JPH0527577B2 - - Google Patents
Info
- Publication number
- JPH0527577B2 JPH0527577B2 JP6810587A JP6810587A JPH0527577B2 JP H0527577 B2 JPH0527577 B2 JP H0527577B2 JP 6810587 A JP6810587 A JP 6810587A JP 6810587 A JP6810587 A JP 6810587A JP H0527577 B2 JPH0527577 B2 JP H0527577B2
- Authority
- JP
- Japan
- Prior art keywords
- glass
- crucible
- rod
- tube
- fiber
- 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 - Lifetime
Links
- 239000011521 glass Substances 0.000 claims description 58
- 239000000835 fiber Substances 0.000 claims description 34
- 238000009987 spinning Methods 0.000 claims description 27
- 239000005387 chalcogenide glass Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 17
- 239000011261 inert gas Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000004519 manufacturing process Methods 0.000 claims description 9
- 230000009477 glass transition Effects 0.000 claims description 4
- 239000011347 resin Substances 0.000 description 10
- 229920005989 resin Polymers 0.000 description 10
- 239000003365 glass fiber Substances 0.000 description 8
- 230000005540 biological transmission Effects 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 238000005253 cladding Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004031 devitrification Methods 0.000 description 4
- 239000011248 coating agent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000011534 incubation Methods 0.000 description 3
- 230000003647 oxidation Effects 0.000 description 3
- 238000007254 oxidation reaction Methods 0.000 description 3
- 229910052711 selenium Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical group [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 229910018110 Se—Te Inorganic materials 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000005243 fluidization Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound 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
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
- C03B37/022—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor from molten glass in which the resultant product consists of different sorts of glass or is characterised by shape, e.g. hollow fibres, undulated fibres, fibres presenting a rough surface
- C03B37/023—Fibres composed of different sorts of glass, e.g. glass optical fibres, made by the double crucible technique
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2201/00—Type of glass produced
- C03B2201/80—Non-oxide glasses or glass-type compositions
- C03B2201/86—Chalcogenide glasses, i.e. S, Se or Te glasses
Landscapes
- Engineering & Computer Science (AREA)
- 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)
- Manufacture, Treatment Of Glass Fibers (AREA)
Description
［産業上の利用分野］
本発明は赤外透過性に優れたコア−クラツド構
造を有するカルコゲナイドガラスフアイバーの製
造方法に関する。
［従来の技術］
カルコゲナイドガラスは赤外透過性及び耐候性
に優れた赤外フアイバー用材料であつて、既に数
多くのガラス組成が報告されている（例えばZ.U.
Borisova、Glassy Semiconductor
Plenumpress、New York、1981）。これらのカ
ルコゲナイドガラス組成の中で、波長10μm付近、
すなわち炭酸ガスレーザー光線の波長領域の光を
低損失で透過し得るものは、Teの含有量が50モ
ル％以上であるGe−Se−Te系であつて、そのフ
アイバー化が検討されている（例えば、勝山俊
夫、松村宏善、電子通信学会全国大会（昭和60年
３月）予稿集p4−256）。しかし、Te含有の高い
ガラスフアイバーは機械的強度が低いため、樹脂
