JP2002095955A - Feeding device for liquid material - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a feeding device for a liquid material, in which stability and controllability are good. SOLUTION: A two-valve three-way changeover valve 15 of an integral structure is equipped with both a diaphragm 152A opening/closing the interval of a port P1 and a port P2 and a diaphragm 152B opening/closing the interval of the port P1 and a port P3. The port P1 is provided between the diaphragm 152A and the diaphragm 152B. When the port P1 and the port P2 communicate, a pipeline 21 becomes dead volume. When the port P1 and the port P3 communicate, a pipeline 22 becomes dead volume. Therefor, the dead volume in a transfer line can be reduced by using the two-valve three-way changeover valve 15 for the transfer line of liquid material and generation of a deposit caused by stagnation of the liquid material can be reduced.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

[0001] 1. Field of the Invention [0002] The present invention relates to a liquid material supply device for supplying a liquid material comprising a liquid organic metal or an organic metal solution to a vaporizer used for CVD film formation.

[0002]

2. Description of the Related Art MOCVD (Metal Organic Chemic) is one of the methods for forming a thin film in a semiconductor device manufacturing process.
al Vapor Deposition method, which has been widely used in recent years due to its superior film quality, film forming speed, step coverage, etc. as compared with sputtering or the like. As a CVD gas supply method used in the MOCVD apparatus, there is a bubbling method, a sublimation method, or the like, but a method in which a liquid material obtained by dissolving a liquid organic metal or an organic metal in an organic solvent is vaporized and supplied immediately before a CVD reactor, It is attracting attention as a better method in terms of controllability and stability.

[0003]

However, the liquid material used in the above-mentioned MOCVD is liable to undergo a hydrolysis reaction, and there is a risk that the material may be deteriorated due to, for example, the formation of a precipitate in the liquid. When the precipitates are generated, malfunction of a valve provided in the liquid feed line, generation of a residue in the vaporizer, and clogging due to the generation of the residue are easily caused.
As a result, there has been a problem that the stability and reproducibility of the flow rate are deteriorated, and the residue becomes particles and reaches the CVD reactor, thereby deteriorating the reproducibility of film formation. In addition, THF (tetrahydrofuran) or the like is used as the organic solvent,
This organic solvent has a disadvantage that it is highly corrosive. Further, the gas dissolved in the liquid material is generated again as bubbles in the line, which is likely to cause poor flow rate control of the liquid material.

Conventionally, a mass flow controller in which a mass flow meter and a flow control valve are integrated has been used for controlling the flow rate of a liquid material. However, a mass flow meter, which is a thermal mass flow meter, is easily affected by the ambient temperature. Has properties. Therefore, it is not preferable to install a mass flow controller near a vaporizer that is in a high temperature state. On the other hand, considering the responsiveness of the flow control, it is preferable that the mass flow controller be installed immediately before the vaporizer. As a result, depending on the installation position of the mass flow controller, there is a problem that either the flow rate control accuracy or the responsiveness is sacrificed, or both are under insufficient installation conditions.

An object of the present invention is to provide a liquid material supply apparatus which suppresses generation of residues and bubbles and has good stability and controllability with respect to liquid material supply.

[0006]

