JPS61186219A - Production of lead-containing fine powder - Google Patents
Production of lead-containing fine powderInfo
- Publication number
- JPS61186219A JPS61186219A JP60024438A JP2443885A JPS61186219A JP S61186219 A JPS61186219 A JP S61186219A JP 60024438 A JP60024438 A JP 60024438A JP 2443885 A JP2443885 A JP 2443885A JP S61186219 A JPS61186219 A JP S61186219A
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- JP
- Japan
- Prior art keywords
- lead
- powder
- fine powder
- precipitant
- precipitate
- 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.)
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Abstract
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明は易焼結性鉛含有微粉末の製造法に関する。[Detailed description of the invention] (Industrial application field) The present invention relates to a method for producing easily sinterable lead-containing fine powder.
一般的に鉛含有酸化物には、強誘電材料・圧電材料・焦
電（Ａ料など■レフ１−ロセラミツクスとして有用なも
のが多い。In general, many lead-containing oxides are useful as ferroelectric materials, piezoelectric materials, pyroelectric materials (A materials, etc.), and are useful as ref.1-roceramics.
エレクトロセラミック部品の小型化、高性能化に伴い高
純度で粒径分布の狭い反応性の高い微粉末原料に対する
要求が高まっている。たとえばドクターブレード法など
により薄膜を形成する際には、表面粗さなどを改善し、
また膜の品質向上のために優れた微粉末を必要とするか
らである。As electroceramic components become smaller and more sophisticated, there is an increasing demand for highly reactive fine powder raw materials with high purity and narrow particle size distribution. For example, when forming a thin film using the doctor blade method, it is necessary to improve the surface roughness, etc.
This is also because excellent fine powder is required to improve the quality of the film.
（従来の技術）
従来、鉛含有酸化物粉末の製造方法としては、鉛含有酸
化物を構成すべき各種金属を含有する酸化物、炭酸塩な
どの化合物粉末を目的組成となるように秤量混合後、仮
焼し、さらに粉砕仮焼による固相反応を何度も繰り返し
て製造するいわゆる同相法がある。(Prior art) Conventionally, a method for producing lead-containing oxide powder involves weighing and mixing compound powders such as oxides and carbonates containing various metals that should constitute the lead-containing oxide so as to have the desired composition. There is a so-called in-phase method in which a solid phase reaction involving calcination, pulverization, and calcination is repeated many times.
この方法では粉砕時に混入する不純物のために高純度の
粉末の製造が困難であった。また粉砕によって効率よく
製造できる粉末の粒径は、数μｍ程度が限界であり、し
かもその粒径も不均一となりやすく反応性に劣る欠点が
あった。With this method, it was difficult to produce highly pure powder due to impurities mixed in during pulverization. Furthermore, the particle size of the powder that can be efficiently produced by pulverization is limited to a few micrometers, and the particle size tends to be non-uniform, resulting in poor reactivity.
これらの同相法の欠点を改良する方法どして、溶液を出
発原料どして粉末を製造する共沈法が知られていて、こ
の方法によれば一般に粒度分布の狭い微粉末が得られる
利点はある。Co-precipitation is a known method for improving the disadvantages of these in-phase methods, in which powder is produced using a solution as a starting material.This method generally has the advantage of producing fine powder with a narrow particle size distribution. There is.
（発明が解決しようとＪ−る問題点）
鉛含有微粉末の調製に有用な共沈法の適用についても、
鉛含有酸化物を構成すべぎ金属のうち、たとえばＭＯな
どは、出発原料溶液中に生成させる沈澱の溶解度が大き
いので溶出によって目的組成が得られ動く沈澱ｐＨを１
２程度まで高める必要があり、この際水酸化す］〜リウ
ムの如ぎを用いれば高ｐ ｌ−１を保持できるわ【プで
はあるが不純物としてのＮａｈ曹昆入する欠点を伴いま
た、カヂオン不純物を入れないめにはアンモニア水など
を用いるを可とするがアンモニア水で保持できる１１
＋−１は高々ｒｌ１１１０，５程度が限界であるため溶
出を防ぐには不充分であった。(Problems to be solved by the invention) Regarding the application of coprecipitation method useful for preparing lead-containing fine powder,
Among the metals that should constitute the lead-containing oxide, for example, MO has a high solubility in the precipitate formed in the starting material solution, so the desired composition can be obtained by elution, and the pH of the moving precipitate can be reduced to 1.
