JPH02188431A - Production of quartz glass - Google Patents
Production of quartz glassInfo
- Publication number
- JPH02188431A JPH02188431A JP739589A JP739589A JPH02188431A JP H02188431 A JPH02188431 A JP H02188431A JP 739589 A JP739589 A JP 739589A JP 739589 A JP739589 A JP 739589A JP H02188431 A JPH02188431 A JP H02188431A
- Authority
- JP
- Japan
- Prior art keywords
- sol
- gel
- quartz glass
- bubbles
- 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
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 238000004519 manufacturing process Methods 0.000 title claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 8
- 239000011521 glass Substances 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 abstract description 18
- 235000019441 ethanol Nutrition 0.000 abstract description 13
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 11
- 239000000203 mixture Substances 0.000 abstract description 8
- 238000005245 sintering Methods 0.000 abstract description 8
- 239000013307 optical fiber Substances 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 239000006260 foam Substances 0.000 abstract 1
- 238000003980 solgel method Methods 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- BDERNNFJNOPAEC-UHFFFAOYSA-N n-propyl alcohol Natural products CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 229910002020 Aerosil® OX 50 Inorganic materials 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000001879 gelation Methods 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 1
- 150000004703 alkoxides Chemical class 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 238000001179 sorption measurement 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
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/12—Other methods of shaping glass by liquid-phase reaction processes
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/012—Manufacture of preforms for drawing fibres or filaments
- C03B37/014—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD]
- C03B37/016—Manufacture of preforms for drawing fibres or filaments made entirely or partially by chemical means, e.g. vapour phase deposition of bulk porous glass either by outside vapour deposition [OVD], or by outside vapour phase oxidation [OVPO] or by vapour axial deposition [VAD] by a liquid phase reaction process, e.g. through a gel phase
Abstract
Description
【発明の詳細な説明】
［産業上の利用分野Ｊ
本発明は、光フアイバ用として使用可能な気泡混入の極
めて少い石英ガラスをゾル−ゲル法を用いて安価に製造
する石英ガラスの製造方法に関するものである。[Detailed Description of the Invention] [Industrial Field of Application J] The present invention provides a method for producing quartz glass that can be used for optical fibers and that can be produced at low cost by using a sol-gel method and has very little air bubbles. It is related to.
［従来の技術］
光ファイバの素材とするための石英ガラスは高純度であ
ることのほかに気泡や異物の混入のないことが要求され
る。[Prior Art] Silica glass used as a material for optical fibers is required not only to have high purity but also to be free from air bubbles and foreign matter.
このような石英ガラスの製造方法としては、今日法〈実
施されている火炎加水分解法をはじめこれまでにもさま
ざまな方法が提案されてきた。Various methods have been proposed for producing such quartz glass, including the flame hydrolysis method currently in use.
ゾル−ゲル法もそのような製造方法の一つであり、具体
的には図に示すような工程に従い光フアイバ用母材ガラ
スを製造するものである。The sol-gel method is one of such manufacturing methods, and specifically, a matrix glass for optical fibers is manufactured according to the steps shown in the figure.
すなわち、図（ａ）に示すように容器２中において原材
料としてのシリカ微粉末を水やアルコールによって溶か
しコロイド状のゾル１ａとなし、これを図（ｂ）のよう
に密封蓋４を有する密閉容器３中に封入し加水分解させ
てゲル１ｂとし、その後回（Ｃ）のように密封蓋４に穴
４ａをＵｎけるなどして前記ゲル１ｂを容器３中で乾燥
させて多孔質のドライゲルＩＣとする。このドライゲル
ＩＣを図（ｄ）のように電気炉５中において加熱焼結さ
せると透明な高純度石英ガラス１ｄとなる。That is, as shown in Figure (a), fine silica powder as a raw material is dissolved in water or alcohol in a container 2 to form a colloidal sol 1a, and this is then placed in a closed container with a sealed lid 4 as shown in Figure (b). After that, as in step (C), holes 4a are made in the sealing lid 4, and the gel 1b is dried in the container 3 to form a porous dry gel IC. do. When this dry gel IC is heated and sintered in an electric furnace 5 as shown in Figure (d), a transparent high-purity quartz glass 1d is obtained.
