JPH1057798A - Liquid material supply device and material supply method - Google Patents

Abstract

PROBLEM TO BE SOLVED: To stable supply a liquid fuel to a carburetor over a long period by providing a vessel for supplying the liquid fuel to the carburetor and a standby vessel in standby state for supply. SOLUTION: A gas supply pipe 111, two vessels 150, 250 in which the liquid fuel is enclosed, and a material supply pipe 127 for supply in the liquid fuel to the carburetor 91 are provided. In the 1st vessel 150 to which a pressurized gas is supplied through a 1st gas line connecting pipe 113, a stop valve is provided at the midst of a 1st gas introducing pipe 151 as a 1st gas introducing valve 161 and a stop valve is provided at the midst of a 1st discharge pipe 153 as a 1st discharge valve 163, and also in the 2nd vessel 250 to which the pressurized gas is supplied through a 2nd gas connecting pipe 213, a stop valve is provided on a 2nd gas introducing pipe 251 as a 2nd gas introducing valve 261 and a stop valve is provided in a 2nd discharge pipe 253 as a 2nd discharge valve 263. As a result, the stable supply of the liquid fuel to the carburetor 91 is continued.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus and a method for stably supplying a glass raw material solution used for producing optical fibers or synthetic quartz glass to a vaporizer such as a vaporizer.

[0002]

2. Description of the Related Art Generally, a vaporizer such as a vaporizer is used as a device for supplying a high-purity raw material gas to a burner. The vaporizer is a gas control system that supplies a vaporized source gas to a reaction system. That is,
The liquid material is vaporized at an atmospheric temperature equal to or higher than the boiling point, and the mass flow controller controls the flow rate stably and accurately. This vaporizer basically includes a gas control unit and a thermostat.

In general, a liquid material of a silicon compound such as silicon tetrachloride is used as a glass raw material for optical fibers and quartz glass. This liquid material is supplied to a vaporizer such as a vaporizer by pressure-feeding from a container such as a cylinder with nitrogen gas or the like. Specifically, the pressure of the liquid material to the vaporizer is regulated by nitrogen or an inert gas (including a gas having a low reactivity with the liquid material as well as the inert gas in the periodic table; hereinafter, referred to as a pressurized gas). By constantly applying a constant pressure (about 1 to ² kg / cm ² ) to the inside of the container. The liquid material is supplied to the vaporizer by this pressurization, and the gas is injected into the container by the amount of the reduced liquid material.

As shown in FIG. 15, such a liquid material supply device includes a pressurized gas line 10, a material supply line 20, a container 50, and the like. The pressurized gas line 10 is
Gas supply pipe 11 for sending pressurized gas to be injected into
And a gas line connection pipe 13 having a gas line connection 15 at the end, which is a connection to the gas introduction pipe 51. The material supply line 20 is connected to a discharge pipe 53 fixed to the container 50 and a material line connection pipe 23 having a material line connection 25 as a connection to the discharge pipe 53 at the end and a vaporizer 91. It is formed by the material supply pipe 27.

[0005] The gas supply pipe 11 has an open / close valve as a gas feed valve 41 at an end thereof, and the gas line connection pipe 13 is connected through the gas feed valve 41. A bypass pipe 29 branches off from the gas line connection pipe 13. The bypass pipe 29 has an opening / closing valve as a line short-circuit valve 43 in the middle thereof, and the other end of the bypass pipe 29 is connected to a material line connection pipe.
Connected to 23. An opening / closing valve as a material receiving valve 45 is provided in the middle of the material line connecting pipe 23.

The material line connecting pipe 23 is provided with a supply valve 47.
Is connected to the material supply pipe 27, a bypass pipe 29 is connected between the material receiving valve 45 and the material line fitting 25,
The exhaust pipe 31 branches off from between the material receiving valve 45 and the supply valve 47, and is connected to a harm removal tower or the like via the exhaust pipe 31 having an open / close valve as the exhaust valve 49. The material supply pipe 27 has an opening / closing valve as a supply valve 47 at one end and connects the other end to the vaporizer 91.

Further, an opening / closing valve as a gas introduction valve 61 is provided on the gas introduction pipe 51 fixed to the container 50. The discharge pipe 53 is provided with a discharge valve 63 in the middle of an open / close valve. When the container 50 is removed, the inside of the container 50 is sealed by closing the gas introduction valve 61 and the discharge valve 63.
In this way, after closing the gas introduction valve 61 and the discharge valve 63, the gas line connection 15 and the material line connection 25 separate the gas line connection pipe 13 and the material line connection pipe 23 from each other.

Then, the gas line connection pipe 13 and the material line connection pipe are connected by the gas line connection 15 and the material line connection 25.
After connecting to 23 and attaching a new container 50, first, the gas introduction valve 61 and the discharge valve 63 of the container main body are opened. Further, the line short-circuit valve 43 of the bypass pipe 29 and the material supply pipe
27 with the supply valve 47 closed, the gas feed valve 41 of the gas supply pipe 11 and the material receiving valve 45 of the material line connection pipe 23.
Is opened, and the exhaust valve 49 of the exhaust pipe 31 is also opened.

Therefore, when the gas feed valve 41 and the gas introduction valve 61 are open, pressurized gas such as nitrogen gas is pressed into the container body, and the liquid material in the container body is discharged through the discharge valve 63. It can be extruded into the material supply line 20. At this time, since the supply valve 47 of the material supply pipe 27 is closed and the exhaust valve 49 of the exhaust pipe 31 is open, the pressurized gas or air existing inside the material line connection pipe 23 is , Sent to the abatement tower via the exhaust pipe 31,
Hazardous components are removed and released to the atmosphere.

Thereafter, the exhaust valve 49 is closed and the supply valve is closed.
When 47 is opened, the liquid material is vaporized 91 through the material supply pipe 27.
Can be sent to When the liquid material is pumped to the vaporizer 91, usually, a gas having low reactivity with the liquid material, that is, an inert gas such as a nitrogen gas is used as the pressurized gas. This pressurized gas is made to have a constant pressure (about 1 to ² kg / cm ² ) through a regulator, and this constant pressure is constantly applied to the inside of the container 50. A system for injecting a pressurized gas into the inside of the device is used.

When replacing the container 50, the container 50 is removed from the joints 15, 25 of the pressurized gas line 10 and the material supply line 20, as described above. At this time, air flows into a part of the material supply line 20, and if the liquid material extruded from the container 50 remains at the portion of the material supply line 20 into which the air has flowed, it causes corrosion. Therefore, it is necessary to remove the liquid material remaining in the material line connection pipe 23 before removing the container 50. For this reason, a bypass pipe is connected to the material line connection pipe 23 in the material supply line 20.
Continue to flow nitrogen gas or inert gas from 29. Also,
The atmosphere mixed into each line after the container 50 is replaced
It also needs to be removed because it contaminates 50 or lines. Generally, such an operation is called purging. The gas used at that time is called a purge gas. The pressurized gas can be used as the purge gas.

Therefore, when removing the container 50, normally, the gas introduction valve 61 and the discharge valve 63 are closed, and the supply valve 47 for sending the liquid material to the vaporizer 91.
Is closed, and the exhaust valve 49 and the line short-circuit valve 43 are opened to perform purging using the pressurized gas as a purge gas. In this purge, the pressurized gas is sent to the material line connection pipe 23 through the bypass pipe 29, and the material line connection pipe 23
The liquid material remaining in the exhaust pipe is discharged to the abatement tower via the exhaust pipe 31.

The conventional purging is performed by using a pressurized gas line.
The gas introduction valve 61 provided in the gas introduction pipe 51 which is a supply port to the container 50 of 10 and the discharge valve 63 provided in the discharge pipe 53 which is a supply port of the liquid material from the container 50 are closed, and further vaporization is performed. The supply valve 47 provided in the material supply line 20 to the vessel 91 is closed, nitrogen gas or an inert gas is kept flowing in each line, and highly corrosive liquid material is removed via the exhaust pipe 31. Was.

[0014]

However, when the liquid material is supplied to the vaporizer by the conventional method, there are the following problems. First, it was not possible to supply the source gas continuously for a long period of time. That is, when the container needs to be replaced, there is a problem that the liquid material cannot be supplied temporarily.

In addition, since it is necessary to perform purging when exchanging the container, it takes a long time to exchange the container. Therefore, the supply of the liquid material to the vaporizer is interrupted for a long time. For this reason, there has been a defect that stable supply of the liquid material cannot be performed by replacing the container. That is, when the temporarily stopped liquid material is supplied to the vaporizer after the replacement of the container, when the temperature of the supplied liquid material is low, several tens of times or more of the normal supply amount is supplied to the vaporization tank at a stretch. You. Therefore, there has been a problem that the temperature of the vaporizer decreases and the amount of generated gas decreases. And as a result,
The amount of gas supplied to the reaction system fluctuates, and stable production in the reaction system cannot be performed. For this reason, when producing synthetic quartz glass, there was a problem that inhomogeneity called striae occurred.

If the purging cannot be performed completely, the following problem occurs. When a corrosive material such as silicon tetrachloride is used for the liquid material, the metal that touched such a liquid material
Even a corrosion-resistant material such as SUS316L is corroded by an acid such as hydrochloric acid generated by a reaction between moisture in the air and a liquid material. In addition, a siloxane-based compound is also generated by a reaction with moisture in the air. Such reaction products and particulate metal impurities cause clogging and mass flow errors inside the mass flow controller connected to the vaporizer. In addition, it may cause internal leakage of the valve and cause a problem.

An object of the present invention is to solve the above-mentioned problem caused by container replacement and to provide an apparatus for stably supplying a liquid material to a vaporizer for a long period of time. That is, since it is unavoidable to supply the liquid material using a container such as a cylinder having a finite volume, the present inventors have proposed a method of pumping the liquid material to the vaporizer and the operation of replacing the container. We focused on the interruption of the supply of the liquid material to the vaporizer and the suppression of fluctuations in the supply amount of the raw material due to the restart of the supply of the liquid material after the replacement of the container. As a result, considering the resumption of the supply of the liquid material after the replacement of the container, the provision of a container that supplies the liquid material to the vaporizer and a standby container that is waiting for the supply are required for a long period of time. It has been found that this is the most effective method for providing stable supply.

