JPWO2018110649A1 - Liquid material supply apparatus, liquid material supply method, liquid supply pipe purging method, and material gas supply system - Google Patents

Abstract

In order to provide a liquid material supply device capable of supplying liquid material at a lower pressure than before while allowing the liquid material to be raised above a desired height, a storage container for storing the liquid material, and the storage A lead-out pipe through which liquid material is led out from the container, a temporary stay part connected to the lead-out pipe and temporarily retaining a predetermined amount of liquid material led out from the storage container, and a temporary stay in the temporary stay part A pressure feeding mechanism configured to bring a gas into contact with the liquid material, and push the gas upward to transport it.

Description

  The present invention relates to a liquid material supply apparatus that supplies a liquid material used in semiconductor manufacturing or the like to a vaporizer or the like.

  In a semiconductor manufacturing process, a liquid material supply device is used to supply a liquid material to a vaporizer such as a bubbler. For example, as shown in Patent Document 1, a carrier gas is introduced from a lead-in pipe into a tank in which the liquid material is stored to pressurize the liquid surface of the liquid material, thereby pumping the liquid material from a lead-out pipe, and Liquid material is supplied to the vessel.

  By the way, it is necessary to avoid interference between pipes connecting liquid material supply devices and vaporizers installed near the floor with other equipment in the factory and pipes connecting them. For this reason, such a pipe can be extended from the connection source liquid material supply device in the vertical direction first and then horizontally in the ceiling, and when reaching the connection destination vaporizer, it can be lowered and connected in the vertical direction. Has been done.

  Furthermore, since the height from the floor to the ceiling is, for example, about 10 m, the liquid material supply device applies pressure to the liquid material so that the liquid column is formed up to the height of the liquid material.

  However, it is becoming difficult to supply the liquid material in a high pressure state as described above to the vaporizer. This is due to the fact that quartz vaporizers, which have corrosion resistance but are inferior to metal vaporizers, are being used as the applications for vaporizing corrosive liquid materials increase. That is, if a liquid material is supplied at a pressure similar to that of a conventional metal vaporizer, the quartz vaporizer may be damaged.

  Further, when a metal pipe is used as a pipe leading from the storage container to the vaporizer, the corrosive liquid material staying in the pipe is supplied after the liquid material is supplied to the vaporizer through the pipe. If left untreated, the corrosion in the piping proceeds, and there arises a problem that the piping stretched in the factory in a relatively short cycle must be replaced.

Japanese Patent No. 5155895

  The present invention has been made in view of the above-described problems, and provides a liquid material supply apparatus that can supply a liquid material at a lower pressure than before while allowing the liquid material to be raised above a desired height. The purpose is to provide. Another object of the present invention is to extend the life of piping.

  That is, the liquid material supply device according to the present invention is connected to the storage container in which the liquid material is stored, the lead-out pipe from which the liquid material is led out to the outside, and the lead-out pipe. A temporary retention portion where the predetermined amount of the derived liquid material is temporarily retained, and a gas is brought into contact with the liquid material temporarily retained in the temporary retention portion, and the gas is pushed upward and transferred by the gas. And a pressure feeding mechanism.

  Further, the liquid material supply method according to the present invention leads the liquid material stored in the storage container in which the liquid material is stored to the outside of the storage container through the outlet pipe, and is temporarily connected to the outlet pipe. Temporarily retaining a predetermined amount of the liquid material in the staying part, bringing the gas into contact with the liquid material temporarily staying in the temporarily staying part, and pushing up with the gas and transferring the material. Features.

  In such a case, only a predetermined amount of the liquid material in the temporary retention portion is transferred upward by applying pressure with gas, so that, for example, in a conventional pipe from the place where the storage container is located to the ceiling As compared with the case where the liquid material is transferred in a liquid-tight state, the pressure required to pump the liquid material can be reduced.

  For this reason, since a low-pressure liquid material can be supplied to devices with low pressure resistance such as a quartz vaporizer, the possibility of breakage can be greatly reduced.

  Only the minimum amount that must be supplied from the liquid material stored in the storage container to another device such as a vaporizer is retained in the temporary retention portion, and only the liquid material in the temporary retention portion is gasified. In order to be able to pressurize and transfer upward, the apparatus further includes an introduction pipe for introducing a gas into the storage container, and the pressure feeding mechanism uses the gas introduced from the introduction pipe to supply the liquid material in the storage container. A first pressure line for transferring the liquid material from the storage container to the temporary retention portion in a state where the liquid surface is pressurized and the outlet pipe is substantially filled with the liquid material, and the first pressure line A liquid return line for transferring the liquid material in the outlet pipe to the outside of the outlet pipe after the liquid material has been transferred to the temporary retention portion by the liquid, and the liquid material is transferred from the inside of the outlet pipe to the outside of the outlet pipe by the liquid return line. Transferred Wherein as long as the lower end of the liquid surface of the liquid material which accumulated temporarily in the temporary retention section and a second pressure line for transporting it pushes upward pressurized with gas.

  Here, in this specification, the “line” is an assembly of a plurality of fluid devices, and is a concept having a function of flowing a liquid material or gas from one place to another place. The “pipe” is a part of the “line”.

  In order to be able to supply gas directly to the liquid material staying in the temporary staying section, gas for transferring the liquid material temporarily staying in the temporary staying section is supplied into the outlet pipe. What is necessary is just to further have a gas supply pipe.

  The pressure feeding means for transferring the liquid material from the storage container to the temporary staying portion and the pressure feeding means for transferring only the predetermined liquid material staying in the temporary staying portion to the vaporizer or the like can be made common. The gas supply pipe is provided so as to connect between the introduction pipe and the lead-out pipe, and the pressure feeding mechanism includes a first valve provided in the introduction pipe, and a gas supply pipe. And a second flow rate controller provided in the introduction pipe and configured to flow gas at a predetermined flow rate, wherein the control unit closes the first valve and opens the second valve. Thus, it is only necessary that the gas is supplied from the gas supply pipe into the outlet pipe.