このゾル−ゲル法は、上述のように中間工程で多孔質の
ドライゲルＩＣが中間製品として形成されるため、その
多孔質物質としての特色を生かし、例えば耐放射線性に
優れたガラス素材とするためのＯＨ基の吸着に利用する
など、ガラス素材の特性の改良を行なう上で便利である
という利点があり、そのよう意味合いからも注目を集め
ている製造方法の一つである。In this sol-gel method, as mentioned above, a porous dry gel IC is formed as an intermediate product in the intermediate process, so by taking advantage of its characteristics as a porous material, it is possible to make, for example, a glass material with excellent radiation resistance. It has the advantage of being convenient for improving the properties of glass materials, such as by using it for adsorption of OH groups, and for this reason, it is one of the manufacturing methods that is attracting attention.
［発明が解決しようとする課題フ
シル−ゲル法は、上記のような利点のほかに、高純度化
も比較的容易である上、ドライゲル製造中や焼結中に割
れやクラックが生じにくいために、比較的マスの大きな
石英ガラスを入手し易いという利点らある。[Problems to be Solved by the Invention] In addition to the above-mentioned advantages, the fusil-gel method has the following advantages: it is relatively easy to achieve high purity, and cracks are less likely to occur during dry gel production and sintering. Another advantage is that it is easy to obtain quartz glass with a relatively large mass.
しかし、この方法は、ゾル中の気泡の切れが悪く、ドラ
イゲル中に気泡が残り易く、結果的に焼結した石英ガラ
ス中に多数の気泡が残存し易くなるという欠点かあり、
これの改善が強く望まれている。However, this method has the disadvantage that the air bubbles in the sol are difficult to cut, and air bubbles tend to remain in the dry gel, resulting in a large number of air bubbles remaining in the sintered quartz glass.
Improvement of this is strongly desired.
本発明の目的は、上記したような従来技術の問題点を解
消し、内部に気泡の残存しない石英ガラスをゾル−ゲル
法により安価に製造する方法を提供しようとするもので
ある。SUMMARY OF THE INVENTION An object of the present invention is to solve the above-mentioned problems of the prior art and to provide a method for manufacturing quartz glass without any air bubbles at a low cost by a sol-gel method.
し課題を解決するための手段］
本発明は、ゾル−ゲル法により石英ガラスを製造するに
際し、微粉末シリカ１モルに対し低級アルコール１〜５
モルおよび水１〜４モルを加えゾル化することを特徴と
するものである。Means for Solving the Problems] The present invention provides that when producing quartz glass by the sol-gel method, 1 to 5 lower alcohols are added to 1 mole of fine powder silica.
It is characterized by adding 1 to 4 moles of water and 1 to 4 moles of water to form a sol.
本発明において使用する微粉末シリカとしては、ＳｉＣ
，ｌ！ａを酸水素炎バーナで加水分解して得られるもの
に限らず、金属アルコキシドを加水分解して得られたシ
リカ微粒子やケイ酸ソーダを原料とする湿式法によれ得
られた微粉末シリカなども使用できる。The fine powder silica used in the present invention includes SiC
,l! Not only those obtained by hydrolyzing a with an oxyhydrogen flame burner, but also fine silica particles obtained by hydrolyzing metal alkoxides and fine powdered silica obtained by a wet method using sodium silicate as a raw material. Can be used.
低級アルコールとしては、メチルアルコール、エチルア
ルコール、プロピルアルコール、ブチルアルコールが好
ましい、これ以上炭素数の大きいアルコールを用いると
、ゾル液の粘度が高くなり、ゾル液中の泡切れが悪くな
り、好ましくない。また、この添加量は１〜５モルの範
囲が好ましく、１モル以下ではゾル液中の泡切れが悪く
なり、５モル以上になるとゲル化しない。As the lower alcohol, methyl alcohol, ethyl alcohol, propyl alcohol, and butyl alcohol are preferable. If an alcohol with a larger number of carbon atoms is used, the viscosity of the sol will increase, making it difficult to remove bubbles in the sol, which is not preferable. . Further, the amount added is preferably in the range of 1 to 5 moles; if it is less than 1 mole, it becomes difficult to remove bubbles in the sol solution, and if it is more than 5 moles, it will not gel.
