JP2668119B2 - Method for producing silicon carbide-silicon metal material - Google Patents
Method for producing silicon carbide-silicon metal materialInfo
- Publication number
- JP2668119B2 JP2668119B2 JP63059437A JP5943788A JP2668119B2 JP 2668119 B2 JP2668119 B2 JP 2668119B2 JP 63059437 A JP63059437 A JP 63059437A JP 5943788 A JP5943788 A JP 5943788A JP 2668119 B2 JP2668119 B2 JP 2668119B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon
- silicon carbide
- metal
- carbide powder
- producing
- 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 - Lifetime
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/515—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
- C04B35/56—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
- C04B35/565—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Ceramic Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Ceramic Products (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は、金属けい素を含浸させることにより、ガス
不透過性にさせた炭化けい素−金属けい素材料の製造方
法に関する。Description: TECHNICAL FIELD The present invention relates to a method for producing a silicon carbide-metal silicon material which is made gas impermeable by impregnating it with silicon metal.
特に、半導体製造用拡散炉に用いる均熱管や加熱炉用
耐熱性構造材として用いられるラジアントチューブの製
造方法に関する。In particular, the present invention relates to a method for manufacturing a soaking tube used in a diffusion furnace for semiconductor manufacturing and a radiant tube used as a heat-resistant structural material for a heating furnace.
一般に、半導体製造用拡散炉に用いられる均熱管は、
半導体材料を均一に焼成する為の部材であるが、均熱管
外部からの不純物の混入を防ぐ為にガス不透過性にする
必要がある。Generally, a soaking tube used in a diffusion furnace for semiconductor manufacturing is:
It is a member for uniformly firing the semiconductor material, but it is necessary to make it gas impermeable in order to prevent impurities from being mixed in from outside the heat equalizing tube.
更に、加熱炉用耐熱構造材として用いられるセラミッ
クスラジアントチューブは使用目的から燃焼ガスがラジ
アントチューブ表面に漏れないようにする為ガス不透過
性が必要となる。Further, a ceramic radiant tube used as a heat-resistant structural material for a heating furnace needs gas impermeability in order to prevent combustion gas from leaking to the surface of the radiant tube for the purpose of use.
従来、上述の用途には、炭化けい素−金属けい素材料
が用いられており、ガス不透過性にする為の方法として
は、従来、再結晶化させた炭化けい素焼成体の気孔部に
金属けい素を含浸させる方法や反応焼結炭化けい素焼成
体の未反応けい素として残留させてガス不透過性にする
方法があるが、再結晶化の工程や反応焼結の工程におい
て少なくとも1850℃、望ましくは2150℃という高温の加
熱装置が必要であり、結果的に製品価格が高くなるとい
う欠点を持っていた。Conventionally, silicon carbide-metal silicon materials have been used for the above-mentioned applications. As a method for making gas impermeable, conventionally, metal pores in a recrystallized silicon carbide fired body are used. There is a method of impregnating silicon or a method of leaving gas as gas-impermeable by leaving it as unreacted silicon in a reaction sintered silicon carbide fired body, but at least 1850 ° C. in a recrystallization step or a reaction sintering step. Desirably, a heating device with a high temperature of 2150 ° C. is required, resulting in a high product price.
又、前記欠点を解消する方法としては、発明者らは、
先に公開特許昭和62年36087号公報にて炭化けい素グリ
ーン体に1414℃〜1800℃の温度で金属けい素を含浸させ
ることにより、ガス不透過性にする方法を開示している
が、1414℃〜1460℃ではグリーン体に金属けい素を含浸
充填させる事はできるが均一に充填することは難しかっ
た。特に金属けい素含浸温度が低いほど金属けい素の含
浸ムラが生ずるという欠点を有していた。Further, as a method for solving the above-mentioned disadvantage, the inventors have
Previously, Japanese Patent Publication No. 36087/1987 discloses a method of impregnating a silicon carbide green body with silicon metal at a temperature of 1414 ° C. to 1800 ° C. to make it impermeable to gas. It was possible to impregnate and fill the green body with metallic silicon at ℃ ~ 1460 ℃, but it was difficult to fill it uniformly. In particular, the lower the impregnation temperature of the metal silicon, the more uneven the impregnation of the metal silicon.