As described above, in the conventional purging, the purging gas is continuously supplied, but complete purging is impossible and it takes time. Therefore, the present inventors have found a purge that can be completely purged in a short time, and adopted the purge when the liquid material is supplied to the vaporizer.

[0019]

According to the present invention, a gas supply pipe having a bifurcated tip having two open / close valves at each of two ends and an open / close valve at each of two branched ends is provided. And the line from these two on-off valves together
A material supply pipe for supplying a liquid material to two vaporizers, two gas line connection pipes for connecting an end of the gas supply pipe and a gas introduction pipe of a container, and an end of the material supply pipe. Each gas line connection pipe having two material line connection pipes for connecting a discharge pipe of a container, and two bypass pipes connecting the gas supply pipe and the material line connection pipe; Has one end connected to the on-off valve provided at the end of the gas supply pipe and the other end has a joint for connecting a gas introduction pipe of a container, and each material line connection pipe has one end connected to the material supply pipe. The other end is connected to the gas supply pipe, and the other end is connected to the material line connection pipe. The other end is connected to the gas supply pipe, and the other end is connected to the material line connection pipe. Each bypass pipe is provided with an open / close valve in the middle, and the container is opened. A gas inlet pipe provided with a valve and a discharge pipe provided with an opening / closing valve, wherein two of the containers each containing a liquid material are detachably attached to each of the joints, and pressurized gas from the gas supply pipe is provided. The liquid material supply device supplies the liquid material of each container to the vaporizer via the material supply pipe while feeding the liquid material to each container.

As described above, two containers enclosing the liquid material are provided, and the tip of the gas supply pipe is branched so that pressurized gas can be injected into each container. Also, the material line connecting pipes respectively connected to the discharge pipes of the two containers are connected to the ends of the two branched material supply pipes.
The two ends were connected to one vaporizer. That is, in addition to having two containers, the pressurized gas line and the material supply line are divided into two systems.

Therefore, when the liquid material in one container is exhausted, the liquid material can be supplied from the other container to the vaporizer, and the supply of the liquid material to the vaporizer can be continued without interruption. Further, it is preferable to provide an abatement apparatus having a vacuum pump, and connect the abatement apparatus to each material line connection pipe by an exhaust pipe having an open / close valve.

As described above, if the abatement apparatus having the vacuum pump is connected to the material line connection pipe, it is possible to perform purging for reducing the pressure of the material line connection pipe and the like. Further, the present invention provides a gas supply pipe having a front end branched into two and having an open / close valve at each of two ends, or two gas supply pipes each having an open / close valve at each end, and the gas supply pipe. A connection pipe having an opening / closing valve in the middle, a gas introduction pipe having an opening / closing valve, and a container filled with a liquid material having a discharge pipe having an opening / closing valve, and two branched pipes. A material supply pipe for supplying a liquid material to one vaporizer by combining lines from the two on-off valves with an on-off valve at each end; an end of the gas supply pipe and the gas in the container; Two gas line connection pipes connecting the introduction pipe, two material line connection pipes connecting the end of the material supply pipe and the discharge pipe of the container, and two bypass pipes; And two connecting pipes, wherein each of the gas line connecting pipes is One end is connected to the on-off valve provided at the end of the gas supply pipe, and the other end has a joint for connecting the gas introduction pipe of the container, and each material line connection pipe is connected to the material supply pipe. One end is connected to the open / close valve provided at the end of the container, and the other end has a joint for connecting the discharge pipe of the container. And the material line connection pipes, each of the connection pipes is provided with an open / close valve in the middle to connect the gas introduction pipe and the discharge pipe in each of the containers, and an abatement apparatus having a vacuum pump. An exhaust pipe having an opening / closing valve in the middle and connecting the abatement apparatus to each of the material line connection pipes or each of the gas line connection pipes; and Liquid material through the material supply pipe Sometimes the liquid material supply device for supplying to the evaporator by.

As described above, according to the liquid material supply apparatus having the container having the connection pipe for connecting the gas introduction pipe and the discharge pipe, the discharge pipe can be connected using the pipe connection valve provided on the connection pipe. A purge line can be formed through the joint. Therefore, the liquid material and the material gas can be reliably removed and purged from the vicinity of the joint separated when the container is removed in a short time.

Then, an abatement apparatus having a vacuum pump is
It has a base, each exhaust pipe connecting each abatement device to any gas line connection pipe or material line connection pipe, and an auxiliary exhaust pipe connecting the both exhaust pipes with an open / close valve in the middle. It is preferable to use a liquid material supply device. As described above, if the liquid material supply device has two abatement devices, the abatement devices can be switched to perform purging even when the performance of the abatement device is reduced. Therefore, it is possible to reliably replace the empty container in a short time.

Further, the method according to the present invention includes two containers, each of which has a gas introduction pipe having an opening / closing valve and a discharge pipe having an opening / closing valve and in which a liquid material is sealed, Two gas line connection pipes each having a joint for connecting the gas introduction pipes and connected to a gas supply pipe by an open / close valve, and an end portion for connecting the discharge pipes of the containers. Two material line connecting pipes each having a joint and each other end connected to the material supply pipe by an open / close valve, and an intermediate open / close valve, the gas supply pipe and the material line connect pipes. And a decontamination device connected to the material line connection pipe by an exhaust pipe having an open / close valve and having a vacuum pump. In front of liquid material When supplying the vaporizer with the pressurized gas from the gas supply pipe, when the liquid material in one of the containers is reduced, supplying the liquid material from the other container to the vaporizer by a valve operation, The on-off valve provided on the discharge pipe of the container having a reduced amount of liquid material and the on-off valve connecting the material line connection pipe connecting the discharge pipe to the material supply pipe are closed, and purge gas is supplied through the bypass pipe. The outlet of the discharge pipe is put in a pressurized state, and the vacuum pump of the abatement apparatus is further purged through the exhaust pipe so that the outlet of the discharge pipe is depressurized. After the purging, the container is replaced. After the replacement, purging under the pressurized state and the depressurized state is performed, and when the inside of the discharge pipe and the material line connection pipe is in the depressurized state, the open / close valve of the discharge pipe It is to supply a method for liquid material to be filled with liquid material inside the material line connection pipe open.

As described above, since the pressurized state and the depressurized state are repeated when the container is replaced, the liquid material remaining inside the material line connection pipe or the like is evaporated under reduced pressure and sucked into the abatement apparatus. As a result, the gas can be pushed out to the abatement apparatus, and the purge can be reliably performed in a short time. Furthermore, since the purging is performed even after the container replacement and the liquid material is injected into the material line connection pipe in a reduced pressure state and filled, the container is switched immediately when the liquid material in another container becomes low. And a liquid material containing no air or purge gas can be sent to the vaporizer.

According to another aspect of the present invention, there are provided two containers having a gas introduction pipe having an opening / closing valve and a discharge pipe having an opening / closing valve and enclosing a liquid material, and each of the containers at the end. Two gas line connection pipes each having a joint for connecting the gas introduction pipes and connected to a gas supply pipe by an open / close valve, and an end portion for connecting the discharge pipes of the containers. Two material line connecting pipes each having a joint and each other end connected to the material supply pipe by an open / close valve, and the gas introducing pipe and the discharge pipe in each container having an open / close valve in the middle. A connecting pipe for connecting
A gas elimination device connected to the gas line connection pipe or the material line connection pipe by an exhaust pipe provided with an on-off valve and having a vacuum pump; and When supplying the vaporizer with the pressurized gas from the supply pipe, when the liquid material in one of the containers is reduced, supplying the liquid material from the other container to the vaporizer by a valve operation,
The open / close valve provided on the discharge pipe of the container with a reduced amount of liquid material and the open / close valve connecting the material line connection pipe connecting the discharge pipe to the material supply pipe were closed and provided on the connection pipe. Opening the open / close valve to make the gas introduction pipe and the discharge pipe communicate with each other, the inside of the gas line connection pipe and the inside of the gas introduction pipe, and the inside of the discharge pipe and the inside of the material line connection pipe. Is performed by repeatedly performing a pressurized state by a purge gas and a pressure-reduced state by the vacuum pump of the abatement apparatus, exchanging the container after the purge, and purging by a pressurized state and a depressurized state after the exchange. Closing the open / close valve of the connection pipe and opening the open / close valve of the discharge pipe when the insides of the discharge pipe and the material line connection pipe are in a decompressed state; Sometimes the interior of the in-connection tube and the supply method of the liquid material be kept full of liquid material.

As described above, in the liquid material supply apparatus using the container having the connecting pipe for connecting the gas introducing pipe and the discharge pipe, the connecting pipe connects the inside of the gas introducing pipe to the inside of the discharging pipe. By performing the purge, the purge gas by the decompression and the pressurization can be reliably flowed to the joint. Therefore, the purge can be reliably performed in a short time. Furthermore, since the purging is performed even after the container replacement and the liquid material is injected into the material line connection pipe in a reduced pressure state and filled, the container is switched immediately when the liquid material in another container becomes low. And a liquid material containing no air or purge gas can be sent to the vaporizer.

