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JPH0297424A - Production of alumina-zirconia double oxides powder - Google Patents

Production of alumina-zirconia double oxides powder

Info

Publication number
JPH0297424A
JPH0297424A JP63251503A JP25150388A JPH0297424A JP H0297424 A JPH0297424 A JP H0297424A JP 63251503 A JP63251503 A JP 63251503A JP 25150388 A JP25150388 A JP 25150388A JP H0297424 A JPH0297424 A JP H0297424A
Authority
JP
Japan
Prior art keywords
alumina
zirconia
slurry
powder
dispersant
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
JP63251503A
Other languages
Japanese (ja)
Inventor
Hirohisa Ishimaru
石丸 博久
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.)
Iwao Jiki Kogyo Co Ltd
Original Assignee
Iwao Jiki Kogyo Co Ltd
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 Iwao Jiki Kogyo Co Ltd filed Critical Iwao Jiki Kogyo Co Ltd
Priority to JP63251503A priority Critical patent/JPH0297424A/en
Publication of JPH0297424A publication Critical patent/JPH0297424A/en
Pending legal-status Critical Current

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  • Compositions Of Oxide Ceramics (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

PURPOSE:To obtain the uniformly dispersed alumina-zirconia double oxides powder by adding a dispersant into the neutral slurry of alumina-zirconia, stirring the mixture with a ball mill, further finely dispersing the slurry and subjecting the slurry to spray drying. CONSTITUTION:Water and acidic dispersion such as acetic acid are added to zirconia powder and alumina powder and the mixture is stirred with the ball mill until the pH attains 2 to 4. The aq. ammonia or/and ammonium carbonate are mixed with the acidic slurry of the alumina-zirconia to produce the neutral slurry of the alumina-zirconia. Further, the dispersant such as ammonium polyacrylate salt is added to the neutral slurry of the alumina-zirconia and the slurry is stirred in the ball mill. Further, the slurry is finely dispersed by an attriter mill, etc., and is subjected to spray drying, by which the double oxides power is obtd. The reason for adding the alkaline dispersant to the slurry in the above-mentioned manner is to obtain the multiple body uniformly dispersed with the alumina and the zirconia as there is difference in delfocculating pH between the alumina and the zirconia in an alkaline region and the complete deflocculation of the slurry of the alumina-zirconia does not, consequently, take place.

Description

【発明の詳細な説明】 (産業上の利用分野) 本発明はアルミナ−ジルコニア焼結体を作るためのアル
ミナ−ジルコニア複合粉体の製造方法に関するものであ
る。
DETAILED DESCRIPTION OF THE INVENTION (Field of Industrial Application) The present invention relates to a method for producing an alumina-zirconia composite powder for producing an alumina-zirconia sintered body.

(従来の技ルドj) 一般にセラミック焼結体において、より低温でち密化さ
せることができれば単に焼結に必要な熱エネルギーの節
約になるのみならず、焼結体の機械的強度の向上にもつ
ながる。これまでアルミナ焼結体の靭性及び強度を改善
するためのアルミナ−ジルコニア焼結体ではアルミナ粉
末とジルコニア粉末とをミルでtl混合しジルコニア微
粒子をアルミナ粒子間に均一に分散する方法により製造
されていた。しかし、このジルコニア微粒子は平均粒径
0,5μIn以下で凝集性が強いのでジルコニアの分散
が不十分で、工業的にそのような微粒子のジルコニアを
分散させたアルミナ焼結体を製造した場合、性能向上に
限界がある。そこで特開昭61−275159号に示さ
れるようにアルミナ粉末とジルコニア粉末とに分散剤を
添加して湿式混合することによりアルミナとジルコニア
とを均一に分散する方法が述べられている。
(Conventional technique) In general, if a ceramic sintered body can be densified at a lower temperature, it will not only save the thermal energy required for sintering, but also improve the mechanical strength of the sintered body. Connect. Until now, alumina-zirconia sintered bodies for improving the toughness and strength of alumina sintered bodies have been produced by mixing alumina powder and zirconia powder in a mill to uniformly disperse zirconia particles among the alumina particles. Ta. However, these zirconia fine particles have an average particle size of 0.5 μIn or less and have strong agglomeration, so the dispersion of zirconia is insufficient. There are limits to improvement. Therefore, as shown in JP-A No. 61-275159, a method is described in which a dispersant is added to alumina powder and zirconia powder and wet-mixed to uniformly disperse alumina and zirconia powder.