  In order to allow a predetermined amount of liquid material to be temporarily retained with a simple structure and to facilitate introduction and transfer of gas to the lower end side of the predetermined liquid material, the temporary retention portion includes the liquid material. What is necessary is just to be provided with the residence chamber which retains temporarily, and the lower end side valve | bulb provided in the lower end part of the said residence chamber.

  A material gas supply system comprising: a liquid material supply device according to the present invention; and a liquid material supply pipe connecting between one or a plurality of vaporizers for vaporizing the liquid material and the temporary retention part. If so, the liquid material can be supplied to the vaporizer at a low pressure, so that the liquid material is corrosive, and the vaporizer is made of quartz and has a low pressure strength. it can.

  In order to allow the remaining liquid material or the like to be purged even in a pipe to which a plurality of vaporizers are connected, the liquid material supply pipe has a main pipe whose one end is connected to the temporary retention part, One or a plurality of branch pipes branching from the main pipe and joining again to the main pipe may be provided, and a plurality of vaporizers may be connected to the branch pipe.

  The present invention is also a liquid material supply device that supplies a liquid material to a supply destination, a storage container that stores the liquid material, and a liquid supply pipe that supplies the liquid material from the storage container to the supply destination. And a purge mechanism for purging the liquid material staying in the liquid supply pipe after the liquid material is supplied from the storage container to the supply destination.

  With such a configuration, after the liquid material is supplied from the storage container to the supply destination via the liquid supply pipe, the liquid material staying in the liquid supply pipe can be purged. Accordingly, by performing the purge operation, it is possible to prevent the liquid material from staying in the liquid supply pipe for a long period of time, thereby extending the life of the liquid supply pipe.

  Further, in the liquid material supply apparatus, the purge mechanism is retained in the liquid supply pipe by the drain line for draining the liquid material staying in the liquid supply pipe to the outside of the liquid supply pipe, and the drain line. And a vent line for venting gas into the liquid supply pipe after draining the liquid material to be discharged.

  In such a case, after the liquid material staying in the liquid supply pipe is drained to the outside, the gas is allowed to pass through the liquid supply pipe, so that the liquid material remaining in the liquid supply pipe is vaporized by the gas. be able to. Thereby, corrosion due to droplets adhering in the liquid supply pipe can be prevented, and the life of the liquid supply pipe can be extended.

  The liquid material supply apparatus further includes a purge completion condition storage unit that stores the purge completion condition, and a purge completion determination unit that determines that the purge is completed when the completion condition is satisfied. It may be.

  If this is the case, the conditions under which the liquid material is purged from the liquid supply pipe to an acceptable level by testing or the like are specified in advance, and the specified conditions are stored in the purge completion condition storage unit as completion conditions. Insufficient purge can be prevented. Further, the minimum purge can be performed in the shortest time, and the work efficiency is improved.

  In this case, the purge completion condition storage unit stores a predetermined ventilation condition in the ventilation line as the completion condition, and the purge completion determination unit determines that the ventilation condition in the ventilation line satisfies the predetermined ventilation condition. In this case, it may be determined that the purge is completed.

  Further, the apparatus further comprises a measuring device that measures a value that varies with vaporization of the liquid material remaining in the liquid supply pipe after the gas is passed through the liquid supply pipe by the ventilation line, and the purge completion condition storage is stored. Unit stores a threshold value of the measurement value measured by the measurement device as the completion condition, and the purge completion determination unit completes the purge when the measurement value measured by the measurement device reaches the threshold value You may comprise so that it may judge. In this case, the purge mechanism further includes a decompression line that decompresses the inside of the liquid supply pipe after the gas is passed through the liquid supply pipe by the ventilation line, and the measurement device is decompressed by the decompression line. You may comprise so that the pressure in a liquid supply pipe | tube may be measured.

  You may comprise the said measuring apparatus so that the pressure in the said liquid supply pipe decompressed by the said pressure reduction line may be measured.

  When a pressure sensor is used as the measuring device, a plurality of pressure sensors each having a different measurement range may be provided. In this way, when measuring the pressure in the liquid supply pipe decompressed by the decompression line by the measuring device, it is possible to prevent the pressure sensor from being damaged by using the pressure sensor in order from the one having the higher measurement range. More specifically, when an attempt is made to measure the pressure in the liquid supply pipe decompressed by the decompression line in a state where the ventilation by the ventilation line is insufficient, the rise in pressure in the liquid supply pipe is measured by the vaporized liquid material. For this reason, if the pressure in the liquid supply pipe is measured with a low measurement range, for example, a vacuum gauge, the measurement range is exceeded and the vacuum gauge is damaged. For this reason, if a pressure sensor with a relatively high measurement range is first measured to grasp a certain pressure and then measured with a pressure sensor in a range that matches the pressure, damage to the pressure sensor can be prevented.

  The drainage line supplies gas into the liquid supply pipe from the side opposite to the storage container side with respect to the supply destination of the liquid supply pipe, and the liquid material staying in the liquid supply pipe is supplied to the storage container. It may be configured to be pumped in.

  With such a configuration, the liquid material staying in the liquid supply pipe can be returned to the storage container and reused.

  The material gas supply system according to the present invention is a liquid material supply apparatus having the purge mechanism, and a supply destination to which the liquid material is supplied by the liquid material supply apparatus, and the liquid material is vaporized to form a material gas. And at least one carburetor for generating the gas.

  Further, the liquid material pipe purging method according to the present invention includes a liquid supply pipe for purging the liquid material staying in the liquid supply pipe after the liquid material stored in the storage container is supplied to the supply destination via the liquid supply pipe. The purging method comprises: draining the liquid material staying in the liquid supply pipe; and venting gas into the liquid supply pipe after the drainage.

