JPH0451498B2 - - Google Patents

Info

Publication number
JPH0451498B2
JPH0451498B2 JP18158984A JP18158984A JPH0451498B2 JP H0451498 B2 JPH0451498 B2 JP H0451498B2 JP 18158984 A JP18158984 A JP 18158984A JP 18158984 A JP18158984 A JP 18158984A JP H0451498 B2 JPH0451498 B2 JP H0451498B2
Authority
JP
Japan
Prior art keywords
silicon dioxide
amorphous silicon
dioxide powder
powder
sintered body
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
Application number
JP18158984A
Other languages
Japanese (ja)
Other versions
JPS6158832A (en
Inventor
Koji Seki
Hiroshi Morishita
Kyoshi Oono
Hiroshi Yokota
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.)
Japan Oxygen Co Ltd
Original Assignee
Japan Oxygen Co Ltd
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 Japan Oxygen Co Ltd filed Critical Japan Oxygen Co Ltd
Priority to JP18158984A priority Critical patent/JPS6158832A/en
Publication of JPS6158832A publication Critical patent/JPS6158832A/en
Publication of JPH0451498B2 publication Critical patent/JPH0451498B2/ja
Granted legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C3/00Glass compositions
    • C03C3/04Glass compositions containing silica
    • C03C3/06Glass compositions containing silica with more than 90% silica by weight, e.g. quartz

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 Compositions (AREA)

Description

【発明の詳細な説明】 〔産業上の利用分野〕 本発明は真空溶融法によつて透明な石英ガラス
を製造するに適した材料に関するものである。
DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to a material suitable for producing transparent quartz glass by a vacuum melting method.

(従来の技術) 従来工業的規模で透明石英ガラスを製造する方
法としてベルヌーイ法あるいは真空溶融法が知ら
れている。ベルヌーイ法は水晶粉又は非晶質二酸
化珪素粉をアルゴン−酸素プラズマ炎あるいは酸
水素炎等の炎中に供給して溶融させ、透明石英ガ
ラスを得るものであり、また真空溶融法は水晶粉
をグラフアイト製ルツボに入れ真空下で長時間焼
結溶融することにより透明石英ガラスを得るもの
である。
(Prior Art) The Bernoulli method or the vacuum melting method has been known as a method for producing transparent quartz glass on an industrial scale. In the Bernoulli method, crystal powder or amorphous silicon dioxide powder is fed into a flame such as an argon-oxygen plasma flame or an oxyhydrogen flame and melted to obtain transparent quartz glass, and in the vacuum melting method, crystal powder is Transparent quartz glass is obtained by placing it in a graphite crucible and sintering and melting it under vacuum for a long time.

〔発明が解決しようとする問題点〕 しかし、ベルヌーイ法では、原料供給の速さに
限度がある等のことから生ずる生産性の悪さ、あ
るいは純度のよい製品を得るにはエネルギーコス
トが高くなるなどの不都合点があり、また真空溶
融法では、前記ベルヌーイ法に比し、泡が多く高
純度のものが期待できず、水晶粉を使用している
ため原料供給に難点がある。
[Problems to be solved by the invention] However, the Bernoulli method suffers from poor productivity due to limitations in the speed of raw material supply, or high energy costs to obtain products with good purity. In addition, compared to the Bernoulli method, the vacuum melting method produces more bubbles and cannot be expected to produce a product of high purity, and since quartz powder is used, there are difficulties in supplying raw materials.

このように透明石英ガラスを得るための原料と
しては非晶質二酸化珪素粉又は水晶粉が通常用い
られ、非晶質二酸化珪素粉を原料とする場合は純
度の高いものが要求され、殊にNa等ガラスの失
透をもたらす不純物の存在は好ましくないとされ
ていた。
In this way, amorphous silicon dioxide powder or quartz powder is usually used as a raw material for obtaining transparent quartz glass, and when amorphous silicon dioxide powder is used as a raw material, high purity is required, especially Na The presence of impurities that cause devitrification of glass was considered undesirable.

