JP3591540B2 - Synthetic quartz glass manufacturing equipment - Google Patents
Synthetic quartz glass manufacturing equipment Download PDFInfo
- Publication number
- JP3591540B2 JP3591540B2 JP23739794A JP23739794A JP3591540B2 JP 3591540 B2 JP3591540 B2 JP 3591540B2 JP 23739794 A JP23739794 A JP 23739794A JP 23739794 A JP23739794 A JP 23739794A JP 3591540 B2 JP3591540 B2 JP 3591540B2
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- synthetic quartz
- exhaust
- target
- furnace frame
- 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
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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
- C03B19/14—Other methods of shaping glass by gas- or vapour- phase reaction processes
- C03B19/1446—Means for after-treatment or catching of worked reactant gases
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
Description
【0001】
【産業上の利用分野】
本発明は合成石英ガラスの製造装置、特に合成石英ガラス製造装置の炉枠あるいは排気手段にシリカ微粒子等が付着するのを防止し、紫外線リソグラフィー用光学素子として使用可能な合成石英ガラス光学部材を製造する製造装置に関する。
【0002】
【従来の技術】
近年、紫外線リソグラフィー用光学素子としての合成石英ガラスには、紫外域での高透過率を達成するために、高純度な合成石英ガラスが用いられる。その有用な製法の一つとして火炎加水分解法が知られている。
火炎加水分解法は、合成石英ガラスの原料となるケイ素化合物を石英ガラス合成用のバーナーから酸水素火炎内へ供給し、加水分解反応させシリカ微粒子を合成、堆積させると同時に溶融ガラス化する合成方法である。
【0003】
従来、この火炎加水分解法によりターゲットを鉛直軸を中心に回転させながらこの上にシリカ微粒子を堆積させ、堆積速度に合わせ石英ガラス合成用のバーナーから合成面の距離を一定に保つよう引き下げながら合成石英ガラスの製造を行ってきた。
その石英ガラス製造装置の炉枠及び排気手段は、これらの装置を作製する上で、切断、加工により容易に形状が得られる金属が用いられていた。
【0004】
【発明が解決しようとする課題】
しかしながら、上記のような金属を使用した製造装置の場合、炉枠及び排気ガス内が酸性の雰囲気となるためため、腐食が生じ、合成を継続することが不可能となる問題があった。また、炉枠に関しては、特に合成された石英ガラス内に不純物を混入させる恐れがあった。さらに、炉枠及び排気手段は、700℃程度の高温にさらされるため、金属の変形により合成を継続することが不可能となる問題もあった。
【0005】
これらを防止する上でも、炉枠及び排気手段内に金属部分を露出させることは、石英ガラスの合成を続けるにあたりマイナスであることがわかった。
【0006】
【課題を解決するための手段】
上記問題点を顧みて、酸性雰囲気及び高温にさらされる金属部分において、鋭意研究を行った結果、これらの酸性雰囲気及び高温にさらされる部分に、耐熱性があり、腐食性ガスに侵されないライニングを施すことを見い出し、問題点の解決を図った。
【0007】
そこで、炉枠と耐火物とからなる炉と、該炉内部に設置されたインゴット形成用のターゲットと、該ターゲットに先端を向けて設置された石英ガラス合成用のバーナーと、前記ターゲット上に堆積されなかったシリカ微粒子を排気する排気手段とからなる合成石英ガラス製造装置に於いて、炉枠の腐食を防止する手段を設けたことを特徴とする合成石英ガラス製造装置(請求項1)を提供する。
【0008】
同様に、排気手段に於ける金属部分の腐食を防止する手段を設けたことを特徴とする合成石英ガラス製造装置(請求項2)を提供する。
【0009】
【作用】
開放系の合成石英ガラスの製造装置において、耐火物までの炉内温度は1500℃程度で合成面温度は1900℃を越える。このインゴット形成用のターゲットに堆積されなかったシリカ微粒子及び加水分解反応により発生したガス(以下排気ガスとする)は、排気管を通じて除害装置まで排気ガスとして運ばれる(排気手段)。この時、炉枠及び排気手段の内面温度は場所により異なるが、700℃程度にまで達する。排気ガスは、酸性のHCl等を含むため、炉枠及び排気手段内に腐食性のガスが充満する。
【0010】
本発明の製造装置は、炉枠及び排気手段に、腐食に強く耐熱性の高い材料、すなわちガラス、セラミックを金属へのライニング材として用いる。または、カーボン材料を用いる。
