JPS59107936A - Manufacture of preform rod - Google Patents
Manufacture of preform rodInfo
- Publication number
- JPS59107936A JPS59107936A JP21907182A JP21907182A JPS59107936A JP S59107936 A JPS59107936 A JP S59107936A JP 21907182 A JP21907182 A JP 21907182A JP 21907182 A JP21907182 A JP 21907182A JP S59107936 A JPS59107936 A JP S59107936A
- Authority
- JP
- Japan
- Prior art keywords
- amount
- reaction
- gecl4
- quartz tube
- pipe
- 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
- 238000004519 manufacturing process Methods 0.000 title claims description 5
- 238000006243 chemical reaction Methods 0.000 claims abstract description 27
- 239000010453 quartz Substances 0.000 claims abstract description 16
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000012159 carrier gas Substances 0.000 claims abstract description 9
- 239000004071 soot Substances 0.000 claims abstract description 6
- 239000002019 doping agent Substances 0.000 claims abstract description 4
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 21
- 229910001882 dioxygen Inorganic materials 0.000 claims description 21
- 239000007789 gas Substances 0.000 claims description 12
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims 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 claims description 2
- 238000000151 deposition Methods 0.000 claims description 2
- 239000005049 silicon tetrachloride Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 10
- 229910006113 GeCl4 Inorganic materials 0.000 abstract description 8
- 238000009826 distribution Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 4
- 230000005540 biological transmission Effects 0.000 abstract description 4
- 239000001301 oxygen Substances 0.000 abstract description 4
- 229910052760 oxygen Inorganic materials 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000005229 chemical vapour deposition Methods 0.000 abstract description 2
- 229910003910 SiCl4 Inorganic materials 0.000 abstract 1
- FDNAPBUWERUEDA-UHFFFAOYSA-N silicon tetrachloride Chemical compound Cl[Si](Cl)(Cl)Cl FDNAPBUWERUEDA-UHFFFAOYSA-N 0.000 abstract 1
- 239000007858 starting material Substances 0.000 abstract 1
- 230000002459 sustained effect Effects 0.000 abstract 1
- 239000013307 optical fiber Substances 0.000 description 11
- 230000007423 decrease Effects 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002360 preparation method Methods 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]
- C03B37/018—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
- C03B37/01807—Reactant delivery systems, e.g. reactant deposition burners
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Geochemistry & Mineralogy (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Chemical & Material Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Light Guides In General And Applications Therefor (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
Description
【発明の詳細な説明】
（発明の技術分野）
本発明は、ｏｖｐ法によるプリフォームロッドの製造方
法に関する。DETAILED DESCRIPTION OF THE INVENTION (Technical Field of the Invention) The present invention relates to a method for manufacturing a preform rod by the OVP method.
（発明の技術的背景）
従来のＯＶＤ法によるブリ７オームロツドの製造方法に
おいては、原料ガスとしての四塩化ケイ素（ＳｔＯｊ＋
）やキャリアガスに水分が含まれ、又ガス供給系の装置
の気密性が不充分であること等から、水分の混入したブ
リフォームロブトしか得ることができなかった。このた
め、プリフォームロッドの脱ＯＨ塞化が種々前えられ、
例えば原料ガスやキャリアガスを石英管に導入する前に
別工程で予熱してその含まれている水分を除去する方法
などが考えられている。(Technical Background of the Invention) In the conventional method for producing 7-ohm rods using the OVD method, silicon tetrachloride (StOj+
) and the carrier gas, and the airtightness of the gas supply system was insufficient, so it was only possible to obtain pre-formed loaves containing moisture. For this reason, various methods of removing OH and clogging the preform rod are being carried out.
For example, a method has been considered in which the raw material gas or carrier gas is preheated in a separate process to remove the moisture contained therein before being introduced into the quartz tube.
（背景技術の問題点）
しかし、この方法は装置規模が大きくなり、また得られ
た光ファイバの伝送帯域が減少してしまう他の欠点が免
れない。(Problems with the Background Art) However, this method inevitably has other drawbacks such as an increase in the scale of the device and a decrease in the transmission band of the obtained optical fiber.
本発明者は、かかる従来の欠点を解消すべく研究を進め
、先ず、アルゴンキャリアガスを用いるＯＶＤ法にて、
原料組成である５ｉａｔ４、Ｇｅｃ／４（四塩化ゲルマ
ニウム）及びＰ ＯＯｚ。The present inventor has conducted research in order to eliminate such conventional drawbacks, and first, using the OVD method using argon carrier gas,
Raw material composition: 5iat4, Gec/4 (germanium tetrachloride) and POOz.