本発明者等は上記の如き実情に鑑み種々考究し
た結果、資源的制約のない非晶質二酸化珪素粉を
原料とした真空溶融法による透明石英ガラスの製
造法を見出した。この方法は、非晶質二酸化珪素
粉を加熱して結晶化させると共に焼結して焼結体
を得、ついでこれを真空下溶融してガラス化させ
ることを特徴とするものであり、本発明はこれを
実施するに好適な材料を提供することを目的とす
るものである。
As a result of various studies in view of the above-mentioned circumstances, the present inventors have discovered a method for producing transparent quartz glass using a vacuum melting method using amorphous silicon dioxide powder as a raw material without resource constraints. This method is characterized by heating amorphous silicon dioxide powder to crystallize it and sintering it to obtain a sintered body, which is then melted under vacuum to vitrify it, and the present invention The purpose of the present invention is to provide materials suitable for carrying out this method.

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

本発明は、上記目的を達成するため、非晶質二
酸化珪素粉を、該二酸化珪素が加熱により結晶化
して焼結体化するに必要なアルカリ金属成分の含
有溶液中に混合せしめて、該アルカリ金属成分を
前記非晶質二酸化珪素粉に付着せしめてなること
を特徴とする透明石英ガラスの製造用材料に係る
ものである。
In order to achieve the above object, the present invention mixes amorphous silicon dioxide powder into a solution containing an alkali metal component necessary for the silicon dioxide to crystallize and sinter by heating. The present invention relates to a material for producing transparent quartz glass, characterized in that it is made by adhering a metal component to the amorphous silicon dioxide powder.

尚、二酸化珪素が加熱により結晶化して焼結体
化するに必要なアルカリ金属成分とは、ナトリウ
ム、カリウム、カルシウム等であつて、本発明で
は、これらの水酸化物あるいはこれらを含む各種
塩類等の化合物であつて、均一に溶解されるもの
を使用する。
Incidentally, the alkali metal components necessary for silicon dioxide to crystallize into a sintered body by heating are sodium, potassium, calcium, etc., and in the present invention, these hydroxides or various salts containing these are used. Use a compound that dissolves uniformly.

〔実施例〕〔Example〕

以下本発明の詳細について説明すると、前記し
たように本発明者等が別途開発した透明石英ガラ
スの製造法においては、従来の方法の如く非晶質
二酸化珪素粉又は水晶粉等の原料を直接ガラス化
せしめるものではなく、原料粉を結晶化すると共
に焼結して焼結体を得る仮焼プロセスを有する。
即ち、非晶質二酸化珪素粉を適宜な容器に充填
し、加熱により焼結して固型物を得、ついでこれ
を真空加熱炉で溶融せしめてガラス化させること
にあり、これによつて、従来の如く原料粉を直接
ガラス化させる方法に比し、生産性が大幅に向上
する。従つてこの方法を実施する上での決め手は
前記仮焼プロセスにおいてて如何に容易に焼結体
を得るかであるが、これと同時に最終的に得られ
るガラスインゴツトの純度が高いことも要求され
る。従来方法によつて明石英ガラスを製造する場
合、品質と生産性とは通常相対的なものであり、
双方を満足させる方法、手段が当然望まれる。
The details of the present invention will be explained below. As mentioned above, in the method for manufacturing transparent quartz glass that was separately developed by the present inventors, raw materials such as amorphous silicon dioxide powder or quartz powder are directly added to the glass as in the conventional method. It is not a process that involves crystallizing raw material powder and sintering it to obtain a sintered body.
That is, amorphous silicon dioxide powder is filled into a suitable container, sintered by heating to obtain a solid product, and then melted in a vacuum heating furnace to vitrify it. Productivity is significantly improved compared to the conventional method of directly vitrifying raw material powder. Therefore, the deciding factor in implementing this method is how easily a sintered body can be obtained in the calcination process, but at the same time, it is also required that the final glass ingot be of high purity. be done. When producing Akira quartz glass by conventional methods, quality and productivity are usually relative;
Naturally, methods and means that satisfy both parties are desired.

