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JP6191222B2 - Manufacturing method of glass base material - Google Patents
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JP6191222B2 - Manufacturing method of glass base material - Google Patents

Manufacturing method of glass base material Download PDF

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JP6191222B2
JP6191222B2 JP2013094258A JP2013094258A JP6191222B2 JP 6191222 B2 JP6191222 B2 JP 6191222B2 JP 2013094258 A JP2013094258 A JP 2013094258A JP 2013094258 A JP2013094258 A JP 2013094258A JP 6191222 B2 JP6191222 B2 JP 6191222B2
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base material
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glass base
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JP2014214066A (en
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和昌 牧原
和昌 牧原
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Sumitomo Electric Industries Ltd
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Description

本発明は、多孔質ガラス母材を焼結して透明化するガラス母材の製造方法に関する。   The present invention relates to a method for manufacturing a glass base material that is made transparent by sintering a porous glass base material.

多孔質ガラス母材を透明化する際、焼結中の炉心管内には、通常不活性ガスであるヘリウムガスを流している。しかしながら、ヘリウムガスは高価であり、ヘリウムガスの使用はコスト増に繋がるため、ヘリウムガスの使用量低減が求められている。特許文献1は、炉内圧変動が小さい焼結初期であれば炉内に流すヘリウムガス(He)の流量を減らすことが可能であり、それにより、製造コストを削減することを開示している。   When making the porous glass base material transparent, helium gas, which is usually an inert gas, is allowed to flow in the furnace core tube during sintering. However, since helium gas is expensive and the use of helium gas leads to an increase in cost, there is a need to reduce the amount of helium gas used. Patent Document 1 discloses that the flow rate of helium gas (He) flowing into the furnace can be reduced at the initial stage of sintering when the pressure fluctuation in the furnace is small, thereby reducing the manufacturing cost.

特開2009−132585号公報JP 2009-132585 A

しかしながら、さらなるコスト削減のため、多孔質ガラス母材を透明化する際に使用するヘリウムガス量の、さらなる低減の要望がある。   However, for further cost reduction, there is a demand for further reduction of the amount of helium gas used when the porous glass base material is made transparent.

そこで、本発明の目的は、ヘリウムガスの使用量を減らし、製造コストを低く抑えることが可能なガラス母材の製造方法を提供することにある。   Accordingly, an object of the present invention is to provide a method for producing a glass base material that can reduce the amount of helium gas used and keep the production cost low.

上記課題を解決することのできる本発明のガラス母材の製造方法は、有効部と非有効部とからなる多孔質ガラス母材を焼結して透明化するガラス母材の製造方法であって、
焼結炉内にヘリウムガスを供給しながら前記有効部を焼結する第1工程と、
前記焼結炉内に窒素ガスまたはアルゴンガスの少なくとも一方を供給しながら前記非有効部を焼結する第2工程と、を含む。
The method for producing a glass base material of the present invention capable of solving the above problems is a method for producing a glass base material by sintering and transparentizing a porous glass base material composed of an effective part and an ineffective part. ,
A first step of sintering the effective part while supplying helium gas into the sintering furnace;
And a second step of sintering the ineffective portion while supplying at least one of nitrogen gas and argon gas into the sintering furnace.

本発明によれば、ヘリウムガスの使用量を減らし、製造コストを低く抑えることができる。   According to the present invention, the amount of helium gas used can be reduced and the manufacturing cost can be kept low.

本発明の一実施形態に係るガラス母材の製造方法に用いられる焼結炉の概略構成図であり、有効部を焼結する状態を示す図である。It is a schematic block diagram of the sintering furnace used for the manufacturing method of the glass base material which concerns on one Embodiment of this invention, and is a figure which shows the state which sinters an effective part. 本発明の一実施形態に係るガラス母材の製造方法に用いられる焼結炉の概略構成図であり、非有効部を焼結する状態を示す図である。It is a schematic block diagram of the sintering furnace used for the manufacturing method of the glass base material which concerns on one Embodiment of this invention, and is a figure which shows the state which sinters an ineffective part.