Then, two containers, each having a gas introduction pipe having an opening / closing valve and a discharge pipe having an opening / closing valve, filled with a liquid material, and the gas introduction pipes of the respective containers are connected to the ends. Two gas line connecting pipes each connected to a gas supply pipe by an open / close valve, and a joint for connecting the discharge pipe of each container at an end portion, and each other Two ends are connected to the material supply pipe by open / close valves, respectively, and two bypasses each having an open / close valve in the middle to connect the gas supply pipe and each material line connect pipe. A pipe, a connecting pipe for connecting the gas introduction pipe and the discharge pipe in each container with an opening / closing valve in the middle, and an exhaust pipe with an opening / closing valve for the gas line connection pipe or the material line connection pipe. Connected and An abatement device equipped with an empty pump, and a liquid material supply device having a liquid material sealed in the container is supplied to a vaporizer by a pressurized gas from the gas supply pipe. When the amount decreases, the liquid material from the other container is supplied to the vaporizer by a valve operation, and the opening / closing valve provided in the gas introduction pipe of the container with the reduced amount of liquid material and the discharge pipe of the container The on / off valve connecting the material line connection pipe connected to the material supply pipe is closed, and the on / off valve of the bypass pipe is opened to remove the liquid material inside the material line connection pipe and the inside of the discharge pipe. Returning to the container, the gas introduction pipe and the discharge pipe are communicated by closing the open / close valve provided on the discharge pipe and opening the open / close valve provided on the connection pipe. Then, the inside of the gas line connection pipe and the inside of the gas introduction pipe, and the inside of the discharge pipe and the inside of the material line connection pipe are pressurized by a purge gas and depressurized by the vacuum pump of the abatement apparatus. Performing a purge that repeats the state, replacing the container after the purge, performing a purge in a pressurized state and a depressurized state even after the exchange, when the inside of the discharge pipe and the material line connection pipe is in a depressurized state There may be a method of supplying a liquid material in which the opening and closing valve of the discharge pipe is opened to fill the inside of the material line connection pipe with the liquid material.

As described above, if the purge gas is caused to flow from the bypass pipe to the material line connection pipe and the liquid material remaining inside the material line connection pipe and the discharge pipe is returned to the container, the performance of the abatement apparatus is reduced. And the amount of liquid material remaining inside the material line connection pipe or the like is small, so that a more reliable purge can be performed in a shorter time. And since the purge is performed even after the container replacement, and the liquid material is injected and filled into the material line connection pipe in a reduced pressure state,
When the liquid material in another container becomes low, the container can be switched immediately, and the liquid material containing no air or purge gas can be sent to the vaporizer.

[0031]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS A first embodiment of a liquid material supply apparatus according to the present invention uses an inert gas from a pressurized gas supply source as shown in FIG.
73, a gas supply pipe 111 for receiving the liquid material and two containers 150 and 250 filled with the liquid material.
And a material supply pipe 127 for sending the liquid material from the containers 150 and 250 to the vaporizer 91.

The gas supply pipe 111 has one end connected to a pressurized gas supply source (not shown). And
As shown in FIG. 1, the other end of the gas supply pipe 111 has a tip branched into two. Further, the gas supply pipe 111
An opening / closing valve is provided as a first gas feed valve 141 at the first end, and an opening / closing valve is also provided as a second gas feed valve 241 at the second end.

Then, a first gas line connection pipe 113 is connected to a first end of the gas supply pipe 111 via a first gas feed valve 141. This first gas line connection pipe 113 is
A first gas line joint 115, which is a joint for connecting to a first gas introduction pipe 151, which is a gas introduction pipe of a container serving as the first container 150, is provided at the end. Also, gas supply pipe 1
Similarly, a second gas line connection pipe 213 is connected to the second end of the eleventh via a second gas feed valve 241. This second
At the end of the gas line connection pipe 213, a second container,
A second gas line joint 215 is provided as a joint for connecting to a second gas introduction pipe 251 which is a gas introduction pipe of the container 250.

The first container 150 to which the pressurized gas is supplied via the first gas line connection pipe 113 and the second container 250 to which the pressurized gas is supplied via the second gas line connection pipe 213 The first container 150 and the second container 250 both have a liquid material sealed therein. The first container 150 includes an opening / closing valve as a first gas introduction valve 161 in the middle of the first gas introduction pipe 151, and an opening / closing valve as a first discharge valve 163 in the middle of the first discharge pipe 153. Then, the first gas introduction pipe 151 and the first discharge pipe 1
The first connection pipe 155 has a first connection pipe 155 for connecting the first connection pipe 53 with the first connection pipe 155. Similarly, in the second container 250, an opening / closing valve is connected to the second gas introduction pipe 251 by the second gas introduction valve 261.
The second discharge pipe 253 is provided with an open / close valve as the second discharge valve 263. Further, a second connection pipe 255 for connecting the second gas introduction pipe 251 and the second discharge pipe 253 is provided, and the second connection pipe 255 is also provided with an open / close valve as a second pipe connection valve 265.

The connecting pipes 155 and 255 are connected to gas introduction pipes 151 and 251.
And the gas line fittings 115, 215 side than the gas introduction valves 161, 261 at the discharge pipes 163, 153 at the discharge pipes 153, 253.
263 is connected to the material line joint 125, 225 side. Further, material line connection pipes 123, 223 connecting the containers 150, 250 and the material supply pipe 127 are provided. The first material line connection pipe 123 connected to the first discharge pipe 153 of the first container 150 has a first material line joint 125 at an end, and an opening / closing valve in the middle of the first material receiving valve 145.
The first material line connection pipe 123 provided as the first material line. The other end of the first material line connection pipe 123 is connected to a first end of the material supply pipe 127 via an opening / closing valve serving as a first supply valve 147.

Similarly, the second material line connecting pipe 223 for connecting to the second discharge pipe 253 is connected to the second material line coupling 225.
At the end and an opening / closing valve in the middle as a second material receiving valve 245 as a second material line connection pipe 223. The other end of the second material line connection pipe 223 is connected to the material supply pipe 1 through an opening / closing valve serving as a second supply valve 247.
27 to be connected to the second end.

The material supply pipe 127 is provided with a first supply valve 147.
And a second end provided with a second supply valve 247.
The pipes from the ends are joined and connected to the vaporizer 91 so that the liquid material from the first container 150 and the liquid material from the second container 250 can be sent to the vaporizer 91. Further, the liquid material supply device is provided with a first bypass pipe 129 connecting the gas supply pipe 111 and the first material line connection pipe 123, and an opening / closing valve is provided in the middle of the first bypass pipe 129. This is provided as a line short-circuit valve 143. Similarly,
A second bypass pipe 229 for connecting the gas supply pipe 111 and the second material line connection pipe 223 is also provided, and an on-off valve is provided as a second line short-circuit valve 243 in the middle of the second bypass pipe 229.

The first gas line connecting pipe 113 has a first gas line connecting pipe.
An abatement apparatus 135 equipped with a vacuum pump is connected via an exhaust pipe 131, and a first exhaust valve 149 is provided in the middle of the first exhaust pipe 131.
Open / close valve. Similarly, the above-mentioned abatement apparatus 135 is connected to the second gas line connection pipe 213 via a second exhaust pipe 231, and an opening / closing valve as a second exhaust valve 249 is provided in the middle of the second exhaust pipe 231. Is provided.

A pipe as a pump exhaust line from the gas supply pipe 111 to the abatement apparatus 135 is further provided. The pipe as the pump exhaust line includes an open / close valve as a check valve 76 and a pump exhaust valve 78, and , A flow meter 83 is provided. This pump exhaust line keeps sending a small amount of inert gas from the gas supply pipe 111 to the abatement apparatus 135 so that moisture and oxygen can be removed by a vacuum pump or the like of the abatement apparatus 135. Further, a pressure switch 81 is provided in the gas supply pipe 111, and when a pressure abnormality occurs, the gas feed valves 141 and 142 are closed. Further, the first gas line connection pipe 11
Pressure gauges 85 and 86 are provided in the third and second gas line connection pipes 213 to detect the pressure of the pressurized gas sent to the first container 150 and the second container 250. A pressure gauge 87 is also provided on the exhaust pipe so that the operating state of the vacuum pump provided on the abatement apparatus 135 can be detected.

When a liquid material is supplied to the vaporizer 91 by the liquid material supply device, first, as shown in FIG. An inert gas as a pressurized gas is sent to the first container 150, and the first discharge valve 163, the first material receiving valve 145, and the first supply valve 147 are opened to open the first container 150.
Is sent to the vaporizer 91.

The opening and closing control of the first gas feed valve 141 is controlled by detecting the pressure in the first container 150 by the first pressure gauge 85 provided in the first gas line connection pipe 113. That is, when the pressure in the first container 150 decreases, the first gas feed valve 141 is opened to increase the pressure in the first container 150 so as to return to a constant pressure, and the pressure in the first container 150 is always kept at a predetermined value. It is controlled to be within the range.

When the liquid material from the first container 150 is being supplied to the vaporizer 91, the pressure is also applied to the inside of the second container 250. That is, the inside of the second discharge pipe 253 and the second material line connection pipe 223 is filled with the liquid material,
As soon as the second supply valve 247 is opened, the liquid material from the second container 250 can be supplied to the vaporizer 91 so that the second container 250
Is in a standby state.

When the amount of the liquid material in the first container 150 is reduced, as shown in FIG.
Opening 241 to send an inert gas, which is a pressurized gas from the gas supply pipe 111, to the second container 250, and opening the second supply valve 247 to supply the liquid material from the second container 250 to the vaporizer 91 It is. At this time, the second gas feed valve 241 detects the pressure in the second container 250 by the second pressure gauge 85 provided in the second gas line connection pipe 213, and performs the opening and closing operation intermittently. This is to stabilize the pressure in the container 250 within a certain range.

Further, by replacing the first container 150 while the liquid material from the second container 250 is being supplied to the vaporizer 91, when the liquid material in the second container 250 runs out, the first container 150 is replaced. To prevent the supply of the material to the vaporizer 91 from being interrupted. As described above, in the present embodiment, in order to stably supply the liquefied material to the vaporizer 91 over a long period of time, the conventional liquid material supply device is improved, two containers are used, and the pressurized gas line and The material supply line is divided into two systems. When one container supplies the liquid material to the vaporizer 91, the other container is a standby container in which the supply of the liquid material is waited. However, the state of the standby container is a standby state in a usable state, and the usable state is a state in which purging after replacement of the container is completed.
Therefore, the standby container in the usable state can supply the liquid material to the vaporizer 91 without delay by opening the gas feed valves 141 and 241 in the pressurized gas line and the supply valves 147 and 247 in the material supply line. is there.

As shown in FIG. 4, the replacement of the empty first container 150 is performed by changing the second container 250 from the standby state to the use state in accordance with the stoppage of the use of the first container 150. After switching to the two containers 250 and bringing the first container 150 into the use stopped state, the first container 150 is subjected to a material return process. Thereafter, the container is replaced by mounting a new container by performing gas purging by evacuation and gas injection, and again performing gas purging by evacuation and gas injection. A pressurization process for filling the liquid material into the one material line connection pipe 123 is performed, and a new first container 150 is set in a standby state.

