JPS63176328A - Feeding of raw material and device therefor - Google Patents
Feeding of raw material and device thereforInfo
- Publication number
- JPS63176328A JPS63176328A JP511187A JP511187A JPS63176328A JP S63176328 A JPS63176328 A JP S63176328A JP 511187 A JP511187 A JP 511187A JP 511187 A JP511187 A JP 511187A JP S63176328 A JPS63176328 A JP S63176328A
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- gas
- conduit
- condenser
- pressure
- 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.)
- Granted
Links
- 239000002994 raw material Substances 0.000 title claims abstract description 99
- 239000007789 gas Substances 0.000 claims abstract description 56
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 239000012159 carrier gas Substances 0.000 claims abstract description 27
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 16
- 239000007788 liquid Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 18
- 239000013307 optical fiber Substances 0.000 abstract description 13
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 230000005587 bubbling Effects 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract description 2
- 239000003990 capacitor Substances 0.000 description 6
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000000463 material Substances 0.000 description 6
- 238000010586 diagram Methods 0.000 description 5
- 230000005540 biological transmission Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4487—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by using a condenser
-
- 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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
- C23C16/4482—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material by bubbling of carrier gas through liquid source material
-
- 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
-
- 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
- C03B2207/88—Controlling the pressure
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Mechanical Engineering (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacture, Treatment Of Glass Fibers (AREA)
- Feeding, Discharge, Calcimining, Fusing, And Gas-Generation Devices (AREA)
- Crystals, And After-Treatments Of Crystals (AREA)
- Chemical Vapour Deposition (AREA)
Abstract
Description
【発明の詳細な説明】
〈発明の属する技術分野〉
この発明は光フアイバ母材の製造や化合物半導体の製造
の際に、供給する原料ガスの流景を精密にコントロール
し反応容器に送給できる原料供給方法およびこの方法を
実施するための装置に関する。[Detailed description of the invention] <Technical field to which the invention pertains> This invention enables precise control of the flow of raw material gas to be supplied to a reaction vessel during the production of optical fiber base materials and compound semiconductor production. The present invention relates to a raw material supply method and an apparatus for implementing this method.
く技術的背景〉
光フアイバ母材や半導体を製造する場合において、原料
液を入れたバブラー器（つまりあわ立て器）にキャリヤ
ガスを送入して原料液をあわ立て（バブリング）、この
時発生する原料ガスをキャリヤガスと混合させて、生じ
た混合ガスを導管内を通して反応容器内に送給する原料
供給方法は公知である。Technical background: When manufacturing optical fiber base materials or semiconductors, carrier gas is fed into a bubbler containing a raw material liquid to foam the raw material liquid (bubbling). A raw material supply method is known in which a raw material gas is mixed with a carrier gas and the resulting mixed gas is fed into a reaction vessel through a conduit.
このような原料供給方法を遂行する装置として、光フア
イバ母材の製造に使用する原料供給装置１３を示すと、
第３図に示すように５ｉＣ１４やＧ ｅ Ｃｌ、などの
原料液ｌを入れた気密なバブラー器″２の外周にヒータ
３を配し、バブラー晋２中の原料２１を所定温度に加熱
する。As a device for carrying out such a raw material supply method, a raw material supply device 13 used for manufacturing an optical fiber base material is shown below.
As shown in FIG. 3, a heater 3 is disposed around the outer periphery of an airtight bubbler ``2'' containing a raw material liquid 1 such as 5iC14 or GeCl, and the raw material 21 in the bubbler 2 is heated to a predetermined temperature.
一方、バブラー器２にはガス供給源（非図示）から導管
４を通してＮ２などのキャリヤガスを供給し、原料液１
中に押入した開放端からキャリヤガスを吹き出させてバ
ブリングし、この時キャリヤガス中に原料ガスが蒸発し
て発生したキャリヤガスと原料ガスの混合ガスをバブラ
ー器の原料液１上部空間に満たし、この空間内に吸入端
６を配した配管７を介しコンデンサ（凝縮器）８を通過
させて反応容器（非図示）へ送給する。On the other hand, a carrier gas such as N2 is supplied to the bubbler 2 from a gas supply source (not shown) through a conduit 4, and the raw material liquid 1 is supplied with a carrier gas such as N2.
