JP4455030B2 - Method for producing transparent synthetic quartz glass - Google Patents
Method for producing transparent synthetic quartz glass Download PDFInfo
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- JP4455030B2 JP4455030B2 JP2003403903A JP2003403903A JP4455030B2 JP 4455030 B2 JP4455030 B2 JP 4455030B2 JP 2003403903 A JP2003403903 A JP 2003403903A JP 2003403903 A JP2003403903 A JP 2003403903A JP 4455030 B2 JP4455030 B2 JP 4455030B2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims description 61
- 238000004519 manufacturing process Methods 0.000 title claims description 14
- 239000010453 quartz Substances 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 18
- 238000010304 firing Methods 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 11
- 238000002844 melting Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 6
- 239000002184 metal Substances 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 5
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 claims description 4
- 230000005484 gravity Effects 0.000 claims description 4
- 239000005049 silicon tetrachloride Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- 238000010438 heat treatment Methods 0.000 description 12
- 238000000034 method Methods 0.000 description 12
- 229910052799 carbon Inorganic materials 0.000 description 11
- 230000008018 melting Effects 0.000 description 7
- 239000010419 fine particle Substances 0.000 description 6
- 239000011521 glass Substances 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000005245 sintering Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
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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
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/06—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction
- C03B19/066—Other methods of shaping glass by sintering, e.g. by cold isostatic pressing of powders and subsequent sintering, by hot pressing of powders, by sintering slurries or dispersions not undergoing a liquid phase reaction for the production of quartz or fused silica articles
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B20/00—Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Glass Melting And Manufacturing (AREA)
Description
本発明は、高純度合成石英粉を加熱焼成して得られる透明合成石英ガラスの製造方法及び合成石英ガラス体に関する。 The present invention relates to a method for producing transparent synthetic quartz glass obtained by heating and firing high-purity synthetic quartz powder, and a synthetic quartz glass body.
透明石英ガラスの製造法のひとつとして、石英ガラス粉をカーボン鋳型に詰めて、真空雰囲気中で、加熱溶融する方法が知られている。この方法は、通常、100μm〜500μmの粒度分布をもつ、天然または合成石英ガラス粉を使用して、1600℃以上の温度域に加熱溶融し、石英ガラス塊を製造する(例えば、特許文献1参照。)。製造された石英ガラス塊は、半導体製造工程の部材に使用され、特に近年、金属不純物が低減され高温処理に適した合成石英が素材として望まれている。
上記の方法によって得られる石英ガラス塊は、内部に微小な泡を含有し、使用可能な部分が少なく、高コストであった。また、加熱溶融時に粉を充填するカーボン鋳型と石英粉は高温で非常に反応し易いため、鋳型が激しく消耗し、また、飛散したカーボン粉は石英粉中に入り込み、泡の原因にもなった。一方、合成石英粉からの石英ガラス塊の製造方法は、適正粒度の合成石英粉体を製造する為の手間とコストが極めて大きいという問題があった。 The quartz glass lump obtained by the above method contained minute bubbles inside, had few usable parts, and was expensive. In addition, the carbon mold and quartz powder that fills the powder when heated and melted react very easily at high temperatures, so the mold was consumed violently, and the scattered carbon powder entered the quartz powder and caused bubbles. . On the other hand, the method for producing a quartz glass lump from synthetic quartz powder has a problem that labor and cost for producing a synthetic quartz powder having an appropriate particle size are extremely large.
本発明は、透明で内部に微少泡の無い石英ガラス体を容易且つ低コストに製造する方法、及び透明で内部に微少泡が無い石英ガラス体を提供することを目的とする。 It is an object of the present invention to provide a method for easily and inexpensively producing a quartz glass body that is transparent and has no microbubbles therein, and a quartz glass body that is transparent and has no microbubbles therein.
上記問題を解決するため、本発明者らは鋭意開発を行い、本発明を完成させた。即ち、本発明の透明合成石英ガラスの製造方法は、BET比表面積が40〜80m2/g、平均粒度が60〜90nm、粒度分布範囲が30〜400nm、見かけ比重が110〜170g/L、HCl含有率が50〜140ppm、含有される金属不純物の総量が2ppm以下である高純度合成石英粉を使用して、少なくとも1方向から、0.1〜100kgf/cm2のプレスをかけて、石英成形体を形成した後、減圧下、又は02、H2、He及びArの少なくとも1種を含む雰囲気中で、1300〜1500℃の温度域において、加熱焼成処理を行うことを特徴とする。 In order to solve the above problems, the present inventors have intensively developed and completed the present invention. That is, the method for producing the transparent synthetic quartz glass of the present invention has a BET specific surface area of 40 to 80 m 2 / g, an average particle size of 60 to 90 nm, a particle size distribution range of 30 to 400 nm, an apparent specific gravity of 110 to 170 g / L, HCl Using high-purity synthetic quartz powder having a content of 50 to 140 ppm and a total amount of metal impurities of 2 ppm or less, applying a press of 0.1 to 100 kgf / cm 2 from at least one direction, quartz molding After the body is formed, heat firing treatment is performed in a temperature range of 1300 to 1500 ° C. under reduced pressure or in an atmosphere containing at least one of 0 2 , H 2 , He and Ar.
前記加熱焼成処理を、加熱溶融中に0.1〜100kgf/cm2のプレスをかけながら行うことが好ましい。 It is preferable to perform the heat-firing treatment while applying a press of 0.1 to 100 kgf / cm 2 during heat melting.
また、前記高純度合成石英粉が、四塩化珪素の火炎加水分解反応によって製造されたものであることが好適である。 The high-purity synthetic quartz powder is preferably produced by flame hydrolysis reaction of silicon tetrachloride.
本合成石英ガラス体は、本発明の方法により製造される透明合成石英ガラス体である。 The synthetic quartz glass body is a transparent synthetic quartz glass body produced by the method of the present invention.
本発明方法は、火炎加水分解後の合成石英粉を直接使用でき、焼成温度が低温であり、カーボン鋳型と反応しない為、コスト的にも非常に優れている。本発明方法により、透明で内部に微少泡の無い石英ガラス体を容易且つ低コストで製造することができる。本発明の合成石英ガラス体は、本発明の製造方法により容易且つ安価に製造することができ、透明で内部に微少泡が無いという甚大な効果を奏する。 The method of the present invention can be used directly with the synthetic quartz powder after flame hydrolysis, the firing temperature is low, and it does not react with the carbon mold, so it is very excellent in terms of cost. By the method of the present invention, it is possible to easily and inexpensively produce a quartz glass body that is transparent and does not have microbubbles inside. The synthetic quartz glass body of the present invention can be produced easily and inexpensively by the production method of the present invention, and has the enormous effect of being transparent and free of microbubbles inside.
以下に本発明の実施の形態を添付図面に基づいて説明するが、図示例は例示的に示されるもので、本発明の技術思想から逸脱しない限り種々の変形が可能なことはいうまでもない。 DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of the present invention will be described below with reference to the accompanying drawings. However, the illustrated examples are illustrative only, and various modifications can be made without departing from the technical idea of the present invention. .
図1は、本発明の透明合成石英ガラスの製造方法における第1の実施の形態の大略手順を示すフローチャートである。図2は、本発明の透明合成石英ガラスの製造方法における第2の実施の形態の大略手順を示すフローチャートである。 FIG. 1 is a flowchart showing a schematic procedure of a first embodiment in a method for producing a transparent synthetic quartz glass of the present invention. FIG. 2 is a flowchart showing a schematic procedure of the second embodiment in the method for producing the transparent synthetic quartz glass of the present invention.