FIG. 1 to FIG. 4, FIG. 7, FIG. 9, FIG. 15, FIG. 17, and FIG.
This will be described in association with. (1) When described in association with FIG. 2 and FIG. 7, the invention of claim 1 is a liquid material 4A to 4C made of a liquid organic metal or an organic metal solution contained in material containers 3A to 3C.
Is applied to the liquid material supply device 1 that supplies the liquid material to the vaporizer 2 via the liquid material transfer lines 6A to 6C, and is provided between the first pipe P2 and the second pipe P1, A first valve body 152A for turning on / off the transfer of fluid between the first pipeline P2 and the second pipeline P1, and a first valve 152A provided between the second pipeline P1 and the third pipeline P3. And a second valve element 152B for turning on and off the transfer of fluid between the second pipe line P1 and the third pipe line P3, and a first valve body 152A and a second valve. The two-piece three-way switching valves 15A to 15C having the second conduit P1 provided between the body 152B and the second pipe P1 are disposed at the branch points where the liquid material transfer lines 6A to 6C branch in three directions. Achieves the above object. (2) When described in association with FIG. 2 and FIG. 9, the invention of claim 2 is a material container 3A to accommodate liquid materials 4A to 4C made of a liquid organic metal or an organic metal solution via a gas supply line 5. 3C, and supply the liquid materials 4A-4C by gas pressure to the liquid material transfer lines 6A-6C.
Is applied to the liquid material supply device 1 that supplies the liquid materials 4A to 4C to the vaporizer 2 through the liquid material transfer lines 6A to 6C, and includes a first pipe P11 and a second pipe P12.
Between the first pipe P11 and the second pipe P
1 to turn on and off the transfer of fluid between
12A, a second pipe provided between the first pipe P11 and the third pipe P13 to turn on / off the transfer of fluid between the first pipe P11 and the third pipe P13. 2 valve body 112B
A third pipe provided between the second pipe P12 and the fourth pipe P14 to turn on / off the transfer of fluid between the second pipe P12 and the fourth pipe P14. Of the first valve body 112A and the second valve body 112C.
B, a first pipeline P11 is provided, and the second valve body 1
12B and a third pipe P12 between the third valve body 112C.
Is provided with an integrated three- and four-way switching valve 10A.
It is provided between the liquid material transfer line 6A and the gas supply line 5 and the material container 3A, connects the first pipe P11 and the gas supply line 5, and connects the second pipe P12 and the gas area of the material container 3A. Are connected, the third pipe P13 is connected to the liquid material transfer line 6A, and the fourth pipe P14 is connected to the material container 3.
The above-described object is achieved by connecting the liquid region A and the gas container line 3A and the switching valve 10A integrally with the gas supply line 5 and the liquid material transfer line 6A. (3) When described in association with FIG. 2 and FIG. 17, the invention of claim 2 is a material container 3A to accommodate liquid materials 4A to 4C made of a liquid organic metal or an organic metal solution via a gas supply line 5. 3C to supply liquid materials 4A to 4C by gas pressure to liquid material transfer lines 6A to 6C.
C to supply the liquid material 4A to 4C to the vaporizer 2 through the liquid material transfer lines 6A to 6C. The material containers 3A to 3C Is provided, and a flexible bag 304 or a bellows-like bag 311 accommodated in the casing 303 and accommodating the liquid materials 4A to 4C. When the gas is supplied into the casing 303, The liquid materials 4A to 4C in the bags 304 and 311 are the material containers 3A.
The above-mentioned object is achieved by being sent to liquid material transfer lines 6A to 6C from .about.3C. (4) In the liquid material supply device 1 according to the third aspect, the liquid material 4A to 4C in the bags 304 and 311 is changed based on a pressure change of the gas supplied into the casing 303. Measuring means 301, 30 for measuring liquid volume
2 is provided. (5) When described in association with FIG. 2 and FIG. 18, the invention of claim 5 is a material container 3 </ b> A to 3 </ b> A which stores liquid materials 4 </ b> A to 4 </ b> C made of a liquid organic metal or an organic metal solution via a gas supply line 5. 3C to supply liquid materials 4A to 4C by gas pressure to liquid material transfer lines 6A to 6C.
C, which is applied to a liquid material supply device that supplies the liquid materials 4A to 4C to the vaporizer 2 through the liquid material transfer lines 6A to 6C, and is filled with the liquid materials 4A to 4C.
And a second bellows-shaped bag 322 connected in series in the direction of expansion and contraction of the first bellows-shaped bag 321 to contract the first bellows 321 by gas supply from the gas supply line 5; A first bellows-shaped bag provided at a connection portion between the first bellows-shaped bag 321 and the second bellows-shaped bag 322 and indicating a position of the connection portion; 321 is contracted, and the liquid material 4A in the first bellows-like bag 321 is shrunk.
The above object is achieved by delivering .about.4C to the liquid material transfer line as 6A.about.6C. (6) Explaining in connection with FIG. 2, the invention according to claim 6 is the liquid material supply device 1 according to any one of claims 1 to 5, wherein the inside is depressurized and the liquid material transfer line is provided. A drain tank 13 for storing a waste liquid discharged at the time of liquid replacement of 6A or at the time of pipe line cleaning is connected via a valve 15A immediately before the liquid material transfer line 6A. (7) Explaining in connection with FIG. 2 and FIG. 15, the invention according to claim 7 is the liquid material supply device 1 according to any one of claims 1 to 5, wherein the liquid material transfer line 6A
The presence or absence of the liquid material 4A to 4C in the liquid material 4A
Detecting means 16 and 164 for detecting the presence or absence of air bubbles generated from the liquid material transfer lines 6A to 6C by using the photoelectric sensor 163. (8) Explaining in connection with FIGS. 1 and 3, the invention of claim 8 is a flow control having thermal mass flow meters 8A to 8C utilizing heat dissipation from a heating element and flow control valves 9A to 9C. The material containers 3A to 3A are controlled while controlling the flow rate by the device.
C is applied to the liquid material supply device 1 that supplies the liquid materials 4A to 4C stored in C to the vaporizer 2 through the liquid material transfer lines 6A to 6C, and includes flow meters 8A to 8C and flow control valves 9A to 9C. And the flow meters 8A to 8C are arranged on the material containers 3A to 3C side of the liquid material transfer lines 6A to 6C, and the flow control valves 9A to 9C are connected to the liquid material transfer lines 6A to 6C.
The above object is achieved by disposing the 6C on the carburetor 2 side. (9) According to a ninth aspect of the present invention, in the liquid material supply device 1 according to the seventh aspect, the flow control valves 9A to 9C are provided with a shut-off mechanism capable of shutting off the supply of the liquid materials 4A to 4C. is there. (10) According to a tenth aspect of the present invention, in the liquid material supply apparatus 1 according to any one of the first to ninth aspects, the liquid material supply lines 1 are provided in the liquid material transfer lines 6A to 6C.
PEEK (polyether ether)
ketone), PTFE (polytetrafluoroethylene), P
One using either I (polyimide) or PBI (polybenzimidazole). (11) Explaining in connection with FIG. 2 and FIG. 4, the invention of claim 11 transfers the liquid material 4A stored in the material containers 3A to 3C to the vaporizer 2 via the liquid material transfer lines 6A to 6C. The filter 21 is applied to the liquid material supply device 1 for supplying and provided in the liquid material transfer lines 6A to 6C.
The above-described object is achieved by using a plurality of layers of a first SUS mesh having a small wire diameter and a second SUS mesh having a large wire diameter. (12) According to a twelfth aspect of the present invention, in the liquid material supply device 1 according to the eleventh aspect, instead of the SUS mesh,
This uses a laminate of PTFE meshes.

