JPH0624859A - Production of ceramic porous body - Google Patents
Production of ceramic porous bodyInfo
- Publication number
- JPH0624859A JPH0624859A JP19917992A JP19917992A JPH0624859A JP H0624859 A JPH0624859 A JP H0624859A JP 19917992 A JP19917992 A JP 19917992A JP 19917992 A JP19917992 A JP 19917992A JP H0624859 A JPH0624859 A JP H0624859A
- Authority
- JP
- Japan
- Prior art keywords
- ceramic
- slurry
- sludge
- synthetic resin
- resin foam
- 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
Links
Landscapes
- Filtering Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、溶融金属ろ過材、通気
性断熱材、厨房用グリスフィルター、触媒担体などに好
適に用いられる通気、通液抵抗の小さいセラミック多孔
体を製造する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a ceramic porous body having a small resistance to ventilation and liquid passage, which is preferably used for a molten metal filter material, a gas permeable heat insulating material, a grease filter for a kitchen, a catalyst carrier and the like.
【０００２】[0002]
【従来の技術及び発明が解決しようとする課題】従来よ
り、内部連通空間を有する三次元網状骨格構造の合成樹
脂発泡体、例えばセル膜のない軟質ポリウレタンフォー
ムをセラミック泥漿に浸漬してセラミック泥漿を合成樹
脂発泡体に付着させた後、余剰泥漿を除去し、次いで乾
燥、焼成することによってセラミック多孔体を製造する
方法が知られている。このようなセラミック多孔体は、
三次元網状骨格構造を有するため、溶融金属ろ過材、通
気性断熱材、厨房用グリスフィルター、触媒担体用など
として広く使用されているが、これらの用途に使用され
るに当っては、できるかぎり通気、通液抵抗（圧力損
失）が少ないこと、言い換えれば目づまりが少ないこと
が求められる。2. Description of the Related Art Conventionally, a synthetic resin foam having a three-dimensional network skeleton structure having an internal communication space, for example, a soft polyurethane foam without a cell membrane is dipped in the ceramic slurry to form the ceramic slurry. A method is known in which a ceramic porous body is manufactured by removing excess sludge after adhering to a synthetic resin foam, and then drying and firing. Such a ceramic porous body,
Since it has a three-dimensional network skeleton structure, it is widely used as a molten metal filter material, a breathable heat insulating material, a grease filter for the kitchen, a catalyst carrier, etc. It is required that the ventilation and liquid passage resistance (pressure loss) be small, in other words, that there be little clogging.
【０００３】通気、通液抵抗が大きいと、例えば、溶融
金属ろ過においてはろ過時間が長くなり、生産性がおち
ると共に、場合によってはろ過途中で溶融金属の温度が
下がり、金属が凝固してしまうという不都合がある。ま
た、触媒担体においては、ジーゼルエンジンパーティキ
ュレイト捕集浄化用担体として用いられる場合、目づま
りが多く、空孔部が少ないと、発生した煤で少ない空孔
部がすぐ埋まり、エンジンに過大な負担がかかり、燃費
を悪化させたり、エンジン寿命を短くしてしまうという
問題がある。If the resistance to aeration and passage is large, for example, in the molten metal filtration, the filtration time will be long, the productivity will decline, and in some cases, the temperature of the molten metal will drop during the filtration and the metal will solidify. There is an inconvenience. In addition, when used as a diesel engine particulate collection and purification carrier in a catalyst carrier, if there are many clogging and there are few holes, the generated soot will immediately fill the less holes, and the engine will be overloaded. Therefore, there are problems that fuel consumption is deteriorated and engine life is shortened.
【０００４】この場合、セラミック多孔体の通気、通液
抵抗を少なくするためには上述したセラミック多孔体製
造時における合成樹脂発泡体に付着した余剰泥漿の除去
が重要であると考えられている。In this case, it is considered important to remove surplus sludge adhering to the synthetic resin foam during the production of the ceramic porous body in order to reduce the ventilation and liquid passage resistance of the ceramic porous body.
【０００５】従来、余剰泥漿の除去手段としては、ロー
ルを用いて合成樹脂発泡体を絞液する方法（特開昭５１
−１４２１６２号公報）、遠心分離による方法（特開昭
５９−３０５９号公報）、遠心分離とエアーブローを組
み合わせる方法（特開昭５７−１７９０６３号公報）な
どが提案されている。Conventionally, as a means for removing surplus sludge, a method of squeezing a synthetic resin foam by using a roll (Japanese Patent Laid-Open No. 51-51945)
No. 142162), a method by centrifugation (Japanese Patent Laid-Open No. 59-3059), a method of combining centrifugal separation and air blow (Japanese Patent Laid-Open No. 57-179063), and the like are proposed.
【０００６】しかし、ロールを用いて絞液する方法によ
れば、得られた製品はロール面の接触表面に均一な目づ
まりが発生すると共に、合成樹脂発泡体内部にも圧縮方
向に沿って壁状の目づまりが発生してしまうという問題
がある。とりわけセル数（直線上２５ｍｍ当りに並ぶ気
泡の数を平均的に表したもの）が１５個以上になると目
づまり度合いが著しく、そのため通気、通液抵抗も非常
に大きくなってしまうという問題があった。However, according to the method of squeezing liquid using a roll, the obtained product has uniform clogging on the contact surface of the roll surface, and a wall-like shape is formed inside the synthetic resin foam along the compression direction. There is a problem that the clogging of occurs. In particular, when the number of cells (which is the average number of bubbles lined up on a straight line of 25 mm) is 15 or more, the degree of clogging is remarkable, and therefore, there is a problem that ventilation and liquid passage resistance also become very large. It was
【０００７】これらの目づまりを防止するためには、ロ
ール間隙を狭め、圧縮率を増大することが有効である
が、絞った後の泥漿の戻りなどにより、三次元網状構造
の合成樹脂発泡体の骨格表面上に泥漿の突起などが形成
したり、あるいは網目間に薄い泥漿の膜を形成したりす
るため、なお目づまりをなくす点で十分でない。また、
ロール間隙を狭めることは泥漿除去量が多くなり、その
結果合成樹脂発泡体に付着しているセラミック泥漿量が
少なくなり、得られるセラミック多孔体のかさ比重が小
さくなって、圧力損失は低いものの焼成後の強度は小さ
く、実用に耐えられないものになってしまうという問題
もあった。特に、あまりロール間隙を狭くすると、ロー
ルにより余剰泥漿を除去した後の泥漿の付着状況が、合
成樹脂発泡体の骨格表面に均一に付着しておらず、一部
付着していない部分があったり、その断面も合成樹脂発
泡体の断面（一般に三角形状）と相似形になり、断面が
丸形状に比べて骨格強度が弱く、このため、焼成後稜線
クラックや骨格欠落などの原因となっていた。In order to prevent such clogging, it is effective to narrow the roll gap and increase the compressibility, but due to the return of the sludge after squeezing, the synthetic resin foam having a three-dimensional network structure Since protrusions of sludge are formed on the skeleton surface or a thin sludge film is formed between the meshes, it is not sufficient to eliminate clogging. Also,
Narrowing the roll gap increases the amount of sludge removed, and as a result, the amount of ceramic sludge adhered to the synthetic resin foam decreases, and the bulk specific gravity of the resulting ceramic porous body decreases, resulting in low pressure loss but firing. There was also a problem that the strength afterwards was too small to be practically used. In particular, if the roll gap is too narrow, the adhesion state of the sludge after removing the excess sludge by the roll is not evenly adhered to the skeleton surface of the synthetic resin foam, and some parts may not be adhered. , Its cross section is also similar to the cross section of synthetic resin foam (generally triangular), and the skeleton strength is weaker than that of the round cross section, which causes ridge line cracks and skeleton loss after firing. .
