JP2568860B2 - Method for manufacturing porous porcelain structure - Google Patents
Method for manufacturing porous porcelain structureInfo
- Publication number
- JP2568860B2 JP2568860B2 JP62258243A JP25824387A JP2568860B2 JP 2568860 B2 JP2568860 B2 JP 2568860B2 JP 62258243 A JP62258243 A JP 62258243A JP 25824387 A JP25824387 A JP 25824387A JP 2568860 B2 JP2568860 B2 JP 2568860B2
- Authority
- JP
- Japan
- Prior art keywords
- porous porcelain
- dew point
- porcelain structure
- whiskers
- coated
- 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.)
- Expired - Fee Related
Links
Landscapes
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
Description
【発明の詳細な説明】 （産業上の利用分野） この発明は、酵素担体、フィルター、断熱材、クロマ
トグラフカラム充填材、吸音材等として使用しうる多孔
質磁器構造体の製造方法に関するものである。Description: TECHNICAL FIELD The present invention relates to a method for producing a porous porcelain structure that can be used as an enzyme carrier, a filter, a heat insulating material, a chromatographic column packing material, a sound absorbing material, and the like. is there.
（従来の技術） 従来、流体用フィルターや生化学反応酵素担体とし
て、表面にシリカ、窒化硅素、ムライト等を素材とする
３次元網目状ウィスカーを形成させた多孔質磁器が提案
されている（特開昭60−118681号、特開昭61−232279
号，特開昭61−270273号，特開昭62−217669号）。(Prior art) Conventionally, a porous porcelain having three-dimensional mesh whiskers made of silica, silicon nitride, mullite, etc. on its surface has been proposed as a filter for a fluid or a biochemical reaction enzyme carrier (particularly). JP-A-60-118681, JP-A-61-232279
No., JP-A-61-270273, JP-A-62-217669).
（発明が解決しようとする課題） しかしながら以上上記、シリカ、あるいはムライトを
素材とする３次元網目状ウィスカーは、充分な強度が得
られないという欠点があり、一方この多孔質磁器を酵素
担体として使用する場合には、酵素の固定化濃度の向
上、あるいは、酵素活性保持のために、ウィスカーの表
面に多くのシラノール基が存在していることが必要であ
るか、窒素硅素を素材とするウィスカーにおいては、更
に複雑な加工を施さない限り、その表面にシラノール基
を確保しえないという欠点があった。(Problems to be Solved by the Invention) However, the above-mentioned three-dimensional mesh whiskers made of silica or mullite have a drawback that sufficient strength cannot be obtained. On the other hand, this porous porcelain is used as an enzyme carrier. In order to improve the immobilized concentration of the enzyme or to maintain the enzyme activity, it is necessary to have many silanol groups on the surface of the whisker, or use a whisker made of silicon nitride Has a drawback that silanol groups cannot be secured on the surface thereof unless further complicated processing is performed.
この発明は、上記従来のものの欠点を改良するもので
あり、簡易な方法で、十分な強度を有し、しかも表面に
多くのシラノール基を保持しうる３次元網目状ウィスカ
ーを有する多孔質磁器を得ることができるものである。The present invention is intended to improve the above-mentioned disadvantages of the prior art, and to provide a porous porcelain having a three-dimensional mesh whisker which has sufficient strength and can hold many silanol groups on the surface by a simple method. What you can get.
（課題を解決するための手段） 表面が硅素酸化物で被覆された３次元網目状ウィスカ
ーを有する多孔質磁器構造体と製造方法であって多孔質
の磁器に硅素粉末を含浸あるいは塗布し、水蒸気露点が
−50℃以上20℃以下の水蒸気及び窒素を含む還元性ガス
雰囲気中で焼成し、更に、温度800℃乃至1400℃の大気
雰囲気中または温度1200℃乃至1600℃、露点30℃以上の
アンモニア分解ガス中で焼成することにより、表面に硅
素酸化物で被覆された３次元網目状ウィスカーを形成さ
せたものである。(Means for Solving the Problems) A porous porcelain structure having a three-dimensional network whisker whose surface is coated with silicon oxide, and a method for manufacturing the porous porcelain structure. Firing in a reducing gas atmosphere containing water vapor and nitrogen having a dew point of -50 ° C or more and 20 ° C or less, and further, in an air atmosphere at a temperature of 800 ° C to 1400 ° C or at a temperature of 1200 ° C to 1600 ° C and ammonia at a dew point of 30 ° C or more By firing in a decomposition gas, a three-dimensional network whisker whose surface is coated with silicon oxide is formed.
なお、還元性ガス雰囲気の水蒸気露点−50℃より低い
と網目構造のウィスカーが形成されなくなり、同様＋20
℃より高くてもウィスカー状のものが得られないから、
水蒸気露点の範囲は−50℃以上＋20℃以下とするもので
ある。If the water vapor dew point of the reducing gas atmosphere is lower than −50 ° C., whiskers having a network structure are not formed, and the
Even if it is higher than ℃, whisker-like thing cannot be obtained,
The range of the water vapor dew point shall be -50 ° C or higher and + 20 ° C or lower.
（作用） 上記の構成を持つので、多孔質磁器の表面を被う窒化
硅素ウィスカーが酸化され、容易に硅素酸化物の被覆を
有する３次元網目状ウィスカーが形成される。(Operation) With the above configuration, the silicon nitride whiskers covering the surface of the porous porcelain are oxidized, and three-dimensional mesh whiskers having a silicon oxide coating are easily formed.
