JPH0251852B2 - - Google Patents
Info
- Publication number
- JPH0251852B2 JPH0251852B2 JP60044676A JP4467685A JPH0251852B2 JP H0251852 B2 JPH0251852 B2 JP H0251852B2 JP 60044676 A JP60044676 A JP 60044676A JP 4467685 A JP4467685 A JP 4467685A JP H0251852 B2 JPH0251852 B2 JP H0251852B2
- Authority
- JP
- Japan
- Prior art keywords
- raw material
- tank
- material tank
- supply device
- auxiliary container
- 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.)
- Expired - Lifetime
Links
- 239000002994 raw material Substances 0.000 claims description 130
- 239000007789 gas Substances 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 25
- 238000001816 cooling Methods 0.000 claims description 20
- 230000008016 vaporization Effects 0.000 claims description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000009835 boiling Methods 0.000 description 11
- 238000010586 diagram Methods 0.000 description 6
- 239000007791 liquid phase Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 229910001873 dinitrogen Inorganic materials 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000013307 optical fiber Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- 229910003902 SiCl 4 Inorganic materials 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- 229920006395 saturated elastomer Polymers 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 230000002411 adverse Effects 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000004065 semiconductor Substances 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
- C23C16/4485—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 without using carrier gas in contact with the source material
-
- 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
Description
【発明の詳細な説明】
＜産業上の利用分野＞
本発明は、光フアイバ母材あるいは半導体等の
製造に用いられるSiCl4、GeCl4などの液体原料を
精密に流量制御しつつ大量にかつ安定して反応容
器に導くことができる原料供給装置に関する。[Detailed Description of the Invention] <Industrial Field of Application> The present invention is directed to the production of liquid raw materials such as SiCl 4 and GeCl 4 used in the production of optical fiber base materials or semiconductors in large quantities and stably while precisely controlling the flow rate. The present invention relates to a raw material supply device that can feed raw materials into a reaction vessel.
＜従来の技術＞
原料供給装置を光フアイバ用母材の製造装置の
場合について説明する。光フアイバ用母材の製造
方法としては、いわゆるVAD法、外付け法、内
付け法等が知られている。このうち、とくに長時
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ーナある
いはプラズマバーナで燃焼させてガラス媒体を生
成し、回転する出発部材に軸方向に堆積させて棒
状の多孔質母材を作り、更にこの多孔質母材を光
フア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が反応容器へ
供給する原料供給装置が必要であつた。このよう
な原料供給装置の一例を第７図に示す。第７図に
示す原料供給装置によれば、気密な原料タンク１
には大気中の酸素また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の外周には原料
液２を気化するためのヒータ３が取付けられてい
る。原料タンク１の上部空間４には原料液が気化
した原料ガスが原料タンク１の温度における蒸気
圧で満されており、原料タンク１の上部空間４と
反応容器（図示せず）との間には原料ガスを送給
する配管５が配置されている。配管５には開閉弁
６、自動弁７、流量制御装置８が介装されてい
る。流量制御装置８には質量流量計（マスフロー
コントローラ）が広く用いられている。流量制御
装置８の一次側には自動弁１０を介在した配管９
が接続されていて、配管９を通じて窒素ガスが供
給されるようになつている。自動弁１０は自動弁
７と連動し、原料供給中は自動弁７が開き自動弁
１０が閉じて原料を反応容器に流し、原料の供給
をしていないときは自動弁７が閉じ自動弁１０が
開いて配管中に窒素ガスを流して配管保護のパー
ジを行なう。<Prior Art> A case will be described in which the raw material supply device is a manufacturing device for optical fiber base material. As methods for manufacturing optical fiber base materials, the so-called VAD method, external attachment method, internal attachment method, etc. are known. Among these, in the VAD method, which requires continuous supply of raw material gas for a particularly long period of time, raw material gas obtained by vaporizing liquid glass raw material is sent to a reaction vessel at above atmospheric pressure and burned in an oxyhydrogen burner or plasma burner. A medium is generated and deposited axially on a rotating starting member to form a rod-shaped porous preform, which is then spun into an optical fiber. For this reason, a raw material supply device that continuously and stably supplies a large amount of raw material gas to the reaction vessel is required. An example of such a raw material supply device is shown in FIG. According to the raw material supply device shown in FIG. 7, an airtight raw material tank 1
There is a raw material liquid 2 that reacts with oxygen or moisture in the atmosphere.