また、1460℃を超える温度下でも、金属けい素の含浸
が時間がかかったり、未含浸部分が残ることもあり、安
定した金属けい素の含浸が望まれていた。Further, even at a temperature higher than 1460 ° C., it may take a long time to impregnate the metal silicon, or an unimpregnated portion may remain, so that stable impregnation of the metal silicon has been desired.
本発明は、上記の問題点を解消するためになされたも
ので、炭化けい素グリーン体に金属けい素を均一に含浸
させるガス不透過性の炭化けい素−金属けい素材料の製
造方法を提供するものである。The present invention has been made to solve the above problems, and provides a method for producing a gas-impermeable silicon carbide-metal silicon material that uniformly impregnates silicon metal into a silicon carbide green body. Is what you do.
本発明は、金属けい素を均一に安定して含浸させるた
めの条件を研究した結果、使用する炭化けい素粉末に含
まれる二酸化けい素の量を規制することにより、今まで
特に困難であった1460℃以下の温度でも容易に金属けい
素を含浸できることを知見した。The present invention, as a result of studying conditions for uniformly and stably impregnating metallic silicon, has been particularly difficult until now by regulating the amount of silicon dioxide contained in the silicon carbide powder used. We have found that metallic silicon can be easily impregnated even at temperatures below 1460 ° C.
すなわち、本発明は炭化けい素粉末を所定の形状に形
成したグリーン体において、出発原料である炭化けい素
粉末を処理し、含有する二酸化けい素量を1.0重量％以
下にし、炭化けい素を成形して得られたグリーン体を窒
素又はアルゴン等の不活性ガス雰囲気もしくは真空中に
て、1414℃〜1800℃の加熱下で、金属けい素を含浸し、
充填することを特徴とする。That is, in the present invention, in a green body in which silicon carbide powder is formed into a predetermined shape, silicon carbide powder as a starting material is treated to reduce the amount of silicon dioxide contained to 1.0% by weight or less, and to form silicon carbide. The green body obtained in an inert gas atmosphere such as nitrogen or argon or in a vacuum, under heating at 1414 ° C to 1800 ° C, impregnated with metallic silicon,
It is characterized by filling.
二酸化けい素が含まれた場合、金属けい素との接触角
が大きいため濡れにくい。このため金属けい素が均一に
安定して含浸されない。一般に市販されている炭化けい
素粉末には二酸化けい素が1.0〜3.0％含まれている。即
ち、該炭化けい素粉末を使用して所定の形状に成形した
グリーン体にも二酸化けい素が1.0〜3.0％以上含まれて
おり、従来、金属けい素の含浸が不均一である原因とな
っていた。When silicon dioxide is included, it is difficult to get wet because the contact angle with the metal silicon is large. Therefore, the metallic silicon is not uniformly and stably impregnated. Generally, commercially available silicon carbide powder contains 1.0 to 3.0% of silicon dioxide. That is, the green body formed into a predetermined shape using the silicon carbide powder also contains silicon dioxide in an amount of 1.0 to 3.0% or more, which has been a cause of non-uniform impregnation of silicon metal. I was
一方本発明では、二酸化けい素の含有量を１重量％以
下になるよう炭化けい素粉末を処理することにより安定
して均一に金属けい素が含浸されるもので、特に1414℃
〜1460℃の温度域での含浸に効果が大きい。On the other hand, in the present invention, by treating the silicon carbide powder so that the content of silicon dioxide is 1% by weight or less, the silicon metal is stably and uniformly impregnated, and particularly 1414 ° C.
Greatly effective for impregnation in the temperature range of ~ 1460 ° C.
上記の炭化けい素粉末から二酸化けい素を取り除く方
法は、フッ化水素酸による処理や真空下での加熱処理に
て容易に行うことができる。また、1414℃〜1800℃の範
囲については、金属けい素の融点である1414℃以上が最
低限必要であることと、1800℃を超えると二酸化けい素
が分解してしまい、二酸化けい素の量を規制する必要が
ないことと製造コストが大巾に高くなる。The method of removing silicon dioxide from the silicon carbide powder can be easily performed by treatment with hydrofluoric acid or heat treatment under vacuum. In addition, for the range of 1414 ° C to 1800 ° C, the minimum required is 1414 ° C or more, which is the melting point of silicon metal, and when it exceeds 1800 ° C, silicon dioxide is decomposed and the amount of silicon dioxide is increased. Need to be regulated and the manufacturing costs are greatly increased.
次に本発明を実施例により説明する。 Next, the present invention will be described with reference to examples.
