JP4014724B2 - Method for producing silica glass - Google Patents
Method for producing silica glass Download PDFInfo
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- JP4014724B2 JP4014724B2 JP08344798A JP8344798A JP4014724B2 JP 4014724 B2 JP4014724 B2 JP 4014724B2 JP 08344798 A JP08344798 A JP 08344798A JP 8344798 A JP8344798 A JP 8344798A JP 4014724 B2 JP4014724 B2 JP 4014724B2
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- graphite
- silica glass
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/09—Other methods of shaping glass by fusing powdered glass in a shaping mould
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
- C03B2201/03—Impurity concentration specified
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- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Re-Forming, After-Treatment, Cutting And Transporting Of Glass Products (AREA)
- Glass Compositions (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は高純度シリカガラスからなる成形体、特には大型円柱あるいは大型リング等の製造方法に関する。このシリカガラス部材は、半導体用耐熱治具及び各種フランジ類、炉心管部品などに応用できる。
【０００２】
【従来の技術】
耐熱金属から構成された空間に結晶質石英粉末を充填し、１７００℃以上に加熱溶融してシリカガラスを製造する方法が、すでに特公昭３５−７９１に記載されている。また最近、特開平９−２０２６３１、特開平９−２０２６３２、特開平９−１８３６２３には、黒鉛材からなる容器とシリカ粉末の接触面にシリカガラスを介在させ、加熱溶融してシリカガラスを製造する方法が開示されている。
【０００３】
【発明が解決しようとする課題】
特公昭３５−７９１では、モ−ルドとして、耐熱金属であるＭｏを用いているが、この方法ではＭｏが高温酸化を受け、ガスとして、得られるシリカガラスに侵入し、汚染するという問題があった。
【０００４】
また、モ−ルドとして、黒鉛材を用いた場合、ＣとＳｉＯ2 との高温反応によって、モ−ルドとシリカガラスが融着し相互に損傷したり、融着を避け得た場合でもモールドの耐久性は著しく低い等の問題があった。
【０００５】
更に、一般の黒鉛材には、１ｐｐｍを遥かに越えるＦｅ，Ｃａなどが含まれており、これら不純物が高温でガス化し、ガラスに侵入し、高純度が保てないという問題もあった。
【０００６】
特開平９−２０２６３１、特開平９−２０２６３２、特開平９−１８３６２３には、黒鉛鋳型とシリカ粉末の間にシリカガラスを介在させることにより、上記問題を解決する方法が開示されている。しかし、この方法は介在させるシリカガラスの加工製造に手間を要し、かつ、シリカガラスは高価であるため、経済性に優れた方法とは言い難い。また、これらの方法は、８インチウェーハー処理サイズの中型部材に適用できるが、１２インチ以上の大型フランジ部材には適用できない。すなわち溶融加熱時間の延長だけではシリカガラス中の集合気泡は除去できない、という問題があった。
【０００７】
本発明の目的は、集合気泡が無く、高純度であり、また外径３００〜５５０ｍｍ、高さ２００ｍｍ程度の大型サイズが可能であるリングを含めたシリカガラスを提供することであり、従来、行われていたシリカガラスブロックから機械加工する方法よりも、極めて材料収率に優れ、高純度黒鉛モ−ルドの耐久性も向上し、経済的にも有利な方法を提供し、特に、半導体製造に使用されるシリカガラス治工具類、例えば、反応管のフランジ、エッチング装置の反応室ライナ−、枚葉式装置部品として有用となるシリカガラスを製造する方法を提供することにある。
【０００８】
【課題を解決するための手段】
本発明者らは上記課題を解決するため鋭意検討した結果、黒鉛モ−ルド自身に複数個の貫通孔を設け、シリカ粉末が蒸発溶融しやすくすることにより、集合気泡を除去できることを見出し、本発明に到達した。
【０００９】
すなわち、本発明は、黒鉛質モ−ルドから構成された空間にシリカ粉末を充填し、１７００℃以上に加熱溶融してシリカガラスを得る方法において、黒鉛質モ−ルドとシリカ粉末の接触面、加熱溶融することを特徴とするシリカガラスの製造方法である。