【０００８】また、遠心分離を用いる方法は、ロール圧
縮方法に比べ、表面目づまり、内部目づまりは減少し、
セラミック骨格は円筒形で断面も丸くなり、泥漿除去と
して理想的であるが、その反面、遠心分離方法はロール
圧縮方法に比べて泥漿除去量が多いので、含浸−遠心分
離−乾燥の操作を数回、一般的には４〜５回繰り返さな
ければならず、生産性が悪く、コストが高くなるという
問題があった。この場合、このような繰り返し工程を減
らすため、泥漿中のセラミック粉体濃度を高くし、高濃
度の泥漿で一回当りの泥漿付着量を増大させることも試
みられているが、高濃度の泥漿であるため、合成樹脂の
網目にセラミック泥漿の膜が形成されてしまい、圧力損
失の低いセラミック多孔体を得ることは困難であった。Further, the method using centrifugal separation reduces surface clogging and internal clogging as compared with the roll compression method,
The ceramic skeleton has a cylindrical shape and a round cross section, which makes it ideal for removing sludge, but on the other hand, the centrifugal separation method has a larger amount of sludge removal than the roll compression method, so several operations of impregnation-centrifugation-drying are required. Times, generally 4 to 5 times, which results in poor productivity and high cost. In this case, in order to reduce such repeated steps, it has been attempted to increase the concentration of the ceramic powder in the sludge and increase the amount of the sludge adhered per one time with the high concentration of the sludge. Therefore, a film of ceramic sludge is formed in the mesh of the synthetic resin, and it is difficult to obtain a ceramic porous body with low pressure loss.
【０００９】更に、遠心分離とエアーブローを組み合わ
せた方法は、上述した含浸−遠心分離−乾燥の繰り返し
工程数は基本的に変わらず、生産性を改善できるもので
はなく、特に本発明者の検討によると、遠心分離にエア
ーブローを組み合わせると、得られるセラミック多孔体
の骨格は細く、十分な強度が得られず、骨格欠落がしば
しば生じるものであった。Further, in the method of combining centrifugation and air blowing, the number of repeating steps of impregnation-centrifugation-drying described above is basically the same and the productivity cannot be improved. According to the above, when air blow is combined with centrifugation, the skeleton of the ceramic porous body obtained is thin, sufficient strength cannot be obtained, and skeleton loss often occurs.
【００１０】本発明は、上記事情に鑑みなされたもの
で、目づまりが少なく、通気、通液抵抗が小さい上、強
度の高いセラミック多孔体を生産性良く製造することが
できるセラミック多孔体の製造方法を提供することを目
的とする。The present invention has been made in view of the above circumstances, and is a method for producing a ceramic porous body which has a low clogging, a small resistance to ventilation and liquid passage, and a highly productive ceramic porous body with high productivity. The purpose is to provide.
【００１１】[0011]
【課題を解決するための手段及び作用】本発明者は、上
記目的を達成するため鋭意検討を重ねた結果、余剰泥漿
の除去方法として、ロールなどによる絞液方法と遠心分
離方法を組み合わせることが有効であることを知見し
た。Means and Actions for Solving the Problems As a result of intensive studies to achieve the above object, the present inventor has found that as a method for removing excess sludge, a squeezing method using a roll or the like and a centrifugal separation method can be combined. It was found to be effective.
