JP3707104B2 - Raw material supply apparatus and raw material supply method - Google Patents

Raw material supply apparatus and raw material supply method Download PDF

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JP3707104B2
JP3707104B2 JP21873995A JP21873995A JP3707104B2 JP 3707104 B2 JP3707104 B2 JP 3707104B2 JP 21873995 A JP21873995 A JP 21873995A JP 21873995 A JP21873995 A JP 21873995A JP 3707104 B2 JP3707104 B2 JP 3707104B2
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raw material
liquid
tank
flow rate
material liquid
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JPH0967129A (en
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渉 菊地
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Sumitomo Electric Industries Ltd
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    • 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]
    • C03B37/01413—Reactant delivery systems
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B2207/00—Glass deposition burners
    • C03B2207/80—Feeding the burner or the burner-heated deposition site
    • C03B2207/85—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid
    • C03B2207/86—Feeding the burner or the burner-heated deposition site with vapour generated from liquid glass precursors, e.g. directly by heating the liquid by bubbling a gas through the liquid

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  • 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)
  • Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
  • Glass Melting And Manufacturing (AREA)
  • Manufacture, Treatment Of Glass Fibers (AREA)

Description

【０００１】
【産業上の利用分野】
本発明は、光ファイバ母材あるいは半導体等の製造に用いられるＳｉＣｌ4 、ＧｅＣｌ4 等の液体原料を精密に流量制御しつつ大量にかつ安定して反応容器に導くことが出来る原料供給装置及び原料供給方法に関する。
【０００２】
【従来の技術】
光ファイバ用母材の製造方法としては、いわゆるＶＡＤ法、外付け法、内付け法などが知られている。この内、特に長時間連続して原料ガスの供給を必要とするＶＡＤ法においては、液体ガラス原料を気化した原料ガスを大気圧以上で反応容器に送り酸水素バ−ナで燃焼させてガラス媒体を生成し、回転する出発母材に基づいて軸方向に堆積させて棒状の多孔質母材を作り、更にこの多硬質母材を光ファイバに紡糸するものである。このために、連続して大量にかつ安定して原料ガスを反応容器へ供給する原料供給装置が用いられている。
【０００３】
このような原料供給装置の１例を図３に示す。図３に示す原料供給装置によれば、気密な原料タンク１には大気中の酸素又は水分と反応する原料液２が収容されていて、原料タンク１の外側には原料液２を気化するためのヒ−タ３が取付けられており、このヒ−タ３は温度センサ４と温度調整器５によって制御され原料液２の温度が精密にコントロ−ルされている。原料タンク１の上部空間６には原料液２が気化した原料ガスが原料タンク１の温度における蒸気圧で満たされており、原料タンク１と反応容器７との間には原料ガスを供給する配管８が配置されている。
【０００４】
配管８には開閉弁９、自動開閉弁１０、流量調整装置１１が取付けられている。この自動開閉弁１０は、外部からの制御により自動的に流路を開閉する装置である。流量調整装置１１は、例えばマスフロ−コントロ−ラ等の質量流量計である。流量調整装置１１の一次側には自動開閉弁１２を介在した配管１３が接続されていて、配管１３を通じて窒素ガスが供給されるようになっている。