をそれぞれ６２ ｃｃ／ｍｉｎ ｓ １９ ｃｃ／ｍｉ
ｎ 、 ７ｃｃ／ｍｉｎの一定に保持し、反応用酸素ガ
ス量を０〜３００ Ｑ ｃｃ／ｍｉｎまで段階的に変化
させ、複数のブリ７オームロツドを作成した。そして、
各ロッドから光ファイバを製造して各ファイバの屈折率
と反応用酸素ガス量との関係を調べたところ、第１図に
示すように、反応用酸素ガス量の減少に伴なって未反応
のＧｅＣｌ４が増大して屈折率差が小さくなっていた。62 cc/min s 19 cc/mi respectively
A plurality of 7-ohm rods were prepared by keeping the reaction oxygen gas constant at 7 cc/min and changing the reaction oxygen gas amount stepwise from 0 to 300 Q cc/min. and,
When optical fibers were manufactured from each rod and the relationship between the refractive index of each fiber and the amount of reaction oxygen gas was investigated, as shown in Figure 1, as the amount of reaction oxygen gas decreased, unreacted GeCl4 increased and the refractive index difference became smaller.
また、反応用酸素ガス量を少なくして作成したプリフォ
ームロッドは水分量が非常に少なく、良好な結果が得ら
れた。これは未反応のａｅａｔ、が水分と反応し、脱水
作用を起こしたことが原因であった。In addition, the preform rod made with a reduced amount of reaction oxygen gas had a very low moisture content, and good results were obtained. This was caused by unreacted aeat reacting with moisture and causing dehydration.
次に、反応用酸素ガス量を８００ ｃｃ／ｍｉｎの一定
にして、ＣＶＤ法によりプリ７オームロツドを作成した
。作成条件としては、キャリアガスＡｔ２５０ ｃ Ｃ
１８１０ノ。を６６ ｃｃ／ｍｉｎ ｓ ＰＯＯＩＢ
を２ｃｃ／ｍｉｎの一定にし、スート堆積回数が１００
回になるまでＧｅＣ／４を０〜１５ ｃｃ／ｍｉｎの範
囲で順次増加させた。得られたプリ７オームロツドから
グレーデッドインデックス型光ファイバを製造し、その
水分を調べたところ、非常に少なく良好な結果が得られ
た。しかし、この得られた光ファイバは、その屈折率こ
う配αが２．５になり、第２図に示すように、屈折率分
布が計算値で示すα−２，０の理想分布（点線）からか
なりずれ、伝送帯域が減少していた。Next, a pre-7 ohm rod was produced by CVD with the amount of oxygen gas for reaction kept constant at 800 cc/min. The preparation conditions are carrier gas At250cC
1810 no. 66 cc/min s POOIB
was kept constant at 2 cc/min, and the number of soot depositions was 100.
The GeC/4 was increased sequentially in the range of 0 to 15 cc/min until the temperature reached 100 cc/min. A graded index optical fiber was manufactured from the obtained pre-7 ohm rod, and when the moisture content was examined, good results were obtained, with very little moisture. However, the obtained optical fiber has a refractive index gradient α of 2.5, and as shown in FIG. There was considerable deviation and the transmission band was reduced.
そこで、本発明者は、反応用酸素ガス量が一定の場合Ｇ
ｅ Ｃ７４の量が増えると酸素、ガス量が少なくなって
未反応ａｅａｔ、が増加し、屈折率分布がずれる点に注
目し、反応用酸素ガス量をＧｅＣ／４に比例させて増加
すれば未反応ＱｅＣ１４を最小に押さえることができ、
これにより屈折率分布のずれをなくして水分の除去を行
うことができることを見出した。Therefore, the inventor proposed that when the amount of oxygen gas for reaction is constant, G
e Note that as the amount of C74 increases, the amount of oxygen and gas decreases and unreacted aeat increases, and the refractive index distribution shifts.If the amount of oxygen gas for reaction is increased in proportion to GeC/4, The reaction QeC14 can be kept to a minimum,
It has been found that this makes it possible to remove moisture while eliminating deviations in the refractive index distribution.
（発明の目的）
本発明の目的は、装置規模を大きくせず、また伝送帯域
を減少させることなく水分の少ないブリ７オームロツド
を作成することができる方法を提供することにある。(Objective of the Invention) An object of the present invention is to provide a method capable of producing a 7-ohm rod with low moisture content without increasing the scale of the device or reducing the transmission band.