水の添加量は１〜４モルの範囲が好ましく、１モル以下
ではゲル化しなくなり、４モル以上になると泡切れが悪
くなる。The amount of water added is preferably in the range of 1 to 4 moles; if it is less than 1 mole, gelation will not occur, and if it is more than 4 moles, foaming will be difficult.
［作用］
本発明か規定した範囲の低級アルコールおよび水により
ゾル化すると、ゾル中の泡切れが格段によくなり、ゾル
−ゲル法の難点であった気泡の残存が解消され、他の確
立された製造方法によったと同様の気泡のない高純度石
英ガラスを製造することかできる。[Function] When the present invention is made into a sol using a lower alcohol and water within the specified range, the bubble breakage in the sol becomes much better, and the remaining bubbles, which were a drawback of the sol-gel method, are eliminated. It is possible to produce high-purity quartz glass without bubbles similar to that produced by the production method described above.
［実施例］ 以下に、本発明について実施ρ１を参照し説明する。[Example] The present invention will be described below with reference to implementation ρ1.
実施例１
商品名Ａｅａｒｏｓｉｌ ｏｘ５０ ６０ｇ （１モル
）にエチルアルコール９２ｇ （２モル）と水３６ｇ（
２モル）を加え、激しく撹拌してゾル化した。Example 1 60 g (1 mol) of Aerosil ox50 (trade name), 92 g (2 mol) of ethyl alcohol and 36 g of water (
2 mol) was added thereto and stirred vigorously to form a sol.
このゾルをフッ素樹脂製の円筒型容器（内径２０ ｒｍ
Ｘ高さ２００ｎｎ）に注入し、密閉して室温に放置し
たところ１７時間後にゲル化した。これをさらに５０℃
で一週間熟成した後、密封蓋に直径０．５間の穴を１個
開け、６０℃で１日、８０℃て１日、１００℃で１日、
１２０℃で１日の順に加熱しドライゲルを作製した。こ
のドライゲルを焼結炉に入れ１２５０℃で焼結してガラ
ス化し、直径的１ 、Ｏｒ＋ｏｎ、長さ約１００間の石
英ガラスロッドを得た。得られた石英ガラスの近赤外吸
収スペクトルを測定した結果、市販の石英ガラスと同様
のピークが見られた。また、比重は２．２３、ビッカー
ス硬さは８１５ｋｇ／止２であり、これも市販のガラス
とほぼ７致しな、さらに、Ｈｅ−Ｎａレーザーで散乱の
様子を調べたところ、小さな散乱が数個見られたか、気
泡による大きな散乱は見られなかった。This sol was poured into a cylindrical container made of fluororesin (inner diameter 20 rm).
When the mixture was injected into a tube (height: 200 nn), sealed and left at room temperature, it gelled after 17 hours. This is further heated to 50℃
After aging for one week, one hole with a diameter of 0.5 mm was made in the sealed lid, and the temperature was 1 day at 60 °C, 1 day at 80 °C, and 1 day at 100 °C.
A dry gel was prepared by heating at 120° C. for one day. This dry gel was placed in a sintering furnace and sintered at 1250° C. to vitrify it to obtain a quartz glass rod with a diameter of 1 mm, Or+on, and a length of about 100 mm. As a result of measuring the near-infrared absorption spectrum of the obtained quartz glass, peaks similar to those of commercially available quartz glass were observed. In addition, the specific gravity is 2.23 and the Vickers hardness is 815 kg/2, which is almost the same as commercially available glass.Furthermore, when we investigated the state of scattering with a He-Na laser, we found several small scattering particles. No significant scattering due to air bubbles was observed.
実施例２
商品名Ｃａｂ−０−３ｉｔ Ｍ５ ６０ｇ ＜１モル
）にｎ−プロピルアルコール９０ｇ（１，５モル）と水
４５ｇ （２，５モル）を加えて、激しく撹拌してゾル
化した。このゾルをフッ素樹脂製の円筒型容器（内径２
０＋ｗｍＸ高さ２００ｆｆｉ目）に注入し密閉して室温
に放置しなところ２１時間後にゲル化した。さらに５０
℃で一週間熟成した後、密封若に直径０．５＋＋ｍの穴
を１個開け１２０℃まで１時間に１℃の速度で昇温して
徐々に乾燥した。Example 2 90 g (1.5 mol) of n-propyl alcohol and 45 g (2.5 mol) of water were added to Cab-0-3it (trade name: M5, 60 g <1 mol) and stirred vigorously to form a sol. This sol was poured into a cylindrical container made of fluororesin (inner diameter 2
When the mixture was injected into a container (0+wm x height 200ffi), sealed and left at room temperature, it turned into a gel after 21 hours. 50 more
After aging for one week at °C, one hole with a diameter of 0.5++ m was made in the sealed container, and the temperature was raised to 120 °C at a rate of 1 °C per hour to gradually dry.
得られたドライゲルを焼結炉に入れ１２５０℃で焼結し
てガラス化し、直径約１０ｍ＋、長さ約１００薗の石英
ガラスロッドを得た。得られた石英ガラスの近赤外吸収
スペクトルを測定した結果、市販の石英ガラスと同様の
ピークが見られた。また、比重は２．１９、ビッカース
硬さは８０２ｋｇ／ａｍ”であり、これも市販の石英ガ
ラスとほぼ一致した。さらにＨｅ−Ｎｅレーザーで散乱
の様子をユ１べたところ、小さな散乱が数個見られたが
、気泡による大きな散乱は見られなかった。The obtained dry gel was placed in a sintering furnace and sintered at 1250° C. to vitrify it to obtain a quartz glass rod with a diameter of about 10 m+ and a length of about 100 mm. As a result of measuring the near-infrared absorption spectrum of the obtained quartz glass, peaks similar to those of commercially available quartz glass were observed. In addition, the specific gravity was 2.19 and the Vickers hardness was 802 kg/am'', which was almost the same as that of commercially available quartz glass.Furthermore, when we examined the state of scattering with a He-Ne laser, we found several small scattering particles. However, no significant scattering due to air bubbles was observed.
実施例３
Ａｅａｒｏｓ＋ｌ ｏｘ５０ ６０ｇ （１モル）にメ
タノール９６ｇ （３モル）と水２７ｇ（１，５モル）
を加え、激しく撹拌してゾル化した。このゾルをフッ素
樹脂製の円筒型容器（内径２０ｏ＋ｍＸ高さ２００ｍ＋
ｎ）に注入し密閉して室温に放置しなところ１５時間後
にゲル化した。さらにこれを５０℃で一週間熟成した後
、密封蓋に直径０．５市の穴を１個開け１２０℃まで１
時間に１℃の速度で昇温して徐々に乾燥してドライゲル
を作製しな、このドライゲルを焼結炉に入れ１２５０℃
で焼結してガラス化し、直径約１０關、長さ約１００Ｉ
ＩＩＩの石英ガラスロッドを得な、得られた石英ガラス
の近赤外吸収スペクトルを測定した結果、市販の石英ガ
ラスと同様のピークが見られた。また、比重は２，１８
、ビッカース硬さは８１３ ｋｉｒ／ Ｉｌ＋ｎ２であ
り、これも市販の石英ガラスとほぼ一致した。Example 3 60 g (1 mol) of Aeros+l ox50, 96 g (3 mol) of methanol and 27 g (1.5 mol) of water
was added and stirred vigorously to form a sol. This sol was poured into a cylindrical container made of fluororesin (inner diameter 20o+m x height 200m+
When the mixture was injected into the container, sealed, and left at room temperature, it turned into a gel after 15 hours. Furthermore, after aging this at 50℃ for one week, one hole with a diameter of 0.5 mm was made in the sealed lid and the temperature was raised to 120℃.
The temperature is increased at a rate of 1°C per hour to gradually dry the dry gel, and this dry gel is placed in a sintering furnace at 1250°C.
It is sintered and vitrified, with a diameter of about 10 mm and a length of about 100 mm.
The quartz glass rod III was obtained, and the near-infrared absorption spectrum of the obtained quartz glass was measured, and as a result, peaks similar to those of commercially available quartz glass were observed. Also, the specific gravity is 2.18
The Vickers hardness was 813 kir/Il+n2, which also almost matched that of commercially available quartz glass.