  Thus, according to the liquid material supply apparatus according to the present invention, the liquid material supply device according to the present invention is configured to transfer a predetermined amount of the liquid material in the temporary retention portion upward by gas, so that the weight of the liquid material itself is reduced. The pressure required for the rise can be reduced. Accordingly, it is possible to supply a low-pressure liquid material to a device such as a vaporizer. Moreover, since the liquid material supply apparatus according to the present invention includes the purge mechanism, the liquid material can be purged from the liquid supply pipe after the liquid material is supplied from the storage container to the supply destination. Thereby, it is possible to prevent the liquid material from staying in the liquid supply pipe for a long time.

The schematic diagram which shows the liquid material supply apparatus which concerns on Embodiment 1 of this invention, and a material gas supply system. The schematic diagram which shows operation | movement of the liquid material supply apparatus in the embodiment. The schematic diagram shown about the purge operation | movement in the material gas supply system in the embodiment. The schematic diagram which shows the structural example of the pumping mechanism in another embodiment of this invention. The schematic diagram shown about the purge operation | movement in the material gas supply system which concerns on Embodiment 2 of this invention. The schematic diagram shown about the purge operation | movement in the material gas supply system which concerns on the same embodiment. The schematic diagram shown about the purge operation | movement in the material gas supply system which concerns on the same embodiment.

200 ... Material gas supply system 100 ... Liquid material supply device 1 ... Storage container 2 ... Temporary residence chamber 3 ... Vaporizer 4 ... Pressure feed mechanism 41 ... First pressurization line 4R: Liquid return line 42: Second pressurization line C: Control unit C1: Purge completion condition storage unit C2: Purge completion determination unit C3: Drainage completion determination unit P1 ..Introducing pipe P2... Gas supply pipe P3... Outlet pipe V1... First valve V2.

  A liquid material supply apparatus 100 and a material gas supply system 200 according to an embodiment of the present invention will be described with reference to the drawings. <Embodiment 1> The material gas supply system 200 of this embodiment is used for supplying various material gases to, for example, a film forming chamber in a semiconductor manufacturing process. In this embodiment, for example, corrosive POCl3, HF, TEOS, or other gas is supplied from a plurality of locations in the chamber.

  As shown in FIG. 1, the material gas supply system 200 includes a plurality of vaporizers 3 (hereinafter also referred to as “supply destinations”) that generate a material gas that is vaporized and introduced into a chamber. And a liquid material supply device 100 for appropriately supplying a liquid material as a raw material to the container 3. In addition, although each vaporizer 3 and the component gas introduction port of the film forming chamber are connected by piping, in FIG. 1, the notation of such piping and the film forming chamber is saved for the sake of simplicity. . The plurality of vaporizers 3 and the liquid material supply device 100 are installed at a height of, for example, about 1 to 2 m from the floor in the factory so that an operator can easily perform adjustment work. On the other hand, a part of the pipes connecting the plurality of vaporizers 3 and the liquid material supply device 100 covers a ceiling about 10 m away from the floor surface in the factory. That is, the pipe first extends in the vertical direction from the liquid material supply device 100 as the connection source, extends in the horizontal direction when reaching the ceiling, and is lowered again in the vertical direction in the vicinity of the plurality of vaporizers 3 as the connection destinations. Each vaporizer 3 is connected. In this way, physical interference between devices other than the liquid material supply device 100 and the plurality of vaporizers 3 and other pipes is less likely to occur.

  The plurality of vaporizers 3 are accommodated in a plurality of racks installed on a floor surface in a factory, and are stacked in the vertical direction. A plurality of vaporizers 3 at each stage share one pipe and are attached to form a vaporizer group. Each vaporizer 3 is further connected to a plurality of branch pipes M2 branched from the main pipe M1. One end of the main pipe M1 is connected to the top surface portion of the liquid material supply apparatus 100, passes through the vicinity of the ceiling of the factory, and is once lowered to the vicinity of the vaporizer 3 arranged at the lowest stage. The main pipe M1 extends upward again from its lowermost stage to the uppermost stage, and the other end is connected to the purge gas introduction pipe of the liquid material supply apparatus 100 through the ceiling. The branch pipe M2 is a loop-like pipe that branches from the main pipe M1 and joins the main pipe M1 again. Each branch pipe M2 and each carburetor group are provided in parallel in the vertical direction. Both ends of the main pipe M1 and the branch pipe M2 are connected by a three-way valve 3V, and each vaporizer 3 is also connected by a three-way valve 3V to each branch pipe M2. That is, by controlling the opening and closing of the three-way valve 3V provided on the main pipe M1, the liquid material and the purge gas can be supplied to the other branch pipe M2 so as not to be introduced into the branch pipe M2. . Further, by controlling the opening and closing of each three-way valve 3V provided in the branch pipe M2, the liquid material is supplied to only a part of the carburetor group, or all the carburetors 3 are closed and the branch is closed. It is also possible to allow the purge gas to pass through the tube M2. The vaporizer 3 is made of quartz having corrosion resistance so that a corrosive liquid material can be handled.

  The liquid material supply apparatus 100 supplies the liquid material to each vaporizer 3 by applying a pressure to the liquid material with a gas such as nitrogen (hereinafter also referred to as a pressurized gas). The liquid material supply apparatus 100 includes a storage container 1 that stores liquid material, a pressure feeding mechanism 4 that transfers the liquid material stored in the storage container 1 to the vaporizer 3, and various surplus gases and liquids. An exhaust mechanism (hereinafter also referred to as a “purge mechanism”) for purging the liquid material in the pipe to the outside when switching materials is provided.

  For the storage container 1, an introduction pipe P <b> 1 for introducing a pressurized gas into an upper portion of the storage container 1 that is not filled with the liquid material, and one end inside the liquid material in the storage container 1. And a lead-out pipe P3 for leading the pressurized liquid material out of the storage container 1 is provided.

  The introduction pipe P1 is connected to a nitrogen gas source, and a flow rate controller MFC (mass flow controller) for controlling the flow rate of the flowing gas is provided on the introduction pipe P1.