【００１０】
本法では、シリカ粉末として、Ｎａ，Ｋ，Ｆｅの各不純物が１ｐｐｍ以下の高純度結晶質石英、または、高純度非結晶質シリカを用い、モ−ルドとして、Ｎａ，Ｋ，Ｆｅ，Ｔｉの各不純物が１ｐｐｍ以下の黒鉛を用いることにより、集合気泡がなく原料とほぼ同純度の高純度シリカガラスを得ることができる。
【００１１】
以下、本発明をさらに詳細に説明する。
【００１２】
本発明の特徴は、集合気泡の無い透明大型シリカガラスが得られることである。そのためにシリカ粉末の加熱中に発生するガスを外界に逃がすための流路断面積を確実に確保することに留意している。すなわち、一番外側の黒鉛質モールド側面には複数個の貫通孔を設ける必要がある。仕込み形状がリング状の場合には更に中央に配置する黒鉛質モールド外側側面にも同様に複数個の貫通孔を設けることが望ましい。また、この貫通孔は対称的に設けることが望ましい。本発明の検討の結果、貫通孔の総断面積は、仕込み形状の立体の総表面積に対して１％以上にすることが望ましい。また、シリカ粉末が溶融した時、通気用の貫通孔からシリカガラスがにじみ出ないように貫通孔断面が円の場合は、直径３ｍｍ未満にすることが望ましい。次に、黒鉛質モールドとシリカ粉末との間には嵩密度０．１〜１．５ｇ／ｃｍ3 の高純度黒鉛からなる多孔質層を介在させる必要がある。この多孔質層は、モールドとシリカの接触を防ぎ、ガスの排出を促進する。嵩密度０．１〜１．５ｇ／ｃｍ3 の高純度黒鉛からなる多孔質層としては、高純度処理された黒鉛フェルト、黒鉛シ−ト、黒鉛粉末を敷いて堆積させたものなどを用いることができる。
【００１３】
黒鉛フェルトとしては、カ−ボン繊維を成形織物とした、嵩密度０．１〜０．４ｇ／ｃｍ3 で、厚さ２〜１０ｍｍのものを用いることが好ましい。
【００１４】
黒鉛シ−トとしては、カ−ボン繊維を成形織物とした、嵩密度０．８〜１．２ｇ／ｃｍ3 で、厚さ０．３〜１ｍｍのものを用いることが好ましい。
【００１５】
黒鉛粉末としては、粒度０．１〜１ｍｍの高純度処理したものが好ましい。黒鉛フェルト、黒鉛粉末堆積物は、いずれも伸縮性と通気性を有するものであり、モ−ルドの破損を防止すると同時に、発生ガスの逃げ道を与える役割を果たす。黒鉛フェルトは黒鉛シ−トに比較して、伸縮性、通気性とも優れた物であり、上記通気の役割を果たすにはより適している。好適な構成として、粉末充填体の側面あるいは上面に黒鉛フェルトを配置して通気性を確保し、底面には黒鉛シートを敷いてガラス底面の平坦度を出すことが挙げられる。
【００１６】
本発明では、集合気泡が無く、Ｎａ，Ｋ，Ｆｅの各不純物が１ｐｐｍ以下の高純度シリカガラスを得ることができる。そのためには、原料として、Ｎａ，Ｋ，Ｆｅ，の各不純物が１ｐｐｍ以下のシリカ粉末を用いる必要がある。粉末は、結晶質、非結晶質いずれでもよい。結晶質としては、天然の結晶質石英、いわゆる水晶を精製した粉末が最も好適である。また、非結晶質としては、ケイ酸ソ−ダ、ハロゲン化ケイ素、シリコンアルコキサイドなどのケイ素源から合成された、いわゆる合成シリカ粉末を用いることができる。
【００１７】
上記粉末の純度を低下させることなく、本発明のプロセスに従ってシリカガラスとするためには、用いる黒鉛モ−ルド並びに黒鉛多孔質層の純度が極めて重要である。すなわち、モ−ルド並びに多孔質層の黒鉛純度はＮａ，Ｋ，Ｆｅ，Ｔｉの各不純物が１ｐｐｍ以下でなければならず、さらに好ましくは０．５ｐｐｍ以下がよい。
【００１８】
特に、一般の黒鉛材には不純物としてＦｅが１０ｐｐｍ以上含まれる場合があり、高純度処理をしたものを用いるのが望ましい。
【００１９】
シリカ粉末を加熱溶融してシリカガラスとする方法は、特に限定されないが、透明性のよいガラスを得る場合、雰囲気を真空あるいはヘリウムなどの軽元素ガスとし、１８００〜１８５０℃の温度に保持させるのがよい。
【００２０】
以下実施例によって、本発明を更に説明するが、本発明は実施例に限定されるものではない。
【００２１】
【実施例】
実施例１
シリカガラスリングの製造実験に用いた黒鉛モ−ルド／黒鉛多孔質層／シリカ粉末の構成を図１に示す。その仕込み形状は外径φ５３０ｍｍ、内径φ４４０ｍｍ、高さ２００ｍｍとした。外側るつぼ側面と中央るつぼ側面にφ３ｍｍの孔を対称的に同数穿孔し、粉体が成す立体の全表面積に対して通気孔の全断面積を１．３％になるようにした。モ−ルドの内側面および外側面に厚さ５ｍｍ、嵩密度０. ２ｇ／ｃｍ3 の高純度黒鉛フェルトを装着し、高純度結晶質石英粉末（平均粒径０．２ｍｍ）を充填した。粉末上面に同様のフェルトを被せた。更にその上に高純度黒鉛のシートを敷き、高純度黒鉛荷重リング（高さ１００ｍｍ，１２ｋｇ）を載せ、粉末上面に１７ｇ／ｃｍ2 の圧力を加えた。モ−ルド底面には厚さ０．４ｍｍ，嵩密度１．０ｇ／ｃｍ3 の高純度黒鉛シ−トを敷いた。この試料をカ−ボン抵抗加熱電気炉に入れ、真空に排気した状態で、室温から１７００℃まで５℃／分で昇温し、１７００℃で３時間保持した後、５℃／分で昇温し、１８５０℃で４０分間保持した後、真空解除し、窒素を導入し、放冷した。この時得られたシリカガラスには筋状集合気泡が全く無かった。
【００２２】
比較例１
図１に示す構成でるつぼ、粉末を用意した。この時、外側るつぼ側面及び中央るつぼ側面にはいずれも通気孔を設けなかった。実施例１と同様の焼成条件で水晶粉末の真空溶融を行った。この時得られたシリカガラスには筋状集合気泡が存在した。
