JPH05352B2 - - Google Patents
Info
- Publication number
- JPH05352B2 JPH05352B2 JP25409984A JP25409984A JPH05352B2 JP H05352 B2 JPH05352 B2 JP H05352B2 JP 25409984 A JP25409984 A JP 25409984A JP 25409984 A JP25409984 A JP 25409984A JP H05352 B2 JPH05352 B2 JP H05352B2
- Authority
- JP
- Japan
- Prior art keywords
- base material
- particle size
- fluorine
- optical fiber
- 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.)
- Expired - Lifetime
Links
- 239000002245 particle Substances 0.000 claims description 42
- 239000000463 material Substances 0.000 claims description 35
- 239000011521 glass Substances 0.000 claims description 33
- 239000005373 porous glass Substances 0.000 claims description 25
- 238000000034 method Methods 0.000 claims description 21
- 239000013307 optical fiber Substances 0.000 claims description 20
- 239000010419 fine particle Substances 0.000 claims description 19
- 238000009826 distribution Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 11
- 238000003980 solgel method Methods 0.000 claims description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 3
- 239000000835 fiber Substances 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 31
- 229910052731 fluorine Inorganic materials 0.000 description 31
- 239000011737 fluorine Substances 0.000 description 31
- 238000005253 cladding Methods 0.000 description 10
- 239000002994 raw material Substances 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 4
- 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 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000000635 electron micrograph Methods 0.000 description 3
- 239000005049 silicon tetrachloride Substances 0.000 description 3
- 238000004438 BET method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000004334 fluoridation Methods 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910005793 GeO 2 Inorganic materials 0.000 description 1
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 229910004742 Na2 O Inorganic materials 0.000 description 1
- 229910004014 SiF4 Inorganic materials 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- ABTOQLMXBSRXSM-UHFFFAOYSA-N silicon tetrafluoride Chemical compound F[Si](F)(F)F ABTOQLMXBSRXSM-UHFFFAOYSA-N 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 238000004017 vitrification 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]
-
- 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]
- C03B37/016—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
-
- 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
- C03B2201/08—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant
- C03B2201/12—Doped silica-based glasses doped with boron or fluorine or other refractive index decreasing dopant doped with fluorine
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B2203/00—Fibre product details, e.g. structure, shape
- C03B2203/10—Internal structure or shape details
- C03B2203/22—Radial profile of refractive index, composition or softening point
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Glass Compositions (AREA)
Description
【発明の詳細な説明】
（産業上の利用分野）
本発明は光フアイバ用母材の製造方法に関し、
詳しくは、多孔質ガラス体を成長させ、その多孔
質ガラス体を高温に保たれた炉の中に保持する
か、または通過させ弗素添加、脱水、透明化する
工程を含む光フアイバ母材の製造方法に関し、上
記光フアイバ母材に弗素により屈折率分布を与え
る方法を提供するものである。DETAILED DESCRIPTION OF THE INVENTION (Industrial Application Field) The present invention relates to a method for manufacturing an optical fiber base material,
Specifically, the production of an optical fiber base material, which includes the steps of growing a porous glass body, holding the porous glass body in a furnace kept at high temperature, or passing the porous glass body through it to add fluoridation, dehydrate it, and make it transparent. Regarding the method, the present invention provides a method for imparting a refractive index distribution to the optical fiber base material using fluorine.