コーテイング等による補強をしなければ実用性に
乏しい。ところが、波長10μm付近は各種樹脂材
料の指紋領域であるため、その波長領域の赤外線
を吸収する。従つて、このような樹脂材料をカル
コゲナイドガラスフアイバーの外周に直接コーテ
イングすることはできない。
この問題点はカルコゲナイドガラスフアイバー
をコア−クラツドの二重構造にした後、その外周
を樹脂でコーテイングすることによつて解決され
る。コア−クラツド構造を有するガラスフアイバ
ーの製造法としては、二重ルツボ法が知られてい
る（金森照寿等、電子通信研究所、研究実用化報
告、32（1983）、2737）。この方法はコアとなるガ
ラスを内側のルツボに、クラツドとなるガラスを
外側のルツボにそれぞれ挿入して溶融し、二重ル
ツボの底部に設けた紡糸ノズルから両ガラスを同
時に押し出してフアイバーとするものである。し
かし、上記したようにTe含有量が50モル％と高
いカルコゲナイドガラス系は、結晶化に対する熱
的安定性が低いために、またAs及びSe等の蒸気
圧が高い成分を含むカルコゲナイドガラス系は、
高温状態でのガラス成分の蒸発によつて組成変動
が起るために、上に述べた二重ルツボ法ではコア
−クラツド構造のカルコゲナイドガラスフアイバ
ーを定常的に製造することが困難である。
このほか、コア−クラツド構造を有するガラス
フアイバーの製造方法として、クラツドとなるチ
ユーブ状のガラスの中にコアとなるロツド状のガ
ラスを挿入し、その先端部を溶融紡糸するロツド
インチユーブ法が、石英ガラスフアイバーの製造
に従来から利用されている。しかし、カルコゲナ
イドガラスは、僅かな温度変化でも粘度が著しく
変動するうえ、その紡糸は非酸化性雰囲気で行な
わなければならないため、ロツドインチユーブ法
をそのままカルコゲナイドガラスフアイバーの製
造に利用することはできない。
［発明が解決しようとする問題点］
上記したように、従来のロツドインチユーブ法
や二重ルツボ法をそのままカルコゲナイドガラス
に適用しても、紡糸中にガラスの酸化や失透を伴
うために、所望の赤外透過性ガラスフアイバーを
得ることができない。本発明はカルコゲナイドガ
ラスを紡糸する際に懸念される酸化や失透の問題
を払拭して、カルコゲナイドガラスから赤外透過
性に優れたコア−クラツド構造のフアイバーを製
造可能ならしめる新しいガラスフアイバー製造法
を提供する。
［問題点を解決するための手段］
本発明に係るガラスフアイバー製造法は、下部
に紡糸ノズルを有する円筒形二重ルツボの内側ル
ツボにカルコゲナイドガラスロツドを、外側ルツ
ボに該ガラスロツドよりも屈折率が低いカルコゲ
ナイドガラスチユーブをそれぞれ挿入し、ルツボ
内部及びルツボ外部を不活性ガス雰囲気に保持
し、紡糸ノズル近傍のチユーブ及びロツドのみを
ガラス転移温度よりも高い温度に加熱しながらガ
ラスチユーブとガラスロツドを同時にルツボの紡
糸ノズルから引き出してコア−クラツド構造を有
するカルコゲナイドガラスフアイバーを得ること
からなる。
［作 用］
本発明の方法に於いて、紡糸ノズル近傍に位置
するガラスチユーブ及びガラスロツドを加熱する
に際しては、予め二重ルツボ内部及びルツボ外周
のノズル近辺を不活性ガスにて充分置換しておく
ことが望ましい。この置換が不充分であると、ガ
ラスチユーブ及びガラスロツドが加熱時に水蒸気
や酸素で侵蝕されることがあるからである。加熱
は二重ルツボ内部及びルツボの紡糸ノズル近傍を
不活性ガス雰囲気に保持し、紡糸ノズル近傍に位
置するガラスチユーブ及びガラスロツドに対して
局部的に行なわれ、これらがガラス転移温度以上
に加熱されて流動化した後は、ルツボ内のガス圧
及び／又はガラスチユーブ及びガラスロツドに加
えられる荷重によつて直ちに紡糸される。従つ
て、紡糸工程中にガラスが酸素で侵されることが
なく、また、フアイバーが切断されることもな
い。そしてまた、長時間ガラス転移温度以上の温
度にさらされることがないので、ガラスに失透が
生ずる心配もない。
加熱温度はガラスチユーブ及びガラスロツドを
103〜108ポイズの範囲の粘度に保持できる温度域
であることが好ましい。ガラスの粘度が103ポイ
ズより低くなると、両ガラスの失透傾向が増大し
たり、得られるフアイバーの真円度が低下するこ
とがある。また、ガラスの粘度が108ポイズより
高い場合は、ガラスが粘性流動しにくくなるた
め、紡糸に要するルツボ内圧及び／又は荷重を増
大しなければならず、このためにフアイバー径の
制御が困難になるうえ、紡糸に際しての線引き速
度が遅くなり、生産性が低下する。
紡糸ノズルの近傍に位置するガラスチユーブと
ガラスロツドは上記の温度域に加熱され、紡糸ノ
ズルから同時に紡糸される。この場合、ガラスチ
ユーブ及びガラスロツドに格別荷重をかけなくて
も、それぞれの自重のみで紡糸することができる
が、加熱温度に於けるガラスチユーブ及びガラス
ロツドの粘度が異なる場合は、その粘度差に応じ
て内側ルツボの内圧と外側ルツボの内圧をそれぞ
れ不活性ガスにて加圧することにより、また粘度
差がない場合は、内側ルツボの内圧と外側ルツボ
の内圧を同じ圧力に不活性ガスで加圧することに
より、紡糸温度を下げ、紡糸に際してのガラスの
失透を抑制することができる。しかし、その場合
でも不活性ガス圧力は５Kg／cm2以下、好ましくは
0.1〜３Kg／cm2の範囲とすべきであつて、５Kg／
cm2を越える過剰加圧はフアイバー径の制御を困難
にし、フアイバーの真円度を低下させる。
また、加熱温度に於けるガラスチユーブ及びガ
ラスロツドの粘度が著しく異なる場合及び得られ
るフアイバーのコア径とクラツド径の比率を厳密
に制御したい場合には、ガラスチユーブ及びガラ
スロツドの上端にそれぞれ独立の荷重を加えるこ
とが有効である。しかし、余り荷重をかけ過ぎる
とガラスチユーブやガラスロツドが破壊される虞
れがあり、フアイバー径の制御も困難になるの
で、荷重の上限は10Kg／cm2程度とすることが適当
である。
［実施例］
次に本発明の方法を実施例に基づいてさらに詳
細に説明する。
実施例 １
第１図に示した構成の装置を使用して、本発明
の方法に従いコア−クラツド構造を有するカルコ
ゲナイドガラスフアイバーを製造した。
まず、フランジ１８の部分で装置の上部を下部
から取りはずし、Ge：25モル％、Se：13モル％、
Te：60モル％、Tl：２モル％の組成で、直径9.5
mm、長さ120mmのコア用ガラスロツド３と、Ge：
24モル％、Se：16モル％、Te：60モル％の組成
で、内径13mm、外径17.5mm、長さ120のクラツド
用ガラスチユーブ４を、第１図に示すように、底
部に紡糸ノズルを備えた二重ルツボの内側ルツボ
１及び外側ルツボ２の中にそれぞれ垂直に収容し
た。ガラスロツド３には５Kg／cm2の荷重−Ａを、
ガラスチユーブ４には20Kg／cm2の荷重−Ｂを加え
た後、耐圧ゴムチユーブ１６及びゴムパツキン１
７を介してフランジ１８を閉じ、二重ルツボの内
部及びその外周をアルゴンガスで充分置換した。
その後、二重ルツボ内への不活性ガス入口７及
び８を閉じ、二重ルツボの紡糸ノズル近傍のみを
局部的に加熱できるヒーター１１を徐々に285℃
まで昇温する。この昇温によつてルツボ内のガラ
スチユーブとガラスロツドの先端は流動化するの
で、不活性ガスにて内側ルツボ１内を、0.5Kg／
cm2に、また外側ルツボ２内を0.8Kg／cm2に加圧し、
流動化したガラスチユーブとガラスロツドをルツ
ボ底部の紡糸ノズルから同様に引き出した。こう
して得られたフアイバーを直ちにコーター１２に
導いて紫外線硬化型樹脂１３をフアイバーにコー
テイングした後、紫外線ランプ１４にて樹脂を硬
化させることにより、コア径420μm、クラツド径
550μm、樹脂コーテイング厚30μm、長さ20mの
カルコゲナイドガラスフアイバーを得た。このフ
アイバーの透過損失値の波長依存性を第２図に示
す。また、フアイバーのガラス組成、紡糸条件及
び最低透過損失値をまとめて第１表に示す。
実施例 ２〜４
ガラス組成及び紡糸条件を第１表に示すごとく
変更した以外は実施例１と同様な方法でコア−ク
ラツド型カルコゲナイドガラスフアイバーを調製
した。各フアイバー径、紡糸条件、最低透過損値
及びその波長を第１表に示す。
比較例 １、２
実施例１及び４でコアに用いたガラスロツドの
みを第１図に示す装置の内側ルツボ１に入れ、ガ
ラスチユーブを使用しなかつた以外は実施例１と
同様な方法で樹脂クラツドフアイバーを製造し
た。この場合の紡糸条件及びフアイバー径も第１
表に
[Industrial Field of Application] The present invention relates to a method for producing a chalcogenide glass fiber having a core-clad structure with excellent infrared transparency. [Prior Art] Chalcogenide glass is a material for infrared fibers with excellent infrared transparency and weather resistance, and many glass compositions have already been reported (for example, ZU
Borisova, Glassy Semiconductor
Plenumpress, New York, 1981). Among these chalcogenide glass compositions, wavelengths around 10 μm,
In other words, the material that can transmit light in the wavelength range of carbon dioxide laser beams with low loss is the Ge-Se-Te system with a Te content of 50 mol% or more, and the creation of fibers is being considered (for example, , Toshio Katsuyama, Hiroyoshi Matsumura, Proceedings of the National Conference of the Institute of Electronics and Communication Engineers (March 1985) p4-256). However, glass fibers with high Te content have low mechanical strength, so they are of little practical use unless they are reinforced with resin coating or the like. However, since the wavelength around 10 μm is the fingerprint region of various resin materials, infrared rays in that wavelength region are absorbed. Therefore, such a resin material cannot be directly coated on the outer periphery of a chalcogenide glass fiber. This problem can be solved by forming a chalcogenide glass fiber into a core-clad double structure and then coating the outer periphery with a resin. A double crucible method is known as a method for producing glass fibers having a core-clad structure (Teruhisa Kanamori et al., Electronic Communication Research Institute, Research and Application Report, 32 (1983), 2737). This method involves inserting the core glass into an inner crucible and the cladding glass into an outer crucible, melting them, and simultaneously extruding both glasses from a spinning nozzle installed at the bottom of the double crucible to form a fiber. It is. However, as mentioned above, chalcogenide glass systems with a high Te content of 50 mol% have low thermal stability against crystallization, and chalcogenide glass systems that contain components with high vapor pressure such as As and Se,
It is difficult to regularly produce chalcogenide glass fibers with a core-clad structure using the above-mentioned double crucible method because compositional fluctuations occur due to evaporation of glass components at high temperatures. In addition, as a manufacturing method for glass fibers having a core-clad structure, there is a rod-in-tube method in which a rod-shaped glass core is inserted into a tube-shaped glass core, and the tip of the rod-shaped glass is melt-spun. , has traditionally been used in the production of quartz glass fibers. However, the viscosity of chalcogenide glass fluctuates significantly even with slight temperature changes, and spinning must be carried out in a non-oxidizing atmosphere, so the rod incubation method cannot be used as is to produce chalcogenide glass fibers. . [Problems to be Solved by the Invention] As mentioned above, even if the conventional rod incubation method or double crucible method is applied as is to chalcogenide glass, oxidation and devitrification of the glass occur during spinning. , the desired infrared transparent glass fiber cannot be obtained. The present invention is a new glass fiber manufacturing method that eliminates the problems of oxidation and devitrification that are a concern when spinning chalcogenide glass, and makes it possible to manufacture fibers with a core-clad structure with excellent infrared transparency from chalcogenide glass. I will provide a. [Means for Solving the Problems] The glass fiber manufacturing method according to the present invention includes a chalcogenide glass rod in the inner crucible of a cylindrical double crucible having a spinning nozzle at the bottom, and a chalcogenide glass rod in the outer crucible having a refractive index higher than that of the glass rod. Insert a chalcogenide glass tube with a low temperature, maintain the inside and outside of the crucible in an inert gas atmosphere, and simultaneously heat the tube and rod near the spinning nozzle to a temperature higher than the glass transition temperature. The method consists of obtaining a chalcogenide glass fiber having a core-clad structure by drawing it out from a spinning nozzle of a crucible. [Function] In the method of the present invention, when heating the glass tube and glass rod located near the spinning nozzle, the interior of the double crucible and the vicinity of the nozzle on the outer periphery of the crucible are sufficiently replaced with inert gas in advance. This is desirable. If this replacement is insufficient, the glass tube and glass rod may be corroded by water vapor and oxygen during heating. Heating is performed by maintaining the interior of the double crucible and the vicinity of the spinning nozzle of the crucible in an inert gas atmosphere, and locally heating the glass tube and glass rod located near the spinning nozzle, so that these are heated above the glass transition temperature. After fluidization, the material is immediately spun by the gas pressure in the crucible and/or the load applied to the glass tube and glass rod. Therefore, the glass is not attacked by oxygen during the spinning process, and the fibers are not cut. Furthermore, since the glass is not exposed to temperatures above the glass transition temperature for a long period of time, there is no fear that the glass will devitrify. The heating temperature depends on the glass tube and glass rod.
