JPH01141817A - Production of translucent alumina material powder - Google Patents

Production of translucent alumina material powder

Info

Publication number
JPH01141817A
JPH01141817A JP62298584A JP29858487A JPH01141817A JP H01141817 A JPH01141817 A JP H01141817A JP 62298584 A JP62298584 A JP 62298584A JP 29858487 A JP29858487 A JP 29858487A JP H01141817 A JPH01141817 A JP H01141817A
Authority
JP
Japan
Prior art keywords
alumina
material powder
soln
powder
alkoxide
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.)
Granted
Application number
JP62298584A
Other languages
Japanese (ja)
Other versions
JP2508541B2 (en
Inventor
Keiichi Iida
飯田 恵一
Shoichi Shimamura
島村 正一
Keisuke Morita
啓介 森田
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 Mining and Cement Co Ltd
Original Assignee
Mitsubishi Mining and Cement Co Ltd
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Publication date
Application filed by Mitsubishi Mining and Cement Co Ltd filed Critical Mitsubishi Mining and Cement Co Ltd
Priority to JP62298584A priority Critical patent/JP2508541B2/en
Publication of JPH01141817A publication Critical patent/JPH01141817A/en
Application granted granted Critical
Publication of JP2508541B2 publication Critical patent/JP2508541B2/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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  • Compositions Of Oxide Ceramics (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

PURPOSE:To obtain alumina material fine powder having high purity and excellent translucency due to homogeneously growing grains, by adding metal Mg to an org. solvent soln. of Al alkoxide in a fixed proportion to the alumina in the soln., thereafter by hydrolyzing, by drying the separated hydrolyzate and by calcining. CONSTITUTION:The Al alkoxide such as aluminum isopropoxide is preferably dissolved in the org. solvent consisting of mixed solvent of isopropanol and benzene. Then, in the org. solvent soln., 0.1-10wt.% metal Mg to the amt. of Al alkoxide in the soln., expressed in terms of alumina is dissolved by heating, and thereafter, the soln. is hydrolyzed. The hydrolyzate is separated from the hydrolyzed liq. by centrifugation, filtration, etc., and dried. The dry material is preferably calcined at >=1,150 deg.C to obtain the target transparent alumina material powder. The material powder has high purity and is highly characteristic fine particle with Mg component homogeneously distributed.

Description

【発明の詳細な説明】 [産業上の利用分野] 本発明は透光性アルミナ(Aj720z )原料粉の製
造方法に係り、特に、均一な粒成長による、高純度で且
つ緻密な、透光性に優れたアルミナ焼結体を得ることが
できる透光性アルミナ原料粉の製造方法に関するもので
ある。
[Detailed Description of the Invention] [Industrial Application Field] The present invention relates to a method for producing translucent alumina (Aj720z) raw material powder. The present invention relates to a method for producing a translucent alumina raw material powder that can produce an alumina sintered body with excellent properties.

[従来の技術] 従来、透光性アルミナにみられるような緻密なアルミナ
焼結体は、高純度な原料粉を成形して得た成形体を焼結
過程において粒成長を抑制して焼結することにより製造
されている。この粒成長の抑制には、MgOの微量添加
が不可欠であり、その添加方法としては ■ AJ2203粉末に所定量のMgO粉末を加え、ボ
ールミル或いは他の機械的操作により混合する。
[Conventional technology] Conventionally, dense alumina sintered bodies such as those found in translucent alumina have been produced by molding high-purity raw material powder and then sintering the molded body by suppressing grain growth during the sintering process. It is manufactured by In order to suppress this grain growth, it is essential to add a small amount of MgO, and the method for adding it is as follows: (1) A predetermined amount of MgO powder is added to AJ2203 powder and mixed by a ball mill or other mechanical operation.

■ A J! 2’02粉末を溶媒に加えてスラリーと
し、この溶液に可溶性のMg塩を添加して混合する。(
又は逆にMg溶解液にAJ!203粉末を添加混合する
。) ■ アルミニウムアルコキシドとマグネシウムアルコキ
シドを共通の溶媒に溶解し混合する。
■ AJ! The 2'02 powder is added to a solvent to form a slurry, and a soluble Mg salt is added to this solution and mixed. (
Or conversely, add AJ to the Mg solution! Add and mix 203 powder. ) ■ Dissolve aluminum alkoxide and magnesium alkoxide in a common solvent and mix.

等が考えられている。etc. are being considered.

■、■の方法でMgOを混合した後は、AfL203粉
末は、通常、濾過、乾燥、仮焼等の工程を経て原料粉末
とされていた。■の方法で混合を行なった場合には、両
アルコキシド混合液を加水分解後、濾過、乾燥、仮焼等
の工程に供していた。
After mixing MgO using methods ① and ②, the AfL203 powder is usually made into a raw material powder through processes such as filtration, drying, and calcining. When mixing was carried out by method (2), the mixed solution of both alkoxides was hydrolyzed and then subjected to steps such as filtration, drying, and calcining.

ところでアルミナ焼結体は、気孔が著しく少なく極めて
緻密に焼結されると透光性を示す。このような透光性を
示す緻密なアルミナ焼結体を得ようとする場合、そのm
密性は用いる原料粉に影響を受ける。原料粉としては高
純度で且つMgOが微量添加されたAiL20s原料粉
末であることが好ましい。このような原料粉を用いるこ
とにより、高純度で粒界や粒子内に気孔又は空孔、を含
まず、また、粒界に不純物の析出もない高特性の焼結体
が得られ、このような焼結体であれば著しく優れた透光
性を示す。
Incidentally, an alumina sintered body exhibits translucency when sintered extremely densely with very few pores. When trying to obtain a dense alumina sintered body that exhibits such translucency, its m
Density is affected by the raw material powder used. The raw material powder is preferably AiL20s raw powder with high purity and a trace amount of MgO added. By using such raw material powder, it is possible to obtain a sintered body with high purity, no pores or voids in the grain boundaries or within the grains, and no precipitation of impurities at the grain boundaries. If it is a sintered body, it exhibits extremely excellent translucency.

[発明が解決しようとする問題点] このような状況のもとで、従来、前記■〜■のような高
純度なアルミナにMgOを添加する方法が考えられてき
たのであるが、これらの方法はそれぞれ次のような欠点
を有していた。
[Problems to be solved by the invention] Under these circumstances, methods of adding MgO to high-purity alumina, such as those described in (1) to (3) above, have been considered. Each had the following drawbacks.

■の方法は、機械的、長時間の粉末同志の混合であるた
めに不純物の混入の問題があるほか、MgOの分布も不
均一となる。■の方法も機械的な混合であるため、やは
りある程度のMgOの不均一な分布は免れない。■の方
法は、■、■の方法に比べ比較的MgOの分布の均一性
は良いものの、アルコキシドは比較的高価であり、2種
のアルコキシドを用いることはコスト高となり、工業的
に不利である。
In method (2), since the powders are mixed mechanically and over a long period of time, there is a problem of contamination with impurities, and the distribution of MgO is also non-uniform. Since the method (2) also involves mechanical mixing, some degree of uneven distribution of MgO is inevitable. Although method (2) has relatively better uniformity of MgO distribution than methods (2) and (2), alkoxides are relatively expensive, and using two types of alkoxides increases costs, which is industrially disadvantageous. .

また、アルコキシドは水分に敏感であるため、取り扱い
が難しく、特にマグネシウムアルコキシドは加水分解が
速く、操作上厳密な注意を怠った場合にはすぐに加水分
解反応を起こして溶媒に不溶となるため、均一混合が困
難となるという欠点もある。しかも、代表的なマグネシ
ウムアルコキシドであるマグネシウムメトキシドは、溶
媒に対する溶解性が低く、溶液中に固体として析出する
場合もあり、取り扱い難いという問題もある。
In addition, alkoxides are sensitive to moisture and are therefore difficult to handle. Magnesium alkoxides in particular hydrolyze quickly, and if strict precautions are not taken during operation, they will immediately undergo a hydrolysis reaction and become insoluble in solvents. Another disadvantage is that uniform mixing becomes difficult. Moreover, magnesium methoxide, which is a typical magnesium alkoxide, has low solubility in solvents and may precipitate as a solid in a solution, making it difficult to handle.

このように、従来の方法では、透光性アルミナ焼結体の
原料粉末として十分に満足し得る原料粉が得られず、そ
の改善が強く望まれていた。
As described above, with the conventional methods, it is not possible to obtain a raw material powder that is fully satisfactory as a raw material powder for a translucent alumina sintered body, and an improvement has been strongly desired.

