JPS63147840A - Production of quartz glass material - Google Patents
Production of quartz glass materialInfo
- Publication number
- JPS63147840A JPS63147840A JP29285186A JP29285186A JPS63147840A JP S63147840 A JPS63147840 A JP S63147840A JP 29285186 A JP29285186 A JP 29285186A JP 29285186 A JP29285186 A JP 29285186A JP S63147840 A JPS63147840 A JP S63147840A
- Authority
- JP
- Japan
- Prior art keywords
- quartz glass
- core
- quartz
- porous
- glass
- 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 64
- 239000000463 material Substances 0.000 title claims abstract description 46
- 238000004519 manufacturing process Methods 0.000 title claims description 45
- 239000011162 core material Substances 0.000 claims abstract description 50
- 238000000034 method Methods 0.000 claims abstract description 34
- 239000005373 porous glass Substances 0.000 claims abstract description 29
- 239000011521 glass Substances 0.000 claims abstract description 21
- 238000004017 vitrification Methods 0.000 claims abstract description 19
- 239000010453 quartz Substances 0.000 claims abstract description 17
- 238000000151 deposition Methods 0.000 claims abstract description 6
- 239000002245 particle Substances 0.000 claims abstract description 6
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 5
- 150000002367 halogens Chemical class 0.000 claims abstract description 5
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 4
- 239000011737 fluorine Substances 0.000 claims abstract description 4
- 239000003575 carbonaceous material Substances 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 6
- 238000005553 drilling Methods 0.000 abstract description 4
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 4
- 238000005520 cutting process Methods 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 238000010297 mechanical methods and process Methods 0.000 abstract 1
- 239000002019 doping agent Substances 0.000 description 8
- 239000013307 optical fiber Substances 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000007789 gas Substances 0.000 description 6
- 238000005253 cladding Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 239000000835 fiber Substances 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- -1 silicon halides Chemical class 0.000 description 3
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 2
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 239000005049 silicon tetrachloride Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000004071 soot Substances 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical class [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005282 brightening Methods 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005340 laminated glass Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910052987 metal hydride Inorganic materials 0.000 description 1
- 150000004681 metal hydrides Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000149 penetrating effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007517 polishing process Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 description 1
- 238000001947 vapour-phase growth Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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]
- C03B37/01466—Means for changing or stabilising the diameter or form of tubes or rods
-
- 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
- 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]
- C03B37/01486—Means for supporting, rotating or translating the preforms being formed, e.g. lathes
- C03B37/01493—Deposition substrates, e.g. targets, mandrels, start rods or tubes
-
- 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]
- C03B37/018—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 glass deposition on a glass substrate, e.g. by inside-, modified-, plasma-, or plasma modified- chemical vapour deposition [ICVD, MCVD, PCVD, PMCVD], i.e. by thin layer coating on the inside or outside of a glass tube or on a glass rod
- C03B37/01884—Means for supporting, rotating and translating tubes or rods being formed, e.g. lathes
- C03B37/01892—Deposition substrates, e.g. tubes, mandrels
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)
- 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」
本発明は、光フアイバ用のブリフィー−ムを製造する際
に好適に用いられろ石英ガラス材の製造方１人に関する
乙のである。DETAILED DESCRIPTION OF THE INVENTION [Industrial Field of Application] The present invention relates to a method for manufacturing a quartz glass material which is suitably used in manufacturing Brifeme for optical fibers.
ご従来技術とその問題へ１
プリフォーム用の石英ガラス材をＴＡ造士ろ方、去とし
て、第・１図に示すような外付は法かある。To the prior art and its problems 1. If the quartz glass material for the preform is made from TA Zoshiro, it is possible to attach it externally as shown in Figure 1.
従来の外付は法では、中実の芯材１． Ｑの７４ ｐに
石英ガラスのすす１１を堆積させ、ついて堆積し、・二
すすを帯溶融して気泡を抜きながら透明カラス化し、つ
いで芯抜きしていた。In the conventional external method, a solid core material 1. Soot 11 of quartz glass was deposited on 74p of Q, and the two soots were melted and formed into transparent glass while removing air bubbles, and then the core was removed.