The temperature range is preferably such that the viscosity can be maintained within the range of 10 3 to 10 8 poise. When the viscosity of the glass is lower than 10 3 poise, the tendency of both glasses to devitrify increases, and the circularity of the resulting fiber may decrease. In addition, if the viscosity of the glass is higher than 108 poise, the glass becomes difficult to viscous flow, so the crucible internal pressure and/or load required for spinning must be increased, which makes it difficult to control the fiber diameter. Furthermore, the drawing speed during spinning becomes slow, resulting in a decrease in productivity. The glass tube and glass rod located in the vicinity of the spinning nozzle are heated to the above temperature range, and are simultaneously spun from the spinning nozzle. In this case, the glass tube and the glass rod can be spun using their own weight without any special load, but if the viscosity of the glass tube and glass rod differs at the heating temperature, depending on the viscosity difference, By pressurizing the inner pressure of the inner crucible and the inner pressure of the outer crucible with inert gas, or if there is no viscosity difference, by pressurizing the inner pressure of the inner crucible and the inner pressure of the outer crucible to the same pressure with inert gas. , it is possible to lower the spinning temperature and suppress devitrification of glass during spinning. However, even in that case, the inert gas pressure should be 5Kg/ cm2 or less, preferably
It should be in the range of 0.1-3Kg/ cm2 , and 5Kg/cm2.
Excessive pressurization exceeding cm 2 makes it difficult to control the fiber diameter and reduces the circularity of the fiber. In addition, if the viscosity of the glass tube and glass rod at the heating temperature is significantly different, or if you want to strictly control the ratio of the core diameter to the cladding diameter of the resulting fiber, apply independent loads to the upper ends of the glass tube and glass rod. It is effective to add However, if too much load is applied, there is a risk that the glass tube or glass rod will be destroyed, and control of the fiber diameter will be difficult, so it is appropriate to set the upper limit of the load to about 10 kg/cm 2 . [Examples] Next, the method of the present invention will be explained in more detail based on Examples. Example 1 A chalcogenide glass fiber having a core-clad structure was manufactured according to the method of the present invention using an apparatus having the configuration shown in FIG. First, remove the upper part of the device from the lower part at the flange 18, Ge: 25 mol%, Se: 13 mol%,
Composition of Te: 60 mol%, Tl: 2 mol%, diameter 9.5
mm, glass rod 3 for the core with a length of 120 mm, and Ge:
A glass tube 4 for cladding with a composition of 24 mol%, Se: 16 mol%, and Te: 60 mol%, with an inner diameter of 13 mm, an outer diameter of 17.5 mm, and a length of 12 mm, is equipped with a spinning nozzle at the bottom as shown in Figure 1. They were housed vertically in the inner crucible 1 and the outer crucible 2 of a double crucible equipped with a. A load of 5Kg/cm 2 is applied to glass rod 3.
After applying a load -B of 20 kg/cm 2 to the glass tube 4, the pressure-resistant rubber tube 16 and the rubber gasket 1 are
The flange 18 was closed via the flange 7, and the inside of the double crucible and its outer periphery were sufficiently replaced with argon gas. Thereafter, the inert gas inlets 7 and 8 into the double crucible are closed, and the heater 11, which can locally heat only the vicinity of the spinning nozzle of the double crucible, is gradually heated to 285°C.
Increase the temperature to. This temperature rise fluidizes the tips of the glass tube and glass rod inside the crucible, so the inside of the inner crucible 1 is heated by 0.5 kg/kg using inert gas.
cm2 , and the inside of the outer crucible 2 is pressurized to 0.8Kg/ cm2 ,
The fluidized glass tube and glass rod were similarly drawn out from the spinning nozzle at the bottom of the crucible. The fiber thus obtained is immediately introduced into the coater 12 to coat the fiber with an ultraviolet curable resin 13, and then cured with an ultraviolet lamp 14 to create a core diameter of 420 μm and a cladding diameter of 420 μm.
