JPS61222966A - Manufacture of silicon nitride porous body - Google Patents

Manufacture of silicon nitride porous body

Info

Publication number
JPS61222966A
JPS61222966A JP6416685A JP6416685A JPS61222966A JP S61222966 A JPS61222966 A JP S61222966A JP 6416685 A JP6416685 A JP 6416685A JP 6416685 A JP6416685 A JP 6416685A JP S61222966 A JPS61222966 A JP S61222966A
Authority
JP
Japan
Prior art keywords
silicon nitride
green
porous body
gypsum
manufacture
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
JP6416685A
Other languages
Japanese (ja)
Inventor
勝 山口
近 稲住
雅芳 近藤
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.)
Hitachi Zosen Corp
Original Assignee
Hitachi Zosen 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 Hitachi Zosen Corp filed Critical Hitachi Zosen Corp
Priority to JP6416685A priority Critical patent/JPS61222966A/en
Publication of JPS61222966A publication Critical patent/JPS61222966A/en
Pending legal-status Critical Current

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Abstract

(57)【要約】本公報は電子出願前の出願データであるた
め要約のデータは記録されません。
(57) [Summary] This bulletin contains application data before electronic filing, so abstract data is not recorded.

Description

【発明の詳細な説明】 産業上の利用分野 本発明は、たとえば俗解用るつぼ、溶解炉用レンガ、ガ
ス吹込管、パーナノズ/L/、分離膜等に利用できる窒
化けい素の多孔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 is a method for producing a porous body of silicon nitride that can be used, for example, in crucibles for general use, bricks for melting furnaces, gas blowing pipes, Parnanos/L/, separation membranes, etc. It is related to.

従来の技術 従来、窒化けい素の多孔体の製造方法として特開昭60
−33272号がある。これはけい素粉末と水を混練し
た水性−懸濁液(略称A液)と発泡性フレタン原液(略
称B液)を混合後、所定のモールドに注入して、発泡、
硬化、乾燥後、窒素ガス中で高温にて窒化焼成するもの
である。
Conventional technology Conventionally, as a method for manufacturing a porous body of silicon nitride, Japanese Patent Application Laid-Open No. 1983
There is No.-33272. This is a mixture of an aqueous suspension (abbreviated as liquid A) made by kneading silicon powder and water and a foamable urethane stock solution (abbreviated as liquid B), and then poured into a predetermined mold to form a foam.
After hardening and drying, it is nitrided and fired at high temperature in nitrogen gas.

発明が解決しようとする問題点 上記従来構成によれば、グリーン(生型)の大小、形状
等に応じて焼成時の昇温速度tt&密にコントロー〜す
る必要があり、そのコントロールを注意深くおこなわな
いと、製品にひび割れが発生するものである。
Problems to be Solved by the Invention According to the above-mentioned conventional configuration, it is necessary to closely control the temperature rise rate tt during firing depending on the size, shape, etc. of the green (green mold), and this control is not performed carefully. This will cause cracks in the product.

本発明は上記問題点を解消した窒化けい素の多孔体の製
造方法を提供することを目的とする。
An object of the present invention is to provide a method for manufacturing a porous silicon nitride body that eliminates the above-mentioned problems.

問題を解決するための手段 上記問題を解決するため、本発明の窒化けい素の多孔体
の製造方法は、けい素粉末および石膏を水と混合し、そ
の石膏の凝固作用を利用してグリーンを成形し、次にそ
のグリーンを窒素ガス中、1150℃〜1450℃の温
度で反応窒化させた後、酸処理するものである。
Means for Solving the Problems In order to solve the above problems, the method for producing a silicon nitride porous body of the present invention mixes silicon powder and gypsum with water, and uses the coagulation effect of the gypsum to create a green material. After molding, the green is subjected to reaction nitridation in nitrogen gas at a temperature of 1150°C to 1450°C, and then treated with acid.

実施例 以下、本発明の一実施例を説明する。まずけい素(Si
 )粉末100重量部、石* (Ca 504 ・’)
N20 )10〜100重重部、水100重量部を十分
混合した後、その水性懸濁液を、たとえばアクリル、塩
化ビニール等からなる不吸性の板上に置いた同様の不吸
性の円筒型内に流し込む。次にそれを10〜20分程度
放置し、石膏の凝固作用でけい素と石膏とからなるグリ
ーン(生型)を形成する。次にそのグリーンを十分乾燥
させた後、それを密閉炉内に入れ、N2雰囲気中、11
50℃〜1450℃で25時間反応窒化焼成を行なう。
EXAMPLE An example of the present invention will be described below. First of all, silicon
) powder 100 parts by weight, stone* (Ca 504 ・')
N20) After thoroughly mixing 10 to 100 parts by weight and 100 parts by weight of water, the aqueous suspension was placed on a non-absorbing plate made of acrylic, vinyl chloride, etc. in a similar non-absorbing cylindrical shape. Pour it inside. Next, it is left to stand for about 10 to 20 minutes, and a green (green mold) made of silicon and gypsum is formed by the coagulation effect of the gypsum. Next, after thoroughly drying the green, it was placed in a closed furnace and heated for 11 hours in an N2 atmosphere.
Reaction nitriding firing is performed at 50° C. to 1450° C. for 25 hours.