【０００５】
自動開閉弁１２は、自動開閉弁１０と連動し、原料供給中は自動開閉弁１０が開き自動開閉弁１２が閉じて原料ガスを反応容器７に流し、原料ガスの供給をしていないときは自動開閉弁１０が閉じ自動開閉弁１２が開いて配管中に窒素ガスを流して配管保護のパ−ジを行なう。
【０００６】
原料タンク１には、図示しない原料液のサ−ビスタンクから常温の原料液が供給され、このための自動開閉弁１５と流量調整弁１６が取付けられた配管１４が配置されている。流量調整弁１６は、手動により流路を一定の流量（以下、流量というときはこの意味での流量、つまり原料が供給されている時の単位時間当たりの流量を言う。）になるように設定することが可能な調整弁であって、反応容器７の全てが稼働したときの反応量に基づいて流量を設定している。
【０００７】
原料タンク１には重量計２３が取付けられており、この重量計２３により原料２の重量をモニタ−している。自動開閉弁１５は、重量計２３の重量に連動して開閉がなされ、これが開くと原料液が原料タンク１に補給され、これが閉じると原料液の原料タンクへの補給が停止する。
【０００８】
半導体ウエハ上に複数の半導体層を積層して半導体を製造する場合等においても同様な原料供給装置が用いられている。
【０００９】
【発明が解決しようとする課題】
光ファイバ用母材の製造方法のＶＡＤ法では、原料タンクから反応容器の各ガスバ−ナに原料ガスを正確かつ安定に流量制御して供給することが要求される。特に多重管バ−ナについては、１個のバ−ナ−でも原料ガスを供給する各環状部分につながる異なるポート毎に原料ガスを制御して供給する必要がある。
ところで、前記従来法では、運転中は原料タンク１の原料の重量を常時計量して内部の原料量が一定限度以下となったときは、間欠的に常温の原料液を配管１４により、所定の気液平衡温度に温度調整している原料タンク１へ補給し、稼働中の原料需給をバランスさせている。
従って、原料タンク１へ原料液を補給する度に原料タンク１の原料ガスの温度が一時的に変動し、これにともない蒸気圧が変動し、反応容器７への原料ガスの供給が変動することがある。このため光ファイバ母材１８の品質が一定せず不良品が生ずることがある。
また半導体を製造する場合においても、同様な原因により不良が生ずる場合がある。
【００１０】
なお、上記供給の不安定化は、原料液の自動調整弁１６の設定流量を、反応容器７が全て稼働したときに合わせて設定しているので、反応容器７が１００％稼動しているときは各瞬時での原料需給バランスがとれているので、上記課題は問題とならない。但し、反応容器７が１つでも稼動を停止するときは、各瞬時での需給バランスにギャップを生じ、上記課題が大きな問題となる場合がある。
【００１１】
【課題を解決するための手段】
本発明は、原料タンク１へ補給する原料液を予め加熱して、原料タンク１へ原料を補給する際の原料タンク１の原料の温度の変動を小さくすることによって蒸気圧の変動を出来るだけ少なくして、反応容器７への原料ガスの供給を安定化させることを特徴とする。 更に、補給する原料液の温度と原料タンク内の原料の温度との間になお若干の温度差がある場合であっても、反応容器７への原料ガスの供給量に不足をきたさない範囲で、原料タンク１への原料液の供給を時間的に極力均等化すことによって、原料タンク１へ原料液を補給する際のタンク１の内部の原料温度の変動を小さくし、反応容器７への原料ガスの供給を安定化させることを特徴とする。
【００１３】
従来、原料タンク１への補液の流量について、反応容器７が全て稼働したときの流量に合わせて一定値に設定していたのを改め、原料液の自動開閉弁と流量調整弁を各々に備えた複数の原料液調整配管を設置し、各々の自動開閉弁を開閉し、常時、反応容器７での稼働状態に見合った流量で原料液を原料タンク１へ補給出来るように改良したことを特徴とするものである。
即ち、
【００１４】
具体的に、請求項１にかかる発明は、原料液を収容する原料タンクと、この原料液を加熱する手段と、前記原料タンク内で気化した原料ガスを複数のバ−ナ−へ導く複数の原料ガス用配管と、この複数の原料ガス用配管それぞれに取付けられた原料ガスの開閉装置及び原料ガスの流量調整装置と、前記原料タンク内の原料の量をモニタ−する重量計と、前記原料タンクへ原料液を補液する原料液用配管とを備えた原料供給装置において、前記原料液用配管の途中に液溜りを設け、この液溜りをヒ−タで加熱し、この液溜りの下流側の原料液用配管の一部区間に複数の原料液調整用配管を設け、前記各原料液調整用配管に設けられた原料液の自動開閉弁と事前に流量を設定された流量調整弁とを介して原料液を前記原料タンクへ補液し、前記原料液調整用配管の数が、前記複数のバ−ナ−の総数と同じか又はそれ以上であり、前記原料ガスの開閉装置は、対応する前記自動開閉弁の開閉と連動して開閉することを特徴とする原料供給装置である。
【００１９】
【作用】
本発明では、原料タンク１へ供給する原料液を予め加熱して供給するので、原料タンク１へ原料を補給する際に、原料タンク１の原料の温度に影響を及ぼすことが少なくなり、その結果蒸気圧の変動が減り、安定的に反応容器７に原料ガスを供給できる。
【００２０】
また、原料タンク１への原料液の供給を時間的に均等化して供給するので、原料補給の際の原料タンク１の内部の原料の温度への影響が少なくなり、蒸気圧の変動が減り、安定的に反応容器７に原料ガスを供給できる。