[0007] In the section of the means for solving the above-mentioned problems, which explains the configuration of the present invention, the drawings of the embodiments of the present invention are used to make the present invention easy to understand. However, the present invention is not limited to the embodiment.

[0008]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to FIGS. FIG. 1 is a diagram showing a schematic configuration of the entire vaporizer. Reference numeral 1 denotes a liquid organic metal, an organic metal solution, or the like (hereinafter, these are referred to as liquid materials).
And a liquid material supply device for supplying the liquid material. The supplied liquid material is vaporized by the vaporizer 2 and provided to the CV provided in the CDV device.
It is supplied to the D reactor. For example, there is an organic metal such as Cu or Ta as a liquid organic metal, and an organic metal solution in which an organic metal such as Ba, Sr, Ti, Pb, or Zr is dissolved in an organic solvent.

The material containers 3A, 3B, 3C provided in the liquid material supply device 1 are filled with liquid materials 4A, 4B, 4C used for MOCVD. For example, BST
When a dielectric film is formed, the raw materials Ba, S
r, Ti dissolved in organic solvent THF is used as liquid material 4
A, 4B, and 4C are used. In addition, the solvent container 3D
Is filled with THF as a solvent 4D. In addition, the containers 3A to 3D are provided according to the number of raw materials,
Not necessarily individual.

A charge gas line 5 and transfer lines 6A to 6D are connected to each of the containers 3A to 3D. When the charge gas is supplied into each of the containers 3A to 3D via the charge gas line 5, gas pressure is applied to the liquid surfaces of the liquid materials 4A to 4C and the solvent 4D filled in each of the containers 3A to 3D, Materials 4A-4C and solvent 4D are extruded into respective transfer lines 6A-6D, respectively. The liquid materials 4A to 4C and the solvent 4D that have been pushed out to the transfer lines 6A to 6D are further transferred to the transfer line 6E by gas pressure, and are mixed in the transfer line 6E.
The carrier gas is supplied to the transfer line 6E from the carrier gas line 7, and the carrier gas, the liquid materials 4A to 4C and the solvent 4D are supplied to the vaporizer 2 in a gas-liquid two-phase flow state. You.

An inert gas such as a nitrogen gas or an argon gas is used as the charge gas and the carrier gas. Further, the liquid material 4A in the transfer lines 6A to 6E.
It is preferable to reduce the amount of 〜4C and the solvent 4D as much as possible. In the present embodiment, 移送 inch piping is used for the transfer lines 6A to 6C.

Each of the transfer lines 6A to 6D has a mass flow meter 8A to 8D and a flow control valve 9 with a shutoff function.
A to 9D are provided. Mass flow meter 8A-8
D monitors the flow rates of the liquid materials 4A to 4C and the solvent 4D while controlling the flow control valves 9A to 9D so that the flow rates of the liquid materials 4A to 4C and the solvent 4D become appropriate. Note that a pump such as a plunger pump may be used instead of the flow control valves 9A to 9D.

FIG. 2 is a diagram showing the liquid material supply device 1 in detail. The liquid material supply device 1 will be described in detail with reference to FIG. In FIG. 2, the material containers 3B, 3C
The configuration of the transfer line for the material container 3A is the same as that of the transfer line for the material container 3A, and is not shown. First, the installation positions of the mass flow meters 8A to 8D and the flow control valves 9A to 9D will be described. As described above, in the conventional apparatus, a mass flow controller in which a mass flow meter and a flow control valve are integrated is used. However, in the liquid material supply apparatus 1 of the present embodiment, each of the transfer lines 6A to 6D is independent. The mass flow meters 8A to 8D and the flow control valves 9A to 9D are provided.

The mass flow meters 8A to 8D are thermal mass flow meters, and utilize the fact that when a fluid is heated, the energy required for a certain temperature rise is proportional to the mass flow rate. The mass flow meters 8A to 8D are provided with a heater for heating the fluid and a pair of thermometers for measuring the temperature difference in the flow direction of the fluid. The amount of heat q of the heater is controlled so that the temperature difference ΔT becomes constant. When the heater is controlled in this manner, the mass flow rate is proportional to the heat quantity q given at that time, so the mass flow rate is obtained from the heat quantity q at that time.

Therefore, in the present embodiment, the mass flow meters 8A to 8D and the flow control valves 9A to 9D are separately and independently provided, and the mass flow meters 8A to 8D are provided in the containers 3A to 3D of the transfer lines 6A to 6D. Installed near,
The flow control valves 9A to 9D were installed at positions near the vaporizer 2 in each of the transfer lines 6A to 6D. With such a configuration, the thermal influence of the vaporizer 2 on the mass flow meters 8A to 8D can be prevented, and the responsiveness can be improved.

FIG. 3 is a view showing the appearance of the flow control valves 9A to 9D provided close to the vaporizer 2. Each of the flow control valves 9A to 9D is connected to ports 91, 92, 93, and 94 provided in the block 90. Block 9
0, a pipe 96 corresponding to the transfer lines 6A to 6E.
A to 96E are respectively formed, and each of the conduits 96A to 96E is formed.
96E has the ports 91 to 94 and port 9 described above.
5, 96 are connected. The ports 95 and 96 connected to the pipe 96E are provided with on-off valves V9 and V6 shown in FIG.

The liquid materials 4A to 4C and the solvent 4D are connected to the respective conduits 96A to 96D through flow control valves 9A to 9D.
Is introduced and mixed in the line 96E. A carrier gas is supplied to the conduit 96E from the port 95, and the conduit 96E
Inside, the mixed liquid of the liquid materials 4A to 4C and the carrier gas are in a gas-liquid two-phase flow state. The liquid material in the gas-liquid two-phase flow state is sent to the vaporizer 2 in FIG. 2 via the on-off valve V6.