  A temporary retention portion 2 for temporarily retaining a predetermined amount of the liquid material derived from the storage container 1 is connected to the outlet pipe P3. The temporary staying portion 2 includes a temporary staying chamber TV formed by using a volume in a pipe connected to the upper side in the vertical direction of the outlet pipe P3, and a lower end side valve provided at the lower end of the temporary staying chamber TV. And an upper end side valve provided on the upper end side of the temporary residence chamber TV. That is, an amount of liquid material that can be accommodated in a volume defined between the lower end side valve and the upper end side valve is temporarily retained, and can be supplied to the vaporizer 3 thereafter. Here, the volume of the temporary residence chamber TV is set to an amount necessary to supply the vaporizer 3.

  Further, in the vicinity of the storage container 1, between the introduction pipe P1 and the lead-out pipe P3, the pressurized gas flowing through the introduction pipe P1 bypasses the storage container 1 and temporarily stays in the temporary retention part 2. A gas supply pipe P2 for directly reaching the liquid material is provided.

  The pumping mechanism 4 temporarily retains a part of the liquid material led out from the storage container 1 in the temporary retention part 2 and then adds the lower end side of the liquid material retained in the temporary retention part 2. It is configured to be pressed with pressurized gas, transferred upward, and supplied to each vaporizer 3. That is, the upstream side and the downstream side of the liquid material delivered from the liquid material supply apparatus 100 to the vaporizer 3 are occupied by gas, and the pressure of the downstream gas is higher than that of the upstream side. It is constituted as follows.

  More specifically, the pressure feeding mechanism 4 includes a first pressure line 41, a liquid return line 4R, and a second pressure line 42 so that movement of at least three kinds of liquid materials can be realized. . The pumping mechanism 4 operates the first pressurization line 41, the liquid return line 4R, and the second pressurization line 42 in this order to ceiling only the liquid material temporarily retained in the temporary retention unit 2. After being lifted to the vicinity, it is pumped to the vaporizer 3. This pressure feeding mechanism 4 includes a plurality of valves provided on the pipes constituting each line and a control unit C that controls the opening and closing of each valve. Realize one action. In the present embodiment, in the introduction pipe P1, the first valve V1 provided near the outside of the storage container 1, the second valve V2 provided in the gas supply pipe P2, and the storage container 1 in the outlet pipe P3. The third valve V3 provided in the vicinity of the outside, the lower end side valve VL forming the temporary retention part 2, and the upper end side valve VU are opened and closed according to a sequence preset by the control part C. .

  The first pressurization line 41 pressurizes the liquid surface of the liquid material in the storage container 1 with the pressurized gas introduced from the introduction pipe P1, and the lead-out pipe P3 is substantially filled with the liquid material. In this state, the liquid material is transferred from the storage container 1 to the temporary retention part 2. In the present embodiment, the first pressurization line 41 is configured so that the liquid material moves in this order through the introduction pipe P1, the storage container 1, the outlet pipe P3, and the temporary retention part 2.

  The liquid return line 4R is for transferring the liquid material in the outlet pipe P3 to the outside of the outlet pipe P3 after the liquid material has been transferred to the temporary retention part 2 by the first pressure line 41. In the present embodiment, the liquid material in the lead-out pipe P3 is changed from the state in which the liquid material is filled in the lead-out pipe P3 at least in a part of the temporary retention portion 2 by the first pressure line 41. The part is returned into the storage container 1.

  The second pressurization line 42 has a lower end side of the liquid material temporarily retained in the temporary retention portion 2 after the liquid material is transferred from the outlet pipe P3 to the outside of the outlet pipe P3 by the liquid return line 4R. The liquid surface is pressurized with gas and pushed up to be transferred. In the present embodiment, the pressurized gas flowing in the introduction pipe P1 is introduced from the gas introduction pipe P1 into the outlet pipe P3 without passing through the storage container 1.

  The exhaust mechanism includes a purge gas supply pipe P4 branched from the introduction pipe P1, the main pipe M1, the branch pipe M2, the temporary retention portion 2, the outlet pipe P3, the gas introduction pipe P1, the introduction pipe P1, the The gas flows in the order of the exhaust pipe P6 branched from the introduction pipe P1 and provided with the suction pump PP, and discharges liquid material, surplus gas, and the like to the outside. The purge gas supply pipe P4 is provided with a fourth valve V4 that is closed when the liquid material is delivered, and a fifth valve V5 is provided in the vicinity of the branch point between the introduction pipe P1 and the exhaust pipe P6. It is. Further, the exhaust pipe P6 is provided with a sixth valve V6 for controlling on / off of exhaust.

  The control unit C is, for example, a computer including a CPU, a memory, input / output means, an A / D / D / A converter, etc., and based on a control program stored in the memory, the flow rate controller MFC, Each valve is controlled to control the pumping of the liquid material and the purge in the pipe.

  Next, the operation of the liquid material supply apparatus 100 when the liquid material is pumped to each vaporizer 3 will be described with reference to FIG. In FIG. 2, the mechanism and piping related to the pressure feeding mechanism 4 in FIG. 1 are simplified.

  As shown in FIG. 2A, in the initial state, the first to fifth valves V5, the lower end side valve VL that forms the temporary staying portion 2, and the upper end side valve VU are closed. From this state, as shown in FIG. 2 (b), a fifth valve V5, a first valve V1, and a first valve are used to introduce pressurized gas into the storage container 1 in which the liquid material is stored by the introduction pipe P1. The 3 valve V3 and the lower end side valve VL are opened, and the first pressure line 41 is first formed.

  As shown in FIG. 2 (b), a pressurized gas having a predetermined flow rate is introduced from the flow rate controller MFC into the storage container 1, so that the liquid level in the storage container 1 is pressed downward. A liquid column of liquid material is formed from the lead-out pipe P3 into the temporary staying portion 2. In other words, the first pressurization line 41 is used to pump the liquid material filled in the pipe up to the vicinity of the storage container 1.

