JP2938926B2 - Silicon carbide member and method of manufacturing the same - Google Patents
Silicon carbide member and method of manufacturing the sameInfo
- Publication number
- JP2938926B2 JP2938926B2 JP9813490A JP9813490A JP2938926B2 JP 2938926 B2 JP2938926 B2 JP 2938926B2 JP 9813490 A JP9813490 A JP 9813490A JP 9813490 A JP9813490 A JP 9813490A JP 2938926 B2 JP2938926 B2 JP 2938926B2
- Authority
- JP
- Japan
- Prior art keywords
- silicon carbide
- silicon
- impregnated
- glassy carbon
- carbide substrate
- 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
Description
【発明の詳細な説明】 （産業上の利用分野） 本発明はシリコン含浸炭化珪素基材の表面にガラス状
カーボン層を有する炭化珪素質部材及びその製造方法に
関する。Description: TECHNICAL FIELD The present invention relates to a silicon carbide member having a glassy carbon layer on the surface of a silicon-impregnated silicon carbide substrate and a method for producing the same.
（先行の技術） 半導体素子製造用の拡散炉の材料として耐熱衝撃性及
び機械的強度に優れた炭化珪素が広く用いられている。(Prior art) Silicon carbide having excellent thermal shock resistance and mechanical strength is widely used as a material of a diffusion furnace for manufacturing semiconductor devices.
炭化珪素の該拡散炉への使用においては、炭化珪素成
形体中の微量の不純物の残留が問題となっている。その
ため半導体用の炭化珪素は、内部の純化を行なって不純
物を取除くとともに、不純物拡散の原因となる気孔中に
シリコンを含浸させ、不純物の拡散を防いでいるのが実
情である。この不純物の除去方法として、例えば炭化珪
素を1300℃程度の温度で塩化水素ガスを吹付ける等の方
法が採用されており、常に拡散炉内を高純度に保つため
に、前述のような純化処理を定期的に行なうことが必要
である。When silicon carbide is used in the diffusion furnace, there is a problem that trace amounts of impurities in the silicon carbide compact remain. Therefore, in fact, silicon carbide for semiconductors is internally purified to remove impurities, and at the same time, silicon is impregnated into pores that cause impurity diffusion to prevent impurity diffusion. As a method of removing the impurities, for example, a method of spraying hydrogen chloride gas on silicon carbide at a temperature of about 1300 ° C. is employed. In order to always keep the inside of the diffusion furnace at a high purity, the above-described purification treatment is performed. It is necessary to carry out regularly.
しかし、上記のような塩化水素ガス等の処理ガスを用
いる純化方法では、処理ガスと含浸したシリコンが反応
し、シリコン含浸炭化珪素基材表面が侵食され、また、
侵食された部分は、拡散炉等として使用するときに、不
純物を残しやすく、次第に半導体用拡散炉としては使え
なくなるという欠点を有していた。However, in the purification method using a processing gas such as a hydrogen chloride gas as described above, the processing gas and the impregnated silicon react, and the silicon-impregnated silicon carbide substrate surface is eroded,
The eroded portion has a disadvantage that when it is used as a diffusion furnace or the like, impurities tend to remain, and the eroded portion gradually becomes unusable as a semiconductor diffusion furnace.
本発明は、以上のような欠点を解消するためになされ
たものであり、純化処理しやすく、なおかつ、純化によ
り、表面が侵されない炭化珪素質部材を提供するもので
ある。The present invention has been made to solve the above-mentioned disadvantages, and provides a silicon carbide-based member that can be easily purified and has a surface that is not damaged by the purification.
（問題点を解決する為の手段） 本発明の炭化珪素質部材はシリコン含浸炭化珪素基材
にガラス状カーボンが含浸及び／又は塗布されその表面
がガラス状カーボンで被覆されているものである。(Means for Solving the Problems) The silicon carbide-based member of the present invention is obtained by impregnating and / or applying glassy carbon to a silicon-impregnated silicon carbide substrate and coating the surface thereof with glassy carbon.
