JPS61168541A - Production of quartz glass - Google Patents
Production of quartz glassInfo
- Publication number
- JPS61168541A JPS61168541A JP1025985A JP1025985A JPS61168541A JP S61168541 A JPS61168541 A JP S61168541A JP 1025985 A JP1025985 A JP 1025985A JP 1025985 A JP1025985 A JP 1025985A JP S61168541 A JPS61168541 A JP S61168541A
- Authority
- JP
- Japan
- Prior art keywords
- sol
- dispersion
- quartz glass
- foreign substances
- gel
- 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.)
- Granted
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 10
- 239000006185 dispersion Substances 0.000 claims abstract description 13
- 239000000126 substance Substances 0.000 claims abstract description 13
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 12
- -1 alkyl silicate Chemical compound 0.000 claims abstract description 10
- 239000011362 coarse particle Substances 0.000 claims abstract description 7
- 238000003980 solgel method Methods 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000001914 filtration Methods 0.000 claims description 4
- 239000000428 dust Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 239000000843 powder Substances 0.000 abstract description 5
- 239000011521 glass Substances 0.000 description 7
- 238000005119 centrifugation Methods 0.000 description 4
- 239000000499 gel Substances 0.000 description 4
- 238000005245 sintering Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000013307 optical fiber Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 229910002012 Aerosil® Inorganic materials 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005350 fused silica glass Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000007500 overflow downdraw method Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/006—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels to produce glass through wet route
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Silicon Compounds (AREA)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、ゾル−ゲル法による石英ガラスの製造方法に
関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for producing quartz glass by a sol-gel method.
従来のアルキルシリケートおよび微粉末シリカを主原料
として用いるゾル−ゲル法による石英ガラス製造におい
ては、調製ゾル中に存在する微粉末シリカの粗大粒子な
らびにゴミ等の異物の除去は、ゾル調製の最終工程とし
て行なっていた。In conventional silica glass production using the sol-gel method using alkyl silicate and finely powdered silica as the main raw materials, the removal of coarse particles of finely divided silica and foreign substances such as dust present in the prepared sol is the final step of sol preparation. It was carried out as
しかし、前述の従来技術では、ゾル調製の最終工程とし
て、粗大粒子および異物の除去を行なうため、アルキル
シリケートの加水分解反応後の脱水重縮合反応がある程
度進行した状態であり、粘性が高く、遠心分離処理にお
いては効率が非常に悪く、−過では、目的とするメツシ
ュのフィルターを通過させるのが非常に困難でへり、し
たがって、ゾル中にかなり、焼結後のガラスの欠陥とな
る粗大粒子および異物を含んだままゲル化し、焼結中に
も消滅させることは困難であり、製造した石英ガラスの
品質レベルを落とすという問題点を有する。However, in the above-mentioned conventional technology, since coarse particles and foreign substances are removed as the final step of sol preparation, the dehydration polycondensation reaction after the hydrolysis reaction of the alkyl silicate has progressed to some extent, resulting in high viscosity and centrifugation. The efficiency of the separation process is very low, and it is very difficult to pass through the target mesh filter and the sol contains large particles and coarse particles that become defects in the glass after sintering. It gels while containing foreign substances, and it is difficult to eliminate them during sintering, which poses a problem of lowering the quality level of the manufactured quartz glass.
そこで本発明は、このような問題点を解決するもので、
その目的とするところは、従来技術を改良することによ
り、ゾル中からの粗大粒子および異物の除去を円滑に高
精度に行ない、ゾル−ゲル法による非常に高品質な石英
ガラスの製造方法を提供するところにある。Therefore, the present invention aims to solve these problems.
The purpose is to provide a method for producing extremely high-quality quartz glass using the sol-gel method by improving the conventional technology to smoothly and precisely remove coarse particles and foreign matter from the sol. It's there.
本発明の方法は、アルキルシリケートおよび微粉末シリ
カを主原料として用いるゾル−ゲル法による石英ガラス
の製造において、微粉末シリカの分散成金調製し、該分
散液中よりシリカの粗大粒子ならびにゴミ等の異物を分
離した後、該分散液とアルキルシリケートを混合し、ゾ
ル調製を行なうことを特徴とする。In the method of the present invention, in the production of quartz glass by the sol-gel method using alkyl silicate and finely powdered silica as main raw materials, finely powdered silica is prepared as a dispersion, and coarse silica particles and dust are removed from the dispersion. The method is characterized in that after separating foreign substances, the dispersion liquid and the alkyl silicate are mixed to prepare a sol.