（従来の技術）
光フアイバ母材に弗素により屈折率分布を与え
る方法として既にいくつかの提案がなされてき
た。第１の方法は気相軸付時に屈折率分布を作ろ
うとするもので、第６図に示される。６１は光フ
アイバのコアとなる部分６４の原料を流すガラス
微粒子合成バーナで、ここにはガラス微粒子原料
である四塩化珪素等を流す。６２は光フアイバの
クラツド６５となる部分の原料を流すガラス微粒
子合成バーナであつて、ここにはガラス微粒子原
料とともに弗素原料を流す。６３はガラス微粒子
が付着してできた多孔質ガラス母材である。しか
しながら、この方法では弗素が拡散し多孔質ガラ
ス母材に一様に添加されてしまい、屈折率分布を
作ることがてきなかつた。(Prior Art) Several proposals have already been made as a method of imparting a refractive index distribution to an optical fiber base material using fluorine. The first method attempts to create a refractive index distribution during vapor phase alignment, and is shown in FIG. Reference numeral 61 denotes a glass fine particle synthesis burner through which a raw material for a portion 64 that will become the core of the optical fiber is passed, and silicon tetrachloride, etc., which is a raw material for glass fine particles, is flowed here. Reference numeral 62 denotes a glass fine particle synthesis burner through which the raw material for the optical fiber cladding 65 is passed, and a fluorine raw material is flowed therein together with the glass fine particle raw material. 63 is a porous glass base material to which glass fine particles are attached. However, in this method, fluorine diffuses and is uniformly added to the porous glass base material, making it impossible to create a refractive index distribution.
第２の方法は、第７図に示される。多孔質ガラ
ス母材は、コア７４にGeO2，P2O5等透明ガラス
化温度を下げる物質を多く含むように作られてい
る。この母材を高温に保たれた炉７７中に挿入す
ると、コア７４はクラツド７５よりも早く収縮す
るため、弗素原料の濃度および弗素添加する期間
を選べば、クラツドのみに弗素を添加し、光フア
イバ母材に屈折率分布を作ることが可能である。
しかしながら、この方法では、屈折率分布を作る
ことはできるものの原理的に純シリカコアの光フ
アイバ母材を作ることが不可能で、弗素によつて
屈折率分布をつけたフアイバの特長を生かしきれ
ないという欠点があつた。 A second method is illustrated in FIG. The porous glass base material is made so that the core 74 contains a large amount of substances such as GeO 2 and P 2 O 5 that lower the transparent vitrification temperature. When this base material is inserted into a furnace 77 kept at a high temperature, the core 74 will shrink faster than the cladding 75, so if the concentration of the fluorine raw material and the period of fluorine addition are selected, fluorine can be added only to the cladding and the core 74 can be exposed to light. It is possible to create a refractive index profile in the fiber matrix.
However, with this method, although it is possible to create a refractive index distribution, it is theoretically impossible to create an optical fiber base material with a pure silica core, and it is not possible to take advantage of the characteristics of a fiber with a refractive index distribution created by fluorine. There was a drawback.
第３の方法は昭和59年度電子通信学会光電波部
門全国大会予稿集２−183などにおいて提案され
た方法であつて、多孔質ガラス母材は、コアとな
る部分とクラツドとなる部分とでは、カサ密度を
変えて作られている。この母材に高温炉中で弗素
添加を行なうと、弗素の拡散しやすいクラツドに
より多くの弗素が添加され、コアとの間に屈折率
差を生じる。この方法で、コア−クラツド間に比
屈折率差0.3％を付けるためには、クラツドのカ
サ密度を〜0.2ｇ／cm3、コアのカサ密度を1.5ｇ／
cm3より大とする必要がある。ところが、カサ密度
1.5ｇ／cm3以上の多孔質ガラス母材から光フアイ
バの伝送損失要因である残留水分を除去すること
は極めて困難であるという欠点があつた。 The third method is the method proposed in Proceedings of the 1983 National Conference of the Institute of Electronics and Communication Engineers, Photo-Radio Division, Proceedings 2-183. They are made with different bulk densities. When fluorine is added to this base material in a high-temperature furnace, more fluorine is added to the cladding, where fluorine easily diffuses, creating a refractive index difference between the cladding and the core. In order to achieve a relative refractive index difference of 0.3% between the core and the cladding using this method, the bulk density of the cladding must be ~0.2 g/cm 3 and the bulk density of the core must be 1.5 g/cm 3 .