ガラス状カーボンは高温において、化学的にも、強度
的にも安定しており、また、気孔が非常に少ないため
に、シリコン含浸炭化珪素基材表面に塗布および／また
は、含浸された場合、純化処理ガス等に対し、反応する
ことなくシリコン含浸炭化珪素基材を保護する役目を有
する。加えて、ガラス状カーボンは、非常に不純物を通
しやすい性質を備えており、そのためシリコン含浸炭化
珪素基材表面に一様にガラス状カーボンを塗布および／
または、含浸してもシリコン含浸炭化珪素基材まで十分
に純化できるものである。Vitreous carbon is chemically and mechanically stable at high temperatures, and has very few pores. Therefore, when it is applied and / or impregnated on the surface of a silicon-impregnated silicon carbide substrate, it is purified. It has a role of protecting the silicon-impregnated silicon carbide substrate without reacting to a processing gas or the like. In addition, glassy carbon has a property of being very easy to pass impurities, so that the glassy carbon is uniformly applied to the surface of the silicon-impregnated silicon carbide substrate and / or
Alternatively, even if it is impregnated, the silicon-impregnated silicon carbide substrate can be sufficiently purified.
本発明のシリコン含浸炭化珪素基材としては、その表
面にCVDによるSiC膜を有するものを用いてもよい。CVD
−SiC膜を有するものにガラス状カーボンを含浸および
／または塗布すれば、HCl等の純化ガスにおかされずに
不純物の低減にさらなる効果をあげることは言うまでも
ない。As the silicon-impregnated silicon carbide substrate of the present invention, a substrate having a SiC film formed by CVD on its surface may be used. CVD
Needless to say, impregnating and / or applying glassy carbon to a material having a SiC film has a further effect in reducing impurities without leaving a purified gas such as HCl.
ガラス状炭素の厚みは特に限定されていないが、0.1
〜1000μｍ、より好ましくは0.5〜200μｍであることが
好ましい。薄すぎれば膜の効果がなく、厚すぎれば不純
物を取除くにくくなる。The thickness of the glassy carbon is not particularly limited, but 0.1
It is preferable that the thickness be in the range of 10001000 μm, more preferably 0.5-200 μm. If the thickness is too small, the film has no effect. If the thickness is too large, it is difficult to remove impurities.
本発明のシリンコ含浸珪素基材は、例えば粒径0.1〜2
00μｍの高純度炭化珪素粉末を原料として公知の方法を
用いて造られる。その方法を簡単に説明すると、純化し
た炭化珪素粉末にフェノール樹脂を加えて、混練して造
粒物を造る。得られた造粒物を用いてプレス成形、押出
成形等を行ない成形体を得る。成形体を約130℃に加熱
してフェノール樹脂を硬化し、仮焼して多孔質炭化珪素
成形体を得る。この多孔質炭化珪素成形体を公知の方法
で純化処理して更に、公知の方法でシリコンを含浸し
て、シリコン含浸炭化珪素基材を得る。The syringe-impregnated silicon substrate of the present invention has, for example, a particle size of 0.1 to 2
It is manufactured using a known method using a high-purity silicon carbide powder of 00 μm as a raw material. Briefly, the method involves adding a phenol resin to purified silicon carbide powder and kneading to produce a granulated product. Press molding, extrusion molding, and the like are performed using the obtained granules to obtain a molded body. The molded body is heated to about 130 ° C. to cure the phenolic resin and calcined to obtain a porous silicon carbide molded body. This porous silicon carbide molded body is purified by a known method and further impregnated with silicon by a known method to obtain a silicon-impregnated silicon carbide substrate.
