JPS61168538A - Mass-production of quartz glass - Google Patents

Mass-production of quartz glass

Info

Publication number
JPS61168538A
JPS61168538A JP1025685A JP1025685A JPS61168538A JP S61168538 A JPS61168538 A JP S61168538A JP 1025685 A JP1025685 A JP 1025685A JP 1025685 A JP1025685 A JP 1025685A JP S61168538 A JPS61168538 A JP S61168538A
Authority
JP
Japan
Prior art keywords
gel
quartz glass
temperature
furnace
dry 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.)
Pending
Application number
JP1025685A
Other languages
Japanese (ja)
Inventor
Motoyuki Toki
元幸 土岐
Sadao Kanbe
貞男 神戸
Satoru Miyashita
悟 宮下
Hirohito Kitabayashi
北林 宏仁
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 JP1025685A priority Critical patent/JPS61168538A/en
Publication of JPS61168538A publication Critical patent/JPS61168538A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/12Other methods of shaping glass by liquid-phase reaction processes

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Silicon Compounds (AREA)
  • Glass Melting And Manufacturing (AREA)

Abstract

PURPOSE:To enable the mass-production of quartz glass with a low-cost apparatus in high efficiency, by producing a dry gel from a metal alkoxide or ultrafine silica powder, and passing the gel through a belt furnace having a temperature gradient varying continuously from room temperature to the required temperature. CONSTITUTION:A raw material at least composed of a metal alkoxide or ultrafine silica powder is hydrolyzed, pH-controlled, and subjected to a sol-gel process to produce a gel, which is dried to a dry gel. A refractory plate 3 is placed on a refractory belt 4 in a belt furnace 1, and the above dry gel 2 is supplied continuously on the refractory plate. The belt furnace 1 is provided with temperature gradient varying continuously from room temperature to a specific temperature and extending from one end to the other end. The dry sol 2 is sintered in the course of being transferred from one end to the other end of the belt furnace 1, and is delivered continuously from the furnace as a completely sintered transparent quartz glass.

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
し、更に詳しくはドライゲルの焼結の量産方法に関する
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, and more particularly to a method for mass production of sintered dry gel.

〔従来の技術〕[Conventional technology]

金属アルコキシドあるいは微粉末シリカを原料とするゾ
ル−ゲル法による石英ガラスの製造方法において、従来
のドライゲルの焼結方法は、ドライゲルを焼結炉に投入
し、炉の温度を室温から適当な昇温プログラムで加熱し
焼結するという、バッチ処理であった。
In the method of manufacturing quartz glass by the sol-gel method using metal alkoxide or fine powder silica as raw materials, the conventional dry gel sintering method involves putting the dry gel into a sintering furnace and raising the temperature of the furnace appropriately from room temperature. It was a batch process that involved heating and sintering according to a program.

〔発明が解決しようとする問題点〕[Problem that the invention seeks to solve]

しかし、前述の従来技術では次のような欠点を有する。 However, the above-mentioned conventional technology has the following drawbacks.

すなわち、従来のバッチ処理では、1回の焼結炉に投入
できるドライゲルの量と焼結プロセスのサイクルタイム
によって、石英ガラスの生産量が決まってしまうため、
よほど大きな焼結炉がないかぎり、効率の良い量産はで
きない。また、大きな焼結炉は大きな電力が必要になる
ため、電気配線工事のコストも大きなものとなってしま
う。
In other words, in conventional batch processing, the amount of quartz glass produced is determined by the amount of dry gel that can be fed into the sintering furnace at one time and the cycle time of the sintering process.
Unless you have a very large sintering furnace, efficient mass production is not possible. Furthermore, since a large sintering furnace requires a large amount of electric power, the cost of electrical wiring work becomes large.

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、電気工事等のコストも小さく
、焼結の量産性の良い製造方法を提供することにある。
Therefore, the present invention aims to solve these problems.
The purpose is to provide a manufacturing method for sintering that has low cost for electrical work and has good mass productivity.

〔問題点を解決するための手段〕[Means for solving problems]

本発明の石英ガラスの量産方法は次のようなものである
。すなわち、金属アルコキシドあるいは微粉末シリカを
原料とし、アルカリあるいは酸のような適当な触媒で加
水分解した後、必要ならばPH値を3〜6に調整し、ゾ
ルをゲル化させる。
The method for mass producing quartz glass of the present invention is as follows. That is, a metal alkoxide or finely powdered silica is used as a raw material, and after hydrolysis with a suitable catalyst such as an alkali or an acid, the pH value is adjusted to 3 to 6 if necessary, and the sol is gelled.