微粉末シリカの分散液（成分は、５ｉｆｔ ｒ ＬＯ＋
ＨＣＪなど）は、粘性が低いため、遠心分離の効率が良
好であり、よシ細かなメツシュのフィルターを通過させ
ることも容易であり、粗大シリカ粒子および異物のゾル
中からの除去が非常に円滑に高精度に行なうことが可能
である。Dispersion of finely powdered silica (components are 5ift r LO+
HCJ, etc.) has low viscosity, so centrifugation efficiency is good, and it is easy to pass through a fine mesh filter, making it very easy to remove coarse silica particles and foreign substances from the sol. It is possible to perform this with high precision.
微粉末シリカ（商品名：アエロジル０Ｘ５０（Ｄｅｇｇ
ｕｓａ社） ） ４５ｋｌ？とｏ、ｏ１ＮＨｃ１１０８
１とを混合し、ディシルバー（分散装置）にて攪拌を４
時間行ない、さらに攪拌しなから一超音波照射を５時間
行なりた。なおこの際、超音波照射による該ゾルの温度
上昇を防ぐため、該ゾルの温度を冷却装置により一定に
保持した。超音波分散後の該ゾルの粘度は、３ｃｐであ
り、従来の最終工程後のゾルに比べ非常に低いものであ
った。次に該ゾルを遠心機にかけ（Ｇ −１５００，３
０ｗ１ｎ）遠心沈降によシ粗大粒子およびゴミ状異物の
分離を行なった。さらにテ過（最終フィルター〇、２〜
２．５μｍ）Ｌ微粉末シリカ分散液を調製した。この後
、該分散液とエチルシリケート（５ｉ（ＯＥｔ ） ４
） １５２１とを混合・攪拌し、加水分解反応を行な
い、さらに、ゾルを均質なものとするため、超音波照射
、遠心分離、濾過等の処理をした。そして、該ゾルのＰ
Ｈ値を３〜６程度に、０．ＩＮアンモニア水を滴下する
ことにより調整した。この後、必要に応じ濾過、遠心分
離などの処理を加え、大きさ３６Ｘ２８Ｘ１２（の〕の
ポリプロピレン製の容器に６００１該ゾルを投入（４０
０枚）し、密閉状態にてゲル化させ、この後、収縮が始
まった時点で、容器のフタを乾燥速度調節のため穴のあ
いた所定の開孔率のものに変え、乾燥機に入れ、室温か
ら昇温速度５℃／ｈｒで６０〜８０℃に加熱し、以後こ
の温度で保持し、１０〜１５日間で大きさ２５．３ｘ
１９．ｓＸ ０．５（ｃｍ）の乾燥ゲルを得た。この乾
燥ゲルを焼結炉に投入し、所定の昇温方法により加熱焼
結し、１３００℃〜１４５０℃にて、透明なガラス体を
得た。このガラスの大きさは１Ｂ、８Ｘ１４．８ｘｏ、
３５（硼〕で、重量は１８０２前後であった。Fine powder silica (product name: Aerosil 0X50 (Degg)
USA company) ) 45kl? and o, o1NHc1108
Mix 1 and stir with a dispersion device.
After stirring for a while, ultrasonic irradiation was carried out for 5 hours without stirring. At this time, in order to prevent the temperature of the sol from increasing due to ultrasonic irradiation, the temperature of the sol was kept constant by a cooling device. The viscosity of the sol after ultrasonic dispersion was 3 cp, which was much lower than the conventional sol after the final step. Next, the sol was centrifuged (G-1500,3
0w1n) Coarse particles and dust-like foreign matter were separated by centrifugal sedimentation. Further filtering (final filter 〇, 2~
2.5 μm)L fine powder silica dispersion was prepared. After this, the dispersion and ethyl silicate (5i(OEt) 4
) 1521 was mixed and stirred to perform a hydrolysis reaction, and further, in order to make the sol homogeneous, it was subjected to treatments such as ultrasonic irradiation, centrifugation, and filtration. Then, P of the sol
Set the H value to about 3-6, 0. Adjustment was made by dropping IN aqueous ammonia. After that, processes such as filtration and centrifugation are added as necessary, and the 6001 sol is put into a polypropylene container with a size of 36 x 28 x 12 (40
0 sheet) and gel it in a sealed state.After this, when the shrinkage starts, change the lid of the container to one with a predetermined porosity with holes to adjust the drying speed, and put it in a dryer. Heated from room temperature to 60-80°C at a temperature increase rate of 5°C/hr, kept at this temperature, and grew to a size of 25.3x in 10-15 days.
19. A dry gel of sX 0.5 (cm) was obtained. This dried gel was put into a sintering furnace and heated and sintered by a predetermined temperature raising method to obtain a transparent glass body at 1300°C to 1450°C. The size of this glass is 1B, 8X14.8xo,
35 (bor), and the weight was around 1802.