Must be larger than cm 3 . However, the bulk density
A drawback is that it is extremely difficult to remove residual moisture, which is a factor in optical fiber transmission loss, from a porous glass base material of 1.5 g/cm 3 or more.
（発明が解決しようとする問題点）
本発明は、上記にて説明した現状に鑑み、従来
法の欠点を解消し、光伝送路として有効な屈折率
分布を持ち、かつ十分に脱水された、光フアイバ
用母材の製造方法を提供することを目的とする。(Problems to be Solved by the Invention) In view of the current situation described above, the present invention solves the drawbacks of the conventional method, and provides a method that has a refractive index distribution effective as an optical transmission path and is sufficiently dehydrated. An object of the present invention is to provide a method for manufacturing a base material for optical fiber.
（問題点を解消するための手段）
本発明は第１図ａ，ｂに示すように多孔質ガラ
ス体を構成するガラス微粒子の粒径を多孔質ガラ
ス体の径方向に変化させることによつて、弗素添
加量を制御しうるという本発明者らの得た知見に
基く、光フアイバ母材に屈折率分布をつける新規
な方法である。(Means for Solving the Problems) The present invention, as shown in FIGS. This is a novel method for imparting a refractive index distribution to an optical fiber base material, based on the knowledge obtained by the present inventors that the amount of fluorine added can be controlled.
すなわち、本発明は多孔質ガラス体を高温に保
たれた炉の中に保有するかまたは通過させて、弗
素添加・脱水・透明化を行ない光フアイバ用母材
を製造する方法において、上記多孔質ガラス体を
形成するガラス微粒子の粒径を多孔質ガラス体の
径方向に変化させ、それにより上記高温炉内で多
孔質ガラス体に添加される弗素量に径方向の分布
をつけることを特徴とする光フアイバ用母材の製
造方法である。 That is, the present invention provides a method for manufacturing an optical fiber base material by holding a porous glass body in a furnace kept at a high temperature or passing it through the furnace to perform fluoridation, dehydration, and transparency. The particle size of the glass fine particles forming the glass body is changed in the radial direction of the porous glass body, thereby giving a radial distribution to the amount of fluorine added to the porous glass body in the high temperature furnace. This is a method for manufacturing an optical fiber base material.
本発明者らは、ガラス微粒子の粒径と弗素添加
量の関係を調べるために、次の２種類の実験を行
つた。 The present inventors conducted the following two types of experiments in order to investigate the relationship between the particle size of glass fine particles and the amount of fluorine added.
まず第１に、粒径（nm）を変えた数種の多孔
質ガラスを作成し、その透明化温度（℃）を測定
し、得られた結果を第２図に示した。 First, several types of porous glasses with different particle sizes (nm) were prepared, and their transparentization temperatures (°C) were measured. The obtained results are shown in Figure 2.
ここで多孔質ガラスの作成法と粒径の関係につ
いて説明する。一酸化炭素炎（CO炎）またはプ
ラズマ炎では、水素が存在しないので、下記(1)式
のような反応が生起していると考えられる。 Here, the relationship between the method for producing porous glass and the particle size will be explained. In carbon monoxide flame (CO flame) or plasma flame, since hydrogen is not present, it is thought that the reaction shown in equation (1) below occurs.
SiCl4＋O2→SiO2＋2Cl2 ……(1)
一方、酸水素炎による場合は、下記(2)式のよう
な反応が考えられる。 SiCl 4 +O 2 →SiO 2 +2Cl 2 ...(1) On the other hand, in the case of oxyhydrogen flame, a reaction as shown in equation (2) below can be considered.