The block 90 includes a mass flow meter 8A.
Flow control valves 9A to 9 provided separately from .about.8D
Since only D is connected, the size of the block 90 can be made compact. Further, since the block 90 is provided close to the carburetor 2 and the flow control valves 9A to 9D with the shutoff function are used, the piping volume between the flow control valves 9A to 9D and the carburetor 2 is reduced. Responsiveness of the flow control can be improved. In addition, since the volume of the pipe after mixing the liquid is small, the deterioration of the mixed liquid due to the stagnation of the mixed liquid can be reduced.

Returning to FIG. 2, the material container 3A and the solvent container 3D have a charge gas line 5 and a transfer line 6 respectively.
A and 6D are detachably connected to each other via a connector C. These connectors C and each container 3A,
3D and a three-way four-way switching valve 10A,
10D are provided, and the containers 3A and 3D are attached and detached integrally with the three- and four-way switching valves 10A and 10D.

In FIG. 2, reference numerals 11 and 12 denote transfer lines 6.
This is an auxiliary line for performing vacuum evacuation of A and 6D, gas purging, solvent cleaning, liquid replacement, and the like, and is connected to a drain tank 13 for storing waste liquid from solvent cleaning and liquid replacement. LS1 and LS2 are sensors for detecting the liquid level of the waste liquid in the drain tank 13. Drain tank 13
Is connected to a vacuum exhaust line 14, and the pressure in the drain tank 13 is reduced. The auxiliary line 11 is connected to the transfer lines 6A and 6D via two- and three-way switching valves 15A and 15D of an integral structure. The auxiliary line 11 is provided with a monitoring device 16, which can determine the state of the fluid flowing in the pipe, for example, whether the fluid is a liquid or a gas. In addition, 3 valve 4 way switching valve 10A, 10D, 2 valve 3
Details of the direction switching valves 15A and 15D and the monitoring device 16 will be described later.

The charge gas line 5, transfer lines 6A, 6D, 6E, carrier gas line 7, auxiliary lines 11, 12 and vacuum exhaust line 14 shown in FIG.
1 to V10, respectively, and each open / close valve V
By appropriately switching the opening / closing of 1 to V10 and the switching of the two-valve three-way switching valve 15, the evacuation, gas purging and solvent cleaning described later are performed. Check valves 17A and 17D are provided in the charge gas line 5, and transfer lines 6A and 6D
Are provided with filters 18A and 18D, respectively.

In the liquid material supply device 1 of the present embodiment,
Filter 1 that is less likely to generate air bubbles in order to ensure liquid sending stability
8A and 18D are provided in the transfer lines 6A and 6D, and the dead volume in the piping is reduced as much as possible so that no precipitate is generated in the liquid material. 4A and 4B are diagrams illustrating details of the filter 18A. FIG. 4A is a cross-sectional view of the filter, and FIG. 4B is a diagram qualitatively illustrating flow rate stability. As shown in FIG. 4 (a), a sheet-shaped filter element 21 is disposed substantially at right angles to the liquid feeding direction in the body 20 of the filter 18A provided in the transfer line 6A. Note that the filter 18D has exactly the same structure as the filter 18A.

The filter element 21 is formed by laminating meshes of stainless steel (SUS) wire rods. In the present embodiment, two types of meshes, a thin wire mesh and a thick wire mesh, are laminated. did. As a result, the filter 18A has a lower pressure loss than the conventional sintered filter and has a good rectifying action, and the generation of bubbles is suppressed and the flow rate is stabilized. Further, the strength of the filter element 21 was improved by using not only a mesh having a small wire diameter but also a mesh having a large wire diameter. The filter element 21 is made of PTFE
May be used, and the corrosion resistance is improved as compared with SUS.

FIG. 4B compares the performance of the filter 18A when the filter element 21 is used with that of the conventional sintered filter.
The filter 18A and the mass flow controller are disposed at intervals of 2 (m) in the piping of (2), and the solvent THF is supplied at a flow rate of 0.8 (m).
1 / min) shows the output of the mass flow controller when flowing at 1 / min). The upper part of FIG. 4B shows a case of a conventional sintered filter, and the output fluctuates up and down due to the generation of bubbles. On the other hand, the lower part shows the case of the filter 18A of the present embodiment, and the output does not fluctuate as in the conventional case, and it can be seen that the flow rate is stable.

In particular, when the flow rate is controlled using a mass flow controller, the differential pressure in the mass flow controller must be at least 0.5 (kg / cm ² ).
Since the air bubbles are easily generated in the filter portion, the above-described filter 18A works more effectively.

When supplying the liquid materials 4A to 4C to the vaporizer 2, the opening and closing of each valve is controlled as shown in FIG. In FIG. 5, when the valve is closed, the valve symbol is shown in black so that the open / closed state of the valve can be easily understood.
The flows of the liquid materials 4A to 4C and the solvent 4D are indicated by solid arrows. As shown in FIG. 5, when supplying the liquid material, each valve unit V22 of the on-off valves V1, V3, V5 to V10, the two-valve three-way switching valve 15A, 15D, and each of the three-valve four-way switching valve 10A, 10D V31,
33 are respectively opened. On the other hand, on-off valve V2,
V4, V5, each valve unit V21 of 2 valve 3 way switching valve 15A, 15D, 3 valve 4 way switching valve 10A, 15
Each valve unit V32 of D is closed.
The two-valve three-way switching valves 15A and 15D and the three-valve 4
Details of the one-way switching valves 10A and 10D will be described later.

When the open / close state of each valve is controlled as shown in FIG. 5, charge gas is introduced into the material containers 3A to 3C and the solvent container 3D, and the liquid materials 4A to 4C and the solvent 4D are removed from the containers 3A to 3D. It is sent out to each of the transfer lines 6A to 6D. The liquid materials 4A to 4C and the solvent 4D sent to the transfer lines 6A to 6D are combined with the transfer line 6E.
At the same time, and is introduced into the vaporizer 2 in a gas-liquid two-phase flow state by the introduced carrier gas.

<< Description of 2-Valve 3-Way Switching Valve >> Next, referring to FIGS. 6 and 7, a 2-valve 3-way switching valve 15 (15A, 1
5D) will be described. FIG. 6 shows a two-valve three-way switching valve 1
5A and 5B show an example of FIG. 5, wherein FIG. 4A is a front view, FIG. 4B is a view from arrow A of FIG. Also, in FIG. 7, (a) is BB of FIG. 6 (b).
It is sectional drawing, (b) is CC sectional drawing of (a).
As shown in the flow diagram of FIG. 6C, the two-valve three-way switching valve 15 has two opening / closing valves V21 and V22 in an integrated structure, and has three ports P1, P2 and
P3. In the present embodiment, the on-off valve V2
1, V22 will be referred to as valve units V21, V22.

Reference numerals 150A and 150B denote valve driving units which are driven by compressed air supplied from the outside. As shown in FIG. 7, a valve unit V2 is provided in the body 151.
2, two diaphragms 152A, 15 for V21
2B are provided, and a valve opening / closing operation is performed by pistons 153A and 153B which are respectively driven in the vertical direction in the figure.

In FIG. 7, the piston 153A has a spring 155
The diaphragm 152A is driven upward by the urging force of A, and the diaphragm 152A is pressed against the valve seat 154A.
On the other hand, the piston 153B is driven downward in the figure by the urging force of the spring 155B, and the diaphragm 152B is pressed against the valve seat 154B. As a result, between port P1 and port P2 and between port P1 and port P3
Are shut off from each other.

In the state of FIG. 7, the air inlet 15
When compressed air is supplied to 6A, the piston 1
53A is driven downward, and the diaphragm 1
52A separates from valve seat 154A. as a result,
The port P1 is communicated with the port P2. On the other hand, when compressed gas is supplied to the air inlet 156B, the piston 153B is driven upward by the gas pressure, and the diaphragm 1
52B separates from valve seat 154B. in this case,
The port P1 is communicated with the port P3.

In the example shown in FIG. 2, ports P1 and P2 are connected to transfer lines 6 (6A and 6D), and port P3 is connected to auxiliary line 11. For example, material container 3A
When the liquid material 4A is sent from the container to the transfer line 6A, the valve unit V22 is opened and the valve unit V21 is closed, and as shown in R1 of FIG.
The liquid material 4A is guided from 1 to the port P2. On the other hand, in the case of pipe cleaning when the material container 3A is attached and detached as described later, the valve unit V22 is closed and the valve unit V21 is opened, and the port P1 is moved from the port P1 to the port P3 as indicated by R2 in FIG. To the washing waste liquid.

Therefore, as shown by the arrow R1, the liquid material 4A
Is sent to the transfer line 6A, the pipe 21 becomes a dead volume, and when the washing waste liquid flows as indicated by an arrow R2, the pipe 20 becomes a dead volume. As shown in FIG. 7A, since the port P1 is provided between the diaphragm 152A and the diaphragm 152B, the pipeline 20 is connected to the port P1 and the diaphragm 15A.
2A, and the pipeline 21 is a space between the port P1 and the diaphragm 152B. On the other hand, when independent opening / closing valves are used for the valve units V21 and V22, respectively, as in the related art, the portions 20 and 21 are piping portions. Therefore, in the present embodiment, the dead volume at the portion where the pipe branches to three directions can be made smaller than before.

<< Description of 3-valve 4-way switching valve >>
The four-way switching valve 10 (10A, 10D) will be described. 8A and 8B are external views showing an example of the three-valve four-way switching valve 10, in which FIG. 8A is a plan view, and FIG. The body 101 has four ports P11 to P14
Are provided, and 100A to 100C are drive units. The flow diagram of the three-valve four-way switching valve 10 is as shown in FIG.
31, V32 and V33 are integrated.

FIG. 9 (b) schematically shows the structure inside the body 101, which is shown in correspondence with the flow diagram of FIG. 9 (a). Each valve unit V31-V
33 have the same structure, and the diaphragms 112A, 112B, 112C, the piston 11
3A, 113B, 113C, valve seat 114A, 1
14B and 114C are provided, respectively. In FIG. 9B, the driving mechanism of the pistons 113A to 113C has the same structure as that of the two-valve three-way switching valve 15 shown in FIG. In the state shown in FIG. 9 (b), each of the diaphragms 112A to 112C is moved by the pistons 113A to 113C to form the valve seats 114A to 114C.
114C and the valve units V31-V
33 are all closed.