本発明者等はこの要求に応えるべく種々考究し
た結果、焼結体を結晶質の状態で得ること、即
ち、非晶質二酸化珪素を加熱によつて容易に結晶
かつ焼結化せしめるため予めアルカリ金属成分を
含有させること、そして含有させたアルカリ金属
成分をガラス化のため溶融する際真空下で処理す
ることにより除去する方法を見出した。前記した
ように従来方法においては結晶化のプロセスはな
い故、原料として使用される非晶質二酸化珪素粉
中には結晶化に起因する成分は不純物として積極
的に除去されるか、かかる不純物を含まないい原
料が選択されるが本発明においては必須条件であ
る。ここで純度の高い透明石英ガラスを得ること
と、原料中に不純物を添加するもしくは純度の低
い非晶質二酸化珪素を選択使用することとは相反
することになるが、仮焼プロセスによつて得られ
た焼結体を真空下で溶融することにより不純成分
を除去する。これは焼結体真空下で加熱溶融して
ガラス化する際に結晶化に寄与したアルカリ金属
が容易に離脱し排気されることによる。
As a result of various studies to meet this demand, the present inventors have found that it is possible to obtain a sintered body in a crystalline state, that is, in order to easily crystallize and sinter the amorphous silicon dioxide by heating, it is possible to prepare the sintered body with alkali in advance. We have found a method for containing a metal component and removing the alkali metal component by treating it under vacuum during melting for vitrification. As mentioned above, since there is no crystallization process in the conventional method, components caused by crystallization in the amorphous silicon dioxide powder used as a raw material are either actively removed as impurities or such impurities are removed. This is an essential condition in the present invention, although raw materials that do not contain such substances are selected. Obtaining transparent quartz glass with high purity is contradictory to adding impurities to raw materials or selectively using amorphous silicon dioxide with low purity, but the Impurity components are removed by melting the sintered body under vacuum. This is because when the sintered body is heated and melted under vacuum to vitrify, the alkali metal that contributed to crystallization is easily separated and exhausted.

非晶質二酸化珪素にアルカリ金属として例えば
Na成分を重量比1000ppm付加したものをルツボ
等の容器に充填し1000℃以上に加熱すると、結晶
化した多孔状の焼結体が得られる。この焼結体は
β−クリストバライトの結晶質をもつものであ
り、加熱により徐々に溶融せず融点が一意的なも
ので約1700℃以上である。一方アルカリ金属成分
が分解脱離する温度は前記融点以下であるから、
焼結体が溶融されるまに不純成分の十分な脱離除
去が可能になる。これは焼結体が結晶化され多孔
質に形成されていることによるもので、焼結体が
溶融されるまでにその内部はほとんど真空化され
る。
For example, as an alkali metal in amorphous silicon dioxide
When a container such as a crucible is filled with 1000 ppm of Na component added by weight and heated to 1000°C or higher, a crystallized porous sintered body is obtained. This sintered body has crystalline β-cristobalite, and does not gradually melt when heated, but has a unique melting point of about 1700°C or higher. On the other hand, since the temperature at which the alkali metal component decomposes and leaves is below the melting point,
Impurity components can be sufficiently desorbed and removed while the sintered body is melted. This is because the sintered body is crystallized and formed porous, and the interior of the sintered body is almost evacuated before it is melted.