It is necessary to increase the concentration to about 2, and in this case, if hydroxide is used, a high p l-1 can be maintained. To prevent impurities from entering, it is possible to use ammonia water, but ammonia water can hold it11.
+-1 had a limit of about rl1110.5, which was insufficient to prevent elution.
このような動点についての有効な解決を与えることが本
発明の目的である。It is an object of the present invention to provide an effective solution for such moving points.
（問題点を解決覆るための手段）
発明者ら゛は共沈する際に溶出しやすい成分を含有する
鉛含有酸化物微粉末の製造方法について研究を行い、本
発明に到達した。(Means for solving and overcoming the problems) The inventors conducted research on a method for producing a lead-containing oxide fine powder containing components that are easily eluted during coprecipitation, and arrived at the present invention.
鉛含有微粉末の製造にあたって、
鉛含有酸化物を構成すべき各種金属を含有する酸性の溶
液及び／又は懸濁液を、沈澱助剤の存在下に、沈澱剤と
反応させ、得られた沈澱物を４５０〜１２００℃で仮焼
して粉末を１ｑる工程、前記工程で得られた粉末に鉛化
合物粉末を添加混合する工程および
前記各工程を経て得られた粉末混合物を温度６００〜１
０００℃で焼成する工程の
各工程を結合することを特徴とする鉛含有微粉末の製造
法である。In producing lead-containing fine powder, an acidic solution and/or suspension containing various metals to constitute the lead-containing oxide is reacted with a precipitant in the presence of a precipitation aid, and the resulting precipitate is A step of calcining the product at 450 to 1200°C to obtain 1 q of powder, a step of adding and mixing lead compound powder to the powder obtained in the above step, and a step of heating the powder mixture obtained through each of the above steps to a temperature of 600 to 1 q.
This is a method for producing lead-containing fine powder, which is characterized by combining the steps of firing at 000°C.
本発明でいう鉛含有酸化物を構成すべき各種金属の具体
例としてはＰｂ、Ｚｒ、Ｔｉ 、ｔＶｌｏ。Specific examples of various metals constituting the lead-containing oxide in the present invention include Pb, Zr, Ti, and tVlo.
Ｎｂ、Ｍｎ、Ｓｎ、Ｚｎ、Ｓｂ、ＡＡ、Ｆｅ。Nb, Mn, Sn, Zn, Sb, AA, Fe.
Ｔａ、Ｃｏ、Ｎｉ、Ｂｉ、Ｗ、ｌｉ、ｓｒ、Ｂａ。Ta, Co, Ni, Bi, W, li, sr, Ba.
Ｃａ、Ｓｅ、Ｌａ、Ｃｕ、Ｙ、Ｙｌｌ、ｌｅ、Ｒ８゜Ｃ
ｄおよびＩｎなどがあげられる。Ca, Se, La, Cu, Y, Yll, le, R8°C
Examples include d and In.
鉛含有酸化物を構成すべき各種金属成分を含有する酸性
の溶液としては特に限定されないが、その例としては硝
酸溶液、塩酸溶液、硫酸溶液などの無機酸溶液、しゆう
酸溶液、ぎ酸溶液などの有機酸溶液またはこれらの混合
溶液などがあげられる。Acidic solutions containing various metal components that should constitute lead-containing oxides are not particularly limited, but examples include inorganic acid solutions such as nitric acid solutions, hydrochloric acid solutions, and sulfuric acid solutions, oxalic acid solutions, and formic acid solutions. Examples include organic acid solutions such as and mixed solutions thereof.
溶液の調製法としては、各種塩類を水に溶解する一般的
方法が用いられる。As a method for preparing the solution, a general method of dissolving various salts in water is used.
次に本発明でいう懸濁液とは、液体中に固体粒子が均一
に分散しているものを指し、たとえば微細な沈澱粒子が
均一に分散したゾル状液などがあげられる。Next, the suspension as used in the present invention refers to a liquid in which solid particles are uniformly dispersed, and includes, for example, a sol-like liquid in which fine precipitated particles are uniformly dispersed.