以上のようにして得たガラスを、光学顕微鏡、集光ラン
プなどにより観察したところ、ガラス中には、１μｍ以
上の異物はほとんどなく、それ以下のものもごくわずか
であった。また、このガラスに関する諸物性分析の結果
は、ビッカース硬度： ８０ ｏｋｇ／關２．比重：２
．２であり、赤外吸収スペクトル、近赤外吸収スペクト
ル、および屈折率など溶融石英ガラスと一致した◇
〔発明の効果〕
このようにして、本発明によシ製造される石英ガラスは
、調製ゾル中に、焼結後のガラス中の異物の原因となる
粗大シリカ粒子、ゴ≧などの異物が存在しないため、非
常に高品質なものである。When the glass obtained as described above was observed using an optical microscope, a condensing lamp, etc., it was found that there were almost no foreign substances larger than 1 μm in the glass, and there were only a few particles smaller than that. In addition, the results of physical property analysis regarding this glass were as follows: Vickers hardness: 80 ok/2. Specific gravity: 2
．． 2, and the infrared absorption spectrum, near-infrared absorption spectrum, and refractive index matched those of fused silica glass◇ [Effects of the Invention] Thus, the quartz glass produced according to the present invention can be It is of very high quality because it does not contain foreign substances such as coarse silica particles or particles that cause foreign substances in the glass after sintering.
また、溶融法などに比べ低コストであるなどの利点をも
つ九め、これまで石英ガラスを使用していた分野ではも
ちろんのこと、高品質な石英ガラスが容易に製造可能で
あることから、ＩＣ用フォトマスク基板、光フアイバー
用母材など、種々の分野に、応用が広がるものと考える
０
以上In addition, it has advantages such as low cost compared to the fusion method, and it can be used not only in fields where quartz glass has been used until now, but also because high-quality quartz glass can be manufactured easily. We believe that the application will expand to various fields such as photomask substrates for optical fibers, base materials for optical fibers, etc.
Claims (2)
として用いるゾル−ゲル法による石英ガラスの製造にお
いて、微粉末シリカの分散液を調製し、該分散液中より
粗大粒子ならびにゴミ等の異物を分離した後、該分散液
とアルキルシリケートを混合し、ゾル調製を行なうこと
を特徴とする石英ガラスの製造法。(1) In the production of quartz glass by the sol-gel method using alkyl silicate and finely powdered silica as main raw materials, a dispersion of finely powdered silica was prepared, and foreign substances such as coarse particles and dust were separated from the dispersion. A method for producing quartz glass, which comprises subsequently mixing the dispersion and an alkyl silicate to prepare a sol.
中からの異物の分離方法としてろ過を用いることを特徴
とする石英ガラスの製造法。(2) A method for producing quartz glass, characterized in that filtration is used as a method for separating foreign substances from a finely powdered silica dispersion according to claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1025985A JPH0674148B2 (en) | 1985-01-23 | 1985-01-23 | Quartz glass manufacturing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1025985A JPH0674148B2 (en) | 1985-01-23 | 1985-01-23 | Quartz glass manufacturing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61168541A true JPS61168541A (en) | 1986-07-30 |
| JPH0674148B2 JPH0674148B2 (en) | 1994-09-21 |
Family
ID=11745315
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1025985A Expired - Lifetime JPH0674148B2 (en) | 1985-01-23 | 1985-01-23 | Quartz glass manufacturing method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0674148B2 (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001053225A1 (en) * | 2000-01-24 | 2001-07-26 | Yazaki Corporation | Sol-gel process for producing synthetic silica glass |
| EP1700830A1 (en) * | 2005-03-09 | 2006-09-13 | Novara Technology S.R.L. | Process for the production of monoliths by means of the invert sol-gel process |
| US7780937B2 (en) | 2005-03-09 | 2010-08-24 | Evonik Degussa Gmbh | Granules based on pyrogenically prepared silicon dioxide, method for their preparation and use thereof |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP1897860A1 (en) * | 2006-09-07 | 2008-03-12 | Degussa Novara Technology S.p.A. | Sol-gel process |
-
1985
- 1985-01-23 JP JP1025985A patent/JPH0674148B2/en not_active Expired - Lifetime
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001053225A1 (en) * | 2000-01-24 | 2001-07-26 | Yazaki Corporation | Sol-gel process for producing synthetic silica glass |
| EP1700830A1 (en) * | 2005-03-09 | 2006-09-13 | Novara Technology S.R.L. | Process for the production of monoliths by means of the invert sol-gel process |
| WO2006094874A1 (en) * | 2005-03-09 | 2006-09-14 | Degussa Novara Technology S.P.A. | Process for the production of monoliths by means of the invert sol-gel process |
| US7780937B2 (en) | 2005-03-09 | 2010-08-24 | Evonik Degussa Gmbh | Granules based on pyrogenically prepared silicon dioxide, method for their preparation and use thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0674148B2 (en) | 1994-09-21 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |