JPH09255337A - Alkaline earth metal titanate powder and method for producing the same - Google Patents

Alkaline earth metal titanate powder and method for producing the same

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Publication number
JPH09255337A
JPH09255337A JP8060952A JP6095296A JPH09255337A JP H09255337 A JPH09255337 A JP H09255337A JP 8060952 A JP8060952 A JP 8060952A JP 6095296 A JP6095296 A JP 6095296A JP H09255337 A JPH09255337 A JP H09255337A
Authority
JP
Japan
Prior art keywords
powder
earth metal
alkaline earth
heating
tio
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.)
Pending
Application number
JP8060952A
Other languages
Japanese (ja)
Inventor
Kenji Azuma
健司 東
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kubota Corp
Original Assignee
Kubota Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kubota Corp filed Critical Kubota Corp
Priority to JP8060952A priority Critical patent/JPH09255337A/en
Publication of JPH09255337A publication Critical patent/JPH09255337A/en
Pending legal-status Critical Current

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  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

PROBLEM TO BE SOLVED: To provide an alkaline earth metal titanate (RTiO3 ) powder useful as a friction and abrasive material, a resin reinforcing material, a filler for coating material or the like and the producing method. SOLUTION: The alkaline earth metal titanate powder is composed of a spherical particle produced by sintering a unit particle having 0.5-5μm average particle diameter and the diameter of the spherical particle is 10-1000μm. The powder is produced by using TiO2 or a titanium compound producing TiO2 by heating, a RO (R is an alkaline earth metal) or an alkaline earth metal compound producing RO by heating and an alkali metal compound of a flux component as raw materials, dry-mix-granulating the powdery mixture or granulating a slurry of the powdery mixture by spray-drying, firing the granulated particle (800-1200 deg.C) and washing the fired material with water or the like to remove the flux component.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は、摩擦・摩耗材,耐
熱材,樹脂補強材,塗料充填材、誘電体材料等として有
用なチタン酸アルカリ土類金属塩粉末の製造方法に関す
る。
TECHNICAL FIELD The present invention relates to a method for producing an alkaline earth metal titanate powder which is useful as a friction / wear material, a heat resistant material, a resin reinforcing material, a paint filler, a dielectric material and the like.

【0002】[0002]

【従来の技術】一般式: RTiO3 〔式中,Rはアルカ
リ土類金属〕で表されるチタン酸アルカリ土類金属(C
aTiO3,BaTiO3 等)は、ペロブスカイト型結晶
構造を有する合成無機化合物である。このものは、誘電
体・圧電体等のエレクトロニクス用素材として実用され
ているが、強度,耐摩耗性,耐熱性等にもすぐれた化合
物である。従って、これらの特性を生かして、例えばブ
レーキ装置の摩擦材,強化プラスチックの補強材,樹脂
塗料の充填材等の各種分野における工学的応用が期待さ
れる。このチタン酸アルカリ土類金属粉末の製造方法と
して、固相合成法,水熱法等が知られている。
2. Description of the Related Art Alkaline earth metal titanates represented by the general formula: RTiO 3 [wherein R is an alkaline earth metal] (C
aTiO 3, BaTiO 3 and the like) are synthetic inorganic compounds having a perovskite type crystal structure. This compound is practically used as a material for electronics such as a dielectric / piezoelectric material, but it is also a compound excellent in strength, abrasion resistance, heat resistance and the like. Therefore, by utilizing these characteristics, engineering applications in various fields such as friction materials for brake devices, reinforcing materials for reinforced plastics, and fillers for resin paints are expected. Known methods for producing this alkaline earth metal titanate powder include solid phase synthesis and hydrothermal methods.

【0003】[0003]