次に沈澱助剤としては、メタノール、エタノールなどの
アルコール類アセ１〜ンなどのケｉ〜ン類、ベンゼント
ルエン、キシレン、トリクレン、クロロセン、過酸化水
素水などがあげられるが、沈澱物の溶解度を低下させる
物質であれば適用可能である。なお沈澱助剤は、上掲し
たところのうち１種又は２種以上を混合して用い１ｑる
。Next, examples of precipitation aids include alcohols such as methanol and ethanol, alcohols such as acetone, benzene toluene, xylene, trichlene, chlorocene, hydrogen peroxide, etc., but the solubility of the precipitate It is applicable to any substance that reduces the The precipitation aid is used in an amount of 1 q of the above-mentioned ones or a mixture of two or more.
沈澱助剤の添加量は、鉛含有酸化物を構成すべき各種金
属を含有する酸性の溶液及び／又は懸濁液に含まれる金
属成分によって異なるが、金属成分の９５モル％以上が
沈澱する量が適当であり、一般に沈澱生成槽内の内容物
量（容量）の６０容量％以下、好ましくは１０〜５０容
量％である。この添加量は沈澱剤との反応ｐＨによって
もかわるが一般にｐＨが低いほど溶出を防ぐ！こめに必
要な添加量は増加する。The amount of precipitation aid added varies depending on the metal components contained in the acidic solution and/or suspension containing various metals that are to constitute the lead-containing oxide, but it should be an amount that precipitates 95 mol% or more of the metal components. is appropriate, and is generally 60% by volume or less, preferably 10 to 50% by volume of the content (volume) in the precipitation tank. The amount added varies depending on the pH of the reaction with the precipitant, but in general, the lower the pH, the more the elution is prevented! The amount of addition required for rice increases.
次に沈澱剤としては、アンモニア水などの無機塩基、炭
酸アンモニウム、しゆう酸アンモニウムなどの各種塩類
やメチルアミン、エチルアミンなどの有機塩基などがあ
げられる。Examples of the precipitant include inorganic bases such as aqueous ammonia, various salts such as ammonium carbonate and ammonium oxalate, and organic bases such as methylamine and ethylamine.
反応ｐＨは５．５以上が好ましくｐＨ７以上がさらに好
ましい。The reaction pH is preferably 5.5 or higher, more preferably 7 or higher.
ｐｌ−１の上限についてはたとえばアンモニア水で効率
的に維持できるｐＨの上限は１０．５程度である。Regarding the upper limit of pl-1, for example, the upper limit of pH that can be efficiently maintained with aqueous ammonia is about 10.5.
共沈方法としては、沈澱助剤及び沈澱剤でｐ ＋−＋を
保持した共沈槽内に充分攪拌を行ないながら、鉛含有酸
化物を構成すべき各種金属を含有する酸性の溶液及び／
又は懸濁液をｌＩＮ霧するなどの方法で導入する方法が
好ましい。As for the coprecipitation method, an acidic solution containing various metals to constitute the lead-containing oxide and/or is placed in a coprecipitation tank in which p +-+ is maintained with a precipitation aid and a precipitant, with sufficient stirring.
Alternatively, it is preferable to introduce the suspension by a method such as lIN atomization.
かくして得られる沈澱物はろ過などの方法によって溶液
部分を除去する。 ”
沈澱物の洗浄は沈澱生成ど同−条件又はそれよりもｐ
Ｈの高い沈澱剤及び／又は沈澱助剤を含む水溶液を用い
ることが洗浄工程中の溶出を防ぐため好ましい。The solution portion of the precipitate thus obtained is removed by a method such as filtration. ” Cleaning of the precipitate should be carried out under the same conditions as the precipitate formation, or even better.
It is preferable to use an aqueous solution containing a precipitant and/or precipitation aid with high H content in order to prevent elution during the washing step.
洗浄は沈澱物中の０℃−やＮＯｓ ”’などの不純物を
除去するため充分性なうことが望ましく、また不純物除
去後、エタノールやアｔ？ ｌ−ンなとで洗浄すること
によって沈澱粒子同志の凝集を防ぐことも有効である。It is desirable that the washing be sufficient to remove impurities such as 0°C and NOs in the precipitate, and after removing the impurities, the precipitated particles can be removed by washing with ethanol or atmospheric water. It is also effective to prevent comrades from clumping together.