SiCl4＋2H2＋O2→SiO2＋4HCl ……(2)
以上のようにCO炎またはプラズマ炎を使用し
た場合と、酸水素炎使用の場合とでは、炎中での
反応自体が異なり、この結果、得られたガラス微
粒子の粒径が異なることを、本発明者らは詳細な
実験により確認した。また、ゾルゲル法の場合は
材料として、市販の粒径既知のSiO2微粒子を用
いることにより粒径を制御できる。 SiCl 4 +2H 2 +O 2 →SiO 2 +4HCl ……(2) As mentioned above, the reaction itself in the flame is different when using a CO flame or plasma flame and when using an oxyhydrogen flame. The present inventors confirmed through detailed experiments that the obtained glass fine particles had different particle sizes. In addition, in the case of the sol-gel method, the particle size can be controlled by using commercially available SiO 2 fine particles of known particle size as the material.
第２図においては、ガラス微粒子粒径120nmは
酸水素炎にて、70nmはプラズマ炎にて、60nmは
CO炎にて、10nmはゾルゲル法にてそれぞれ合成
したものを用いた。 In Figure 2, glass fine particles with a particle size of 120 nm are measured using an oxyhydrogen flame, 70 nm using a plasma flame, and 60 nm using an oxyhydrogen flame.
The 10 nm samples were synthesized using the sol-gel method using a CO flame.
第２図から明らかなように、粒径100nmのガラ
ス微粒子からなる多孔質ガラス母材の透明化には
1600℃以上が必要であるが、粒径10nmの粒子か
らなる多孔質ガラス母材は1300℃で透明化でき
た。 As is clear from Figure 2, it is difficult to make a porous glass base material made of glass fine particles with a particle size of 100 nm transparent.
Although a temperature of 1600°C or higher is required, a porous glass base material consisting of particles with a particle size of 10 nm could be made transparent at 1300°C.
第２、SiO2多孔質ガラスに弗素添加をするに
あたり、弗素原料（SF6及びSiF4）を流す際の高
温炉の温度を変化させ、弗素添加量を比屈折率差
として測定したところ、第３図に示すような結果
が得られた。第３図において、
PSF6，PSiF4：弗素原料の分圧
ｔ：弗素添加時間（時間）
Ｔ：弗素添加温度（℃）
△ｎ（Ｆ）：比屈折率差 である。 Second, when adding fluorine to SiO 2 porous glass, we varied the temperature of the high-temperature furnace when flowing the fluorine raw materials (SF 6 and SiF 4 ) and measured the amount of fluorine added as a relative refractive index difference. The results shown in Figure 3 were obtained. In FIG. 3, P SF6 , P SiF4 : partial pressure of fluorine raw material t: fluorine addition time (hours) T: fluorine addition temperature (°C) △n(F): relative refractive index difference.
第３図から明らかなように、温度条件と弗素添
加量との関係において、SF6とSiF4では違いは見
られなかつた。 As is clear from FIG. 3, no difference was observed between SF 6 and SiF 4 in the relationship between temperature conditions and the amount of fluorine added.
本発明者等が、以上の結果を検討した結果、次
のようなことが判明した。すなわち、粒径が小さ
いガラス微粒子でできた多孔質ガラス母材は透明
化が比較的低温で完了するため弗素添加量は小さ
くなる。これに対して、粒径が大きいガラス微粒
子でできたガラス母材は、比較的高温まで透明化
が完了しないため、弗素添加量は大きくなる。 As a result of the inventors' study of the above results, the following findings were found. That is, since transparency of a porous glass base material made of glass fine particles with a small particle size is completed at a relatively low temperature, the amount of fluorine added is small. On the other hand, a glass base material made of fine glass particles with a large particle size does not become completely transparent until a relatively high temperature, so the amount of fluorine added becomes large.
したがつて、多孔質ガラス体のガラス微粒子に
径方向の粒径分布をつければ、弗素添加量も径方
向に分布させることができる。 Therefore, if the glass particles of the porous glass body are given a radial particle size distribution, the amount of fluorine added can also be distributed in the radial direction.