図1に示した如く、BET比表面積が40〜80m2/g、平均粒度が60〜90nm、粒度分布範囲が30〜400nm、見かけ比重が110〜170g/L、HCl含有率が50〜140ppm、含有される金属不純物の総量が2ppm以下である高純度合成石英粉を準備し(ステップ100)、少なくとも1方向から、0.1〜100kgf/cm2のプレスをかけて、石英成形体を形成した後(ステップ102)、減圧下、又は02、H2、He及びArの少なくとも1種を含む雰囲気中で、1300〜1500℃の温度域において、加熱焼成することによって(ステップ104)、内部に微少泡が無い透明合成石英ガラス体を得ることができる。 As shown in FIG. 1, the BET specific surface area is 40 to 80 m 2 / g, the average particle size is 60 to 90 nm, the particle size distribution range is 30 to 400 nm, the apparent specific gravity is 110 to 170 g / L, the HCl content is 50 to 140 ppm, A high-purity synthetic quartz powder having a total amount of contained metal impurities of 2 ppm or less was prepared (step 100), and a quartz compact was formed by applying a press of 0.1 to 100 kgf / cm 2 from at least one direction. After (step 102), by heating and baking in a temperature range of 1300 to 1500 ° C. under reduced pressure or in an atmosphere containing at least one of 0 2 , H 2 , He and Ar (step 104), the inside A transparent synthetic quartz glass body having no microbubbles can be obtained.
上記高純度合成石英粉は、上記特性を有するものであれば特に限定されないが、四塩化珪素を火炎加水分解して得られた、合成石英微粒子が好適である。 The high-purity synthetic quartz powder is not particularly limited as long as it has the above properties, but synthetic quartz fine particles obtained by flame hydrolysis of silicon tetrachloride are suitable.
上記ステップ102は、一般的なプレス機を用いて加圧成形することができる。加圧条件は、0.1kgf/cm2〜100kgf/cm2の範囲であればよいが、0.3kgf/cm2〜10kgf/cm2の範囲が好ましく、1kgf/cm2〜10kgf/cm2の範囲がより好ましい。
The
上記ステップ104は、公知の加熱溶融炉中で、1300℃〜1500℃で焼成される。加熱温度が1300℃未満では燒結が不十分となり、1500℃を超えると、石英粉とカーボン鋳型との反応性が高まる。本発明は焼成温度が低温であるため、カーボン鋳型と反応せず、高い経済的効果を奏するものである。焼成温度までの昇温速度は、1200℃〜焼成温度までの範囲で、0.1℃/分〜5℃/分の範囲が好ましい。0.1℃/分未満では、遅すぎて工業的ではなく、5℃/分を超えると、燒結後のガラス体内部に泡が残る。
The
上記ステップ104は、02、H2、He及びArの少なくとも1種を含む雰囲気中で行うか、又は減圧下で行うものである。上記雰囲気中であれば圧力の限定はなく、また、減圧下であればいかなる雰囲気でもよい。また、上記ステップ104を、02、H2、He及びArの少なくとも1種を含む雰囲気中で、減圧下で行ってもよい。
また、図2に示した如く、ステップ100及びステップ102を上記と同様に行った後、加熱溶融中に0.1〜100kgf/cm2のプレスをかけながら、加熱焼成することにより(ステップ105)、内部に微少泡が無い透明合成石英ガラス体を得ることができる。
Further, as shown in FIG. 2, after performing
上記ステップ105は、例えば、ホットプレス等により、0.1〜100kgf/cm2のプレスをかけながら、1300℃〜1500℃で加熱焼成処理を行うものであり、該プレスを加熱溶融中に同時に行うことが透明化にはより効果的である。加圧条件は、0.1〜100kgf/cm2の範囲であればよいが、0.3kgf/cm2〜10kgf/cm2の範囲が好ましく、1kgf/cm2〜10kgf/cm2の範囲がより好ましい。焼成温度までの昇温速度は、1200℃〜焼成温度までの範囲で、0.1℃/分〜5℃/分の範囲が好ましい。0.1℃/分未満では、遅すぎて工業的ではなく、5℃/分を超えると、燒結後のガラス体内部に泡が残る。
In
以下に実施例をあげて本発明をさらに具体的に説明するが、これらの実施例は例示的に示されるもので限定的に解釈されるべきでないことはいうまでもない。 The present invention will be described more specifically with reference to the following examples. However, it is needless to say that these examples are shown by way of illustration and should not be construed in a limited manner.