また、排気ガスは排気手段を通過するにしたがい、その温度が低下し、熱対策を施こす必要がない80℃以下の低温となる。あるいは、排気経路内部もしくは外部の散水、または排気経路を2重構造とし、その間を水冷する等の方法により、排気経路の温度を低下させる。この低温部分には、加工性、耐食性に優れ、コスト削減できる塩化ビニールを使用する。また、内部を観察する必要がある部分では、透明性のあるポリカーボネート、アクリルまたは透明塩化ビニールを使用する。シール材やガスケットとしては耐食性、耐熱性に優れ弾力性があるテフロン系樹脂を使用する。
【0011】
ガラスをライニング材とする場合、パイレックスガラスが主に使用されるが、金属との親和性、及び耐熱性が高ければ他のガラスであっても使用可能である。また、仮に金属との親和性が低い場合であっても、多層構造のライニングを施すことにより、例えば石英ガラスの非常に優れた耐熱性及び耐酸性、小さい熱膨張率、熱衝撃に強い炉枠あるいは排気手段を得ることができる。しかし、実際はコスト面において最もバランスの取れているのが、パイレックスガラスであるため、これが用いられている。
【0012】
セラミックスのライニング材としては、リン酸アンモニウム、酸化マグネシウム及び結晶質シリカを含有する水和硬化組成物等が挙げられる。セラミックスによるライニングは、耐熱性の向上に対する効果が大きい。また、アルミナ、アルミナーシリカ系のセラミックファイバーをライニング材として用いた場合には、断熱性を向上させることができる。
【0013】
カーボンは、他の材料に比べ、耐熱性の面で劣るが、加工性が優れている。従って、本発明により金属での構成では不可能であった、製造装置の補修なしに連続的に合成石英ガラスの製造を行うことが可能となる。
また、シリカ微粒子はHClを含む排気ガスの内で金属の炉枠及び排気手段に付着し、腐食により穴などが開く問題点を引き起こすばかりではなく、錆を発生させ、摩擦係数を高くすることでさらにシリカ微粒子の付着し安い面を形成していた。
【0014】
この様に、シリカ微粒子が付着し排気経路が狭くなると、排気流量の制御が困難となる。この現象が発生したとき、炉内からの排気量に変動を与えるため、インゴットの成長方向に垂直な方向の屈折率勾配が高均質で、かつ半径方向の屈折率分布についても安定した合成石英ガラスを得ること、すなわちインゴット内での屈折率のばらつきを少なくすることは困難であったが、本発明により、腐食性に優れたガラスあるいはセラミックライニング、カーボン材を使用することで、これらのシリカ微粒子を付着が防止でき、品質に影響を与えることなく石英ガラスの合成を行うことができる。
【0015】
【実施例】
〔比較例1〕
合成石英ガラス製造装置として、鋳物の炉床板の上に金属製の炉枠を置き、その中に排気口を設けた。この耐火物の内容量は126lで下部は炉床板及び耐火物共に開放型である。この様な装置を用いて、原料として使用されるケイ素化合物を60〜100℃の範囲で昇温し気化させ、石英ガラス用のバーナーの中心から酸水素炎と共に火炎加水分解させることによりターゲットに吹き付け、シリカ微粒子を合成、堆積させ、ターゲットに堆積されなかったシリカ微粒子等の排気ガスは、排気口を受けた排気管を通じて除害装置へと導かれる。排気ガスの影響により、この時炉枠及び排気管には錆が生じ、通常の合成では排気管に10日程で穴が開き、合成を継続することが不可能となった。また、炉枠の耐久試験を行った場合は、約30日程で穴が開き合成の継続が不可能となることがわかった。さらに、除害装置のフランジ部分の固定用ボルトにステンレス製のボルトを使用していたが、30日程で錆が生じボルトの交換が必要となり、またフランジの開閉が非常に困難になった。
〔実施例1〕
比較例1の合成石英ガラス製造装置において、炉枠内側にセラミックライニングを施し、排気管にグラスライニング管を使用し、また除害処理装置のフランジ部分のボルトに、アクリルを使用し同様の合成を行った(図1)。
【0016】
そうしたところ、連続で30日の合成を行っても炉枠及び排気管に穴を生じることはなく、ステンレス製のボルトとは対照的に全く錆を生じないため、製造装置の継続運転が可能であった。また、ボルトの交換はほぼ不要となった。
本実施例により、炉枠及び排気手段にガラス、セラミックのライニングを施し耐久試験を行った際、穴の開く例はなく非常に耐腐食性に優れた炉枠及び排気手段であることが確認された。また、炉枠及び排気管に穴が開くことがなくなったため、排気ガスが大気へ放出されることなく安全性が非常に高くなった。
【0017】
また、排気ガスが低温となる除害装置のフランジ部分には塩化ビニール及びポリカーボネートを使用した場合にも同様の効果が得られることが確認された。
本発明の効果は実施例に限ったことではない。
【0018】
【発明の効果】
以上の様に、本発明に従う合成石英ガラス製造装置に伴う炉枠及び排気手段に、上記した様な腐食を防止する手段を施すことにより、製造装置の耐久性が上がり、各部品の交換がほとんどなくなったため、大幅なコスト削減になった。さらに、本発明は排気手段にシリカ微粒子が付着することを防ぐことができるため、高品質の合成石英ガラスが得られる。
【図面の簡単な説明】
【図1】実施例1で用いた合成石英ガラス製造装置の模式図である。
【符号の説明】
1 バーナー
2 ターゲット
3 インゴット
4 炉床
5 セラミックスライニングを施した炉枠
6 耐火物
7 除害装置
8 排気ファン
9 フランジ
10 グラスライニング管[0001]
[Industrial applications]
The present invention manufactures a synthetic quartz glass optical member that can be used as an optical element for ultraviolet lithography by preventing silica fine particles and the like from adhering to a synthetic quartz glass manufacturing apparatus, particularly a furnace frame or an exhaust means of the synthetic quartz glass manufacturing apparatus. To a manufacturing apparatus.