A chalcogenide glass fiber of 550 μm, resin coating thickness of 30 μm, and length of 20 m was obtained. FIG. 2 shows the wavelength dependence of the transmission loss value of this fiber. Further, the glass composition of the fiber, spinning conditions, and minimum transmission loss value are summarized in Table 1. Examples 2 to 4 Core-clad chalcogenide glass fibers were prepared in the same manner as in Example 1, except that the glass composition and spinning conditions were changed as shown in Table 1. Table 1 shows each fiber diameter, spinning conditions, minimum transmission loss value, and its wavelength. Comparative Examples 1 and 2 Only the glass rods used for the cores in Examples 1 and 4 were placed in the inner crucible 1 of the apparatus shown in Figure 1, and resin cracking was carried out in the same manner as in Example 1, except that the glass tube was not used. Manufactured Tudo fiber. The spinning conditions and fiber diameter in this case are also
on the table
【表】
示す。また、比較例１で得られた樹脂クラツドフ
アイバーの透過損失値の波長依存性を第２図に示
す。第２図から明らかな通り、樹脂クラツドフア
イバーは、波長５〜11μmの領域で樹脂による吸
収が生じているため、透過損失値は5dB／ｍ程度
増加した。
［効 果］
本発明の方法によれば、結晶化に対して安定で
ないために、従来のロツドインチユーブ法が二重
ルツボ法では製造が不可能であつたコア−クラツ
ド型カルコゲナイドガラスフアイバーを、ガラス
の酸化や失透を伴わずに製造することができる。
そして、コア−クラツド型カルコゲナイドガラス
フアイバーは、これに樹脂をコーテイングしても
赤外透過性が損われることがないので、本発明の
方法はカルコゲナイドガラスフアイバーの実用性
を高めるうえで極めて有益である。[Table] Shown. Further, the wavelength dependence of the transmission loss value of the resin-clad fiber obtained in Comparative Example 1 is shown in FIG. As is clear from FIG. 2, in the resin-clad fiber, absorption by the resin occurs in the wavelength range of 5 to 11 μm, so the transmission loss value increased by about 5 dB/m. [Effects] According to the method of the present invention, core-clad chalcogenide glass fibers, which could not be produced by the conventional rod incubation method or the double crucible method because they are not stable against crystallization, can be produced. can be produced without oxidation or devitrification of the glass.
Furthermore, since the core-clad chalcogenide glass fiber does not lose its infrared transmittance even if it is coated with resin, the method of the present invention is extremely useful in increasing the practicality of the chalcogenide glass fiber. .
第１図は本発明の実施例で使用したフアイバー
製造装置の概略断面図である。第２図は実施例１
及び比較例１で得たガラスフアイバーの透過損失
値の波長依存性を示すグラフである。
１：内側ルツボ、２：外側ルツボ、３：コア用
ガラスロツド、４：クラツド用ガラスチユーブ、
５：荷重−Ａ、６：荷重−Ｂ、７：内側ルツボ加
圧用不活性ガス入口、８：外側ルツボ加圧用不活
性ガス入口、９：ルツボ外周雰囲気制御用不活性
ガス入口、１０：ルツボ外周雰囲気制御用不活性
ガス出口、１１：局部加熱用ヒーター、１２：コ
ーター、１３：紫外線硬化型樹脂、１４：紫外線
ランプ、１５：プリントローラー、１６：耐圧ゴ
ムチユーブ、１７：ゴムパツキン、１８：フラン
ジ。
FIG. 1 is a schematic cross-sectional view of a fiber manufacturing apparatus used in an example of the present invention. Figure 2 shows Example 1
2 is a graph showing the wavelength dependence of the transmission loss value of the glass fiber obtained in Comparative Example 1. 1: Inner crucible, 2: Outer crucible, 3: Glass rod for core, 4: Glass tube for cladding,
5: Load-A, 6: Load-B, 7: Inert gas inlet for pressurizing the inner crucible, 8: Inert gas inlet for pressurizing the outer crucible, 9: Inert gas inlet for controlling the crucible periphery atmosphere, 10: Crucible periphery Inert gas outlet for atmosphere control, 11: Heater for local heating, 12: Coater, 13: Ultraviolet curing resin, 14: Ultraviolet lamp, 15: Print roller, 16: Pressure-resistant rubber tube, 17: Rubber packing, 18: Flange.