A heater 3 for vaporizing the raw material liquid 2 is attached to the outer periphery of the raw material tank 1. The upper space 4 of the raw material tank 1 is filled with raw material gas obtained by vaporizing the raw material liquid at the vapor pressure at the temperature of the raw material tank 1, and there is a gap between the upper space 4 of the raw material tank 1 and the reaction vessel (not shown). A pipe 5 for supplying raw material gas is arranged. The piping 5 is provided with an on-off valve 6, an automatic valve 7, and a flow rate control device 8. A mass flow meter (mass flow controller) is widely used as the flow rate control device 8. A piping 9 with an automatic valve 10 interposed on the primary side of the flow control device 8
is connected, and nitrogen gas is supplied through piping 9. The automatic valve 10 is interlocked with the automatic valve 7, and when the raw material is being supplied, the automatic valve 7 opens and the automatic valve 10 is closed to flow the raw material into the reaction vessel, and when the raw material is not being supplied, the automatic valve 7 is closed and the automatic valve 10 is opened and nitrogen gas flows into the pipe to purge the pipe to protect it.
第７図に示した原料供給装置を用いて原料ガス
を反応容器へ導く手順は次の如くである。原料を
供給していない状態では自動弁７は閉じ、自動弁
１０が開いて配管５の反応容器側は窒素ガスによ
りパージされている。このような状態から原料供
給を開始するためには、まず、ヒータ３を加熱し
原料タンク内の原料液を加熱し、原料タンクの上
部空間４の原料ガス圧力を大気圧以上の所定の値
にする。例えば、原料液がSiCl4で原料ガスの圧
力を１Kg／cm2Ｇにするためには、原料タンクの温
度を80℃まで加熱する。次に自動弁１０を閉じ、
自動弁７を開けて、原料ガスを反応容器へ送る。
この際流量制御装置８は原料ガスの送給量を必要
な流量に制御する。原料ガス供給の終了時には、
自動弁７を閉じ、自動弁１０を開いて配管５内を
窒素ガスでパージする。さらに、短時間で原料ガ
スの供給を再開しない場合は、ヒータ３を切り原
料タンクを冷却する。また、再開が比較的早く予
定されるときには、ヒータ３を入れたまま保温に
している。 The procedure for introducing the raw material gas into the reaction vessel using the raw material supply device shown in FIG. 7 is as follows. When raw materials are not being supplied, the automatic valve 7 is closed, the automatic valve 10 is opened, and the reaction vessel side of the piping 5 is purged with nitrogen gas. In order to start supplying raw materials from this state, first, the heater 3 is heated to heat the raw material liquid in the raw material tank, and the raw material gas pressure in the upper space 4 of the raw material tank is brought to a predetermined value higher than atmospheric pressure. do. For example, if the raw material liquid is SiCl 4 and the pressure of the raw material gas is to be 1 Kg/cm 2 G, the temperature of the raw material tank is heated to 80°C. Next, close the automatic valve 10,
Open the automatic valve 7 and send the raw material gas to the reaction vessel.
At this time, the flow rate control device 8 controls the feed rate of the raw material gas to a required flow rate. At the end of raw material gas supply,
The automatic valve 7 is closed and the automatic valve 10 is opened to purge the inside of the pipe 5 with nitrogen gas. Furthermore, if the supply of raw material gas is not restarted in a short time, the heater 3 is turned off and the raw material tank is cooled. Furthermore, when restarting is scheduled relatively soon, the heater 3 is left on to keep warm.
＜発明が解決しようとする問題点＞
上述した第７図に示す構成で原料ガスの送給を
止めてもなお、ヒータ３を入れており、原料タン
クが一定温度、例えば80℃で保たれているとき、
原料タンク内は完全な均一温度になる。この状態
では原料タンク内では温度分布による熱対流や沸
騰が生じなくなり平衡状態で液面での気液相変化
のみが生じている。このような状態で急激に自動
弁７を開いて大流量の原料ガスを反応容器へ送ろ
うとする場合、気相原料ガスが流出して原料タン
ク内圧が低下しても、沸騰が安定して開始しない
欠点を有し、また場合によつては原料タンク内圧
が原料ガス飽和蒸気圧より一時的に小さくなるた
め突沸が生じ流量制御された原料供給を安定して
行なうことができず、しかも、突沸の場合には配
管部品の破損が最悪の事態として生ずる欠点があ
る。<Problems to be Solved by the Invention> In the configuration shown in FIG. 7 described above, even if the supply of raw material gas is stopped, the heater 3 is still turned on and the raw material tank is maintained at a constant temperature, for example, 80°C. When you are there,
The temperature inside the raw material tank is completely uniform. In this state, heat convection and boiling due to temperature distribution no longer occur in the raw material tank, and only gas-liquid phase changes occur at the liquid level in an equilibrium state. In such a situation, if you suddenly open the automatic valve 7 to send a large flow of raw material gas to the reaction vessel, even if the gas phase raw material gas flows out and the internal pressure of the raw material tank decreases, boiling will start stably. In addition, in some cases, the internal pressure of the raw material tank becomes temporarily lower than the saturated vapor pressure of the raw material gas, resulting in bumping, making it impossible to stably supply raw materials with a controlled flow rate. In this case, there is a drawback that the worst case scenario is damage to piping parts.
また、沸騰開始後原料タンクは完全に定常状態
にあつて、タンクの壁温と原料の液温と気温とが
略同じであるので、急に原料ガスを流出すること
による潜熱の流出量が非常に多くなつても壁すな
わちヒータからの熱伝達が充分期待できず、液温
が一定時間下がりつづけ、この結果飽和蒸気圧と
略等しい流量制御装置の一次側ガス圧が減少し、
一定の一次二次圧力差を必要とする流量制御装置
による安定した流量制御ができなくなる。 In addition, after the start of boiling, the raw material tank is in a completely steady state, and the wall temperature of the tank, the liquid temperature of the raw material, and the air temperature are approximately the same, so the amount of latent heat flowing out due to the sudden flow of raw material gas is extremely low. Even if the temperature increases, sufficient heat transfer from the wall or heater cannot be expected, and the liquid temperature continues to drop for a certain period of time.As a result, the primary gas pressure of the flow rate control device, which is approximately equal to the saturated vapor pressure, decreases.
Stable flow control by a flow control device that requires a constant primary and secondary pressure difference becomes impossible.
そこで、本発明は上述の欠点に鑑み、ヒータに
て原料タンクを保温しているときでも原料タンク
内に温度分布を作ることにより、気液相の交換を
活発にして沸騰を常に行なわせて安定した沸騰を
行なうと共に突沸を防止し、しかも急激な原料供
給量の増加に対してもヒータからの熱伝達を充分
に行ない原料供給不足を防ぎ安定した流量制御を
行なう原料供給装置の提供を目的とする。 Therefore, in view of the above-mentioned drawbacks, the present invention creates a temperature distribution in the raw material tank even when the raw material tank is kept warm by a heater, thereby actively exchanging the gas-liquid phase and constantly boiling. The purpose of the present invention is to provide a raw material supply device that performs stable boiling and prevents bumping, and also performs sufficient heat transfer from the heater even when the raw material supply amount increases rapidly, thereby preventing a shortage of raw material supply and performing stable flow control. do.
＜問題を解決するための手段＞
上述の目的を達成する本発明は、大気中の酸素
または水分と反応する原料液を下部に有し上部に
この原料液が気下した原料ガスを収容する原料タ
ンクと、この原料液の蒸気圧が大気圧以上になる
までこの原料液を加熱する手段と、上記原料タン
ク内で気化された原料ガスを反応容器へ導く配管
と、この配管に介装された開閉及び流量制御を行
なう装置とを備える原料供給装置において、上記
原料タンク内で気化された原料ガスを冷却して上
記タンクにて熱対流を生じる機構を上記原料タン
クに備えたことを特徴とする。<Means for Solving the Problems> The present invention, which achieves the above-mentioned object, has a raw material liquid in the lower part that reacts with oxygen or moisture in the atmosphere, and a raw material liquid in the upper part that accommodates the raw material gas released from the raw material liquid. a tank, a means for heating the raw material liquid until the vapor pressure of the raw material liquid becomes equal to or higher than atmospheric pressure, a pipe for guiding the raw material gas vaporized in the raw material tank to the reaction vessel, and a pipe installed in the pipe. A raw material supply device comprising a device for opening/closing and controlling flow rate, characterized in that the raw material tank is equipped with a mechanism that cools the raw material gas vaporized in the raw material tank and generates thermal convection in the tank. .
＜作用＞
原料ガスを冷却する機構を備えたことにより、
原料タンク内に温度分布を連続して作ることがで
き、気液相の相変化を活発化でき沸騰が安定して
行なわれる。<Function> By being equipped with a mechanism to cool the raw material gas,
It is possible to create a continuous temperature distribution within the raw material tank, which activates the phase change between the gas and liquid phases, resulting in stable boiling.
＜実施例＞
ここで、第１図ないし第６図を参照して本発明
の実施例を説明する。なお、第７図と同一部分に
は同符号を付す。第１図ないし第６図において、
１は原料タンク、２は原料液、３はヒータ、４は
上部空間、５は配管、６は開閉弁、７，１０は自
動弁、８は流量制御装置、９は配管であり、この
機能は従来と同じである。<Example> Here, an example of the present invention will be described with reference to FIGS. 1 to 6. Note that the same parts as in FIG. 7 are given the same reference numerals. In Figures 1 to 6,
1 is a raw material tank, 2 is a raw material liquid, 3 is a heater, 4 is an upper space, 5 is piping, 6 is an on-off valve, 7 and 10 are automatic valves, 8 is a flow rate control device, and 9 is piping. Same as before.
第１図において、原料タンク１の上蓋には補助
容器１１が取付けられるが、この補助容器１１
は、くびれた開口部を連続部分１２として原料タ
ンク１の上部空間４に連通されている。しかも、
この補助容器１１はそれ自体外部から冷却するも
のであり、水冷又は空冷手段（公知のものが多種
あるので図示省略する）が備えられている。第１
図に示す補助容器１１はくびれた開口部を有する
が、くびれていなくともすなわち筒状の補助容器
でも何ら差支えない。 In FIG. 1, an auxiliary container 11 is attached to the upper lid of a raw material tank 1.
is connected to the upper space 4 of the raw material tank 1 using a constricted opening as a continuous portion 12. Moreover,
The auxiliary container 11 itself is cooled from the outside, and is equipped with water cooling or air cooling means (not shown as there are many known types). 1st
Although the auxiliary container 11 shown in the figure has a constricted opening, there is no problem with the auxiliary container having a cylindrical shape even if it is not constricted.
このように補助容器１１は原料タンク１の上部
空間４と連通させた場合、上部空間４の原料ガス
は、補助容器１１内で凝縮するので、自動弁７が
閉じていて原料ガスが送られなくとも、その凝縮
による分だけ開口部から原料ガスが入り、凝縮液
は開口部を伝つて原料タンク１内に戻ることにな
る。すなわち、補助容器１１の冷却量をある程度
多めにしておき、熱対流を起こし気液相変化を活
発にして沸騰が生じている状態にしておけばよ
い。 When the auxiliary container 11 is communicated with the upper space 4 of the raw material tank 1 in this way, the raw material gas in the upper space 4 condenses within the auxiliary container 11, so the automatic valve 7 is closed and the raw material gas is not sent. In either case, raw material gas enters from the opening by the amount due to the condensation, and the condensed liquid returns to the raw material tank 1 through the opening. In other words, the amount of cooling of the auxiliary container 11 may be increased to a certain extent to cause thermal convection to activate the gas-liquid phase change and bring about boiling.
かかる状態で自動弁７が開かれても、もともと
沸騰しているので沸騰開始による不安定現象は生
せず、また冷却により熱伝達も確保されているの
で原料タンクの内圧低下が極めて少なく流量制御
装置に悪影響を及ぼさない。 Even if the automatic valve 7 is opened in such a state, since the raw material is already boiling, there will be no instability due to the start of boiling, and since heat transfer is ensured by cooling, the internal pressure of the raw material tank will not drop significantly and the flow rate will be controlled. Does not adversely affect the equipment.
第２図に示す構成は、第１図に示すものとは異
なり、原料タンク１の上部に支持された補助容器
１１が、配管１３ａ，１３ｂを通じて原料タンク
１と連通されている構成である。より詳しくは、
補助容器１１の下部を配管１３ａを介して原料タ
ンク１内の原料液２中に通し、補助容器１１の下
部以外の部分（第２図では上部）を配管１３ｂを
介して原料タンク１の上部空間４に通している。
したがつて、気化された原料ガスは配管１３ｂを
通つて補助容器１１に入り、また、補助容器１１
にて液体に凝縮された原料は、配管１３ａを通つ
て原料タンク１の原料液２内に入ることになる。
かかる第２図の構造は、補助容器１１の冷却を増
大させ、例えば空冷から水冷にして循環量を多く
するときには重要になり、例えば10の原料タン
クから５／min程度の原料ガスを反応容器へ送
り出す場合はともかく、数十／min〜100／
min程度の原料ガスを送り出す場合は有用であ
る。 The configuration shown in FIG. 2 is different from that shown in FIG. 1 in that an auxiliary container 11 supported on the upper part of the raw material tank 1 is communicated with the raw material tank 1 through pipes 13a and 13b. For more details,
The lower part of the auxiliary container 11 is passed through the pipe 13a into the raw material liquid 2 in the raw material tank 1, and the part other than the lower part (the upper part in FIG. 2) of the auxiliary container 11 is passed through the pipe 13b into the upper space of the raw material tank 1. I'm passing 4.
Therefore, the vaporized raw material gas enters the auxiliary container 11 through the pipe 13b, and also enters the auxiliary container 11.
The raw material condensed into liquid in step 1 enters the raw material liquid 2 in the raw material tank 1 through the pipe 13a.
The structure shown in FIG. 2 becomes important when increasing the cooling of the auxiliary container 11, for example, changing from air cooling to water cooling to increase the circulation rate. Regardless of when sending out, tens of minutes/min to 100/
It is useful when sending out raw material gas of about min.
更に、第３図は他の変形例である。原料タンク
１から反応容器に大流量の原料ガスを供給する場
合、補助容器１１による循環量が反応容器へ供給
する側にとり負担となつて熱伝達量が少なくなる
ため、結果として原料ガスを反応容器に充分送れ
ないおそれがある。このため、第３図のように補
助容器１１への配管１３ｂに開閉弁１４を介在さ
せ、反応容器への供給中はこの開閉弁１４を閉じ
るようにすることもできる。この場合、補助容器
１１と原料タンク１との間の開閉弁１４を第１自
動弁とし、かつ自動弁７を第２自動弁として、第
２自動弁７を開く前すなわち原料ガスを反応容器
に送出する前、第１自動弁１４が開かれており、
また、第２自動弁７を開いた後には直後に又は一
定時間後に第１自動弁１４を閉じるようにするの
がよい。この場合、第１自動弁１４の閉成を第２
自動弁７の開放直後又は一定時間後としたのは、
配管抵抗や原料タンク１の気相分の容積により弁
の開閉が液相から気相変化の状態に影響するまで
時間遅れがあるため、開閉のタイミングをずらし
て安定な流量制御を行なうことによる。 Furthermore, FIG. 3 shows another modification. When supplying a large flow rate of raw material gas from the raw material tank 1 to the reaction vessel, the amount of circulation through the auxiliary vessel 11 becomes a burden on the side supplying the reaction vessel, reducing the amount of heat transfer. There is a possibility that sufficient data may not be sent. Therefore, as shown in FIG. 3, an on-off valve 14 may be interposed in the pipe 13b to the auxiliary container 11, and the on-off valve 14 may be closed during supply to the reaction container. In this case, the on-off valve 14 between the auxiliary container 11 and the raw material tank 1 is used as the first automatic valve, and the automatic valve 7 is used as the second automatic valve. Before sending out, the first automatic valve 14 is opened,
Further, it is preferable to close the first automatic valve 14 immediately after opening the second automatic valve 7 or after a certain period of time. In this case, the closing of the first automatic valve 14 is
Immediately after opening the automatic valve 7 or after a certain period of time is as follows.
Because there is a time delay until the opening and closing of the valve affects the state of change from the liquid phase to the gas phase due to piping resistance and the volume of the gas phase in the raw material tank 1, stable flow rate control is performed by shifting the timing of opening and closing.