実施例 内容積13のステンレス製円透容器に脱イオン
水5を入れ、常温、常圧下で脱イオン水を撹拌
しつつ非晶質二酸化珪素粉500g加えて、水−二
酸化珪素混合系を得た。つぎにアルカリ金属成分
としてNa成分をNaOHの形で添加混合する。こ
の場合、Na成分の添加量は、二酸化珪素に付着
するNa成分が、最終的に重量比で約1000ppmと
なるよう調整され、そのために水−二酸化珪素混
合系に2300ppmのNa成分を1規定NaOHの形で
50ml添加した。これによつて、非晶質二酸化珪素
粉にNaが均一にイオンとして付着する。ついで
この混合系を約60分撹拌操作した後、フイルター
プレスによつて固液液分離し、さらに乾燥処理を
行つて、二酸化珪素粉にNa成分が重量比で
1000ppm程度物理吸着もしくは化学結合された粉
体が得られた。得られた粉体は、略50μm〜500μ
mの粒径を持つものであり、原料粉である非晶質
二酸化珪素粉が約0.02μmの微粉であつたものが、
凝集されたものであり、適宜の径に調粒される。
Example Deionized water 5 was placed in a transparent stainless steel container with an internal volume of 13, and 500 g of amorphous silicon dioxide powder was added while stirring the deionized water at room temperature and under normal pressure to obtain a water-silicon dioxide mixed system. . Next, a Na component in the form of NaOH is added and mixed as an alkali metal component. In this case, the amount of Na component added is adjusted so that the final weight ratio of Na component attached to silicon dioxide is approximately 1000 ppm, and for this purpose, 2300 ppm of Na component is added to the water-silicon dioxide mixed system using 1 N NaOH. in the form of
Added 50ml. As a result, Na is uniformly attached to the amorphous silicon dioxide powder as ions. Next, after stirring this mixed system for about 60 minutes, solid-liquid separation was performed using a filter press, and further drying treatment was performed to obtain a silicon dioxide powder containing Na components in a weight ratio.
A powder with about 1000 ppm of physical adsorption or chemical bonding was obtained. The obtained powder has a size of approximately 50 μm to 500 μm.
m, and the raw material powder, amorphous silicon dioxide powder, was a fine powder of about 0.02 μm.
It is agglomerated and granulated to an appropriate diameter.

このようにして得られた二酸化珪素粉、内径
120mm、高さ150mmのムライト質でなる円筒容器に
充填した後、電気炉で1100℃まで加熱した。これ
により76mmφ×91mmのクリストバライト結晶相を
持つ円柱状の焼結体が得られたので、これを500
℃以上に保持して真空加熱炉に搬入し、0.5mb以
下の真空下で1750℃まで加熱してガラス化した。
この時の昇温温バランンスとしては1600℃まで3
時間、1750℃で1時間であり、これにより80mmφ
×45mmで重量約500gの透明な石英ガラスを得た。
Silicon dioxide powder thus obtained, inner diameter
After filling a cylindrical container made of mullite with a diameter of 120 mm and a height of 150 mm, the mixture was heated to 1100°C in an electric furnace. As a result, a cylindrical sintered body with a cristobalite crystal phase of 76 mmφ x 91 mm was obtained.
The material was maintained at a temperature above 10°C and transported into a vacuum heating furnace, and heated to 1750°C under a vacuum of 0.5 mb or less to vitrify it.
At this time, the temperature increase balance is 3 to 1600℃.
The time is 1 hour at 1750℃, which results in 80mmφ
A transparent quartz glass with a size of 45 mm and a weight of about 500 g was obtained.

本発明はかかる知見に基づくものであるが、結
晶化に必要なアルカリ金属成分としては前記焼結
体の融点以下で分解脱離するものであれば、任意
ではあるが、本発明者等の知見によるとNaを使
用することが好ましい。又含有量は結晶化に必要
な量であり、100ppm以上2000ppm程度で満足で
きる効果が得られる。なおアルカリ金属成分は均
一な状態で非晶質二酸化珪素粉に存在することが
要求され、例えば適量の水にNa成分を加えたも
のに非晶質二酸化珪素粉を混合した後脱水し乾燥
することにより、粉体にNa成分を所望量均一に
付着させることができる。
The present invention is based on such knowledge, but the alkali metal component necessary for crystallization may be any one that decomposes and leaves below the melting point of the sintered body, but is based on the knowledge of the present inventors. According to , it is preferable to use Na. Further, the content is the amount necessary for crystallization, and a satisfactory effect can be obtained with a content of 100 ppm or more and about 2000 ppm. Note that the alkali metal component is required to be present in the amorphous silicon dioxide powder in a uniform state; for example, the amorphous silicon dioxide powder is mixed with an appropriate amount of water to which a Na component is added, then dehydrated and dried. Accordingly, the desired amount of Na component can be uniformly adhered to the powder.