その焼成時には3 Si + 2 N2−” Si3 
N4の反応と同時に1200℃以上の温度においてCa
 S04− CaO+ 502↑++02Tなる反応が
起こり、焼成体中の石膏部は実質CaOとCa 504
との混合体となる。この焼成体を酸(たとえば塩酸、流
酸等)で1時間から2時間煮沸すると、Ca0%Ca 
504は酸により溶解し、素地として窒化けい素のみが
ab、多孔性反応焼結窒化けい禦が得られる。
At the time of firing, 3 Si + 2 N2-” Si3
Ca at a temperature of 1200℃ or higher simultaneously with the reaction of N4.
S04- CaO+ 502↑++02T reaction occurs, and the gypsum part in the fired body is essentially CaO and Ca 504
It becomes a mixture with. When this calcined body is boiled in acid (for example, hydrochloric acid, hydrochloric acid, etc.) for 1 to 2 hours, Ca0%Ca
504 is dissolved in acid, and porous reaction sintered silicon nitride with only silicon nitride as a base material is obtained.

ここで反応焼成温度が1150℃以下であると、末度応
の金属けい素が多怠に残留し、!た1450’C以上に
なると金属けい素が溶解して窒化が進まないため、焼成
温度は1150℃〜1450’Cとする。またグリーン
の石膏が10重量部以下であると、十分に凝固が起こら
ず、100重量部以上であると、円筒型内に流し込むに
は、抗性が高すぎるスラIJ +となるため、石膏は1
0〜loO重量部とする。さらに板および円筒型として
アクリル、塩化ビニール等を用いたのは、半永久的に用
いることができるためである。
If the reaction firing temperature is below 1150°C, a very large amount of metallic silicon will remain! If the temperature exceeds 1450'C, metal silicon will dissolve and nitriding will not proceed, so the firing temperature is set at 1150°C to 1450'C. Furthermore, if the amount of green plaster is less than 10 parts by weight, it will not coagulate sufficiently, and if it is more than 100 parts by weight, it will become a slurry with too high resistance to be poured into a cylindrical mold. 1
0 to loO parts by weight. Furthermore, the reason why acrylic, vinyl chloride, etc. were used for the plate and cylinder is that it can be used semi-permanently.

次に別表にけい素と石膏との比率を変えた場合の効果を
示す。
Next, the effect of changing the ratio of silicon and gypsum is shown in the attached table.

別表 次に石膏添加欺とグリーンおよび焼成体との関係は図の
ようになる。
The relationship between the addition of gypsum and green and fired bodies is shown in the attached table.

発明の効果 以上述べたごとく本発明によれば、反応窒化させた後、
酸処理して石膏部を溶解して多孔性にするものであるか
ら、焼成時の温度コントロールが容易であり、ひび割れ
のおそれはない。
Effects of the Invention As described above, according to the present invention, after reactive nitriding,
Since it is treated with acid to dissolve the gypsum part and make it porous, it is easy to control the temperature during firing and there is no risk of cracking.

【図面の簡単な説明】[Brief explanation of the drawing]

図は本発明の一実施例を示すグラフである。 The figure is a graph showing one embodiment of the present invention.

Claims (1)

【特許請求の範囲】[Claims] 1、けい素粉末および石膏を水と混合し、その石膏の凝
固作用を利用してグリーンを成形し、次にそのグリーン
を窒素ガス中、1150℃〜1450℃の温度で反応窒
化させた後、酸処理することを特徴とする窒化けい素の
多孔体の製造方法。
1. Mix silicon powder and gypsum with water, form a green using the coagulation effect of the gypsum, and then react and nitride the green at a temperature of 1150°C to 1450°C in nitrogen gas. A method for producing a porous silicon nitride body, the method comprising acid treatment.
JP6416685A 1985-03-27 1985-03-27 Manufacture of silicon nitride porous body Pending JPS61222966A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP6416685A JPS61222966A (en) 1985-03-27 1985-03-27 Manufacture of silicon nitride porous body

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP6416685A JPS61222966A (en) 1985-03-27 1985-03-27 Manufacture of silicon nitride porous body

Publications (1)

Publication Number Publication Date
JPS61222966A true JPS61222966A (en) 1986-10-03

Family

ID=13250202

Family Applications (1)

Application Number Title Priority Date Filing Date
JP6416685A Pending JPS61222966A (en) 1985-03-27 1985-03-27 Manufacture of silicon nitride porous body

Country Status (1)

Country Link
JP (1) JPS61222966A (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63312931A (en) * 1987-06-15 1988-12-21 Honda Motor Co Ltd Production of ceramic-metallic composite body
EP0757024A1 (en) 1995-07-26 1997-02-05 Sumitomo Electric Industries, Ltd. Silicon nitride porous body and method of preparing the same

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS63312931A (en) * 1987-06-15 1988-12-21 Honda Motor Co Ltd Production of ceramic-metallic composite body
EP0757024A1 (en) 1995-07-26 1997-02-05 Sumitomo Electric Industries, Ltd. Silicon nitride porous body and method of preparing the same
US5846460A (en) * 1995-07-26 1998-12-08 Sumitomo Electric Industries, Ltd. Method of preparing silicon nitride porous body

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