【発明が解決しようとする課題】固相合成法は、酸化チ
タン(TiO2 )または加熱によりTiO2 となるチタ
ン化合物とアルカリ土類金属酸化物(RO)または加熱
によりROとなる化合物の混合物を焼成して目的とする
化合物を合成するものであり、その焼成処理は高温度
(約1350℃以上)で行われる。このため、反応過程
で粒子の成長や焼結が生じ、焼成処理後、反応生成物の
粉砕を必要とし、また得られる粉末も粒度分布の比較的
広いものとなり、目的に応じて分級が必要となる。他
方、水熱合成法では、粒径が微細(サブミクロン)で粒
度分布もシャープなチタン酸アルカリ土類金属塩粉末を
得ことができる反面、比較的粗粒の粉末(数μmないし
それ以上の粗粒粉末)を得ることは困難である。サブミ
クロンの微細粒子は、流動性・分散性が低く、均質で緻
密性の高い成型品を得ることが困難である。しかも水熱
合成反応は、高価なオートクレーブ等の反応容器を必要
とし、製造コストが高く、大量生産にも不向きである等
の難点があり、工業的な製造法とはいえない。本発明
は、上記に鑑み、流動性・分散性がよく、ハンドリング
や作業性に優れ、種々の材料に複合して優れた特性を示
すチタン酸アルカリ土類金属粉末およびその粉末を、特
殊な反応容器を必要とせず、比較的低温域での焼成反応
により、効率よく収得することができる製造方法を提供
するものである。
The solid phase synthesis method involves the use of a mixture of titanium oxide (TiO 2 ) or a titanium compound that turns into TiO 2 when heated and an alkaline earth metal oxide (RO) or a compound that turns into RO when heated. The target compound is synthesized by firing, and the firing process is performed at a high temperature (about 1350 ° C. or higher). For this reason, particle growth and sintering occur in the reaction process, and it is necessary to pulverize the reaction product after the firing treatment, and the resulting powder also has a relatively wide particle size distribution, and classification is necessary according to the purpose. Become. On the other hand, in the hydrothermal synthesis method, although an alkaline earth metal titanate powder having a fine particle size (submicron) and a sharp particle size distribution can be obtained, on the other hand, a relatively coarse particle (several μm or more) It is difficult to obtain a coarse powder). Submicron fine particles have low fluidity and dispersibility, and it is difficult to obtain a homogeneous and highly dense molded product. In addition, the hydrothermal synthesis reaction requires an expensive reaction container such as an autoclave, has a high manufacturing cost, and is not suitable for mass production. Therefore, it cannot be said to be an industrial manufacturing method. In view of the above, the present invention provides an alkaline earth metal titanate powder having excellent fluidity and dispersibility, excellent handling and workability, and excellent properties in combination with various materials, and a special reaction of the powder. It is intended to provide a production method capable of obtaining efficiently by a firing reaction in a relatively low temperature range without requiring a container.

【0004】[0004]

【課題を解決するための手段】本発明のチタン酸アルカ
リ土類金属粉末は、平均粒径0.5〜5μmの単位粒子
が焼結してなる粒径10〜1000μmの球状粒子であ
ることを特徴としている。上記チタン酸アルカリ土類金
属粉末は、原料粉末を湿式噴霧造粒する工程を含む第1
の製造方法により、または原料粉末を乾式混合造粒する
工程を含む第2の製造法により効率よく製造される。本
発明の第1の製造方法は、フラックス成分であるアルカ
リ金属化合物を溶解した溶液に、TiO2 または加熱に
よりTiO2 を生成するチタン化合物粉末と、RO〔式
, Rはアルカリ土類金属元素を表す〕または加熱によ
りROを生成するアルカリ土類金属化合物粉末とを混合
してスラリーとなし、スラリーを噴霧乾燥した後、その
造粒粉を温度800〜1200℃で焼成処理し、または
スラリーを温度800〜1200℃の雰囲気中に噴霧し
て造粒粉を焼成し、ついで、焼成物からフラックス成分
および未反応物質を洗浄除去する、ことを特徴としてい
る。本発明の第2の製造方法は、フラックス成分である
アルカリ金属化合物、TiO2 または加熱によりTiO
2 を生成するチタン化合物、およびRO〔式中, Rは前
記と同義〕または加熱によりROを生成するアルカリ土
類金属化合物からなる粉末混合物を混合造粒し、その造
粒粉を温度800〜1200℃で焼成処理した後、焼成
物からフラックス成分および未反応物質を洗浄除去す
る、ことを特徴としている。
The alkaline earth metal titanate powder of the present invention is a spherical particle having a particle size of 10 to 1000 μm obtained by sintering unit particles having an average particle size of 0.5 to 5 μm. It has a feature. The alkaline earth metal titanate powder includes a step of wet spray granulating a raw material powder.
Or the second production method including the step of dry-mixing and granulating the raw material powder. The first production method of the present invention, the solution of alkali metal compound is a flux component, and a titanium compound powder to produce a TiO 2 by TiO 2 or heating in RO [wherein, R is an alkaline earth metal element Or an alkaline earth metal compound powder that produces RO by heating is mixed to form a slurry, and the slurry is spray-dried, and then the granulated powder is calcined at a temperature of 800 to 1200 ° C., or the slurry is It is characterized in that the granulated powder is fired by spraying in an atmosphere of a temperature of 800 to 1200 ° C., and then the flux component and unreacted substances are washed and removed from the fired product. The second manufacturing method of the present invention is a method of producing an alkali metal compound which is a flux component, TiO 2 or TiO by heating.
Titanium compound to produce a 2, and RO [wherein, R as defined above] The powder mixture is mixed granulation consisting of alkaline earth metal compound that produces RO or by heating, the temperature and the granulated powder 800-1200 After the calcination treatment at ℃, the flux components and unreacted substances are washed and removed from the calcinated product.