〔発明の効果〕〔Effect of the invention〕

本発明に係る透明石英ガラス用材料は、以上の
説明から明らかなように非晶質二酸化珪素粉にア
ルカリ金属成分を含有せしめたものであるから、
仮焼により結晶化した焼結体を得るに容易であ
る。即ちアルカリ金属を含まない非晶質二酸化珪
素により結晶化した焼結体を得ようとした場合
は、1500℃以上に加熱しても容易に結晶化せずし
かも結晶化前の加熱温度で焼結化するため、得ら
れた焼結体は非多孔質のものでありガラス化工程
における不純物除去を困難にする。しかるに本発
明による材料使用した場合は、1100℃程度の加熱
温度で結晶化した焼結体が得られるので生産性が
高く、かつこれを真空溶融によりガラス化した場
合不純物の除去が容易になり純度のよい透明石英
ガラスが得られる。
As is clear from the above description, the transparent quartz glass material according to the present invention is a material in which amorphous silicon dioxide powder contains an alkali metal component.
It is easy to obtain a crystallized sintered body by calcining. In other words, when trying to obtain a crystallized sintered body using amorphous silicon dioxide that does not contain alkali metals, it does not crystallize easily even when heated to 1500°C or higher, and it is sintered at a heating temperature before crystallization. Because of this, the obtained sintered body is non-porous, making it difficult to remove impurities during the vitrification process. However, when the material according to the present invention is used, productivity is high because a sintered body that is crystallized at a heating temperature of about 1100°C can be obtained, and when it is vitrified by vacuum melting, impurities can be easily removed and purity can be improved. A transparent quartz glass with good quality can be obtained.

Claims (1)

【特許請求の範囲】[Claims] 1 非晶質二酸化珪素粉を仮焼して焼結体を得、
ついでこれを真空下溶融してガラス化させる透明
石英ガラス製造法に使用される材料であつて、前
記非晶質二酸化珪素粉を、該二酸化珪素が加熱に
より結晶化して焼結体化するに必要なアルカリ金
属成分の含有溶液中に混合せしめて、該アルカリ
金属成分を前記非晶質二酸化珪素粉に付着せしめ
てなることを特徴とする透明石英ガラス用材料。
1 Calcinate amorphous silicon dioxide powder to obtain a sintered body,
A material used in a transparent quartz glass manufacturing method in which the amorphous silicon dioxide powder is then melted under vacuum and vitrified, and is necessary for the amorphous silicon dioxide powder to be crystallized and sintered by heating. 1. A material for transparent quartz glass, characterized in that the amorphous silicon dioxide powder is mixed with a solution containing an alkali metal component to cause the amorphous silicon dioxide powder to adhere to the amorphous silicon dioxide powder.
JP18158984A 1984-08-30 1984-08-30 Material for transparent quartz glass Granted JPS6158832A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP18158984A JPS6158832A (en) 1984-08-30 1984-08-30 Material for transparent quartz glass

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP18158984A JPS6158832A (en) 1984-08-30 1984-08-30 Material for transparent quartz glass

Publications (2)

Publication Number Publication Date
JPS6158832A JPS6158832A (en) 1986-03-26
JPH0451498B2 true JPH0451498B2 (en) 1992-08-19

Family

ID=16103449

Family Applications (1)

Application Number Title Priority Date Filing Date
JP18158984A Granted JPS6158832A (en) 1984-08-30 1984-08-30 Material for transparent quartz glass

Country Status (1)

Country Link
JP (1) JPS6158832A (en)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE3773306D1 (en) * 1986-02-28 1991-10-31 Nippon Oxygen Co Ltd METHOD FOR PRODUCING GLASS.
JPS62212234A (en) * 1986-02-28 1987-09-18 Nippon Sanso Kk Production of glass
DE3771963D1 (en) * 1986-02-28 1991-09-12 Nippon Oxygen Co Ltd METHOD FOR PRODUCING GLASS.

Also Published As

Publication number Publication date
JPS6158832A (en) 1986-03-26

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