JPH0674148B2 - Quartz glass manufacturing method - Google Patents
Quartz glass manufacturing methodInfo
- Publication number
- JPH0674148B2 JPH0674148B2 JP1025985A JP1025985A JPH0674148B2 JP H0674148 B2 JPH0674148 B2 JP H0674148B2 JP 1025985 A JP1025985 A JP 1025985A JP 1025985 A JP1025985 A JP 1025985A JP H0674148 B2 JPH0674148 B2 JP H0674148B2
- Authority
- JP
- Japan
- Prior art keywords
- sol
- quartz glass
- fine powder
- glass
- dispersion liquid
- 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
Links
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
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。TECHNICAL FIELD The present invention relates to a method for producing silica 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 the production of quartz glass by a sol-gel method using a conventional alkyl silicate and fine powder silica as main raw materials, the removal of foreign particles such as coarse particles of fine powder silica and dust present in the prepared sol is the final step of sol preparation. I was doing.
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、目的とするメッシ
ュのフィルター通過させるのが非常に困難であり、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 technique, coarse particles and foreign substances are removed as the final step of the sol preparation, so that the dehydration polycondensation reaction after the hydrolysis reaction of the alkyl silicate has progressed to some extent, the viscosity is high, and the centrifugal force is high. It is very inefficient in the separation process, and if it is excessive, it is very difficult to pass the target mesh through the filter, and therefore, coarse particles and foreign substances, which are defects in the glass after sintering, are considerably contained in the sol. It is difficult to gel while containing it, and to eliminate it during sintering, and there is a problem that the quality level of the produced quartz glass is lowered.
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、ソル−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 solves such a problem,
The object is to improve the prior art by smoothly removing coarse particles and foreign substances from the sol with high accuracy, and to provide a method for producing a very high quality quartz glass by the sol-gel method. There is a place to do it.
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液を調製し、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。The method of the present invention, in the production of quartz glass by the sol-gel method using alkyl silicate and fine powder silica as the main raw material, to prepare a dispersion liquid of fine powder silica, coarse particles of silica and dust etc. from the dispersion liquid. After separating the foreign matter of (1), the dispersion and the alkyl silicate are mixed to prepare a sol.
微粉末シリカの分散液（成分は、SiO4,H2O,HClなど）
は、粘性が低いため、遠心分離の効率が良好であり、よ
り細かなメッ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 fine powder silica (The components are SiO 4 , H 2 O, HCl, etc.)
Has a low viscosity, has good centrifugal efficiency, and can easily pass through a filter with a finer mesh, so that coarse silica particles and foreign substances can be removed from the sol very smoothly and with high precision. It is possible to do.
部粉末シリカ（商品名：アエロジルOX50（Degguss
社））45kgと0.01NHCl108とを混合し、ディゾルバー
（分散装置）にて撹拌を４時間行ない、さらに撹拌しな
がら、超音波照射を５時間行なった。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＝1500,30min）遠心沈降により粗大粒子およびゴ
ミ状異物の分離を行なった。さらに過（最終フィルタ
ー0.2〜2.5μｍ）し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（Si（OEt）４）132
とを混合・撹拌し、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、
過等の処理をした。そして、該ゾルのPH値を３〜６程
度に、0.1Nアンモニア水を滴下することにより調整し
た。この後、必要に応じ過、遠心分離などの処理を加
え、大きさ36×28×12〔cm〕のポリプロピレン製の容器
に600g該ゾルを投入（400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25.3×19.5×0.5〔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18.8×14.8×0.35〔cm〕で、重量は18
0g前後であった。Part powder silica (Product name: Aerosil OX50 (Degguss
45 kg) and 0.01N HCl 108 were mixed and stirred with a dissolver (dispersion device) for 4 hours, and ultrasonic waves were irradiated for 5 hours while further stirring. At this time, in order to prevent the temperature rise of the sol 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 that of the sol after the conventional final step. Next, the sol was put into a centrifuge (G = 1500, 30 min) to separate coarse particles and dust-like foreign matters by centrifugal sedimentation. Further, a fine powder silica dispersion liquid was prepared by filtering (final filter 0.2 to 2.5 μm). After this, the dispersion and ethyl silicate (Si (OEt) 4 ) 132
And are mixed and stirred to carry out a hydrolysis reaction.