純化処理の方法とは、例えば、（ｉ）1300℃程度の温
度下で塩化水素ガスを吹き付ける公知の方法、又は（i
i）不活性ガスをキャリヤーガスとしてハロゲン又はハ
ロゲン化水素の雰囲気下で1600〜2000℃の温度に加熱す
る公知の方法等が挙げられる。The purification method is, for example, (i) a known method of blowing hydrogen chloride gas at a temperature of about 1300 ° C., or (i)
i) A known method in which an inert gas is used as a carrier gas and heated to a temperature of 1600 to 2000 ° C. in an atmosphere of halogen or hydrogen halide is used.
炭化珪素基材にガラス状炭素を含浸及び／又は塗布し
ガラス状カーボンを被覆する方法は公知の方法を適用し
得る。A known method can be applied to the method of impregnating and / or applying glassy carbon to the silicon carbide substrate and coating the glassy carbon.
以下にその例を記載する。 An example is described below.
（１）フラン樹脂やフェノール樹脂等の熱硬化性樹脂に
酸触媒を所要のモル比で混合し、初期縮合物を生成す
る。(1) An acid catalyst is mixed with a thermosetting resin such as a furan resin or a phenol resin in a required molar ratio to generate an initial condensate.
ハロゲン化水素でエッチング処理された炭化珪素基材
をオートクレーブに入れ約20mmHg程度で減圧処理した後
に、該熱硬化性樹脂初期縮合物をオートクレーブ中に注
入する。引き続き、オートクレーブ中に空気を導入し、
約4kg/cm2以上に加圧して熱硬化性樹脂初期縮合物を炭
化珪素基材に含浸、且つその表面を被覆する。得られた
含浸・被覆された炭化珪素基材を不活性ガス雰囲気下で
1,000〜2,000℃で焼成してガラス状カーボンで被覆され
た炭化珪素質部材を得る。The silicon carbide substrate etched with hydrogen halide is placed in an autoclave and subjected to a reduced pressure treatment at about 20 mmHg, and then the thermosetting resin precondensate is injected into the autoclave. Continue to introduce air into the autoclave,
The silicon carbide substrate is impregnated with the thermosetting resin precondensate by applying a pressure of about 4 kg / cm 2 or more, and its surface is coated. The obtained impregnated and coated silicon carbide substrate is placed under an inert gas atmosphere.
It is fired at 1,000 to 2,000 ° C. to obtain a silicon carbide member coated with glassy carbon.
シリコン含浸炭化珪素基材の表面がなめらかな場合
は、熱硬化性樹脂初期縮合物をその表面に塗布し、不活
性ガス雰囲気中で1,000〜2,000℃で焼成してガラス状カ
ーボンで被覆された炭化珪素質部材を得る。If the surface of the silicon-impregnated silicon carbide substrate is smooth, a thermosetting resin precondensate is applied to the surface and calcined at 1,000 to 2,000 ° C in an inert gas atmosphere to form a carbonized carbonized substrate. A silicon member is obtained.
本発明で用いるガラス状カーボンの前駆体として用い
る熱硬化性樹脂には、フェノール系やフラン系初期縮合
物以外、メラミン等のガラス状カーボンを生成する他の
前駆体を用いても、本発明の目的を奏効し得る。The thermosetting resin used as a precursor of the glassy carbon used in the present invention, other than a phenol-based or furan-based initial condensate, even when using other precursors that produce glassy carbon such as melamine, the present invention It can serve its purpose.
（２）フルフリールアルコールにｐ−トルエンスルフォ
ン酸を加えて得た粘度1000−4000ポイズの混合液を炭化
珪素基材に塗布し、得られた塗布された炭化珪素基材を
不活性ガス雰囲気下で1,000〜2,000℃で焼成してガラス
状カーボンで被覆された炭化珪素質部材を得る。(2) A 1000-4000 poise mixed solution obtained by adding p-toluenesulfonic acid to furfuryl alcohol is applied to a silicon carbide substrate, and the obtained applied silicon carbide substrate is placed in an inert gas atmosphere. It is baked at 1,000 to 2,000 ° C. below to obtain a silicon carbide member coated with glassy carbon.