更に、開閉弁１４を自動弁とし、この自動弁を
流量制御装置に連動させ、流量制御８から送出さ
れる流量が一定量より少ないとき自動弁１４を開
き、多いとき自動弁１４を閉じ、または上記流量
が一定量より少ないとき上記自動弁１４をあけ、
多くなつて一定時間後自動弁１４を閉じるように
してもよい。この流量制御装置８と自動弁１４と
の連動は、流量制量をワイドレンジで変化させる
とき、補助容器１１を含む循環ルートの使用の是
非を制御流量のしきい値を設けて管理した方が好
ましいことによる。 Furthermore, the on-off valve 14 is an automatic valve, and this automatic valve is linked to a flow rate control device, so that when the flow rate sent out from the flow rate control 8 is less than a certain amount, the automatic valve 14 is opened, and when it is higher, the automatic valve 14 is closed. When the flow rate is less than a certain amount, the automatic valve 14 is opened;
The automatic valve 14 may be closed after a certain period of time when the number of times increases. The interlock between the flow rate control device 8 and the automatic valve 14 is such that when changing the flow rate control over a wide range, it is better to manage the use of the circulation route including the auxiliary container 11 by setting a threshold value for the control flow rate. Depends on what's desirable.
第４図ないし第６図は、今までの説明と異なり
補助容器を備えず原料タンク１に冷却部品を直接
備えた例を示す。すなわち、第４図は原料タンク
１の上蓋１ａ又は上部に冷却フイン１５を備えた
場合を示し、第５図は、原料タンク１の上蓋１ａ
に空冷又は液冷用の配管１６を備えた場合を示
し、更に第６図は原料タンク１の上部空間４に空
冷又は液冷用の配管１７を備えた場合を示したも
のである。これら直接冷却の構成としては他にも
種々の変形例がある。 4 to 6 show an example in which a cooling part is directly provided in the raw material tank 1 without providing an auxiliary container, unlike the previous explanation. That is, FIG. 4 shows the case where the cooling fins 15 are provided on the upper lid 1a or the upper part of the raw material tank 1, and FIG.
FIG. 6 shows a case where the upper space 4 of the raw material tank 1 is provided with a pipe 17 for air cooling or liquid cooling. There are various other variations of these direct cooling configurations.
＜発明の効果＞
以上説明したように本発明によれば、原料タン
ク自体、又は上部空間の冷却更には冷却循環ルー
トの形成により、温度分布を生じて気液相の交換
を活発にでき沸騰を常に生じさせたことにより、
安定した沸騰突沸の防止、安定した流量制御を行
なうことができる。<Effects of the Invention> As explained above, according to the present invention, by cooling the raw material tank itself or the upper space, and by forming a cooling circulation route, a temperature distribution is generated to actively exchange the gas-liquid phase, and boiling can be prevented. By constantly causing
Stable prevention of boiling and bumping and stable flow control can be performed.
第１図ないし第６図は本発明の実施例で、第１
図は一例の構成図、第２図は他の例の構成図、第
３図はその他の例の構成図、第４図は冷却フイン
を備えた構成図、第５図及び第６図は冷却配管を
備えた構成図、第７図は従来の構成図である。
図面中、１は原料タンク、３はヒータ、４は上
部空間、５は配管、６は開閉弁、７は自動弁、８
は流量制御装置、１１は補助容器、１３ａ，１３
ｂは配管、１４は開閉弁、１５は冷却フイン、１
６，１７は冷却配管である。
1 to 6 show embodiments of the present invention;
The figure is a configuration diagram of one example, Figure 2 is a configuration diagram of another example, Figure 3 is a configuration diagram of another example, Figure 4 is a configuration diagram with cooling fins, and Figures 5 and 6 are cooling A configuration diagram including piping, FIG. 7 is a conventional configuration diagram. In the drawing, 1 is a raw material tank, 3 is a heater, 4 is an upper space, 5 is piping, 6 is an on-off valve, 7 is an automatic valve, 8
11 is a flow rate control device, 11 is an auxiliary container, 13a, 13
b is a pipe, 14 is an on-off valve, 15 is a cooling fin, 1
6 and 17 are cooling pipes.