このゲルを適当な乾燥条件で収縮乾燥させドライゲルと
する。第1図に示すベルト炉の耐熱ベルト上に耐熱板を
置きその上に上記ドライゲルを連続的に投入する。ドラ
イゲルはベルト炉の一端から他端まで移動中に焼結が進
行し、他端を出る時には焼結が終了し透明な石英ガラス
となシ、連続的に透明石英ガラスを得ることができる。
This gel is shrink-dried under appropriate drying conditions to obtain a dry gel. A heat-resistant plate is placed on the heat-resistant belt of the belt furnace shown in FIG. 1, and the dry gel is continuously poured onto the heat-resistant plate. Sintering of the dry gel progresses while it is moving from one end of the belt furnace to the other, and when it leaves the other end, the sintering is completed and becomes transparent quartz glass.Transparent quartz glass can be continuously obtained.

@1図において、1はベルト炉、2はドライゲル、3は
耐熱板、4は耐熱ベルト、5は荷車、6はドライゲルが
焼結終了した石英ガラスである。また第2図はベルト炉
の一端から他端までの温度分布である。
@1 In Figure 1, 1 is a belt furnace, 2 is a dry gel, 3 is a heat-resistant plate, 4 is a heat-resistant belt, 5 is a cart, and 6 is a quartz glass in which the dry gel has been sintered. Moreover, FIG. 2 shows the temperature distribution from one end of the belt furnace to the other end.

ドライゲルの入口部の温度は室温であり、出口は焼結温
度になっている〇 以上の焼結の量産方法により、石英ガラスが連続的に製
造できるようになり量産性に優れている。
The temperature at the inlet of the dry gel is room temperature, and the temperature at the outlet is at the sintering temperature.The sintering mass production method described above enables continuous production of quartz glass and is excellent in mass productivity.

〔実施例〕〔Example〕

以下、実施例で本発明の詳細な説明する。 Hereinafter, the present invention will be explained in detail with reference to Examples.

実施例1゜ 精製した市販のシリコンエトキシド20BOf(10モ
ル)に0.01規定の塩酸2800+tA!を加え、激
しく攪拌して加水分解した0次にこの溶液に超微粉末シ
リカ(表面積50 m”/ fのアエロジル0X50)
900F(15モル)を攪拌しながら加え、超音波振動
をかけた。さらに遠心分離によりてダマ状物を取り除い
た。このゾルに0.1規定のアンモニア水を滴下してP
H値が4.0になるように調整した。次にこのゾル全ポ
リプロピレン製箱型容器CW30 X D 30 X 
H10備)10個に高さが1cIrLになるよう仕込ん
だ。密閉し、20℃で放置しゲル化し、−夜装置した。
Example 1 0.01N hydrochloric acid 2800+tA was added to purified commercially available silicon ethoxide 20BOf (10 mol)! was added and hydrolyzed by vigorous stirring. Ultrafine powdered silica (Aerosil 0X50 with a surface area of 50 m"/f) was added to this solution.
900F (15 mol) was added with stirring and ultrasonic vibration was applied. Further, clumps were removed by centrifugation. Add 0.1N ammonia water dropwise to this sol and P
The H value was adjusted to 4.0. Next, this sol box-shaped container made entirely of polypropylene CW30
H10) 10 pieces were prepared so that the height was 1 cIrL. The mixture was sealed tightly and allowed to stand at 20°C to form a gel, and was then stored overnight.

次に容器のフタを開口率0.8 %のものに替え、室温
から60℃に昇温し10日間この温度で乾燥させたとこ
ろ、室温に放置しても割れない安定なド・ライゲルが1
0個得られた。
Next, the lid of the container was changed to one with an open area ratio of 0.8%, the temperature was raised from room temperature to 60°C, and the lid was dried at this temperature for 10 days.
0 pieces were obtained.