(実施例1)
四塩化珪素を火炎加水分解で得られた合成石英ガラス微粒子(スート微粒子)を採集し、内径600mm×高さ500mmのカーボン鋳型中に、65kg充填し、カーボン製の上下移動可能な蓋をして、プレス機(TOYO HYDRAULIC EQIPMENT CO.LTD製、商品名:ENERPAC HYDRAULIC PRESS)にセットして、上方から1kgf/cm2の圧力を加えてプレスし石英成形体を作成した。
Example 1
Synthetic quartz glass fine particles (soot fine particles) obtained by flame hydrolysis of silicon tetrachloride are collected, filled into a carbon mold with an inner diameter of 600 mm and a height of 500 mm, and covered with a carbon movable lid. Then, it was set in a press machine (manufactured by TOYO HYDRAULIC EQIPMENT CO.LTD, trade name: ENERPAC HYDRAULIC PRESS), and pressed by applying a pressure of 1 kgf / cm 2 from above to produce a quartz molded body.
その後、蓋をはずし、底と側面のカーボン鋳型と一緒に、得られた石英成形体を加熱溶融炉の中にセットして、1×10-2mmHg以下に減圧後、加熱を開始し、1200℃までは、1時間で昇温させ、1200℃から1400℃までは、2℃/分で昇温させ、1400℃で1時間保持し、降温させた。室温に冷却後、鋳型とともに石英ガラス塊を取り出した。 Thereafter, the lid is removed, and the resulting quartz molded body is set in a heating and melting furnace together with the carbon molds on the bottom and side surfaces. After reducing the pressure to 1 × 10 −2 mmHg or less, heating is started, and 1200 The temperature was raised to 1 ° C. in 1 hour, the temperature was raised from 1200 ° C. to 1400 ° C. at 2 ° C./min, held at 1400 ° C. for 1 hour, and the temperature was lowered. After cooling to room temperature, the quartz glass block was taken out together with the mold.
得られた石英ガラス塊は、500φ×150mmで、1mm以上の微小泡の無い、高純度な透明合成石英ガラス体が得られた。ガラス体の純度は、金属不純物の総含有量が1ppm以下あり、OH基濃度が100ppm、Cl濃度は30ppm未満であった。 The obtained quartz glass block was 500φ × 150 mm, and a high-purity transparent synthetic quartz glass body having no fine bubbles of 1 mm or more was obtained. As for the purity of the glass body, the total content of metal impurities was 1 ppm or less, the OH group concentration was 100 ppm, and the Cl concentration was less than 30 ppm.
なお、使用した合成石英ガラス微粒子の特性は、BET比表面積が60m2/g、平均粒度が70nm、粒度分布範囲が40〜300nm、見かけ比重が140g/L、HCl含有率が100ppm、含有される金属不純物の総量が0.8ppmであった。 The characteristics of the synthetic quartz glass fine particles used include a BET specific surface area of 60 m 2 / g, an average particle size of 70 nm, a particle size distribution range of 40 to 300 nm, an apparent specific gravity of 140 g / L, and an HCl content of 100 ppm. The total amount of metal impurities was 0.8 ppm.
(実施例2)
実施例1と同様の合成石英ガラス微粒子を用いて、実施例1と同様、該石英ガラス微粒子をカーボン鋳型中に充填し、上下移動可能な蓋をして、プレス機にセットした後、上方から1kgf/cm2の圧力を加えて石英成形体を形成した。その後、プレスした状態のまま、加熱溶融炉の中にセットして、1×10-2mmHg以下に減圧後、実施例1と同様の温度条件で加熱焼成を行い、石英ガラス塊を得た。
(Example 2)
Using the same synthetic silica glass fine particles as in Example 1, the silica glass fine particles are filled in a carbon mold, covered with a vertically movable lid, set in a press machine, and then from above. A quartz compact was formed by applying a pressure of 1 kgf / cm 2 . Then, in the pressed state, it was set in a heating and melting furnace, reduced in pressure to 1 × 10 −2 mmHg or less, and then heated and fired under the same temperature conditions as in Example 1 to obtain a quartz glass lump.