ガラス微粒子を径方向に粒径分布をつける手段
としては、上述のようにガラス微粒子を作成する
方法を、酸水素炎、CO炎、プラズマ炎あるいは
ゾルゲル法等により条件を変化させたり、各方法
を組合せることにより可能である。 As a means of creating particle size distribution in the radial direction of glass fine particles, the method of creating glass fine particles as described above can be changed by changing the conditions using oxyhydrogen flame, CO flame, plasma flame, sol-gel method, etc., or by using each method. This is possible by combining them.
〈実施例〉
実施例 １
第４図のような配置で出発材を引上げつつ出発
材４６にガラス微粒子を付着させていつた。コア
部分４４を作るバーナ４１には、一酸化炭素、酸
素、四塩化硅素を送りこみ酸化反応によつてガラ
ス微粒子を作成した。クラツド部４５を作るバー
ナ４２には、酸素、水素、四塩化硅素を送りこ
み、加水分解反応によつてガラス微粒子を作成し
た。バーナ４１によつて合成されたガラス微粒子
の粒径をBET法を用いて測定すると60nmであ
り、一方、バーナ４２によつて合成されたガラス
微粒子の粒径は120nmであつた。これらのガラス
微粒子の電子顕微鏡写真を第５図ａ及びｂに示
す。<Examples> Example 1 Glass particles were attached to the starting material 46 while the starting material was pulled up in the arrangement shown in FIG. Carbon monoxide, oxygen, and silicon tetrachloride were fed into the burner 41 for forming the core portion 44, and glass fine particles were formed by an oxidation reaction. Oxygen, hydrogen, and silicon tetrachloride were fed into the burner 42 forming the cladding part 45, and glass fine particles were produced by a hydrolysis reaction. The particle size of the glass particles synthesized by burner 41 was measured using the BET method and was 60 nm, while the particle size of the glass particles synthesized by burner 42 was 120 nm. Electron micrographs of these glass particles are shown in FIGS. 5a and 5b.
このようにして作られた多孔質ガラス母材を
SiF4のモル濃度が３％となるようなHe雰囲気中
で脱水・弗素添加・透明化を行なつたところ、コ
ア部の比屈折率差が−0.05％、クラツド部の比屈
折率が−0.32％の透明な光フアイバ用母材が得ら
れた。この光フアイバ用母材を線引後伝送損失特
性を測定した結果、0.2dB／Km（波長1.55μ）が得
られ、また波長1.38μでの水の吸収も1.5dB／Kmと
極めて小さかつた。 The porous glass base material made in this way
When dehydration, fluorine addition, and transparency were performed in a He atmosphere where the molar concentration of SiF 4 was 3%, the relative refractive index difference in the core part was -0.05%, and the relative refractive index in the cladding part was -0.32. % of a transparent optical fiber base material was obtained. As a result of measuring the transmission loss characteristics of this optical fiber base material after drawing, it was found that 0.2 dB/Km (wavelength 1.55 μ) was obtained, and the absorption of water at a wavelength of 1.38 μ was extremely small at 1.5 dB/Km. .
尚この実施例で示した一酸化炭素炎の代りにプ
ラズマ炎を用い酸化反応でコア部のガラス微粒子
を作成することも可能である。この場合粒径は
75nmであつた。電子顕微鏡写真を第５図ｃに示
す。また、SiF4の代りにSF6を用いて弗素添加を
行なつても同様の結果が得られている。 Incidentally, it is also possible to use a plasma flame instead of the carbon monoxide flame shown in this example to create the glass fine particles of the core portion through an oxidation reaction. In this case the particle size is
It was 75nm. An electron micrograph is shown in Figure 5c. Similar results were also obtained when fluorine was added using SF 6 instead of SiF 4 .
