JPH0558605A - Production of ceramic composite powder - Google Patents

Production of ceramic composite powder

Info

Publication number
JPH0558605A
JPH0558605A JP24445091A JP24445091A JPH0558605A JP H0558605 A JPH0558605 A JP H0558605A JP 24445091 A JP24445091 A JP 24445091A JP 24445091 A JP24445091 A JP 24445091A JP H0558605 A JPH0558605 A JP H0558605A
Authority
JP
Japan
Prior art keywords
ceramic
alkoxide
particles
composite powder
suspension
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
JP24445091A
Other languages
Japanese (ja)
Inventor
Yasuyuki Ogata
康行 緒方
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.)
Mitsubishi Materials Corp
Original Assignee
Mitsubishi Materials 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 Mitsubishi Materials Corp filed Critical Mitsubishi Materials Corp
Priority to JP24445091A priority Critical patent/JPH0558605A/en
Publication of JPH0558605A publication Critical patent/JPH0558605A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/009After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B41/00After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
    • C04B41/45Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
    • C04B41/4584Coating or impregnating of particulate or fibrous ceramic material

Abstract

PURPOSE:To obtain a ceramic composite powder having plural functions such as electric function, mechanical function and magnetic function. CONSTITUTION:A metal alkoxide is dissolved in an organic solvent to prepare the alkoxide solution and ceramic particles are dispersed in the solution to prepare a ceramic suspension. Water is added to the suspension and the alkoxide is hydrolyzed to prepare a composite in which hydrolyzed product of the alkoxide is attached to the surface of the above-mentioned ceramic particles. The hydrolyzed product of alkoxide is converted to metal oxide particles by dry-heating the composite to provide the objective ceramic composite powder in which the ceramic particles are contained as nuclei and the metal oxide particles are attached around the nuclei.

Description

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

【0001】[0001]

【産業上の利用分野】本発明は電気的機能、機械的機
能、磁気的機能等の複数の機能を兼備したセラミック複
合粉体の製造方法に関するものである。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a ceramic composite powder having a plurality of functions such as an electric function, a mechanical function and a magnetic function.

【0002】[0002]

【従来の技術】ファインセラミックスは通常ある特定の
性質、即ち電気的機能、機械的機能、磁気的機能等を個
別に有するように製造されている。例えば、機械的機能
を有するセラミックスはAl23やZrO2を主成分と
するセラミック粉体を原料に用いてつくられ、誘電体セ
ラミックスではBaTiO3を主成分とするセラミック
粉体を原料に用いてつくられる。しかし機械的性質と誘
電的性質というように諸機能を同時に併せ持つセラミッ
ク複合粉体は現在開発されていない。従来、この種のセ
ラミック複合粉体を製造する一般的な方法は、所定の組
成になるようにセラミック原料粉体を成分毎に秤量し、
各成分を十分に混合して均一にした後、これを焼成する
方法である。この方法は十分均質な組成にするために、
一旦焼成したものを粉砕し、混合と焼成を何度も繰り返
さなければならない。
2. Description of the Related Art Fine ceramics are usually manufactured so as to individually have certain specific properties, that is, electrical function, mechanical function, magnetic function and the like. For example, a ceramic having a mechanical function is made by using a ceramic powder containing Al 2 O 3 or ZrO 2 as a main component, and a dielectric ceramic is produced by using a ceramic powder containing BaTiO 3 as a main component. Be done. However, no ceramic composite powder has been developed so far, which has various functions such as mechanical properties and dielectric properties at the same time. Conventionally, a general method for producing this type of ceramic composite powder is to weigh the ceramic raw material powder for each component so as to have a predetermined composition,
This is a method in which the respective components are sufficiently mixed and homogenized, and then this is fired. This method requires a homogeneous composition
It is necessary to grind what is once fired, and to repeat mixing and firing many times.

【0003】[0003]

【発明が解決しようとする課題】しかしこの方法により
十分に混合しても、混合前の微細な原料粉体は凝集し易
いため、混合物の平均粒径はミクロンオーダの均一な組
成になりにくい。理想的な均一な組成のセラミックスを
得るためには、原料粉体として予め所定の組成になって
いるようなセラミックス−セラミックス原料粉末を用い
ることが望ましいが、このような目的に適するセラミッ
クス−セラミックス複合粉末の製造方法は現在未だ見い
だされていない。
However, even if it is sufficiently mixed by this method, since the fine raw material powder before mixing easily aggregates, the average particle size of the mixture is unlikely to have a uniform composition on the order of microns. In order to obtain a ceramics having an ideal uniform composition, it is desirable to use a ceramics-ceramics raw material powder having a predetermined composition as a raw material powder, but a ceramics-ceramics composite suitable for such purpose is used. A method for producing powder has not yet been found.

【0004】本発明の目的は、各種の機能を複合して同
時に併せ持つセラミック複合粉体の製造方法を提供する
ことにある。
It is an object of the present invention to provide a method for producing a ceramic composite powder which has various functions in a composite form and has them at the same time.

【0005】[0005]

【課題を解決するための手段】上記目的を達成するため
に、本発明のセラミックス複合粉体の製造方法は、有機
溶剤に金属アルコキシドを溶解してアルコキシド溶液を
調製する工程と、この溶液にセラミック粒子を分散して
セラミック懸濁液を調製する工程と、この懸濁液に水を
加えて前記アルコキシドを加水分解し、この加水分解生
成物が前記セラミック粒子の表面に付着した複合体を調
製する工程と、この複合体を乾燥加熱して前記加水分解
生成物を金属酸化物粒子に変え、前記セラミック粒子を
核として、その周りに金属酸化物粒子が付着したセラミ
ック複合粉体を得る工程とを含む方法である。
In order to achieve the above object, a method for producing a ceramic composite powder of the present invention comprises a step of dissolving a metal alkoxide in an organic solvent to prepare an alkoxide solution, and a ceramic in the solution. Dispersing the particles to prepare a ceramic suspension and adding water to the suspension to hydrolyze the alkoxide and to prepare a composite in which the hydrolysis product adheres to the surface of the ceramic particles. And a step of drying and heating the composite to convert the hydrolysis product into metal oxide particles, and using the ceramic particles as a core to obtain a ceramic composite powder having metal oxide particles attached thereto. It is a method including

【0006】以下、本発明を詳述する。 (a) セラミック懸濁液の調製 所定の一種または二種以上の金属アルコキシドをこれを
溶解することのできる有機溶剤に溶解する。金属アルコ
キシドのアルキル基としては、炭素数1〜20のものを
含む。金属元素としては有機金属を合成可能な元素はす
べて含む。Na,K,Cs等のアルカリ金属、Mg,C
a,Sr,Ba等のアルカリ土類金属、Ti,V,C
r,Mn,Fe,Co,Ni,Y,Zr,Nb,Mo,
Hf,Ta,W,Re等の遷移金属、Cu,Zn,A
l,Cd等の金属、B,Si,Ga,Ge,As,S
e,In,Sn,Sb,Te,Pb,Bi等の半金属、
La,Ce,Sm等の希土類元素を含む。有機溶剤とし
ては、アルコール類、ケトン類、ベンゼン、キシレン等
の芳香族化合物等が挙げられる。
The present invention will be described in detail below. (a) Preparation of Ceramic Suspension A predetermined one kind or two or more kinds of metal alkoxides are dissolved in an organic solvent capable of dissolving them. The alkyl group of the metal alkoxide includes those having 1 to 20 carbon atoms. The metal element includes all elements capable of synthesizing an organic metal. Alkali metals such as Na, K, Cs, Mg, C
Alkaline earth metal such as a, Sr, Ba, Ti, V, C
r, Mn, Fe, Co, Ni, Y, Zr, Nb, Mo,
Transition metals such as Hf, Ta, W, Re, Cu, Zn, A
Metals such as l and Cd, B, Si, Ga, Ge, As, S
semimetals such as e, In, Sn, Sb, Te, Pb and Bi,
It contains rare earth elements such as La, Ce and Sm. Examples of the organic solvent include alcohols, ketones, aromatic compounds such as benzene and xylene, and the like.