  From this state, as shown in FIG. 2 (c), the fifth valve V5 is closed to stop the introduction of the pressurized gas, and the lower end side valve VL is closed to enter the temporary residence chamber TV by a predetermined amount. Liquid material is trapped. At this time, the sixth valve V6 is opened, and the gas in the introduction pipe P1 in the vicinity of the storage container 1 is exhausted to the outside through the exhaust pipe P6 and returned to a low pressure state.

  Next, as shown in FIG. 2 (d), the fifth valve V5 on the introduction pipe P1 and the second valve V2 on the gas introduction pipe P1 are opened, and pressurized gas is supplied to the outlet pipe. In the P3, it is introduced below the lower end side valve VL. At this time, the liquid material in the outlet pipe P3 is partially returned to the storage container 1 by the pressure of the pressurized gas.

  Thereafter, as shown in FIG. 2 (e), the first valve V1 of the introduction pipe P1 and the sixth valve V6 of the exhaust pipe P6 are opened, and the inside of the storage container 1 and the inside of the outlet pipe P3 are in the atmosphere. Opened to a low pressure state.

  Further, as shown in FIG. 2 (f), the first valve V1 of the introduction pipe P1, the third valve V3 of the outlet pipe P3, and the two sixth valves V6 of the exhaust pipe P6 are closed, respectively. When the valve is opened, pressurized gas is supplied from the flow rate controller MFC to the space above the third valve V3 in the outlet pipe P3 via the gas supply pipe P2, and the temporary residence chamber The lower end of the liquid material temporarily staying in the TV is pressed upward. At this time, the flow rate and flow rate realized by the flow rate controller MFC are set so that the liquid material temporarily retained in the temporary retention portion 2 proceeds in a state where the pipe is sealed without a gap.

  As a result, as shown in FIG. 2 (g), a predetermined amount of the liquid material in the temporary retention portion 2 is pumped to the vaporizer 3 with the upstream side and the downstream side sandwiched between gases.

  As described above, according to the liquid material supply apparatus 100 of the present embodiment, the liquid material separated by a predetermined amount in the temporary retention unit 2 is pressurized with pressurized gas to the height of the factory ceiling. For example, the weight of the liquid material as compared with the case where the liquid material is transferred in a state where all of the pipes from the place where the storage container 1 is located to the ceiling is filled with the liquid material as in the prior art. Can reduce the pressure required for pumping.

  For this reason, even if the vaporizer 3 is made of quartz corresponding to a corrosive liquid material, the pressure applied to the vaporizer 3 can be made smaller than before, and the possibility of breakage can be greatly reduced.

  Further, the first pressurization line 41, the liquid return line 4R, and the second pressurization line 42 as in the present embodiment can be switched by switching the opening and closing of each valve, so that one nitrogen source can be used. Two types of pressurization methods can be realized. For this reason, the structure as the said liquid material supply apparatus 100 can be simplified.

  Next, the operation at the time of purging will be described.

  In the liquid material supply apparatus 100, the control unit C closes the first valve V1 of the introduction pipe P1 and the third valve V3 of the outlet pipe P3 so that gas does not pass into the storage container 1. To. On the other hand, the other valves are opened, and the three-way valve 3V of each vaporizer 3 is closed so that the pressurized gas does not flow into the vaporizer 3, and the pressurized gas enters the branch pipe M2. Open for passage. Further, the three-way valve 3V provided between the main pipe M1 and the branch pipe M2 is opened so that pressurized gas can pass between the main pipe M1 and the branch pipe M2.

  When the opening / closing of each valve is controlled in this way, as shown in FIG. 3, the nitrogen gas supplied from the flow rate controller MFC in the introduction pipe P1 first flows through the purge gas supply pipe P4 as the purge gas and flows into the main pipe M1. Will flow into the other end side, and will flow in a folded manner while descending step by step from the uppermost branch pipe M2. The branch pipe M2 is connected to the main pipe M1 in a U-shape, and is configured so that there is no dead end. Therefore, the purge gas does not stay in the branch pipe M2, and again enters the main pipe M1. Return to. That is, the residue remaining in the branch pipe M2 can be discharged to the liquid material supply apparatus 100 side without flowing to the downstream film forming chamber or the like. For this reason, the film formation chamber is not contaminated by impurities or the like by the purge, and it is possible to change the liquid material or the like in a shorter time. The purge gas that has passed through all the branch pipes M2 passes from the one end side of the main pipe M1 through the temporary retention part 2, the lead-out pipe P3, the gas supply pipe P2, and the introduction pipe P1 in this order. It is discharged from the pipe P6 to the outside.

  <Embodiment 2> This embodiment is a modification of the purge mechanism in the material gas supply system 200 according to Embodiment 1, and has the same configuration as the material gas supply system 200 according to Embodiment 1. However, in the present embodiment, unlike the first embodiment, the liquid material supply device 100 includes the main pipe M1 and each branch pipe M2. Further, in the present embodiment, the piping for supplying the liquid material from the storage container 1 to the vaporizer 3, specifically, the outlet pipe P3, the main pipe M1, and each branch pipe M2 are collectively expressed as a liquid supply pipe P0. . The purge mechanism according to the present embodiment is particularly effective when pipes that are easily corroded, such as metal pipes, are used as the pipes.

  In addition to the configuration of the liquid material supply apparatus 100 according to the first embodiment, the liquid material supply apparatus 100 according to the present embodiment includes a purge mechanism 5 and a measurement apparatus for measuring the pressure in the liquid supply pipe P0. And a purge completion condition storage unit C1 that stores a purge completion condition by the purge mechanism 5 and a purge completion determination unit C2 that determines that the purge is completed when the completion condition is satisfied. Hereinafter, these configurations will be described in detail.

  The purge mechanism 5 stays in the liquid supply pipe P0 without being supplied to the vaporizer 3 after supplying the liquid material from the storage container 1 to the vaporizer 3 via the liquid supply pipe P0 by the pressure feeding mechanism 4. The liquid material is purged out of the liquid supply pipe P0.