In order to make the sol homogeneous, ultrasonic irradiation, centrifugation,
I've done the same. Then, the PH value of the sol was adjusted to about 3 to 6 by dropping 0.1N ammonia water. After this, if necessary, treatment such as filtration and centrifugation is added, and 600 g of the sol is put into a polypropylene container having a size of 36 × 28 × 12 [cm] (400 sheets) and gelled in a closed state. After that, when the shrinkage started, the lid of the container was changed to one having a predetermined opening rate with holes to adjust the drying rate, and the container was placed in a dryer and heated from room temperature at a heating rate of 5 ° C / hr for 60- 80
The mixture was heated to ℃ and kept at this temperature for 10 to 15 days to obtain a dry gel having a size of 25.3 × 19.5 × 0.5 [cm]. The 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 18.8 x 14.8 x 0.35 [cm], and the weight is 18
It was around 0g.
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:800kg/mm2,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。When the glass obtained as described above was observed with an optical microscope, a condensing lamp, etc., there were almost no foreign substances of 1 μm or more in the glass, and very few foreign substances were smaller than that. Moreover, the results of various physical properties analysis on this glass were Vickers hardness: 800 kg / mm 2 , specific gravity: 2.2, which were in agreement with the fused silica glass such as infrared absorption spectrum, near infrared absorption spectrum, and refractive index.
このようにして、本発明により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、ゴミなどの異物が存在しないため、
非常に高品質のものである。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ため、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、光ファイバー用母材など、種々の分野に、
応用が広がるものと考える。Thus, the quartz glass produced by the present invention, in the prepared sol, coarse silica particles that cause foreign matter in the glass after sintering, because there is no foreign matter such as dust,
It is of very high quality. In addition, because it has advantages such as lower cost than the melting method, it is not only in the field where quartz glass has been used so far, but high quality quartz glass can be easily manufactured. For various fields such as photomask substrates and optical fiber base materials,
I think that the application will spread.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 宮下 悟 長野県諏訪市大和３丁目３番５号 株式会 社諏訪精工舎内 (72)発明者 北林 宏仁 長野県諏訪市大和３丁目３番５号 株式会 社諏訪精工舎内 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Satoru Miyashita 3-5 Yamato, Suwa City, Nagano Prefecture Suwa Seikosha Co., Ltd. (72) Hirohito Kitabayashi 3-5 Yamato City, Suwa City, Nagano Prefecture Stock company Suwa Seiko building
Claims (2)
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、ゾル調製を行う
ことを特徴とする石英ガラスの製造方法。1. In the production of quartz glass by a sol-gel method using an alkyl silicate and fine powder silica as main raw materials, a dispersion liquid of fine powder silica is prepared, and coarse particles and foreign matters such as dust are removed from the dispersion liquid. After the separation, the dispersion liquid and an alkyl silicate are mixed to prepare a sol, which is a method for producing quartz glass.
の範囲第１項記載の石英ガラスの製造方法。2. The method for producing quartz glass according to claim 1, wherein the separation is performed by filtration.
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 JPS61168541A (en) | 1986-07-30 |
| JPH0674148B2 true 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 (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008028797A1 (en) * | 2006-09-07 | 2008-03-13 | Degussa Novara Technology S.P.A. | Sol-gel process |
Families Citing this family (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 |
| EP1700824A1 (en) | 2005-03-09 | 2006-09-13 | Degussa AG | Granules based on pyrogenically prepared silicon dioxide, method for their preparation and use thereof |
| 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 |
-
1985
- 1985-01-23 JP JP1025985A patent/JPH0674148B2/en not_active Expired - Lifetime
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008028797A1 (en) * | 2006-09-07 | 2008-03-13 | Degussa Novara Technology S.P.A. | Sol-gel process |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61168541A (en) | 1986-07-30 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| EXPY | Cancellation because of completion of term |