【0007】得られたアルコキシド溶液にセラミック粒
子を加えて分散させ、セラミック懸濁液を調製する。こ
のセラミック粒子は公知の粉砕法、化学合成法で作られ
る微粉からなり、焼結特性からサブミクロンの領域の粒
度、好ましくは1μm以下の粒径を有する酸化物セラミ
ック粉体である。本発明の目的を達成するために、この
セラミック粒子である酸化物は上記金属アルコキシドの
加水分解を通じて得られる金属酸化物と異なる機能を有
する。このアルコキシド溶液の濃度及びセラミック粒子
の分散量は本発明の複合粉体の最終用途に応じて決めら
れるが、アルコキシド溶液の濃度は0.1〜10モル/
Lが、またセラミック粒子の分散量は上記有機溶剤に対
して5〜100重量%が好ましい。なお、セラミック懸
濁液は、最初に有機溶剤にセラミック粒子を分散させ、
次いでこの分散液に金属アルコキシドを溶解させて調製
してもよい。セラミック粒子を分散させる際に、超音波
を加えれば、セラミック粒子が均一に分散し、好まし
い。
Ceramic particles are added to and dispersed in the obtained alkoxide solution to prepare a ceramic suspension. These ceramic particles are fine powders produced by a known pulverization method or chemical synthesis method, and are oxide ceramic powders having a particle size in the submicron region, preferably 1 μm or less, due to the sintering characteristics. In order to achieve the object of the present invention, the oxide that is the ceramic particles has a function different from that of the metal oxide obtained through the hydrolysis of the metal alkoxide. The concentration of the alkoxide solution and the dispersion amount of the ceramic particles are determined according to the end use of the composite powder of the present invention, but the concentration of the alkoxide solution is 0.1 to 10 mol /
L and the dispersion amount of the ceramic particles are preferably 5 to 100% by weight with respect to the organic solvent. The ceramic suspension is prepared by first dispersing the ceramic particles in an organic solvent,
Then, a metal alkoxide may be dissolved in this dispersion to prepare the dispersion. When ultrasonic waves are applied when dispersing the ceramic particles, the ceramic particles are uniformly dispersed, which is preferable.

【0008】(b) アルコキシドの加水分解 このように調製されたセラミック懸濁液に水を加えて、
金属アルコキシドの加水分解を起こさせる。一般にアル
コキシドの加水分解生成物は数10〜数1000オング
ストロームの極めて微細な粒子であるため、加水分解生
成物の活性エネルギは極めて高く、それ自身が有機溶剤
中に単独で安定して分散することは困難であり、従っ
て、アルコキシド加水分解生成物の粒子は自発的に有機
溶剤中に浮遊しているセラミック粒子の表面上に付着す
る。
(B) Hydrolysis of alkoxide Water was added to the ceramic suspension thus prepared,
Causes hydrolysis of metal alkoxides. Generally, the hydrolysis product of the alkoxide is extremely fine particles of several tens to several thousand angstroms, and therefore the active energy of the hydrolysis product is extremely high, and the alkoxide itself cannot be stably dispersed in an organic solvent. Difficult, and therefore particles of the alkoxide hydrolysis product spontaneously deposit on the surface of the ceramic particles suspended in the organic solvent.

【0009】(c) セラミック複合粉体の製造 上記懸濁液から有機溶剤と水を含む液体を蒸発させるこ
とにより、或いは懸濁液を遠心分離又は濾過して分離物
を乾燥することにより、アルコキシド加水分解生成物が
セラミックス粒子に付着して成る複合物が得られる。こ
の複合物を金属アルコキシドが分解して金属酸化物を生
成する温度以上であって、この金属酸化物がセラミック
粒子と反応する温度未満で加熱すると、セラミック粒子
を核として、その周りに金属酸化物粒子が付着した二層
構造を有するセラミック複合粉体が得られる。
(C) Manufacture of ceramic composite powder The alkoxide is prepared by evaporating a liquid containing an organic solvent and water from the above suspension, or by centrifuging or filtering the suspension to dry the separated product. A composite is obtained in which the hydrolysis product adheres to the ceramic particles. When this composite is heated at a temperature higher than the temperature at which the metal alkoxide decomposes to form a metal oxide and lower than the temperature at which the metal oxide reacts with the ceramic particles, the ceramic particles serve as nuclei and the metal oxide surrounds them. A ceramic composite powder having a two-layer structure with particles attached is obtained.

【0010】また上述のような本発明の製造工程を繰返
すことにより、三層以上の構造を持つセラミック複合粉
体を製造することができる。
By repeating the manufacturing process of the present invention as described above, a ceramic composite powder having a structure of three or more layers can be manufactured.

