JPS61232230A - Production of quartz glass - Google Patents

Production of quartz glass

Info

Publication number
JPS61232230A
JPS61232230A JP7288385A JP7288385A JPS61232230A JP S61232230 A JPS61232230 A JP S61232230A JP 7288385 A JP7288385 A JP 7288385A JP 7288385 A JP7288385 A JP 7288385A JP S61232230 A JPS61232230 A JP S61232230A
Authority
JP
Japan
Prior art keywords
sol solution
sol
quartz glass
centrifugal force
filter
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.)
Pending
Application number
JP7288385A
Other languages
Japanese (ja)
Inventor
Hirohito Kitabayashi
北林　宏仁
Sadao Kanbe
貞男 神戸
Motoyuki Toki
元幸 土岐
Satoru Miyashita
悟 宮下
Tetsuhiko Takeuchi
哲彦 竹内
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Seiko Epson Corp
Original Assignee
Seiko Epson Corp
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Seiko Epson Corp filed Critical Seiko Epson Corp
Priority to JP7288385A priority Critical patent/JPS61232230A/en
Publication of JPS61232230A publication Critical patent/JPS61232230A/en
Pending legal-status Critical Current

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
    • C03C3/00—Glass compositions
    • C03C3/04—Glass compositions containing silica
    • C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
    • 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
    • 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
    • C03C2201/00—Glass compositions
    • C03C2201/02—Pure silica glass, e.g. pure fused quartz
    • 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
    • C03C2203/00—Production processes
    • C03C2203/20—Wet processes, e.g. sol-gel process
    • C03C2203/26—Wet processes, e.g. sol-gel process using alkoxides
    • 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
    • C03C2203/00—Production processes
    • C03C2203/20—Wet processes, e.g. sol-gel process
    • C03C2203/34—Wet processes, e.g. sol-gel process adding silica powder

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

PURPOSE:To obtain a uniform and high-quality quartz glass free of contaminant, by filtering a sol solution used as a raw material once or more in sol-gel process, and gelling the sol solution under centrifugal force. CONSTITUTION:Sol solution composed mainly of an alkyl silicate and ultrafine silica powder is filtered once or more with a filter to remove the undissolved lumps larger than the mesh size of the filter. The filtrate is gelled under centrifugal force to remove large silica aggregate formed by the local gelation in the pH-control of the sol solution.

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.

〔発明の概要〕[Summary of the invention]

本発明は、ゾル−ゲル法による石英ガラスの製造方法に
おいて、原料ゾル溶液をフィルターを用いて濾過した後
ＰＨ調整し、該ゾル溶液に遠心力をかけながらゲル化さ
せ几ことにより、結晶、気泡、不定形状の異物のない均
質で高品質な石英ガラスを製造したものである。The present invention is a method for manufacturing quartz glass using a sol-gel method, in which a raw sol solution is filtered using a filter, the pH is adjusted, and the sol solution is gelled while applying centrifugal force, thereby removing crystals and bubbles. , manufactured from homogeneous, high-quality quartz glass free of irregularly shaped foreign particles.

〔従来の技術〕[Conventional technology]

従来のゾル−ゲル法による石英ガラスの製造方法は、整
理ム２０６４９の様にアルキルシリケートおよび超微粉
末シリカを主原料とするゾル溶液を遠心分離して超微粉
末のダマ状物を取り除き、該ゾル溶液をｐＨ３〜６の範
囲になるよう調整してから遠心力をかけながらゲル化さ
せてい友。The conventional sol-gel method for producing quartz glass involves centrifuging a sol solution containing alkyl silicate and ultrafine powder silica as main raw materials to remove lumps of ultrafine powder. Adjust the sol solution to a pH range of 3 to 6 and then apply centrifugal force to gel it.

〔発明が解決しようとする問題点及び目的〕しかし、前
述の従来技術では、分散させる超微粉末シリカ濃度が高
い場合、ダマ状物を取り除く几めの遠心分離に時間がか
か、す、ま几ダマ状物を確実に取り除けないという問題
点を有する。[Problems and objects to be solved by the invention] However, in the above-mentioned prior art, when the concentration of ultrafine powdered silica to be dispersed is high, it takes time to perform thorough centrifugation to remove lumps. There is a problem that the lump-like material cannot be removed reliably.

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プロセス時間を短縮し均質で高
品質な石英ガラスを確実に製造するところにある。Therefore, the present invention aims to solve these problems.
The purpose is to reduce process time and reliably produce homogeneous, high-quality quartz glass.