即ち、従来は比較的長い期間について原料の需給をバランスさせていたので、各瞬時でみると需給バランスは必ずしもバランスしておらず、１度に多量に常温の原料液が原料タンクに供給され蒸気圧が変動し安定供給を害する場合があるが、本発明により各瞬時でも原料需給をバランスさせるのて、原料タンクの原料温度の変動が減少し、反応容器７への原料ガスの安定供給をはかることができる。
【００２１】
これにより、製品である光ファイバ母材の品質を一定とすることが出来る。また、製品である半導体の不良を減らすことが出来る。
【００２２】
【実施例】
以下、添付図面を参照しながら本発明の実施例を詳細に説明する。なお、図面の説明おいて同一の要素には同一の符号を付し、重複する説明を省略する。
【００２３】
第１の実施例について説明する。図１は、本実施例にかかる原料供給装置である。図１において、原料タンク１へ原料液を補給する配管１４の途中に、液溜り２２を設け、この部分をヒ−タ１９により加熱する。これにより、原料液に十分余熱を与え、原料タンク１へ補給する際の原料タンク１の内部の原料液の温度の変動を小さくする。
【００２４】
また、反応容器７への原料ガスの流量に応じて、原料タンク１への原料液の補液の流量を設定することにより、原料タンク１への原料液の供給を時間的に最大限均して、原料タンク１へ原料液を補給する際の原料温度の変動を極力小さくし、反応容器７への原料ガスの供給を安定化させる。
このため、原料タンク１へ原料液を補給する配管１４を、各反応容器のバ−ナ−に対応して複数設け、これに自動開閉弁２０と流量調整弁１６を取付け、各反応容器の各バ−ナ−への原料ガスの流量に応じて、対応する各配管内の流量を設定のうえ相互に独立に原料液を原料タンク１へ補給するものである。
本実施例は、稼働中の各反応容器７の各バ−ナ−への各配管８の原料ガスの流量は一定で殆ど変わらないという事実にもとづくものであり、これにより配管１４に取付けた流量調整弁１６の流量は一度設定しておけばその後は原則として調整は不要である。
【００２５】
具体的には、原料タンク１へ原料液を補給する配管１４は、反応容器７のバ−ナ−１７と同じ数が設置されており、各配管１４1 、１４2 、 １４3 には、それぞれ自動開閉弁２０1 、２０2 、２０3 と流量調整弁１６1 、１６2 、１６3 が取付けられていて、各反応容器７1 、７2 、７3 の各バ−ナ−１７1 、１７2 、１７3 への原料ガスの供給量に応じてそれぞれ独立に調整制御する。これら原料液の各自動開閉弁２０1 、２０2 、２０3 は、これと対応する原料ガスの各自動開閉弁１０1 、１０2 、１０3 が開いたら開き、同じくこれが閉じたら閉じるように制御する。原料液の各流量調整弁１６1 、１６2 、１６3 は、これと対応する 反応容器７1 、７2 、７3 の各バ−ナ−１７1 、１７2 、１７3 へ原料液２を気化させ供給する各蒸気量と原料タンク１への原料液の各補給量とがそれぞれ同じか又は後者が若干大きくなるように調整しておく。
【００２６】
これにより、例えば反応容器７1 のみが稼働しているときは、このバ−ナ−１７1 に供給される原料ガスの自動開閉弁１０1 、原料液を制御する自動開閉弁２０1 、流量調整弁１６等によって反応容器７1 での反応量に見合った原料液が原料タンク１へ補給され、原料タンク１での原料の温度変化を減少させることが出来る。
【００２７】
これにより、反応容器７の一部の反応容器の運転が停止され稼働状態が変動する場合であっても、原料タンク１には常に原料液２が気化した分だけの原料液を、配管１４を介して原料タンク１へ補給すことが出来、反応容器７への原料ガスの供給量が安定する。
また自動開閉弁２０の作動回数が従来の作動回数に比較して格段に減少し、その寿命も伸びる効果もある。
【００２８】
本実施例では、配管８、１４は、反応容器７のバ−ナ−１７とそれぞれ同数設けたが、これに限るものでなく、反応容器７に多重管バ−ナがある場合には、この多重管バ−ナ−の異なるポ−ト毎に配管８が設けられ、この複数の配管８のそれぞれに配管１４が対応することになる。
【００２９】
本実施例は、特に新しい部品を必要とせず、従来設備に用いていた特性のよく分かった部品を用いて実用化できる点に利点がある。
【００３０】
次に第２の実施例について説明する。図２に本実施例にかかる原料供給装置を示す。本実施例は、一つの配管１４に、例えば液体を対象とするマスフロ−コントロ−ラなどの流量制御装置２１を設け、各反応容器７のバ−ナ−１７への原料ガスの総流量に応じて、この流量制御装置２１により配管１４から原料液を原料タンク１へ補給するものである。
【００３１】
具体的には、図２に示すように、原料タンク１へ原料液を補給する配管１４に自動制御可能な流量制御装置２１を取付ける。この流量制御装置２１を、配管８に取付けた流量調整装置１１で計測した原料ガスの総流量に応じて自動制御することで、常に原料液２が気化した分だけの原料液を、原料タンク１に補給することができ、これにより反応容器７への原料ガスの供給量を安定化することができる。また、自動弁１５の作動回数を格段に減少させることが出来る。
【００３２】
本実施例では、各反応容器７に１つのバ−ナ−１７と１つの配管８を設けたケ−スであるが、これに限るものでなくバ−ナ−１７と配管８が複数の場合であってもよい。
【００３３】
【効果】
以上説明したように、本発明によれば、反応容器への原料ガスの供給を安定化させることにより、製品である光ファイバ母材の品質を安定化させ、結果としてこれを紡糸して得た光ファイバの品質が向上する。半導体の製造に用いた場合には、半導体の品質が向上する。