【0005】[0005]

【発明の実施の形態】本発明のチタン酸アルカリ土類金
属粉末は、平均粒径0.5〜5μmの単位粒子からなる
焼結体であり、その粒径は10〜1000μmである。
このものは真球に近似する形状を有し、サブミクロンの
微細粒子からなる粉末に比し、良好な流動性,分散性を
備えている。粒子(焼結体)の粒径は、原料粉末の造粒
条件により制御され、粒子を構成する単位粒子の粒径は
焼成処理温度(焼成処理温度は原料中のフラックス成分
の配合割合により変化する)により制御される。本発明
のよるチタン酸アルカリ土類金属粉末の製造法において
は、原料中にフラックス成分(アルカリ金属化合物)が
配合されることにより、焼成処理工程で生成するフラッ
クスの融液を介してRO(アルカリ土類金属酸化物)と
TiO2との反応が促進され、約800〜1200℃の
比較的低温域で効率よく所定の反応を達成することがで
きる。更に、フラックス成分は水に可溶であるので、焼
成物からのフラックスの除去は、水等で焼成物を洗浄処
理することにより容易に溶解除去される。焼成物は機械
的粉砕処理を必要とせず、焼成物の洗浄処理工程で、軽
度の攪拌ないし振動を付加する簡単な措置で、造粒粉の
形状をほぼそのまま有する球形状のチタン酸アルカリ土
類金属粉末を処理液中から効率よく回収することができ
る。
BEST MODE FOR CARRYING OUT THE INVENTION The alkaline earth metal titanate powder of the present invention is a sintered body composed of unit particles having an average particle size of 0.5 to 5 μm, and the particle size is 10 to 1000 μm.
It has a shape close to a true sphere, and has good fluidity and dispersibility as compared with powder consisting of submicron fine particles. The particle size of the particles (sintered body) is controlled by the granulation conditions of the raw material powder, and the particle size of the unit particles constituting the particles is the firing temperature (the firing temperature changes depending on the mixing ratio of the flux component in the raw material). ) Controlled by. In the method for producing an alkaline earth metal titanate powder according to the present invention, a flux component (alkali metal compound) is mixed in a raw material so that RO (alkali The reaction between the (earth metal oxide) and TiO 2 is promoted, and a predetermined reaction can be efficiently achieved in a relatively low temperature range of about 800 to 1200 ° C. Furthermore, since the flux component is soluble in water, the flux can be easily removed from the fired product by washing the fired product with water or the like. The calcined product does not require mechanical pulverization, and the spherical alkaline earth titanate that has almost the same shape as the granulated powder can be obtained by a simple measure that adds mild agitation or vibration in the cleaning process of the calcined product. The metal powder can be efficiently recovered from the treatment liquid.