(発明が解決しようとする′:a題) ところが、アルミナとジルコニアとではその密度に違い
があり、またアルミナ粒子とジルコニア粒、子とではそ
の粒径が大きく異なり、アルミナ粉末とジルコニア粉末
とをこのように分散剤を添加して湿式混合しても粒径の
大小により粒径の小さいジルコニア粒子が液の上方に偏
在しやすいと云う欠点があった。しかもアルカリ性での
両者の最適分散のI) I(に違いがあり、通常アルミ
ナの分散に11(点がおかれており、アルミナ粉末とジ
ルコニア粉末との均一分散が不十分であった。本発明の
目的はこのような従来のアルミナ−ジルコニア複合粉体
の製造方法における以上のような欠点を解消することを
目的とし、たちのである。
(Problem to be solved by the invention: A) However, there is a difference in density between alumina and zirconia, and a large difference in particle size between alumina particles and zirconia particles. Even if a dispersant is added and wet-mixed in this way, there is a drawback that zirconia particles with small particle sizes tend to be unevenly distributed above the liquid depending on the size of the particles. Moreover, there is a difference in the optimal dispersion of the two in alkaline conditions, and a score of 11 (point 11) is usually given to the dispersion of alumina, resulting in insufficient uniform dispersion of alumina powder and zirconia powder.The present invention The purpose of the present invention is to eliminate the above-mentioned drawbacks in the conventional method for producing alumina-zirconia composite powder.

(1題を解決するための手段) 本発明はこの目的を達成させるため、従来技術に於ける
湿式混合の前段としてアルミナ粉末及びジルコニア粉末
を酸性の分散剤で分散し、さらにこの酸性スラリーを解
 分散状態で凝集させアルミナ−ジルコニアの均一混合
物を得、これを湿式混合のJに<科としたものである。
(Means for Solving Problem 1) In order to achieve this object, the present invention disperses alumina powder and zirconia powder with an acidic dispersant as a pre-stage of wet mixing in the prior art, and further disperses this acidic slurry. A uniform mixture of alumina and zirconia was obtained by agglomerating in a dispersed state, and this was used as a wet-mixing method.

すなわちアルミナ粉末とジルコニア粉末とに水と酢酸等
の酸性分散液とを添加、ボールミルで攪拌してP Hを
2〜4にしてアルミナ粉末とジルコニア粉末とを均一分
散させ、このアルミナ−ジルコニアの酸性スラリーにア
ンモニア水或は/及び炭酸アンモニウムを混ぜアルミナ
−ジルコニアの中性スラリーとなし、このアルミナ−ジ
ルコニアの中性スラリーにポリアクリル酸アンモニウム
塩等の分散剤を加えボールミルで攪拌し、更に71−ラ
イターミルにて細かに分散した後スプレードライしたも
のである。なお、本発明の酸性分散剤としては混合して
pHが2〜4程度となる酢酸等が好適である。また、中
和のための中和剤としてはアンモニア水。
That is, water and an acidic dispersion such as acetic acid are added to alumina powder and zirconia powder, and the alumina powder and zirconia powder are uniformly dispersed by stirring with a ball mill to adjust the pH to 2 to 4. The slurry is mixed with aqueous ammonia and/or ammonium carbonate to obtain a neutral slurry of alumina-zirconia, and a dispersant such as ammonium polyacrylate is added to the neutral slurry of alumina-zirconia and stirred in a ball mill. It was finely dispersed using a lighter mill and then spray-dried. In addition, as the acidic dispersant of the present invention, acetic acid or the like whose pH becomes about 2 to 4 when mixed is suitable. Also, ammonia water is used as a neutralizing agent for neutralization.