【００２３】
実施例２
図２に示す構成でるつぼ、粉末を用意した。ここで、実施例１と比較して、外側るつぼと高純度黒鉛外周リングは共通である。焼成するシリカガラスリング幅を更に広いものとするため、中央るつぼの形状を小さくした。実施例１の場合と同様に外側るつぼ側面と中央るつぼ側面に１．３％の通気孔を設けた。水晶粉末の仕込み形状は外径φ５２０ｍｍ、内径φ３４０ｍｍ、高さ２００ｍｍとした。側面の高純度フェルトは２重にした。また、底面の高純度黒鉛シートも２重にした。高純度黒鉛荷重は厚み５０ｍｍ、重量１０．１ｋｇで粉体上面への圧力が８ｇ／ｃｍ2 かかるようにした。焼成条件は１７００℃の保持を１０時間とした。昇温速度は５℃／分、最高温度は１８５０℃で４０分は実施例１と同じである。この時得られたシリカガラスには筋状集合気泡が全く無かった。
【００２４】
比較例２
図２に示す構成でるつぼ、粉末を用意した。この時、外側るつぼ側面及び中央るつぼ側面にはいずれも通気孔を設けなかった。実施例２と同様の焼成条件で水晶粉末の真空溶融を行った。この時得られたシリカガラスには筋状集合気泡が存在した。
【００２５】
実施例３
円柱状のシリカガラスの製造実験に用いた黒鉛モ−ルド／黒鉛多孔質層／シリカ粉末の構成を図３に示す。仕込み形状はφ１５０ｍｍ×高さ２００ｍｍとした。蓋、側面外筒、底面板を分離型とした。荷重用円柱は搭載せず、通気孔としては側面外筒及び蓋に２．４％確保した。焼成条件は昇温速度は５℃／分、１７００℃の保持を１０時間、最高温度は１８５０℃で４０分とした。この時得られたシリカガラスには筋状集合気泡が全く無かった。
【００２６】
比較例３
図３に示す構成でるつぼ、粉末を用意した。この時、外側るつぼ側面には通気孔を設けなかった。実施例３と同様の焼成条件で水晶粉末の真空溶融を行った。この時得られたシリカガラスには筋状集合気泡が存在した。
【００２７】
実施例１〜３及び比較例１〜３で得られた結果を、まとめて以下の表１に示す。
【００２８】
【表１】
【発明の効果】
本発明から製造されるシリカガラスは集合気泡が無く、高純度である。従来、行われていたシリカガラスブロックから機械加工する方法に比較すると、極めて材料収率に優れる。高純度黒鉛モ−ルドの耐久性も向上し、経済的にも有利な方法となる。特に、半導体製造に使用されるシリカガラス治工具類、例えば、反応管のフランジ、エッチング装置の反応室ライナ−、枚葉式装置部品として有用となる。
【図面の簡単な説明】
【図１】実施例１で使用した黒鉛モールド、黒鉛多孔質層、シリカ粉末の断面構造を示す。
【符号の説明】
▲１▼：高純度黒鉛モールド
▲２▼：高純度黒鉛荷重
▲３▼：シリカ原料粉末
▲４▼：高純度黒鉛フェルト
▲５▼：高純度黒鉛シート
▲６▼：高純度黒鉛外周リング
▲７▼：通気孔
【図２】実施例２で使用した黒鉛モールド、黒鉛多孔質層、シリカ粉末の断面構造を示す。
【符号の説明】
▲１▼：高純度黒鉛モールド
▲２▼：高純度黒鉛荷重
▲３▼：シリカ原料粉末
▲４▼：高純度黒鉛フェルト
▲５▼：高純度黒鉛シート
▲６▼：高純度黒鉛外周リング
▲７▼：通気孔
【図３】実施例３で使用した黒鉛モールド、黒鉛多孔質層、シリカ粉末の断面構造を示す。
【符号の説明】
▲１▼：高純度黒鉛モールド
▲３▼：シリカ原料粉末
▲４▼：高純度黒鉛フェルト
▲５▼：高純度黒鉛シート
▲７▼：通気孔[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a molded body made of high-purity silica glass, in particular, a method for producing a large cylinder or large ring. This silica glass member can be applied to heat-resistant jigs for semiconductors, various flanges, furnace core tube parts, and the like.
[0002]
[Prior art]
Japanese Patent Publication No. 35-791 has already described a method for producing silica glass by filling crystalline quartz powder in a space composed of a refractory metal and heating and melting it to 1700 ° C. or higher. Recently, Japanese Patent Laid-Open Nos. 9-202631, 9-202632, and 9-183623 disclose that silica glass is produced by interposing silica glass on the contact surface between a graphite material container and silica powder, and heating and melting the glass. A method is disclosed.