The carrier gas is blown out from the open end pushed inside to create bubbles, and at this time, the mixed gas of the carrier gas and the raw material gas generated by evaporation of the raw material gas in the carrier gas fills the upper space of the raw material liquid 1 of the bubbler, The liquid is fed to a reaction vessel (not shown) through a condenser (condenser) 8 through a pipe 7 having a suction end 6 disposed in this space.
上記原料供給装置において、バブラー器２内に送るキャ
リヤガスの流量は導管４に介装した精密流量計５によっ
て一定量となるようにコントロールされている。また、
コンデンサ８は循環水等によってバブラー器２の温度よ
りも低い一定温に保持され、配管７によってコンデンサ
ｓ内を通る原料ガスとキャリヤガスの混合ガスは原料ガ
スの一部が凝縮しこの低められた一定温度での原料ガス
と混合ガスの飽和蒸気となり、反応容器内へ送られる。In the above raw material supply device, the flow rate of the carrier gas sent into the bubbler device 2 is controlled to be a constant amount by a precision flow meter 5 interposed in the conduit 4. Also,
The condenser 8 is maintained at a constant temperature lower than the temperature of the bubbler 2 by circulating water, etc., and the mixed gas of raw material gas and carrier gas passing through the condenser s through the pipe 7 is lowered by condensing a part of the raw material gas. The raw material gas and mixed gas become saturated vapor at a constant temperature and are sent into the reaction vessel.
反応容器に送られる原料ガスの単位時間当りの流量Ｑ６
は、キャリヤガスの単位時間当りの流量をＱｏ、コンデ
ンサ８の湿度をＴ１温度Ｔにおける原料液の飽和蒸気圧
をＰ、（Ｔ）、コンデンサ出口の配管圧力をＰとすると
、これらの間に
で表わされる関係がある。第３図に示す構造の原料供給
装置では、キャリヤガスの流量Ｑ。Flow rate per unit time of raw material gas sent to the reaction vessel Q6
is the flow rate per unit time of the carrier gas, T1 is the humidity of the condenser 8, P is the saturated vapor pressure of the raw material liquid at temperature T, (T), and P is the piping pressure at the outlet of the condenser. There is a relationship that is expressed. In the raw material supply device having the structure shown in FIG. 3, the carrier gas flow rate Q.
およびコンデンサ温度Ｔを精密にコントロールし、原料
ガスの流量ＱＳを一定に保持できるとされていた。It was said that the condenser temperature T could be precisely controlled and the flow rate QS of the source gas could be kept constant.
〈発明が解決しようとする問題点〉
ところが上述した、従来の原料供給装置（原料供給方法
）では、コンデンサ８の出口側におけろ混合ガスの圧力
は一定であるとの考えの下に原料を供給していた。<Problems to be Solved by the Invention> However, in the conventional raw material supply device (raw material supply method) described above, the raw material is supplied based on the idea that the pressure of the mixed gas at the outlet side of the condenser 8 is constant. was supplying.
しかし、気相軸付は法（いわゆるｒＶＡＤ法」）におけ
る光フアイバ母材の反応容器は通常常圧下で使用してい
るので、コンデンサの出口側配管圧力と反応容器との間
の圧力損失が一定であるか、非常に小さいとしても、上
述した反応容器は常圧下にあるので、その絶対圧力は大
気圧の変動に応じて変動し、その変動分が原料ガスの流
量Ｑ９の変動となる。However, since the reaction vessel made of optical fiber base material in the vapor phase axis method (so-called rVAD method) is usually used under normal pressure, the pressure loss between the condenser outlet piping pressure and the reaction vessel is constant. Even if it is very small, since the above-mentioned reaction vessel is under normal pressure, its absolute pressure fluctuates in accordance with the fluctuations in atmospheric pressure, and the fluctuation amount becomes a fluctuation in the flow rate Q9 of the raw material gas.