まず、二酸化けい素の量が1.8重量％含む、粒径１〜6
00μｍの炭化けい素粉末をフッ化水素酸に24時間浸した
のち、純水にて水洗した。二酸化けい素の量は0.5％に
なった。上記の炭化けい素粉末に、セルロース系バイン
ダー、可塑剤としてのポリエチレングリコール、及び水
を加えて、混練した後、外径φ255mm、内径φ240mm、長
さ200mmのチューブ状に成形してグリーン体を得た。約1
50℃で乾燥後、該グリーン体の内径側に金属けい素を置
いて、アルゴン雰囲気1450℃の温度で金属けい素を含浸
させた。得られた炭化けい素−金属けい素材料に0.5kg/
cm2のエアー圧力をかけた時のエアーもれはなく、ガス
不透過性であり、均一に金属けい素が含浸されていた。First, a particle size of 1 to 6 containing 1.8% by weight of silicon dioxide.
After immersing the silicon carbide powder of 00 μm in hydrofluoric acid for 24 hours, it was washed with pure water. The amount of silicon dioxide was 0.5%. To the above silicon carbide powder, a cellulosic binder, polyethylene glycol as a plasticizer, and water were added, kneaded, and then formed into a tube having an outer diameter of 255 mm, an inner diameter of 240 mm, and a length of 200 mm to obtain a green body. Was. About 1
After drying at 50 ° C., metallic silicon was placed on the inner diameter side of the green body, and impregnated with metallic silicon at a temperature of 1450 ° C. in an argon atmosphere. The obtained silicon carbide-metallic silicon material has a weight of 0.5 kg /
There was no air leakage when an air pressure of 2 cm was applied, the gas was impermeable, and the silicon metal was uniformly impregnated.
まず、二酸化けい素の量が1.1重量％含む粒径１〜600
μｍの炭化けい素粉末を上記実施例と同寸法に成形し、
グリーン体を得た。約150℃で乾燥后、上記実施例と同
様にして1450℃の温度で金属けい素を含浸させた。得ら
れた、炭化けい素−金属けい素材料に0.5kg/cm2のエア
ー圧力をかけた時エアーもれが見られた。First, a particle diameter of 1 to 600% containing 1.1% by weight of silicon dioxide.
μm silicon carbide powder was molded to the same dimensions as the above example,
I got a green body. After drying at about 150 ° C., it was impregnated with silicon metal at a temperature of 1450 ° C. in the same manner as in the above example. When an air pressure of 0.5 kg / cm 2 was applied to the obtained silicon carbide-metal silicon material, air leakage was observed.
以上、述べたように、本発明によれば、使用する炭化
けい素粉末に含まれる二酸化けい素の量を1.0重量％以
下に規制し、且つ、1414℃〜1800℃の温度域で金属けい
素を含浸することにより、金属けい素を安定的で均一に
含浸することができる。従来、特に低温域（1414℃〜14
60℃）で金属けい素を含浸させた場合、金属けい素の含
浸ムラが生じたのに比べ、本発明は炭化けい素粉末に含
まれる二酸化けい素の量を1.0重量％以下にすることに
より、容易に含浸できた。本発明が半導体製造用拡散炉
の均熱管や耐熱構造材としてのラジアントチューブを製
造する上で産業上の効果は大きい。As described above, according to the present invention, the amount of silicon dioxide contained in the silicon carbide powder used is regulated to 1.0% by weight or less, and the metal silicon is used in the temperature range of 1414 ° C to 1800 ° C. By impregnating, metal silicon can be stably and uniformly impregnated. Conventionally, especially in the low temperature range (1414 ℃ ~ 14
(60 ° C.), when impregnated with silicon metal, the metal silicon impregnation unevenness occurred, but the present invention reduces the amount of silicon dioxide contained in the silicon carbide powder to 1.0% by weight or less. , Could be easily impregnated. INDUSTRIAL APPLICABILITY The present invention has a great industrial effect in producing a soaking tube for a semiconductor manufacturing diffusion furnace and a radiant tube as a heat-resistant structural material.
Claims (2)
リーン体に金属けい素を含浸して得られる炭化けい素−
金属けい素材料の製造方法において、出発原料である炭
化けい素粉末を処理し、含有する二酸化けい素量を1.0
重量％以下にし、炭化けい素を成形して得られたグリー
ン体を不活性ガス雰囲気もしくは真空中にて、1414℃〜
1800℃の加熱下で金属けい素を含浸し、充填することを
特徴とする炭化けい素−金属けい素材料の製造方法。1. A silicon carbide powder obtained by impregnating a green body formed of a silicon carbide powder into a predetermined shape with metal silicon.