[0003]
[Problems to be solved by the invention]
In Japanese Examined Patent Publication No. 35-791, Mo, which is a refractory metal, is used as a mold, but this method has a problem that Mo undergoes high-temperature oxidation and enters into the resulting silica glass as a gas and contaminates it. It was.
[0004]
In addition, when a graphite material is used as a mold, even if the mold and silica glass are fused and damaged due to a high temperature reaction between C and SiO 2 , the mold can be avoided. There were problems such as extremely low durability.
[0005]
Furthermore, general graphite materials contain Fe, Ca, and the like far exceeding 1 ppm, and there is a problem that these impurities gasify at a high temperature and penetrate into the glass, so that high purity cannot be maintained.
[0006]
Japanese Patent Application Laid-Open Nos. 9-202631, 9-202632, and 9-183623 disclose methods for solving the above problems by interposing silica glass between a graphite mold and silica powder. However, this method requires time and effort for processing and manufacturing the silica glass to be interposed, and the silica glass is expensive, so it is difficult to say that it is an economical method. In addition, these methods can be applied to a medium-sized member having an 8-inch wafer processing size, but cannot be applied to a large-sized flange member having a size of 12 inches or more. That is, there is a problem that the aggregated bubbles in the silica glass cannot be removed only by extending the melting and heating time.
[0007]
An object of the present invention is to provide a silica glass including a ring which has no aggregate bubbles, has high purity, and can have a large size of an outer diameter of 300 to 550 mm and a height of about 200 mm. Compared to the conventional method of machining from a silica glass block, the material yield is extremely superior, the durability of the high purity graphite mold is improved, and an economically advantageous method is provided. It is an object of the present invention to provide a method for producing silica glass which is useful as a silica glass jig and tool to be used, for example, a flange of a reaction tube, a reaction chamber liner of an etching apparatus, and a single wafer apparatus part.