炭酸アンモニウム、あるいはアンモニア水と炭酸アンモ
ニウムとを混合したアルカリ性の溶液を用いる。この中
和剤による中性スラリーはアルミナとジルコニアとが均
一に分散された状態で凝集される。このアルミナ−ジル
コニア凝集体を含む中性スラリーは、アルミナ、ジルコ
ニアが凝集しているため、アルミナ−ジルコニアの粘度
の高いスラリーとなる。この凝集された中性のアルミナ
−ジルコニア粒子を含むスラリーにアルカリ性の分散、
剤を混合してボールミルで混合し、更にアトライターミ
ルにて細かに分11シし粘度の低いアルミナ−ジルコニ
アの分散したスラリーとなるわけである。なお1分散剤
としてはポリアクリル酸アンモニウムj−等の焼成後灰
分が残らない有機性の分;1ぐ剤を用いる。
Use ammonium carbonate or an alkaline solution of aqueous ammonia and ammonium carbonate. The neutral slurry produced by this neutralizing agent is agglomerated in a state in which alumina and zirconia are uniformly dispersed. This neutral slurry containing alumina-zirconia aggregates is a highly viscous alumina-zirconia slurry because alumina and zirconia are aggregated. An alkaline dispersion is applied to the slurry containing the agglomerated neutral alumina-zirconia particles.
The ingredients are mixed in a ball mill, and further finely divided in an attritor mill to form a slurry in which alumina-zirconia is dispersed and has a low viscosity. As the dispersant, an organic dispersant such as ammonium polyacrylate that leaves no ash after firing is used.

(作用) 本発明に於てアルミナ粉末とジルコニア粉末とをI) 
82〜4の酸性スラリーに解膠し、さらに凝集させるの
は、アルミナ粉末とジルコニア粉末との粒径差にもとす
くジルコニア粉末の偏在がないように、アルミナとジル
コニアとを均一に分散した状態でアルミナ−ジルコニア
の凝集体を得るためである。また、このアルミナ−ジル
コニアの凝集体にポリアクリル酸アンモニウム塩等のア
ルカリ性の分散剤を添加するのは、アルミナとジルコニ
アとではアルカリ性領域で解Jll 1) H領域に違
いがあるため、アルミナ−ジルコニアのスラリーは完全
に解膠されずアルミナとジルコニアとが均一に分散した
アルミナ−ジルコニア複合粉体を得るた、めである。
(Function) In the present invention, alumina powder and zirconia powder I)
Peptizing the acidic slurry of No. 82-4 and further agglomerating it is due to the difference in particle size between the alumina powder and the zirconia powder.Alumina and zirconia are uniformly dispersed so that the zirconia powder is not unevenly distributed. This is to obtain alumina-zirconia aggregates. In addition, adding an alkaline dispersant such as ammonium polyacrylate to this alumina-zirconia aggregate is important because alumina and zirconia have different alkaline regions. This is to obtain an alumina-zirconia composite powder in which the slurry is not completely peptized and alumina and zirconia are uniformly dispersed.

(実施例) 次に本発明の実施例を述べる。(Example) Next, examples of the present invention will be described.

X旌■ユ アルミナ(昭和電工製1608G−1平均粒径0 、6
1t rn ) 800 gとイツトリアで安定化した
ジルコニア(東ソー製T 7. OY平均粒径0.37
重m)200gとを規定の酢酸水溶液と混ぜ固形分50
重tJ(%となし、容」ij 2000 m lのアル
ミナ製ボッ1−ミルで8時間攪拌する。このアルミナ−
ジルコニアを分散した酸性スラリーのP Hは3゜5で
あった。この酸性スラリーに最初P[(6,5までアン
モニア水を混合し2次にP H7まで炭酸アンモニウム
を混合し、アルミナ−ジルコニアの凝集体(平均粒径1
0um)を含むスラリーを得る。この人ラリ−のPHは
7.2程度である1次に、このスラリーにポリアクリル
酸アンモニウム塩を混ぜ、ボールミルで10時間混合分
散し、更に分散を良くするため10分間アトライターミ
ルで混合攪拌する。出来たスラリーのP Hは9,8で
、あった6又、スラリーの粘度はLOOcpであった。
X 旌■ Yualumina (Showa Denko 1608G-1 average particle size 0, 6
1 t rn ) 800 g and Ittria stabilized zirconia (Tosoh T 7. OY average particle size 0.37
Mix 200g of solids with the specified acetic acid aqueous solution to obtain a solid content of 50
Stir in a 2000 ml alumina bottle mill for 8 hours.
The pH of the acidic slurry in which zirconia was dispersed was 3.5. This acidic slurry was first mixed with ammonia water up to P[(6.5), and then with ammonium carbonate until pH7.
A slurry containing 0 um) is obtained. The pH of this slurry is about 7.2. First, ammonium polyacrylate is mixed with this slurry, mixed and dispersed in a ball mill for 10 hours, and then mixed and stirred in an attritor mill for 10 minutes to improve the dispersion. do. The pH of the resulting slurry was 9.8, the viscosity of the slurry was LOOcp.