Ｃ問題点を解決する之めの手段〕 本発明の石英ガラスの製造方法は、アルキルシリケート
および超微粉末シリカを主原料とするゾル−ゲル法によ
る石英ガラスの製造方法において、原料ゾル溶液をＰＨ
Ａａまでの工程の中で少なくとも一回フィルターを用い
て濾過し几後、該ゾル溶液に遠心力をかけながらゲル化
させることを特徴とする。Means for Solving Problem C] The method for producing quartz glass of the present invention is a method for producing quartz glass by a sol-gel method using alkyl silicate and ultrafine powder silica as main raw materials.
The sol solution is characterized in that it is filtered at least once using a filter during the steps up to Aa, and then gelled while applying centrifugal force to the sol solution.

本発明においてフィルターの孔径は５０μｍであり、よ
り好ましくは２０μｍ１さらに好ましくは１０μｍであ
る。In the present invention, the pore size of the filter is 50 μm, more preferably 20 μm, and even more preferably 10 μm.

ゾル溶液のゲル化に際しては、ＰＨ値が低すぎるとゲル
化時間が長くなり乾燥中にゲルが割れて大きなゲルが得
られず、またＰＨが高すぎるとゲル化時間が短くなり品
質が悪くなる。従ってゾル溶液ｔ−ＰＨ３〜６の範囲に
なるよう調整してゲル化させるのが好ましい。When gelling a sol solution, if the pH value is too low, the gelation time will be long and the gel will crack during drying, making it impossible to obtain a large gel.If the pH value is too high, the gelation time will be short and the quality will deteriorate. . Therefore, it is preferable to adjust the sol solution t-PH to a range of 3 to 6 for gelation.

遠心力をかけながらゲル化する際、５００Ｇを越える遠
心力をかけ之ゾルｒｓ液は、分散粒子の沈降によりゾル
溶液の分ｔｌＪＩＩヲひきおこし、乾燥収縮中に大きな
そりや割れを生じる。ま友達心力が小さ過ぎると、ゾル
溶液が重力により下方へ片寄るので、５０Ｇ以上の遠心
力が好ましい。During gelation while applying a centrifugal force, the sol rs solution subjected to a centrifugal force exceeding 500 G causes the sol solution to settle due to sedimentation of dispersed particles, causing large warps and cracks during drying and shrinkage. If the centripetal force is too small, the sol solution will be biased downward due to gravity, so a centrifugal force of 50 G or more is preferable.

〔作用〕[Effect]

本発明の上記の構成によれば、超微粉末シリカ濃度の高
いゾル溶液においても、フィルタ一孔径より大きなダマ
状吻は確実に除去することが可能となり、ｔｅゾル溶液
のＰＨｇ４整時の局所的ゲル化により新ｔに生成した大
粒径シリカや攪拌によってゾル溶液中に取り込まれた空
気は、５０Ｇ〜５００Ｇの遠心力金かけながらゲル化さ
せることにより、大粒径シリカはゲル層の外側に空気は
内側に押しやられて、研壱後のガラス中から取り除くこ
とができる。According to the above configuration of the present invention, even in a sol solution with a high concentration of ultrafine powder silica, it is possible to reliably remove lump-like proboscises larger than the diameter of one pore of the filter, and localized when the PHg4 of the TE sol solution is adjusted. The large particle size silica newly generated by gelation and the air taken into the sol solution by stirring are gelled while applying centrifugal force of 50G to 500G, and the large particle size silica is transferred to the outside of the gel layer. Air is forced inward and can be removed from the glass after polishing.

〔実施例１〕 ？＋［した市販のエチルシリケート２．５Ｌと１０１規
定の塩酸水溶液２ｔｆ：激しく攪拌し、無色透明の均一
溶液を得比、そこに超微粉末シリカ（商品名アエロジル
ｏｘｓｏ、アエロジル社）５６０１を徐々に添加し、充
分に攪拌し之。さらにこのゾル溶液に超音波ｔ−４時間
照射して超微粉末シリカの分散を確実なものとし友。該
ゾル溶液を順次５０μｍ、２０μｍ、１０μｍのフィル
ターを用いて濾過し几。この濾液を攪拌しなから（Ｌ１
規定のアンモニア水を添加してＰ　Ｈ４，５に１１整し
た。[Example 1]? + 2.5 L of commercially available ethyl silicate and 2 tf of 101 N aqueous hydrochloric acid solution: Stir vigorously to obtain a colorless and transparent homogeneous solution, and gradually add ultrafine powdered silica (trade name: Aerosil oxso, Aerosil Co., Ltd.) 5601. Add and stir thoroughly. Furthermore, this sol solution was irradiated with ultrasonic waves for 4 hours to ensure the dispersion of the ultrafine powdered silica. The sol solution was sequentially filtered using 50 μm, 20 μm, and 10 μm filters. Do not stir this filtrate (L1
The pH was adjusted to 4.5 by adding specified aqueous ammonia.