さらにＨｅ−Ｎｅレーザーで散乱の様子を調べたところ
、小さな散乱が数個みられたが、気泡による大きな散乱
は見られなかった。Furthermore, when the state of scattering was investigated using a He-Ne laser, several small scatterings were observed, but no large scattering due to bubbles was observed.
比較例Ｉ
Ａｅａｒｏｓｉｌ ｏｘ５０ ６０ｇ （１モル）にメ
タノール２９ｇ （０，９モル）と水５４ｇ （３モル
）を加えて、激しく撹拌してゾル化しな、このゾルをフ
ッ素樹脂製の円筒型容器（内径２０關×高さ２００ ＋
ｕ＋ ）に注入し密閉して室温に放置したところ１８時
間後にゲル化した。Comparative Example I To 60 g (1 mol) of Aerosil ox50, 29 g (0.9 mol) of methanol and 54 g (3 mol) of water were added and stirred vigorously to form a sol. 20 cm x height 200 +
When the mixture was injected into a container (u+), sealed, and left at room temperature, it turned into a gel after 18 hours.
しかし、この時ゾル中の泡切れが悪く、気泡がたくさん
残った。このゲルを５０℃で一週間熟成した後、密封蓋
に直径０．５＋＋＋＋ｎの穴を１個開け１２０℃まで１
時間に１°Ｃの速度で昇温して徐々に乾燥した。得られ
たドライゲルを焼結炉に入れ１２５０°Ｃで焼結してガ
ラス化し、直径約１０＋ｕ＋、長さ約１０（ｌｎｍの石
英ガラスロッドを得た。しかし、Ｈｅ−Ｎｅレーザーで
散乱の様子を調べなところ、気泡による大きな散乱が多
数見られた。However, at this time, the bubbles in the sol did not break easily, and many bubbles remained. After aging this gel at 50℃ for one week, make one hole with a diameter of 0.5++++n in the sealed lid and heat it to 120℃.
The temperature was increased at a rate of 1°C per hour to gradually dry the film. The obtained dry gel was placed in a sintering furnace and sintered at 1250°C to vitrify it to obtain a silica glass rod with a diameter of about 10+u+ and a length of about 10 (lnm). Upon closer inspection, we found that there was a lot of large scattering caused by air bubbles.
比較例２
Ｃａｂ−０−３ｉｌ Ｍ５ ６０ｇ （１モル）にエ
タノール２３５ｇ （５，１モル）と水２７ｇ（１，５
モル２を加え、激しく撹拌してゾル化した。このゾルを
フッ素樹脂製の円筒型容器（内径２０ ｎｍ Ｘ高さ２
００ ｍｎ ）に注入し密閉して室温に放置したが、−
ａ間装置してもゲル化しなかった。Comparative Example 2 60 g (1 mol) of Cab-0-3il M5, 235 g (5.1 mol) of ethanol and 27 g (1,5 mol) of water
2 moles were added and stirred vigorously to form a sol. This sol was placed in a cylindrical container made of fluororesin (inner diameter 20 nm x height 2
00 mn), sealed and left at room temperature, but -
It did not gel even after being exposed to the apparatus for a period of a day.
比較例３
Ａｅａｒｏｓｉｌ ｏｘ５０ ６０ｇ （１モル）にｎ
−プロピルアルコール１２０ｇ＜２モル）と水１６ｇ（
０，９モル）を加え、激しく撹拌してゾル化した。この
ゾルをフッ素樹脂製の円筒型容器（内径２０市×高さ２
００ ＋＋ｎ＋ ）に注入し密閉して室温に放置したが
、−週間放置してもゲル化しなかった。Comparative Example 3 Aerosil ox50 60g (1 mol)
- 120 g of propyl alcohol <2 mol) and 16 g of water (
0.9 mol) was added and stirred vigorously to form a sol. This sol was poured into a cylindrical container made of fluororesin (inner diameter 20mm x height 2mm).
00++n+), the mixture was sealed and left at room temperature, but gelation did not occur even after being left for -week.