多孔質ガラス母材を焼結して透明化する際、通常は、ガラス中へのガス溶解度の大きい不活性ガスである、ヘリウムガスを炉心管内に流している。このヘリウムガスに替えて、安価な窒素ガスまたはアルゴンガスなどの他の不活性ガスを用いると、気泡発生などの問題が生じることがある。
本発明者は、多孔質ガラス母材には、光ファイバ化される(製品となる)部分である有効部と、光ファイバ化されない(製品とならない)部分である非有効部とがあることに着目した。非有効部を未焼結のままにすると、その後の有効部の線引時に焼結が進み、母材が変形するなどの不具合が生じるので、非有効部も焼結させることが必要である。ところが、非有効部のガラスに気泡などが生じても、非有効部は線引きすることはないので、製造される(製品となる)光ファイバ自体には問題は生じない。
このようにして、本発明者は鋭意検討した結果、多孔質ガラス母材のうち非有効部を焼結する間は、ヘリウムガスに替えて安価な窒素ガス(またはアルゴンガス)を用いる製造方法を見出した。これにより、製造される光ファイバの品質を保ったまま、製造コストを低減することができる。
When the porous glass base material is made transparent by sintering, helium gas, which is an inert gas having high gas solubility in glass, is usually allowed to flow into the furnace tube. If other inert gas such as cheap nitrogen gas or argon gas is used instead of this helium gas, problems such as bubble generation may occur.
The present inventor has that the porous glass base material has an effective portion that is a portion that becomes an optical fiber (product becomes) and an ineffective portion that is a portion that is not made optical fiber (not a product). Pay attention. If the non-effective part is left unsintered, sintering proceeds at the time of drawing the effective part thereafter, and problems such as deformation of the base material occur, so it is necessary to also sinter the non-effective part. However, even if bubbles or the like are generated in the glass of the ineffective portion, the ineffective portion is not drawn, so that there is no problem in the manufactured optical fiber (product).
Thus, as a result of intensive studies, the present inventor has devised a manufacturing method that uses inexpensive nitrogen gas (or argon gas) instead of helium gas while sintering the ineffective portion of the porous glass base material. I found it. Thereby, manufacturing cost can be reduced, maintaining the quality of the optical fiber manufactured.

[本願発明の実施形態の説明]
本願発明の実施形態に係るガラス母材の製造方法は、
(1)有効部と非有効部とからなる多孔質ガラス母材を焼結して透明化するガラス母材の製造方法であって、
焼結炉内にヘリウムガスを供給しながら前記有効部を焼結する第1工程と、
前記焼結炉内に窒素ガスまたはアルゴンガスの少なくとも一方を供給しながら前記非有効部を焼結する第2工程と、を含む。
有効部での焼結の際(第1工程)はヘリウムガスを用いるのに対し、非有効部を焼結する際(第2工程)は、ヘリウムガスよりも安価な窒素ガスまたはアルゴンガスを用いるので、焼結時全体での使用するガスのコストを下げることができる。非有効部は、焼結されても光ファイバにならない部分であるので、窒素ガスまたはアルゴンガスを用いて焼結した結果気泡が生じても、製品となる光ファイバに影響を及ぼさない。従って、得られる光ファイバの品質を損なうことなく、製造コストを削減することができる。なお、第2工程では、ヘリウムが若干量混入してもよい。
[Description of Embodiment of Present Invention]
A method for producing a glass base material according to an embodiment of the present invention is as follows:
(1) A method for producing a glass base material by sintering and transparentizing a porous glass base material comprising an effective part and an ineffective part,
A first step of sintering the effective part while supplying helium gas into the sintering furnace;
And a second step of sintering the ineffective portion while supplying at least one of nitrogen gas and argon gas into the sintering furnace.
Helium gas is used for sintering in the effective part (first step), whereas nitrogen gas or argon gas, which is cheaper than helium gas, is used for sintering the ineffective part (second step). Therefore, the cost of the gas used at the time of sintering can be reduced. Since the ineffective portion is a portion that does not become an optical fiber even if sintered, even if bubbles are generated as a result of sintering using nitrogen gas or argon gas, the product optical fiber is not affected. Therefore, the manufacturing cost can be reduced without deteriorating the quality of the obtained optical fiber. In the second step, a slight amount of helium may be mixed.