【００１２】即ち、内部連通空間を有する三次元網状骨
格構造の合成樹脂発泡体をセラミック泥漿に浸漬し、合
成樹脂発泡体にセラミック泥漿を付着させた後、余剰泥
漿を除去する際、まずロールなどにより合成樹脂発泡体
を絞液した後、遠心分離を行なうこと、この場合特に好
ましくは上記セラミック泥漿よりも低粘度の第２のセラ
ミック泥漿を用いて絞液した合成樹脂発泡体に再度セラ
ミック泥漿を付着した後に遠心分離を行なうことが有効
であり、これによってロール等を用いた絞液方法で生じ
た合成樹脂発泡体の表面及び内部の膜状目づまり部分を
簡単に除去することができ、従来の余剰泥漿除去方とし
て絞液方法を採用した場合に得られるセラミック多孔体
の圧力損失が大きいという問題点を改善することができ
ると共に、このように絞液した後、遠心分離を行なう場
合は、絞液方法で生じた合成樹脂発泡体の余剰泥漿によ
る目づまりを除去するだけで足り、合成樹脂発泡体の格
子表面に対するセラミック泥漿の付着量を十分なものに
保持できるので、得られるセラミック多孔体の強度も高
く、セラミック泥漿への合成樹脂発泡体の浸漬回数が１
回、場合によっては２回で済むことを知見したものであ
る。特に、上述したように、絞液後、再度セラミック泥
漿を付着させ、これを遠心分離して余剰泥漿を除去する
こと、しかもこの場合再度のセラミック泥漿の付着に最
初のセラミック泥漿より低粘度のものを使用することに
より、ロール等による絞液方法を採用した場合における
合成樹脂発泡体へのセラミック泥漿の不均一付着が確実
に解消され、得られるセラミック多孔体の骨格が円筒状
で断面が円形に近くなり、通気、通液抵抗が小さくなる
ことを見い出したものである。従って、絞液法と遠心分
離法とを上記のように組み合わせることにより、従来の
遠心分離法のように４〜５回のセラミック泥漿浸漬工程
が必要であるという作業の繁雑さがなく、生産性よく低
コストで目づまりの可及的に減少した低圧力損失を有す
るセラミック多孔体を製造することができ、この場合、
絞液条件、遠心分離条件を適宜制御することにより、セ
ラミック多孔体の、かさ比重や圧力損失を容易にコント
ロールすることができ、用途に見合った製品を得ること
ができることを見い出し、本発明をなすに至ったもので
ある。That is, a synthetic resin foam having a three-dimensional net-like skeleton structure having an internal communication space is dipped in the ceramic sludge to adhere the ceramic sludge to the synthetic resin foam, and then the surplus sludge is removed when removing the excess sludge. After squeezing the synthetic resin foam by means of centrifuging, it is particularly preferable in this case to again squeeze the synthetic resin foam on the synthetic resin foam squeezed using the second ceramic sludge having a viscosity lower than that of the above ceramic sludge. It is effective to centrifuge after adhering, which makes it possible to easily remove the film-like clogging portion on the surface and inside of the synthetic resin foam generated by the squeezing method using a roll or the like. It is possible to solve the problem that the pressure loss of the porous ceramic body obtained when the squeezing method is adopted as the method for removing the excess sludge is large. When centrifuging after squeezing the liquid, it is sufficient to remove the clogging of the synthetic resin foam caused by the squeezing method due to excess sludge, and the amount of ceramic sludge adhered to the lattice surface of the synthetic resin foam is sufficient. The strength of the resulting ceramic porous body is high, and the number of times the synthetic resin foam is immersed in the ceramic slurry is 1
It was found that the number of times, or in some cases, twice was sufficient. In particular, as described above, after squeezing the liquid, the ceramic sludge is adhered again, and the excess sludge is removed by centrifuging it, and in this case, the ceramic sludge with a lower viscosity than the first ceramic sludge is adhered again. By using, the uneven adhesion of the ceramic sludge to the synthetic resin foam when the squeezing method using a roll etc. is reliably eliminated, and the skeleton of the resulting ceramic porous body has a cylindrical shape and a circular cross section. It has been found that the air flow and the liquid flow resistance become close to each other. Therefore, by combining the squeezing method and the centrifugal separation method as described above, it is possible to eliminate the complexity of the work of requiring 4 to 5 times of the ceramic sludge immersing step as in the conventional centrifugal separation method, and to improve the productivity. It is possible to produce a ceramic porous body that has a low pressure loss that is as low as possible and reduces clogging at low cost.
By appropriately controlling the squeezing conditions and the centrifugation conditions, it has been found that the bulk specific gravity and pressure loss of the ceramic porous body can be easily controlled, and a product suitable for the application can be obtained, and the present invention is made. It came to.
【００１３】従って、本発明は、内部連通空間を有する
三次元網状骨格構造の合成樹脂発泡体をセラミック泥漿
に浸漬して合成樹脂発泡体にセラミック泥漿を付着させ
た後、余剰泥漿を除去し、次いで乾燥、焼成して三次元
網状骨格構造のセラミック多孔体を製造する方法におい
て、余剰泥漿を除去する方法として、セラミック泥漿が
付着した合成樹脂発泡体を圧縮して余剰泥漿を絞り出
し、これを好ましくは乾燥し、再度セラミック泥漿に浸
漬してセラミック泥漿を付着させた後、遠心分離により
余剰泥漿を除去するようにしたことを特徴とするセラミ
ック多孔体の製造方法を提供する。Therefore, according to the present invention, a synthetic resin foam having a three-dimensional net-like skeleton structure having an internal communication space is immersed in a ceramic slurry to adhere the ceramic slurry to the synthetic resin foam, and then the excess slurry is removed. Then, in a method for producing a ceramic porous body having a three-dimensional network structure by drying and firing, as a method for removing excess sludge, the synthetic resin foam adhered with the ceramic sludge is compressed to squeeze out excess sludge, which is preferably used. The present invention provides a method for producing a ceramic porous body, which comprises drying, immersing in ceramic sludge again to adhere the ceramic sludge, and then removing excess slurry by centrifugation.
【００１４】以下、本発明について更に詳しく説明する
と、本発明のセラミック多孔体の製造に用いる合成樹脂
発泡体としては、内部連通空間を有する三次元網状骨格
構造を有すればいずれのものでも良く、例えば軟質ポリ
ウレタンフォーム、特にセル膜のない軟質ポリウレタン
フォームが好適に使用することができる。なお、セル数
としては特に制限されないが、本発明においては従来法
によれば目づまりが生じ易かった１３〜３０の範囲のも
のを有効に使用することができ、本発明によればかかる
セル数の大きいもの（網目の径の小さいもの）を用いて
も目づまりの小さいセラミック多孔体を得ることができ
る。The present invention will be described in more detail below. The synthetic resin foam used for producing the ceramic porous body of the present invention may be any one as long as it has a three-dimensional network skeleton structure having an internal communication space, For example, a flexible polyurethane foam, especially a flexible polyurethane foam having no cell membrane can be preferably used. The number of cells is not particularly limited, but in the present invention, those in the range of 13 to 30 in which clogging is likely to occur according to the conventional method can be effectively used, and according to the present invention, Even if a large one (having a small mesh diameter) is used, a ceramic porous body with little clogging can be obtained.