二〇よう１ヱ従来の製造方法にあっては、ｄ明化さ（ｔ
たガラスを再び溶融軟化させてご材ｌＯを抜き取らねば
ならない。このｆ二ぬ、ｉ道、？：Ｊつ石英ガラス（オ
フつ製造方法では、多ｔｔの加熱二不ルギーかＺ要とな
り製造コストか高騰するとｊＩミに、こ投３作業が大掛
かりになる問題があった。20-1ヱ In the conventional manufacturing method, d brightening (t
The glass must be melted and softened again to extract the lO. This f2nu, i way? : J2 quartz glass (with the off-site manufacturing method, there was a problem that the manufacturing cost would rise due to the need for multiple tts of heating or Z, resulting in a large-scale work.
また一方、山付は法でプリフォームを製造する際の出発
部材に用いられる石英ガラス材として石英管がある。従
来この石英管を製造するには、第５図ないし第７図に示
すように、まず酸水素火炎Ａ中に天然水晶粉を通過させ
て溶融し、これを堆積させて透明なガラス塊１２を製造
し、次いで、このガラス塊Ｉ２に穴をあけてインゴット
１３とし、このインゴット１３を加熱炉１４で細く引き
伸ばして石英管１５としていた。On the other hand, a quartz tube is a quartz glass material used as a starting member when manufacturing a preform by the Yamazuki method. Conventionally, in order to manufacture this quartz tube, as shown in FIGS. 5 to 7, natural quartz powder is first passed through an oxyhydrogen flame A to melt it, and then deposited to form a transparent glass lump 12. Then, a hole was made in this glass lump I2 to form an ingot 13, and this ingot 13 was stretched thinly in a heating furnace 14 to form a quartz tube 15.
ところが、このような石英管の製造方法にあっては、イ
ンゴット１３を作成する際にガラス塊１２を溶融軟化さ
せてから穴開しなければならず、大掛かりな製造作業を
伴う不満があった。However, in such a method of manufacturing a quartz tube, when creating the ingot 13, the glass gob 12 must be melted and softened before drilling, which is a dissatisfaction with the large-scale manufacturing work involved.
加えて、この石英管の製造方法にあっては、天然水晶粉
を酸水素火炎Ａ中て溶融する際に多くのＯＨ基が混入す
るため（通常１５０ ｐｐｍオーダ）、この方法で製造
された石英管は、直接光ファイバのクラッド材料には利
用できず、改めてその内周にＯＨ基の少ないクラッド材
料を厚く積層しなければならない不満があった。In addition, in this method for manufacturing quartz tubes, when natural quartz powder is melted in oxyhydrogen flame A, a large amount of OH groups (usually on the order of 150 ppm) is mixed in, so the quartz tube manufactured by this method The tube cannot be used directly as a cladding material for an optical fiber, and there is a dissatisfaction that a cladding material with few OH groups must be laminated thickly on its inner periphery.
「問題点を解決するための手段」
そこで、本発明の石英ガラス材の製造方法にあっては、
管状であって、石英ガラスよりも硬度が低くかつ石英ガ
ラスよりも耐熱性を有する材料からなる芯材の外周に石
英を主成分とするガラス微粒子を堆積さ什て多孔質ガラ
ス層を形成することにより、上記問題点の解決を図った
。"Means for Solving the Problems" Therefore, in the method for manufacturing a quartz glass material of the present invention,
Forming a porous glass layer by depositing glass particles containing quartz as a main component around the outer periphery of a core material that is tubular and made of a material that has lower hardness than quartz glass and has higher heat resistance than quartz glass. We attempted to solve the above problems.
以下、第１図および第２図を参照して本発明の石英ガイ
ド材の製造方法を詳しく説明する。Hereinafter, the method for manufacturing a quartz guide material of the present invention will be explained in detail with reference to FIGS. 1 and 2.