The piston 113 is moved from the state shown in FIG.
When A is driven to the left in the figure, the diaphragm 112A separates from the valve seat 114A and the ports P11 and P12
Communicates with When the piston 113C is driven rightward in the figure, the diaphragm 112C is moved to the valve seat 11.
Ports P13 and P14 communicate with each other at a distance from 4C. In the body 101, a conduit 115 communicating with the port P11 is provided.
When the piston 113B is driven upward, the diaphragm 112B separates from the valve seat 114B and the pipeline 1 communicates with the port P13.
15 communicates with the pipeline 116. That is, the port P1
1 and the port P13 are communicated.

In the example shown in FIG. 2, the port P11 is connected to the connector C side of the charge gas line 5,
Reference numeral 12 is connected to the material container 3A and the solvent container 3D. Port P13 is connected to transfer line 6 (6A, 6A).
The port P14 is connected to the material container 3A and the solvent container 3D. For example, the liquid material 4A is transferred from the material container 3A to the transfer line 6A.
Is transmitted, the valve unit V is supplied as shown in FIG.
32 is closed and the valve units V31 and V33 are opened.

At this time, the charge gas is supplied as shown in FIGS.
As shown in R3 of (a), it flows from the port P11 to the port P12 and is introduced into the material container 3A, and the liquid material 4A in the material container 3A (see FIG. 5) flows from the port P14 to the port P.
13 and sent out to the transfer line 6A. In the case of gas purging and pipe cleaning described later, FIG.
(A) The valve units V31 and V33 are closed and the valve unit V32 is opened, and a charge gas or a cleaning solvent flows from the port P11 to the port P13 as indicated by R6.

In the case of the three-valve four-way switching valve 10 as well, the dead volume can be reduced similarly to the two-valve three-way switching valve 15 described above. That is, when the circuit as shown in FIG. 9A is configured by independent open / close valves as in the related art, each of the valve units V31 to V33 is replaced with an open / close valve. In this case, FIG.
Portions indicated by reference numerals 120 and 121 in (a) have a piping configuration, so that the dead volume must be large.
On the other hand, in the present embodiment, a three-way four-way switching valve 10 having an integral structure is used, and a conduit 11 formed in a body 101 is used.
By making the volume of 5,116 smaller than that of the piping structure, the dead volume could be made smaller than before.

As described above, each three-way four-way switching valve 1
Reference numerals 0A and 10D are provided on the material container 3A and the solvent container 3D side with respect to the connector C. When refilling the material, each of the three-valve and four-way switching valves 10A and 10D and each of the containers 3A and 3D are integrated. It is attached and detached at part C. For example, when the material container 3A is to be detached from the charge gas line 5 and the transfer line 6A at the connector C, the open / close valve V is switched from the state shown in FIG.
3, V6 and the valve units V22, V31 and V33 are closed, and the opening and closing valves V2 and V4 and the valve units V21 and V32 are opened.

By controlling the valve opening / closing state in this way,
Solvent 4D sent from solvent container 3D to transfer line 6D
Is the opening / closing valve V2 → the auxiliary line 12 → the opening / closing valve V4
It flows in the order of the valve unit V32, the valve unit V21, and the auxiliary line 11, and is discharged to the drain tank 13. By flowing the solvent 4D through such a path, FIG.
The liquid material 4A remaining in the pipe line F1 indicated by the thick solid line 0 (a) is washed by the solvent 4D, and the washing waste liquid is discharged to the drain tank 13 through the auxiliary line 11. The pipe F1 is connected to the ports P11 and P11 in FIG.
It corresponds to P13 and conduits 115 and 116.

When the washing of the line F1 is completed, the material container 3A and the three-way four-way switching valve 10A are integrally removed from the connector C. After refilling the material container 3A with the liquid material 4A, it is connected to the connector C again. After the washing of the pipe line F1 is completed, FIG.
The valve may be switched between open and closed as shown in FIG. 2B, and the inside of the pipe F1 may be purged with a charge gas to remove the solvent in the pipe F.

As described above, the material container 3A and the three-way / four-way switching valve 10A have a structure that can be integrally removed from the lines 5 and 6A, and after the line F1 is cleaned as shown in FIG. If you remove 3A,
The liquid material does not remain in the pipe line F1, which is a portion that comes into contact with the atmosphere. As a result, even when the attachment / detachment operation of the material container 3A is performed, the reaction product between the liquid material 4A and the atmosphere remains in the line F1.
Does not occur within.

Incidentally, the above-described two-valve three-way switching valve 1
In 5A to 15D and 3-valve 4-way switching valves 10A to 10D, diaphragms 152A, 152B, 112A to 1
12C and valve seats 154A, 154B, 114A ~
When a resin material is used for 114C, PEEK (polyether ether ketone), PTF which is excellent in heat resistance and chemical resistance are used.
E (polytetrafluoroethylene), PI (polyimide), PBI (polybenzimidazole) and the like are preferably used. By using such a material, durability can be improved.

<< Description of Cleaning Operation >> Next, the cleaning operation before the start of the vaporization operation will be described. In the present embodiment, a description will be given of evacuation, gas purging, and solvent cleaning during the cleaning operation. In an actual cleaning operation, these steps are used in various combinations so that effective in-line cleaning is performed. For example, vacuum cleaning (or gas purging) → solvent cleaning is performed, or solvent cleaning is performed after performing vacuuming and gas purging several times. After the solvent cleaning, a gas purge for removing the cleaning liquid may be performed in some cases.

(1) Vacuuming First, the transfer lines 6A to 6A using the exhaust line 14
D, the evacuation of the auxiliary lines 11 and 12 will be described. FIG. 11 is a view showing the valve opening / closing state at the time of evacuation. The opening / closing valves V6, V9, V10, and the A3 valve 4-way switching valve 10A provided in the material containers 3A, 3D,
Each of the 10D valve units V31 and V33 is in a flat state, and the others are in an open state. When the valve opening / closing is controlled in this manner, the charge gas line 5, the transfer lines 6A to 6A
D and auxiliary lines 11 and 12 are evacuated lines 14
Is evacuated by a not-shown evacuation device.

(2) Gas Purge FIG. 12 is a view showing the open / close state of the valve at the time of gas purge, in which the open / close valve 10 of FIG. 11 is switched from the closed state to the open state. The charge gas flows through the charge gas line 5, the transfer lines 6A to 6D and the auxiliary lines 11 and 12 as indicated by the dashed arrows, and
Is discharged to the connected drain tank 13.

(3) Solvent Washing FIG. 13 is a view showing a valve opening and closing state at the time of solvent washing. In this embodiment, pipe washing is performed using the solvent 4D in the solvent container 3D. The valve opening / closing state shown in FIG. 13 is changed from the state shown in FIG.
The valve unit V32 of the one-way switching valve 10D is switched from the open state to the closed state, and the three-way four-way switching valve 10D
The valve units V31 and V33 of D are switched from the closed state to the open state.

Pressurized charge gas is supplied into the solvent container 3D from the charge gas line 5, and the solvent 4D in the solvent container 3D is sent out to the transfer line 6D. The solvent 4D sent to the transfer line 6D is at a branch point P40.
What flows in the transfer line 6D in the direction of the flow control valve 9D in the upper part of the figure and the auxiliary line 1 through the opening / closing valve V2
Divided into those flowing to 2.

The solvent 4D flowing into the auxiliary line 12 from the branch point P40 is further divided into two at the branch point P41. The branch branched downward at the branch point 41P is the valve unit V32 of the opening / closing valve V4 → the 3-valve 4-way switching valve 10A → the valve unit V of the 2-valve 3-way switching valve 15A.
It flows in the order of 22 → transfer line 6A, and is guided in the transfer line 6A toward the flow control valve 9A.

On the other hand, the flow of the solvent 4D branched upward in the drawing at the branch point P41 is guided to the material container 3B through the auxiliary line 12. Although the illustration of the piping system for the material containers 3B and 3C is omitted in FIGS. 2 and 11, the piping system for the material container 3A, that is, the on-off valve V2
The same auxiliary line 12, charge gas line 5, transfer line 6A, auxiliary line 11, and valves and the like provided on these lines as shown on the right side of the drawing are provided for the material containers 3B and 3C. ing. Then, the solvent 4 is passed through the same route as in the piping system of the material container 3A.
D is introduced and guided in the transfer lines 6B and 6C toward the flow control valves 9B and 9C. Transfer lines 6A-6D
The solvent 4D in the tank merges in the transfer line 6E, and is connected to the drain tank 1 via the on-off valve V5 and the auxiliary line 11.
3

<< Explanation of the liquid replacement operation >>
When the transfer lines 6A to 6D have been cleaned by performing gas purging and solvent cleaning, liquid replacement for filling the transfer lines 6A to 6D with the liquid materials 4A to 4C and the solvent 4D is performed. In that case, when the inside of the pipe is filled with the charge gas at the end of the cleaning operation, “gas → liquid” replacement is performed, and when the inside of the pipe is filled with the solvent 4D, “liquid → liquid” replacement is performed. Done.

FIG. 14 is a view showing the valve opening / closing state at the time of liquid replacement, and the opening / closing valves V1, V3, V5, V7, V
8, V10, each valve unit V22 of the two-valve three-way switching valve 15A, 15D and the three-valve four-way switching valve 10A,
Each of the 10D valve units V31 and V33 is opened, and the on-off valves V2, V4, V6, V9, and 2 valves 3
Valve unit V21 of one-way switching valves 15A and 15D
The valve units V32 of the three-way and four-way switching valves 10A and 10D are closed.

At this time, the inside of each of the transfer lines 6A to 6C is changed from the charge gas or the cleaning liquid (solvent 4D) to the liquid material 4A.
4C, and the inside of the transfer line 6D is replaced with the solvent 4D from the charge gas or the cleaning liquid. Liquid material 4A-4C and solvent 4 filling transfer lines 6A-6D
D, after being mixed in the transfer line 6E, is connected to the drain tank 1 via the opening / closing valve V5 and the auxiliary line 11.
It is discharged to 3.

During this replacement operation, the monitoring device 16 detects whether or not the charge gas or the cleaning liquid in the pipe has been completely replaced by the liquid materials 4A to 4C and the solvent 4D. FIG. 15 is a conceptual diagram of the monitoring device 16. A conduit 160 to which the auxiliary line 11 is connected is formed in the monitoring device 16, and the auxiliary line 11 connected to the upper side in the figure is formed.
(The charge gas, the liquid materials 4A to 4C) which flowed into the monitoring device 16 from the above are guided to the auxiliary line 11 connected to the lower side after passing through the pipeline 160.

In the middle of the conduit 160, a light transmitting window 161 formed of a light transmitting member such as glass is provided.
In the monitoring device 16, a light emitting element 162 and a light receiving element 163 are provided so as to face each other with a light transmission window 161 interposed therebetween, and are controlled by a control unit 164. For example, an LED or the like is used for the light emitting element 162, and a photodiode or a phototransistor is used for the light emitting element 163.