(2)ヘリウムガスを供給して前記有効部を焼結する前記第1工程が終了した後、前記焼結炉内に窒素ガスまたはアルゴンガスの少なくとも一方を供給して前記非有効部を焼結する前記第2工程を行う。
多孔質ガラス母材は、上下端に非有効部を含むことがあるが、有効部を焼結する前に窒素ガスまたはアルゴンガスで非有効部である部分を焼結してしまうと、有効部でヘリウムガスに切り替えたとしても、有効部に気泡が発生してしまう場合がある。このため、最初はヘリウムを流し、有効部が完全に焼結された後に、窒素ガスまたはアルゴンガスの少なくとも一方を供給して焼結することにより、有効部に気泡が発生することを確実に防ぎつつ、製造コストを削減することができる。
(2) After the first step of sintering the effective part by supplying helium gas, at least one of nitrogen gas or argon gas is supplied into the sintering furnace to sinter the ineffective part The second step is performed.
The porous glass base material may include an ineffective portion at the upper and lower ends, but if the portion that is an ineffective portion is sintered with nitrogen gas or argon gas before the effective portion is sintered, the effective portion Even if the gas is switched to helium gas, bubbles may be generated in the effective portion. For this reason, helium is first flowed, and after the effective part has been completely sintered, at least one of nitrogen gas and argon gas is supplied to sinter, thereby reliably preventing bubbles from being generated in the effective part. However, the manufacturing cost can be reduced.

(3)前記第2工程では、前記焼結炉内に、ヘリウムを含まずに窒素ガスのみを供給する。
第2工程において、ヘリウムガスを全く含まず、且つアルゴンガスよりも安価な窒素ガスを使用することにより、さらにコストを効果的に削減することができる。
(3) In the second step, only nitrogen gas is supplied into the sintering furnace without containing helium.
In the second step, by using nitrogen gas that does not contain any helium gas and is cheaper than argon gas, the cost can be further effectively reduced.

[本願発明の実施形態の詳細]
本発明の実施形態に係るガラス母材の製造方法の具体例を、以下に図面を参照しつつ説明する。
なお、本発明はこれらの例示に限定されるものではなく、特許請求の範囲によって示され、特許請求の範囲と均等の意味および範囲内でのすべての変更が含まれることが意図される。
[Details of the embodiment of the present invention]
Specific examples of the method for producing a glass base material according to the embodiment of the present invention will be described below with reference to the drawings.
In addition, this invention is not limited to these illustrations, is shown by the claim, and intends that all the changes within the meaning and range equivalent to a claim are included.

図1は、本発明の一実施形態に係るガラス母材の製造方法に用いられる焼結炉の概略構成図であり、有効部を焼結する状態を示す図である。図2は、本発明の一実施形態に係るガラス母材の製造方法に用いられる焼結炉の概略構成図であり、非有効部を焼結する状態を示す図である。   FIG. 1 is a schematic configuration diagram of a sintering furnace used in a method for producing a glass base material according to an embodiment of the present invention, and shows a state in which an effective part is sintered. FIG. 2 is a schematic configuration diagram of a sintering furnace used in the method for producing a glass base material according to an embodiment of the present invention, and shows a state in which an ineffective portion is sintered.

図1および図2に示した焼結炉1は、多孔質ガラス母材3を加熱して焼結し、透明化させるものである。この焼結炉1は、炉心管2と、ヒータ4と、ガス供給用流路5と、第1吸気弁6と、第2吸気弁7と、排気用流路8および排気弁8aを備えている。   A sintering furnace 1 shown in FIGS. 1 and 2 heats and sinters a porous glass base material 3 to make it transparent. The sintering furnace 1 includes a furnace core tube 2, a heater 4, a gas supply passage 5, a first intake valve 6, a second intake valve 7, an exhaust passage 8 and an exhaust valve 8a. Yes.