【0006】本発明のチタン酸アルカリ土類金属粉末の
製造原料として使用される上記チタン化合物は、精製ア
ナターゼ粉末,精製ルチル粉末,各種化合物(ハロゲン
化物,硫酸塩,硝酸塩,水和物等)等であり、アルカリ
土類金属化合物としては、Mg,Ca,Sr,Ba等の
酸化物,炭酸塩,硫酸塩,硝酸塩,ハロゲン化物(塩化
物,弗化物等),水酸化物等が使用される。また、フラ
ックス成分であるアルカリ金属化合物は、K,Na,L
i,Rb等の炭酸塩、ハロゲン化合物(塩化物,弗化
物,臭化物,沃化物)等であり、これらはその1種ない
し2種以上を混合使用してよい。
The titanium compound used as a raw material for producing the alkaline earth metal titanate powder of the present invention includes purified anatase powder, purified rutile powder, various compounds (halides, sulfates, nitrates, hydrates, etc.), etc. As the alkaline earth metal compound, oxides such as Mg, Ca, Sr and Ba, carbonates, sulfates, nitrates, halides (chlorides, fluorides), hydroxides, etc. are used. . In addition, the alkali metal compound that is the flux component is K, Na, L
Carbonates such as i and Rb, halogen compounds (chlorides, fluorides, bromides, iodides) and the like, and these may be used alone or in admixture of two or more.

【0007】上記チタン化合物とアルカリ土類金属化合
物は、目的物であるチタン酸アルカリ土類金属の生成反
応〔TiO2 +RO→RTiO3 〕に必要な量比、すな
わちTiO2 とROとが等モル比となる割合に配合され
る。アルカリ金属化合物(フラックス成分)は、焼成処
理工程で融液を生成し、TiO2 とROとの反応を促進
する役割を有する。その配合量が少ないと、反応促進効
果が不足し、他方多量に配合すると焼成処理後のフラッ
クスの除去量が多くなり、また不必要な増量は却って反
応率の低下を招く。かかる観点より、その配合量は、チ
タン化合物とアルカリ土類金属化合物の合計量の約1〜
20重量%の範囲内が適当である。
The above-mentioned titanium compound and alkaline earth metal compound are in a molar ratio required for the desired reaction of alkaline earth metal titanate [TiO 2 + RO → RTiO 3 ], that is, TiO 2 and RO are equimolar. It is blended in a ratio to be a ratio. The alkali metal compound (flux component) has a role of generating a melt in the firing treatment step and accelerating the reaction between TiO 2 and RO. If the blending amount is too small, the reaction accelerating effect is insufficient. On the other hand, if the blending amount is too large, the amount of the flux removed after the firing treatment is large, and an unnecessary increase in the amount causes a decrease in the reaction rate. From this viewpoint, the blending amount is about 1 to 1 of the total amount of the titanium compound and the alkaline earth metal compound.
A range of 20% by weight is suitable.

【0008】上記原料粉末の造粒は、粉末混合物のスラ
リーをスプレードライヤーで噴霧乾燥し、または粉末混
合物の乾式混合造粒処理により行われる。噴霧乾燥処理
を適用する場合のスラリーの調製は、フラックス成分
(アルカリ金属化合物)を適量の水(例えば、原料粉末
総量の約1〜3倍量)に溶解し、その溶液にチタン化合
物粉末およびアルカリ土類金属粉末を添加し混合するこ
とにより行えばよい。造粒粉の粒径は、約10〜100
0μmに調整される。造粒粉の焼成処理は、800〜1
200℃の温度域に適当時間(例えば1〜3Hr)保持
することにより行われる。処理温度を800℃以上とす
るのは、それより低い温度では、反応の完結に長時間を
要し、他方1200℃を超える高温度では、生成するペ
ロブスカイト結晶粒の成長粗大化や粒子同士の焼結を生
じ、製品粉末の球状粒子形態が損なわれるからである。
原料粉末の造粒を湿式噴霧乾燥により行う場合は、スラ
リーを、温度800〜1200℃に保持された高温雰囲
気中に噴霧し、造粒粉をその雰囲気中に適当時間(数秒
〜数十秒)保持するようにしてもよい。この場合は、噴
霧による造粒と焼成処理とを一工程で済ませることがで
きる。
The above-mentioned raw material powder is granulated by spray-drying a slurry of the powder mixture with a spray dryer or by dry-mixing granulation of the powder mixture. When applying the spray drying treatment, the slurry is prepared by dissolving the flux component (alkali metal compound) in an appropriate amount of water (for example, about 1 to 3 times the total amount of the raw material powder), and adding titanium compound powder and alkali to the solution. It may be performed by adding and mixing an earth metal powder. The particle size of the granulated powder is about 10 to 100.
It is adjusted to 0 μm. Baking treatment of granulated powder is 800-1
It is carried out by maintaining the temperature range of 200 ° C. for an appropriate time (for example, 1 to 3 hours). The treatment temperature of 800 ° C. or higher requires a long time to complete the reaction at lower temperatures, while at a high temperature of more than 1200 ° C., the growth and coarsening of perovskite crystal grains to be formed and the burning of particles are performed. This is because binding occurs and the spherical particle form of the product powder is impaired.
When the raw material powder is granulated by wet spray drying, the slurry is sprayed in a high temperature atmosphere maintained at a temperature of 800 to 1200 ° C., and the granulated powder is kept in the atmosphere for an appropriate time (several seconds to several tens of seconds). You may make it hold | maintain. In this case, the granulation by spraying and the firing treatment can be completed in one step.