This material return processing is performed by the first gas feed valve.
After the 141 and the first supply valve 147 are closed to put the first container 150 into the use stop state, the first line short-circuit valve 143 is opened. In this way, by opening the first line short-circuit valve 143, the gas supply pipe 111 and the first material line connection pipe 123 are communicated as shown in FIG. It can be led to the one material line connecting pipe 123. Therefore, the liquid material remaining inside the first material line connection pipe 123 and the first discharge pipe 153 can be returned to the first container 150.

At this time, the first gas introduction valve 161
May be left open or closed as shown in the table of FIG. in this way,
After returning the liquid material remaining in the first material line connection pipe 123 and the first discharge pipe 153 to the first container 150, as shown in FIG. 11, the first discharge valve 163 and the first gas introduction valve 161 are provided.
Is closed, and the first line short-circuit valve 143 is further closed. Further, the first pipe connection valve and the first exhaust valve 149 of the connecting pipe are opened, and as shown in FIG. .

At this time, the pump exhaust valve 78 provided in the pump exhaust line is closed, the vacuum pump of the abatement apparatus 135 is operated, and the pressure of the first exhaust pipe 131 is reduced to a stable reduced pressure by the vacuum pump. Thereafter, the first exhaust valve 149 is opened. As described above, by opening the first pipe connection valve 165 provided in the first connection pipe 155, the first gas introduction pipe 1 is opened.
The communication between the first discharge pipe 153 and the first discharge pipe 153 can be established.
Also, the first gas feed valve 141 and the first gas introduction valve 161,
By closing the first discharge valve 163 and the first supply valve 147, the first gas line connection pipe 113 and the first gas introduction pipe 151, which are pressurized gas lines to the first container 150, are connected to the first container 150. The interior of each of the first discharge pipe 153 and the first material line connection pipe 123, which are the material supply lines, can be closed spaces. By reducing the pressure in the closed space by the vacuum pump, the liquid material adhering and remaining inside the first discharge pipe 153 and the first material line connection pipe 123 can be evaporated.

Next, by closing the first exhaust valve 149 and opening the first line short-circuit valve 143, the inert gas which is a pressurized gas is supplied to the first discharge pipe 153 via the first material line connection pipe 123. Or the first, as shown in FIG.
The gas feed valve 141 is opened, and pressurized gas is fed into the first discharge pipe 153 via the first gas line connection pipe 113, the first gas introduction pipe 151, and the first connection pipe 155, and a gas press-fit state is established.

Then, the first short-circuit valve or the first gas feed valve 141 is closed again and the first exhaust valve 149 is closed.
open. Therefore, it is possible to perform vacuuming to exhaust the liquid material and the vaporized gas of the liquid material together with the inert gas pressurized into the closed space such as the first discharge pipe 153 to the abatement apparatus 135, and repeat the gas pressurizing and the vacuuming. Thus, gas purging can be performed.

As described above, the gas purge by repeating the gas injection and the evacuation is performed to remove the liquid material and the vaporized gas of the liquid material remaining in the first discharge pipe 153 and the first material line connection pipe 123. Later, the first gas line joint
The first container 150 is removed from the first material line joint 115 and the first material line coupling 125, and the container replacement for mounting a new first container 150 is performed.

When removing the first container 150,
The first exhaust valve 149 is closed, the first line short-circuit valve 143 and the first gas feed valve 141 are opened, and the first container 150 is removed with the inside of the first discharge pipe 153 and the like being in a pressurized state. Therefore, as shown in FIG.
From the first gas line connection pipe 113 via the first gas feed valve 141 and the inert gas from the first material line connection pipe 123 via the first short-circuit valve. become. As described above, by injecting the inert gas from the open ends of the first gas line connection pipe 113 and the first material line connection pipe 123, the gas line connection pipe 113 provided with the joints 115 and 215 and the material line connection pipe 123 External air can be prevented from flowing into the pipe from the end.

Then, the first liquid material is newly sealed.
When the container 150 is attached, the first line short-circuit valve 143 and the first gas feed valve 141 are closed, and the first pipe connection valve 165 of the first container 150 is opened to open the first gas introduction pipe 151 and the first discharge pipe 15.
3, and the chamber is evacuated as shown in FIG. Further, the first exhaust valve 149 is closed, the first line short-circuit valve 143 or the first gas feed valve 141 is opened, and gas injection is performed to pressurize the first discharge pipe 153 and the like. By performing gas purging, the first discharge pipe 153
For example, water remaining on the inside is removed.

After the first container 150 is newly attached and the water and other gases are purged, the first pipe connection valve 165 is switched from the reduced pressure state of the first discharge pipe 153 by evacuation shown in FIG. Close the first gas introduction pipe 151 and the first discharge pipe 15
Cut off communication with 3. Then, as shown in FIG. 9, the first discharge valve 163 is opened, and the liquid material is sucked into the first discharge pipe 153 and the first material line connection pipe 123. Further, the first exhaust valve 149 is closed, and as shown in FIG.
The first gas supply valve 141 and the first gas introduction valve 161 are opened, a pressurized gas is sent into the first container 150, and the first container 150 is subjected to a pressurization process to surely supply the first discharge pipe 153 with the liquid material. The inside of the first material line connecting pipe 123 is filled and the first container 150 is filled.
Is in a standby state.

Thereafter, as shown in the table of FIG. 11, the standby state of the first container 150 is maintained with the first gas feed valve 141 closed. Therefore, when the liquid material in the second container 250 runs out, the first supply valve 147 and the first gas feed valve 1
Open the liquid material from the first container 150 immediately after opening the vaporizer 9
One that can be supplied. In addition, the second container 250
After using the liquid material of the second container 250, the first container 150
When the mode is switched to, the liquid return of the second container 250, the gas purge, the container replacement, and the gas purge and the container pressurization are similarly performed. Then, the second container 250 is replaced while the first container 150 is being used, and the second container 250 is placed in a standby state.

As described above, this liquid material supply device is
Since a single container can be provided, the liquid material can be continuously supplied to the vaporizer 91 by switching the container to be used. In addition, since a vacuum pump is provided in the abatement apparatus 135, the first discharge pipe 153 and the first material line connection pipe 123 or the second discharge pipe 253 and the second material line connection pipe 223 are reduced by this vacuum pump. In addition, the liquid material remaining in the pipe is evaporated and vaporized, and the gas purge can be reliably performed in a short time. Therefore, the container can be quickly and safely replaced.

Further, purging is performed even after the containers 150 and 250 are exchanged, and the liquid material is supplied to the material line connection pipes 123 and 223 while the interiors of the discharge pipes 153 and 253 and the material line connection pipes 123 and 223 are evacuated.
Since the inside of the material supply line 223 is filled, the material supply line can be in a state where air, purge gas, and the like are not contained. Therefore, when switching the containers 150 and 250 to be used, a stable supply of the liquid material to the vaporizer 91 can be performed without mixing a purge gas or the like into the liquid material.

Further, they are pipes which can perform the operation of replacing the container and the operation of supplying the liquid material from the container independently. Therefore, it is possible to solve the problem caused by the container replacement, and in the production of synthetic quartz glass, it is necessary to produce high-quality quartz glass without causing striae and inhomogeneity due to regular container replacement. Can be. That is, if the purge gas remains in the supply line of the liquid material after the purging after replacing the container, the purge gas is simultaneously sent to the vaporizer 91 when the liquid material is supplied by switching the container to be used. When the purge gas is sent to the vaporizer 91 in this way, in order to cause a change in the state of the vaporizer 91, the purged line is maintained in a vacuum state so that the purge gas or the like does not remain in the material supply line. However, leaving the line in a vacuum will cause contamination,
A liquid material supply device is provided in which the gas introduction valve and the discharge valve of the standby container are opened, and the material receiving valve is also opened to make the discharge pipe and the material line connection pipe stand by while the liquid material is filled. Here, if the gas introduction valve and discharge valve of the standby container are opened, the internal pressure of the standby container can be measured by the pressure gauge 85,8.
It can also be monitored in step 6 to avoid overpressure and prevent the container from bursting.

The abatement apparatus 135 has a liquid trap and an abatement tower upstream of the vacuum pump in addition to the vacuum pump. Gas and the like are adsorbed and removed by a detoxification tower arranged downstream of the liquid trap, and the gas sucked from a material line connection pipe or the like is released to the atmosphere in a harmless state.

Further, each of the containers 150 and 250 has its gas introduction pipe 1
Since there are connecting pipes 155 and 255 for communicating the 15,215 and the discharge pipes 153 and 253, the pressurized gas is sent to the discharge pipes 153 and 253 and the material line connecting pipes 123 and 223 through the connecting pipes 155 and 255, and
The gas in 3,253 and the material line connection pipes 123, 223 can be reliably moved to perform gas purging quickly and reliably.

In the liquid material supply apparatus shown in FIG. 1, the first exhaust pipe 131 is connected to the first gas line connecting pipe 113, and the second exhaust pipe 131 is connected to the second gas pipe 113.
Although the exhaust pipe 231 is connected to the second gas line connection pipe 213, as shown in FIG. 12, the first exhaust pipe 131 and the second exhaust pipe 231 are respectively connected to the first material line connection pipe 123 and the second material line It may be connected to the connection pipe 223. On the other hand, gas introduction pipe 1
When connecting the exhaust pipes 131 and 231 to the material line connection pipes 123 and 223 by providing the connection pipes 155 and 255 for communicating the discharge pipes 153 and 253 with the discharge pipes 153 and 253, the purge gas is supplied through the connection pipes 155 and 255 without using the vacuum pump of the abatement apparatus 135. The discharge pipe 153,2
53, discharge pipes 153, 253 and material line connection pipes 123, 223
Purge gas is continuously flowed through the exhaust pipes 131 and 231 through
The liquid material and the vaporized gas of the liquid material can be reliably removed from the inside of the discharge pipes 153 and 253 and the material line connection pipes 123 and 223. Also in this case, reliable gas purging can be performed in a short time.