（発明の概要）
本発明は、アルゴンキャリアガスを用いるＣＶＤ法にお
いて、反応用酸素ガス量を、Ｇ ｅ ０１４の増加に比
例させて順次増大することを特徴とする。(Summary of the Invention) The present invention is characterized in that in a CVD method using an argon carrier gas, the amount of oxygen gas for reaction is gradually increased in proportion to the increase in G e 014.
（発明の実施例） 以下、本発明の詳細な説明する。(Example of the invention) The present invention will be explained in detail below.
先ず、石英管をガラス旋盤に取り付け、１分間に数十回
転の速度で回転させ、この石英管に、８ ｉＣｌ ４６
２ ＣＣ／ｆ２１ ＠ ｎ ｓ Ｐ ＯＣｊ ＠ ７
ＣＣ／ｍｉｎ 一定で導入すると共にＱｅ！ Ｃｚ、
を０〜３６ｃｃ／ｍｉｎまで変化させ、又反応用酸素ガ
スを１００ｃｃ／ｍｉｎから１０００ｃｃ／ｍｉｎまで
変化させて導入する。キャリアガスとしてアルゴンを用
いる。First, a quartz tube was attached to a glass lathe, rotated at a speed of several tens of revolutions per minute, and 8 iCl 46 was applied to the quartz tube.
2 CC/f21 @ n s P OCj @ 7
In addition to introducing constant CC/min, Qe! Cz,
The rate of reaction oxygen gas is varied from 0 to 36 cc/min, and the rate of reaction oxygen gas is varied from 100 cc/min to 1000 cc/min. Argon is used as a carrier gas.
反応用酸素ガス量は次式によって決定されているＯ
ｎ ｍ ａ ｘ ３
但し、Ｘ ｔはｉ層目のスートを堆積するのに用いる反
応用酸素ガス量、Ｇ ｅ ｉはｉ層目のスートを堆積す
るのに用いるＱｅＱｊ４流量、Ｘｍａｘは最終回にスー
トを作成するに用いる反応用酸素ガス量、ｏｅｍａｘ
は最終回にスートを作成するのに用いるＱｅＯｊ４流
量、Ｂｉｏｔ、及びＰＱＣｊＢはこれら原料ガスの反応
に必要な酸素ガス量をそれぞれ示す。The amount of oxygen gas for reaction is determined by the following formula: O n m a x 3 where, QeQj4 flow rate used to deposit, Xmax is the amount of reaction oxygen gas used to create soot in the final step, oemax
represents the QeOj4 flow rate used to create soot in the final step, Biot, and PQCjB each represent the amount of oxygen gas required for the reaction of these raw material gases.
次に、前記各ガスの導入と同時に１．加熱源としての酸
水素バーナを原料ガスの流れる方向に沿って、即ち石英
管の軸方向に沿って移動し、石英管の管外壁を局部的に
連続して加熱する。この加熱によりドーパントを含む原
料ガスと反応用酸素ガスが反応し、８ ｉ ０！ 、Ｇ
ｅ Ｏｔ 、Ｐｔ Ｏｓから成るスートが石英管内壁に
堆積する。この堆積したスートは移行してきたバーナに
より高温度で加熱されガラス化される。バーナは石英管
のガス導入端から排出端まで移動されると、迅速にガス
導入端に戻され、再び同一動作を繰り返す。この場合ド
ーパントであるＧ ｅ’ ０１４の流量が徐々に増加し
ているので、石英管には順次屈折率の相違するガラス層
が積層されることになる。Next, at the same time as introducing each of the above gases, 1. An oxyhydrogen burner serving as a heating source is moved along the flow direction of the raw material gas, that is, along the axial direction of the quartz tube, to locally and continuously heat the outer wall of the quartz tube. This heating causes the raw material gas containing the dopant to react with the reaction oxygen gas, resulting in 8 i 0! ,G
Soot consisting of eOt, PtOs is deposited on the inner wall of the quartz tube. This deposited soot is heated at high temperature by the transferred burner and vitrified. When the burner is moved from the gas introduction end to the discharge end of the quartz tube, it is quickly returned to the gas introduction end and the same operation is repeated again. In this case, since the flow rate of the dopant G e' 014 is gradually increased, glass layers having different refractive indexes are successively laminated on the quartz tube.
このようにして、ブリ７オームレツドを作成した後この
ロッドを用いてグレーデッドインデックス型光ファイバ
を製造し、そのαと帯域を調べた。After creating a 7-ohm rod in this way, a graded index optical fiber was manufactured using this rod, and its α and band were investigated.