乾燥を行なう場合の方法としては通常の加熱乾燥、真空
乾燥の他噴霧乾燥方法、振動流動乾燥法、ドラムドライ
Ａ７−乾燥法、フィルムエバポレーター乾燥法などの方
法がある。Drying methods include conventional heating drying, vacuum drying, spray drying, vibration fluidized drying, drum drying A7-drying, film evaporator drying, and the like.
粉末同志の凝集を防ぐことは微粉末を得る際に重要であ
るがこの点仮焼の前及び／又は後にボールミル、振動ボ
ールミル、ジェットミルなどによる解砕を行なうことは
有効である。Preventing agglomeration of powders is important when obtaining fine powder, and in this respect it is effective to perform crushing using a ball mill, vibrating ball mill, jet mill, etc. before and/or after calcination.
仮焼温度は４５０℃より低い温度のとき沈澱物中の水分
などの除去が不充分であり次に述べる工程において秤量
仕込みする際に目的組成とすることが回動となる。また
、１２００℃より高い場合には粉末同志の焼結などによ
る凝集が起こり反応性が低下覆る訓点があり、またエネ
ルギー的にも高温での仮焼は実際的でない。When the calcination temperature is lower than 450°C, removal of moisture in the precipitate is insufficient, and rotation is required to achieve the desired composition when weighing and charging in the next step. Further, if the temperature is higher than 1200° C., agglomeration occurs due to sintering of powders, resulting in decreased reactivity, and calcining at high temperatures is not practical in terms of energy.
従って仮焼温度は４５０〜１２００℃が好ましり６００
〜１０００℃がさらに好ましい。Therefore, the calcination temperature is preferably 450 to 1200°C.
-1000 degreeC is more preferable.
次の工程で用いる鉛化合物としては、酸化鉛（ＰＩ）
０． ＰＩ］ ３０４ ） 、炭酸鉛、塩基性炭酸鉛水
酸化鉛、しゆう酸鉛、ぎ酸鉛などが挙げられる。The lead compound used in the next step is lead oxide (PI).
0. PI] 304), lead carbonate, basic lead carbonate, lead hydroxide, lead oxalate, lead formate, and the like.
鉛化合物粉末の粉末特性としては、混合性のよい微粉末
が好ましい。Regarding the powder characteristics of the lead compound powder, a fine powder with good mixability is preferable.
混合方法としては通常使用される方法、例えば乳鉢やボ
ールミルなどの混合機によることができる。なお乾式混
合」；りもアルコール、アセ１〜ンなどを用いた湿式混
合の方が効率も良く好ましい。The mixing method may be a commonly used method, for example, using a mixer such as a mortar or a ball mill. Note that wet mixing using limo alcohol, acetin, etc. is more efficient and preferable.
鉛化合物粉末の混合量は目的とする相を形成する化学問
論量よりも８モル％以下の過剰量を混合することが目的
とする組形成のため及び粉末の反応性を高めるために有
効である。The amount of lead compound powder to be mixed is 8 mol% or less in excess of the chemical stoichiometric amount to form the desired phase, which is effective for forming the desired group and increasing the reactivity of the powder. be.
次に焼成工程の処理温度が６００℃より低いと反応の効
率が低く一方１０００℃より高い温度では鉛化合物が融
解などを起こしやすく粉末同志の固い凝集を形成しやす
く微粉末となりにくい。したがって焼成温度は６００〜
１０００ ’Ｃを要し、そのうち７００〜９００℃がよ
り好ましくなかでも７５０〜８５０℃が一層好ましい。Next, if the treatment temperature in the firing step is lower than 600°C, the efficiency of the reaction will be low, while if the temperature is higher than 1000°C, the lead compound will easily melt and form hard agglomerates of powders, making it difficult to form fine powders. Therefore, the firing temperature is 600~
1000'C, more preferably 700-900°C, and most preferably 750-850°C.
（実施例）
実施例１
金属濃度１．０２モル／βの塩化ジルコニル水溶液と金
属濃度１．６３モル／βの四塩化チタン水溶液を、Ｚｒ
：丁１の原子比で０，１２５ ： ０，４３７５とな
るように混合し、該溶液に金属ＭＯ粉末及び金属Ｍｎ粉
末をｒ： ：ＭＯ：Ｍｎの原子比で３０：１０：１と
なるように攪拌しながら加え、紫色溶液を得た。(Example) Example 1 A zirconyl chloride aqueous solution with a metal concentration of 1.02 mol/β and a titanium tetrachloride aqueous solution with a metal concentration of 1.63 mol/β were mixed with Zr.