このスラリーはスプレードライヤーで造粒乾燥されアル
ミナ−ジルコニアが均一に分散された粒子を得る。
This slurry is granulated and dried with a spray dryer to obtain particles in which alumina-zirconia is uniformly dispersed.

なお、出来たアルミナ−ジルコニアの造粒物を1500
kg/aイで成形し、1550℃で焼成した。
In addition, the resulting alumina-zirconia granules were
kg/a, and fired at 1550°C.

出来た焼成物の相対密度は98ヅ1、曲げ強度は850
0 kg / cJであった。また本実施例の造粒物は
通常のアルミナ−ジルコニア焼結体(焼成湿度1600
℃)よりより低温で焼結体を得る事ができる。
The relative density of the baked product is 98㎜1, and the bending strength is 850.
It was 0 kg/cJ. Further, the granules of this example are ordinary alumina-zirconia sintered bodies (sintering humidity 1600
It is possible to obtain a sintered body at a lower temperature than (℃).

ル3d肚1 実施例1と同様に配合したアルミナ粉末とジルコニア粉
末にポリアクリル酸アンモニウム塩を添加ボールミルで
48時間アトライターミルで1時間混合しスプレードラ
イヤーで乾燥、実施例1と同様に成形、焼成した。焼成
体の特性は曲げ強度6500 kg / aJなお、焼
成M1度1600℃の焼結体の相対密度98%、010
ブ強度7200kg/aJであった。
1. Add polyacrylic acid ammonium salt to alumina powder and zirconia powder mixed in the same manner as in Example 1. Mix in a ball mill for 48 hours and in an attritor mill for 1 hour, dry in a spray dryer, mold in the same manner as in Example 1, Fired. The characteristics of the sintered body are bending strength of 6500 kg/aJ.The relative density of the sintered body after firing M1 degree of 1600℃ is 98%, 010
The strength was 7200 kg/aJ.

(、効果) 本発明は以上のようにアルミナ粉末とジルコニア粉末と
に酢酸等の酸性分散液を混ぜ酸性のスラリーとしている
ため、この酸性スラリーの中にはアルミナとジルコニア
の粉末は十分に解胎され、均一に分散される。
(Effects) As described above, the present invention mixes alumina powder and zirconia powder with an acidic dispersion such as acetic acid to form an acidic slurry. and evenly distributed.

しかも、このアルミナ−ジルコニアを分散した酸性スラ
リーはその後アンモニア水等の塩基性塩で凝集されるが
この凝集体はアルミナとジルコニアが十分にM、膠1分
散されているためアルミナとジルコニアの凝集体となる
。このアルミナ−ジルコニア凝集体を更に分散させるた
め、アルミナの一次粒子、ジルコニアの一次粒子が接合
した状態で分散されるためアルミナ−ジルコニアが粒径
差により偏在しない均一に分散されたスラリーを得るこ
とができ、これをスプレードライヤーで乾燥すれば均一
に分散したアルミナ−ジルコニア複金粉体を得ることが
できる。この複合粉体を成形、焼成すると、比較的低い
温度でしかも強度的に大きなジルコニアが均一に分散さ
れた焼結体を得ること、ができる。また、このアルミナ
−ジルコニア複合PJ)体はアルカリ性であり成形時、
成形機等に腐食等の問題が生ずることもない6
Moreover, this acidic slurry in which alumina-zirconia is dispersed is then aggregated with a basic salt such as aqueous ammonia, but since alumina and zirconia are sufficiently dispersed in M and glue, the aggregates are alumina and zirconia aggregates. becomes. In order to further disperse this alumina-zirconia aggregate, the primary particles of alumina and the primary particles of zirconia are dispersed in a bonded state, making it possible to obtain a uniformly dispersed slurry in which the alumina-zirconia is not unevenly distributed due to the difference in particle size. By drying this with a spray dryer, uniformly dispersed alumina-zirconia composite gold powder can be obtained. By molding and firing this composite powder, it is possible to obtain a sintered body in which zirconia having high strength is uniformly dispersed at a relatively low temperature. In addition, this alumina-zirconia composite PJ) body is alkaline and during molding,
No problems such as corrosion will occur in molding machines, etc.6

Claims (1)