たとえば大気圧が７６０±１０ｍＨｇ（約１．３％）変
動すると、５ｉＣｊ４をコンデンサ温度３６．０℃（飽
和蒸気圧３６６ ｍＨｇ ）で供給した場合、原料ガス
の流量Ｑ６の誤差ΔＱ９は、となり、約±１．３％の大
気圧変動に対して±２．５％の原料ガス流量変動を生ず
る。従来はこの程度の原料ガスの流量誤差は無視してき
たが、より安定した光フアイバ母材を作製するためには
、この変動を無視することができない。For example, when the atmospheric pressure fluctuates by 760±10 mHg (approximately 1.3%) and 5iCj4 is supplied at a condenser temperature of 36.0°C (saturated vapor pressure 366 mHg), the error ΔQ9 in the raw material gas flow rate Q6 becomes approximately A fluctuation in the raw material gas flow rate of ±2.5% occurs for a fluctuation in atmospheric pressure of ±1.3%. Conventionally, errors in the flow rate of raw material gas of this magnitude have been ignored, but in order to produce a more stable optical fiber base material, this variation cannot be ignored.
この発明は、このような原料供給方法における従来方法
の欠点を除去するためになされたものであって、反応容
器内の圧力が変動しても安定した流量で原料ガスを反応
容器へ送給できる原料供給方法を提供しようとするもの
である。This invention was made in order to eliminate the drawbacks of the conventional raw material supply method, and it is possible to feed raw material gas to the reaction vessel at a stable flow rate even if the pressure inside the reaction vessel fluctuates. The purpose is to provide a raw material supply method.
また、この発明はこのように反応容器の圧力が変動して
も安定した流量で反応容器に原料ガスを送給できる原料
供給装置を提供しようとするものである。Another object of the present invention is to provide a raw material supply device that can feed raw material gas to a reaction vessel at a stable flow rate even when the pressure in the reaction vessel fluctuates.
く問題点を解決するための手段および作用〉上述の目的
を達成するための、この発明にかかる原料供給方法は気
密なバブラー器に入れた原料液にキャリヤガスを毎時一
定量送って原料液をバブリングし、この時発生する原料
ガスを上記キャリヤガスに混合させ、生成した混合ガス
を一定温度で飽和蒸気として反応容器内へ送給する原料
供給方法において、原料ガスを反応容器へ送給する間、
反応容器へ送給する混６合ガスの飽和蒸気のガス圧を一
定に維持するようにコントロールして原料ガスを送給す
ることを特徴とするものである。Means and operation for solving the problems> In order to achieve the above-mentioned object, the raw material supply method according to the present invention supplies a constant amount of carrier gas to the raw material liquid in an airtight bubbler device every hour. In a raw material supply method that involves bubbling, mixing the raw material gas generated at this time with the carrier gas, and supplying the generated mixed gas as saturated vapor at a constant temperature into the reaction vessel, the raw material gas is supplied to the reaction vessel. ,
This method is characterized in that the raw material gas is fed while controlling the gas pressure of the saturated vapor of the mixed gas to be fed to the reaction vessel to be kept constant.
このように、反応容器に送給する混合ガスの飽和蒸気の
絶対圧力が一定になるようにコントロールするから、反
応容器の圧力が変動しても送給する原料ガスの流量は一
定になる。In this way, since the absolute pressure of the saturated vapor of the mixed gas supplied to the reaction vessel is controlled to be constant, the flow rate of the raw material gas to be supplied remains constant even if the pressure of the reaction vessel fluctuates.
また、上述した原料供給方法を遂行するための装置は一
定流量のキャリヤガスを送入すべく流量計を介して開放
端を原料液内に挿入した導管が設けられ原料液を気密に
入れたバブラー器と；上記キャリヤガスの流入によりバ
ブリングされた原料液から発生した原料ガスとキャリヤ
ガスの混合ガスを定温度に保持したコンデンサに導く導
管と、このコンデンサにより生成した上記混合ガスの飽
和蒸気をコンデンサから反応容器へ導く導管と、当該導
管内の混合ガスの飽和蒸気の圧力を一定に維持すべくコ
ントロールする圧力制御手段とから構成することを特徴
とするものである。In addition, the device for performing the above-mentioned raw material supply method is a bubbler in which a conduit whose open end is inserted into the raw material liquid via a flow meter is installed to supply a constant flow rate of carrier gas, and the raw material liquid is airtightly filled. A conduit that guides the mixed gas of the raw material gas and carrier gas generated from the bubbled raw material liquid by the inflow of the carrier gas to a condenser maintained at a constant temperature, and a conduit that directs the saturated vapor of the mixed gas generated by the condenser to the condenser. This system is characterized by comprising a conduit leading from the gas to the reaction vessel, and a pressure control means for controlling the pressure of the saturated vapor of the mixed gas in the conduit to maintain it constant.
この発明の原料供給装置は以上のように構成されている
から、大気圧の変動を受けないコンデンサの出口と反応
容器間の導管中に送入されたキャリヤガスと原料ガスの
混合ガスの絶対圧力を圧力制御手段により一定に維持す
るから、コンデンサ出口の飽和蒸気の圧力Ｐ０を反応容
器の変動に関係なく一定に維持することができる。Since the raw material supply device of the present invention is configured as described above, the absolute pressure of the mixed gas of carrier gas and raw material gas fed into the conduit between the outlet of the condenser and the reaction vessel is not affected by atmospheric pressure fluctuations. is kept constant by the pressure control means, so the pressure P0 of saturated steam at the outlet of the condenser can be kept constant regardless of fluctuations in the reaction vessel.
したがって、式（１１にしたがって、コンデンサ温度Ｔ
１キャリヤガスの流量一定という条件に加え、飽和蒸気
のコンデンサ出口側圧力Ｐ０も精密にコントロールされ
るようになっているから、原料ガスの流量Ｑ、は従来の
原料供給装置にくらべて精密にコントロールされる。Therefore, according to equation (11), the capacitor temperature T
1 In addition to the condition that the flow rate of the carrier gas is constant, the condenser outlet pressure P0 of saturated steam is also precisely controlled, so the flow rate Q of the raw material gas can be controlled more precisely than in conventional raw material supply devices. be done.
く実 施 例〉
つぎに、この発明の原料供給装置の実施例に基づいて、
同時に原料供給方法についても具体的に説明する。Embodiment Next, based on an embodiment of the raw material supply device of the present invention,
At the same time, a raw material supply method will also be specifically explained.
第１図はこの発明の代表的な原料供給装置の概略構成を
示す。この原料供給装置１３Ａは、気密なバブラー器２
に原料液１金入れ、バブラー器２の外周にヒータ３を配
し、バブラー襞２内原料ｗ！ｔ、１を所定温度に保持す
る。FIG. 1 shows a schematic configuration of a typical raw material supply device of the present invention. This raw material supply device 13A includes an airtight bubbler device 2
Place the raw material liquid in the container, place the heater 3 around the outer periphery of the bubbler device 2, and place the raw material inside the bubbler fold 2! t,1 is maintained at a predetermined temperature.
バブラー器２内原料液１中に開放端を突込むようにして
バブラー器２外のガス供給源（非図示。）からキャリヤ
ガスを一定流量で供給すべく導管４が精密流量計５を介
して原料液中に送られている。A conduit 4 is inserted into the raw material liquid 1 through a precision flow meter 5 to supply carrier gas at a constant flow rate from a gas supply source (not shown) outside the bubbler 2 with its open end inserted into the raw material liquid 1 in the bubbler 2. is being sent to.
バブラー器２に入れた原料液１の上部空間には吸収端６
を配した導管７が配され、他端はコンデンサ８を通って
反応容器（非図示）に導かれる。導管７のコンデンサ８
の二次側（出口側）には圧力変換器９がとりつけられ、
その下流にはコントロールバルブ１０が設けられている
。There is an absorption edge 6 in the upper space of the raw material liquid 1 put into the bubbler device 2.
A conduit 7 is provided, the other end of which is led to a reaction vessel (not shown) through a condenser 8. conduit 7 capacitor 8
A pressure transducer 9 is installed on the secondary side (outlet side) of the
A control valve 10 is provided downstream thereof.
コントロールバルブ１０の開度は１ｔｉｌｔｌＷ１１に
よって圧力変換器９の出力信号が予め設定した値１２と
等しくなるよう制御される。The opening degree of the control valve 10 is controlled by 1tiltlW11 so that the output signal of the pressure transducer 9 becomes equal to a preset value 12.
この原料供給装置１３Ａの反応容器に送給される原料ガ
スの流量Ｑ、は
となる。式（１）と（３）の違いはコンデンサ８の出口
での圧力もが圧力変換器９で測定される圧力にほぼ等し
く、この圧力を一定になるようにコントロールされてい
るので、式（３）のＱｓは、コンデンサの温度Ｔ１キャ
リヤガスの流量Ｑ。The flow rate Q of the raw material gas fed to the reaction vessel of this raw material supply device 13A is as follows. The difference between equations (1) and (3) is that the pressure at the outlet of the capacitor 8 is almost equal to the pressure measured by the pressure transducer 9, and this pressure is controlled to be constant, so equation (3) ) is the temperature T1 of the condenser and the flow rate Q of the carrier gas.
およびコンデンサ８の出口での圧力Ｐ７が全て精密にコ
ントロールされることにより、従来装Ｗ１３（第３図に
示す）より正確になる。and the pressure P7 at the outlet of the condenser 8 are all precisely controlled, making it more accurate than the conventional system W13 (shown in FIG. 3).
つまり、原料ガスの流量Ｑ、を大気圧の変動を受けない
ようにすることができろ。In other words, it is possible to prevent the flow rate Q of the raw material gas from being affected by atmospheric pressure fluctuations.
本実施例の原料供給装置ｌｌ ３Ａを使用して気相軸付
は法でグレーデツトインデックス形（Ｇｒａｄｅｄ １
ｎｄｘ ｔｙｐｅ）光フアイバ１００本を作り１．３μ
ｍにおける伝送帯域特性分布を調べたところ第２図に示
すごとき分布ヒストグラムが得られた。Using the raw material supply device II 3A of this example, the gas phase shaft is attached to a graded index type (Graded 1
ndx type) Make 100 optical fibers and 1.3μ
When the transmission band characteristic distribution at m was investigated, a distribution histogram as shown in FIG. 2 was obtained.
製造条件は本実施例においては圧力変換器の圧力が絶対
圧９１０ｎｍＨｇになるようにコントロールバルブを制
御した。これに加えキャリヤガス流量と原料ガス流量の
比がほぼ一定になるようにコンデンサ温度Ｔを従来の原
料供給装置より高くした。例えば５ｉＣｊ４の原料供給
装置のコンデンサ温度が従来例では４２℃であったもの
を本実施例では４７℃に上昇させた。またバブラー客語
の温度はコンデンサ温度よりそれぞれ高くなるように設
定した。In this example, the manufacturing conditions were such that the control valve was controlled so that the pressure of the pressure transducer became an absolute pressure of 910 nmHg. In addition, the condenser temperature T was set higher than in the conventional raw material supply device so that the ratio of the carrier gas flow rate to the raw material gas flow rate was approximately constant. For example, the capacitor temperature of the 5iCj4 raw material supply device was 42°C in the conventional example, but was raised to 47°C in this example. In addition, the temperature of the bubbler was set higher than the condenser temperature.
その他の条件は両者でほぼ同じであるがそれぞれ平均帯
域が最大になるように微調整しているので完全に同じで
はない。また多孔質光フアイバ母材が生産されない以降
の工程は両者同じである。Other conditions are almost the same for both, but they are not completely the same because they are finely adjusted to maximize the average band. Further, the steps after the porous optical fiber base material is not produced are the same for both methods.
一方、従来の原料供給装置１３により、同１ 様の条件
で光ファイバを作ったときに得られる光ファイバの１．
３μｍの伝送帯域分布は第４図のごときものであった。On the other hand, when an optical fiber is produced using the conventional raw material supply device 13 under the same conditions as 1.
The transmission band distribution of 3 μm was as shown in FIG.
第２図と第４図を比較すれば本発明による原料供給装置
を使うことにより帯域特性のバラツキを小さくすること
ができ光ファイバの特性を安定に保つことは明らかであ
る。Comparing FIG. 2 and FIG. 4, it is clear that by using the raw material supply device according to the present invention, variations in band characteristics can be reduced and the characteristics of the optical fiber can be kept stable.
なお、本実施例においては全てコンデンサの存在する原
料供給装置についてのみ説明したがコンデンサが存在し
ない原料供給装置においても同様の効果が得られるのは
明らかである。この場合圧力変換器はバブラー器と反応
客語の間の導管中に設置してもバブラー器上部空間に設
置してもよい。In this embodiment, only the raw material supply apparatus in which a capacitor is present has been described, but it is clear that similar effects can be obtained in a raw material supply apparatus in which a capacitor is not present. In this case, the pressure transducer may be installed in the conduit between the bubbler and the reactor or in the space above the bubbler.
〈発明の効果〉
思上の説明から明らかなように、この発明にかかる原料
供給方法あるいは装置によれば、反応容器内の圧力（た
とえば大気圧）が変動しても、原料ガスを一定の流量で
送給することができるから光ファイバや半導体などの特
性が安定したもの製造することができる。<Effects of the Invention> As is clear from the hypothetical explanation, according to the raw material supply method or device according to the present invention, the raw material gas can be supplied at a constant flow rate even if the pressure in the reaction vessel (for example, atmospheric pressure) fluctuates. Since it can be fed in a single step, it is possible to manufacture products with stable characteristics such as optical fibers and semiconductors.
しかも、方法にしても装置にしても従来の方法および装
置において単に反応８諾に送る混合ガスの飽和蒸気の圧
力を一定となるようにコント四−ルするだけであるから
、極めて容易に行うことができる。Moreover, in the conventional method and apparatus, the pressure of the saturated vapor of the mixed gas sent to the reaction mixture is simply controlled to be constant, so it can be carried out extremely easily. Can be done.
第１図は実施例にかかるこの発明の原料供給装置の要部
概略構成図、第２図は第１図に示す原料供給装置を用い
て製造した光ファイバの伝送域帯（１，３μｍ）におけ
る製品の分布曲線図、第３図は従来の原料供給装置の要
部概略構成図、第４図は第３図の原料供給装置を用いて
製造した光ファイバの伝送域帯における製品の分布曲線
図である。
図 中、
１・・・原料液、
２・・・バブラー器、
３・・・ヒータ、
４．７・・導管、
５・・・精密流量計、
６・・・導ｖ７の吸入端、
８・・コンデンサ（凝縮器）、
９・・・圧力変換器、
１０・・・コントロールバルブ、
１１・・・制細器、
１２・・・設定値、
１３・・従来の原料供給装置、
１３Ａ・・・この発明の原料供給装置。FIG. 1 is a schematic diagram of the main parts of a raw material supply device of the present invention according to an embodiment, and FIG. 2 is a diagram showing the transmission band (1.3 μm) of an optical fiber manufactured using the raw material supply device shown in FIG. 1. Product distribution curve diagram, Figure 3 is a schematic diagram of the main parts of a conventional raw material supply device, and Figure 4 is a product distribution curve diagram in the transmission band of the optical fiber manufactured using the raw material supply device of Figure 3. It is. In the figure, 1... Raw material liquid, 2... Bubbler, 3... Heater, 4. 7... Conduit, 5... Precision flow meter, 6... Suction end of conduit v7, 8... - Condenser (condenser), 9... Pressure transducer, 10... Control valve, 11... Throttle device, 12... Set value, 13... Conventional raw material supply device, 13A... A raw material supply device of this invention.