該ゾル溶液■ｌＥ１図に示すようにポリプロピレン製の
容器■に深さ１ａｎになるように仕込みフタ■をし几後
、第２図に示す工うに遠心分離機■に装着し、モータ■
を回転させて１５０Ｇの遠心力をかけながらゲル化させ
第３図に示すような形状のゲル■を得た。ゲル化時間は
約１時間であつ几。As shown in Figure 1, the sol solution (1E1) is poured into a polypropylene container (2) to a depth of 1 ann, covered with a lid (2), and then placed in a centrifugal separator (3) as shown in Figure 2.
was rotated and gelatinized while applying a centrifugal force of 150 G to obtain a gel (2) having a shape as shown in FIG. Gel time is about 1 hour.

得られ几ゲル■を５５℃で２週間乾燥させ友後、１２０
℃／ｈｒの昇温速度で１４００℃迄加熱すると石英ガラ
スが製造でき九〇 この石英ガラスの曲面状の内側および大粒径シリカの存
在する外側を研磨して、幅ｊ　０ｃＷＩＸ　Ｉ　Ｑｃｍ
×厚さ２朋の石英ガラス板が得られた。この石英ガラス
を光学顕微鏡で観察し友ところ１μｍ以上の異物、気泡
、結晶は見られず、高品質なガラスであつ几。The resulting gel was dried at 55°C for 2 weeks, and then dried at 120°C.
Silica glass can be produced by heating up to 1400°C at a temperature increase rate of °C/hr.90 The curved inside of this quartz glass and the outside where large grain size silica is present are polished to a width of j 0c WIX I Qcm.
A quartz glass plate with a thickness of 2 mm was obtained. When this quartz glass was observed under an optical microscope, no foreign matter, bubbles, or crystals larger than 1 μm were found, indicating that the glass was of high quality.

〔比較例１〕 精製し九市販のエチルシリケート２．２ｔと０．０１規
定の塩酸水溶液２−ｓｔｔ−激しく攪拌し、無色透明の
均一溶液を得九。そこに超微粉末シリカを１１３０１Ｆ
ｆ、徐々に添加し、充分に攪拌したｏさらにこのゾル溶
液に超音波を４時間照射して超微粉末シリカの分散を確
実なものとじ几。該ゾル溶液（以後ゾル溶液人と呼ぶ）
を次に示す３種類の比較実験を行った。[Comparative Example 1] 2.2 tons of purified commercially available ethyl silicate and 2-stt of 0.01N aqueous hydrochloric acid were vigorously stirred to obtain a colorless and transparent homogeneous solution. Add ultrafine powder silica to it 11301F.
f. Gradually add the silica and stir thoroughly. o Further, irradiate this sol solution with ultrasonic waves for 4 hours to ensure the dispersion of the ultrafine powdered silica. The sol solution (hereinafter referred to as sol solution person)
The following three types of comparative experiments were conducted.

実験１：ゾル溶４ＬＡ　ｆ　順次５０μｑ、２０μｍ。Experiment 1: Sol solution 4LA f sequentially 50μq and 20μm.

１０μｍのフィルターでろ過し、該ゾ ル溶液’ｊｉ（Ｌ１規定のアンモニア水でＰＨを４．５
に調整してから２００Ｇの遠心力をかけながらゲル化し
友。Filter with a 10 μm filter, and adjust the sol solution to pH 4.5 with L1 normal ammonia water.
After adjusting the temperature, it gels while applying a centrifugal force of 200G.

実験２：ゾル溶液Ａを５００Ｇの遠心力で１時間遠心分
離した後、その上ずみ溶液の ＰＨを４．５に調整してから２０（ＩＧの遠心力をかけ
ながらゲル化し几。Experiment 2: After centrifuging the sol solution A at 500 G centrifugal force for 1 hour, the pH of the resulting solution was adjusted to 4.5, and gelatinized while applying the centrifugal force of 20°C (IG).

実験５：ゾル溶液人を５００Ｇの遠心力で５時間遠心分
離した後、その上ずみ溶液の ＰＨを４．５に調整してから２００Ｇの遠心力をかけな
がらゲル化し九。Experiment 5: After centrifuging the sol solution at 500G centrifugal force for 5 hours, the pH of the resulting solution was adjusted to 4.5 and gelatinized while applying 200G centrifugal force.9.