[0008]
[Means for Solving the Problems]
As a result of intensive studies to solve the above problems, the present inventors have found that the aggregated bubbles can be removed by providing a plurality of through holes in the graphite mold itself and facilitating evaporation and melting of the silica powder. The invention has been reached.
[0009]
That is, the present invention is a method of filling silica powder in a space composed of a graphite mold and heating and melting to 1700 ° C. or higher to obtain silica glass. In the method of obtaining contact between the graphite mold and the silica powder, It is a method for producing silica glass, characterized by heating and melting.
[0010]
In this method, high-purity crystalline quartz or high-purity amorphous silica containing 1 ppm or less of each impurity of Na, K, and Fe is used as silica powder, and Na, K, Fe, and Ti are used as molds. By using graphite having 1 ppm or less of each impurity, it is possible to obtain a high purity silica glass having no bubbles and almost the same purity as the raw material.
[0011]
Hereinafter, the present invention will be described in more detail.
[0012]
A feature of the present invention is that a transparent large silica glass free from aggregated bubbles is obtained. Therefore, it is noted that the flow path cross-sectional area for allowing the gas generated during the heating of the silica powder to escape to the outside is ensured. That is, it is necessary to provide a plurality of through holes on the side surface of the outermost graphite mold. When the charged shape is a ring shape, it is desirable to provide a plurality of through holes in the same manner on the outer side surface of the graphite mold disposed at the center. Further, it is desirable to provide the through holes symmetrically. As a result of the study of the present invention, it is desirable that the total cross-sectional area of the through-hole is 1% or more with respect to the total surface area of the charged solid. In addition, when the silica powder is melted, the diameter of the through-hole cross section is preferably less than 3 mm so that the silica glass does not ooze out from the through-hole for ventilation. Next, it is necessary to interpose a porous layer made of high-purity graphite having a bulk density of 0.1 to 1.5 g / cm 3 between the graphite mold and the silica powder. This porous layer prevents contact between the mold and the silica and promotes gas discharge. As a porous layer made of high-purity graphite having a bulk density of 0.1 to 1.5 g / cm 3 , a high-purity-treated graphite felt, a graphite sheet, or a material deposited with graphite powder is used. Can do.
[0013]
As the graphite felt, it is preferable to use a carbon fiber having a bulk density of 0.1 to 0.4 g / cm 3 and a thickness of 2 to 10 mm.
[0014]
As the graphite sheet, it is preferable to use a carbon fiber made of carbon fiber having a bulk density of 0.8 to 1.2 g / cm 3 and a thickness of 0.3 to 1 mm.
[0015]
As the graphite powder, a high-purity treated particle having a particle size of 0.1 to 1 mm is preferable. Both the graphite felt and the graphite powder deposit have stretchability and air permeability, and prevent the mold from being damaged, and at the same time provide a escape path for the generated gas. Graphite felt is superior in both stretchability and air permeability as compared with graphite sheet, and is more suitable for the above-mentioned role of ventilation. As a preferred configuration, a graphite felt is disposed on the side surface or top surface of the powder filler to ensure air permeability, and a graphite sheet is laid on the bottom surface to increase the flatness of the glass bottom surface.
[0016]
In the present invention, it is possible to obtain a high-purity silica glass having no aggregated bubbles and containing 1 ppm or less of Na, K, and Fe impurities. For this purpose, it is necessary to use silica powder having Na, K and Fe impurities of 1 ppm or less as raw materials. The powder may be either crystalline or amorphous. As the crystalline material, natural crystalline quartz, that is, a powder obtained by purifying so-called quartz is most preferable. As the amorphous material, so-called synthetic silica powder synthesized from a silicon source such as soda silicate, silicon halide, silicon alkoxide, or the like can be used.
[0017]
In order to obtain silica glass in accordance with the process of the present invention without reducing the purity of the powder, the purity of the graphite mold used and the graphite porous layer is extremely important. That is, the graphite purity of the mold and the porous layer must be 1 ppm or less for Na, K, Fe, and Ti impurities, and more preferably 0.5 ppm or less.