  Specifically, the purge mechanism 5 includes a drain line 51, a vent line 52, and a decompression line 53 so that at least three operations for purging the liquid material from the liquid supply pipe P0 can be realized. Yes. Then, the purge mechanism 5 purges the liquid material staying in the liquid supply pipe P0 by operating the drain line 51, the vent line 52, and the decompression line 53 in this order.

  The purge mechanism 5 includes a plurality of valves provided on the pipes that constitute each line, and a control unit C ′ that controls the opening and closing of each valve. And three operation | movement is implement | achieved by changing the combination of opening and closing of each valve | bulb by control part C '. Specifically, in the present embodiment, the first valve V1, the fifth valve V5, each three-way valve 3V, and each vaporizer 3 connected to the branch pipe M2 are provided in the liquid supply pipe P0. A three-way valve 3V 'provided in the gas supply pipe P2, a second valve V2 provided in the gas supply pipe P2, a third valve V3 provided in the lead-out pipe P3, a lower end side valve VL, an upper end side valve VU, and a purge gas supply A fourth valve V4 provided in the pipe P4, a sixth valve V6 installed in a pipe opened to the atmosphere of the exhaust pipe P6, and a sixth valve arranged in a pipe connected to the suction pump PP of the exhaust pipe P6 V6 ′ is opened and closed according to a sequence preset by the control unit C ′.

  The drain line 51 introduces the gas (gas) supplied from the purge gas supply pipe P4 into the liquid supply pipe P0, pumps the liquid material staying in the liquid supply pipe P0, and drains it into the storage container 1. To do. Accordingly, in the present embodiment, the purge gas supply pipe P4, the liquid supply pipe P0, the storage container 1, and the exhaust pipe P6 are configured to communicate with each other.

  The ventilation line 52 introduces the gas (gas) supplied from the purge gas supply pipe P4 again into the liquid supply pipe P0 drained by the drain line 51, and vaporizes the liquid material remaining in the liquid supply pipe P0. In this state, the liquid material supply apparatus 100 is exhausted to the outside. Therefore, in this embodiment, the purge gas supply pipe P4, the liquid supply pipe P0, the gas supply pipe P2, and the exhaust pipe P6 are configured to communicate with each other.

  The decompression line 53 is for decompressing the inside of the liquid supply pipe P0 vented by the vent line 51. Therefore, in this embodiment, the purge gas supply pipe P4, the liquid supply pipe P0, the gas supply pipe P2, and the exhaust pipe P6 extending from the closed fourth valve V4 are configured to communicate with each other. P2 communicates with a pipe connected to the suction pump PP.

  The control unit C ′ is a computer including, for example, a CPU, a memory, input / output means, an A / D / D / A converter, and the like, and based on a control program stored in the memory, a flow rate controller MFC, The purge in the piping is controlled by controlling each valve, the measuring device PS, and the like.

  The measuring device PS includes two pressure sensors PS1 and PS2 having different measurable measurement ranges, and each pressure sensor PS1 and PS2 is connected to an exhaust pipe P6. One of the two pressure sensors PS1, PS2 is a vacuum gauge.

  The purge completion condition storage unit C1 stores a purge completion condition by the purge mechanism 5 and is provided, for example, in a part of a memory provided in the control unit C ′. As the completion condition, a threshold value of the pressure value measured by the measuring device PS is stored. More specifically, in a state where the inside of the liquid supply pipe P0 is not sufficiently purged, the liquid material remaining in the liquid supply pipe P0 is vaporized, and the pressure value measured by the measuring device PS increases. Therefore, in a state where the inside of the liquid supply pipe P0 is purged to an acceptable level, the pressure value measured by the measuring device is set as a threshold value and set as a completion condition.

  The purge completion determination unit C2 measures the pressure in the liquid supply pipe P0 depressurized by the depressurization line 53 by the measuring device PS, and the pressure value becomes equal to or less than the threshold value stored in the purge completion condition storage unit C1. In addition, it is determined that the purge is completed, and is provided in the control unit C ′, for example. When the purge completion determination unit determines that the purge is completed, the purge operation by the purge mechanism 5 is stopped.

  Next, the purge operation of the liquid material supply apparatus 100 according to the present embodiment will be described with reference to FIGS. 5 to 7, white valves indicate an open state, and black valves indicate a closed state.

  For example, after a liquid material is supplied to the vaporizer 3 connected to the lowermost branch pipe M2 by the pressure feeding mechanism 4, when a purge start signal is input to the control unit C ′, the control unit C ′ As shown in FIG. 5, the first valve V1, the third valve V3, the fourth valve V4, the lower end side valve VL, the upper end side valve VU, and the sixth valve V6 are opened and the second valve V2 is opened. The fifth valve V5 and the sixth valve V6 ′ are closed. Further, each three-way valve 3V and each three-way valve 3V ′ are controlled so that the main pipe M1 of the liquid supply pipe P0 communicates with only the lowermost branch pipe M2. Thereby, the drainage line 51 is formed. Then, the liquid material staying in the liquid supply pipe P 0 is pumped by the gas supplied from the purge gas supply pipe P 4 and discharged into the storage container 1.

  The liquid material in the storage container 1 is shaken while the liquid is being drained into the storage container 1, and when the drainage is completed in the storage container 1, the shake that has occurred in the storage container 1 is subsided. Using this, when a load cell is installed in the storage container 1 and the measured value by the load cell is stabilized with respect to the control unit C ′, it is determined that the drainage of the liquid material from the liquid supply pipe P0 to the storage container 1 is completed. A drainage completion determination unit C3 is provided to determine whether the drainage is completed.