（発明の効果） 本発明の炭化珪素質部材は、ハロゲンガス又はハロゲ
ン化水素で純化処理することによって、炭化珪素部材中
のシリコンが侵食（エッチング）されることなく、また
ガラス状カーボンも全く侵食されることなく炭化珪素部
材の内部まで純化することが出来る。更に、シリコン含
浸炭化珪素基材とガラス状カーボン層との接着力が強
く、剥離がほとんど起らず、耐熱衝撃性及び機械的強度
の優れた炭化珪素質部材である。(Effect of the Invention) By purifying the silicon carbide member of the present invention with a halogen gas or hydrogen halide, the silicon in the silicon carbide member is not eroded (etched), and the glassy carbon is completely eroded. It is possible to purify even the inside of the silicon carbide member without being performed. Further, the silicon carbide-based member has a strong adhesive force between the silicon-impregnated silicon carbide substrate and the glassy carbon layer, hardly peels off, and has excellent thermal shock resistance and mechanical strength.
従って、本発明の炭化珪素質部材は半導体素子製造用
の拡散炉の材料として有用なものである。Therefore, the silicon carbide-based member of the present invention is useful as a material for a diffusion furnace for manufacturing semiconductor devices.
以下、実施例によって本発明を詳細に説明するが、本
発明はこれら実施例に限定されるものではない。Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited to these examples.
実施例及び比較例 純化した炭化珪素粉末にバインダーとしてフェノール
樹脂を加えて、混練して造粒物を造り、得られた造粒物
を用いてプレス成形を行ない成形体を得た。成形体を乾
燥後1800℃で仮焼して、次いで純化し、さらに1600℃の
溶融シリコンに含浸してシリコン含浸炭化珪素基材を得
た。得られたシリコン含浸炭化珪素基材にフルフリルア
ルコールにパラトルエンスルホン酸を加え、粘性を調整
したものを所定の厚さまで塗布し、不活性雰囲気で1600
℃まで昇温し、シリコン含浸炭化珪素基材の表面に０μ
ｍ（比較例）、２μｍ（実施例１）、75μｍ（実施例
２）、500μｍ（実施例３）、1500μｍ（比較例２）の
ガラス状カーボン膜厚を有するシリコン含浸炭化珪素部
材を得た。該シリコン含浸炭化珪素部材をそれぞれ1300
℃に加熱し、塩化水素ガスを用いて純化を行なった。Examples and Comparative Examples A phenol resin was added as a binder to purified silicon carbide powder, and the mixture was kneaded to produce a granulated product, and the obtained granulated product was subjected to press molding to obtain a molded product. After drying, the compact was calcined at 1800 ° C., then purified, and further impregnated with molten silicon at 1600 ° C. to obtain a silicon-impregnated silicon carbide substrate. To the resulting silicon-impregnated silicon carbide substrate was added furfuryl alcohol and p-toluenesulfonic acid, the viscosity of which was adjusted to a predetermined thickness, and applied in an inert atmosphere at 1600.
Temperature to 0 ° C, and the surface of silicon-impregnated silicon carbide
A silicon-impregnated silicon carbide member having a glassy carbon film thickness of m (Comparative Example), 2 μm (Example 1), 75 μm (Example 2), 500 μm (Example 3), and 1500 μm (Comparative Example 2) was obtained. Each of the silicon-impregnated silicon carbide members was 1300
C. and purified using hydrogen chloride gas.
結果は次表の通りであった。 The results were as shown in the following table.