As shown in FIGS. 12 and 13, the material receiving valves 145, 245 provided in the material line connecting pipes 123, 223, respectively.
May be omitted. And the exhaust pipes 131,231
For example, when connecting near the material line joints 125 and 225, even when connecting the containers 150 and 250 that do not have the connection pipes 155 and 255, the purge gas via the bypass pipes 129 and 229 is used to separate the material line joints 125 and 225 serving as a separation part of the containers 150 and 250.
The gas purge can be performed quickly and reliably by performing a gas purge that continuously flows so as to flow immediately adjacent to the gas, or by performing a gas purge that combines gas press-fitting and vacuuming using a vacuum pump.

As shown in FIG. 14, two gas supply pipes connected to a pressurized gas supply source (not shown) for receiving an inert gas are provided. It may be. In this case, a first gas supply pipe 111 and a second gas supply pipe 211 are provided, and an auxiliary connection pipe 117 for connecting the first gas supply pipe 111 and the second gas supply pipe 211 is provided. An opening / closing valve as an auxiliary connection valve 119 is provided in the middle of the pipe 117.

As described above, if the first gas supply pipe 111 and the second gas supply pipe 211 are provided so that the pressurized gas can be supplied to each of the two containers 150 and 250, 1
The inert gas from the pressurized gas supply source can be sent by the gas supply pipe 111, and the inert gas from the pressurized gas supply source can be sent to the second container 250 by the second gas supply pipe 211.
By providing the auxiliary connection pipe 117 having the auxiliary connection valve 119, it is also possible to switch the pressurized gas supply source when a problem occurs in the pressurized gas supply source, so that the liquid material can be more surely switched. Can be supplied to the vaporizer 91 without interrupting the supply.

Further, as shown in FIG.
And a first exhaust pipe 131 connecting the first abatement apparatus 135 to the first gas line connecting pipe 113 or the first material line connecting pipe 123.
And a second exhaust pipe 231 for connecting the second abatement apparatus 235 to the second gas line connection pipe 213 or the second material line connection pipe 223. The first exhaust pipe 131 and the second exhaust pipe 231 An auxiliary exhaust pipe 137 for connecting the air supply and the exhaust gas may be provided. This auxiliary exhaust pipe 1
37 is provided with an opening / closing valve as an auxiliary exhaust valve 139.

In this case, in the event of malfunction of the abatement devices 135 and 235 such as a failure of the vacuum pump and a decrease in the capacity of the liquid trap and the abatement tower, the abatement devices 135 and 235 are switched to perform gas purging and container replacement. Can be. The first gas line connection pipe 113 and the first material line connection pipe 123 are connected to the second
The gas line connecting pipe 213 and the second material line connecting pipe 223 are arranged so that the first container 150 and the second container 250 can be brought close to each other so that a gas introducing pipe and a discharge pipe can be connected and attached to each connecting pipe. ing.

As described above, by disposing the first container 150 and the second container 250 close to each other and setting one of the containers in a standby state, the temperature of the liquid material in both the containers 150 and 250 is set to a temperature close to the natural temperature. When switching the container to be used, the vaporizer
Reduce the temperature change of the liquid material supplied to 91
Variations in vaporization conditions at 91 can be prevented. As described above, in the present embodiment, since the container and the standby container are placed in the same environment, there is no difference in temperature and pressure between the two containers 150 and 250, and the temperature and pressure of the liquid material supplied to the vaporizer 91 even after the container is replaced. Can be kept constant. As a result, it is possible to prevent a change in the amount of gas generated in the vaporizer 91 due to a change in the temperature of the liquid material supplied when the container is replaced, which has conventionally been a problem.

Further, each of the pressurized gas lines and the material supply lines provided in the containers 150 and 250 is constituted by a pipe which can perform the operation of replacing the container and the operation of supplying the liquid material from the container independently. Even when the container becomes unusable due to container replacement or component replacement, the other container can supply the liquid material to the vaporizer 91 without interruption.

Therefore, by continuously providing and using two or more containers capable of supplying the liquid material to the vaporizer 91 as described above, it is possible to continuously supply the liquid material.
In controlling the opening / closing operation shown in FIG. 11, it is preferable to control each of these opening / closing valves by using a microcomputer or the like. As described above, the entire liquid material supply device is computer-controlled, so that work efficiency can be improved and erroneous operations can be prevented. As a control program, a counter is used to determine the number of times of vacuuming or gas injection, and a program for controlling the opening and closing control of each valve by a computer using a timer is used as the number of times. This is preferable because the time setting can be easily changed.

In each of the above embodiments, the gas introduction pipe 151,
251 is provided with gas introduction valves 161,261 and discharge pipes 153,253
Are provided with discharge valves 163, 263, connection pipes 155, 255 for connecting the gas introduction pipes 151, 251 and the discharge pipes 153, 253, and pipe connection valves 165, 265 provided between the connection pipes 155, 255. However, a three-way valve is provided midway between the gas introduction pipes 151, 251 and the discharge pipes 153, 253 to provide the gas introduction pipes 151, 251 and the discharge pipes 153, 253.
Connection pipes 155 and 255 are connected to each other, and one of the three-way valves allows the inside of the connection pipes 155 and 255 to be in communication with the gas line joints 115 and 215 or in communication with the inside of the container body, and further, the inside of the container body is connected to the gas line. The connection between the connection pipes 155 and 255 is switched by the other three-way valve between the connection pipes 155 and 255, and the connection between the connection pipes 155 and 255 or the connection to the inside of the container body. In communication with the material line fittings 125 and 225,
May be switched.

As described above, two three-way valves may be used instead of using three open / close valves of the gas introduction valve, the discharge valve, and the pipe connection valve for each of the containers 150 and 250. Similarly, the line short-circuit valves 143 and 243 of the bypass pipes 129 and 229 are omitted, the gas supply valves 111 and 241 are three-way valves, and the gas supply pipe 111, the bypass pipes 129 and 229 and the gas line connection pipes 113 and 213 are connected, and the other ends of the bypass pipes 129 and 229 are three-way. It may be connected to the material receiving valves 145 and 245 as valves. [Comparative Example 1] Using a liquid material of silicon tetrachloride filled in a container 50 of a liquid material supply device shown in FIG. Generate. The resulting raw material gas is led to the reaction system, diluted with a carrier gas from the center of a quartz glass multi-tube burner, and jetted into an oxyhydrogen flame. A high-purity synthetic quartz glass ingot was synthesized. However, container
Nitrogen gas was used as a pressurized gas for pumping the liquid material of silicon tetrachloride stored in 50 to the vaporizer 91 and a purge gas for purging.

The supply of the liquid material to the vaporizer 91 was performed by monitoring the weight of the container 50, and was replaced with a different container depending on the remaining amount of the liquid material (5 kg or less). For this reason, the restraining time of the operator is long, and the operation for replacing the container 50 requires skill. Further, when replacing the container 50, in order to prevent the pressurized gas line 10 and the material supply line 20 from being polluted, the supply of the liquid material to the vaporizer 91 was intermittent. .

With the above apparatus, a high-purity quartz glass ingot having a diameter of 250 mm and a height of 500 mm was synthesized.
A side surface perpendicular to the growth direction of the obtained ingot was processed for inspection of striae, and the striae was observed by a projection method. As a result, striae were detected in the high-purity quartz glass ingot. It is considered that the heterogeneous layer different from the other portions is caused by mixing of the purge gas and fluctuation of the amount of gas supplied to the reaction system. Embodiment 1 A two-container and abatement apparatus shown in FIG.
Using a liquid material supply device provided with 135, a liquid material of silicon tetrachloride is distilled and vaporized in a vaporizer 91 to generate a high-purity silicon tetrachloride gas (raw material gas). The raw material gas thus obtained is introduced into a reaction system, diluted with a carrier gas from the center of a quartz glass multi-tube burner, jetted into an oxyhydrogen flame, and has a diameter of 250 mm and a height of 500 m by a direct method.
m high-purity quartz glass was synthesized. Nitrogen gas was used as a pressurized gas for purging the liquid material of silicon tetrachloride stored in the containers 150 and 250 to the vaporizer 91 and a purge gas.

When the container is replaced, the purge for removing the liquid material remaining in the pressurized gas line and the material supply line is performed by evacuation using the vacuum pump of the abatement apparatus 135 and introduction of gas by purging gas. This was carried out by employing a repeated press-in purge. In addition, the control of each valve is automatically performed by computer control, thereby shortening the purge time and eliminating any human operation error. The number of repetitive purging of evacuation-gas injection is detected by a counter, and
The times of pressurization and depressurization in evacuation and gas injection were each detected by a timer, and each could be freely selected. For this reason, it was possible to easily change the conditions such as the purge time and the number of times that had conventionally been required to change the program.

FIG. 1 shows a method for pressure-feeding a liquid material to the vaporizer 91.
The device will be described in detail. The pressurized gas is supplied via a regulator 71 and a filter 73. The pressurized gas line has a pressure switch 81, a check valve 75, a gas feed valve 141, 241 which is an open / close valve, and a pressure gauge 85,
86 were installed. The pressure switch 81 is for detecting a decrease in the pressure of the pressurized gas, and the pressure gauges 85 and 86 monitor the internal pressure of the containers 150 and 250.

In this embodiment, the pressurized gas is supplied to the containers 150 and 25
A value higher than the internal pressure of 0 (2 kg / cm ² ) was set to 5 kg / cm ² . The gas feed valves 141 and 241 of the pressurized gas line were opened only at the time of pressurization in order to prevent the back diffusion of the liquid material causing the contamination of the line. The internal pressure of the containers 150 and 250 was set to a desired value during the supply of the liquid material by opening and closing the gas feed valves 141 and 241 while reflecting the monitoring results of the pressure gauges 85 and 86. In addition, container for some reason such as accident, fire
In order to avoid the worst case where the internal pressure of 150,250 becomes overpressure and the containers 150,250 explode, etc. A mechanism for preventing the container from being ruptured was provided.

That is, the exhaust valves 149 and 249 were programmed to be normally closed, but opened when the internal pressure of the container monitored by the pressure gauges 85 and 86 exceeded 3.0 kg / cm ² . The abatement apparatus 135 is provided with an abatement tower or the like upstream of the pump to protect the vacuum pump. This abatement tower also
It also serves to stop the reverse diffusion of oil from the vacuum pump.