また、原料液の原料タンクへの補給を時間的に均すことにより自動開閉弁の開閉の頻度が少なくなり、自動開閉弁の寿命が伸びるという効果もある。
【００３４】
【図面の簡単な説明】
【図１】第１の実施例の原料供給装置を示す。
【図２】第２の実施例の原料供給装置を示す。
【図３】従来の原料供給装置を示す。
【符号の説明】
１：原料タンク
２：原料液
３、１９：ヒ−タ
４：温度センサ
５：温度調整器
６：上部空間
７：反応容器
８、１４：配管
９：開閉弁
１０、１２、１５、２０：自動開閉弁
１１：流量調整装置
１６：流量調整弁
１７：バ−ナ
１８：光ファイバ母材
２１：流量制御装置
２２：液溜り
２３：重量計[0001]
[Industrial application fields]
The present invention relates to a raw material supply apparatus and a raw material capable of stably and stably introducing a liquid raw material such as SiCl 4 or GeCl 4 used for manufacturing an optical fiber preform or a semiconductor into a reaction vessel in a large amount while controlling the flow rate precisely. It relates to a supply method.
[0002]
[Prior art]
As a method for manufacturing an optical fiber preform, a so-called VAD method, an external method, an internal method, and the like are known. Among these, in the VAD method that requires the supply of the raw material gas continuously for a long time, the raw material gas obtained by vaporizing the liquid glass raw material is sent to the reaction vessel at atmospheric pressure or higher and burned in the oxyhydrogen burner. And is deposited in the axial direction on the basis of the rotating starting base material to form a rod-shaped porous base material, and this multi-hard base material is spun into an optical fiber. For this reason, a raw material supply apparatus that continuously supplies a large amount of raw material gas to the reaction vessel is used.
[0003]
An example of such a raw material supply apparatus is shown in FIG. According to the raw material supply apparatus shown in FIG. 3, the airtight raw material tank 1 contains the raw material liquid 2 that reacts with oxygen or moisture in the atmosphere, and the raw material liquid 2 is vaporized outside the raw material tank 1. The heater 3 is attached, and this heater 3 is controlled by a temperature sensor 4 and a temperature regulator 5 so that the temperature of the raw material liquid 2 is precisely controlled. The upper space 6 of the raw material tank 1 is filled with the raw material gas obtained by vaporizing the raw material liquid 2 at the vapor pressure at the temperature of the raw material tank 1, and a pipe for supplying the raw material gas between the raw material tank 1 and the reaction vessel 7. 8 is arranged.