:Mn is mixed in an atomic ratio of 0,125:0,4375, and the metal MO powder and metal Mn powder are mixed in the solution so that the atomic ratio of :MO:Mn is 30:10:1. was added to the solution with stirring to obtain a purple solution.
これとは別に水酸化ニオブ沈澱を用いて金属製８一
度０．４２２ｍ０１ ／βのニオブのしゆう耐酸性溶液
を調製した。Separately, an acid-resistant solution of niobium of 0.422 m01/β was prepared using niobium hydroxide precipitate.
このニオブのしゆう耐酸性溶液中のニオブ金属１モルに
対してしゆう酸三水和物（Ｈ２Ｃ２０４・２Ｈ２０）を
３９０ｇの割合でニオブのしゆう耐酸性溶液に添加し、
さらに前記Ｚｒ 、Ｔｉ 、Ｍ（］およびＭｎを含む紫
色溶液をＮｂ：ＭＵの原子比で２：１となるように添加
し茶褐色溶液を得た。Adding 390 g of oxalic acid trihydrate (H2C204.2H20) to the acid-resistant solution of niobium per mole of niobium metal in the acid-resistant solution of niobium,
Further, the purple solution containing Zr 2 , Ti 2 , M(] and Mn was added at an atomic ratio of Nb:MU of 2:1 to obtain a brownish brown solution.
この溶液をエタノール（沈澱助剤）及びアンモニア水（
沈澱剤）でｐ ｌ−１９，０に保持された共沈槽内に攪
拌しながら噴霧して沈澱を生成させた。このときのエタ
ノール（沈澱助剤）の添加量は、共沈槽内の内容物に対
して５０容量％であった。This solution was mixed with ethanol (precipitation aid) and aqueous ammonia (
The mixture was sprayed with stirring into a co-precipitation tank maintained at PL-19.0 using a precipitant (precipitant) to form a precipitate. The amount of ethanol (precipitation aid) added at this time was 50% by volume based on the content in the coprecipitation tank.
生成した沈澱をろ過し、次にエタノール５０容量％を含
むｐＨ１ｉのアンモニア水を用いて洗浄し、得られた沈
澱物を温度８０℃で乾燥した。The generated precipitate was filtered and then washed with aqueous ammonia of pH 1i containing 50% by volume of ethanol, and the resulting precipitate was dried at a temperature of 80°C.
ろ液中に溶出する金属成分を分析したが溶出は認められ
なかった。乾燥物を解砕後、温度９００℃で１時間仮焼
して粉末を得た。この粉末を走査型電子顕微鏡で観察し
たところ粒径０．３μｍ程度のそろった微粉末であった
。The metal components eluted into the filtrate were analyzed, but no elution was observed. After crushing the dried material, it was calcined at a temperature of 900° C. for 1 hour to obtain a powder. When this powder was observed with a scanning electron microscope, it was found to be a fine powder with a uniform particle size of about 0.3 μm.
この粉末９６．２６００（］に対して酸化鉛（Ｐｂ ０
）２２３．２０００（］をアセ］・ンを用いて湿式混合
したのち温度７８０℃で１時間焼成して鉛含有酸化物粉
末を得た。この粉末は走査型電子顕微鏡観察の結果０．
３μｍ程度の非常に粒度のそろった微粉末であつ １．
：。Lead oxide (Pb 0
)223.2000() was wet mixed using ace]・n and then calcined at a temperature of 780°C for 1 hour to obtain a lead-containing oxide powder.As a result of scanning electron microscopy observation, this powder had a lead-containing oxide powder.
It is a fine powder with a very uniform particle size of about 3 μm. 1.
:.
また不純物分析を行なったところ炭素、塩素及び不純物
金属は１０ｐｐｍ以下で高純度であることが判明した。Further, an impurity analysis revealed that carbon, chlorine, and impurity metals were 10 ppm or less, indicating high purity.
この粉末の反応性を評価するためにこの微粉末３．０ｇ
を成形圧力１０００Ｋ （］ ／ ｃｉで直径２０ｍｍ
φのディスク状に成形し、温度１１５０℃で１時間焼結
を行なった。3.0g of this fine powder to evaluate the reactivity of this powder.
Molding pressure 1000K (] / ci and diameter 20mm
It was formed into a disk shape of φ and sintered at a temperature of 1150° C. for 1 hour.
その結果、焼結密度は７，９４ （］ ／ ｃＩｌｌで
あり、はぼ理論密度の焼結体を得た。As a result, the sintered body had a sintered density of 7.94 (]/cIll, which was approximately the theoretical density).
比較例１
実施例１においてエタノール（沈澱助剤）を添加しない
以外は同様にして沈澱を生成させた。ろ液を分析したと
ころＭ（＋が２６モル％溶出していることがわかった。Comparative Example 1 A precipitate was produced in the same manner as in Example 1 except that ethanol (precipitation aid) was not added. Analysis of the filtrate revealed that 26 mol% of M(+ was eluted.
このように沈澱助剤を加えない場合には多量の溶出があ
り目的組成とすることはできない。As described above, if a precipitation aid is not added, a large amount of elution occurs and the desired composition cannot be obtained.
実施例２
実施例１で用い！：Ｚｒ 、Ｔｉ 、Ｍ（１、Ｍｎおよ
びＮｂを含む茶褐色溶液にざらに金属濃度１．０１モル
／βの塩化ストロンチウム水溶液をＺｒ：Ｓｒの原子比
で０．１２５ ： ０，０５となる」；うに混合して
溶液を調製した。Example 2 Used in Example 1! : Zr, Ti, M (1, strontium chloride aqueous solution with a metal concentration of 1.01 mol/β is added to a brown solution containing Mn and Nb at a Zr:Sr atomic ratio of 0.125: 0.05); A solution was prepared by mixing the sea urchins.
これにより実施例１と同一の操作でＺｒ、Ｔｉ。As a result, Zr and Ti were obtained by the same operation as in Example 1.
Ｍｆｌ 、 Ｍｎ 、 ＮｌｌおよびＳｒを含む仮焼粉
末を得！こ 。Obtain calcined powder containing Mfl, Mn, Nll and Sr! child .
この場合も沈澱生成の際のる液中の金属成分の溶出は認
められなかった。In this case as well, no elution of metal components from the liquid during precipitation formation was observed.
得られた粉末は粒径０．３μｍ程度の粒度のそろった微
粉末であつＩＣ６
この微粉末１０１．４４１ｇに対して一酸化鉛（Ｐｂ
Ｏ） ２１２．０４００（］をアセトンを用いて湿式
混合したのち温度１８０℃で１時間焼成して鉛含有酸化
物微粉末を得た。The obtained powder is a fine powder with a uniform particle size of about 0.3 μm, and has an IC6 value of lead monoxide (Pb) per 101.441 g of this fine powder.
O) 212.0400() was wet-mixed using acetone and then fired at a temperature of 180° C. for 1 hour to obtain a lead-containing oxide fine powder.
この粉末の特性は実施例１とほぼ同様であった。The properties of this powder were almost the same as in Example 1.
（発明の効果）
本発明は沈澱生成時に沈澱助剤を用いることにより従来
アンモニア水などの沈澱剤だけでは沈澱生成が困難であ
ったアルカリ土類金属などを含む原液から効率的に沈澱
を生成することが可能である。従って高純度で組成の均
一性の高い粒径の均一な易焼結性鉛含有酸化物微粉末が
得られる。(Effects of the Invention) By using a precipitation aid during precipitation generation, the present invention can efficiently produce a precipitate from a stock solution containing alkaline earth metals, etc., which was previously difficult to produce using only a precipitant such as aqueous ammonia. Is possible. Therefore, easily sinterable lead-containing oxide fine powder with high purity, highly uniform composition, and uniform particle size can be obtained.