炉心管2は、例えば多孔質ガラス母材3が挿入される有底円筒状に形成された管である。この炉心管2の上端壁9には、多孔質ガラス母材3の上端から上方に延びるシード棒10が昇降自在に挿通する開口11を有している。
ヒータ4は、炉心管2内に挿入された多孔質ガラス母材3を加熱する。炉心管2の底部には、ガス供給用流路5が接続されている。ガス供給用流路5の途中には、炉心管2内に供給される窒素(N)ガスまたはアルゴン(Ar)ガスを供給する際に開く第1吸気弁6と、ヘリウム(He)ガスを供給する際に開く第2吸気弁7と、が設けられている。また、炉心管2の上端側の周壁には、炉内のガスを排気するための排気用流路8が接続され、排気用流路8の途中には排気弁8aが設けられている。なお、炉心管2に供給されるガスの一部は、シード棒10と開口11との間の隙間から外部に排出される。
The core tube 2 is a tube formed in a bottomed cylindrical shape into which the porous glass base material 3 is inserted, for example. An upper end wall 9 of the core tube 2 has an opening 11 through which a seed bar 10 extending upward from the upper end of the porous glass base material 3 is inserted so as to be movable up and down.
The heater 4 heats the porous glass base material 3 inserted into the furnace core tube 2. A gas supply flow path 5 is connected to the bottom of the core tube 2. In the middle of the gas supply flow path 5, a first intake valve 6 that opens when supplying nitrogen (N 2 ) gas or argon (Ar) gas supplied into the core tube 2 and helium (He) gas are provided. A second intake valve 7 that is opened when the supply is performed is provided. Further, an exhaust passage 8 for exhausting the gas in the furnace is connected to the peripheral wall on the upper end side of the core tube 2, and an exhaust valve 8 a is provided in the middle of the exhaust passage 8. A part of the gas supplied to the core tube 2 is discharged to the outside through a gap between the seed rod 10 and the opening 11.

また、焼結炉1の炉心管2に挿入される多孔質ガラス母材3は、光ファイバ化される部分である有効部3aと、光ファイバ化されない部分である非有効部3bとを有する。有効部3aは、光ファイバのコアとなる部分と、クラッドとなる部分を有し、製品となる部分である。なお、図1および図2において、非有効部3bは多孔質ガラス母材3内の破線よりも上の部分であるが、最下端に非有効部が存在する場合もありうる。   Moreover, the porous glass base material 3 inserted into the furnace core tube 2 of the sintering furnace 1 has an effective portion 3a that is a portion that is made into an optical fiber and an ineffective portion 3b that is a portion that is not made into an optical fiber. The effective part 3a is a part that has a part that becomes a core of an optical fiber and a part that becomes a clad and becomes a product. 1 and 2, the ineffective portion 3b is a portion above the broken line in the porous glass base material 3, but there may be an ineffective portion at the lowermost end.

[ガラス母材の製造方法]
次に、本実施形態のガラス母材の製造方法について説明する。
まず、図1に示すように、多孔質ガラス母材3を焼結炉1の炉心管2内に挿入する。このとき、多孔質ガラス母材3の下端部(すなわち、有効部3aの焼結開始端)がヒータ4の高さに配置される。
[Glass base material manufacturing method]
Next, the manufacturing method of the glass base material of this embodiment is demonstrated.
First, as shown in FIG. 1, the porous glass base material 3 is inserted into the core tube 2 of the sintering furnace 1. At this time, the lower end portion of the porous glass base material 3 (that is, the sintering start end of the effective portion 3 a) is disposed at the height of the heater 4.