Claims (1)
の内側ルツボにカルコゲナイドガラスロツドを、
外側ルツボに該ガラスロツドよりも屈折率が低い
カルコゲナイドガラスチユーブをそれぞれ挿入
し、ルツボ内部及びルツボ外部を不活性ガス雰囲
気に保持し、紡糸ノズル近傍のチユーブ及びロツ
ドのみをガラス転移温度よりも高い温度に加熱し
ながらガラスチユーブとガラスロツドを同時にル
ツボの紡糸ノズルから引き出すことを特徴とする
コア−クラツド構造を有するカルコゲナイドガラ
スフアイバーの製造方法。 ２ チユーブ及びロツドの加熱温度がこれらを
103〜108ポイズの粘度に保持できる温度であるこ
とを特徴とする特許請求の範囲第１項記載の方
法。 ３ ルツボ内のチユーブ及びロツドを加熱するに
際して、内側ルツボ内及び外側ルツボ内をそれぞ
れ独立に不活性ガスにて加圧することを特徴とす
る特許請求の範囲第１項記載の方法。 ４ ルツボ内の不活性ガスの圧力が５Kg／cm2以下
であることを特徴とする特許請求の範囲第３項記
載の方法。 ５ ルツボ内のチユーブ及びロツドを加熱するに
際して、チユーブ及びロツドの上端にそれぞれ荷
重をかけることを特徴とする特許請求の範囲第１
項又は第３項記載の方法。 ６ チユーブ及びロツドの上端にかける荷重が10
Kg／cm2以下であることを特徴とする特許請求の範
囲第５項記載の方法。[Claims] 1. A chalcogenide glass rod is placed in the inner crucible of a cylindrical double crucible with a spinning nozzle at the bottom.
A chalcogenide glass tube with a refractive index lower than that of the glass rod is inserted into the outer crucible, the inside and outside of the crucible are maintained in an inert gas atmosphere, and only the tube and rod near the spinning nozzle are heated to a temperature higher than the glass transition temperature. A method for producing a chalcogenide glass fiber having a core-clad structure, which comprises simultaneously drawing out a glass tube and a glass rod from a spinning nozzle of a crucible while heating. 2 The heating temperature of the tube and rod
The method according to claim 1, characterized in that the temperature is such that the viscosity can be maintained at a viscosity of 10 3 to 10 8 poise. 3. The method according to claim 1, wherein when heating the tubes and rods in the crucible, the inside of the inner crucible and the inside of the outer crucible are independently pressurized with an inert gas. 4. The method according to claim 3, wherein the pressure of the inert gas in the crucible is 5 kg/cm 2 or less. 5. Claim 1, characterized in that when heating the tube and rod in the crucible, a load is applied to the upper ends of the tube and rod, respectively.
or the method described in paragraph 3. 6 The load applied to the upper end of the tube and rod is 10
The method according to claim 5, characterized in that the amount is less than Kg/cm 2 .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6810587A JPS63236729A (en) | 1987-03-24 | 1987-03-24 | Production of chalcogenide glass fiber having core clad structure |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP6810587A JPS63236729A (en) | 1987-03-24 | 1987-03-24 | Production of chalcogenide glass fiber having core clad structure |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63236729A JPS63236729A (en) | 1988-10-03 |
| JPH0527577B2 true JPH0527577B2 (en) | 1993-04-21 |
Family
ID=13364126
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP6810587A Granted JPS63236729A (en) | 1987-03-24 | 1987-03-24 | Production of chalcogenide glass fiber having core clad structure |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63236729A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5879426A (en) * | 1996-08-12 | 1999-03-09 | The United States Of America As Represented By The Secretary Of The Navy | Process for making optical fibers from core and cladding glass rods |
| IT1288836B1 (en) * | 1996-11-19 | 1998-09-24 | Cselt Centro Studi Lab Telecom | ACTIVE SINGLE-MODE OPTICAL FIBERS AND PROCEDURE FOR THEIR REALIZATION |
| DE19963867C1 (en) | 1999-12-30 | 2001-06-13 | Schott Glas | Apparatus for re-melting glass rods e.g., semi-finished products comprises a sleeve, a crucible located below the sleeve and having a run-off, a heater for heating the inside of the crucible and a run-off sleeve connected to the crucible |
-
1987
- 1987-03-24 JP JP6810587A patent/JPS63236729A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63236729A (en) | 1988-10-03 |
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