本発明の製造方法にあっては、管状に形成された芯材ｌ
か用いられろ。この芯材１は、製造される石英ガラス材
をなす石英ガラスよりも硬度か低くかつ同石英ガラスよ
りも耐熱性を有する材料によって形成されている。その
ような材料としては、カーボン等の炭素系材料の他、本
質的には石英ガラスより硬いが多孔質焼結体とすること
により実際上の切削性を確保したところのアルミナ、ノ
ルコニア、ボロンナイトライド等を挙げろことができる
。In the manufacturing method of the present invention, a core material l formed in a tubular shape
Or be used. The core material 1 is made of a material that has lower hardness than the quartz glass that makes up the quartz glass material to be manufactured, and has higher heat resistance than the quartz glass. Examples of such materials include carbon-based materials such as carbon, as well as alumina, norconia, and boronite, which are essentially harder than quartz glass but have achieved practical machinability by forming porous sintered bodies. You can list rides, etc.
この芯材ｌは多孔質であることが望ましい。多孔質の芯
材ｌは、カーボン、アルミナ等の多孔質な材料で芯材ｌ
を形成することによって得ることかできるが、管体にそ
の外周から内周に貫通する孔を多数穿設することによっ
て乙製造できる。まｆ二、アルミナ扮等の粉体を管状に
焼結することによってし作成できる。It is desirable that this core material l be porous. The porous core material is a porous material such as carbon or alumina.
However, it can be manufactured by drilling a large number of holes penetrating the tube from its outer periphery to its inner periphery. It can be made by sintering powder such as alumina into a tube shape.
本発明の製造方法にあっては、第１図に示すように、芯
材ｌの外周に石英を主成分とするガラス微粒子を堆積さ
せて多孔質ガラス層２を形成する。In the manufacturing method of the present invention, as shown in FIG. 1, a porous glass layer 2 is formed by depositing glass particles containing quartz as a main component around the outer periphery of a core material 1.
この多孔質ガラス層２の形成は、火炎加水分解や熱酸化
反応などを利用した周知の気相成長法によって行なわれ
る。多孔質ガラス層２を形成するのに用いる原料として
は、四塩化珪素等の珪素のハロゲン化物、あるいは珪素
の水素化物、珪素のアルコレートなとがめろ。また、屈
折率を制御するために、必要に応して、四塩化ゲルマニ
ウムなとの金属ハロゲン化物、金属水素化物、金属アル
コレート等を用いろ。この多孔質ガラス層２の形成は若
干低めの温度（通常約１３００°Ｃ以下）で行なわれる
。温度が高すぎると、積層されたガラス層が透明で緻密
な乙のとなり、製造雰囲気中の水分や０１１基がガラス
中に混入して除去し難くなる問題が生じる。This porous glass layer 2 is formed by a well-known vapor phase growth method using flame hydrolysis, thermal oxidation reaction, or the like. Raw materials used to form the porous glass layer 2 include silicon halides such as silicon tetrachloride, silicon hydrides, and silicon alcoholates. Further, in order to control the refractive index, a metal halide such as germanium tetrachloride, a metal hydride, a metal alcoholate, etc. may be used as necessary. This porous glass layer 2 is formed at a slightly lower temperature (usually about 1300° C. or lower). If the temperature is too high, the laminated glass layers become transparent and dense, causing the problem that moisture and 011 groups in the manufacturing atmosphere mix into the glass and become difficult to remove.
本発明の製造方法にあっては、前記のように多孔質ガラ
ス層２を形成した後、この多孔質ガラス層２の透明ガラ
ス化処理と芯抜き処理とを行う。In the manufacturing method of the present invention, after forming the porous glass layer 2 as described above, the porous glass layer 2 is subjected to a transparent vitrification treatment and a coring treatment.
これら透明ガラス化処理と芯抜き処理は、いずれを先に
行っても良い。Either of the transparent vitrification treatment and the core removal treatment may be performed first.
前記透明ガラス化処理は、多孔質ガラス層２を加熱溶融
して透明ガラスとする処理である。透明ガラス化処理に
おいては、まず、多孔質ガラス層２が溶融しない程度の
高温（通常約９００℃以下）で、多孔質ガラス層２中に
残留した水分又びＯＩＩ基を除去する処理（脱０１−Ｉ
基工程）を行い、その後多孔質ガラス層２をより高温で
（通常的１４００ ’Ｃ〜１７００℃）溶融して透明化
する（透明化工程）。The transparent vitrification treatment is a treatment in which the porous glass layer 2 is heated and melted to form transparent glass. In the transparent vitrification process, first, the moisture and OII groups remaining in the porous glass layer 2 are removed at a high temperature (usually about 900° C. or lower) that does not melt the porous glass layer 2 (de-01 -I
After that, the porous glass layer 2 is melted at a higher temperature (typically 1400'C to 1700C) and made transparent (transparency process).
本発明の製造方法によれば、この透明ガラス化処理を所
定のドーパントを含むガス雰囲気下で行うことにより、
所定のドーパントが添加さノーｆ二石英ガラス材を製造
できる。その場合、少なくとも前記透明化工程をドーパ
ントを含むガス雰囲気下で行う。フッ素等のハロゲンを
含むガス雰囲気下で透明ガラス化処理を行えば、クラツ
ド材に適した屈折率の小さい石英ガラス材を製造できる
。According to the manufacturing method of the present invention, by performing this transparent vitrification treatment in a gas atmosphere containing a predetermined dopant,
It is possible to produce a no-f disilica glass material to which certain dopants are added. In that case, at least the transparentization step is performed in a gas atmosphere containing a dopant. By performing transparent vitrification treatment in a gas atmosphere containing halogen such as fluorine, a quartz glass material with a low refractive index suitable for a cladding material can be manufactured.
上記芯抜き処理は、芯材１を取り除く工程である。芯抜
さ処理は、第２図に示すようなドリル３を用いｆこ穴あ
け加工やバイトを用いた中ぐり加工によって行なわれる
。この加工に際しては、芯材１の中空部分１ａを下穴と
して用いる。そしてまず、ドリル３等により芯材ｌの外
周部分を僅かに残して芯＋４１を取り除き、その後研摩
処理によって残る芯材ｌの外周部分を取り除くことが望
ましい。この芯抜き処理に先立って上記透明ガラス化処
理が完了している場合には、研摩処理の際に同時に透明
化されたガラス層の内面研摩が行なわれる。The core removal process is a process of removing the core material 1. The coring process is performed by drilling using a drill 3 or boring using a cutting tool as shown in FIG. During this processing, the hollow portion 1a of the core material 1 is used as a pilot hole. First, it is desirable to remove the core + 41 with a drill 3 or the like, leaving only a small portion of the outer periphery of the core material 1, and then remove the remaining outer periphery of the core material 1 by polishing. If the transparent vitrification process is completed prior to this coring process, the inner surface of the transparent glass layer is simultaneously polished during the polishing process.
以上の処理によって作成された石英ガラス材は、先に芯
抜き処理を行いその後透明ガラス化処理しｆこ場合には
棒状のものとなり、透明ガラス化処理後に芯抜き処理し
ｊ二場合にはパイプ状の乙のとなる。The quartz glass material created by the above process is first subjected to a core removal process and then to a transparent vitrification process.In this case, it is made into a rod shape, and after the transparent vitrification process, a core removal process is performed. It becomes the second party of the state.
パイプ状に形成された石英ガラス材はプリフォームのク
ラッド相当部分を形成するガラス材料として好適に利用
される。また棒状に形成された石英ガラス材はコア相当
部分を形成するガラス材料として好適にＩＩＩ用できる
。A quartz glass material formed into a pipe shape is suitably used as a glass material forming a portion corresponding to the cladding of the preform. Moreover, a quartz glass material formed into a rod shape can be suitably used as a glass material for forming a portion corresponding to the core.
「作用」
本発明の製造方法によれば、管状であって、石英ガラス
より乙硬度が低い芯Ｕｔを用いたので、芯材１をドリル
３等を用いて機械的に容易に取り除くことかできる。芯
材ｌの中空部分１ａは、トリル加工等の機械加工に際し
て、工具を導くあるいは工具を挿入する下穴として機能
する。"Function" According to the manufacturing method of the present invention, since the core Ut is tubular and has a lower hardness than quartz glass, the core material 1 can be easily removed mechanically using a drill 3 or the like. . The hollow portion 1a of the core material 1 functions as a pilot hole for guiding or inserting a tool during machining such as trilling.
また、本発明の製造方法に用いる芯材Ｉは石英ガラスよ
りも耐熱性を有する材料によって形成されているので、
ガラス微粒子を堆積させて多孔質ガラス層２を形成する
際にも十分耐える。Furthermore, since the core material I used in the manufacturing method of the present invention is made of a material that is more heat resistant than quartz glass,
It can withstand the formation of the porous glass layer 2 by depositing glass particles.
また、本発明の製造方法では、芯材ｌの周囲に多孔質な
ガラス層２を形成するので、透明ガラス化処理の際、孔
を介してガラス層２の内部の水分やＯ）［基を容易に除
去できる。従って、本発明の製造方法によれば、ＯＩＩ
基の残留量の少ない石英ガラスを製造できる。In addition, in the manufacturing method of the present invention, since the porous glass layer 2 is formed around the core material l, during the transparent vitrification treatment, moisture inside the glass layer 2 and O) Can be easily removed. Therefore, according to the manufacturing method of the present invention, OII
It is possible to produce quartz glass with a small amount of residual groups.
また、本発明の製造方法において、多孔質ガラス層２の
透明ガラス化処理を、所定のドーパント特にフッ素等の
ハロゲンを含有するガス雰囲気下で行えば、多孔質ガラ
ス層２の孔を通じてその内部までガスが速やかに拡散す
るので、多孔質ガラス層２の内部にまで均一にドーパン
トを添加できろ。従って、本発明の製造方法によれば、
均質な石英ガラスを製造できる。In addition, in the manufacturing method of the present invention, if the transparent vitrification treatment of the porous glass layer 2 is performed in a gas atmosphere containing a predetermined dopant, especially a halogen such as fluorine, it is possible to penetrate the inside of the porous glass layer 2 through the pores of the porous glass layer 2. Since the gas diffuses quickly, the dopant can be added evenly into the interior of the porous glass layer 2. Therefore, according to the manufacturing method of the present invention,
Can produce homogeneous quartz glass.
またさらに、本発明の製造方法において、炭素系（４料
からなる芯材１など多孔質な芯材を用いると、多孔質ガ
ラス層２の透明ガラス化処理を芯Ｉ第１に装着した状態
で行っｆコ場合、芯材１の中空部分１ａおよび多数の孔
を介してガラス層２の内部か；）ｔＪ、水分・ＯＨ基の
除去、およびドーパントの添加が進行するので、これら
の処理か速やかにかつ高度におこζられろ。従って、多
孔質な芯材１を用いた場合には、より高品質な石英ガラ
スを製造することができる。Furthermore, in the manufacturing method of the present invention, when a porous core material such as the core material 1 made of carbon-based (four materials) is used, the transparent vitrification treatment of the porous glass layer 2 is applied to the core I first. When this process is carried out, removal of moisture and OH groups and addition of dopants proceed through the hollow portion 1a of the core material 1 and numerous holes inside the glass layer 2; Be extremely excited. Therefore, when porous core material 1 is used, higher quality quartz glass can be manufactured.
１一実施例」
以下、実施例に沿って本発明の石英ガラス手４の製造方
法を詳しく説明する。11 Embodiments Hereinafter, the method for manufacturing the quartz glass hand 4 of the present invention will be described in detail with reference to Examples.
外径２８ｍｍ、内径２１ｍｍ、肉Ｆ７３．５ｍｍ１長さ
５００ｍｍのカーボン製の管状芯材Ｉを準備し、外付は
法によって多孔質ガラス層２を形成しｆこ。多孔質ガラ
ス層２は、高温の酸水素火炎の中に四塩化珪素を通して
生成せしめたノリ力のすすによって形成された。キャリ
アガスにはアルゴンを用いた。形成された多孔質ガラス
層２は厚さＩ Ｏ，２ｍｍ１長さ４５０ｍｍであった。A carbon tubular core material I having an outer diameter of 28 mm, an inner diameter of 21 mm, a thickness of 73.5 mm, and a length of 500 mm was prepared, and a porous glass layer 2 was formed on the outside by a method. The porous glass layer 2 was formed by soot produced by passing silicon tetrachloride through a high temperature oxyhydrogen flame. Argon was used as the carrier gas. The formed porous glass layer 2 had a thickness of IO, 2 mm and a length of 450 mm.
次いで多孔質ガラス層２か形成された芯材１を所定のガ
スが流入する加熱炉に送り込み透明ガラス化処理した。Next, the core material 1 on which the porous glass layer 2 was formed was sent into a heating furnace into which a predetermined gas was introduced, and was subjected to a transparent vitrification treatment.
処理条件は第１表の通りである。The processing conditions are shown in Table 1.
以下余白
第１表
透明ガラス化処理して得られたものは、芯材ｌの外周に
透明な石英ガラスが被覆されたパイプ状のものであった
。次ぎにこのパイプの芯材ｌの部分をドリルを用いて削
り落とし、石英ガラスからなるガラスパイプを得た。こ
のガラスパイプの内面を更に機械研摩して、パイプ状の
石英ガラス材を得た。The material obtained by the transparent vitrification treatment was a pipe-shaped material in which the outer periphery of the core material 1 was coated with transparent quartz glass. Next, the core material 1 of this pipe was ground down using a drill to obtain a glass pipe made of quartz glass. The inner surface of this glass pipe was further mechanically polished to obtain a pipe-shaped quartz glass material.
作成された石英ガラス材は内径２８．５ｍｍ、外径３４
．５ｎ＋ａ＋、長さ４２０ｍｍであった。この石英ガラ
ス材の屈折率は、純粋石英の屈折率（１，４５８）より
も約０．３４％低い値であった。また残留Ｏ）Ｉ基量は
１０ｐｐｂと非常に低能塵であった。The created quartz glass material has an inner diameter of 28.5 mm and an outer diameter of 34 mm.
．． 5n+a+, length 420mm. The refractive index of this quartz glass material was about 0.34% lower than the refractive index of pure quartz (1,458). Further, the amount of residual O)I groups was 10 ppb, which was extremely low-potency dust.
カーボン製の芯材ｌの研削はカーボンの硬度が低いため
容易であった。また、ドリル３は芯材ｌの中空部分！ａ
に導かれて、芯材ｌを正確に除去した。その結果、パイ
プ状の石英ガラス材を極めて容易に製造できた。Grinding of the core material 1 made of carbon was easy because carbon has low hardness. Also, the drill 3 is the hollow part of the core material l! a
Guided by this method, the core material 1 was accurately removed. As a result, a pipe-shaped quartz glass material could be manufactured extremely easily.
次５に、得られたパイプ状石英ガラス材を用いて内付は
法（ＭＣＶＤ法）によりプリフォームを作成した。製造
条件は第２表の通りである。Next, using the obtained pipe-shaped quartz glass material, a preform was created by the inner attachment method (MCVD method). The manufacturing conditions are shown in Table 2.
以下余白
第２表
デボジンヨン終了後、酸水素バーナの火力を高めて石英
ガラス材の表面温度が１９５０℃になるように加熱して
コラップスし、プリフォームを作成した。Table 2 (margins below) After the debossing was completed, the heating power of the oxyhydrogen burner was increased to heat and collapse the quartz glass material to a surface temperature of 1950° C. to create a preform.
次ぎに、このプリフ（−−ムを線引き炉で２１００℃に
加熱しつつ紡糸して光ファイバを作成した。Next, this prefume was heated to 2100° C. in a drawing furnace and spun to produce an optical fiber.
得られｆ二元ファイバの屈折率分布を第３図に示す。The refractive index distribution of the obtained f-binary fiber is shown in FIG.
また、その伝送特性は次の通りである。Moreover, its transmission characteristics are as follows.
ファイバ型 単一モードファイバ
伝送損失 ４．５ｄＢ／ｋｍ（波長１．３８μｍ）
０．１８ｄＢ／ｋｍ（波長１．５５μｊりモードフィー
ルド直径 １１．５μｍ第２モードのカット
オフ波長 １．４９μｍこれらの結果から、本発明の
製造方法によれば、今後長距離伝送に使用されると期待
されている波長１．５５μだの伝送にも好適に利用でき
る低損□失な光ファイバを提供できることが判明した。Fiber type Single mode fiber transmission loss 4.5dB/km (wavelength 1.38μm)
0.18 dB/km (wavelength: 1.55 μj, mode field diameter: 11.5 μm, second mode cutoff wavelength: 1.49 μm) From these results, according to the manufacturing method of the present invention, it is expected that it will be used for long-distance transmission in the future. It has been found that it is possible to provide a low-loss optical fiber that can be suitably used for transmission at the expected wavelength of 1.55μ.
なお、上記実施例にあってはパイプ状の石英ガラス材を
製造しこれを内付は法の出発部材である石英管に用いた
例を示したが、パイプ状の石英ガラス材をコラプシング
して中実化すれば、軸付は法および外付は法によってプ
リフォーム形成する際の出発部材に用いることもできる
。In the above example, a pipe-shaped quartz glass material was manufactured and used for the quartz tube, which is the starting material for the inner mounting method, but it is also possible to collapse the pipe-shaped quartz glass material If it is made solid, it can also be used as a starting member when forming a preform by the shaft-mounting method or the external-mounting method.
「発明の効果」
本発明の石英ガラス材の製造方法によれば、芯材をドリ
ル等を用いて機械的に容易に取り除くことかでさるめで
、芯抜きを小規模な装置で行うことができるうえ、加熱
する必要がないので芯抜きに要するエネルギーを節減で
きる。従って、本発明の製造方法によれば光ファイバの
製造に用いる石英ガラス材を容易にかつ安価に製造でき
る。しから、本発明の製造方法によれば、芯材を取り除
いた部分に孔か形成されるので、内骨は法に用いられる
石英管を容易に製造することができる。"Effects of the Invention" According to the method for manufacturing a quartz glass material of the present invention, the core material can be easily and smoothly removed mechanically using a drill, etc., and the core material can be removed using small-scale equipment. Moreover, since there is no need for heating, the energy required for core removal can be saved. Therefore, according to the manufacturing method of the present invention, the quartz glass material used for manufacturing optical fibers can be manufactured easily and inexpensively. However, according to the manufacturing method of the present invention, a hole is formed in the portion from which the core material has been removed, so that it is possible to easily manufacture a quartz tube for use in the internal rib method.
また、本発明の製造方法にあっては、芯材の周囲に多孔
質なガラス層を形成するので、透明ガラス化処理の際、
混入しｆこ水分や０１１基の除去およびドーパントの添
加を多数の孔を介して行うことかできる。よって、本発
明の製造方法によれば、ＯＮ基の残留が少なくかつ均一
にドーパントが添加された高品質の石英ガラス材を製造
できる。In addition, in the manufacturing method of the present invention, since a porous glass layer is formed around the core material, during the transparent vitrification treatment,
Removal of mixed water and 011 groups and addition of dopants can be performed through a large number of holes. Therefore, according to the manufacturing method of the present invention, it is possible to manufacture a high-quality quartz glass material with few remaining ON groups and to which dopants are uniformly added.
従って、本発明の石英ガラス材の製造方法によればクラ
ッド居の内面側すなわちコアに接する部分を形成できる
高品質の石英管を提供することができる。Therefore, according to the method for manufacturing a quartz glass material of the present invention, it is possible to provide a high-quality quartz tube in which the inner surface side of the cladding, that is, the portion in contact with the core can be formed.
第１図及び第２図は本発明の製造方法を説明するための
斜視図、第３図は実施例で製造した光ファイバの屈折率
分布を示すグラフ、第４図は従来の石英ガラス材を製造
する方法の１例を示す斜視図、第５図ないし第７図は従
来のパイプ状の石英ガラストイを製造する方法を示す斜
視図である。
■・芯材、２・・・多孔質ガラス層。1 and 2 are perspective views for explaining the manufacturing method of the present invention, FIG. 3 is a graph showing the refractive index distribution of the optical fiber manufactured in the example, and FIG. 4 is a graph showing the refractive index distribution of the optical fiber manufactured in the example. FIGS. 5 to 7 are perspective views showing an example of a manufacturing method. FIGS. 5 to 7 are perspective views showing a conventional method of manufacturing a pipe-shaped quartz glass toy. ■ Core material, 2... Porous glass layer.
Claims (5)
ガラスより耐熱性を有する材料からなる芯材の外周に、
石英を主成分とするガラス微粒子を堆積させて多孔質ガ
ラス層を形成し、その後多孔質ガラス層の透明ガラス化
処理と芯抜き処理を行うことを特徴とする石英ガラス材
の製造方法。(1) On the outer periphery of a core material that is tubular and made of a material that has lower hardness than quartz glass and has higher heat resistance than quartz glass,
A method for producing a quartz glass material, which comprises depositing glass particles containing quartz as a main component to form a porous glass layer, and then subjecting the porous glass layer to transparent vitrification treatment and core removal treatment.
ス雰囲気下で行うことを特徴とする特許請求の範囲第１
項記載の石英ガラス材の製造方法。(2) Claim 1, characterized in that the transparent vitrification treatment is performed in a gas atmosphere containing halogen.
A method for producing a quartz glass material as described in Section 1.
許請求の範囲第２項記載の石英ガラス材の製造方法。(3) The method for manufacturing a quartz glass material according to claim 2, wherein the halogen is fluorine.
求の範囲第１項ないし第３項記載の石英ガラス材の製造
方法。(4) The method for producing a quartz glass material according to any one of claims 1 to 3, wherein the core material is porous.
あることを特徴とする特許請求の範囲第１項ないし第４
項記載の石英ガラス材の製造方法。(5) Claims 1 to 4 characterized in that the core material is made of a carbon-based material.
A method for producing a quartz glass material as described in Section 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29285186A JPS63147840A (en) | 1986-12-09 | 1986-12-09 | Production of quartz glass material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29285186A JPS63147840A (en) | 1986-12-09 | 1986-12-09 | Production of quartz glass material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS63147840A true JPS63147840A (en) | 1988-06-20 |
Family
ID=17787188
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29285186A Pending JPS63147840A (en) | 1986-12-09 | 1986-12-09 | Production of quartz glass material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63147840A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5292483A (en) * | 1991-06-28 | 1994-03-08 | Beckman Instruments, Inc. | Detecting a radiation signal |
| EP1000908A2 (en) * | 1998-10-08 | 2000-05-17 | Heraeus Quarzglas GmbH | Method for producing quartz glass preform for optical fibers |
| WO2002010081A1 (en) * | 2000-07-31 | 2002-02-07 | Shin-Etsu Quartz Products Co., Ltd. | Mandrel for producing quartz glass and optical fiber matrix using the mandrel, optical fiber, production method for quartz glass element |
| EP1256554A1 (en) * | 2001-05-11 | 2002-11-13 | Alcatel | Step index optical fibre with doped core and cladding, preform and manufacturing process for such a fibre |
-
1986
- 1986-12-09 JP JP29285186A patent/JPS63147840A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5292483A (en) * | 1991-06-28 | 1994-03-08 | Beckman Instruments, Inc. | Detecting a radiation signal |
| EP1000908A2 (en) * | 1998-10-08 | 2000-05-17 | Heraeus Quarzglas GmbH | Method for producing quartz glass preform for optical fibers |
| EP1000908A3 (en) * | 1998-10-08 | 2001-05-02 | Heraeus Quarzglas GmbH | Method for producing quartz glass preform for optical fibers |
| WO2002010081A1 (en) * | 2000-07-31 | 2002-02-07 | Shin-Etsu Quartz Products Co., Ltd. | Mandrel for producing quartz glass and optical fiber matrix using the mandrel, optical fiber, production method for quartz glass element |
| US7198247B2 (en) | 2000-07-31 | 2007-04-03 | Shin-Etsu Quartz Products Co., Ltd. | Mandrel for producing quartz glass and production method for optical fiber mother material, optical fiber and quartz glass body using the same |
| EP1256554A1 (en) * | 2001-05-11 | 2002-11-13 | Alcatel | Step index optical fibre with doped core and cladding, preform and manufacturing process for such a fibre |
| FR2824642A1 (en) * | 2001-05-11 | 2002-11-15 | Cit Alcatel | INSPECTION FIBER WITH DOPED SHEATH AND HEAD INDEX, PREFORM AND METHOD OF MANUFACTURE FOR SUCH A FIBER |
| US6904213B2 (en) | 2001-05-11 | 2005-06-07 | Alcatel | Step index optical fiber with doped cladding and core, a preform, and a method of fabricating such a fiber |
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