[0004]
On the pipe 8, an on-off valve 9, an automatic on-off valve 10, and a flow rate adjusting device 11 are attached. The automatic opening / closing valve 10 is a device that automatically opens and closes a flow path by external control. The flow rate adjusting device 11 is a mass flow meter such as a mass flow controller. A pipe 13 with an automatic opening / closing valve 12 is connected to the primary side of the flow rate adjusting device 11, and nitrogen gas is supplied through the pipe 13.
[0005]
The automatic open / close valve 12 is linked with the automatic open / close valve 10, and when the raw material is being supplied, the automatic open / close valve 10 is opened and the automatic open / close valve 12 is closed to flow the raw material gas to the reaction vessel 7. The automatic opening / closing valve 10 is closed and the automatic opening / closing valve 12 is opened, and a nitrogen gas is allowed to flow through the piping to purge the piping.
[0006]
The raw material tank 1 is provided with a normal temperature raw material liquid from a raw material liquid service tank (not shown), and a pipe 14 to which an automatic opening / closing valve 15 and a flow rate adjusting valve 16 are attached is disposed. The flow rate adjusting valve 16 is manually set to a constant flow rate (hereinafter referred to as a flow rate in this sense, that is, a flow rate per unit time when a raw material is supplied). It is a regulating valve that can be used, and the flow rate is set based on the reaction amount when all of the reaction vessels 7 are operated.
[0007]
A weight scale 23 is attached to the raw material tank 1, and the weight of the raw material 2 is monitored by the weight scale 23. The automatic open / close valve 15 is opened and closed in conjunction with the weight of the weigh scale 23. When the automatic open / close valve 15 is opened, the raw material liquid is supplied to the raw material tank 1, and when this is closed, the supply of the raw material liquid to the raw material tank is stopped.
[0008]
The same raw material supply apparatus is also used when a semiconductor is manufactured by laminating a plurality of semiconductor layers on a semiconductor wafer.
[0009]
[Problems to be solved by the invention]
In the VAD method of the optical fiber preform manufacturing method, it is required to supply the raw material gas from the raw material tank to each gas burner of the reaction vessel with accurate and stable flow rate control. In particular, for a multi-tube burner, it is necessary to control and supply the source gas for each different port connected to each annular portion for supplying the source gas even with one burner.
By the way, in the conventional method, when the weight of the raw material in the raw material tank 1 is constantly measured during operation and the amount of the internal raw material becomes below a certain limit, the normal temperature raw material liquid is intermittently supplied through the pipe 14 to a predetermined amount. The raw material tank 1 that is temperature-adjusted to the gas-liquid equilibrium temperature is replenished to balance the supply and demand of raw materials during operation.
Therefore, every time the raw material liquid is supplied to the raw material tank 1, the temperature of the raw material gas in the raw material tank 1 is temporarily changed, the vapor pressure is changed accordingly, and the supply of the raw material gas to the reaction vessel 7 is changed. There is. For this reason, the quality of the optical fiber preform 18 is not constant and a defective product may occur.
Also, when manufacturing semiconductors, defects may occur due to the same cause.
[0010]
In addition, the destabilization of the supply is set when the flow rate of the automatic adjustment valve 16 for the raw material liquid is set when all of the reaction vessels 7 are operated, so when the reaction vessels 7 are operating 100%. Since the supply and demand balance of raw materials at each instant is balanced, the above problem does not become a problem. However, when even one reaction vessel 7 stops operating, there is a gap in the supply and demand balance at each moment, and the above problem may become a big problem.
[0011]
[Means for Solving the Problems]
In the present invention, the raw material liquid to be replenished to the raw material tank 1 is heated in advance, and the fluctuation of the vapor pressure is minimized by reducing the fluctuation of the temperature of the raw material in the raw material tank 1 when the raw material tank 1 is replenished with the raw material. Thus, the supply of the raw material gas to the reaction vessel 7 is stabilized. Furthermore, even if there is a slight temperature difference between the temperature of the raw material liquid to be replenished and the temperature of the raw material in the raw material tank, the supply amount of the raw material gas to the reaction vessel 7 is not limited. The supply of the raw material liquid to the raw material tank 1 is equalized as much as possible in time, thereby reducing the fluctuation of the raw material temperature inside the tank 1 when the raw material liquid is supplied to the raw material tank 1, and the raw material to the reaction vessel 7 is reduced. It is characterized by stabilizing the supply of gas.