第1図に示したベルト炉の温度分布全第2図のように設
定し、ドライゲルを1個づつ一端から投入し、連続的に
10個投入した。24時時間量初の投入のドライゲルが
焼結されて透明な石英ガラスとなって出てきた。それか
らつづけて焼結後の石英ガラスが10個当てきており、
連続的にドライゲルを焼結することができることが分か
った。
The temperature distribution of the belt furnace shown in FIG. 1 was set as shown in FIG. 2, and the dry gels were introduced one by one from one end, and 10 pieces were continuously introduced. The dry gel that was first introduced during the 24-hour period was sintered and came out as transparent quartz glass. After that, 10 pieces of sintered quartz glass arrived.
It has been found that dry gels can be sintered continuously.

以上実施例に示したように、本発明の製造方法を用いれ
ば連続的にドライゲルが焼結できるため、量産性良く石
英ガラスが製造できる。
As shown in the examples above, using the manufacturing method of the present invention allows dry gel to be sintered continuously, so silica glass can be manufactured with good mass productivity.

また、本発明の手法は、本実施例で示したシリコンエト
キシドと微粉末シリカを原料とするゾル−ゲル法に限定
されるものではない。またベルト炉の構造、その内部の
温度分布、温度については本実施例以外に種々考えられ
るが、本発明の適用範囲は本実施例に限定されるもので
ないことは明らかである。
Further, the method of the present invention is not limited to the sol-gel method using silicon ethoxide and finely powdered silica as raw materials as shown in this example. In addition, various types of belt furnace structure, internal temperature distribution, and temperature can be considered other than this example, but it is clear that the scope of application of the present invention is not limited to this example.

〔発明の効果〕〔Effect of the invention〕

以上述べたように、本発明によれば、ゾル−ゲル法によ
るドライゲルの焼結の量産が効率良く容易に実施できる
ので、石英ガラス製造の量産化に大きく買献する。
As described above, according to the present invention, mass production of dry gel sintering by the sol-gel method can be carried out efficiently and easily, which greatly contributes to the mass production of quartz glass manufacturing.

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

第1図は、本発明のドライゲルの焼結用ベルト炉の概略
図である。また第2図は第1図のベルト炉の内部の温度
分布を示す図である。 以上
FIG. 1 is a schematic diagram of a belt furnace for sintering dry gel according to the present invention. Further, FIG. 2 is a diagram showing the temperature distribution inside the belt furnace of FIG. 1. that's all

Claims (1)

【特許請求の範囲】[Claims] 少なくとも金属アルコキシドあるいは超微粉末シリカを
原料とするゾル−ゲル法により石英ガラスを製造する低
温合成法において、ドライゲルを焼結し透明な石英ガラ
スとする工程で、一端から他端まで連続的に室温から所
定の温度まで温度勾配のつけてあるベルト炉の室温の一
端から連続的にドライゲルを投入し、ベルト炉内部を移
動し、所定の温度になっている他端に移動することによ
り焼結し、石英ガラスとする石英ガラスの量産方法。
In the low-temperature synthesis method in which silica glass is produced by the sol-gel method using at least metal alkoxide or ultrafine powdered silica as raw materials, the process of sintering dry gel to form transparent quartz glass is performed continuously at room temperature from one end to the other. The dry gel is continuously introduced from one end of the belt furnace at room temperature, which has a temperature gradient from , a method for mass production of quartz glass.
JP1025685A 1985-01-23 1985-01-23 Mass-production of quartz glass Pending JPS61168538A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP1025685A JPS61168538A (en) 1985-01-23 1985-01-23 Mass-production of quartz glass

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP1025685A JPS61168538A (en) 1985-01-23 1985-01-23 Mass-production of quartz glass

Publications (1)

Publication Number Publication Date
JPS61168538A true JPS61168538A (en) 1986-07-30

Family

ID=11745233

Family Applications (1)

Application Number Title Priority Date Filing Date
JP1025685A Pending JPS61168538A (en) 1985-01-23 1985-01-23 Mass-production of quartz glass

Country Status (1)

Country Link
JP (1) JPS61168538A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115724436A (en) * 2022-12-19 2023-03-03 贵州航天乌江机电设备有限责任公司 Preparation method of hydrophobic silica gradient aerogel with adjustable structure

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115724436A (en) * 2022-12-19 2023-03-03 贵州航天乌江机电设备有限责任公司 Preparation method of hydrophobic silica gradient aerogel with adjustable structure

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