The pressure gauge 87 has exhaust valves 149 and 249 at its ends at the time of vacuum evacuation and gas injection, and the pressure of the vacuum pump line connected at the other end to the vacuum pump indicates the failure of the vacuum pump. The system was installed so that the line could be automatically shut off when the vacuum could not be maintained due to the above conditions. In the present embodiment, since one abatement apparatus 135 is provided, the abatement apparatus 135 or the second exhaust valve 24
What is necessary is just to detect the pressure at one point between 9 and the abatement apparatus 135.

Hereinafter, the containers 150 and 250 are cut off with a joint,
Take the case of supplying the liquid material in the other standby container as an example,
The control operation of each line in the supply of the liquid material and the container replacement by the two systems will be described for each mode. First, in order to replace the container, the remaining liquid in the pipe is put into the container.
Return for 0 seconds (reconstitution). Next, vacuum evacuation and gas injection into the piping are performed. The inside of the pipe is evacuated by a vacuum pump for a time (1 minute) set by a timer, and then the inside of the pipe is filled with nitrogen gas (5 seconds). This is repeated the number of times (100 times) set by the counter (gas purge).
Separate the device from the empty container with a joint and connect the container filled with fresh liquid material (removal).

In order to make the container stand by in a usable state, the air mixed in the pipe by removing the container was removed.
Again, vacuum evacuation and gas injection are performed as described above. However, in order to prevent nitrogen gas from remaining in the piping, the process is finally completed in a vacuum state (gas purge). Further, in order to keep the inside of the vacuum pipe free from contamination and to use a new container at any time, pressurize the container with nitrogen gas to the upper limit of 2.2 kg / cm ^{2 of the} pressure gauge (pressurization). Finally, in order to maintain the internal pressure of the new container, to enable the supply of liquid material at any time, and to detect an overpressure state or abnormality of the internal pressure of the container, monitor the internal pressure of the container with a pressure gauge and wait (standby). .

The high-purity quartz glass ingot obtained by the above-described apparatus for supplying the liquid material to the vaporizer 91 completely eliminated fluctuations at the time of switching the containers, and was able to supply the liquid material stably. Was not detected. This embodiment is inexpensive as compared with the apparatus of the second embodiment, and the apparatus can be made smaller. However, since the pressurized gas supply source is shared, for example, when the joint is removed, the liquid material may be reversely diffused from the container of the other joint due to the relationship between the pressure levels. Therefore, in that case, it is necessary not to open the gas feed valve of the used container. [Example 2] In an apparatus having a pressurized gas line, an abatement apparatus and the like shown in FIG. 14 independently in each container, a liquid material of silicon tetrachloride was used, and the liquid was distilled and vaporized in a vaporizer 91.
Generates high-purity silicon tetrachloride gas (raw material gas). The resulting raw material gas was introduced into the reaction system, diluted with a carrier gas from the center of a quartz glass multi-tube burner, and spouted into an oxyhydrogen flame to synthesize a high-purity synthetic quartz glass ingot by the direct method. . Nitrogen gas was used as a pressurized gas for pumping the liquid material of silicon tetrachloride stored in the container to the vaporizer 91 and a purge gas for purging.

When the container was replaced, the purging for removing the liquid material remaining in the pressurizing line and the material supply line was performed by repeatedly purging with vacuum and gas injection using a vacuum pump. In addition, the operation is performed automatically by computer control, thereby shortening the purge time and completely eliminating human operation errors. The number of repetitions of purging by evacuation and gas injection can be freely selected by a counter, and the evacuation and pressurization time by a purge gas can be freely selected by a timer. For this reason, it is possible to easily change the conditions of the purge time and the number of times, which had conventionally been required to change the program.

FIG. 1 shows a method of pressure-feeding a liquid material to the vaporizer 91.
This will be specifically described in Section 4. The pressurized gas is supplied from each gas supply pipe 111, 211 via a regulator 71 and a filter 73. In addition to the pressure switch 81 and the check valve 75, the gas feed valves 141 and 241 and the pressure gauge 8
5,86 were installed respectively. The two pressure switches 81 provided on each of the gas supply pipes 111 and 211 are for detecting a decrease in the pressure of the pressurized gas, and the pressure gauges 85 and 86 monitor the internal pressure of the containers 150 and 250.

In the present embodiment, the pressurized gas was set to a value higher than the internal pressure of the container (2 kg / cm ² ) and 5 kg / cm ² . The gas feed valves 141 and 241 of the pressurized gas line were opened only at the time of pressurization in order to prevent the back diffusion of the liquid material causing the contamination of the line. The internal pressure of the containers 150 and 250 was set to a desired value during the supply of the liquid material by opening and closing the gas feed valves 141 and 241 while reflecting the monitoring results of the respective pressure gauges.

Further, in order to avoid the worst case in which the internal pressure of the containers 150 and 250 becomes excessively high due to an accident, a fire, or the like and the containers 150 and 250 explode, the pressure gauges 85 and 8 are used.
A rupture prevention mechanism for the container, which opens and closes the exhaust valves 149 and 249 based on the monitoring result of 6 and guides the liquid material in the line to the abatement apparatus, is provided. That is, the exhaust valves 149 and 249 were normally closed, but were programmed to open when the internal pressure of the containers 150 and 250 monitored by the pressure gauges 85 and 86 exceeded 3.0 kg / cm ² .

The abatement device is used to protect the vacuum pump.
An abatement tower is installed upstream of the pump. The abatement tower also serves to stop the back diffusion of oil from the vacuum pump. The pressure gauges 87 and 88 were installed so that the line could be automatically shut off when the pressure in the vacuum pump line could not be maintained due to a failure of the vacuum pump during vacuum evacuation and gas injection.

Hereinafter, a case where the liquid material in the first container 150 is exhausted and the liquid material is supplied in the standby container will be described as an example, and the control operation of each line in a series of supply of the liquid material and replacement of the container will be described for each mode. I do. First, in order to replace the container, the residual liquid in the material supply line is poured into the first container 150.
Return for 0 seconds (reconstitution). Next, vacuum evacuation and gas injection into the piping are performed. The inside of the pipe is evacuated by a vacuum pump for a time (1 minute) set by a timer, and then a line partitioned by opening and closing the valve shown in FIG. 11 is filled with nitrogen gas (5 seconds). This is repeated the number of times (100 times) set by the counter (gas purge). The empty first container 150 of the present apparatus is cut off, and the new first container 150 is replaced with the old first container 150 and connected (removed).

In order to keep the new first container 150 ready for use, the vacuum and gas injection are performed again in the same manner as described above in order to remove the air and moisture mixed in the line by replacing the container. However, in order to prevent the purge gas from remaining in the piping, the process is finally completed in a vacuum state (gas purge). Further, the vacuum line is not contaminated and the first container
The internal pressure of the container 150 is a pressure gauge so that 150 can be used at any time.
Pressurize with nitrogen gas to the upper limit of 2.2 kg / cm ^{2 of} 85 (pressurization). Finally, while maintaining the internal pressure of the first container 150, the liquid material can be supplied at any time, and the internal pressure of the first container 150 is monitored by the pressure gauge 85 in order to detect an overpressure state or abnormality of the internal pressure of the container. The first container 150 is put on standby (standby).

By performing the above control operations, the liquid material is vaporized while exchanging the containers 150 and 250 using the apparatus of the present invention.
1 was continuously fed. A side surface perpendicular to the growth direction of a high-purity quartz glass ingot having a diameter of 250 mm and a height of 500 mm obtained using this apparatus was processed for striae inspection,
Striae were observed by the projection method. As a result, no striae due to the container replacement were detected in the obtained quartz glass ingot.

Therefore, in this apparatus, it was confirmed that there was no fluctuation at the time of switching the container and that the supply of the liquid material was stable. In addition, since the present apparatus has two independent pressurized gas lines, it can be used as a pressurized gas line for each container. That is, one can be used for pressurization and the other can be used for purging. In addition, regulator 71, filter 7
3. Valves (not shown) were provided before and after consumables such as pumps, and were individually replaceable. By opening and closing the auxiliary connection valve 119, it is possible to perform the replacement of the parts without interrupting the supply of the pressurization or the purge gas.

The auxiliary exhaust valves 139 are normally closed, and the vacuum pumps of the abatement devices 135 and 235 can be used for each of the containers 150 and 250. Thereby, the life of the vacuum pump can be extended. And pressure gauge 87,88
By automatically opening and closing the auxiliary exhaust valve 139 based on the detected value of, normal operation of a series of vacuum pumps during evacuation and gas injection can be guaranteed.

[0092]

According to the invention of the present application, the gas supply pipe having a tip divided into two and having an opening / closing valve at each end and the two ends provided with the opening / closing valve are combined into one vaporizer. A material supply pipe for supplying a liquid material to the container, a gas line connection pipe for connecting each end of the gas supply pipe to a gas introduction pipe of each container,
A material line connection pipe that connects each end of the material supply pipe to the discharge pipe of each container, and a bypass pipe that connects the gas supply pipe and each material line connection pipe, and each bypass pipe has an open / close valve. Each container has an opening / closing valve in its gas introduction pipe and discharge pipe, and two of the containers filled with the liquid material can be attached to and detached from the gas line connection pipe and each material line connection pipe by joints, respectively. A liquid material supply device that supplies a liquid material in each container to a vaporizer through a material supply tube while sending pressurized gas from a tube to each container.

Accordingly, two containers are provided, and when one container is replaced, the liquid material can be supplied to the vaporizer from the other container. For this reason, since the supply of the liquid material to the vaporizer can be performed stably without interruption, the product can be stably obtained without changing the amount of gas generated in the vaporizer. In particular, if the liquid material supply device is arranged close to the container, the change of the temperature of the liquid material supplied to the vaporizer can be prevented even when the used container is switched, and the amount of gas generated by the vaporizer can be changed. Can be prevented.