[0013]
Previously, the flow rate of the replacement fluid to the raw material tank 1 was set to a constant value in accordance with the flow rate when all the reaction vessels 7 were operated, and each was equipped with an automatic on-off valve and a flow rate adjustment valve for the raw material solution. In addition, it has been improved so that the raw material liquid can be replenished to the raw material tank 1 at a flow rate corresponding to the operating state of the reaction vessel 7 at all times by installing a plurality of raw material liquid adjusting pipes , opening and closing each automatic on-off valve. It is what.
That is,
[0014]
Specifically, the invention according to claim 1 includes a raw material tank that contains a raw material liquid, a means for heating the raw material liquid, and a plurality of gasses that are vaporized in the raw material tank to a plurality of burners. A raw material gas pipe, a raw material gas switching device and a raw material gas flow rate adjusting device attached to each of the plurality of raw material gas pipes, a weigh scale for monitoring the amount of raw material in the raw material tank, and the raw material In a raw material supply apparatus having a raw material liquid pipe for replenishing the raw material liquid to the tank, a liquid reservoir is provided in the middle of the raw material liquid pipe, and the liquid reservoir is heated by a heater, downstream of the liquid reservoir A plurality of raw material liquid adjusting pipes are provided in a part of the raw material liquid piping, and an automatic opening / closing valve of the raw material liquid provided in each of the raw material liquid adjusting pipes and a flow rate adjusting valve whose flow rate is set in advance are provided. and replacement fluid raw material liquid to the raw material tank through said original The number of liquid adjusting pipe, said plurality of bar - Na - is the total number equal to or greater than the of the opening and closing device of the raw material gas, the opening and closing in conjunction with opening and closing of the corresponding automatic opening and closing valve This is a raw material supply device.
[0019]
[Action]
In the present invention, since the raw material liquid supplied to the raw material tank 1 is heated and supplied in advance, when the raw material is supplied to the raw material tank 1, the temperature of the raw material in the raw material tank 1 is less affected. The fluctuation of the vapor pressure is reduced, and the raw material gas can be stably supplied to the reaction vessel 7.
[0020]
Moreover, since the supply of the raw material liquid to the raw material tank 1 is equalized in time, the influence on the temperature of the raw material inside the raw material tank 1 during the replenishment of the raw material is reduced, and the fluctuation of the vapor pressure is reduced. The source gas can be stably supplied to the reaction vessel 7.
In other words, since the supply and demand of raw materials has been balanced for a relatively long period of time, the balance of supply and demand is not always balanced when viewed instantaneously, and a large amount of room temperature raw material liquid is supplied to the raw material tank at one time. Although the pressure may fluctuate and the stable supply may be harmed, the present invention balances the supply and demand of the raw material even at each instant, so that the fluctuation of the raw material temperature in the raw material tank is reduced and the stable supply of the raw material gas to the reaction vessel 7 is achieved. be able to.
[0021]
Thereby, the quality of the optical fiber preform which is a product can be made constant. Further, it is possible to reduce defects in the semiconductor that is the product.
[0022]
【Example】
Hereinafter, embodiments of the present invention will be described in detail with reference to the accompanying drawings. In the description of the drawings, the same elements are denoted by the same reference numerals, and redundant description is omitted.
[0023]
A first embodiment will be described. FIG. 1 shows a raw material supply apparatus according to this embodiment. In FIG. 1, a liquid reservoir 22 is provided in the middle of a pipe 14 for supplying the raw material liquid to the raw material tank 1, and this portion is heated by a heater 19. Thereby, sufficient heat is given to the raw material liquid, and the fluctuation of the temperature of the raw material liquid in the raw material tank 1 when the raw material tank 1 is supplied is reduced.