[問題点を解決するための手段] 上記従来の問題点を解決すべく、本発明者らは、鋭意研
究を重ねた結果、アルミニウムアルコキシドを含む有機
溶媒溶液に、特定量の金属マグネシウムを混合すること
により、透光性アルミナ焼結体の原料粉末として、極め
て優れた特性を有する原料粉が得られることを見出し、
本発明を完成させた。
[Means for Solving the Problems] In order to solve the above-mentioned conventional problems, the present inventors, as a result of extensive research, have discovered that a specific amount of magnesium metal is mixed into an organic solvent solution containing aluminum alkoxide. We have discovered that by doing this, we can obtain a raw material powder with extremely excellent properties as a raw material powder for translucent alumina sintered bodies.
The present invention has been completed.

本発明は、アルミニウムアルコキシドの有機溶媒溶液に
、該溶液中のアルミナに対するマグネシア換算で0.1
〜10重量%の金属マグネシウムを加えた後、加水分解
し、得られる加水分解生成物を加水分解液から分離し、
乾燥及び仮焼することを特徴とする透光性アルミナ原料
粉の製造方法を要旨とするものである。
The present invention provides an organic solvent solution of aluminum alkoxide with 0.1% magnesia equivalent to alumina in the solution.
After adding ~10% by weight of magnesium metal, hydrolysis is performed, and the resulting hydrolysis product is separated from the hydrolyzate,
The gist of this invention is a method for producing translucent alumina raw material powder, which is characterized by drying and calcining.

以下、本発明の詳細な説明する。The present invention will be explained in detail below.

アルミニウムアルコキシドとしては、アルミニウムイソ
プロポキシドが挙げられる。その他、アルミニウムエト
キシド、アルミニウムターシャリ−ブトキシド等のアル
ミニウムアルコキシドも採用可能である。
Examples of aluminum alkoxides include aluminum isopropoxide. In addition, aluminum alkoxides such as aluminum ethoxide and aluminum tert-butoxide can also be used.

このようなアルミニウムアルコキシドを溶解させる有機
溶媒としては、イソプロピルアルコール、エタノール、
n−プロピルアルコール、n−ブチルアルコール等のア
ルコールと、ベンゼン、トルエン、キシレン等との混合
溶媒等が挙げられる。特に、本発明においては、溶解性
等の面からイソプロピルアルコールとベンゼンとの混合
溶媒が好ましく、その混合割合はイソプロピルアルコー
ル:ベンゼン=1:10〜1 : 200 (重量比)
程度とするのが好ましい。
Organic solvents for dissolving such aluminum alkoxides include isopropyl alcohol, ethanol,
Examples include mixed solvents of alcohols such as n-propyl alcohol and n-butyl alcohol, and benzene, toluene, and xylene. In particular, in the present invention, a mixed solvent of isopropyl alcohol and benzene is preferred from the viewpoint of solubility, etc., and the mixing ratio is isopropyl alcohol:benzene = 1:10 to 1:200 (weight ratio).
It is preferable to set it as approximately.

このような有機溶媒に溶解させるアルミニウムアルコキ
シドの量については、用いる溶媒の種類等によっても左
右され、特に制限はないが、通常は溶媒12に対し30
0〜400gのアルミニウムアルコキシドを溶解させる
The amount of aluminum alkoxide to be dissolved in such an organic solvent depends on the type of solvent used and is not particularly limited, but it is usually 30 to 12 parts of the solvent.
Dissolve 0-400 g of aluminum alkoxide.

溶解方法としては特に制限はないが、ベンゼン等の溶媒
にアルミニウムイソプロポキシド等のアルミニウムアル
コキシドを混合溶解し、これにイソプロピルアルコール
等を添加混合するのが好ましい。
Although there are no particular limitations on the dissolution method, it is preferable to mix and dissolve an aluminum alkoxide such as aluminum isopropoxide in a solvent such as benzene, and then add and mix isopropyl alcohol or the like.

次いで、このようにして得られたアルミニウムアルコキ
シドの有機溶媒溶液に、溶液中のアルミニウムアルコキ
シドのアルミナ換算量に対するマグネシア換算量で、0
.1〜10重量%の金属マグネシウムを添加して加熱溶
解した後、加水分解する。
Next, to the organic solvent solution of aluminum alkoxide obtained in this way, an amount of 0 magnesia equivalent to the alumina equivalent amount of aluminum alkoxide in the solution was added.
.. 1 to 10% by weight of magnesium metal is added, heated and dissolved, and then hydrolyzed.

この場合、金属マグネシウムの溶解には、塩化第二水銀
、塩化マグネシウム或いは四塩化炭素等の触媒を必要と
するが、本発明においては、不純物として残存すること
のない四塩化炭素を触媒として用いることが好ましい。
In this case, a catalyst such as mercuric chloride, magnesium chloride, or carbon tetrachloride is required to dissolve metallic magnesium, but in the present invention, carbon tetrachloride, which does not remain as an impurity, is used as a catalyst. is preferred.

