JPH01298036A - Production of quartz glass base material - Google Patents
Production of quartz glass base materialInfo
- Publication number
- JPH01298036A JPH01298036A JP12578788A JP12578788A JPH01298036A JP H01298036 A JPH01298036 A JP H01298036A JP 12578788 A JP12578788 A JP 12578788A JP 12578788 A JP12578788 A JP 12578788A JP H01298036 A JPH01298036 A JP H01298036A
- Authority
- JP
- Japan
- Prior art keywords
- glass body
- metal oxide
- porous glass
- raw material
- oxygen
- 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 15
- 239000000463 material Substances 0.000 title claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 title claims description 3
- 239000005373 porous glass Substances 0.000 claims abstract description 31
- 239000007789 gas Substances 0.000 claims abstract description 25
- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 24
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 24
- 239000011521 glass Substances 0.000 claims abstract description 19
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 15
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000001301 oxygen Substances 0.000 claims abstract description 14
- 239000010453 quartz Substances 0.000 claims description 3
- 238000000034 method Methods 0.000 abstract description 24
- 230000003287 optical effect Effects 0.000 abstract description 3
- 239000000377 silicon dioxide Substances 0.000 abstract description 3
- 229910006113 GeCl4 Inorganic materials 0.000 abstract description 2
- 239000013307 optical fiber Substances 0.000 abstract description 2
- IEXRMSFAVATTJX-UHFFFAOYSA-N tetrachlorogermane Chemical compound Cl[Ge](Cl)(Cl)Cl IEXRMSFAVATTJX-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052681 coesite Inorganic materials 0.000 abstract 2
- 229910052906 cristobalite Inorganic materials 0.000 abstract 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract 2
- 229910052682 stishovite Inorganic materials 0.000 abstract 2
- 229910052905 tridymite Inorganic materials 0.000 abstract 2
- -1 GeCl4) Chemical class 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000001307 helium Substances 0.000 abstract 1
- 229910052734 helium Inorganic materials 0.000 abstract 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 abstract 1
- 239000002019 doping agent Substances 0.000 description 9
- 238000010586 diagram Methods 0.000 description 4
- 230000008021 deposition Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- XHXFXVLFKHQFAL-UHFFFAOYSA-N phosphoryl trichloride Chemical compound ClP(Cl)(Cl)=O XHXFXVLFKHQFAL-UHFFFAOYSA-N 0.000 description 2
- 229910015844 BCl3 Inorganic materials 0.000 description 1
- 240000001548 Camellia japonica Species 0.000 description 1
- 229910019213 POCl3 Inorganic materials 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000018597 common camellia Nutrition 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- FAQYAMRNWDIXMY-UHFFFAOYSA-N trichloroborane Chemical compound ClB(Cl)Cl FAQYAMRNWDIXMY-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]
- C03B37/01446—Thermal after-treatment of preforms, e.g. dehydrating, consolidating, sintering
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Thermal Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Glass Melting And Manufacturing (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
Abstract
Description
【発明の詳細な説明】
（産業上の利用分野）
この発明は、光ファイバ、光学レンズ、光部品等に好適
な石英系ガラス母材の製造方法に関するもので、屈折率
分布にゆらぎのない均一なものを提供する。Detailed Description of the Invention (Field of Industrial Application) The present invention relates to a method for manufacturing a silica-based glass base material suitable for optical fibers, optical lenses, optical components, etc. provide something.
（従来の技術）
この種の石英系ガラス母材の製造には、通常ＶＡＤ法、
外付は法、ゾルグル法等が用いられている。例えばＶＡ
Ｄ法においては、酸水素バーナ内に主原料ガスとしての
５ｉＣ１４と、ドーパントとしてのＧｅＣ１，、ＰＯＣ
ｌ３．ＢＣｌ、等を送込み、火炎加水分解反応もしくは
熱酸化反応させて得られるＳｉＯ□とＧｅＯ□、 Ｐ、
０． 、Ｂ、Ｏ，等とからなるガラス微粉末を回転する
棒状態の先端に堆積させて多、孔質ガラス体とし、しか
るのもこの多孔質ガラス体を透明ガラス化していた。(Prior art) This type of quartz-based glass base material is usually manufactured using the VAD method,
For external methods, methods such as the method and the Zorgu method are used. For example, VA
In method D, 5iC14 as the main raw material gas and GeC1, POC as the dopant are placed in the oxyhydrogen burner.
l3. SiO□ and GeO□, P, which are obtained by feeding BCl, etc. and causing a flame hydrolysis reaction or thermal oxidation reaction.