[0094] In the invention described in claim 2, the abatement apparatus having a vacuum pump is a liquid material supply apparatus connected to each of the material line connection pipes by an exhaust pipe having an open / close valve. Therefore, when the container is replaced, the container is evacuated, the purge is performed in a short time, and the container can be replaced quickly. Further, after the container is replaced, vacuum is drawn to prevent impurities such as air and purge gas from remaining in the material supply line when the liquid material is supplied from the new container to the vaporizer, and such impurities are supplied to the vaporizer. Sending can be prevented.

Further, according to the third aspect of the present invention, the tip is 2
A gas supply pipe branched into two and having an open / close valve at each end, or two gas supply pipes each having an open / close valve at each end, and a gas introduction pipe and a discharge pipe each having an open / close valve. And a material supply pipe for supplying the liquid material to one vaporizer by combining two ends having an opening and closing valve, and each end of the gas supply pipe with the container. A gas line connecting pipe connected to the gas introduction pipe, a material line connecting pipe connecting each end of the material supply pipe to the discharge pipe of the container, and further, a bypass pipe and a connecting pipe, each of which has an open / close valve A gas supply pipe is connected to each material line connection pipe, each connection pipe is provided with an open / close valve to connect a gas introduction pipe and a discharge pipe of the container, and an abatement apparatus having a vacuum pump is provided. Exhaust that connects the harm device to each material line connection pipe or each gas line connection pipe When one in which a liquid material supply system having a. Therefore, it is a liquid material supply device that has a connection pipe that connects the gas introduction pipe and the discharge pipe, and can form a purge line including a joint that is a disconnection point of the container, and performs a reliable purge in a short time. It is possible to carry out quick container exchange. For this reason, when one of the containers is empty, the liquid material is continuously supplied to the vaporizer while the container is easily replaced. During the supply, impurities such as air and purge gas are prevented from remaining in the material supply line, so that such impurities can be prevented from being sent to the vaporizer.

The invention described in claim 4 has two of the abatement apparatuses having a vacuum pump, and connects each abatement apparatus to any one of a gas line connection pipe and a material line connection pipe. This is a liquid material supply device having an auxiliary exhaust pipe connecting the two exhaust pipes with an opening / closing valve. Therefore, when replacing the container, even if the performance of one of the abatement equipment is reduced, by switching the abatement equipment,
Purging and evacuation can always be performed reliably in a short time, and the container can be quickly replaced so that impurities such as air and purge gas do not remain in the material supply line.

Further, the invention according to claim 5 is characterized in that two containers of a liquid material sealed with a gas introduction pipe provided with an opening / closing valve and a discharge pipe provided with an opening / closing valve are provided at the ends. Each having a joint for connecting the gas introduction pipe of each container and connected to the gas supply pipe by an open / close valve;
Two material lines each having a gas line connection pipe and a joint for connecting the discharge pipe of each of the containers at one end and each other end connected to the material supply pipe by an open / close valve. A connection pipe, two bypass pipes each having an opening / closing valve in the middle and connecting the gas supply pipe and each of the material line connection pipes, and an exhaust pipe having an opening / closing valve are connected to the material line connection pipe. And abatement device equipped with a vacuum pump, when supplying the liquid material to the vaporizer by the liquid material supply device having, when the liquid material in one container is reduced, the liquid material from the other container to the vaporizer Close the open / close valve provided on the discharge pipe of the container that has supplied and reduced the amount of liquid material and the open / close valve at the other end of the material line connection pipe connecting this discharge pipe, and pressurize the discharge pipe with purge gas via the bypass pipe State, and further purging the discharge pipe through the exhaust pipe to reduce the pressure, performing replacement of the container after the purging, purging under the pressurized state and the reduced pressure state even after the replacement, and purging the discharge pipe and the material line connection pipe. A method of supplying a liquid material in which the opening and closing valve of the discharge pipe is opened to fill the inside of the material line connection pipe with the liquid material when the inside is in a reduced pressure state.

Therefore, purging can be reliably performed in a short time by pressurizing and depressurizing, and the material supply line is reliably filled with the liquid material after the container is replaced, so that the preparation of the supply of the liquid material by the new container can be quickly performed. Can be done. For this reason, a stable supply of the liquid material to the vaporizer can be maintained. And further, the invention described in claim 6 is:
It has two containers, each of which has a gas introduction pipe having an opening / closing valve and a discharge pipe having an opening / closing valve and in which a liquid material is sealed, and a joint for connecting the gas introduction pipe of each of the containers at an end. And two gas line connection pipes each connected to a gas supply pipe by an open / close valve, and a joint for connecting the discharge pipe of each of the containers at one end, and each other end has an open / close valve. And two material line connecting pipes connected to the material supply pipes, a connecting pipe connecting the gas introduction pipe and the discharge pipe in each of the containers with an open / close valve in the middle, and an open / close valve. An abatement device connected to the gas line connection pipe or the material line connection pipe by an exhaust pipe and having a vacuum pump, and supplying the liquid material to the vaporizer by a liquid material supply device having Less material When it becomes low, the liquid material is supplied to the vaporizer from the other container, and the opening / closing valve provided on the discharge pipe of the container with reduced liquid material and the other end of the material line connection pipe connecting this discharge pipe. Close the on-off valve and open the on-off valve provided on the connecting pipe to make the gas introduction pipe and the discharge pipe communicate with each other. The inside of the gas line connection pipe and the inside of the gas introduction pipe, the inside of the discharge pipe, and the material line connection pipe The interior of the container is subjected to a purge of repeating a pressurized state and a depressurized state, the container is replaced after the purging, the purging is performed under the pressurized state and the depressurized state even after the replacement, and a discharge pipe and a material line connection pipe are provided. Is a method of supplying a liquid material in which the inside of the material line connection pipe is filled with the liquid material by closing the open / close valve of the connection pipe and opening the open / close valve of the discharge pipe when the inside of the pipe is in a reduced pressure state.

Therefore, purging can be performed in a short time by pressurizing and depressurizing, by performing a purge line using the joint between the discharge pipe and the material line connecting pipe, where the container is removed. In addition, the pressure is increased and reduced even after the container is replaced, so that the material supply line can be reliably filled with the liquid material, and the preparation of the supply of the liquid material by a new container can be quickly performed. For this reason, a stable supply of the liquid material to the vaporizer can be maintained.

Further, the invention according to claim 7 is characterized in that two containers, each of which has a gas introduction pipe provided with an on-off valve and a discharge pipe provided with an on-off valve and in which a liquid material is sealed, Two gas line connection pipes each having a joint for connecting the gas introduction pipe of each container and connected to the gas supply pipe by an open / close valve, and the discharge pipe of each container at an end. For connecting two material lines connected to the material supply pipe by opening and closing valves, respectively, and an opening and closing valve in the middle to connect the gas supply pipe to each of the material line. Two bypass pipes respectively connecting pipes, a connecting pipe having an opening / closing valve in the middle to connect the gas introduction pipe and the discharge pipe in each container, and an exhaust pipe having an opening / closing valve to form the gas. Line connection pipe or the above material When the liquid material is supplied to the vaporizer by the liquid material supply device having an abatement device connected to the IN connection pipe and having a vacuum pump, when the liquid material in one container is reduced, the liquid material is supplied from the other container. The liquid material is supplied to the vaporizer, and the open / close valve provided on the gas introduction pipe of the container in which the liquid material has been reduced and the open / close valve at the other end of the material line connection pipe connected to the discharge pipe of this container are closed, and the bypass pipe is closed. Open the on-off valve to return the liquid material inside the material line connection pipe to the container, close the on-off valve provided on the discharge pipe, open the on-off valve provided on the connecting pipe, and establish a communication state between the gas introduction pipe and the discharge pipe. The inside of the gas line connection pipe and the inside of the gas introduction pipe, the inside of the discharge pipe and the inside of the material line connection pipe are repeatedly purged by repeatedly pressurizing and depressurizing. After the replacement, purging under the pressurized state and the depressurized state is performed, and when the inside of the discharge pipe and the material line connection pipe is in the depressurized state, the opening and closing valve of the discharge pipe is opened and the inside of the material line connection pipe is filled with the liquid material. This is a method for supplying a liquid material to be filled.

Therefore, since the liquid is returned by opening the on-off valve of the bypass pipe, the amount of liquid material remaining inside the material line connection pipe and the discharge pipe can be reduced, and deterioration of the abatement apparatus can be reduced. it can. Further, the residual amount of the liquid material inside the material line connection pipe and the discharge pipe is reduced, and the joint between the discharge pipe and the material line connection pipe where the container is removed is purged with a purge line, and the pressure and pressure are reduced. Reliable purging can be performed in a short time. Furthermore,
Pressurization and decompression are performed even after the container is replaced, so that the material supply line can be reliably filled with the liquid material, and the supply of the liquid material using a new container can be quickly performed. For this reason, a stable supply of the liquid material to the vaporizer can be maintained.

[Brief description of the drawings]

FIG. 1 is a conceptual diagram showing an example of a liquid material supply device according to the present invention.

FIG. 2 is a conceptual diagram showing a flow of a fluid in a use state of the liquid material supply device according to the present invention.

FIG. 3 is a conceptual diagram showing a flow of a fluid in switching a container of the liquid material supply device according to the present invention.

FIG. 4 is a diagram showing an example of a procedure for exchanging containers in the liquid material supply device according to the present invention.

FIG. 5 is a conceptual diagram showing a flow of a fluid in the container replacement of the liquid material supply device according to the present invention.

FIG. 6 is a conceptual diagram showing a flow of a fluid in the container replacement of the liquid material supply device according to the present invention.

FIG. 7 is a conceptual diagram showing a flow of a fluid in the container replacement of the liquid material supply device according to the present invention.

FIG. 8 is a conceptual diagram showing a flow of a fluid in the container replacement of the liquid material supply device according to the present invention.

FIG. 9 is a conceptual diagram showing a flow of a fluid in the container replacement of the liquid material supply device according to the present invention.

FIG. 10 is a conceptual diagram showing a flow of a fluid in the container replacement of the liquid material supply device according to the present invention.

FIG. 11 is a view showing valve states in respective states in the liquid material supply device according to the present invention.

FIG. 12 is a conceptual diagram showing another embodiment of the liquid material supply device according to the present invention.