【0009】焼成処理の後、焼成物を洗浄処理に付して
フラックス成分(および未反応残留物)を除去し、つい
で液中から粉末を回収し、脱水乾燥することにより、目
的物であるチタン酸アルカリ土類金属塩〔RTiO3
粉末を得る。洗浄処理は水を処理液として行うことがで
きる。焼成物を水中に浸漬し、プロペラ等による軽度の
攪拌流あるいは振動を付加することにより、フラックス
成分(および未反応残留物)の溶解除去と、製品粉末粒
子の解砕を効率よく短時間で達成することができる。得
られる製品粉末は、原料粉末混合物の乾式混合または湿
式噴霧乾燥による粒状物の粒子形態をほぼそのまま受け
継いだ真球に近い球形状を有する。
After the firing treatment, the fired product is subjected to a washing treatment to remove the flux component (and unreacted residue), and then the powder is recovered from the liquid and dehydrated and dried to obtain the target product titanium. Acid alkaline earth metal salt [RTiO 3 ]
Get a powder. The washing treatment can be performed using water as the treatment liquid. By immersing the fired product in water and applying a mild stirring flow or vibration with a propeller etc., the flux components (and unreacted residue) are dissolved and removed, and the product powder particles are efficiently crushed in a short time. can do. The product powder obtained has a spherical shape close to a true sphere, which inherits the particle morphology of the granular material obtained by dry mixing or wet spray drying of the raw material powder mixture.

【0010】[0010]

【実施例】【Example】

〔実施例1〕フラックス成分として炭酸カリウム(K2
CO3 )を水に溶解し、これにチタン化合物として精製
アナターゼ(TiO2 )粉末およびアルカリ土類金属と
して炭酸カルシウム(CaCO3 )粉末(平均粒径:
1.5μm)を加え、攪拌混合してスラリーを調製す
る。スラリーをスプレードライヤーで噴霧乾燥(乾燥温
度200℃)し、造粒粉を得る。造粒粉を焼成処理(処理
温度 1000 ℃)した後、焼成物を水中に投入し、軽度の
攪拌流下に洗浄処理し、フラックス成分および未反応物
質を溶解除去する。液中から粉末を回収し、脱水乾燥
(110℃)して製品粉末を得る。
[Example 1] As a flux component, potassium carbonate (K 2
CO 3 ) is dissolved in water, and purified anatase (TiO 2 ) powder as a titanium compound and calcium carbonate (CaCO 3 ) powder as an alkaline earth metal (average particle size:
1.5 μm), and mixed by stirring to prepare a slurry. The slurry is spray-dried with a spray dryer (drying temperature 200 ° C) to obtain granulated powder. After the granulated powder is calcined (treatment temperature 1000 ° C), the calcined product is put into water and washed under a slight agitation flow to dissolve and remove flux components and unreacted substances. The powder is recovered from the liquid and dehydrated and dried (110 ° C.) to obtain a product powder.

【0011】〔実施例2〕アルカリ土類金属として炭酸
バリウム(BaCO3 )を使用する点を除いて、実施例
1と同一の処理条件により、製品粉末を得る。
Example 2 A product powder is obtained under the same processing conditions as in Example 1 except that barium carbonate (BaCO 3 ) is used as the alkaline earth metal.

【0012】〔実施例3〕スラリーをスプレードライヤ
ーで高温雰囲気(温度: 1000℃)中に噴霧し、造粒
粉をその雰囲気中に所定時間保持することにより、造粒
と焼成処理を行う点を除いて実施例1と同一の処理条件
により、製品粉末を得る。
[Embodiment 3] The slurry is sprayed in a high temperature atmosphere (temperature: 1000 ° C.) with a spray dryer, and the granulated powder is held in the atmosphere for a predetermined time to perform granulation and firing treatment. A product powder is obtained under the same processing conditions as in Example 1 except for the above.