(第1工程)
最初に、以下の第1工程を実施する。
第1吸気弁6は閉じた状態で第2吸気弁7を開けて、ガス供給用流路5から焼結用の不活性ガスとして炉心管2内にヘリウムガスを供給する。このとき、炉内が陽圧になるようにヘリウムガスの供給・排気流量を調整する。この供給されたヘリウムガスの雰囲気中で、ヒータ4により所定の加熱を行うことで、多孔質ガラス母材3の有効部3aを焼結させる。このように有効部3aをその下端側から焼結させながら、徐々に多孔質ガラス母材3の位置を下げていく。そして、図2に示すように、炉心管2内で多孔質ガラス母材3を吊り下げる位置が所定位置(例えば、非有効部3bがヒータ4の高さと同じ位置)まで到達すると、有効部3a全体が完全に焼結された状態になる。
(First step)
First, the following first step is performed.
With the first intake valve 6 closed, the second intake valve 7 is opened, and helium gas is supplied into the furnace tube 2 as an inert gas for sintering from the gas supply flow path 5. At this time, the supply / exhaust flow rate of helium gas is adjusted so that the inside of the furnace becomes a positive pressure. The effective portion 3a of the porous glass base material 3 is sintered by performing predetermined heating with the heater 4 in the atmosphere of the supplied helium gas. In this manner, the position of the porous glass base material 3 is gradually lowered while the effective portion 3a is sintered from the lower end side. Then, as shown in FIG. 2, when the position where the porous glass base material 3 is suspended in the core tube 2 reaches a predetermined position (for example, the position where the ineffective portion 3b is the same as the height of the heater 4), the effective portion 3a. The whole is completely sintered.

(第2工程)
次に、以下の第2工程を実施する。
第2吸気弁7を閉じ、第1吸気弁6を開けて炉心管2内に窒素ガスまたはアルゴンガスを供給する。なお、ヘリウムガスから窒素ガスまたはアルゴンガスに切り替えても、炉内に外気が混入することを防止するために、炉内を陽圧に保つ必要がある。このため、ヘリウムとほぼ同じ量の窒素ガスまたはアルゴンガスを供給しながら、圧力を調整する。そして、窒素ガスまたはアルゴンガスの雰囲気中で、ヒータ4により所定の加熱を行うことで、多孔質ガラス母材3の非有効部3bを焼結させる。
(Second step)
Next, the following second step is performed.
The second intake valve 7 is closed, the first intake valve 6 is opened, and nitrogen gas or argon gas is supplied into the furnace core tube 2. Even if the helium gas is switched to nitrogen gas or argon gas, it is necessary to keep the inside of the furnace at a positive pressure in order to prevent outside air from being mixed into the furnace. For this reason, the pressure is adjusted while supplying substantially the same amount of nitrogen gas or argon gas as helium. And the ineffective part 3b of the porous glass base material 3 is sintered by performing predetermined heating with the heater 4 in the atmosphere of nitrogen gas or argon gas.

以上のようにして、多孔質ガラス母材3の全体が焼結され、透明化したガラス母材が得られる。本実施形態のガラス母材の製造方法によれば、ヘリウムガスのみで多孔質ガラス母材3全体を焼結させる場合に比べて、ヘリウムガスの使用量が1/8〜1/10減少し、製造コストが約10%削減できる。   As described above, the entire porous glass base material 3 is sintered to obtain a transparent glass base material. According to the glass base material manufacturing method of the present embodiment, the amount of helium gas used is reduced by 1/8 to 1/10 compared to the case where the entire porous glass base material 3 is sintered with only helium gas. The manufacturing cost can be reduced by about 10%.