Claims (4)
を毎時一定量送って原料液をバブリングし、この時発生
した原料ガスと上記キャリヤガスの混合ガスを一定温度
での飽和蒸気として反応容器内へ送給する原料供給方法
において、原料ガスを反応容器へ送給する間、反応容器
へ送給する混合ガスの飽和蒸気のガス全圧を一定に維持
するようにコントロールしながら原料ガスを送給するこ
とを特徴とする原料供給方法。(1) A fixed amount of carrier gas is sent every hour to the raw material liquid in an airtight bubbler to bubble the raw material liquid, and the mixed gas of the raw material gas and the carrier gas generated at this time is converted into saturated vapor at a constant temperature into a reaction vessel. In this raw material supply method, while the raw material gas is being supplied to the reaction vessel, the raw material gas is supplied while controlling the total gas pressure of the saturated vapor of the mixed gas to be supplied to the reaction vessel to be kept constant. A raw material supply method characterized by:
して開放端を原料液内に挿入した導管が設けられ原料液
を気密に入れたバブラー器と；上記キャリヤガスの流入
によりあわ立てられた原料液から発生した原料ガスとキ
ャリヤガスの混合ガスを定温度に保持したコンデンサに
導く導管と、このコンデンサにより生成した上記混合ガ
スの飽和蒸気をコンデンサから反応容器へ導く導管と、
当該導管内の混合ガスの飽和蒸気の圧力を一定に維持す
べくコントロールする圧力制御手段とからなることを特
徴とする原料供給装置。(2) A bubbler device that is equipped with a conduit whose open end is inserted into the raw material liquid via a flow meter to feed a constant flow rate of carrier gas, and the raw material liquid is airtightly filled; a conduit that leads a mixed gas of raw material gas and carrier gas generated from the raw material liquid to a condenser maintained at a constant temperature, and a conduit that leads saturated vapor of the mixed gas generated by the condenser from the condenser to the reaction vessel;
A raw material supply device comprising: pressure control means for controlling the pressure of saturated steam of the mixed gas in the conduit to maintain it constant.
度に保持することを特徴とする特許請求の範囲第（２）
項記載の原料供給装置。(3) Claim (2) characterized in that the temperature of the condenser is maintained at a lower temperature than the temperature of the bubbler device.
Raw material supply device as described in section.
する特許請求の範囲第（２）項又は第（３）項記載の原
料供給装置。(4) The raw material supply device according to claim (2) or (3), wherein the reaction vessel is configured to carry out the reaction under normal pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP511187A JPH085690B2 (en) | 1987-01-14 | 1987-01-14 | Raw material supply method and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP511187A JPH085690B2 (en) | 1987-01-14 | 1987-01-14 | Raw material supply method and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63176328A true JPS63176328A (en) | 1988-07-20 |
| JPH085690B2 JPH085690B2 (en) | 1996-01-24 |
Family
ID=11602241
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP511187A Expired - Fee Related JPH085690B2 (en) | 1987-01-14 | 1987-01-14 | Raw material supply method and device |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH085690B2 (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0240440U (en) * | 1988-09-08 | 1990-03-19 | ||
| JPH0621740U (en) * | 1992-08-21 | 1994-03-22 | 徳山曹達株式会社 | Mixed gas monomer feeder |
| WO1997014180A1 (en) * | 1995-10-12 | 1997-04-17 | Semitool, Inc. | Semiconductor processing using vapor mixtures |
| EP0949212A1 (en) * | 1998-04-09 | 1999-10-13 | Lucent Technologies Inc. | Methods of and systems for vapor delivery control in optical preform manufacture |
| EP0951052A2 (en) * | 1998-03-27 | 1999-10-20 | Kosho Komiya | Bubbler apparatus and condenser for use with the bubbler apparatus |
-
1987
- 1987-01-14 JP JP511187A patent/JPH085690B2/en not_active Expired - Fee Related
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0240440U (en) * | 1988-09-08 | 1990-03-19 | ||
| JPH0621740U (en) * | 1992-08-21 | 1994-03-22 | 徳山曹達株式会社 | Mixed gas monomer feeder |
| WO1997014180A1 (en) * | 1995-10-12 | 1997-04-17 | Semitool, Inc. | Semiconductor processing using vapor mixtures |
| US5954911A (en) * | 1995-10-12 | 1999-09-21 | Semitool, Inc. | Semiconductor processing using vapor mixtures |
| EP0951052A2 (en) * | 1998-03-27 | 1999-10-20 | Kosho Komiya | Bubbler apparatus and condenser for use with the bubbler apparatus |
| EP0951052A3 (en) * | 1998-03-27 | 2003-03-05 | Kosho Komiya | Bubbler apparatus and condenser for use with the bubbler apparatus |
| EP0949212A1 (en) * | 1998-04-09 | 1999-10-13 | Lucent Technologies Inc. | Methods of and systems for vapor delivery control in optical preform manufacture |
| US6161398A (en) * | 1998-04-09 | 2000-12-19 | Lucent Technologies, Inc. | Methods of and systems for vapor delivery control in optical preform manufacture |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH085690B2 (en) | 1996-01-24 |
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