加水分解は、得られた溶液中に水を直接追加することに
より行うことができる。その他、加圧容器から吹き出す
水蒸気流に接触させる方法も採用可能である。
Hydrolysis can be carried out by adding water directly into the resulting solution. In addition, it is also possible to employ a method in which the material is brought into contact with a stream of water vapor blown out from a pressurized container.

加水分解生成物は、遠心分離、濾過或いは減圧蒸留等に
より加水分解液から分離し、乾燥を行つた後に、仮焼す
ることにより原料粉末を得ることができる。この場合、
仮焼は1150℃以上の温度で行なうのが好ましいが、
必要以上に高い温度で仮焼すると、微粉末が粒成長する
ため注意を要する。仮焼は1150〜1300℃程度で
行なうのが好適である。
The hydrolyzed product is separated from the hydrolyzed liquid by centrifugation, filtration, vacuum distillation, etc., dried, and then calcined to obtain a raw material powder. in this case,
It is preferable to perform calcination at a temperature of 1150°C or higher, but
Care must be taken as calcining at a temperature higher than necessary will cause grain growth of the fine powder. Calcination is preferably carried out at about 1150 to 1300°C.

このような本発明の方法により得られる粉末は、高純度
であり、かつマグネシア成分が均一に分布した高特性微
粒子である。
The powder obtained by the method of the present invention is highly pure and has high characteristics fine particles in which the magnesia component is uniformly distributed.

[作用] 本発明の方法においては、反応過程における接触相手が
水だけであり、機械的操作による不純物の混入がないた
め高純度化が可能である。また、液相中で反応が進行し
、金属マグネシウムが完全に溶解するために、マグネシ
ア成分が極めて均一に分布した粉末が得られる。
[Function] In the method of the present invention, water is the only contact partner in the reaction process, and there is no contamination of impurities due to mechanical operations, so high purity can be achieved. Furthermore, since the reaction proceeds in the liquid phase and metal magnesium is completely dissolved, a powder in which the magnesia component is extremely uniformly distributed can be obtained.

[実施例] 以下、実施例を挙げて本発明をより具体的に説明するが
、本発明はその要旨を超えない限り、以下の実施例に限
定されるものではない。
[Examples] Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited to the following Examples unless it exceeds the gist thereof.

実施例1 アルミニウムイソプロポキシド740.18gをベンゼ
ン1.5j2中に投入し、マグネチックスターラーを用
いて完全に溶解するまで攪拌した。
Example 1 740.18 g of aluminum isopropoxide was placed in 1.5j2 of benzene and stirred using a magnetic stirrer until completely dissolved.

この溶液にイソプロピルアルコール100mAを加えた
後、AjZ203に対するMgO換算で0.1重量%と
なるよう金属マグネシウム0.11gと触媒として四塩
化炭素5mJ2を加え、75℃で一昼夜還流しながら反
応させた。得られた溶液に蒸留水100m1を少量ずつ
滴下して加水分解したところ沈殿物が生成した。この加
水分解生成物である沈殿物を減圧蒸留装置により加水分
解液から分離した後、100℃で一昼夜乾燥して粉末を
得た。得られた粉末は室温下では水酸化物であるため、
1250℃で2時間仮焼してアルミナ原料粉末とした。
After adding 100 mA of isopropyl alcohol to this solution, 0.11 g of metallic magnesium and 5 mJ2 of carbon tetrachloride as a catalyst were added to give a concentration of 0.1% by weight in terms of MgO relative to AjZ203, and the mixture was allowed to react at 75°C under reflux all day and night. When the obtained solution was hydrolyzed by dropping 100 ml of distilled water little by little, a precipitate was generated. The precipitate, which is the hydrolysis product, was separated from the hydrolyzate using a vacuum distillation apparatus, and then dried at 100° C. for one day to obtain a powder. Since the obtained powder is a hydroxide at room temperature,
It was calcined at 1250°C for 2 hours to obtain an alumina raw powder.

この原料粉末を電子顕微鏡によりその粒径を測定したと
ころ、粒径500A〜600Aの均一な微粒子であり、
又、化学分析を行った結果、不純物が0.1重量%以下
の極めて高純度な物質であることが判明した。
When the particle size of this raw material powder was measured using an electron microscope, it was found to be uniform fine particles with a particle size of 500A to 600A.
Further, as a result of chemical analysis, it was found that the material was extremely pure with impurities of 0.1% by weight or less.