得られた石英ガラス塊は、500φ×150mmで、1mm以上の微小泡の無い、高純度な透明合成石英ガラス体が得られた。ガラス体の純度も実施例1と同様の結果であった。 The obtained quartz glass block was 500φ × 150 mm, and a high-purity transparent synthetic quartz glass body having no fine bubbles of 1 mm or more was obtained. The purity of the glass body was the same as in Example 1.
(比較例1)
粒径分布範囲が100μm〜500μmの天然石英ガラス粉を、内径600mm×高さ500mmのカーボン鋳型中に充填し、加熱溶融炉の中にセットして、1200℃までは、1時間で昇温させ、1200℃から1750℃までは、2℃/分で昇温させ、1750℃で1時間保持し、降温させた。室温に冷却後、鋳型とともに石英ガラス塊を取り出した。
(Comparative Example 1)
Natural quartz glass powder having a particle size distribution range of 100 μm to 500 μm is filled in a carbon mold having an inner diameter of 600 mm and a height of 500 mm, set in a heating and melting furnace, and heated up to 1200 ° C. in one hour. The temperature was raised from 1200 ° C. to 1750 ° C. at 2 ° C./min, held at 1750 ° C. for 1 hour, and lowered. After cooling to room temperature, the quartz glass block was taken out together with the mold.
得られた石英ガラス塊は、600φ×350mmであった。塊中央付近に1〜4mmφの微小な泡を含む部分が、300φ×300mmの範囲に存在し、使用可能な部分は、全体の40%程度であった。使用後のカーボン鋳型は、石英粉との接触部分が激しく消耗していた。ガラス体の純度は実施例1と同様であった。 The obtained quartz glass block was 600φ × 350 mm. A portion including 1 to 4 mmφ fine bubbles was present in the vicinity of the center of the lump in a range of 300φ × 300 mm, and the usable portion was about 40% of the whole. After use, the carbon mold was heavily consumed in contact with the quartz powder. The purity of the glass body was the same as in Example 1.
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KR20180094087A (en) | 2015-12-18 | 2018-08-22 | 헤래우스 크바르츠글라스 게엠베하 & 컴파니 케이지 | Preparation of Silica Glass Products from Silica Granules |
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 |
CN108698883A (en) | 2015-12-18 | 2018-10-23 | 贺利氏石英玻璃有限两合公司 | The mist projection granulating of silica in quartz glass preparation |
EP3390291A1 (en) * | 2015-12-18 | 2018-10-24 | Heraeus Quarzglas GmbH & Co. KG | Quartz glass made from pyrogenic silicon dioxide granulate having low oh, cl, and al content |
CN108698893A (en) | 2015-12-18 | 2018-10-23 | 贺利氏石英玻璃有限两合公司 | It is melted in crucible in refractory metal and prepares quartz glass body |
US11952303B2 (en) | 2015-12-18 | 2024-04-09 | Heraeus Quarzglas Gmbh & Co. Kg | Increase in silicon content in the preparation of quartz glass |
CN108698888A (en) | 2015-12-18 | 2018-10-23 | 贺利氏石英玻璃有限两合公司 | Preparation in quartz glass preparation as the silica dioxide granule through carbon doping of intermediary |
WO2017103166A2 (en) | 2015-12-18 | 2017-06-22 | Heraeus Quarzglas Gmbh & Co. Kg | Production of a silica glass article in a multichamber furnace |
CN108698880B (en) | 2015-12-18 | 2023-05-02 | 贺利氏石英玻璃有限两合公司 | Preparation of opaque quartz glass bodies |
CN112624579B (en) * | 2020-12-03 | 2021-09-17 | 东海县奥兰石英科技有限公司 | Preparation method and device for producing large-diameter transparent quartz lump by integrated method |
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