  Next, when the drainage completion determination unit C3 determines that the drainage is completed, the control unit C ′ starts the second valve from the state where the drainage line 51 is formed as shown in FIG. V2 is opened, and the first valve V1 and the third valve V3 are closed. Thereby, the ventilation line 52 is formed. The gas supplied from the purge gas supply pipe P4 passes through the liquid supply pipe P0. As a result, the liquid material remaining in the liquid supply pipe P0 is vaporized and exhausted to the outside of the liquid material supply apparatus 100.

  The aeration condition by the aeration line 52, specifically, the flow rate of gas flowing to the liquid supply pipe P0, the aeration time, the aeration frequency, etc. are set in advance in the memory of the control unit C ′. According to the venting conditions, the venting line 52 vents the liquid supply pipe P0.

  Next, when the ventilation by the ventilation line 52 is completed, the control unit C ′ opens the sixth valve V6 ′ and the fourth valve V4 from the state where the ventilation line 52 is formed, as shown in FIG. And the sixth valve V6 is closed. Thereby, the decompression line 53 is formed. The inside of the liquid supply pipe P0 is depressurized by the intake pump PP.

  Note that the decompression condition by the decompression line 53, specifically, the decompression time and the like are preset in the memory of the control unit C ′, and the decompression to the liquid supply pipe P0 by the decompression line 53 according to the set decompression condition. Is implemented.

  Next, when the decompression by the decompression line 53 is completed, the control unit C ′ closes the sixth valve V6 ′. As a result, the upstream side and the downstream side of the liquid supply pipe P0 are closed.

  Next, the purge completion determination unit C2 acquires a pressure value from the pressure sensor PS1 (sensor having a high measurement range), and if the pressure value is not a value that can be measured by the pressure sensor PS2 (sensor having a low measurement range). Then, ventilation through the ventilation line 52 is started again. On the other hand, when the value can be measured by the pressure sensor PS2, the measurement by the pressure sensor PS2 is started. Subsequently, the purge completion determination unit C2 acquires the pressure value from the pressure sensor PS2, and determines that the barge operation has been completed when the pressure value is equal to or less than the threshold value stored in the purge completion condition storage unit C1. Then, the purge operation is finished. On the other hand, when the threshold value stored in the purge completion condition storage unit C1 is exceeded, the ventilation through the ventilation line 52 is started again.

  Thereafter, until the purge completion determination unit C2 determines that the purge operation has been completed, the ventilation by the ventilation line 52, the decompression by the decompression line 53, and the measurement by the measuring device are repeatedly performed.

  As the completion condition stored in the purge completion condition storage unit C1, for example, a ventilation condition by a ventilation line necessary for purging the liquid material in the liquid supply pipe P0 to an acceptable level is measured in advance by a test or the like. The predetermined ventilation condition may be set as the completion condition. In this case, it is not necessary to install a measuring device. Further, when the ventilation by the ventilation line 52 is performed, the vaporization of the liquid material in the liquid supply pipe P0 is reduced, and the concentration of the material gas in the liquid supply pipe P0 is lowered. Completion conditions may be set based on the material gas concentration in P0. In this case, a concentration sensor may be installed as a measuring device instead of a pressure sensor.

  Further, the drainage completion determination unit C3 may determine based on the flow rate value measured by the flow rate sensor of the flow rate control device MFC. Specifically, when the liquid material is drained by the drain line 51, while the liquid material stays in the liquid supply pipe P0, the liquid material is pumped by the gas derived from the flow control device MFC. The measured flow rate measured by the flow sensor of the device MFC is lower than the set flow rate. On the other hand, when the liquid material in the liquid supply pipe P0 is discharged into the storage container 1, the measured flow rate measured by the flow rate sensor of the flow rate control device MFC approaches the set flow rate. By using this, when the measured flow rate of the flow rate sensor of the flow rate control device MFC approaches the set flow rate within a predetermined range, it is determined that the drainage of the liquid material from the liquid supply pipe P0 to the storage container 1 is completed. May be.

  Note that the purge mechanism 5 according to the present embodiment is a method other than the pressure feeding mechanism 4 according to the first embodiment, for example, for pumping the liquid material stored in the storage container 1 to the vaporizer 3 by a conventional method. Can be applied.

  <Other Embodiments> In the embodiment, one nitrogen source is used as a pressurized gas and a purge gas, or separate pressurizing methods are realized in the first pressurizing line and the second pressurizing line. However, for example, a plurality of nitrogen sources may be prepared, and the lower part of the liquid material staying in the temporary staying portion may be pressurized with gas and fed as in the above embodiment. More specifically, as shown in FIG. 4, the gas supply pipe is eliminated, and a nitrogen source and a flow rate controller different from those provided in the introduction pipe with respect to the outlet pipe are provided. You may make it guide | lead out the liquid material temporarily retained in the temporary retention part to the vaporizer by attaching the 2nd pressurization piping.

  The temporary retention portion only needs to be connected to the outlet pipe, and does not necessarily have to be disposed above the outlet pipe. For example, the temporary retention portion may be provided at substantially the same height with respect to the storage container. The liquid material supply pipe connected to such a temporary staying part is provided so as to extend upward, for example, and the gas contacts the liquid material in the temporary staying part by a pressure feeding mechanism, and temporarily stays in the gas. The liquid material may be pumped from the section to the liquid material supply pipe and transferred upward. That is, in order to be able to enjoy the effects of the present invention, it is sufficient if the liquid material in the temporary staying part is pressurized and fed from below to above with a gas such as a pressurized gas. . Further, the upper end side valve may be omitted, and the temporary staying portion may be configured by defining the temporary staying chamber in the pipe only by the lower end side valve.

  Further, the pressurized gas is not limited to nitrogen gas, and may be other rare gas, for example. The vaporizer to which the liquid material is supplied by the liquid material supply device according to the present invention is not limited to quartz, but may be made of metal such as stainless steel or resin such as PFA or PTEFE. In addition, the liquid material supply apparatus according to the present invention may be used to supply a predetermined amount of liquid material other than the vaporizer.

  In addition, various modifications and combinations of embodiments may be performed without departing from the spirit of the present invention.