（実施例） 更に、実施例を詳説する。硅素粉末（試薬250メッシ
ュパス）100g、第３ブチルアルコール（試薬）80mlを、
内容積500mlの容器に入れ、径10φ、純度99.9％のアル
ミナ球石300gと共に、120RPMで20時間粉砕混合し、スラ
リーとなした上、このスラリーに、気孔径25u.気孔率40
％、10φ×14φ×300l大のアルミナ多孔体を浸す。この
ようにして得られたものを、アンモニア分解ガス雰囲気
中で、水蒸気露点−１℃で、温度1330℃として１時間焼
成する。その焼成品を、更に、大気雰囲気中で温度を10
50℃あるいは1350℃として１時間焼成する。これにより
表面が第１図あるいは第２図の走査型電子顕微鏡写真が
示すような硅素酸化物で被覆された窒化硅素ウィスカー
からなる３次元網目構造を有する多孔質磁器構造体が得
られる。(Example) Furthermore, an Example is described in detail. 100 g of silicon powder (reagent 250 mesh pass) and 80 ml of tertiary butyl alcohol (reagent)
Placed in a container having an inner volume of 500 ml, pulverized and mixed with 300 g of alumina spheres having a diameter of 10φ and a purity of 99.9% at 120 RPM for 20 hours to form a slurry, and the slurry has a pore diameter of 25 u.
%, Soak a 10φ × 14φ × 300l large alumina porous body. The thus obtained product is fired in an ammonia decomposition gas atmosphere at a steam dew point of -1 ° C and a temperature of 1330 ° C for 1 hour. The fired product is further cooled to 10
Bake for 1 hour at 50 ° C or 1350 ° C. As a result, a porous porcelain structure having a three-dimensional network structure composed of silicon nitride whiskers whose surfaces are covered with silicon oxide as shown in the scanning electron micrographs of FIG. 1 or FIG. 2 is obtained.
（発明の効果） 以上の通り、この発明は構成されるので、容易に表面
に硅素酸化物で被覆された３次元網目状ウィスカーを有
する多孔質磁器構造体を得ることができ、しかも十分な
強度並びに酵素の固定化濃度の向上あるいは酵素活性保
持のために必要なウィスカー表面でのシラノール基保持
が可能となるので、この構造体は、酵素固定化担体とし
てだけでなく、ガスストーブの燃焼板、クロマトグラフ
のカラム充填材や無菌濾過膜としても応用可能となる。(Effects of the Invention) As described above, since the present invention is constituted, it is possible to easily obtain a porous porcelain structure having three-dimensional mesh whiskers coated on its surface with silicon oxide, and having sufficient strength. In addition, since it is possible to improve the concentration of immobilized enzyme or to retain silanol groups on the surface of whiskers necessary for maintaining enzyme activity, this structure is used not only as an enzyme-immobilized carrier but also as a gas stove combustion plate, It can also be applied as a column packing material for a chromatograph or a sterile filtration membrane.
第１図は最終焼成を大気雰囲気中温度1050℃として行っ
た場合の３次元網目構造すなわち粒子構造の走査型電子
顕微鏡写真であり、第２図は同じく温度1350℃とした場
合の粒子構造の電子顕微鏡写真であり、各Ａ、Ｂ、Ｃは
それぞれ倍率が500倍、2000倍、10000倍である。FIG. 1 is a scanning electron micrograph of the three-dimensional network structure, that is, the particle structure when the final baking is performed in an air atmosphere at a temperature of 1050 ° C., and FIG. 2 is an electron of the particle structure when the temperature is also 1350 ° C. It is a microscope photograph, and each of A, B, and C has a magnification of 500 times, 2000 times, and 10,000 times, respectively.
Claims (1)
状ウィスカーを有する多孔質磁器構造体の製造方法であ
って、多孔質の磁器に硅素粉末を含浸あるいは塗布し、
水蒸気露点が−50℃以上20℃以下の水蒸気及び窒素を含
む還元性ガス雰囲気中で焼成し、更に、温度800℃乃至1
400℃の大気雰囲気中または温度1200乃至1600℃、露点3
0℃以上のアンモニア分解ガス中で焼成する多孔質磁器
構造体の製造方法。1. A method for producing a porous porcelain structure having three-dimensional mesh whiskers whose surface is coated with silicon oxide, wherein the porous porcelain is impregnated or coated with silicon powder.
Sintering is performed in a reducing gas atmosphere containing steam and nitrogen having a steam dew point of −50 ° C. or more and 20 ° C. or less.
400 ℃ air atmosphere or 1200 ~ 1600 ℃, dew point 3
A method for producing a porous porcelain structure fired in an ammonia decomposition gas at 0 ° C. or higher.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62258243A JP2568860B2 (en) | 1987-10-15 | 1987-10-15 | Method for manufacturing porous porcelain structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP62258243A JP2568860B2 (en) | 1987-10-15 | 1987-10-15 | Method for manufacturing porous porcelain structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01103969A JPH01103969A (en) | 1989-04-21 |
| JP2568860B2 true JP2568860B2 (en) | 1997-01-08 |
Family
ID=17317517
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP62258243A Expired - Fee Related JP2568860B2 (en) | 1987-10-15 | 1987-10-15 | Method for manufacturing porous porcelain structure |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2568860B2 (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3769739B2 (en) * | 1994-11-17 | 2006-04-26 | 住友電気工業株式会社 | Porous ceramic film and manufacturing method thereof |
-
1987
- 1987-10-15 JP JP62258243A patent/JP2568860B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01103969A (en) | 1989-04-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |