この第4工程が、本発明方法のもう一つの大きな特徴
である。仮に第4工程を省いて、次の第5、第6の工程
に進んでもペロブスカイト単相の粉末は得られ難い。こ
れは、組成の不均一性に起因すると思われる。This fourth step is another major feature of the method of the present invention. Even if the fourth step is omitted and the process proceeds to the next fifth and sixth steps, it is difficult to obtain a perovskite single-phase powder. This is believed to be due to compositional non-uniformity.
第5工程 この工程は、生成した沈澱物を濾過し洗浄したのち乾
燥する工程で、その条件は通常の条件でよい。Fifth Step This step is a step of filtering, washing, and drying the generated precipitate, and the conditions may be ordinary conditions.
第6工程 第5工程で得られた粉末を仮焼解砕する工程である。
仮焼は、前の工程で得られた粉末の結晶性の向上、すな
わちペロブスカイト相の割合の増大および粒度の調整の
ために実施されるものである。仮焼温度としては、余り
低いと仮焼の効果が不十分であり、また、過度に高いと
粉末が粗大化し、解砕によっても微細にならなくなる。
通常500〜1000℃の範囲が好ましい。Sixth step This is a step of calcining and pulverizing the powder obtained in the fifth step.
The calcination is performed to improve the crystallinity of the powder obtained in the previous step, that is, to increase the ratio of the perovskite phase and adjust the particle size. If the calcination temperature is too low, the effect of calcination is insufficient, and if it is excessively high, the powder becomes coarse and does not become fine even by crushing.
Usually, the range of 500 to 1000 ° C is preferable.
解砕は、仮焼において粗大化した粒子や凝集した粒子
を、例えば平均粒径で0.5μm程度に微細化するため実
施する。The disintegration is performed in order to reduce the particles coarsened or agglomerated in the calcination to, for example, about 0.5 μm in average particle diameter.
上記第1工程から第6工程までを経て製造された粉末
は、圧電体や誘導体の素子等の機能性セラミックス製造
用原料としてきわめて優れた特性を有している。The powder produced through the first to sixth steps has extremely excellent properties as a raw material for producing a functional ceramic such as a piezoelectric or derivative element.
Pb(Mg1/3Nb2/3)0.65Ti0.35O3の粉末を製造した実施
例を掲げる。An example in which a powder of Pb (Mg 1/3 Nb 2/3 ) 0.65 Ti 0.35 O 3 was produced will be described.
(工程) 硝酸マグネシウム〔Mg(NO3)2・6H2O〕18.4gを水10
0mlに溶解した水溶液に、四塩化チタン(TiCl4)の水溶
液(Ti分16.7%)31.gを混合して、室温で20分撹拌し、
マグネシウムとチタンの均一溶液を得た。この溶液に五
塩化ニオブ(NbCl5)36.9gを含むアルコール溶液60mlを
撹拌しつつ添加し、60℃で30分間反応させ、Mg−Ti−Nb
の均一溶液を生成させた。(Step) magnesium nitrate [Mg (NO 3) 2 · 6H 2 O ] was 18.4g water 10
To an aqueous solution dissolved in 0 ml, 31.g of an aqueous solution of titanium tetrachloride (TiCl 4 ) (Ti content: 16.7%) was mixed and stirred at room temperature for 20 minutes.
A homogeneous solution of magnesium and titanium was obtained. To this solution, 60 ml of an alcohol solution containing 36.9 g of niobium pentachloride (NbCl 5 ) is added with stirring, and the mixture is reacted at 60 ° C. for 30 minutes to obtain Mg-Ti-Nb
Yielded a homogeneous solution of
(工程) 水酸化カリウム(KOH)140gを水300mlに溶解した水溶
液に、硝酸鉛〔Pb(NO3)2〕133.0gを水250mlに溶解し
た水溶液を加えて、室温で30分間反応させて鉛の水酸化
物沈澱を生成させた。(Step) To an aqueous solution in which 140 g of potassium hydroxide (KOH) was dissolved in 300 ml of water, an aqueous solution in which 133.0 g of lead nitrate [Pb (NO 3 ) 2 ] was dissolved in 250 ml of water was added. Produced a hydroxide precipitate.
(工程) 工程で生成した沈澱を含む懸濁液に工程で生成し
た均一溶液を撹拌しつつ添加し、室温で30分間反応さ
せ、Mg−Ti−Nbの水酸化物沈澱を生成させた。(Step) The homogeneous solution formed in the step was added to the suspension containing the precipitate formed in the step while stirring, and reacted at room temperature for 30 minutes to form a hydroxide precipitate of Mg-Ti-Nb.
(工程) 上記の沈澱物を含む懸濁液をオートクレーブに移し
て、圧力8atm、温度180℃で5時間反応させ、目的の酸
化物を生成沈殿させた。(Step) The suspension containing the precipitate was transferred to an autoclave and reacted at a pressure of 8 atm and a temperature of 180 ° C. for 5 hours to produce and precipitate a target oxide.
(工程) 生成した沈澱物を濾過し、室温の水で充分洗浄した
後、120℃で15時間乾燥を行った。(Step) The generated precipitate was filtered, sufficiently washed with water at room temperature, and then dried at 120 ° C for 15 hours.
(工程) 工程で得られた粉末を、大気中800℃で2時間仮焼
し、ボールミルで解砕した。(Step) The powder obtained in the step was calcined in air at 800 ° C. for 2 hours, and was crushed by a ball mill.
以上の工程で得られた粉末〔Pb(Mg1/3Nb2/3)0.65Ti
0.35O3〕は、ほぼペロブスカイト単相であり、粒度が0.
5μm、総量約95gであった。The powder obtained by the above process [Pb (Mg 1/3 Nb 2/3 ) 0.65 Ti
0.35 O 3 ) is almost a single phase of perovskite and has a particle size of 0.
5 μm, total amount was about 95 g.
第2図は、上記実施例の方法で得られた粉末のX線回
折パターンである。FIG. 2 is an X-ray diffraction pattern of the powder obtained by the method of the above example.
比較例として本発明方法と異なる方法で製造した粉末
のX線回折パターンを第3図〜第5図に示す。この比較
例の製造条件は下記のとおりである。As comparative examples, X-ray diffraction patterns of powders produced by a method different from the method of the present invention are shown in FIGS. The manufacturing conditions of this comparative example are as follows.
(比較例1…第3図) PbO、MgO、TiO2、およびNb2O5を原料として、一般的
な固相法で1000℃×1時間の焼成を行い、実施例と同組
成の粉末を合成した。第3図はその粉末のX線回折パタ
ーンである。(Comparative Example 1 FIG. 3) Using PbO, MgO, TiO 2 , and Nb 2 O 5 as raw materials, firing was performed at 1000 ° C. for 1 hour by a general solid-phase method to obtain a powder having the same composition as that of the example. Synthesized. FIG. 3 is an X-ray diffraction pattern of the powder.
(比較例2…第4図) 実施例と同じ原料を使用して工程を実施せず、工程
でMg、Nb、Tiの溶液をそれぞれ別々に添加して合成
し、その外は実施例と同じに処理して粉末を得た。その
X線回折パターン第4図を示す。(Comparative Example 2 ... FIG. 4) The same raw materials as in the example were not used to carry out the process, but Mg, Nb, and Ti solutions were separately added in the process and synthesized. To obtain a powder. FIG. 4 shows the X-ray diffraction pattern.
(比較例3…第5図) 実施例と同じ原料を使用して、工程を実施せず、そ
の外の条件は実施例と同じにして粉末を製造した。その
粉末のX線回折パターンが第5図である。(Comparative Example 3 FIG. 5) A powder was produced using the same raw materials as in the example, without performing the steps, and under the same other conditions as in the example. FIG. 5 shows an X-ray diffraction pattern of the powder.
第1表に、上記の実施例と比較例で合成した粉末の粒
度とペロブスカイト化率を示す。Table 1 shows the particle sizes and perovskite conversion rates of the powders synthesized in the above Examples and Comparative Examples.
ペロブスカイト化率は第2図〜第5図のX線回折パタ
ーンから、ペロブスカイトの(110)面のピーク強度IPe
とパイロクロアの(222)面のピーク強度IPyより で評価した。From the X-ray diffraction patterns shown in FIGS. 2 to 5, the perovskite conversion rate was determined from the peak intensity I Pe of the (110) plane of the perovskite.
And Pyrochlore (222) peak intensity I Py Was evaluated.
なお、第1表の実施例1というのは、前記実施例で得
た粉末であり、実施例2〜4は同じようにして得た組成
の異なる粉末である。 Example 1 in Table 1 is the powder obtained in the above example, and Examples 2 to 4 are powders obtained in the same manner and having different compositions.
第1表から明らかなように、本発明の実施例で得られ
た粉末は、ほぼペロブスカイト単相であり、しかも粒径
が0.5μm以下と微細である。As is clear from Table 1, the powder obtained in the examples of the present invention is almost a single phase of perovskite, and has a fine particle size of 0.5 μm or less.
比較例では、ペロブスカイト単相の粉末は得られず、
粒径が比較的小さな比較例2のものはペロブスカイト化
率が著しく悪い。In the comparative example, a perovskite single phase powder was not obtained,
In Comparative Example 2 having a relatively small particle size, the perovskite conversion rate is extremely poor.
(発明の効果) 本発明方法は、近年用途が拡大している一般式ABO3の
ペロブスカイト型複合酸化物のうち、特にB成分として
Nbを含むものの製造に好適である。この方法によれば、
パイロクロア相の生成が抑制されペロブスカイト単相の
微細な粉末が製造できる。(Effect of the Invention) The method of the present invention is particularly useful as a component B among the perovskite-type composite oxides of the general formula ABO 3 whose use is expanding in recent years.
It is suitable for the production of those containing Nb. According to this method,
The formation of a pyrochlore phase is suppressed, and a fine powder of a perovskite single phase can be produced.
本発明は、物性の優れたセラミックス誘電体、圧電体
等の製造に大きな寄与をなすものである。The present invention makes a great contribution to the production of ceramic dielectrics, piezoelectrics, and the like having excellent physical properties.
第1図は、本発明方法の工程を説明する図、 第2図は、本発明の実施例で得られた粉末のX線回折パ
ターン、 第3図、第4図および第5図は、比較例で得られた粉末
のX線回折パターン、 である。FIG. 1 is a view for explaining the steps of the method of the present invention, FIG. 2 is an X-ray diffraction pattern of the powder obtained in an example of the present invention, FIG. 3, FIG. 4 and FIG. 3 is an X-ray diffraction pattern of the powder obtained in the example.
Claims (1)
だしAは:PbまたはPbとBa、Sr、Ca、La、Liの少なくと
も一種類の成分であり、Bは、NbとZn、Mg、Zr、Ti、N
i、Fe、W、Mnの少なくとも一種類の成分であり、Oは
酸素である)で表される複合ペロブスカイト型酸化物粉
末の製造方法。 Nbを含む溶液と他のB成分の少なくとも一種類を含
む溶液を混合し反応させ、NbとB成分の均一溶液を生成
させる工程。 反応容器内で、PbまたはPbと他のA成分の少なくと
も一種類を含む溶液をアルカリ金属水溶液と反応させ
て、PbまたはPbと他のA成分の水酸化物沈殿を生成させ
る工程。 上記反応容器内にの工程で生成させた溶液を加え
て、NbとB成分の水酸化物沈殿を生成させる工程。 反応容器内で水熱反応を行わせる工程。 濾過、洗浄および乾燥する工程。 粉末を仮焼および解砕する工程。1. A general formula ABO 3 comprising the following steps (where A is: Pb or at least one component of Pb and Ba, Sr, Ca, La, Li; B is Nb, Zn, Mg , Zr, Ti, N
i is a component of at least one of Fe, W, and Mn, and O is oxygen). A step of mixing and reacting a solution containing Nb and a solution containing at least one other component B to generate a uniform solution of Nb and the component B; A step of causing Pb or a solution containing at least one of Pb and another A component to react with an aqueous alkali metal solution in a reaction vessel to generate a hydroxide precipitate of Pb or Pb and another A component. A step of adding the solution generated in the step in the reaction vessel to form a hydroxide precipitate of Nb and B components. A step of causing a hydrothermal reaction in the reaction vessel. Filtration, washing and drying. The step of calcining and crushing the powder.
Priority Applications (1)
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JP34039689A JP2866416B2 (en) | 1989-12-28 | 1989-12-28 | Method for producing perovskite-type composite oxide powder |
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JP34039689A JP2866416B2 (en) | 1989-12-28 | 1989-12-28 | Method for producing perovskite-type composite oxide powder |
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JPH03199123A JPH03199123A (en) | 1991-08-30 |
JP2866416B2 true JP2866416B2 (en) | 1999-03-08 |
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- 1989-12-28 JP JP34039689A patent/JP2866416B2/en not_active Expired - Fee Related
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