実施例 ２
ゾルゲル法を用いて径３mmφ、長さ90mmの多孔
質母材を作成した。BET法で求めた、この多孔
質母材の平均粒子粒は15nmであつた。この多孔
質母材の外側にVAD法（加水分解反応）で作成
したガラス微粒子（粒径110nm）を外付けし、
SiF4濃度が30％のHe雰囲気中で脱水・弗素添
加・透明化を行なつた。得られた光フアイバ用母
材は透明で気泡を含まず、コア部の比屈折率差は
−0.02％、クラツド部の比屈折率差は−0.5％で
あつた。Example 2 A porous base material with a diameter of 3 mmφ and a length of 90 mm was created using the sol-gel method. The average particle size of this porous base material determined by the BET method was 15 nm. Glass particles (particle size 110 nm) made by VAD method (hydrolysis reaction) are attached to the outside of this porous base material.
Dehydration, fluorine addition, and transparency were performed in a He atmosphere with a SiF 4 concentration of 30%. The obtained optical fiber base material was transparent and did not contain bubbles, and the relative refractive index difference in the core portion was -0.02%, and the relative refractive index difference in the cladding portion was -0.5%.
（発明の効果）
以上に記したように、径方向に粒径分布を持つ
多孔質ガラス母材に、高温炉中で弗素添加を行な
うことにより、）屈折率分布を作ることがで
き、）コアは微量の弗素以外の添加物を含ま
ず、）OH吸収の少ない光フアイバ用母材を製
造することが可能となつた。(Effects of the invention) As described above, by adding fluorine to a porous glass base material having a particle size distribution in the radial direction in a high-temperature furnace, it is possible to create a refractive index distribution, and a core contains no additives other than trace amounts of fluorine, making it possible to produce optical fiber base materials with low OH absorption.
第１図ａおよびｂは本発明における多孔質ガラ
ス体の径方向のガラス微粒子粒径分布を示す図、
第２図は粒径と透明化温度の関係を示すグラフ、
第３図は弗素添加量と添加時の温度の関係を示す
グラフ、第４図、第６図および第７図は本発明の
実施態様を説明する図、第５図ａ〜ｃは本発明の
実施例で得られた多孔質母材のガラス微粒子の粒
子構造を示す電子顕微鏡写真である（倍率3000
倍）。第６図及び第７図は従来法の説明図である。
FIGS. 1a and 1b are diagrams showing the particle size distribution of glass fine particles in the radial direction of the porous glass body in the present invention,
Figure 2 is a graph showing the relationship between particle size and clearing temperature.
Figure 3 is a graph showing the relationship between the amount of fluorine added and the temperature during addition; Figures 4, 6 and 7 are diagrams explaining embodiments of the present invention; Figures 5 a to c are graphs showing the relationship between the amount of fluorine added and the temperature during addition; This is an electron micrograph showing the particle structure of glass particles in the porous base material obtained in Examples (magnification: 3000).
times). FIGS. 6 and 7 are explanatory diagrams of the conventional method.
１ 重量百分率で、P2O570〜85％、Al2O313〜18
％、B2O3１〜６％、SiO20.2〜３％、Li2Ｏ＋Na2
Ｏ＋K2O0.3〜３％、MgO＋BaO＋SrO＋ZnO0.5
〜８％、CuO1〜５％からなる組成を有する近赤
外カツトフイルタガラス。
1 In weight percentage, P 2 O 5 70-85%, Al 2 O 3 13-18
%, B2O3 1-6 %, SiO2 0.2-3%, Li2O + Na2
O+ K2O0.3 ~3%, MgO+BaO+SrO+ZnO0.5
Near-infrared cut filter glass having a composition of ~8% CuO and 1~5% CuO.