乾燥、焼結後顕微鏡観察を行った。実験１．実験３の石
英ガラスについては、気泡、結晶、不定形状の異物はほ
とんど無く高品質であつ几、実験２の石英ガラスについ
ては、気泡、結晶は無いが不定形状の異物が若干存在し
品質的には良くなかった。After drying and sintering, microscopic observation was performed. Experiment 1. The quartz glass in Experiment 3 had almost no bubbles, crystals, or irregularly shaped foreign matter, and was of high quality.The quartz glass in Experiment 2 had no bubbles or crystals, but there were some irregularly shaped foreign matter, and the quality was poor. was not good.

フィルターを使つｔ場合と同品質レベルのガラスを得る
には、遠心分離操作だけの場合長時間を要することとな
つｔｏ 〔発明の効果〕 以上述べ几ように本発明に工れば、原料ゾル溶液をｐａ
ｗ４整までの工程の中で少なくとも一回フィルターを用
いて濾過した後、゛核ゾル溶液に遠心力をかけながらゲ
ル化させｔ後、乾燥、焼結させ几ことにより、結晶、気
泡、不定形状の異物のない均質で高品質な石英ガラスを
製造できる効果を有するσ まｔ本発明によれば、ゾル溶液中の未分散ダマ状物を除
く遠心分離操作をフィルターによる濾過操作に変更する
ことにより、プロセス時間ノ短縮化が可能になり、量産
性にも大きなメリットを有するＯ[Effects of the Invention] As described above, if the present invention is applied as described above, the raw material sol can be solution to pa
After filtration using a filter at least once during the process up to W4, the nuclear sol solution is gelled while applying centrifugal force, and then dried and sintered to remove crystals, bubbles, and irregular shapes. According to the present invention, by changing the centrifugation operation to remove undispersed lumps in the sol solution to a filtration operation using a filter, O

【図面の簡単な説明】[Brief explanation of the drawing]

第１図はゾル溶液の容器への仕込状態図、第２図はゾル
の遠心分離機への装着状態囚、第３図はゲルの形状図で
ある。 以　　上FIG. 1 is a diagram of the sol solution being charged into a container, FIG. 2 is a diagram of the sol being installed in a centrifuge, and FIG. 3 is a diagram of the shape of the gel. that's all

Claims (1)

【特許請求の範囲】[Claims] アルキルシリケートおよび超微粉末シリカを主原料とす
るゾル−ゲル法による石英ガラスの製造方法において、
原料ゾル溶液をＰＨ調整までの工程の中で少なくとも一
回フィルターを用いて濾過した後、該ゾル溶液に遠心力
をかけながらゲル化させることを特徴とする石英ガラス
の製造方法。In a method for producing quartz glass by a sol-gel method using alkyl silicate and ultrafine powder silica as main raw materials,
A method for producing quartz glass, which comprises filtering a raw material sol solution using a filter at least once during the process up to pH adjustment, and then gelling the sol solution while applying centrifugal force.
JP7288385A 1985-04-05 1985-04-05 Production of quartz glass Pending JPS61232230A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP7288385A JPS61232230A (en) 1985-04-05 1985-04-05 Production of quartz glass

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP7288385A JPS61232230A (en) 1985-04-05 1985-04-05 Production of quartz glass

Publications (1)

Publication Number Publication Date
JPS61232230A true JPS61232230A (en) 1986-10-16

Family

ID=13502175

Family Applications (1)

Application Number Title Priority Date Filing Date
JP7288385A Pending JPS61232230A (en) 1985-04-05 1985-04-05 Production of quartz glass

Country Status (1)

Country Link
JP (1) JPS61232230A (en)

Similar Documents

Publication Publication Date Title
JP3203694B2 (en) Manufacturing method of quartz glass
JPS61232230A (en) Production of quartz glass
JPS62105936A (en) Production of quartz glass
JPS61232233A (en) Production of quartz glass
JPS61168537A (en) Production of quartz glass
JPH0348140B2 (en)
JPS6197136A (en) Production of quartz glass
JPH0383805A (en) Production of spherical hydroxyapatite
JPH0674148B2 (en) Quartz glass manufacturing method
JPS62207723A (en) Production of glass
JPH01270531A (en) Production of formed glass body
JPH01270530A (en) Production of formed glass body
JPH0196027A (en) Production of glass
JPS6158818A (en) Manufacture of quartz glass
JPS62119124A (en) Production of glass
JPS61178426A (en) Production of quartz glass
JPS62167230A (en) Production of glass tube
JPH0776101B2 (en) Method for manufacturing glass molded body
JPS632820A (en) Production of glass
JPS62226821A (en) Production of glass
JPS63144127A (en) Production of quartz glass
JPH02302332A (en) Production of platy silica glass
JPS63112435A (en) Production of quartz glass
JPS62246827A (en) Production of glass
JPS63297226A (en) Production of short-wavelength laser beam transmitting quartz glass