【００１５】次に、本発明で用いるセラミック泥漿は、
セラミック粉末を水に懸濁した液であり、通常のセラミ
ック多孔体製造に使用されているものを用いることがで
きる。泥漿特性としては、弱いチクソトロピックを示す
ものが良い。例えばセラミック粉末としては、一次粒子
から構成されているものが良く、この場合酸化物、非酸
化物の種類は問わない。二次粒子の場合は、泥漿作成時
に沈降が著しいため、チクソトロピック性を示さないと
共に、泥漿除去の際、合成樹脂発泡体の骨格に泥漿が均
一に付着しない場合が生じる。好適に使用される酸化物
セラミックとしては、例えばアルミナ、コーディライ
ト、ムライト、ジルコニアなどが挙げられ、非酸化物セ
ラミックとしては、例えば炭化ケイ素、窒化ケイ素など
が挙げられる。Next, the ceramic slurry used in the present invention is
It is a liquid obtained by suspending ceramic powder in water, and may be a liquid that is used in ordinary production of a ceramic porous body. As the sludge characteristics, those exhibiting a weak thixotropic property are preferable. For example, the ceramic powder is preferably composed of primary particles, and in this case, the type of oxide or non-oxide does not matter. In the case of secondary particles, since the sedimentation is remarkable during the preparation of the sludge, it does not exhibit thixotropic properties, and when the sludge is removed, the sludge may not evenly adhere to the skeleton of the synthetic resin foam. Suitable oxide ceramics include, for example, alumina, cordierite, mullite, zirconia, and the like, and non-oxide ceramics include, for example, silicon carbide and silicon nitride.
【００１６】本発明で用いるセラミック泥漿には、セラ
ミック粉末のほか、必要に応じて木節粘土、カオリナイ
ト、磁器土などの粘土鉱物；ポリビニルアルコール、カ
ルボキシメチルセルロースなどの有機高分子；シリカゾ
ル、アルミナゾル、第１リン酸アルミニウムなどの無機
結合剤などを配合することができる。また、焼結を促進
するため、カルシウム、バリウム、リチウム、ボロンな
どの金属酸化物を焼結助剤として添加することができ
る。In the ceramic slurry used in the present invention, in addition to ceramic powder, clay minerals such as kibushi clay, kaolinite, and porcelain earth; organic polymers such as polyvinyl alcohol and carboxymethyl cellulose; silica sol, alumina sol, An inorganic binder such as monoaluminum phosphate can be blended. Further, in order to promote the sintering, a metal oxide such as calcium, barium, lithium or boron can be added as a sintering aid.
【００１７】また、本発明で用いるセラミック泥漿の粘
度は、２０℃で５０〜２５０ポイズ、特に１００〜２０
０ポイズの範囲とすることが作業性の点から好ましい。The viscosity of the ceramic slurry used in the present invention is 50 to 250 poise at 20 ° C., particularly 100 to 20 poise.
The range of 0 poise is preferable from the viewpoint of workability.
【００１８】本発明のセラミック多孔体の製造方法は、
このようなセラミック泥漿に合成樹脂発泡体を浸漬し、
合成樹脂発泡体にセラミック泥漿を付着させた後、余剰
泥漿を除去する際、ロール等により合成樹脂発泡体を圧
縮して余剰泥漿を絞り出す絞液工程を経た後、更に合成
樹脂発泡体を遠心分離する遠心分離工程を行なう。The method for producing a ceramic porous body of the present invention comprises:
Immerse synthetic resin foam in such ceramic slurry,
After the ceramic sludge is attached to the synthetic resin foam, when removing the excess sludge, the synthetic resin foam is compressed by rolls and the excess sludge is squeezed out, and then the synthetic resin foam is further centrifuged. The centrifugation step is performed.
【００１９】まず、合成樹脂発泡体にセラミック泥漿を
含浸により十分付着させた後、焼成後所定のかさ比重に
なるように合成樹脂発泡体を圧縮する。圧縮方法として
は、例えばロール、圧締などの方法を採用し得、ロール
を使用する時には、上記かさ比重になるようにロール間
隙を決めるが、一般的に圧縮率は１０〜５０％の範囲が
良く、またロール本数（対）は所定のかさ比重が得られ
れば１本以上何本でも良い。この場合、本発明において
は、このように絞液処理した後、再度合成樹脂発泡体を
第２のセラミック泥漿に浸漬し、セラミック泥漿を付着
させることが好ましいが、このように再度のセラミック
泥漿付着処理を行なう場合、上記絞液処理は焼成後のか
さ比重設定値の６０〜８０％になるような圧縮率で合成
樹脂発泡体を絞液することが好ましい。First, after the ceramic slurry is sufficiently adhered to the synthetic resin foam by impregnation, the synthetic resin foam is compressed after firing to have a predetermined bulk specific gravity. As a compression method, for example, a method such as roll or compression can be adopted. When a roll is used, the roll gap is determined so as to have the above-mentioned bulk specific gravity. Generally, the compression rate is in the range of 10 to 50%. The number of rolls (pair) may be one or more as long as a predetermined bulk specific gravity is obtained. In this case, in the present invention, it is preferable to immerse the synthetic resin foam in the second ceramic sludge again to adhere the ceramic sludge after the squeezing treatment as described above. When the treatment is performed, it is preferable that the squeezing treatment is performed by squeezing the synthetic resin foam at a compression rate such that the set value of the bulk specific gravity after firing is 60 to 80%.