[0018]
Particularly, a general graphite material may contain 10 ppm or more of Fe as an impurity, and it is desirable to use a material that has been subjected to a high purity treatment.
[0019]
The method of heating and melting the silica powder to form silica glass is not particularly limited. However, when obtaining a glass with good transparency, the atmosphere is a light element gas such as vacuum or helium, and the temperature is maintained at 1800 to 1850 ° C. Is good.
[0020]
EXAMPLES Hereinafter, the present invention will be further described with reference to examples, but the present invention is not limited to the examples.
[0021]
【Example】
Example 1
The structure of the graphite mold / graphite porous layer / silica powder used in the production experiment of the silica glass ring is shown in FIG. The charged shape was an outer diameter of 530 mm, an inner diameter of 440 mm, and a height of 200 mm. The same number of holes of 3 mm in diameter were drilled symmetrically on the outer crucible side surface and the central crucible side surface so that the total cross-sectional area of the vent hole was 1.3% with respect to the total surface area of the solid formed by the powder. A high-purity graphite felt having a thickness of 5 mm and a bulk density of 0.2 g / cm 3 was attached to the inner and outer surfaces of the mold and filled with high-purity crystalline quartz powder (average particle size 0.2 mm). A similar felt was placed on the upper surface of the powder. Further, a high purity graphite sheet was laid thereon, a high purity graphite load ring (height 100 mm, 12 kg) was placed thereon, and a pressure of 17 g / cm 2 was applied to the upper surface of the powder. A high purity graphite sheet having a thickness of 0.4 mm and a bulk density of 1.0 g / cm 3 was laid on the bottom of the mold. The sample was placed in a carbon resistance heating electric furnace and evacuated to a vacuum, the temperature was raised from room temperature to 1700 ° C. at 5 ° C./minute, held at 1700 ° C. for 3 hours, and then heated at 5 ° C./minute. After holding at 1850 ° C. for 40 minutes, the vacuum was released, nitrogen was introduced, and the mixture was allowed to cool. The silica glass obtained at this time had no streak-like air bubbles.
[0022]
Comparative Example 1
A crucible and powder were prepared in the configuration shown in FIG. At this time, neither the outer crucible side surface nor the central crucible side surface was provided with a vent hole. The crystal powder was vacuum-melted under the same firing conditions as in Example 1. In the silica glass obtained at this time, streak-like air bubbles were present.
[0023]
Example 2
A crucible and powder were prepared in the configuration shown in FIG. Here, compared with Example 1, the outer crucible and the high purity graphite outer peripheral ring are common. In order to make the silica glass ring to be fired wider, the shape of the central crucible was reduced. As in the case of Example 1, 1.3% vent holes were provided on the outer crucible side surface and the central crucible side surface. The crystal powder was charged in an outer diameter of 520 mm, an inner diameter of 340 mm, and a height of 200 mm. The high purity felt on the side was doubled. Also, the high-purity graphite sheet on the bottom was doubled. The high-purity graphite load was 50 mm in thickness and 10.1 kg in weight, and the pressure on the upper surface of the powder was 8 g / cm 2 . The firing condition was set at 1700 ° C. for 10 hours. The heating rate was 5 ° C./min, the maximum temperature was 1850 ° C., and 40 minutes was the same as in Example 1. The silica glass obtained at this time had no streak-like air bubbles.
[0024]
Comparative Example 2
A crucible and powder were prepared in the configuration shown in FIG. At this time, neither the outer crucible side surface nor the central crucible side surface was provided with a vent hole. The crystal powder was vacuum-melted under the same firing conditions as in Example 2. In the silica glass obtained at this time, streak-like air bubbles were present.
[0025]
Example 3
FIG. 3 shows the structure of graphite mold / graphite porous layer / silica powder used in the production experiment of cylindrical silica glass. The charged shape was φ150 mm × height 200 mm. The lid, side outer cylinder, and bottom plate were separated. The loading cylinder was not mounted, and 2.4% was secured as a ventilation hole in the side outer cylinder and the lid. The firing conditions were a temperature rising rate of 5 ° C./min, a holding at 1700 ° C. for 10 hours, and a maximum temperature of 1850 ° C. for 40 minutes. The silica glass obtained at this time had no streak-like air bubbles.