【特許請求の範囲】[Claims]  ジルコニア粉末とアルミナ粉末とに水と酢酸等の酸性
分散液とを添加、ボールミルで攪拌してPHを2〜4と
なし、このアルミナ−ジルコニアの酸性スラリーにアン
モニア水或は/及びに炭酸アンモニウムを混ぜアルミナ
−ジルコニアの中性スラリーとなし、更にこのアルミナ
−ジルコニアの中性スラリーにポリアクリル酸アンモニ
ウム塩等の分散剤を加えボールミルで撹拌して、更にア
トライターミル等にて細かに分散してスプレードライし
たことを特徴とするアルミナ−ジルコニア複合粉体の製
造方法。
Add water and an acidic dispersion such as acetic acid to zirconia powder and alumina powder, stir in a ball mill to adjust the pH to 2 to 4, and add ammonia water or/and ammonium carbonate to this alumina-zirconia acid slurry. A neutral slurry of mixed alumina-zirconia is prepared, and then a dispersant such as ammonium polyacrylate is added to this neutral slurry of alumina-zirconia, stirred in a ball mill, and further finely dispersed in an attritor mill, etc. A method for producing an alumina-zirconia composite powder characterized by spray drying.
JP63251503A 1988-10-04 1988-10-04 Production of alumina-zirconia double oxides powder Pending JPH0297424A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP63251503A JPH0297424A (en) 1988-10-04 1988-10-04 Production of alumina-zirconia double oxides powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP63251503A JPH0297424A (en) 1988-10-04 1988-10-04 Production of alumina-zirconia double oxides powder

Publications (1)

Publication Number Publication Date
JPH0297424A true JPH0297424A (en) 1990-04-10

Family

ID=17223777

Family Applications (1)

Application Number Title Priority Date Filing Date
JP63251503A Pending JPH0297424A (en) 1988-10-04 1988-10-04 Production of alumina-zirconia double oxides powder

Country Status (1)

Country Link
JP (1) JPH0297424A (en)

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04317453A (en) * 1991-04-11 1992-11-09 Murata Mfg Co Ltd Production of ceramic green sheet
US7708788B2 (en) 1996-09-30 2010-05-04 Hitachi Chemical Co, Ltd. Cerium oxide abrasive and method of polishing substrates
CN101941836A (en) * 2010-08-30 2011-01-12 济源市更新瓷料有限公司 Low-temperature ceramic-firing high-density alumina ceramic granulation powder and preparation method thereof
US7871308B2 (en) 1997-12-18 2011-01-18 Hitachi Chemical Company, Ltd. Abrasive, method of polishing target member and process for producing semiconductor device
JP2013514960A (en) * 2009-12-21 2013-05-02 コンセホ スペリオール デ インベスティガシオネス シエンティフィカス(セエセイセ) COMPOSITE MATERIAL WITH CONTROLLED CTE, INCLUDING OXIDE CERAMIC AND PROCESS FOR OBTAINING THE COMPOSITE MATERIAL

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH04317453A (en) * 1991-04-11 1992-11-09 Murata Mfg Co Ltd Production of ceramic green sheet
US7708788B2 (en) 1996-09-30 2010-05-04 Hitachi Chemical Co, Ltd. Cerium oxide abrasive and method of polishing substrates
US7867303B2 (en) 1996-09-30 2011-01-11 Hitachi Chemical Co., Ltd. Cerium oxide abrasive and method of polishing substrates
US7871308B2 (en) 1997-12-18 2011-01-18 Hitachi Chemical Company, Ltd. Abrasive, method of polishing target member and process for producing semiconductor device
US7963825B2 (en) 1997-12-18 2011-06-21 Hitachi Chemical Company, Ltd. Abrasive, method of polishing target member and process for producing semiconductor device
US8137159B2 (en) 1997-12-18 2012-03-20 Hitachi Chemical Company, Ltd. Abrasive, method of polishing target member and process for producing semiconductor device
US8162725B2 (en) 1997-12-18 2012-04-24 Hitachi Chemical Company, Ltd. Abrasive, method of polishing target member and process for producing semiconductor device
US8616936B2 (en) 1997-12-18 2013-12-31 Hitachi Chemical Company, Ltd. Abrasive, method of polishing target member and process for producing semiconductor device
JP2013514960A (en) * 2009-12-21 2013-05-02 コンセホ スペリオール デ インベスティガシオネス シエンティフィカス(セエセイセ) COMPOSITE MATERIAL WITH CONTROLLED CTE, INCLUDING OXIDE CERAMIC AND PROCESS FOR OBTAINING THE COMPOSITE MATERIAL
CN101941836A (en) * 2010-08-30 2011-01-12 济源市更新瓷料有限公司 Low-temperature ceramic-firing high-density alumina ceramic granulation powder and preparation method thereof

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