なお、上記実施形態では、下部に有効部、上部に非有効部がある例について述べたが、ガラス母材の下部にも非有効部が存在する場合もある。この場合、最初に窒素ガスまたはアルゴンガスで非有効部を焼結してからガスを切り替え、ヘリウムを流して有効部を焼結すると、有効部で気泡が生じてしまう。このため、有効部を焼結する前には、窒素ガスまたはアルゴンガスを流さずに焼結する必要があり、この場合は、非有効部であってもヘリウムガスで焼結することが必要である。
また、窒素ガスはアルゴンガスよりも安価であるので、上記実施形態において、アルゴンガスよりも窒素ガスを用いる方がコスト的に有利である。
なお、第2工程において、窒素ガスまたはアルゴンガスを単独で用いるのではなく、窒素ガスとアルゴンガスとを混合して供給するようにしてもよい。また、若干量のヘリウムが混合してもよいが、上記したように、窒素ガスのみを用いる方が、コスト的に有利である。
In the above embodiment, an example in which there is an effective portion at the lower portion and an ineffective portion at the upper portion has been described. However, an ineffective portion may also exist at the lower portion of the glass base material. In this case, when the ineffective portion is first sintered with nitrogen gas or argon gas, the gas is switched, and when helium is flowed to sinter the effective portion, bubbles are generated in the effective portion. For this reason, before the effective part is sintered, it is necessary to sinter without flowing nitrogen gas or argon gas. In this case, even the ineffective part needs to be sintered with helium gas. is there.
Further, since nitrogen gas is less expensive than argon gas, in the above embodiment, it is more cost-effective to use nitrogen gas than argon gas.
In the second step, nitrogen gas or argon gas may not be used alone, but nitrogen gas and argon gas may be mixed and supplied. Although a slight amount of helium may be mixed, it is advantageous in terms of cost to use only nitrogen gas as described above.

また、上記実施形態のガラス母材の製造方法において、多孔質ガラス母材3の有効部3aと非有効部3bの境目の部分では、有効部3aの焼結終了側端部と非有効部3bの焼結開始側端部とを同時に焼結する時間帯が生じる。この時間帯に入ると同時に第2工程に移行し、供給するガスをヘリウムガスから窒素ガスまたはアルゴンガスに切り替えて非有効部3bの焼結を開始してもよいし、徐々に窒素ガスまたはアルゴンガスの割合を増やしていってもよい。   Moreover, in the manufacturing method of the glass base material of the said embodiment, in the part of the boundary of the effective part 3a of the porous glass base material 3, and the ineffective part 3b, the end part of sintering end side of the effective part 3a and the ineffective part 3b The time zone which sinters simultaneously the sintering start side edge part of this arises. At the same time as entering this time zone, the process proceeds to the second step, the gas to be supplied is switched from helium gas to nitrogen gas or argon gas, and sintering of the ineffective portion 3b may be started. You may increase the ratio of gas.

1 焼結炉
2 炉心管
3 多孔質ガラス母材
3a 有効部
3b 非有効部
4 ヒータ
5 ガス供給用流路
6 第1吸気弁
7 第2吸気弁
8 排気用流路
8a 排気弁
9 上端壁
10 シード棒
11 開口
DESCRIPTION OF SYMBOLS 1 Sintering furnace 2 Furnace core tube 3 Porous glass base material 3a Effective part 3b Ineffective part 4 Heater 5 Gas supply flow path 6 First intake valve 7 Second intake valve 8 Exhaust flow path 8a Exhaust valve 9 Upper end wall 10 Seed stick 11 Opening

Claims (2)

有効部と非有効部とからなる多孔質ガラス母材を焼結して透明化するガラス母材の製造方法であって、
焼結炉内にヘリウムガスを供給しながら前記有効部を焼結する第1工程と、
前記焼結炉内に窒素ガスまたはアルゴンガスの少なくとも一方を供給しながら前記非有効部をヒータにより所定の加熱を行うことで焼結する第2工程と、を含み、
前記第1工程が終了した後、前記第2工程を行う、ガラス母材の製造方法。
A method for producing a glass base material by sintering and transparentizing a porous glass base material composed of an effective part and an ineffective part,
A first step of sintering the effective part while supplying helium gas into the sintering furnace;
Look including a second step for sintering by performing predetermined heating by the heater of the invalid portion while supplying at least one of nitrogen gas or argon gas into the sintering furnace,
A method for producing a glass base material , wherein the second step is performed after the first step is completed .
前記第2工程では、前記焼結炉内に、ヘリウムを含まずに窒素ガスのみを供給する、請求項1に記載のガラス母材の製造方法。 The method for producing a glass base material according to claim 1, wherein in the second step, only nitrogen gas is supplied into the sintering furnace without containing helium .
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