0. , B, O, etc., was deposited on the tip of a rotating rod to form a porous glass body, and this porous glass body was made into transparent glass.
なお得られる透明ガラス体のドーパント濃度の制御は、
酸水素バーナ内に供給されるドーパントガスの主原料ガ
スに対する濃度を制御することで行っていた。The dopant concentration of the resulting transparent glass body can be controlled by
This was done by controlling the concentration of the dopant gas supplied into the oxyhydrogen burner relative to the main raw material gas.
（発明が解決しようとする課題）
しかしＶＡＤ法におけるガラス微粒子の堆積面の温度を
空間的に一定にすることはできないので、回転引上げら
れつつある堆積面に対してバーナ炎が回転対称にはおか
れていないと第２図に示すようなドーパント濃度のゆら
ぎが生じてしまう。図において横軸ｒは透明ガラス体の
半径を、縦軸はドーパント濃度を示す、このようなドー
パント濃度のゆらぎは、いわゆる外付は法においても同
様に生じるもので、第３図はその様子を示したものであ
る。なお図において横軸、縦軸は第２図と同一である。(Problem to be solved by the invention) However, in the VAD method, the temperature of the deposition surface of glass particles cannot be kept constant spatially, so the burner flame is not placed rotationally symmetrically with respect to the deposition surface that is being rotated and pulled up. Otherwise, fluctuations in the dopant concentration as shown in FIG. 2 will occur. In the figure, the horizontal axis r indicates the radius of the transparent glass body, and the vertical axis indicates the dopant concentration.Such fluctuations in dopant concentration also occur in the so-called external method, and Figure 3 shows this situation. This is what is shown. In the figure, the horizontal and vertical axes are the same as in FIG. 2.
（課題を解決するための手段）
この発明は、以上の観点からドーパント濃度のゆらぎを
極力抑制した方法を提供するもので、予めＳｉＯ□から
なる多孔質ガラス体を作り、これを金属酸化物形成原料
ガスと酸素とを含む雰囲気内に収容し、この雰囲気下で
加熱処理して金属酸化物とＳｉＯ□とからなる多孔質ガ
ラス体とし、しかる後これを高温に加熱して透明ガラス
化するようにしたものである。(Means for Solving the Problems) In view of the above, the present invention provides a method that suppresses fluctuations in dopant concentration as much as possible, by preparing a porous glass body made of SiO It is housed in an atmosphere containing raw material gas and oxygen, and heat-treated in this atmosphere to form a porous glass body made of metal oxide and SiO□, which is then heated to a high temperature to become transparent glass. This is what I did.
なおこの方法は、最初に多孔質ガラス体を得、それから
透明ガラス化する方法であるからいわゆるＶＡＤ法、外
付は法、ゾルゲル法等の手段の如何を問わずいずれでも
よい、さらに加熱手段としての炉には、金属酸化物形成
原料ガスと酸素とがＳｉＯ□多孔質ガラス体内で反応し
て一定の濃度を形成するように均一温度ゾーンの長い炉
を用いられる。Note that this method is a method of first obtaining a porous glass body and then converting it into transparent glass, so any method such as the so-called VAD method, an external method, a sol-gel method, etc. may be used. A furnace with a long uniform temperature zone is used so that the metal oxide forming raw material gas and oxygen react in the SiO□ porous glass body to form a constant concentration.
（作用）
金属酸化物形成原料ガスと酸素がＳｉＯ□からなる多孔
質ガラス体内に均一に入り、そこで反応して金属酸化物
を形成するため一定濃度の金属酸化物を含むＳｉＯ□多
孔質ガラス体が得られる。したがってこの多孔質ガラス
体を透明ガラス化すれば金属酸化物の濃度にゆらぎのな
い透明ガラス体とすることができる。(Function) Metal oxide forming raw material gas and oxygen uniformly enter the porous glass body made of SiO□ and react there to form a metal oxide, so the SiO□ porous glass body contains a certain concentration of metal oxide. is obtained. Therefore, by converting this porous glass body into transparent glass, it is possible to obtain a transparent glass body with no fluctuation in the metal oxide concentration.