Claims (1)
に、沈澱剤と反応させ、得られた沈澱物を４５０〜１２
００℃で仮焼して粉末を得る工程、 前記工程で得られた粉末に鉛化合物粉末を 添加混合する工程および 前記各工程を経て得られた粉末混合物を温 度６００〜１０００℃で焼成する工程 の各工程を結合することを特徴とする鉛含有微粉末の製
造法。[Claims] 1. In the production of lead-containing fine powder, an acidic solution and/or suspension containing various metals to constitute a lead-containing oxide is added to a precipitating agent in the presence of a precipitating agent. The precipitate obtained was reacted with 450-12
A step of calcining at 00°C to obtain a powder, a step of adding and mixing lead compound powder to the powder obtained in the above step, and a step of firing the powder mixture obtained through each of the above steps at a temperature of 600 to 1000°C. A method for producing lead-containing fine powder, which is characterized by combining each process.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60024438A JPS61186219A (en) | 1985-02-13 | 1985-02-13 | Production of lead-containing fine powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60024438A JPS61186219A (en) | 1985-02-13 | 1985-02-13 | Production of lead-containing fine powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61186219A true JPS61186219A (en) | 1986-08-19 |
| JPH0251847B2 JPH0251847B2 (en) | 1990-11-08 |
Family
ID=12138149
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60024438A Granted JPS61186219A (en) | 1985-02-13 | 1985-02-13 | Production of lead-containing fine powder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61186219A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61232217A (en) * | 1985-04-08 | 1986-10-16 | Natl Inst For Res In Inorg Mater | Production of low-temperature sinterable powdery raw material for producing dielectric ceramic |
| JPS63156054A (en) * | 1986-12-17 | 1988-06-29 | 株式会社デンソー | Manufacture of polycomponent ceramics |
| JPS63156056A (en) * | 1986-12-17 | 1988-06-29 | 株式会社デンソー | Manufacture of high permittivity ceramics |
| JPS63233036A (en) * | 1987-03-23 | 1988-09-28 | 科学技術庁無機材質研究所長 | Manufacture of polycomponent ceramics |
| JPS63248774A (en) * | 1987-04-03 | 1988-10-17 | 科学技術庁無機材質研究所長 | Manufacture of polycomponent ceramics |
| JPS63291844A (en) * | 1987-05-26 | 1988-11-29 | Nippon Denso Co Ltd | Production of optical ceramics |
| JPS63291843A (en) * | 1987-05-26 | 1988-11-29 | Nippon Denso Co Ltd | Production of optical ceramics |
| JPS6479060A (en) * | 1987-09-22 | 1989-03-24 | Mitsui Mining & Smelting Co | Production of compound oxide ceramics |
| JPH01259583A (en) * | 1988-04-11 | 1989-10-17 | Mitsui Toatsu Chem Inc | Synthesis of pb-ba-zr-ti uniform oxide powder |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6153119A (en) * | 1984-08-21 | 1986-03-17 | Denki Kagaku Kogyo Kk | Lead-containing oxide powder and its preparation |
-
1985
- 1985-02-13 JP JP60024438A patent/JPS61186219A/en active Granted
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6153119A (en) * | 1984-08-21 | 1986-03-17 | Denki Kagaku Kogyo Kk | Lead-containing oxide powder and its preparation |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61232217A (en) * | 1985-04-08 | 1986-10-16 | Natl Inst For Res In Inorg Mater | Production of low-temperature sinterable powdery raw material for producing dielectric ceramic |
| JPS63156054A (en) * | 1986-12-17 | 1988-06-29 | 株式会社デンソー | Manufacture of polycomponent ceramics |
| JPS63156056A (en) * | 1986-12-17 | 1988-06-29 | 株式会社デンソー | Manufacture of high permittivity ceramics |
| JPS63233036A (en) * | 1987-03-23 | 1988-09-28 | 科学技術庁無機材質研究所長 | Manufacture of polycomponent ceramics |
| JPS63248774A (en) * | 1987-04-03 | 1988-10-17 | 科学技術庁無機材質研究所長 | Manufacture of polycomponent ceramics |
| JPS63291844A (en) * | 1987-05-26 | 1988-11-29 | Nippon Denso Co Ltd | Production of optical ceramics |
| JPS63291843A (en) * | 1987-05-26 | 1988-11-29 | Nippon Denso Co Ltd | Production of optical ceramics |
| JPS6479060A (en) * | 1987-09-22 | 1989-03-24 | Mitsui Mining & Smelting Co | Production of compound oxide ceramics |
| JPH01259583A (en) * | 1988-04-11 | 1989-10-17 | Mitsui Toatsu Chem Inc | Synthesis of pb-ba-zr-ti uniform oxide powder |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0251847B2 (en) | 1990-11-08 |
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| EXPY | Cancellation because of completion of term |