【0013】〔実施例4〕精製アナターゼ(Ti
2 )、炭酸カルシウム(CaCO3 )および炭酸カリ
ウム(K2 CO3 )の混合粉末(粉末粒度: 実施例1と
同じ)を乾式混合造粒機で造粒し、焼成処理に付す。つ
いで焼成物を水中に投入し、攪拌下に1Hrを要してフ
ラックス成分および未反応物質を洗浄除去する。液中か
ら粉末を回収し、脱水乾燥(110℃)して製品粉末を
得る。
Example 4 Purified anatase (Ti
O 2 ), calcium carbonate (CaCO 3 ) and potassium carbonate (K 2 CO 3 ) mixed powder (powder particle size: the same as in Example 1) is granulated by a dry mixing granulator and subjected to a firing treatment. Then, the fired product is put into water, and 1 Hr is required with stirring to wash and remove the flux components and unreacted substances. The powder is recovered from the liquid and dehydrated and dried (110 ° C.) to obtain a product powder.

【0014】表1に各実施例の製造条件の詳細および製
品粉末を示す。得られた粉末は、いずれも健全なペロブ
スカイト型結晶構造を有し、その粒子形状はほぼ真球の
球形状を有している(走査型電子顕微鏡観察)。
Table 1 shows the details of the production conditions and the product powder of each example. Each of the obtained powders has a sound perovskite type crystal structure, and the particle shape thereof has a substantially spherical spherical shape (scanning electron microscope observation).

【0015】[0015]

【表1】 [Table 1]

【0016】[0016]

【発明の効果】本発明のチタン酸アルカリ土類金属粉末
は、比較的粗粒の球状粒子形態を有するので、流動性・
分散性が良好で、ハンドリング・作業性に優れ、摩擦・
摩耗材,耐熱材,樹脂補強材,塗料充填材、誘電体材料
等として好適である。本発明によれば、水熱法のような
特殊な反応容器を必要とせず、また従来の固相合成法と
異なって比較的低温度域での焼成処理により、上記のチ
タン酸アルカリ土類金属塩粉末が得られる。その製造工
程においては、焼成物を粉砕処理する必要もなく、焼成
処理後、フラックス成分を溶解除去する洗浄処理によ
り、所望の粒度を有する製品粉末を収得することができ
る。
Industrial Applicability The alkaline earth metal titanate powder of the present invention has a relatively coarse spherical particle morphology, so that the fluidity
Good dispersibility, excellent handling and workability, friction
It is suitable as a wear material, heat resistant material, resin reinforcing material, paint filling material, dielectric material and the like. According to the present invention, a special reaction vessel such as the hydrothermal method is not required, and unlike the conventional solid-phase synthesis method, the alkaline earth metal titanate is treated by the firing treatment in a relatively low temperature range. A salt powder is obtained. In the manufacturing process, it is not necessary to pulverize the calcined product, and after the calcination process, a product powder having a desired particle size can be obtained by a washing process for dissolving and removing the flux component.

Claims (3)