[0002]
[Prior art]
In recent years, high purity synthetic quartz glass has been used for synthetic quartz glass as an optical element for ultraviolet lithography in order to achieve high transmittance in the ultraviolet region. The flame hydrolysis method is known as one of the useful production methods.
The flame hydrolysis method is a synthesis method in which a silicon compound, which is a raw material of synthetic quartz glass , is supplied from a burner for synthesizing quartz glass into an oxyhydrogen flame, and a hydrolysis reaction is performed to synthesize and deposit silica fine particles. It is.
[0003]
Conventionally, by this flame hydrolysis method, silica particles are deposited on the target while rotating the target about the vertical axis, and synthesized while lowering the distance of the synthetic surface from the burner for synthesizing quartz glass according to the deposition rate We have been manufacturing quartz glass.
For the furnace frame and the exhaust means of the quartz glass manufacturing apparatus, a metal whose shape can be easily obtained by cutting and processing in producing these apparatuses has been used.
[0004]
[Problems to be solved by the invention]
However, in the case of the manufacturing apparatus using the above-mentioned metal, since the furnace frame and the exhaust gas have an acidic atmosphere, there is a problem that corrosion occurs and it becomes impossible to continue the synthesis. Further, regarding the furnace frame, there is a possibility that impurities may be mixed into the synthesized quartz glass. Furthermore, since the furnace frame and the exhaust means are exposed to a high temperature of about 700 ° C., there has been a problem that the synthesis cannot be continued due to deformation of the metal.
[0005]
In order to prevent these problems, it has been found that exposing the metal part in the furnace frame and the exhaust means is a negative factor in continuing the synthesis of quartz glass.
[0006]
[Means for Solving the Problems]
In light of the above problems, as a result of intensive research on metal parts exposed to an acidic atmosphere and high temperatures, the parts exposed to these acidic atmospheres and high temperatures have a heat-resistant lining that is not attacked by corrosive gas. I found out how to apply it and tried to solve the problem.