【００２０】また、再度のセラミック泥漿付着処理を行
なう場合、その付着量は所定かさ比重の４０〜２０％と
することが好ましい。このためには、第２のセラミック
泥漿として、上記最初のセラミック泥漿付着処理で用い
たセラミック泥漿よりも低粘度化したものを用いること
が好ましい。この場合、低粘度化の程度は特に制限され
ないが、最初のセラミック泥漿を１．５〜３倍に希釈し
た程度の粘度であることが好ましい。１．５倍より希釈
率が少ないような粘度では泥漿付着が多すぎる場合が生
じ、３倍より希釈率が多いような粘度では、泥漿は均一
に希釈するが、付着量が少なく、このため骨格が丸くな
らず、しかも更に泥漿に浸漬が必要になる場合が生じ
る。ここで、第２のセラミック泥漿の泥漿成分は１回目
の浸漬に使用したものと同じであっても異なってもよい
が、最初のセラミック泥漿と第２のセラミック泥漿との
成分組成が異なる場合、最初のセラミック泥漿より得ら
れるセラミックの１０００℃の熱膨張係数Ａと第２のセ
ラミック泥漿より得られるセラミックの１０００℃の熱
膨張係数Ｂとの差（Ａ−Ｂ）×１００／Ａが±１０％以
内、より好ましくは±５％以内であることが推賞され
る。上記熱膨張係数の差が±１０％の範囲を外れた場
合、焼成中熱膨張係数の差によりクラックが発生する場
合が生じる。When the ceramic sludge adhesion treatment is carried out again, it is preferable that the adhesion amount is 40 to 20% of the predetermined bulk specific gravity. For this purpose, it is preferable to use, as the second ceramic slurry, one having a viscosity lower than that of the ceramic slurry used in the first ceramic slurry attachment process. In this case, the degree of lowering the viscosity is not particularly limited, but the viscosity is preferably such that the initial ceramic slurry is diluted 1.5 to 3 times. If the viscosity is such that the dilution ratio is less than 1.5 times, too much sludge adhesion may occur, and if the viscosity is more than 3 times higher, the sludge will be diluted uniformly, but the adhesion amount will be small, and therefore the skeleton It may not be round and may require further immersion in slurry. Here, the sludge component of the second ceramic slurry may be the same as or different from that used in the first dipping, but when the component composition of the first ceramic slurry and the second ceramic slurry are different, The difference (A−B) × 100 / A between the thermal expansion coefficient A of 1000 ° C. of the ceramic obtained from the first ceramic slurry and the thermal expansion coefficient B of 1000 ° C. of the ceramic obtained from the second ceramic slurry is ± 10%. It is recommended that it is within, more preferably within ± 5%. When the difference in the coefficient of thermal expansion is out of the range of ± 10%, cracks may occur due to the difference in the coefficient of thermal expansion during firing.
【００２１】このように絞液工程と遠心分離工程とでセ
ラミック泥漿成分を相違させることにより、種々の特性
のセラミック多孔体を得ることができる。例えば、絞液
工程では炭化ケイ素系泥漿を用い、遠心分離工程ではム
ライト系の泥漿を用い、炭化ケイ素系セラミックからな
る骨格をムライト系セラミックで被覆することにより、
高温使用下における熱衝撃性を維持しつつ炭化ケイ素の
耐酸化性能を向上させることができる。By thus differentiating the components of the ceramic sludge in the squeezing process and the centrifugal separation process, it is possible to obtain a ceramic porous body having various characteristics. For example, by using silicon carbide-based sludge in the squeezing step and using mullite-based sludge in the centrifugation step, by coating the skeleton made of silicon carbide-based ceramic with mullite-based ceramic,
It is possible to improve the oxidation resistance performance of silicon carbide while maintaining the thermal shock resistance under high temperature use.
【００２２】なお、勿論最初のセラミック泥漿と第２の
セラミック泥漿との成分組成を同じにすることもできる
が、この場合第２のセラミック泥漿は、最初のセラミッ
ク泥漿を上述した希釈率で希釈することにより調製する
ことができる。Of course, the first ceramic slurry and the second ceramic slurry may have the same composition, but in this case, the second ceramic slurry dilutes the first ceramic slurry at the above-mentioned dilution ratio. It can be prepared by
【００２３】遠心分離は、遠心分離機内のサンプル受け
皿に合成樹脂発泡体をセットし、１０〜２０Ｇ、特に１
３〜１７Ｇの遠心力を５〜１５秒、特に７〜１０秒加え
ることにより行なうことが好ましい。１０Ｇより遠心力
が低かったり、５秒より遠心力を加える時間が少ないと
泥漿除去の効果が生じない場合があり、一方、２０Ｇよ
り高くしたり、１５秒より遠心力を加える時間が長いと
合成樹脂発泡体がつぶれ、かえって目づまりが発生する
場合が生じる。なお、遠心分離機内にセットする場合、
合成樹脂発泡体のセル長径方向（発泡方向）を回転中心
方向に合わせることが好ましい。For centrifugation, synthetic resin foam is set in a sample pan in the centrifuge, and 10 to 20 G, especially 1
It is preferable to apply a centrifugal force of 3 to 17 G for 5 to 15 seconds, particularly 7 to 10 seconds. If the centrifugal force is lower than 10G or if the centrifugal force is applied for less than 5 seconds, the sludge removal effect may not be produced. On the other hand, if the centrifugal force is higher than 20G or the centrifugal force is applied for longer than 15 seconds, it will be combined. The resin foam may be crushed to cause clogging. When setting in a centrifuge,
It is preferable that the cell major axis direction (foaming direction) of the synthetic resin foam is aligned with the rotation center direction.
【００２４】また、上述した絞液工程と遠心分離工程に
加えて、絞液を終了した後、あるいは遠心分離が終了し
た後、セラミック泥漿が付着した合成樹脂発泡体に更に
圧縮空気を吹きつけ、骨格間に膜状に付着した泥漿を吹
き飛ばすことも効果的である。In addition to the above-mentioned squeezing step and centrifuging step, after the squeezing solution is finished or after the centrifugal separation is finished, compressed air is further blown to the synthetic resin foam adhered with the ceramic sludge, It is also effective to blow off the mud adhered in a film form between the skeletons.
【００２５】以上のような遠心分離工程が終了した後、
セラミック泥漿が付着した合成樹脂発泡体を、通常の方
法と同様に４０〜８０℃で水分が除去するまで乾燥し、
次いで１２００〜１５００℃で焼成することにより三次
元網状構造のセラミック多孔体を得ることができる。After the centrifugation step as described above is completed,
The synthetic resin foam to which the ceramic sludge has adhered is dried at 40 to 80 ° C. in the same manner as a usual method until water is removed,
Then, by firing at 1200 to 1500 ° C., a ceramic porous body having a three-dimensional network structure can be obtained.
【００２６】なお、付着したセラミック泥漿を乾燥した
後の焼成前、又は焼成後に釉薬をスプレー等の方法によ
り吹きつけて付着させることにより、セラミック多孔体
の骨格を補強することができる。The skeleton of the ceramic porous body can be reinforced by spraying a glaze by a method such as spraying after the adhered ceramic slurry is dried and before firing or after firing.