゛ この粉末を成形して得られた成形体を1600℃で
焼成し、アルミナ焼結体試料を製造した。この試料面を
表面分析した結果、MgOが均一に分散していることが
確認された。またこの原料粉末を用いて1.5 t /
 c rdにて円板状に加圧成形し、1800℃で8時
間真空炉内で焼成して得られた焼結体は、0.75mm
の厚さで92%の全透過率を示した。
゛ The molded body obtained by molding this powder was fired at 1600°C to produce an alumina sintered body sample. As a result of surface analysis of this sample surface, it was confirmed that MgO was uniformly dispersed. Also, using this raw material powder, 1.5 t/
The sintered body obtained by pressure forming into a disc shape at 1800°C for 8 hours in a vacuum furnace has a diameter of 0.75 mm.
It showed a total transmittance of 92% at a thickness of .

この結果から、本発明で得られる原料粉末によれば、極
めて優れた透光性を有するアルミナ焼結体を製造するこ
とができることが明らかである。
From these results, it is clear that the raw material powder obtained according to the present invention can produce an alumina sintered body having extremely excellent translucency.

[発明の効果] 以上詳述したように、本発明の透光性アルミナ原料粉の
製造方法は、アルミニウムアルコキシドと金属マグネシ
ウムを原料とし、両者の混合溶液を加水分解し、更に加
熱処理するものであって、均−径かつ高純度でしかもM
gOが均一に分布した高特性微粒子を極めて容易に低コ
ストで製造することができる。
[Effects of the Invention] As detailed above, the method for producing translucent alumina raw material powder of the present invention uses aluminum alkoxide and metallic magnesium as raw materials, hydrolyzes a mixed solution of both, and further heat-treats. It has a uniform diameter, high purity, and M
High-performance fine particles in which gO is uniformly distributed can be produced extremely easily and at low cost.

従って、このような本発明で得られるアルミナ粉を透光
性アルミナ焼結体の原料として使用することにより、透
光度が著しく改善された透光性アルミナ焼結体を得るこ
とが可能とされる。
Therefore, by using the alumina powder obtained by the present invention as a raw material for a translucent alumina sintered body, it is possible to obtain a translucent alumina sintered body with significantly improved light transmittance. Ru.

代理人 弁理士  重 野   剛Agent: Patent Attorney Tsuyoshi Shigeno

Claims (3)

【特許請求の範囲】[Claims] (1)アルミニウムアルコキシドの有機溶媒溶液に、該
溶液中のアルミナに対するマグネシア換算で0.1〜1
0重量%の金属マグネシウムを加えた後、加水分解し、
得られる加水分解生成物を加水分解液から分離し、乾燥
及び仮焼することを特徴とする透光性アルミナ原料粉の
製造方法。
(1) Add 0.1 to 1 in terms of magnesia to alumina in the solution to an organic solvent solution of aluminum alkoxide.
After adding 0% by weight of metallic magnesium, hydrolyzing it,
A method for producing a translucent alumina raw material powder, which comprises separating the resulting hydrolysis product from a hydrolysis solution, drying and calcining.
(2)アルミニウムアルコキシドがアルミニウムイソプ
ロポキシドであることを特徴とする特許請求の範囲第1
項に記載の方法。
(2) Claim 1, characterized in that the aluminum alkoxide is aluminum isopropoxide.
The method described in section.
(3)有機溶媒がアルコールを含有することを特徴とす
る特許請求の範囲第1項又は第2項に記載の方法。
(3) The method according to claim 1 or 2, wherein the organic solvent contains alcohol.
JP62298584A 1987-11-26 1987-11-26 Method for producing translucent alumina raw material powder Expired - Lifetime JP2508541B2 (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP62298584A JP2508541B2 (en) 1987-11-26 1987-11-26 Method for producing translucent alumina raw material powder

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP62298584A JP2508541B2 (en) 1987-11-26 1987-11-26 Method for producing translucent alumina raw material powder

Publications (2)

Publication Number Publication Date
JPH01141817A true JPH01141817A (en) 1989-06-02
JP2508541B2 JP2508541B2 (en) 1996-06-19

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Country Link
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110256058A (en) * 2019-06-10 2019-09-20 青海圣诺光电科技有限公司 A kind of preparation method of crystalline ceramics high purity alumina powder

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110256058A (en) * 2019-06-10 2019-09-20 青海圣诺光电科技有限公司 A kind of preparation method of crystalline ceramics high purity alumina powder

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