[0007]
Therefore, a furnace composed of a furnace frame and a refractory, a target for forming an ingot installed inside the furnace, a burner for synthesizing quartz glass installed with its tip directed toward the target, and a stack on the target An apparatus for producing synthetic quartz glass, comprising means for preventing corrosion of a furnace frame in an apparatus for producing synthetic quartz glass comprising exhaust means for exhausting silica particles which have not been removed (claim 1). Do.
[0008]
Similarly, there is provided a synthetic quartz glass manufacturing apparatus (claim 2) characterized in that a means for preventing corrosion of a metal portion in an exhaust means is provided.
[0009]
[Action]
In an open type synthetic quartz glass manufacturing apparatus, the furnace temperature up to a refractory is about 1500 ° C. and the synthetic surface temperature exceeds 1900 ° C. Silica fine particles not deposited on the target for forming the ingot and gas generated by the hydrolysis reaction (hereinafter, referred to as exhaust gas) are carried as exhaust gas to the abatement apparatus through an exhaust pipe (exhaust means). At this time, the inner surface temperature of the furnace frame and the evacuation means varies depending on the location, but reaches about 700 ° C. Since the exhaust gas contains acidic HCl or the like, the furnace frame and the exhaust means are filled with corrosive gas.
[0010]
The manufacturing apparatus of the present invention uses a material that is resistant to corrosion and has high heat resistance, that is, glass or ceramic, as a lining material for metal, for the furnace frame and the exhaust means. Alternatively, a carbon material is used.
Further, as the exhaust gas passes through the exhaust means, its temperature decreases, and becomes a low temperature of 80 ° C. or less where it is not necessary to take any thermal measures. Alternatively, the temperature of the exhaust path is lowered by water spraying inside or outside the exhaust path, or by forming the exhaust path in a double structure and cooling the space between the two. For this low temperature part, vinyl chloride which is excellent in workability and corrosion resistance and can reduce the cost is used. Also, in areas where the inside needs to be observed, use transparent polycarbonate, acrylic or transparent vinyl chloride. A Teflon-based resin having excellent corrosion resistance and heat resistance and elasticity is used as the sealing material and gasket.
[0011]
When glass is used as the lining material, Pyrex glass is mainly used, but other glasses can be used as long as they have high affinity for metal and high heat resistance. Also, even if the affinity with metal is low, by applying a multilayer structure lining, for example, a furnace frame that is highly resistant to heat and acid, a small coefficient of thermal expansion, and thermal shock of quartz glass. Alternatively, exhaust means can be obtained. However, since Pyrex glass is actually the most balanced in terms of cost, it is used.
[0012]
Examples of the ceramic lining material include a hydrated hardening composition containing ammonium phosphate, magnesium oxide and crystalline silica. Lining with ceramics has a great effect on improving heat resistance. When alumina or alumina-silica ceramic fiber is used as the lining material, the heat insulating property can be improved.
[0013]
Carbon is inferior in heat resistance as compared with other materials, but is excellent in workability. Therefore, according to the present invention, it is possible to continuously produce synthetic quartz glass without repairing the production apparatus , which is not possible with a metal configuration.
In addition, the silica fine particles adhere to the metal furnace frame and the exhaust means in the exhaust gas containing HCl, causing not only a problem that a hole or the like is opened due to corrosion, but also rust and a high friction coefficient. Further, the silica fine particles adhered to the surface to form a cheap surface.
[0014]
As described above, when the silica fine particles adhere and the exhaust path narrows, it becomes difficult to control the exhaust flow rate. When this phenomenon occurs, synthetic quartz glass with a highly uniform refractive index gradient in the direction perpendicular to the growth direction of the ingot and a stable refractive index distribution in the radial direction is used to vary the displacement from the furnace. Although it was difficult to obtain, that is, to reduce the variation of the refractive index in the ingot, according to the present invention, by using a glass or ceramic lining, carbon material excellent in corrosive, these silica fine particles Can be prevented, and quartz glass can be synthesized without affecting the quality.