１μｍ〜1000μｍのガラス状カーボン膜を有するもの
は基材の純度、膜のライフが飛躍的に向上するのに対
し、膜なしおよび0.1μｍ未満の薄膜は基材の純度は非
常に良い（良く純化される）が純化ガラスにより、基材
中のシリコンがエッチングされる。また、薄膜は耐食性
に劣り、1000μｍより厚い超厚膜はヒートサイクル時に
熱膨張係数の違いから応力が発生し、クラックが生じ、
純度低下を招くことがわかる。 Those having a glassy carbon film of 1 μm to 1000 μm dramatically improve the purity of the substrate and the life of the film, while those without the film and thin films of less than 0.1 μm have very good substrate purity (good purification). The silicon in the base material is etched by the purified glass. In addition, the thin film is inferior in corrosion resistance, and the super-thick film thicker than 1000 μm generates stress due to the difference in the coefficient of thermal expansion during the heat cycle, causing cracks,
It can be seen that the purity is reduced.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 角谷 雅之 山形県西置賜郡小国町大字小国町378番 地 東芝セラミツクス株式会社小国製造 所内 (72)発明者 外谷 栄一 山形県西置賜郡小国町大字小国町378番 地 東芝セラミツクス株式会社小国製造 所内 (72)発明者 稲葉 毅 山形県西置賜郡小国町大字小国町378番 地 東芝セラミツクス株式会社小国製造 所内 (72)発明者 目黒 和教 山形県西置賜郡小国町大字小国町378番 地 東芝セラミツクス株式会社小国製造 所内 (56)参考文献 特開 昭63−55183（ＪＰ，Ａ) 特開 昭63−35452（ＪＰ，Ａ) (58)調査した分野(Int.Cl.6，ＤＢ名) C04B 41/87 C04B 41/89 ──────────────────────────────────────────────────続 き Continuing on the front page (72) Inventor Masayuki Kadoya 378 Oguni-machi, Oguni-machi, Oguni-machi, Nishiokitama-gun, Yamagata Prefecture Inside the Oguni Plant of Toshiba Ceramics Co., Ltd. 378 Toshiba Ceramics Co., Ltd.Oguni Works (72) Inventor Takeshi Inaba Oguni-machi, Oguni-machi, Nishiokitama-gun, Yamagata Prefecture 378 Toshiba Ceramics Co., Ltd.Oguni Works (72) Inventor Kazunori Meguro Ogunimachi, Nishiokitama-gun, Yamagata Prefecture 378 Oguni-machi Oguni-machi Toshiba Ceramics Co., Ltd. Oguni Works (56) References JP-A-63-55183 (JP, A) JP-A-63-35452 (JP, A) (58) Fields investigated (Int. . 6 , DB name) C04B 41/87 C04B 41/89
Claims (2)
状カーボン層を有する炭化珪素質部材。1. A silicon carbide-based member having a glassy carbon layer on the surface of a silicon-impregnated silicon carbide substrate.
材にガラス状カーボンの前駆体を含浸及び／又は塗布
し、熱処理することから成る炭化珪素質部材の製造方
法。2. A method for producing a silicon carbide-based member, comprising impregnating and / or applying a precursor of glassy carbon to a silicon carbide substrate which has been impregnated with silicon and purified, and heat-treated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9813490A JP2938926B2 (en) | 1990-04-13 | 1990-04-13 | Silicon carbide member and method of manufacturing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP9813490A JP2938926B2 (en) | 1990-04-13 | 1990-04-13 | Silicon carbide member and method of manufacturing the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03295882A JPH03295882A (en) | 1991-12-26 |
| JP2938926B2 true JP2938926B2 (en) | 1999-08-25 |
Family
ID=14211776
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP9813490A Expired - Fee Related JP2938926B2 (en) | 1990-04-13 | 1990-04-13 | Silicon carbide member and method of manufacturing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2938926B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2011146506A (en) * | 2010-01-14 | 2011-07-28 | Sumco Corp | Susceptor for vapor phase growth device, and vapor phase growth device |
| JP2017024923A (en) * | 2015-07-16 | 2017-02-02 | イビデン株式会社 | Ceramic composite material |
-
1990
- 1990-04-13 JP JP9813490A patent/JP2938926B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH03295882A (en) | 1991-12-26 |
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