Claims (1)
さいガラス微粒子でできた多孔質ガラス棒の外側
に、粒径の大きいガラス微粒子を外付けすること
によつて、粒径の径方向分布を作る特許請求の範
囲第１項記載の光フアイバ用母材の製造方法。 ７ 粒径の小さいガラス微粒子からなる多孔質ガ
ラス棒はゾルゲル法で作成される特許請求の範囲
第６項記載の光フアイバ用母材の製造方法。 ８ 粒径の小さいガラス微粒子からなる多孔質ガ
ラス棒はプラズマ炎を用いて作成される特許請求
の範囲第６項記載の光フアイバ用母材の製造方
法。 ９ 粒径の小さいガラス微粒子からなる多孔質ガ
ラス棒は、一酸化炭素炎を用いて作成される特許
請求の範囲第６項記載の光フアイバ用母材の製造
方法。Method for manufacturing fiber base material. 6. When producing the above porous glass body, the radial distribution of particle size can be controlled by externally attaching glass fine particles with a large particle size to the outside of a porous glass rod made of fine glass particles with a small particle size. A method for producing an optical fiber base material according to claim 1. 7. The method for producing an optical fiber base material according to claim 6, wherein the porous glass rod made of fine glass particles having a small particle size is produced by a sol-gel method. 8. The method for manufacturing an optical fiber base material according to claim 6, wherein the porous glass rod made of fine glass particles having a small particle size is produced using a plasma flame. 9. The method for producing an optical fiber base material according to claim 6, wherein the porous glass rod made of fine glass particles having a small particle size is produced using carbon monoxide flame.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25409984A JPS61132532A (en) | 1984-12-03 | 1984-12-03 | Method for manufacturing base material for optical fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP25409984A JPS61132532A (en) | 1984-12-03 | 1984-12-03 | Method for manufacturing base material for optical fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61132532A JPS61132532A (en) | 1986-06-20 |
| JPH05352B2 true JPH05352B2 (en) | 1993-01-05 |
Family
ID=17260206
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP25409984A Granted JPS61132532A (en) | 1984-12-03 | 1984-12-03 | Method for manufacturing base material for optical fiber |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61132532A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015227259A (en) * | 2014-05-30 | 2015-12-17 | 住友電気工業株式会社 | Production method of porous silica tube, and porous silica tube |
| JP6265961B2 (en) * | 2015-11-10 | 2018-01-24 | 古河電気工業株式会社 | Optical fiber preform manufacturing method |
-
1984
- 1984-12-03 JP JP25409984A patent/JPS61132532A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61132532A (en) | 1986-06-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP0249230B1 (en) | Glass preform for dispersion shifted single mode optical fiber and method for the production of the same | |
| EP0161680B1 (en) | Method for producing glass preform for optical fiber | |
| US5221309A (en) | Method for producing glass preform for optical fiber | |
| US4690504A (en) | Quartz glass-made optical fibers and a method for the preparation thereof | |
| JPS61117126A (en) | Method for manufacturing base material for optical fiber | |
| JPS60260434A (en) | Manufacture of anhydrous glass preform for optical transmission | |
| KR890001125B1 (en) | Quartz glass fiber optic fiber containing fluorine and P2O5 | |
| CA1266403A (en) | Method for producing glass preform for optical fiber containing fluorine in cladding | |
| JPH05352B2 (en) | ||
| JPS6022658B2 (en) | Fiber for optical communication | |
| KR100878709B1 (en) | How to make optical fiber by adjusting oxygen stoichiometry | |
| JPH0820574B2 (en) | Dispersion shift fiber and manufacturing method thereof | |
| JPS6090843A (en) | Manufacture of glass base material for optical fiber | |
| JPS6131324A (en) | Production of base material for optical fiber | |
| JPS6289B2 (en) | ||
| JPH01145346A (en) | Method for manufacturing base material for optical fiber | |
| JPS6081038A (en) | Manufacture of optical glass fiber containing tio2 | |
| JPH01275442A (en) | Production of optical fiber preform | |
| JPS6313946B2 (en) | ||
| JPS6051635A (en) | Quartz optical fiber | |
| JP2831842B2 (en) | Manufacturing method of optical fiber base material | |
| JPH0239457B2 (en) | ||
| JPH0525821B2 (en) | ||
| JPS59137333A (en) | Manufacture of base material for optical fiber | |
| JPS61251539A (en) | Optical fiber |