[0024]
In addition, by setting the flow rate of the raw material liquid supplement to the raw material tank 1 according to the flow rate of the raw material gas to the reaction vessel 7, the supply of the raw material liquid to the raw material tank 1 is leveled to the maximum with time. The fluctuation of the raw material temperature when supplying the raw material liquid to the raw material tank 1 is minimized, and the supply of the raw material gas to the reaction vessel 7 is stabilized.
Therefore, a plurality of pipes 14 for replenishing the raw material liquid to the raw material tank 1 are provided corresponding to the burners of each reaction container, and an automatic opening / closing valve 20 and a flow rate adjusting valve 16 are attached thereto, In accordance with the flow rate of the raw material gas to the burner, the flow rate in each corresponding pipe is set and the raw material liquid is replenished to the raw material tank 1 independently of each other.
The present embodiment is based on the fact that the flow rate of the raw material gas in each pipe 8 to each burner of each reaction vessel 7 in operation is constant and hardly changes. Once the flow rate of the adjusting valve 16 is set, in principle, no adjustment is necessary thereafter.
[0025]
Specifically, the same number of pipes 14 for replenishing the raw material liquid to the raw material tank 1 are installed as the burners 17 of the reaction vessel 7, and each of the pipes 14 1 , 14 2 , and 14 3 is provided with Automatic open / close valves 20 1 , 20 2 , and 20 3 and flow rate adjusting valves 16 1 , 16 2 , and 16 3 are attached to the respective burners 17 1 , 17 of the reaction vessels 7 1 , 7 2 , 7 3. 2 and 17 3 are adjusted and controlled independently according to the amount of source gas supplied to 17 3 . These automatic opening / closing valves 20 1 , 20 2 , 20 3 for the raw material liquid are controlled so that they are opened when the corresponding automatic opening / closing valves 10 1 , 10 2 , 10 3 for the corresponding raw material gas are opened, and are also closed when this is closed. To do. Each flow regulating valve 16 1 , 16 2 , 16 3 of the raw material liquid supplies the raw material liquid 2 to each burner 17 1 , 17 2 , 17 3 of the corresponding reaction vessel 7 1 , 7 2 , 7 3. Each vapor amount to be vaporized and supplied and each replenishment amount of the raw material liquid to the raw material tank 1 are respectively the same or adjusted so that the latter becomes slightly larger.
[0026]
Thus, for example, when only the reaction container 7 1 is operating, the bar - Na -17 automatic opening and closing valve 10 1 of the raw material gas supplied to the 1, the automatic opening and closing valve 20 1 for controlling the raw material liquid flow rate adjustment material solution commensurate with the reaction volume in the reaction vessel 71 by the valve 16 or the like is replenished to the raw material tank 1, it is possible to reduce the temperature change of the material in the material tank 1.
[0027]
As a result, even when the operation of some reaction vessels of the reaction vessel 7 is stopped and the operating state fluctuates, the raw material liquid corresponding to the amount of the vaporized raw material liquid 2 is always supplied to the raw material tank 1 through the pipe 14. Thus, the raw material tank 1 can be replenished, and the supply amount of the raw material gas to the reaction vessel 7 is stabilized.
In addition, the number of operations of the automatic opening / closing valve 20 is significantly reduced as compared with the conventional number of operations, and the life of the automatic opening / closing valve 20 is increased.
[0028]
In this embodiment, the same number of pipes 8 and 14 as the burners 17 of the reaction vessel 7 are provided. However, the present invention is not limited to this, and when the reaction vessel 7 has a multi-tube burner, A pipe 8 is provided for each different port of the multiple pipe burner, and a pipe 14 corresponds to each of the plurality of pipes 8.
[0029]
This embodiment is advantageous in that it does not require any new parts and can be put into practical use by using parts with well-known characteristics used in conventional equipment.
[0030]
Next, a second embodiment will be described. FIG. 2 shows a raw material supply apparatus according to this example. In this embodiment, a flow rate control device 21 such as a mass flow controller for liquid is provided in one pipe 14, and according to the total flow rate of the raw material gas to the burner 17 of each reaction vessel 7. Thus, the raw material liquid is supplied to the raw material tank 1 from the pipe 14 by the flow rate control device 21.