[0015]
【Example】
[Comparative Example 1]
As a synthetic quartz glass manufacturing apparatus, a metal furnace frame was placed on a cast hearth plate, and an exhaust port was provided therein. The refractory has an inner volume of 126 l, and the lower part is open type for both the hearth plate and the refractory. Using such an apparatus, a silicon compound used as a raw material is heated and vaporized in the range of 60 to 100 ° C., and is flame-hydrolyzed from the center of a quartz glass burner together with an oxyhydrogen flame and sprayed onto a target. Then, the silica fine particles are synthesized and deposited, and the exhaust gas such as the silica fine particles not deposited on the target is guided to the abatement apparatus through the exhaust pipe which receives the exhaust port. At this time, the furnace frame and the exhaust pipe were rusted due to the influence of the exhaust gas, and a hole was formed in the exhaust pipe in about 10 days in the ordinary synthesis, so that synthesis could not be continued. In addition, when a durability test was performed on the furnace frame, it was found that a hole was opened in about 30 days and synthesis could not be continued. Further, stainless steel bolts were used as fixing bolts for the flange portion of the abatement apparatus. However, rust occurred in about 30 days, requiring replacement of the bolts, and opening and closing the flanges became very difficult.
[Example 1]
In the synthetic quartz glass manufacturing apparatus of Comparative Example 1, a ceramic lining was provided on the inside of the furnace frame, a glass lining pipe was used for an exhaust pipe, and acrylic was used for bolts of a flange portion of the detoxification apparatus, and the same synthesis was performed. (Figure 1).
[0016]
In such a case, even if the synthesis is performed continuously for 30 days, no holes are formed in the furnace frame and the exhaust pipe, and no rust is generated at all in contrast to the stainless steel bolts, so that the manufacturing apparatus can be continuously operated. there were. Also, the replacement of bolts is almost unnecessary.
According to this example, when the furnace frame and the exhaust means were subjected to glass and ceramic lining and a durability test was performed, it was confirmed that the furnace frame and the exhaust means were extremely excellent in corrosion resistance without any holes. Was. Further, since holes were not formed in the furnace frame and the exhaust pipe, the exhaust gas was not released to the atmosphere, and the safety was extremely enhanced.
[0017]
It was also confirmed that the same effect was obtained when vinyl chloride and polycarbonate were used for the flange portion of the abatement system where the exhaust gas temperature was low.
The effects of the present invention are not limited to the embodiments.
[0018]
【The invention's effect】
As described above, by applying the above-described means for preventing corrosion to the furnace frame and exhaust means associated with the synthetic quartz glass manufacturing apparatus according to the present invention, the durability of the manufacturing apparatus is increased and replacement of each part is almost impossible. This has led to significant cost savings. Further, according to the present invention, it is possible to prevent the silica fine particles from adhering to the exhaust means, so that high-quality synthetic quartz glass can be obtained.
[Brief description of the drawings]
FIG. 1 is a schematic diagram of a synthetic quartz glass manufacturing apparatus used in Example 1.
[Explanation of symbols]
DESCRIPTION OF SYMBOLS 1
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23739794A JP3591540B2 (en) | 1994-09-30 | 1994-09-30 | Synthetic quartz glass manufacturing equipment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP23739794A JP3591540B2 (en) | 1994-09-30 | 1994-09-30 | Synthetic quartz glass manufacturing equipment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH08104527A JPH08104527A (en) | 1996-04-23 |
| JP3591540B2 true JP3591540B2 (en) | 2004-11-24 |
Family
ID=17014792
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP23739794A Expired - Lifetime JP3591540B2 (en) | 1994-09-30 | 1994-09-30 | Synthetic quartz glass manufacturing equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP3591540B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2002045628A (en) * | 2000-08-07 | 2002-02-12 | Shin Etsu Chem Co Ltd | Exhaust gas treatment method and apparatus during production of synthetic quartz |
| EP1441992A1 (en) * | 2001-09-27 | 2004-08-04 | Corning Incorporated | Improved methods and furnaces for fused silica production |
-
1994
- 1994-09-30 JP JP23739794A patent/JP3591540B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH08104527A (en) | 1996-04-23 |
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