Claims (1)
下部に有し上部にこの原料液が気化した原料ガス
を収容する原料タンクと、この原料液の蒸気圧が
大気以上になるまでこの原料液を加熱する手段
と、蒸気原料タンク内で気化された原料ガスを反
応容器へ導く配管と、この配管に介装された開閉
及び流量制御を行なう装置とを備える原料供給装
置において、上記原料タンク内で気化された原料
ガスを冷却して上記原料タンクにて熱対流を生じ
る機構を上記原料タンクに備えたことを特徴とす
る原料供給装置。 ２ 上記特許請求の範囲第１項記載の原料供給装
置において、上記機構は、原料タンクと連通しか
つ冷却される補助容器にて形成されることを特徴
とする原料供給装置。 ３ 上記特許請求の範囲第２項記載の原料供給装
置において、上記補助容器は上記原料供給装置に
おいて、上記補助容器は上記原料タンクの上部空
間と連通することを特徴とする原料供給装置。 ４ 上記特許請求の範囲第２項記載の原料供給装
置において、上記補助容器の下部と原料タンク内
の原料液中との間に配管が施され、かつ上記補助
容器の下部以外の部分と上記原料タンクの上部空
間とが連通されることを特徴とする原料供給装
置。 ５ 上記特許請求の範囲第３項又は第４項に記載
の原料供給装置において、上記補助容器と上記原
料タンクの上部空間とは開閉弁を介して連通され
ることを特徴とする原料供給装置。 ６ 上記特許請求の範囲第１項記載の原料供給装
置において、原料タンクの上蓋又は上部に冷却機
構を取付けたことを特徴とする原料供給装置。 ７ 上記特許請求の範囲第１項記載の原料供給装
置において原料タンク内部の上部空間に冷却機構
を備えたことを特徴とする原料供給装置。[Claims] 1. A raw material tank having a raw material liquid reacting with oxygen or moisture in the atmosphere in the lower part and containing a raw material gas obtained by vaporizing this raw material liquid in the upper part, and a raw material tank having a vapor pressure higher than that of the atmosphere. In a raw material supply device comprising: a means for heating the raw material liquid until the raw material liquid reaches A raw material supply device, characterized in that the raw material tank is equipped with a mechanism that cools the raw material gas vaporized in the raw material tank and generates thermal convection in the raw material tank. 2. The raw material supply device according to claim 1, wherein the mechanism is formed of an auxiliary container that communicates with the raw material tank and is cooled. 3. The raw material supply device according to claim 2, wherein the auxiliary container is in communication with the upper space of the raw material tank. 4. In the raw material supply device according to claim 2, piping is provided between the lower part of the auxiliary container and the raw material liquid in the raw material tank, and the part other than the lower part of the auxiliary container and the raw material A raw material supply device characterized by communicating with an upper space of a tank. 5. The raw material supply device according to claim 3 or 4, wherein the auxiliary container and the upper space of the raw material tank are communicated with each other via an on-off valve. 6. The raw material supply device according to claim 1, characterized in that a cooling mechanism is attached to the upper lid or upper part of the raw material tank. 7. A raw material supply device according to claim 1, characterized in that a cooling mechanism is provided in the upper space inside the raw material tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4467685A JPS61205629A (en) | 1985-03-08 | 1985-03-08 | Raw material feeder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP4467685A JPS61205629A (en) | 1985-03-08 | 1985-03-08 | Raw material feeder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61205629A JPS61205629A (en) | 1986-09-11 |
| JPH0251852B2 true JPH0251852B2 (en) | 1990-11-08 |
Family
ID=12698043
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP4467685A Granted JPS61205629A (en) | 1985-03-08 | 1985-03-08 | Raw material feeder |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61205629A (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP7229792B2 (en) | 2018-02-05 | 2023-02-28 | 株式会社フジクラ | Method for producing porous glass particulates, device for producing porous glass particulates, and method for producing glass base material |
| US11393703B2 (en) * | 2018-06-18 | 2022-07-19 | Applied Materials, Inc. | Apparatus and method for controlling a flow process material to a deposition chamber |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58135146A (en) * | 1982-02-03 | 1983-08-11 | Fujikura Ltd | Preparation of base material for optical fiber |
| JPS605029A (en) * | 1983-06-21 | 1985-01-11 | Agency Of Ind Science & Technol | Method for feeding vaporized raw material for producing optical glass |
-
1985
- 1985-03-08 JP JP4467685A patent/JPS61205629A/en active Granted
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58135146A (en) * | 1982-02-03 | 1983-08-11 | Fujikura Ltd | Preparation of base material for optical fiber |
| JPS605029A (en) * | 1983-06-21 | 1985-01-11 | Agency Of Ind Science & Technol | Method for feeding vaporized raw material for producing optical glass |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61205629A (en) | 1986-09-11 |
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