【００２７】このようにして得られたセラミック多孔体
は、合成樹脂発泡体が消失した三次元網状骨格構造を有
し、網目を構成している骨格形状が円筒型で、断面が丸
みを帯び、高強度で目づまりのない低圧力損失のもので
ある。The ceramic porous body thus obtained has a three-dimensional net-like skeleton structure in which the synthetic resin foam disappears, the skeleton forming the mesh is cylindrical, and the cross section is rounded. It has high strength and low pressure loss without clogging.
【００２８】[0028]
【実施例】以下、実施例と比較例を示し、本発明を具体
的に示すが、本発明は下記の実施例に制限されるもので
はない。なお、以下の例において部はいずれも重量部で
ある。EXAMPLES Hereinafter, the present invention will be specifically shown by showing Examples and Comparative Examples, but the present invention is not limited to the following Examples. In the following examples, all parts are parts by weight.
【００２９】［実施例１］コージライト５０部、アルミ
ナ４０部、カルシア５部、カオリナイト５部に水２０部
を加え、更に解膠剤としてケブラテオ０．１部、バイン
ダーとしてポリビニルアルコール３部を加え、セラミッ
ク泥漿を作成した。粘度は１３０ポイズであった。Example 1 50 parts of cordierite, 40 parts of alumina, 5 parts of calcia, 5 parts of kaolinite, 20 parts of water were added, and 0.1 part of quebrateo was used as a peptizer and 3 parts of polyvinyl alcohol was used as a binder. In addition, a ceramic slurry was created. The viscosity was 130 poise.
【００３０】この泥漿に、直線上２５ｍｍ当りに並ぶ気
泡の数が１３個で長さ２５０×幅１２０×厚さ２５ｍｍ
のセル膜のない三次元網状骨格構造を有する合成樹脂発
泡体を浸漬した後、間隙１２ｍｍの一対のロールに通し
て余剰泥漿を除去し、その後、６０℃で６時間乾燥し
た。乾燥後の重量は１８５ｇであった。In this sludge, the number of bubbles arranged in a line on a straight line of 25 mm is 13 and the length is 250 × width 120 × thickness 25 mm.
The synthetic resin foam having a three-dimensional network skeleton structure without a cell membrane was dipped, passed through a pair of rolls with a gap of 12 mm to remove excess sludge, and then dried at 60 ° C. for 6 hours. The weight after drying was 185 g.
【００３１】次いで、上記セラミック泥漿を水で２倍に
希釈して粘度を５ポイズに調整した泥漿に上記乾燥した
合成樹脂発泡体を発泡体中の気泡が抜けるように徐々に
浸漬した。浸漬後、セラミック泥漿から引き上げ、遠心
分離機にセットし、１５Ｇ、１０秒間遠心力を加えて余
剰泥漿を除去した。その後、６０℃で６時間乾燥した。
乾燥後の重量は３０７ｇであった。次いで１３５０℃で
焼成した。得られたセラミック多孔体は２７３ｇで、大
きさは長さ２４３×幅１１６×厚さ２４ｍｍであった。Next, the dried synthetic resin foam was gradually dipped in a slurry whose viscosity was adjusted to 5 poise by diluting the ceramic slurry with water twice, so that bubbles in the foam could escape. After the immersion, the ceramic slurry was pulled up, set in a centrifuge, and subjected to centrifugal force of 15 G for 10 seconds to remove excess slurry. Then, it dried at 60 degreeC for 6 hours.
The weight after drying was 307 g. Then, it was fired at 1350 ° C. The obtained ceramic porous body was 273 g and had a size of length 243 × width 116 × thickness 24 mm.
【００３２】得られたセラミック多孔体について、かさ
比重を測定すると共に、５０×５０×２５ｍｍに切り出
し、管径４０ｍｍ，風速１０ｍ／ｓで圧力損失を測定
し、また、長さ１５０×幅３５×厚さ２４ｍｍに切り出
し、スパン１２０ｍｍ，クロスヘッドスピード１０ｍｍ
／ｍｉｎで曲げ強度を測定し、更に目視により骨格形状
を観察した。結果を表１に併記する。The bulk density of the obtained ceramic porous body was measured, cut into 50 × 50 × 25 mm, the pressure loss was measured at a pipe diameter of 40 mm and a wind speed of 10 m / s, and the length was 150 × width 35 ×. Cut to a thickness of 24 mm, span 120 mm, crosshead speed 10 mm
The bending strength was measured at / min, and the skeleton shape was visually observed. The results are also shown in Table 1.
【００３３】［実施例２］実施例１と同様にセラミック
泥漿を作成し、この泥漿に同様の合成樹脂発泡体を浸漬
した。Example 2 A ceramic slurry was prepared in the same manner as in Example 1, and the same synthetic resin foam was immersed in this slurry.
【００３４】次いで、泥漿が付着した合成樹脂発泡体を
間隙１４ｍｍの一対のロールに通して余剰泥漿を除去し
た後、６０℃で６時間乾燥した。乾燥後の重量は２２５
ｇであった。Next, the synthetic resin foam to which the sludge adhered was passed through a pair of rolls having a gap of 14 mm to remove excess sludge, and then dried at 60 ° C. for 6 hours. Weight after drying is 225
It was g.
【００３５】次に、上記セラミック泥漿を水で２．５倍
に希釈し、粘度を１ポイズに調整した泥漿に上記乾燥し
た合成樹脂発泡体を浸漬し、遠心分離機で実施例１と同
様に余剰泥漿を除去した後、同様に乾燥した。乾燥後の
重量は３００ｇであった。その後１３５０℃で実施例１
と同様に焼成して長さ２４３×幅１１６×厚さ２４ｍｍ
の２７０ｇのセラミック多孔体を得た。Next, the ceramic slurry was diluted 2.5 times with water, the dried synthetic resin foam was immersed in the slurry having a viscosity adjusted to 1 poise, and a centrifugal separator was used to carry out the same procedure as in Example 1. After removing excess sludge, it was similarly dried. The weight after drying was 300 g. Then at 1350 ° C. Example 1
Fired in the same way as length 243 x width 116 x thickness 24 mm
270 g of a ceramic porous body was obtained.
【００３６】得られたセラミック多孔体について実施例
１と同様に試験を行った。結果を表１に併記する。The same tests as in Example 1 were conducted on the obtained ceramic porous body. The results are also shown in Table 1.