比較例４
Ｃａｂ−ｏ−８ｉｔ Ｍ５ ６０ （１モル）にエタ
ノール４６ｇ（１モル）と水７４ｇ（４，１モル）を加
え、激しく撹拌してゾル化した。このゾルをフッ素樹脂
製の円筒型容８（内径２０關×高さ２００ ｒｍ ）に
注入し、密閉して室温に放置しなところ２６時間後にゲ
ル化した。Comparative Example 4 46 g (1 mol) of ethanol and 74 g (4.1 mol) of water were added to Cab-o-8it M5 60 (1 mol), and the mixture was vigorously stirred to form a sol. This sol was poured into a cylindrical volume 8 (inner diameter 20 mm x height 200 rm) made of fluororesin, sealed and left at room temperature, where it gelled after 26 hours.
しかし、この時のゾル中の泡切れが悪く、気泡がたくさ
ん残った。このゲルを５０℃で一週間熟成した後、密封
蓋に直径０．５＋ｍの穴を１個開け１２０℃まで１時間
に１℃の速度で昇温して徐々に乾煉した。得られたドラ
イゲルを焼結炉に入れ１２５０℃で焼結してガラス化し
、直径的１０１ｗ１ｌ、長さ約１１００ｎの石英カラス
ロッドを得た。However, at this time, the bubbles in the sol were not easily removed, and many bubbles remained. After this gel was aged at 50°C for one week, one hole with a diameter of 0.5+ m was made in the sealed lid and the temperature was raised to 120°C at a rate of 1°C per hour, and the gel was gradually fermented. The obtained dry gel was placed in a sintering furnace and sintered at 1250° C. to vitrify it to obtain a quartz glass rod having a diameter of 101 w1 l and a length of about 1100 n.
Ｈｅ−Ｎｅレーザーで散乱の様子を調べなところ、気泡
による大きな散乱が多数見られた。When examining the state of scattering using a He-Ne laser, many large scatterings due to bubbles were observed.
１Ｃニドライゲル、 １ｄ：焼結石英ガラス、 ５：電気炉。1C Nidrigel, 1d: Sintered quartz glass, 5: Electric furnace.
［発明の効果］
以上の通り、本発明に係る製造方法によれば、加える水
と低級アルコールの最′ｉＭ範囲が見出されたことでゾ
ル−ゲル法を用い市販の高純度石英ガラスと同等の気泡
のない品質良好な石英ガラスを安価な製造コストで入手
できるものであり、アルコールや水は高純度のものが容
易に得られることを考慮すれば、微粉末シリカとして高
純度のものを用いることにより光フアイバ用に使用でき
る高純度石英ガラスを製造することを可能ならしめる。[Effect of the invention] As described above, according to the manufacturing method of the present invention, the maximum iM range of water and lower alcohol to be added has been found, and it is equivalent to commercially available high-purity quartz glass using the sol-gel method. Considering that high-quality silica glass without bubbles can be obtained at a low manufacturing cost, and high-purity alcohol and water can be easily obtained, high-purity fine powder silica is used. This makes it possible to produce high-purity quartz glass that can be used for optical fibers.
図は、ゾル−ゲル法の工程を示す説明図である。 ｌａ：ゾル、 ■ｂニゲル、 The figure is an explanatory diagram showing the steps of the sol-gel method. la: sol, ■b Nigel,
Claims (1)
モルおよび水１〜４モルを加えて撹拌混合してゾル化し
、これを経時的にゲル化した後乾燥してドライゲルとし
、その後加熱焼結して透明ガラスとする石英ガラスの製
造方法。(1) 1 to 5 lower alcohols per 1 mole of fine powder silica
A method for producing quartz glass, in which 1 to 4 moles of water are added and stirred to form a sol, the gel is gelated over time and then dried to form a dry gel, and then heated and sintered to form transparent glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP739589A JPH02188431A (en) | 1989-01-13 | 1989-01-13 | Production of quartz glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP739589A JPH02188431A (en) | 1989-01-13 | 1989-01-13 | Production of quartz glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH02188431A true JPH02188431A (en) | 1990-07-24 |
Family
ID=11664719
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP739589A Pending JPH02188431A (en) | 1989-01-13 | 1989-01-13 | Production of quartz glass |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH02188431A (en) |
-
1989
- 1989-01-13 JP JP739589A patent/JPH02188431A/en active Pending
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