[0031]
Specifically, as shown in FIG. 2, a flow rate control device 21 that can be automatically controlled is attached to a pipe 14 that supplies the raw material liquid to the raw material tank 1. By automatically controlling the flow rate control device 21 according to the total flow rate of the raw material gas measured by the flow rate adjusting device 11 attached to the pipe 8, the raw material liquid that is always vaporized from the raw material liquid 2 is always supplied to the raw material tank 1. Thus, the supply amount of the raw material gas to the reaction vessel 7 can be stabilized. Further, the number of operations of the automatic valve 15 can be significantly reduced.
[0032]
In this embodiment, each reaction vessel 7 is provided with one burner 17 and one pipe 8. However, the present invention is not limited to this case, and there are a plurality of burners 17 and pipes 8. It may be.
[0033]
【effect】
As described above, according to the present invention, by stabilizing the supply of the raw material gas to the reaction vessel, the quality of the optical fiber preform that is the product is stabilized, and as a result, this is obtained by spinning. The quality of the optical fiber is improved. When used for semiconductor manufacturing, the quality of the semiconductor is improved.
In addition, by leveling the replenishment of the raw material liquid into the raw material tank over time, the frequency of opening and closing of the automatic open / close valve is reduced, and the life of the automatic open / close valve is extended.
[0034]
[Brief description of the drawings]
FIG. 1 shows a raw material supply apparatus according to a first embodiment.
FIG. 2 shows a raw material supply apparatus according to a second embodiment.
FIG. 3 shows a conventional raw material supply apparatus.
[Explanation of symbols]
1: Raw material tank 2: Raw material liquid 3, 19: Heater 4: Temperature sensor 5: Temperature controller 6: Upper space 7: Reaction vessel 8, 14: Pipe 9: On-off valves 10, 12, 15, 20: Automatic On-off valve 11: Flow rate adjusting device 16: Flow rate adjusting valve 17: Burner 18: Optical fiber preform 21: Flow rate control device 22: Liquid reservoir 23: Weigh scale

Claims (1)

原料液を収容する原料タンクと、この原料液を加熱する手段と、前記原料タンク内で気化した原料ガスを複数のバ−ナ−へ導く複数の原料ガス用配管と、この複数の原料ガス用配管それぞれに取付けられた原料ガスの開閉装置及び原料ガスの流量調整装置と、前記原料タンク内の原料の量をモニタ−する重量計と、前記原料タンクへ原料液を補液する原料液用配管とを備えた原料供給装置において、
前記原料液用配管の途中に液溜りを設け、この液溜りをヒ−タで加熱し、この液溜りの下流側の原料液用配管の一部区間に複数の原料液調整用配管を設け、前記各原料液調整用配管に設けられた原料液の自動開閉弁と事前に流量を設定された流量調整弁とを介して原料液を前記原料タンクへ補液し、
前記原料液調整用配管の数が、前記複数のバ−ナ−の総数と同じか又はそれ以上であり、前記原料ガスの開閉装置は、対応する前記自動開閉弁の開閉と連動して開閉することを特徴とする原料供給装置。A raw material tank for containing the raw material liquid, means for heating the raw material liquid, a plurality of raw material gas pipes for guiding the raw material gas vaporized in the raw material tank to a plurality of burners, and a plurality of the raw material gases A source gas switching device and a source gas flow rate adjusting device attached to each of the pipes, a weigh scale for monitoring the amount of the source material in the source tank, and a source liquid pipe for supplementing the source liquid to the source tank In the raw material supply apparatus comprising
A liquid reservoir is provided in the middle of the raw material liquid piping, the liquid reservoir is heated with a heater, and a plurality of raw material liquid adjusting pipes are provided in a partial section of the raw material liquid piping on the downstream side of the liquid reservoir, The raw material liquid is supplemented to the raw material tank through an automatic opening / closing valve of the raw material liquid provided in each raw material liquid adjustment pipe and a flow rate adjusting valve whose flow rate is set in advance ,
The number of the raw material liquid adjusting pipes is equal to or more than the total number of the plurality of burners, and the raw material gas opening / closing device opens and closes in conjunction with opening and closing of the corresponding automatic opening / closing valve. The raw material supply apparatus characterized by the above-mentioned.
JP21873995A 1995-08-28 1995-08-28 Raw material supply apparatus and raw material supply method Expired - Fee Related JP3707104B2 (en)

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JP3707104B2 true JP3707104B2 (en) 2005-10-19

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