【００３７】［比較例１］水の配合量を２８部とした以
外は実施例１と同様にセラミック泥漿を作成した。この
泥漿の粘度は５ポイズであった。[Comparative Example 1] A ceramic slurry was prepared in the same manner as in Example 1 except that the amount of water was 28 parts. The viscosity of this slurry was 5 poise.
【００３８】この泥漿に実施例１と同様の合成樹脂発泡
体を浸漬し、次いで泥漿が付着した合成樹脂発泡体を遠
心分離機にセットし、遠心力１５Ｇ、５秒間の条件で余
剰泥漿を除去した後、乾燥した。これらの浸漬−遠心分
離−乾燥の操作を更に３回繰り返した。なお、最後の１
回は、上記泥漿に水を加えて粘度を１ポイズに調整して
浸漬した。A synthetic resin foam similar to that used in Example 1 was dipped in the slurry, and the synthetic resin foam having the slurry adhered thereto was set in a centrifuge to remove excess slurry under the conditions of a centrifugal force of 15 G and 5 seconds. And then dried. These dipping-centrifuging-drying operations were repeated three more times. The last one
For the rotation, water was added to the above slurry to adjust the viscosity to 1 poise and it was immersed.
【００３９】次いで、１３５０℃で焼成し、長さ２４４
×幅１１７×厚さ２４ｍｍの２６５ｇのセラミック多孔
体を得た。得られたセラミック多孔体について実施例１
と同様に試験を行った。結果を表１に併記する。Then, it is fired at 1350 ° C. to have a length of 244.
265 g of a ceramic porous body having a width of 117 and a thickness of 24 mm was obtained. Example 1 of the obtained ceramic porous body
The test was conducted in the same manner as. The results are also shown in Table 1.
【００４０】［比較例２］水の配合量を１８部とした以
外は実施例１と同様にセラミック泥漿を調整した。この
セラミック泥漿の粘度は１６０ポイズであった。[Comparative Example 2] A ceramic slurry was prepared in the same manner as in Example 1 except that the amount of water was 18 parts. The viscosity of this ceramic slurry was 160 poise.
【００４１】この泥漿に実施例１と同様の合成樹脂発泡
体を浸漬し、泥漿が付着した合成樹脂発泡体をロール間
隙１４ｍｍの一対のロールに通し、余剰泥漿を除去し
た。A synthetic resin foam similar to that used in Example 1 was immersed in the slurry, and the synthetic resin foam having the slurry adhered thereto was passed through a pair of rolls having a roll gap of 14 mm to remove excess slurry.
【００４２】次いで乾燥した後、１３５０℃で焼成して
長さ２４５×幅１１５×厚さ２４ｍｍの２７０ｇのセラ
ミック多孔体を得た。得られたセラミック多孔体につい
て実施例１と同様に試験を行った。結果を表１に併記す
る。Next, after drying, it was fired at 1350 ° C. to obtain 270 g of a ceramic porous body having a length of 245 × a width of 115 × a thickness of 24 mm. The obtained porous ceramic body was tested in the same manner as in Example 1. The results are also shown in Table 1.
【００４３】[0043]
【表１】 [Table 1]
【００４４】表１の結果より、本発明方法によって得ら
れたセラミック多孔体は、遠心分離によって得られたも
の（比較例１）、ロール圧縮によって得られたもの（比
較例２）に比べ、圧力損失が低く、かつ曲げ強度が大き
いことが認められる。From the results shown in Table 1, the ceramic porous body obtained by the method of the present invention has a higher pressure than those obtained by centrifugation (Comparative Example 1) and roll compression (Comparative Example 2). It is recognized that the loss is low and the bending strength is high.
【００４５】［実施例３］炭化ケイ素９０部、カオリナ
イト１０部に水２５部を加え、更に解膠剤としてゲブラ
チオ０．１部、バインダーとしてポリビニルアルコール
３部を加え、粘度１５０ポイズのセラミック泥漿を作成
した。この泥漿に直線上２５ｍｍ当たりに並ぶ気泡の数
が９個で、長さ２５０×幅１２０×厚さ２５ｍｍのセル
膜のない三次元網状骨格構造を有する合成樹脂発泡体を
浸漬した後、間隙１２ｍｍの一対のロールに通して余剰
泥漿を除去し、その後６０℃で６時間乾燥した。乾燥後
の重量は１９０ｇであった。なお、このセラミック泥漿
を焼成することによって得られるセラミックの熱膨張係
数は４．９×１０-6（１０００℃）であった。Example 3 90 parts of silicon carbide, 10 parts of kaolinite, 25 parts of water, 0.1 part of gebrathio as a deflocculant, and 3 parts of polyvinyl alcohol as a binder were added, and a ceramic slurry having a viscosity of 150 poise was added. It was created. After dipping a synthetic resin foam having a cell membrane-less three-dimensional reticulated skeleton structure having a length of 250 mm, a width of 120 mm, and a thickness of 25 mm, in which 9 cells are arranged in a line on a straight line per 25 mm, a gap is 12 mm. Excess sludge was removed by passing through a pair of rolls, and then dried at 60 ° C. for 6 hours. The weight after drying was 190 g. The coefficient of thermal expansion of the ceramic obtained by firing this ceramic slurry was 4.9 × 10 −6 (1000 ° C.).
【００４６】次いで、ムライト９０部、カオリナイト１
０部に水３５部を加え、更に解膠剤としてゲブラチオ
０．１部、バインダーとしてポリビニルアルコール３部
を加え、粘度８ポイズのセラミック泥漿を作成した。な
お、このセラミック泥漿を焼成することによって得られ
るセラミックの熱膨張係数は５．２×１０-6（１０００
℃）である。Next, 90 parts of mullite and 1 of kaolinite
35 parts of water was added to 0 part, 0.1 part of gebrathio as a deflocculant and 3 parts of polyvinyl alcohol as a binder were added to prepare a ceramic slurry having a viscosity of 8 poises. The coefficient of thermal expansion of the ceramic obtained by firing this ceramic slurry is 5.2 × 10 −6 (1000
℃).