In the method for producing a silicon metal material, a silicon carbide powder as a starting material is treated, and the amount of silicon dioxide contained is reduced to 1.0.
The green body obtained by forming silicon carbide in an amount of not more than 14% by weight is heated to 1414 ° C in an inert gas atmosphere or vacuum.
A method for producing a silicon carbide-silicon metal material, comprising impregnating and filling silicon metal under heating at 1800 ° C.
項１記載の方法。2. The method according to claim 1, wherein the inert gas is nitrogen or argon.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63059437A JP2668119B2 (en) | 1988-03-15 | 1988-03-15 | Method for producing silicon carbide-silicon metal material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63059437A JP2668119B2 (en) | 1988-03-15 | 1988-03-15 | Method for producing silicon carbide-silicon metal material |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH01234370A JPH01234370A (en) | 1989-09-19 |
| JP2668119B2 true JP2668119B2 (en) | 1997-10-27 |
Family
ID=13113255
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63059437A Expired - Lifetime JP2668119B2 (en) | 1988-03-15 | 1988-03-15 | Method for producing silicon carbide-silicon metal material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2668119B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP5048266B2 (en) | 2006-04-27 | 2012-10-17 | 株式会社アライドマテリアル | Heat dissipation board and manufacturing method thereof |
| CN114430733B (en) * | 2019-10-02 | 2023-05-09 | 日本碍子株式会社 | Refractory material |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS6036374A (en) * | 1983-08-09 | 1985-02-25 | セントラル硝子株式会社 | Purification of non-oxide ceramic powder |
| JPS6236087A (en) * | 1985-08-06 | 1987-02-17 | 東海高熱工業株式会社 | Granular sic-dispersed metal silicon heat-resistant material |
-
1988
- 1988-03-15 JP JP63059437A patent/JP2668119B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH01234370A (en) | 1989-09-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPS624349B2 (en) | ||
| US5571758A (en) | Nitrogen-reacted silicon carbide material | |
| JPH05186266A (en) | Production of carbon fiber-reinforced silicon carbide composite ceramic | |
| KR890008059A (en) | Porous membrane and its manufacturing method | |
| CN107868998A (en) | A kind of silicon nitride fiber and preparation method thereof | |
| JP2668119B2 (en) | Method for producing silicon carbide-silicon metal material | |
| KR100520436B1 (en) | Method for Making Oxidation Protective Double Coating for Carbon/Carbon Composite | |
| US4122220A (en) | Method for reducing the gas permeability of a sintered porous silicon nitride body | |
| JP2919901B2 (en) | Melting crucible equipment | |
| JP3378608B2 (en) | Method for producing silicon carbide substrate for jig for semiconductor production | |
| KR100520435B1 (en) | Method for Making Oxidation Protective Coating for Carbon/Carbon Composite | |
| JPS6241768A (en) | Manufacture of aluminum nitride sintered body | |
| JPH0359033B2 (en) | ||
| JPH10253259A (en) | Material of roller for roller hearth furnace and manufacture thereof | |
| JP2794679B2 (en) | Method for producing high-density ITO sintered body | |
| JP3277295B2 (en) | Method for producing high-temperature silicon carbide heating element | |
| JPH01115888A (en) | Production of jig for producing semiconductor | |
| KR970063316A (en) | Cathode using a thermo-pellet and its manufacturing method | |
| JPS5544208A (en) | Manufacture for diaphragm for speaker | |
| JPS583996B2 (en) | Chimitunatanka Keiso Shitsu Keitaino Seizouhouhou | |
| JPH0431364A (en) | Production of silicon carbide sintered compact | |
| JPH05310473A (en) | Silicon carbide member | |
| JPS5939769A (en) | Method of sintering silicon nitride | |
| JPH0532356B2 (en) | ||
| JP2000211972A (en) | Silicon carbide heating element and its production |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| R250 | Receipt of annual fees |
Free format text: JAPANESE INTERMEDIATE CODE: R250 |
|
| EXPY | Cancellation because of completion of term | ||
| FPAY | Renewal fee payment (event date is renewal date of database) |
Free format text: PAYMENT UNTIL: 20080704 Year of fee payment: 11 |