【特許請求の範囲】[Claims] 【請求項1】 平均粒径0.5〜5μmの単位粒子が焼
結してなる粒径10〜1000μmの球状粒子であるこ
とを特徴とするチタン酸アルカリ土類金属粉末。
1. An alkaline earth metal titanate powder, which is a spherical particle having a particle size of 10 to 1000 μm formed by sintering unit particles having an average particle size of 0.5 to 5 μm.
【請求項2】 フラックス成分であるアルカリ金属化合
物を溶解した溶液に、TiO2 または加熱によりTiO
2 を生成するチタン化合物粉末と、RO〔式中, Rはア
ルカリ土類金属元素を表す〕または加熱によりROを生
成するアルカリ土類金属化合物粉末とを混合してスラリ
ーとなし、 スラリーを噴霧乾燥した後、その造粒粉を温度800〜
1200℃で焼成処理し、またはスラリーを温度800
〜1200℃の雰囲気中に噴霧して造粒粉を焼成し、 ついで、焼成物からフラックス成分および未反応物質を
洗浄除去する、ことを特徴とする請求項1に記載のチタ
ン酸アルカリ土類金属粉末の製造方法。
2. A solution in which an alkali metal compound as a flux component is dissolved is added to TiO 2 or TiO by heating.
The titanium compound powder that produces 2 is mixed with RO [in the formula , R represents an alkaline earth metal element] or the alkaline earth metal compound powder that produces RO by heating to form a slurry, and the slurry is spray-dried. After that, the granulated powder is heated to a temperature of 800 to
Calcination at 1200 ° C. or slurry temperature at 800
The alkaline earth metal titanate according to claim 1, characterized in that the granulated powder is fired by spraying in an atmosphere of ~ 1200 ° C, and then the flux component and unreacted substances are washed and removed from the fired product. Powder manufacturing method.
【請求項3】 フラックス成分であるアルカリ金属化合
物、TiO2 または加熱によりTiO2 を生成するチタ
ン化合物、およびRO〔式中, Rはアルカリ土類金属元
素を表す〕または加熱によりROを生成するアルカリ土
類金属化合物からなる粉末混合物を混合造粒し、その造
粒粉を温度800〜1200℃で焼成処理した後、焼成
物からフラックス成分および未反応物質を洗浄除去す
る、ことを特徴とする請求項1に記載のチタン酸アルカ
リ土類金属粉末の製造方法。
Wherein the alkali metal compound is a flux component, the titanium compound to produce a TiO 2 by TiO 2 or heating, and RO [wherein, R represents an alkaline earth metal element] alkali to generate the RO or by heating A method of mixing and granulating a powder mixture comprising an earth metal compound, firing the granulated powder at a temperature of 800 to 1200 ° C., and then washing and removing flux components and unreacted substances from the fired product. Item 2. A method for producing an alkaline earth metal titanate powder according to Item 1.
JP8060952A 1996-03-18 1996-03-18 Alkaline earth metal titanate powder and method for producing the same Pending JPH09255337A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP8060952A JPH09255337A (en) 1996-03-18 1996-03-18 Alkaline earth metal titanate powder and method for producing the same

Publications (1)

Publication Number Publication Date
JPH09255337A true JPH09255337A (en) 1997-09-30

Family

ID=13157247

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JPH09255337A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0856489A1 (en) * 1997-01-31 1998-08-05 Kubota Corporation Powder of titanium compounds
WO1999053215A1 (en) * 1998-04-09 1999-10-21 Alliedsignal Inc. Metal titanates for friction stabilization of friction materials
JP2013139384A (en) * 2013-02-19 2013-07-18 Sumitomo Osaka Cement Co Ltd Method for producing metal oxide nanoparticle
WO2013115183A1 (en) * 2012-01-30 2013-08-08 日本化学工業株式会社 Dielectric ceramic material and process for producing coarse particles of perovskite-type composite oxide for use therein
WO2019130941A1 (en) * 2017-12-26 2019-07-04 株式会社クボタ Composite titanium oxide compound, composite titanium oxide compound production method, and friction material

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP0856489A1 (en) * 1997-01-31 1998-08-05 Kubota Corporation Powder of titanium compounds
US5962551A (en) * 1997-01-31 1999-10-05 Kubota Corporation Powder of titanium compounds
WO1999053215A1 (en) * 1998-04-09 1999-10-21 Alliedsignal Inc. Metal titanates for friction stabilization of friction materials
WO2013115183A1 (en) * 2012-01-30 2013-08-08 日本化学工業株式会社 Dielectric ceramic material and process for producing coarse particles of perovskite-type composite oxide for use therein
JP2013155071A (en) * 2012-01-30 2013-08-15 Nippon Chem Ind Co Ltd Dielectric ceramic material, and method for producing coarse particle of perovskite-type composite oxide used therefor
JP2013139384A (en) * 2013-02-19 2013-07-18 Sumitomo Osaka Cement Co Ltd Method for producing metal oxide nanoparticle
WO2019130941A1 (en) * 2017-12-26 2019-07-04 株式会社クボタ Composite titanium oxide compound, composite titanium oxide compound production method, and friction material
JP2019112277A (en) * 2017-12-26 2019-07-11 株式会社クボタ Composite titanate compound, manufacturing method of composite titanate compound, and friction material
US11846336B2 (en) 2017-12-26 2023-12-19 Kubota Corporation Complex titanate compound, method of preparing same, and friction material

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