【００４７】この低粘度セラミック泥漿に上記乾燥した
合成樹脂発泡体を発泡体中の気泡が抜けるように徐々に
浸漬した。浸漬後、セラミック泥漿から引き上げ、遠心
分離機にセットし、実施例１と同条件で余剰泥漿を除去
した。その後、６０℃で６時間乾燥した。乾燥後の重量
は３１５ｇであった。The dried synthetic resin foam was gradually immersed in this low-viscosity ceramic slurry so that the bubbles in the foam could escape. After the immersion, the ceramic slurry was pulled up, set in a centrifuge, and the excess slurry was removed under the same conditions as in Example 1. Then, it dried at 60 degreeC for 6 hours. The weight after drying was 315 g.
【００４８】これを１３５０℃で焼成した。得られたセ
ラミック多孔体は２８１ｇであり、大きさは長さ２４８
×幅１１８×厚さ２５ｍｍであった。このセラミック多
孔体の圧力損失及び曲げ強度を実施例１と同様に測定
し、更に目視により骨格形状を観察した。また、耐酸化
性を評価するため、長さ１５０×幅３５×厚さ２５ｍｍ
に切り出し、１４００℃の電気炉に１００時間放置し、
放置後の曲げ強度を測定した。結果を表２に示す。This was baked at 1350 ° C. The obtained ceramic porous body weighed 281 g and had a length of 248 g.
The width was 118 mm and the thickness was 25 mm. The pressure loss and bending strength of this ceramic porous body were measured in the same manner as in Example 1, and the skeleton shape was visually observed. Also, in order to evaluate the oxidation resistance, length 150 × width 35 × thickness 25 mm
Cut into pieces and left in an electric furnace at 1400 ° C for 100 hours,
The bending strength after standing was measured. The results are shown in Table 2.
【００４９】[0049]
【表２】 [Table 2]
【００５０】[0050]
【発明の効果】本発明のセラミック多孔体の製造方法に
よれば、通気、通液抵抗が低く、強度も十分なセラミッ
ク多孔体を生産性良く製造することができる。According to the method for producing a ceramic porous body of the present invention, it is possible to produce a ceramic porous body having low ventilation and liquid passage resistance and sufficient strength with high productivity.
Claims (6)
造の合成樹脂発泡体をセラミック泥漿に浸漬して合成樹
脂発泡体にセラミック泥漿を付着させた後、余剰泥漿を
除去し、次いで乾燥、焼成して三次元網状骨格構造のセ
ラミック多孔体を製造する方法において、余剰泥漿を除
去する方法として、セラミック泥漿が付着した合成樹脂
発泡体を圧縮して余剰泥漿を絞り出した後、遠心分離に
より余剰泥漿を除去するようにしたことを特徴とするセ
ラミック多孔体の製造方法。1. A synthetic resin foam having a three-dimensional reticulated skeleton structure having an internal communication space is immersed in a ceramic slurry to adhere the ceramic slurry to the synthetic resin foam, and then excess slurry is removed, followed by drying and firing. In the method for producing a ceramic porous body having a three-dimensional reticulated skeleton structure, as a method for removing excess slurry, the synthetic resin foam adhered with the ceramic slurry is compressed to squeeze out the excess slurry, and then the excess slurry is centrifuged. A method for producing a ceramic porous body, comprising:
を除去する方法として、セラミック泥漿が付着した合成
樹脂発泡体を圧縮して余剰泥漿を絞り出した後、乾燥
し、再度第２のセラミック泥漿に浸漬してセラミック泥
漿を付着させ、次いで遠心分離により余剰泥漿を除去す
るようにしたことを特徴とするセラミック多孔体の製造
方法。2. The method according to claim 1, wherein the excess sludge is removed by compressing the synthetic resin foam adhered with the ceramic sludge to squeeze out the excess sludge, and then drying the second sludge. A method for producing a porous ceramic body, characterized in that the ceramic sludge is soaked in the above to adhere the ceramic sludge and then the surplus sludge is removed by centrifugation.
ック泥漿より低粘度のものである請求項２に記載の方
法。3. The method of claim 2, wherein the second ceramic slurry has a lower viscosity than the first ceramic slurry.
ミックの熱膨張係数Ａと第２のセラミック泥漿から得ら
れるセラミックの熱膨張係数Ｂとの差（Ａ−Ｂ）×１０
０／Ａが±１０％以内にある請求項２又は３に記載の方
法。4. The difference (A−B) × 10 between the coefficient of thermal expansion A of the ceramic obtained from the first ceramic slurry and the coefficient of thermal expansion B of the ceramic obtained from the second ceramic slurry.
The method according to claim 2 or 3, wherein 0 / A is within ± 10%.
ク泥漿を水で希釈したものである請求項３又は４に記載
の方法。5. The method according to claim 3, wherein the second ceramic slurry is a dilution of the original ceramic slurry with water.
のセラミック泥漿の配合成分とが互いに異なるものであ
る請求項２乃至４のいずれか１項に記載の方法。6. The first ceramic slurry formulation and the second.
The method according to any one of claims 2 to 4, wherein the compounding components of the ceramic sludge are different from each other.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19917992A JP3287019B2 (en) | 1992-07-02 | 1992-07-02 | Method for producing porous ceramic body |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP19917992A JP3287019B2 (en) | 1992-07-02 | 1992-07-02 | Method for producing porous ceramic body |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0624859A true JPH0624859A (en) | 1994-02-01 |
| JP3287019B2 JP3287019B2 (en) | 2002-05-27 |
Family
ID=16403465
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP19917992A Expired - Fee Related JP3287019B2 (en) | 1992-07-02 | 1992-07-02 | Method for producing porous ceramic body |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3287019B2 (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1245549A2 (en) | 2001-03-28 | 2002-10-02 | Asahi Glass Company Ltd. | Process for preparing silicate porous product |
| CN113134893A (en) * | 2020-01-20 | 2021-07-20 | 西部宝德科技股份有限公司 | Preparation method of ceramic fiber filter tube for high-temperature flue gas purification |
-
1992
- 1992-07-02 JP JP19917992A patent/JP3287019B2/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1245549A2 (en) | 2001-03-28 | 2002-10-02 | Asahi Glass Company Ltd. | Process for preparing silicate porous product |
| CN113134893A (en) * | 2020-01-20 | 2021-07-20 | 西部宝德科技股份有限公司 | Preparation method of ceramic fiber filter tube for high-temperature flue gas purification |
Also Published As
| Publication number | Publication date |
|---|---|
| JP3287019B2 (en) | 2002-05-27 |
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