[0026]
Comparative Example 3
A crucible and powder were prepared in the configuration shown in FIG. At this time, no vent hole was provided on the side surface of the outer crucible. The quartz powder was vacuum melted under the same firing conditions as in Example 3. In the silica glass obtained at this time, streak-like air bubbles were present.
[0027]
The results obtained in Examples 1 to 3 and Comparative Examples 1 to 3 are collectively shown in Table 1 below.
[0028]
[Table 1]
【The invention's effect】
The silica glass produced from the present invention has no aggregated bubbles and is highly pure. Compared to the conventional method of machining from a silica glass block, the material yield is extremely excellent. The durability of the high purity graphite mold is also improved, and this is an economically advantageous method. In particular, it is useful as a silica glass tool used in semiconductor manufacturing, for example, a flange of a reaction tube, a reaction chamber liner of an etching apparatus, and a single wafer type apparatus part.
[Brief description of the drawings]
1 shows a cross-sectional structure of a graphite mold, a graphite porous layer, and silica powder used in Example 1. FIG.
[Explanation of symbols]
(1): High purity graphite mold (2): High purity graphite load (3): Silica raw material powder (4): High purity graphite felt (5): High purity graphite sheet (6): High purity graphite outer ring (7) ▼: Ventilation hole FIG. 2 shows a cross-sectional structure of the graphite mold, graphite porous layer, and silica powder used in Example 2.
[Explanation of symbols]
(1): High purity graphite mold (2): High purity graphite load (3): Silica raw material powder (4): High purity graphite felt (5): High purity graphite sheet (6): High purity graphite outer ring (7) ▼: Ventilation hole FIG. 3 shows a cross-sectional structure of the graphite mold, graphite porous layer, and silica powder used in Example 3.
[Explanation of symbols]
(1): High purity graphite mold (3): Silica raw material powder (4): High purity graphite felt (5): High purity graphite sheet (7): Vent
Claims (4)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08344798A JP4014724B2 (en) | 1998-03-30 | 1998-03-30 | Method for producing silica glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP08344798A JP4014724B2 (en) | 1998-03-30 | 1998-03-30 | Method for producing silica glass |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH11278857A JPH11278857A (en) | 1999-10-12 |
| JP4014724B2 true JP4014724B2 (en) | 2007-11-28 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP08344798A Expired - Fee Related JP4014724B2 (en) | 1998-03-30 | 1998-03-30 | Method for producing silica glass |
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| Country | Link |
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| JP (1) | JP4014724B2 (en) |
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| US10618833B2 (en) | 2015-12-18 | 2020-04-14 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a synthetic quartz glass grain |
| US10676388B2 (en) | 2015-12-18 | 2020-06-09 | Heraeus Quarzglas Gmbh & Co. Kg | Glass fibers and pre-forms made of homogeneous quartz glass |
| US10730780B2 (en) | 2015-12-18 | 2020-08-04 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
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| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
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| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
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| US10618833B2 (en) | 2015-12-18 | 2020-04-14 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a synthetic quartz glass grain |
| US10676388B2 (en) | 2015-12-18 | 2020-06-09 | Heraeus Quarzglas Gmbh & Co. Kg | Glass fibers and pre-forms made of homogeneous quartz glass |
| US10730780B2 (en) | 2015-12-18 | 2020-08-04 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a multi-chamber oven |
| US11053152B2 (en) | 2015-12-18 | 2021-07-06 | Heraeus Quarzglas Gmbh & Co. Kg | Spray granulation of silicon dioxide in the preparation of quartz glass |
| US11236002B2 (en) | 2015-12-18 | 2022-02-01 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of an opaque quartz glass body |
| US11299417B2 (en) | 2015-12-18 | 2022-04-12 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of a quartz glass body in a melting crucible of refractory metal |
| US11339076B2 (en) | 2015-12-18 | 2022-05-24 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of carbon-doped silicon dioxide granulate as an intermediate in the preparation of quartz glass |
| US11492285B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies from silicon dioxide granulate |
| US11492282B2 (en) | 2015-12-18 | 2022-11-08 | Heraeus Quarzglas Gmbh & Co. Kg | Preparation of quartz glass bodies with dew point monitoring in the melting oven |
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| JPH11278857A (en) | 1999-10-12 |
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