【0011】[0011]

【作用】金属アルコキシドの有機溶液にセラミック粒子
が分散した懸濁液に水を添加すると、アルコキシドが加
水分解される。その生成物は極めて微細で高活性である
ため、懸濁液中に浮遊しているセラミック粒子の表面に
容易に付着するとともに低温の加熱により容易に金属酸
化物を生成する。この結果、セラミック複合粉体の内核
を構成するセラミック粒子と外核を構成する金属酸化物
は互いに化学反応を生じることなく二層またはそれ以上
の多層構造を維持する。
When the water is added to the suspension in which the ceramic particles are dispersed in the organic solution of the metal alkoxide, the alkoxide is hydrolyzed. Since the product is extremely fine and highly active, it easily adheres to the surface of the ceramic particles suspended in the suspension and easily forms a metal oxide by heating at low temperature. As a result, the ceramic particles forming the inner core and the metal oxide forming the outer core of the ceramic composite powder maintain a multilayer structure of two or more layers without causing chemical reaction with each other.

【0012】[0012]

【発明の効果】以上述べたように、本発明によれば、セ
ラミック複合粉体の内核を構成するセラミック粒子の周
りに製造工程中においてこれと化学反応しない金属酸化
物の粒子を外核として付着させることができ、内核と外
核の各々の材料の機能を自由に選択できる。これによ
り、複数の機能を同時に併せて持つセラミック複合粉体
が得られる。
As described above, according to the present invention, metal oxide particles which do not chemically react with the ceramic particles constituting the inner core of the ceramic composite powder during the manufacturing process are attached as the outer core. The function of each material of the inner core and the outer core can be freely selected. As a result, a ceramic composite powder having a plurality of functions simultaneously can be obtained.

【0013】[0013]

【実施例】次に本発明の実施例を説明する。エタノール
100gにジルコニウムブトキシド[Zr(OC49
4]20gを溶解し、この溶液に市販のBaTiO3粉末
(平均粒径0.3μm)2gを加え、超音波により分散
させて、チタン酸バリウム懸濁液を調製した。この懸濁
液に水20gを加えて、Zr(OC494を加水分解
し、Zrの水和物を生成させた。この水和物は極めて微
粒子であるため、生成と同時に懸濁液に浮遊しているB
aTiO3粒子の表面に付着した。このBaTiO3粒子
を含有する懸濁液を80℃で一晩(16時間)加熱し懸
濁液の溶媒を蒸発して乾燥した。この乾燥物を400℃
で1時間加熱した。得られた粉体の粒径は約0.6μm
であり、X線回折の結果からBaTiO3とZrO2から
構成されていることが判明した。
EXAMPLES Next, examples of the present invention will be described. Zirconium butoxide [Zr (OC 4 H 9 ) was added to 100 g of ethanol.
4 ] 20 g was dissolved, 2 g of commercially available BaTiO 3 powder (average particle size 0.3 μm) was added to this solution, and the mixture was ultrasonically dispersed to prepare a barium titanate suspension. 20 g of water was added to this suspension to hydrolyze Zr (OC 4 H 9 ) 4 to produce a hydrate of Zr. Since this hydrate is extremely fine particles, it is suspended in the suspension as soon as it is formed.
It adhered to the surface of the aTiO 3 particles. The suspension containing the BaTiO 3 particles was heated at 80 ° C. overnight (16 hours) and the solvent of the suspension was evaporated to dryness. This dried product is 400 ℃
Heated for 1 hour. The particle size of the obtained powder is about 0.6 μm
From the result of X-ray diffraction, it was found to be composed of BaTiO 3 and ZrO 2 .

Claims (2)

【特許請求の範囲】[Claims] 【請求項1】 有機溶剤に金属アルコキシドを溶解して
アルコキシド溶液を調製する工程と、この溶液にセラミ
ック粒子を分散してセラミック懸濁液を調製する工程
と、この懸濁液に水を加えて前記アルコキシドを加水分
解し、この加水分解生成物が前記セラミック粒子の表面
に付着した複合体を調製する工程と、この複合体を乾燥
加熱して前記加水分解生成物を金属酸化物粒子に変え、
前記セラミック粒子を核として、その周りに金属酸化物
粒子が付着したセラミック複合粉体を得る工程とを含む
セラミック複合粉体の製造方法。
1. A step of dissolving a metal alkoxide in an organic solvent to prepare an alkoxide solution, a step of dispersing ceramic particles in the solution to prepare a ceramic suspension, and adding water to the suspension. A step of hydrolyzing the alkoxide, preparing a complex in which the hydrolysis product is attached to the surface of the ceramic particles, and drying and heating the complex to convert the hydrolysis product into metal oxide particles,
A method of producing a ceramic composite powder, which comprises the step of obtaining a ceramic composite powder having metal oxide particles attached to the periphery of the ceramic particles as a core.
【請求項2】 アルコキシド溶液に超音波を加えてセラ
ミック粒子を分散する請求項1記載のセラミック複合粉
体の製造方法。
2. The method for producing a ceramic composite powder according to claim 1, wherein ultrasonic waves are applied to the alkoxide solution to disperse the ceramic particles.
JP24445091A 1991-08-29 1991-08-29 Production of ceramic composite powder Pending JPH0558605A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP24445091A JPH0558605A (en) 1991-08-29 1991-08-29 Production of ceramic composite powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP24445091A JPH0558605A (en) 1991-08-29 1991-08-29 Production of ceramic composite powder

