JPH03122026A - Production of oxynitride glass clad optical fiber preform - Google Patents
Production of oxynitride glass clad optical fiber preformInfo
- Publication number
- JPH03122026A JPH03122026A JP1257951A JP25795189A JPH03122026A JP H03122026 A JPH03122026 A JP H03122026A JP 1257951 A JP1257951 A JP 1257951A JP 25795189 A JP25795189 A JP 25795189A JP H03122026 A JPH03122026 A JP H03122026A
- Authority
- JP
- Japan
- Prior art keywords
- sol
- preform
- porous glass
- glass
- 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
- 239000011521 glass Substances 0.000 title claims abstract description 21
- 239000013307 optical fiber Substances 0.000 title claims abstract description 7
- 238000004519 manufacturing process Methods 0.000 title claims description 4
- 239000005373 porous glass Substances 0.000 claims abstract description 19
- 150000004703 alkoxides Chemical class 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000012298 atmosphere Substances 0.000 claims abstract description 6
- 230000005540 biological transmission Effects 0.000 claims abstract description 5
- 238000005253 cladding Methods 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 4
- 230000003287 optical effect Effects 0.000 claims description 4
- 239000007789 gas Substances 0.000 claims description 3
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 claims description 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000012239 silicon dioxide Nutrition 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 238000000034 method Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000006073 displacement reaction Methods 0.000 description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 2
- 238000004017 vitrification Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- -1 propatool Chemical compound 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- 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]
- C03B37/01413—Reactant delivery systems
- C03B37/01433—Reactant delivery systems for delivering and depositing additional reactants as liquids or solutions, e.g. for solution doping of the porous glass preform
-
- 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]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/02—Pure silica glass, e.g. pure fused quartz
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/06—Doped silica-based glasses
- C03B2201/20—Doped silica-based glasses doped with non-metals other than boron or fluorine
- C03B2201/24—Doped silica-based glasses doped with non-metals other than boron or fluorine doped with nitrogen, e.g. silicon oxy-nitride glasses
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Optical Fibers, Optical Fiber Cores, And Optical Fiber Bundles (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は、強度特性、耐水特性に優れたオキシナイト
ライドガラスクラッド光ファイバ母材の製造方法に関す
るもので、コア用ロッドとクラッドとの密着性に優れ、
かつクラッドガラス内にＮを均一に含ませ得る方法を提
供する。Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for manufacturing an oxynitride glass clad optical fiber preform with excellent strength and water resistance properties, and relates to a method for manufacturing an oxynitride glass clad optical fiber preform with excellent strength and water resistance. excellent in sex,
Moreover, a method is provided in which N can be uniformly included in the clad glass.
（従来の技術）
従来のオキシナイトライドガラスクラッド光ファイバ母
材の製造方法は、予めＳｉのアルコキシドを出発原料と
し、これを水と反応させてゾルを作り、この中に別途用
意した光伝送用のコアとなるロッドを浸漬し、次にこの
ロッドの周りのゾルを乾燥させてゲルとし、このゲルを
ＮＨ，を含む雰囲気で加熱処理してオキシナイトライド
化し、最後に高温で処理して透明ガラス化するという方
法であった。(Prior art) The conventional method for producing an oxynitride glass-clad optical fiber base material uses Si alkoxide as a starting material and reacts it with water to create a sol, in which a separately prepared optical fiber is prepared. The core rod is immersed in the sol, the sol around the rod is dried to form a gel, this gel is heated in an atmosphere containing NH, to form oxynitride, and finally it is processed at high temperature to make it transparent. The method was to make it vitrified.
（発明が解決しようとする課題）
しかしながら、この方法では出発ロッドとゲルガラスと
の密着が弱く、加熱処理に伴うゲルガラスの収縮時に亀
裂や界面でのズレ、泡等が生して目的とする高強度ガラ
スクランドを得ることが困難であった。(Problems to be Solved by the Invention) However, in this method, the adhesion between the starting rod and the gel glass is weak, and cracks, displacement at the interface, bubbles, etc. occur when the gel glass shrinks due to heat treatment, resulting in the creation of high strength It was difficult to obtain glass crud.
（課題を解決するだめの手段）
この発明は、上記の問題の解決を図ったもので、その特
徴とするところは、Ｓｉのアルコキシドに、少なくとも
水を加えてゾルとなし、このゾル内に別途用意した光伝
送用コアガラスロッドの周りにクラッド用の５ｉＯｚか
らなる多孔質ガラス体が形成されてなるプリフォームを
浸漬して前記多孔質ガラス体内にゾルを含浸させ、つい
でプリフォームを取出して乾燥させて前記多孔質ガラス
体内のゾルをゲルとなし、引き続いてこのプリフォーム
を加熱炉に入れて、窒素含有ガスを含む雰囲気内で加熱
処理して前記ゲルが含浸された多孔質ガラス体を透明ガ
ラス化することにある。(Means for Solving the Problem) This invention is an attempt to solve the above problem, and is characterized by adding at least water to Si alkoxide to form a sol, and adding a separate layer to the sol. A preform in which a porous glass body made of 5 iOz for cladding is formed around a prepared optical transmission core glass rod is immersed to impregnate the sol into the porous glass body, and then the preform is taken out and dried. The sol in the porous glass body is turned into a gel, and then this preform is placed in a heating furnace and heated in an atmosphere containing nitrogen gas to make the porous glass body impregnated with the gel transparent. It consists in vitrification.
Ｓｉのアルコキシドとしては、テトラエトキシシラン５
ｉ（ＯＣ２Ｉ（ｓ）４．メチルトリエトキシシランＣＨ
３５ｉ（ＯＣ２ｔ１５） ３．テトラメトキンシランＳ
ｉ （ＯＣＩＩ ：ｌ） −テトラプロポキシシラン
５ｉ（ＯＣ＋１Ｉｔ） ４．テトラブトキシウシランＳ
ｉ （ＱＣ＜ｔｌ、）４．があげられる。As the Si alkoxide, tetraethoxysilane 5
i(OC2I(s)4. Methyltriethoxysilane CH
35i (OC2t15) 3. Tetramethquinsilane S
i (OCII:l)-tetrapropoxysilane 5i (OC+1It) 4. Tetrabutoxysilan S
i (QC<tl,)4. can be given.
また、ゾルとする際に水に加えて反応速度制御のために
他の溶媒、例えばメタノール、エタノール、プロパツー
ル、ブタノールなどのアルコールを加えたり、塩酸、水
酸化アンモニウムなどを加えても良い。Further, when forming a sol, other solvents such as alcohols such as methanol, ethanol, propatool, butanol, hydrochloric acid, ammonium hydroxide, etc. may be added to control the reaction rate in addition to water.
（作 用）
光伝送用のコアロッドの周りにクラッドとなるＳｉＯ□
からなる多孔質ガラス体が形成されたロッドを用意し、
これをＳｉのアルコキシドからなるツルの中に浸して多
孔質ガラス内にゾルを含浸させるので、コアロッドとク
ラッドとの間の密着性は十分であり、またゾルは多孔質
ガラス内に均一に入るので、これをＮと置換させてやる
ことで５ｉ０２内にＮが均一に含まれたクラッドとする
ことができる。(Function) SiO□ forms a cladding around the core rod for optical transmission.
Prepare a rod in which a porous glass body consisting of
This is immersed in a vine made of Si alkoxide to impregnate the sol into the porous glass, so the adhesion between the core rod and the cladding is sufficient, and the sol enters the porous glass uniformly. By replacing this with N, it is possible to obtain a cladding in which N is evenly contained in 5i02.
（実施例）
直径１５陥、長さ４００ ｍｍのＧｅ０ｚ Ｈ５ｉＯｚ
ガラスロンドの周りに、外付は法によってＳｉＯ□から
なる多孔質ガラスを堆積させて外径１００ ｍｍ、長さ
５００Ｍのプリフォームとした。そのときのトーチに送
ったガスの種類および供給量は以下の表１のとおりであ
った。(Example) Ge0z H5iOz with 15 holes in diameter and 400 mm in length
Around the glass rond, porous glass made of SiO□ was deposited by an external method to form a preform with an outer diameter of 100 mm and a length of 500 M. The types and amounts of gases sent to the torch at that time were as shown in Table 1 below.
表１
このプリフォームを電気炉に入れ、１０００〜２０００
゛Ｃに加熱して収縮させ、カサ密度０．５ｇ／ｃｍとし
た。一方、Ｓｉのアルコキシドの中からメチルトリエト
キシシランＣＨ３５ｉ（ＯＣｄｌｓ）４を選んでこれを
表２に示す材料とともに攪拌してゾルを作成した。Table 1 This preform was placed in an electric furnace and
It was heated to ゛C to shrink to a bulk density of 0.5 g/cm. On the other hand, methyltriethoxysilane CH35i (OCdls)4 was selected from Si alkoxides and stirred with the materials shown in Table 2 to prepare a sol.
表２
得られた溶液に前記プリフォームを浸し、約２日放置し
た。次にプリフォームを取出して８０°Ｃのオーブンに
入れ約２日乾燥した。次にこれを再び炉に入れ炉内にＮ
＋＋３２４２／分、Ｈｅ５１／分、Ｎ２１！／分供給し
つつ雰囲気温度を８００〜１０００°Ｃに維持して２時
間処理した。最後に炉内にＨｅを３１／分供給しつつ雰
囲気温度を１４００〜１５００°Ｃに上げて透明ガラス
化して直径３５朧、長さ３５０ｍｍのプリフォームを得
た。Table 2 The preform was immersed in the obtained solution and left for about 2 days. Next, the preform was taken out and placed in an oven at 80°C to dry for about 2 days. Next, put this in the furnace again and add N to the furnace.