（実施例）
第１図は、この発明方法に用いられる装置を示したもの
で、ｌはＶＡＤ法により得られた５１０２多孔質ガラス
体で、回転自在かつ上下動可能に支承されている。２は
石英ガラス製の炉心管、３は炉心管２の底部に設けられ
たガス供給口で、ＧｅＣ１＜ 。(Example) FIG. 1 shows an apparatus used in the method of the present invention, in which 1 is a 5102 porous glass body obtained by the VAD method, which is supported so as to be rotatable and movable up and down. 2 is a core tube made of quartz glass, 3 is a gas supply port provided at the bottom of the core tube 2, and GeC1<.
ＢＣｌ３ 、 ＰＯＣｌ３などの金属酸化物形成原料ガ
ス、酸素、Ｈｅが供給される。４は炉心管２の上側部に
設けられたガス排出口、５は炉心管２の上部に設けられ
たＳｉＯ□多孔質ガラス体導入口である。６は炉心管２
を囲むヒータで、ＳｉＯ□多孔質ガラス体全体を均一に
加熱すために十分に長いヒートゾーンを備えている０以
上の構成において、炉心管２内に８１０２多孔質ガラス
体１を吊るし、ガス供給口３から金属酸化物形成原料ガ
ス、酸素およびＨｅを供給してＳｉＯ□多孔質ガラス体
１内に金属酸化物形成原料ガスと′酸素とが十分に充填
されるようにする。Metal oxide forming raw material gases such as BCl3 and POCl3, oxygen, and He are supplied. Reference numeral 4 designates a gas discharge port provided at the upper side of the furnace core tube 2, and reference numeral 5 represents a SiO□ porous glass body inlet provided at the upper portion of the furnace core tube 2. 6 is the furnace core tube 2
The 8102 porous glass body 1 is suspended in the furnace tube 2 in a configuration of 0 or more with a heat zone long enough to uniformly heat the entire SiO□ porous glass body with a heater surrounding the The metal oxide forming raw material gas, oxygen and He are supplied from the port 3 so that the SiO□ porous glass body 1 is sufficiently filled with the metal oxide forming raw material gas and oxygen.
次にヒータ６を動作させて炉心管２内を金属酸化物形成
原料ガスと酸素とが反応しつる温度に維持してＳｉＯ□
多孔質ガラス体内に金属酸化物を形成させる。最後に金
属酸化物形成原料ガスの供給を断ち、酸素とＨｅとを供
給しつつ炉心管２内をさらに高温にして金属酸化物を含
むＳｉＯ□多孔質ガラス体を透明ガラス化する。Next, the heater 6 is operated to maintain the inside of the furnace tube 2 at a temperature at which the metal oxide forming raw material gas and oxygen react with each other.
Metal oxides are formed within the porous glass body. Finally, the supply of the metal oxide forming raw material gas is cut off, and while supplying oxygen and He, the temperature inside the furnace tube 2 is further increased to convert the SiO□ porous glass body containing the metal oxide into transparent glass.
（具体例）
ＳｉＯ□多孔質ガラス体を得るためにＶＡＤ法を採用し
た。多重管バーナ内にＨ２５β／分、 ０２１０１２７
分、５ｉＣ１４５００ｃｃ ７分、Ａｒ ２００ ｃｃ
７分を供給し、生成されるＳｉＯ□ガラス微粒子をタ
ーゲット先端に堆積させ直径５０１１１！８φ 、長さ
４００ｍｌ１ の５ｉＯｚ多孔質ガラス体とした。次
にこの多孔質ガラス体を第１図に示す電気炉内に入れし
ばら（Ｈｅで置換した。この電気炉のヒータの均熱ゾー
ンは５００ ｍｌＩｎである。それから炉内を１０００
℃まで徐々に昇温させるとともにＨｅ３ｇ、７分、Ｇｅ
Ｃｌ４２０ＯＩ２／分、０□ λ℃／分流しつつ５時間
処理した。この後ＧｅＣｌ４を止め、 Ｈｅ ５ε／分
、０□５０ ｃｃ ７分流しつつ１６５０ ℃まで昇温
して透明ガラス体とした。この透明ガラス体を延伸し、
その上に石英ガラスバイブを被せてコラップスした。か
くして得られたプリフォームの屈折率分布をアナライザ
を用いて測定したところゆらぎのない均一なものであっ
た。(Specific Example) A VAD method was adopted to obtain a SiO□ porous glass body. H25β/min in multi-tube burner, 0210127
min, 5iC14500cc 7 min, Ar 200 cc
7 minutes, and the generated SiO□ glass particles were deposited on the tip of the target to form a 5iOz porous glass body with a diameter of 50111!8φ and a length of 400ml1. Next, this porous glass body was placed in the electric furnace shown in Fig. 1 and replaced with He for a while.The soaking zone of the heater of this electric furnace was 500 mlIn.
Gradually raise the temperature to ℃ and add 3g of He, 7 minutes,
The treatment was carried out for 5 hours while flowing Cl420OI2/min and 0□ λ°C/min. Thereafter, the GeCl4 was stopped, and the temperature was raised to 1650° C. while flowing He 5ε/min and 0□50 cc for 7 minutes to obtain a transparent glass body. Stretch this transparent glass body,
I put a quartz glass vibrator on top of it and collapsed it. When the refractive index distribution of the thus obtained preform was measured using an analyzer, it was found to be uniform with no fluctuation.
なお、金属酸化物形成原料ガス濃度およびその多孔質ガ
ラス体内への拡散時間を調整することにより緩やかな椿
屈折率分布を持った透明ガラス体を得ることができる。Note that a transparent glass body having a gentle camellia refractive index distribution can be obtained by adjusting the concentration of the metal oxide forming raw material gas and the time for its diffusion into the porous glass body.
（発明の効果）
この発明方法は、以上のように予めＳｉＯ□多孔質ガラ
ス体を用意し、これを金属酸化物形成用ガスと酸素との
雰囲気内に収容してこれらガスを多孔質ガラス体内に充
填させ、そのうえで加熱処理することにより金属酸化物
形成用ガスと酸素との反応により生成される金属酸化物
を多孔質ガラス体内に含ませる方法であるので、金属酸
化物を多孔質ガラス体内にゆらぎのない状態でドーピン
グすることができる。(Effects of the Invention) In the method of the present invention, a SiO□ porous glass body is prepared in advance as described above, and this is housed in an atmosphere of a metal oxide forming gas and oxygen to allow these gases to enter the porous glass body. This method involves filling the porous glass body with the metal oxide produced by the reaction between the metal oxide forming gas and oxygen, and then heat-treating it. Doping can be done without fluctuation.
第１図は、この発明方法に用いられる装置の概略説明図
。第２図は、ＶＡＤ法により得られた母材のドーパント
濃度のゆらぎの様子を示す説明図、第３図は、外付は法
により得られた母材のドーパントａ度のゆらぎの様子を
示す説明図。
図において１：ＳｉＯ□多孔質ガラス体、２：石英炉心
管、３：ガス供給口、６：ヒータ。FIG. 1 is a schematic explanatory diagram of an apparatus used in the method of this invention. Figure 2 is an explanatory diagram showing the fluctuations in the dopant concentration of the base material obtained by the VAD method, and Figure 3 is an explanatory diagram showing the fluctuations in the dopant a degree of the base material obtained by the external method. Explanatory diagram. In the figure, 1: SiO□ porous glass body, 2: quartz furnace tube, 3: gas supply port, 6: heater.
Claims (1)
原料ガスと酸素とを含む雰囲気内で加熱処理して金属酸
化物とＳｉＯ＿２とからなる多孔質ガラス体とし、しか
る後これを高温に加熱して透明ガラス化することを特徴
とする石英系ガラス母材の製造方法。A porous glass body made of SiO_2 is heat-treated in an atmosphere containing metal oxide forming raw material gas and oxygen to form a porous glass body made of metal oxide and SiO_2, which is then heated to a high temperature. A method for producing a quartz-based glass base material characterized by converting it into transparent glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12578788A JPH01298036A (en) | 1988-05-25 | 1988-05-25 | Production of quartz glass base material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP12578788A JPH01298036A (en) | 1988-05-25 | 1988-05-25 | Production of quartz glass base material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH01298036A true JPH01298036A (en) | 1989-12-01 |
Family
ID=14918852
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP12578788A Pending JPH01298036A (en) | 1988-05-25 | 1988-05-25 | Production of quartz glass base material |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH01298036A (en) |
-
1988
- 1988-05-25 JP JP12578788A patent/JPH01298036A/en active Pending
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