この結果、α−１，９で計算値のα−１，９と全く同一
になり、帯域が１．２ＧＨｚ−に＋ あった０また、
この光ファイバは低ＯＨ基を示した。As a result, α-1,9 is exactly the same as the calculated value α-1,9, and the band is at 1.2 GHz-0.
This optical fiber exhibited low OH groups.
比較のために、反応用酸素ガス量を１００ＯＣＣ／ｍｉ
ｎ の一定にし、上述と同一の原料ガス及び製造条件
でブリ７オームロンドを作成し、このロッドから光ファ
イバを製造したところ、光ファイバのｆｆ −２，５で
、帯域が１００〜２００ＭＨ２−ｋＩＩ＋であった。尚
、反応用酸素ガス量が少なかったので、光ファイバを低
ＯＲに保持することはできた。For comparison, the amount of oxygen gas for reaction was 100OCC/mi.
When n was kept constant and a Buri 7 ohm rond was created using the same raw material gas and manufacturing conditions as described above, and an optical fiber was manufactured from this rod, the optical fiber had a band of 100 to 200 MH2-kII+ at ff -2,5. Met. Note that since the amount of oxygen gas for reaction was small, it was possible to maintain the optical fiber at a low OR.
（発明の効果）
本発明によれば、反応用酸素ガスの石英管への導入量を
、ＧｅＣｌ４の導入量の増加に比例させて増大すること
で、ＧｅＣｌ４の反応を促進しつつ小量の未反応Ｇｅ０
１４にて脱水作用を保持できる。従って、水分が少なく
、所定の屈折率分布が得られるプリフォーム胃ツドを作
成することができるので、低損失、高帯域の光ファイバ
を提供することができる。(Effects of the Invention) According to the present invention, by increasing the amount of reaction oxygen gas introduced into the quartz tube in proportion to the increase in the amount of GeCl4 introduced, the reaction of GeCl4 is promoted and a small amount of unused gas is removed. Reaction Ge0
The dehydration effect can be maintained at 14. Therefore, it is possible to create a preformed tube that contains less water and has a predetermined refractive index distribution, so that a low-loss, high-bandwidth optical fiber can be provided.
第１図は反応用酸素ガスと得られた光７アイパの屈折率
差との関係を示す線図、第２図は反応用酸素ガス量を少
なくして作成したブリ、７オームロ１「
ラドから成る光ファイバの屈折率分布図である。Figure 1 is a diagram showing the relationship between the reaction oxygen gas and the refractive index difference of the obtained light 7 Aiper. 1 is a refractive index distribution diagram of an optical fiber made of
Claims (1)
料ガスとしての四塩化ケイ素とドーパントとしての四塩
化ゲルマニウムをアルゴンキャリアガスにより担持して
反応用酸素ガスと共に導入し、加熱源を前記回転してい
る石英管の両端間で往復運動させて前記石英管の外周壁
を加熱し、前記石英管の内壁に順次スートを堆積させて
ブリ７オームロツドを製造する方法において、前記反応
用酸素ガスの前記石英管への導入量を、前記四塩化ゲル
マニウムの前記石英管への導入量の増加に比例させて順
次増大するツ ことを特徴とするブリフォームロブトの製造方法。[Scope of Claims] Silicon tetrachloride as a raw material gas and germanium tetrachloride as a dopant are supported by an argon carrier gas and introduced together with a reaction oxygen gas into a quartz tube which is supported and rotated by a glass lathe, In the method of manufacturing a 7-ohm rod by reciprocating a heating source between both ends of the rotating quartz tube to heat the outer circumferential wall of the quartz tube and sequentially depositing soot on the inner wall of the quartz tube, A method for producing a pre-formed robot, characterized in that the amount of reaction oxygen gas introduced into the quartz tube is gradually increased in proportion to the increase in the amount of germanium tetrachloride introduced into the quartz tube.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21907182A JPS59107936A (en) | 1982-12-13 | 1982-12-13 | Manufacture of preform rod |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP21907182A JPS59107936A (en) | 1982-12-13 | 1982-12-13 | Manufacture of preform rod |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPS59107936A true JPS59107936A (en) | 1984-06-22 |
Family
ID=16729806
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP21907182A Pending JPS59107936A (en) | 1982-12-13 | 1982-12-13 | Manufacture of preform rod |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS59107936A (en) |
-
1982
- 1982-12-13 JP JP21907182A patent/JPS59107936A/en active Pending
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