++3242/min, He51/min, N21! The treatment was carried out for 2 hours while maintaining the ambient temperature at 800 to 1000° C. while supplying the solution at 100° C./min. Finally, while supplying He into the furnace at 31/min, the ambient temperature was raised to 1,400 to 1,500°C to obtain transparent vitrification to obtain a preform with a diameter of 35 mm and a length of 350 mm.
得られたプリフォームには、泡や傷がなくコアとクラッ
ドとの境界面にもズレや剥離が認められなかった。また
、クラッド用ガラス内のＮの含有量を測定したところ３
４％と十分に、かつ均一に含まれていた。The obtained preform had no bubbles or scratches, and no displacement or peeling was observed at the interface between the core and the cladding. In addition, when the N content in the cladding glass was measured, 3
It was contained sufficiently and uniformly at 4%.
（発明の効果）
この発明によると、Ｓｉのアルコキシドに水を加えてゾ
ルとし、この中に別途用意した光伝送用コアロッド上に
ＳｉＯ□からなる多孔質ガラス体を形成したプリフォー
ムを浸して内部にゾルを含浸させ、ついでゾルを乾燥さ
せた後窒素含有ガス雰囲気で加熱処理し、しかるのち多
孔質ガラス体を透明ガラス化してクラッド用ガラスとす
るので、コア用ガラスとクラッド用ガラスとの間の境界
面に泡、傷が生じることがなく、また亀裂や剥離がなく
、さらには多孔質ガラス体内にゾルが均一にゆきわたる
ためＮとの置換が均等に行われ、以ってＮを均一に含ん
だクラッド用ガラスを有する母材とすることができる。(Effects of the Invention) According to this invention, water is added to Si alkoxide to form a sol, and a preform in which a porous glass body made of SiO□ is formed on a separately prepared core rod for optical transmission is immersed in the sol. The sol is impregnated into the glass, and then the sol is dried and then heat-treated in a nitrogen-containing gas atmosphere.Then, the porous glass body is made into transparent glass to form the cladding glass. There are no bubbles or scratches on the interface, and there are no cracks or peeling, and the sol spreads evenly within the porous glass body, so replacement with N is evenly carried out, so N is uniformly distributed. The base material may have a cladding glass containing the cladding glass.
Claims (1)
し、このゾル内に別途用意した光伝送用コアガラスロッ
ドの周りにクラッド用のＳｉＯ＿２からなる多孔質ガラ
ス体が形成されてなるプリフォームを浸漬して前記多孔
質ガラス体内にゾルを含浸させ、ついでプリフォームを
取出して乾燥させて前記多孔質ガラス体内のゾルをゲル
になし、引き続いてこのプリフォームを加熱炉に入れて
、窒素含有ガスを含む雰囲気内で加熱処理して前記ゲル
が含浸された多孔質ガラス体を透明ガラス化することを
特徴とするオキシナイトライドガラスクラッド光ファイ
バ母材の製造方法。At least water is added to Si alkoxide to form a sol, and a preform in which a porous glass body made of SiO_2 for cladding is formed around a separately prepared core glass rod for optical transmission is immersed in this sol. the porous glass body is impregnated with a sol, then the preform is removed and dried to turn the sol in the porous glass body into a gel, and the preform is then placed in a heating furnace to contain a nitrogen-containing gas. 1. A method for producing an oxynitride glass-clad optical fiber preform, characterized in that the porous glass body impregnated with the gel is made into transparent glass by heat treatment in an atmosphere.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1257951A JPH03122026A (en) | 1989-10-04 | 1989-10-04 | Production of oxynitride glass clad optical fiber preform |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP1257951A JPH03122026A (en) | 1989-10-04 | 1989-10-04 | Production of oxynitride glass clad optical fiber preform |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH03122026A true JPH03122026A (en) | 1991-05-24 |
Family
ID=17313484
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1257951A Pending JPH03122026A (en) | 1989-10-04 | 1989-10-04 | Production of oxynitride glass clad optical fiber preform |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03122026A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005059291A1 (en) * | 2005-12-09 | 2007-06-14 | Heraeus Quarzglas Gmbh & Co. Kg | Quartz glass component formation by impregnating a preform with a silicic acid solution, drying and sintering |
-
1989
- 1989-10-04 JP JP1257951A patent/JPH03122026A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005059291A1 (en) * | 2005-12-09 | 2007-06-14 | Heraeus Quarzglas Gmbh & Co. Kg | Quartz glass component formation by impregnating a preform with a silicic acid solution, drying and sintering |
| DE102005059291B4 (en) * | 2005-12-09 | 2009-02-12 | Heraeus Quarzglas Gmbh & Co. Kg | Method for the production of a quartz glass component |
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