  ADVANTAGE OF THE INVENTION According to this invention, the pressure required for a raise can be reduced by reducing the weight itself of a body material, for example, the liquid material supply apparatus which can supply a low pressure liquid material to apparatuses, such as a vaporizer, can be provided. .

Claims (18)

A storage container in which the liquid material is stored;
A lead-out pipe through which liquid material is led out from the storage container;
A temporary retention part connected to the outlet pipe and temporarily retaining a predetermined amount of liquid material derived from the storage container;
A liquid material supply device comprising: a pressure feeding mechanism configured to bring a gas into contact with the liquid material temporarily retained in the temporary retention portion, and push the gas upward and transport the gas. An introduction pipe for introducing gas into the storage container;
The pressure feeding mechanism is
The liquid material in the storage container is pressurized by the gas introduced from the introduction pipe, and the liquid material is transferred from the storage container to the temporary retention portion in a state where the outlet pipe is substantially filled with the liquid material. A first pressure line for transferring
A liquid return line for transferring the liquid material in the outlet pipe to the outside of the outlet pipe after the liquid material has been transferred to the temporary retention portion by the first pressure line;
After the liquid material is transferred from the outlet pipe to the outside of the outlet pipe by the liquid return line, the liquid surface on the lower end side of the liquid material temporarily retained in the temporary retaining portion is pressurized with gas and pushed upward to be transferred. The liquid material supply device according to claim 1, further comprising a second pressure line.   The liquid material supply apparatus according to claim 1, further comprising a gas supply pipe that supplies a gas for transferring the liquid material temporarily retained in the temporary retention portion into the outlet pipe. The gas supply pipe is provided to connect between the introduction pipe and the outlet pipe;
The pressure feeding mechanism is
A first valve provided in the introduction pipe;
A second valve provided in the gas supply pipe;
A control unit that controls opening and closing of at least the first valve and the second valve;
A flow rate controller for flowing gas at a predetermined flow rate provided in the introduction pipe,
The liquid material supply according to claim 3, wherein the control unit is configured to close the first valve and open the second valve so that gas is supplied from the gas supply pipe into the outlet pipe. apparatus. The temporary retention part is
A retention chamber in which the liquid material is temporarily retained;
The liquid material supply apparatus according to claim 1, further comprising a lower end side valve provided at a lower end portion of the staying chamber. A liquid material supply device according to any one of claims 1 to 5,
A material gas supply system comprising: one or a plurality of vaporizers that vaporize a liquid material; and a liquid material supply pipe that connects between the temporary retention part. Liquid material supply pipe
A main pipe having one end connected to the temporary retention part;
One or a plurality of branch pipes branched from the main pipe and joined to the main pipe again,
The material gas supply system according to claim 6, wherein a plurality of vaporizers are connected to the branch pipe. The liquid material stored in the storage container in which the liquid material is stored is led out of the storage container through the outlet pipe, and a predetermined amount of the liquid material is temporarily retained in the temporary retaining portion connected to the outlet pipe. And
A liquid material supply method comprising: bringing a gas into contact with the liquid material temporarily retained in the temporary retention portion, and pushing the gas upward with the gas and transporting the gas. A liquid material supply device for supplying a liquid material to a supply destination,
A storage container in which the liquid material is stored;
A liquid supply pipe for supplying a liquid material from the storage container to the supply destination;
A liquid material supply apparatus, comprising: a purge mechanism that purges the liquid material staying in the liquid supply pipe after the liquid material is supplied from the storage container to the supply destination. The purge mechanism is
A drainage line for draining the liquid material staying in the liquid supply pipe to the outside of the liquid supply pipe;
The liquid material supply apparatus according to claim 9, further comprising: a ventilation line for allowing gas to flow into the liquid supply pipe after the liquid material staying in the liquid supply pipe is drained by the drainage line. A purge completion condition storage unit for storing the purge completion condition;
The liquid material supply apparatus according to claim 1, further comprising a purge completion determination unit that determines that the purge is completed when the completion condition is satisfied. The purge completion condition storage unit stores a predetermined ventilation condition in the ventilation line as the completion condition,
The liquid material supply apparatus according to claim 11, wherein the purge completion determination unit is configured to determine that the purge is completed when an aeration condition in the aeration line satisfies the predetermined aeration condition. And further comprising a measuring device that measures a value that varies with vaporization of the liquid material remaining in the liquid supply pipe after the gas is passed through the liquid supply pipe by the ventilation line.
The purge completion condition storage unit stores a threshold value of a measurement value measured by the measuring device as the completion condition,
12. The liquid material supply device according to claim 11, wherein the purge completion determination unit is configured to determine that the purge is completed when a measurement value measured by the measurement device reaches the threshold value. The purge mechanism further includes a pressure reducing line that decompresses the liquid supply pipe after the gas is passed through the liquid supply pipe by the ventilation line,
The liquid material supply apparatus according to claim 13, wherein the measurement apparatus is configured to measure a pressure in the liquid supply pipe decompressed by the decompression line. The measuring device includes a plurality of pressure sensors;
The liquid material supply device according to claim 14, wherein each of the plurality of pressure sensors has a different pressure range.   The drain line supplies gas into the liquid supply pipe from the side opposite to the storage container side to the supply destination of the liquid supply pipe, and the liquid material staying in the liquid supply pipe is stored in the storage container. The liquid material supply device according to claim 10, wherein the liquid material supply device is configured to pump. The liquid material supply device according to any one of claims 9 to 16,
A material gas supply system comprising at least one vaporizer that is a supply destination for supplying a liquid material by the liquid material supply device and generates a material gas by vaporizing the liquid material. . A liquid supply pipe purging method for purging the liquid material staying in the liquid supply pipe after supplying the liquid material stored in the storage container to the supply destination via the liquid supply pipe,
Draining the liquid material staying in the liquid supply pipe;
Venting gas into the liquid supply pipe after the drainage, and a method for purging a liquid material pipe.

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