FIG. 13 is a conceptual diagram showing another embodiment of the liquid material supply device according to the present invention.

FIG. 14 is a conceptual diagram showing another embodiment of the liquid material supply device according to the present invention.

FIG. 15 is a conceptual diagram of a conventional liquid material supply device.

[Explanation of symbols]

 Reference Signs List 10 Pressurized gas line 11, 111, 211 Gas supply pipe 13, 113, 213 Gas line connection pipe 15, 115, 215 Gas line joint 117 Auxiliary connection pipe 119 Auxiliary connection valve 20 Material supply line 23, 123, 223 Material line connection Pipe 25, 125, 225 Material line joint 27, 127 Material supply pipe 29, 129, 229 Bypass pipe 31, 131, 231 Exhaust pipe 135, 235 Extinguishing device 137 Auxiliary exhaust pipe 139 Auxiliary exhaust valve 41, 141, 241 Gas feed Valve 43, 143, 243 Line short-circuit valve 45, 145, 245 Material receiving valve 47, 147, 247 Supply valve 49, 149, 249 Exhaust valve 50, 150, 250 Container 51, 151, 251 Gas introduction pipe 53, 153, 253 Discharge pipe 155,2 55 Connecting pipe 61,161,261 Gas introduction valve 63,163,263 Discharge valve 165,265 Pipe connection valve 71 Regulator 73 Filter 75,76 Check valve 78 Pump exhaust valve 81 Pressure switch 83 Flow meter 85,86,87, 88 Pressure gauge 91 Vaporizer

Claims (7)

[Claims] 1. A gas supply pipe having a front end branched into two parts, an opening / closing valve at each of two ends, and an opening / closing valve at each of two branched ends.
A material supply pipe for supplying a liquid material to one vaporizer together with lines from the on-off valves, and two gas line connections for connecting an end of the gas supply pipe and a gas introduction pipe of a container. A pipe; two material line connection pipes for connecting an end of the material supply pipe and a discharge pipe of the container; and 2 connecting the gas supply pipe and the material line connection pipe.
The gas line connection pipe has one end connected to the open / close valve provided at an end of the gas supply pipe, and the other end has a joint for connecting a gas introduction pipe of a container. Each material line connecting pipe has one end connected to the open / close valve provided at the end of the material supply pipe and the other end connected to a discharge pipe of the container, and one end connected to the gas supply pipe. Each of the bypass pipes connected to a pipe and the other end connected to a material line connection pipe is provided with an opening / closing valve in the middle, and the container is provided with the gas introduction pipe having an opening / closing valve and the discharge pipe having an opening / closing valve. Two of the containers each containing a liquid material are detachably connected to each of the joints, and while the pressurized gas from the gas supply pipe is sent to each of the containers, the liquid material in each of the containers is supplied to the material supply pipe. To the vaporizer via Liquid material supply apparatus according to claim Rukoto. 2. The liquid material supply apparatus according to claim 1, wherein an abatement apparatus having a vacuum pump is connected to each of the material line connection pipes by an exhaust pipe having an opening / closing valve. 3. A gas supply pipe having a front end branched into two and having an open / close valve at each of two ends, or two gas supply pipes each having an open / close valve at each end, and this gas supply pipe. An auxiliary connection pipe having an on-off valve in the middle connected thereto, a gas inlet pipe having an on-off valve, and a container having a discharge pipe having an on-off valve and filled with a liquid material; Each end has an open / close valve,
A material supply pipe for supplying a liquid material to one vaporizer together with lines from two on-off valves, and two gas line connections for connecting an end of the gas supply pipe and the gas introduction pipe of the container. A pipe, two material line connection pipes connecting the end of the material supply pipe and the discharge pipe of the container, and further, two bypass pipes and two connection pipes, One end of each gas line connection pipe is connected to the on-off valve provided at the end of the gas supply pipe, and the other end has a joint for connecting the gas introduction pipe of the container, The connection pipe has one end connected to the open / close valve provided at the end of the material supply pipe, and a joint for connecting the discharge pipe of the container to the other end, and each of the bypass pipes has an open / close valve in the middle. The gas supply pipe and the material line connection pipe Each of the connection pipes includes an opening / closing valve in the middle to connect the gas introduction pipe and the discharge pipe in each container, and a detoxification device having a vacuum pump; and an opening / closing valve in the middle. An exhaust pipe connecting the abatement apparatus to each of the material line connection pipes or each of the gas line connection pipes, and pressurizing the liquid material of the container with the material supply pipe by pressurized gas from the gas supply pipe. A liquid material supply device, wherein the liquid material is supplied to the vaporizer via a liquid crystal display. 4. An exhaust pipe which has two said abatement apparatuses having a vacuum pump, and each said abatement apparatus is connected to any one of said gas line connection pipes or said material line connection pipes, and The liquid material supply device according to claim 3, further comprising an auxiliary exhaust pipe having an on-off valve and connecting the exhaust pipes. 5. A container having a gas introduction pipe provided with an opening / closing valve and a discharge pipe provided with an opening / closing valve and containing a liquid material therein, and the gas introduction pipe of each of the containers connected to an end portion. Two gas line connecting pipes each connected to a gas supply pipe by an open / close valve, and a joint for connecting the discharge pipe of each container at an end portion, and each other Two ends are connected to the material supply pipe by open / close valves, respectively, and two bypasses each having an open / close valve in the middle to connect the gas supply pipe and each material line connect pipe. A liquid material supply device having a pipe, and an abatement apparatus connected to the material line connection pipe by an exhaust pipe having an open / close valve and having a vacuum pump; Pressurized gas When supplying the liquid material to the vaporizer, when the liquid material in one of the containers is low, the liquid material from the other container is supplied to the vaporizer by a valve operation, and the liquid material in the container in which the liquid material is low is reduced. The on / off valve provided on the discharge pipe and the on / off valve connecting the material line connection pipe connecting the discharge pipe to the material supply pipe are closed, and the mouth of the discharge pipe is purged with the purge gas through the bypass pipe. A purging operation is performed in which the port of the discharge pipe is depressurized by the vacuum pump of the abatement apparatus through the exhaust pipe, and the container is replaced after the purging. A purge is performed in a state and a reduced pressure state, and when the inside of the discharge pipe and the material line connection pipe is in a reduced pressure state, the open / close valve of the discharge pipe is opened to open the inside of the material line connection pipe. A method for supplying a liquid material, characterized in that the portion is filled with a liquid material. 6. A container having a gas introduction pipe having an opening / closing valve and a discharge pipe having an opening / closing valve and containing a liquid material, and the gas introduction pipe of each of the containers is connected to an end portion. Two gas line connecting pipes each connected to a gas supply pipe by an open / close valve, and a joint for connecting the discharge pipe of each container at an end portion, and each other Two material line connecting pipes each having an open / close valve connected to the material supply pipe, a connecting pipe including an open / close valve in the middle and connecting the gas introduction pipe and the discharge pipe in each of the containers, A liquid material supply device having an exhaust pipe equipped with an open / close valve connected to the gas line connection pipe or the material line connection pipe and a detoxification apparatus equipped with a vacuum pump. From supply pipe When supplying the vaporizer with the pressurized gas, when the liquid material in one of the containers is reduced, the liquid material from the other container is supplied to the vaporizer by a valve operation, and the liquid material is reduced. The open / close valve provided on the discharge pipe of the container and the open / close valve connecting the material line connecting pipe connecting the discharge pipe to the material supply pipe are closed, and the open / close valve provided on the connecting pipe is opened. The gas introduction pipe and the discharge pipe to communicate with each other,
The inside of the gas line connection pipe and the inside of the gas introduction pipe, and the inside of the discharge pipe and the inside of the material line connection pipe, a pressurized state by a purge gas and a depressurized state by the vacuum pump of the abatement apparatus. After the purging, the container is exchanged. After the exchange, the purging under the pressurized state and the depressurized state is performed, and when the inside of the discharge pipe and the material line connection pipe is in the depressurized state, the connection is performed. A method for supplying a liquid material, comprising closing the open / close valve of a pipe and opening the open / close valve of the discharge pipe to fill the inside of the material line connection pipe with a liquid material. 7. A container having a gas introduction pipe provided with an opening / closing valve and a discharge pipe provided with an opening / closing valve and containing a liquid material, and the gas introduction pipe of each of the containers is connected to an end portion. Two gas line connecting pipes each connected to a gas supply pipe by an open / close valve, and a joint for connecting the discharge pipe of each container at an end portion, and each other Two ends are connected to the material supply pipe by open / close valves, respectively, and two bypasses each having an open / close valve in the middle to connect the gas supply pipe and each material line connect pipe. A pipe, a connecting pipe for connecting the gas introduction pipe and the discharge pipe in each container with an opening / closing valve in the middle, and an exhaust pipe with an opening / closing valve for the gas line connection pipe or the material line connection pipe. Connected and vacuum pump When supplying the liquid material sealed in the container to the vaporizer by the pressurized gas from the gas supply pipe, the liquid material supply device having When this happens, the liquid material from the other container is supplied to the vaporizer by a valve operation, and the opening / closing valve provided in the gas introduction pipe of the container in which the liquid material has been reduced and the discharge pipe of this container are provided. The on / off valve connecting the connected material line connection pipe to the material supply pipe is closed, and the on / off valve of the bypass pipe is opened to store the liquid material inside the material line connection pipe and the inside of the discharge pipe in the container. And closing the open / close valve provided on the discharge pipe and opening the open / close valve provided on the connection pipe to bring the gas introduction pipe and the discharge pipe into communication with each other. The inside of the gas line connection pipe and the inside of the gas introduction pipe, the inside of the discharge pipe and the inside of the material line connection pipe, a pressurized state by a purge gas and a depressurized state by the vacuum pump of the abatement apparatus. The container is replaced after the purging, and the purging is performed under the pressurized state and the depressurized state even after the replacement, and the discharge is performed when the inside of the discharge pipe and the material line connection pipe are in the depressurized state. A method for supplying a liquid material, characterized in that an opening / closing valve of the pipe is opened to fill the inside of the material line connection pipe with a liquid material.