Publications (1)

Publication Number Publication Date
JPH0558605A true JPH0558605A (en) 1993-03-09

Family

ID=17118837

Family Applications (1)

Application Number Title Priority Date Filing Date
JP24445091A Pending JPH0558605A (en) 1991-08-29 1991-08-29 Production of ceramic composite powder

Country Status (1)

Country Link
JP (1) JPH0558605A (en)

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998035920A1 (en) * 1997-02-18 1998-08-20 Cabot Corporation Dispersible, metal oxide-coated, barium titanate materials
WO2003004416A1 (en) * 2001-07-04 2003-01-16 Showa Denko K. K. Barium titanate and its production method
US6656590B2 (en) 2001-01-10 2003-12-02 Cabot Corporation Coated barium titanate-based particles and process
US6673274B2 (en) 2001-04-11 2004-01-06 Cabot Corporation Dielectric compositions and methods to form the same
JP2007091549A (en) * 2005-09-29 2007-04-12 Showa Denko Kk Shell component-containing perovskite composite oxide powder and its manufacturing method
US7431911B2 (en) 2001-07-04 2008-10-07 Showa Denko K.K. Barium titanate and production and process thereof
USRE42433E1 (en) 2000-02-28 2011-06-07 Samsung Sdi Co., Ltd. Positive active material for rechargeable lithium battery and method of preparing same
CN113402203A (en) * 2021-06-18 2021-09-17 Oppo广东移动通信有限公司 Ceramic composite material, preparation method thereof, shell and electronic equipment

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58185440A (en) * 1982-04-21 1983-10-29 Seiko Epson Corp Synthetic silica glass and preparation thereof
JPS59169905A (en) * 1983-03-16 1984-09-26 Inoue Japax Res Inc Production of metal double oxide
JPS62148213A (en) * 1985-12-23 1987-07-02 株式会社東芝 Manufacture of material for ceramics
JPH0218441A (en) * 1988-07-07 1990-01-22 Shin Etsu Chem Co Ltd Vinyl chloride resin composition
JPH0350105A (en) * 1989-04-07 1991-03-04 Nippon Shokubai Kagaku Kogyo Co Ltd Production of inorganic oxide grains
JPH03164408A (en) * 1989-07-20 1991-07-16 Solvay & Cie Manufacture of composite material of metal oxide, composite powder material of metal oxide and ceramic material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS58185440A (en) * 1982-04-21 1983-10-29 Seiko Epson Corp Synthetic silica glass and preparation thereof
JPS59169905A (en) * 1983-03-16 1984-09-26 Inoue Japax Res Inc Production of metal double oxide
JPS62148213A (en) * 1985-12-23 1987-07-02 株式会社東芝 Manufacture of material for ceramics
JPH0218441A (en) * 1988-07-07 1990-01-22 Shin Etsu Chem Co Ltd Vinyl chloride resin composition
JPH0350105A (en) * 1989-04-07 1991-03-04 Nippon Shokubai Kagaku Kogyo Co Ltd Production of inorganic oxide grains
JPH03164408A (en) * 1989-07-20 1991-07-16 Solvay & Cie Manufacture of composite material of metal oxide, composite powder material of metal oxide and ceramic material

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1998035920A1 (en) * 1997-02-18 1998-08-20 Cabot Corporation Dispersible, metal oxide-coated, barium titanate materials
USRE42433E1 (en) 2000-02-28 2011-06-07 Samsung Sdi Co., Ltd. Positive active material for rechargeable lithium battery and method of preparing same
US6656590B2 (en) 2001-01-10 2003-12-02 Cabot Corporation Coated barium titanate-based particles and process
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