When the mixed liquid of the liquid materials 4A to 4C and the solvent 4D is flowing through the conduit 160, the light transmittance is lower than when the charged gas or the solvent 4D is flowing. The light receiving amount of the light also decreases. Therefore, assuming that the received light amount when the solvent 4D or the charge gas flows through the conduit 160 is W1 and the received light amount when the mixed liquid is flowing through the conduit 160 is W2, W1>W3> W2 is satisfied. A suitable reference light receiving amount W3 is set. And the received light amount W
Changes from “W ≧ W3” to “W <W3”,
The controller 164 determines that the “gas → liquid” replacement or the “liquid → liquid” replacement of the transfer lines 6A to 6D has been completely completed, and ends the replacement work. When the replacement operation is completed, the valve opening / closing state is switched as shown in FIG. 5 to start the vaporization operation.

In the above-described example, the monitoring device 16 is used for checking the replacement status at the time of liquid replacement. For example, the monitoring device 16 is provided in the transfer lines 6A to 6D to determine the generation of bubbles and the presence or absence of the liquid. You can also. Also, JP-A-11-3
An absorption spectrometer 200 as disclosed in Japanese Patent No. 45774 may be provided on the auxiliary line 11 as shown in FIG. 14 to determine the deterioration of the liquid and the mixing state of the liquid.

When measuring the remaining amounts of the liquid materials 4A to 4C and the solvent 4D in the material containers 3A to 3C and the solvent container 3D, a general liquid level sensor is used from the viewpoint of chemical resistance. Can not do. Therefore, in the above-described embodiment, the remaining amount is calculated by calculating the product of the flow rate and the time measured by the mass flow meters 9A to 9D. Further, the remaining amount of liquid can be calculated from the pressure change of the pressurized gas (charge gas) in the containers 3A to 3D.

FIG. 16 is an enlarged view of the material container 3A of FIG. 2, and the material container 3A is shown in cross section. Material container 3
A pressure gauge 301 is provided on the charge gas line side of A via a pipe 300. Reference numeral 302 denotes a remaining amount measuring device that calculates the remaining amount of liquid in the material container 3A from a change in pressure detected by the pressure gauge 301. When measuring the liquid level,
After supplying the pressurized charge gas into the material container 3A, the open / close valve V1 is closed, and the pressure change is measured by the pressure gauge 301 while the liquid material 4A is delivered in a fixed amount or a predetermined time has elapsed. The sending amount at this time is measured by the mass flow meter 9A shown in FIG.

However, even when the same amount of the liquid material 4A is delivered, the case where the liquid level changes from L1 to L2,
When the liquid level changes from L3 to L4, the pressure change in the container 3A during that time differs. For example, when the liquid level changes from L1 to L2, the pressure change is larger than when the liquid level changes from L3 to L4. Remaining amount measuring device 302
The relational expression between the remaining amount of liquid and the pressure change is stored in advance, and the remaining amount of liquid is calculated by substituting the change in pressure detected by the pressure gauge 301 into the relational expression.

In the example shown in FIG. 16, a liquid container 4A is filled with a liquid material 4A, a pressurized charge gas is introduced into the container 3A, and the liquid material 4A is delivered to a transfer line 6A by gas pressure. are doing. At this time, since the pressurized charge gas is in direct contact with the liquid surface, the liquid material 4A
The charged gas is easily dissolved into the gas, and the dissolved gas is released again in the transfer line 6A, so that bubbles are easily generated. Therefore, by using the containers 30 and 31 as shown in FIG. 17 as the material containers 3A to 3C and the solvent container 3D, such a dissolved gas amount can be reduced. Further, it is possible to prevent moisture in the charge gas from being absorbed by the liquid material.

In FIG. 17, (a) shows the first material container.
It is sectional drawing which shows the modification of (a), (b) is sectional drawing which shows the 2nd modification. In the container 30 shown in FIG.
An airtight bag 304 made of a chemical resistant material such as PTFE is stored in the casing 303.
3 and a bag 304. The liquid material 4A is stored in the bag 304, and the bag 304 and the casing 30
A pressurized charge gas is introduced into a space S1 between the charge gas 3 and a charge gas line 5 through a charge gas line 5. The bottom of the bag 304 is fixed to the casing 303. When the bag 304 is crushed in the right and left direction in the figure by the pressure of the charge gas, the liquid material 4A in the bag 304 passes through the pipe 305 and the three- and four-way switching valve 10A. It is sent to the transfer line 6A.

On the other hand, in the container 31 shown in FIG.
Metal such as SUS or PTF instead of the bag 304 of the container 30
The bellows 311 formed of E or the like
3 are provided. Bellows 311 and casing 3
When a charge gas is introduced into the space S1 between
The bellows 311 contracts upward in the figure due to the gas pressure, and the liquid material 4A contained in the bellows 311 is transferred via the pipe 312 and the three- and four-way switching valve 10A to the transfer line 6A.
Sent to

FIG. 18 is a sectional view showing a third modification of the material container. The material container 32 has bellows 321 and 322. The upper and lower ends of the bellows 321 are fixed to the upper plate 323A and the moving plate 323B, respectively, and the upper and lower ends of the bellows 322 are moving plates 323B.
And the lower plate 323C. The upper plate 323A and the lower plate 323C are connected by a rod 324 and a nut 325, and the interval between the plates 323A and 323C is kept at a predetermined interval.

A liquid material is accommodated in the bellows 321, and a pipe 3 is provided through the upper plate 323 A.
26 allows filling and discharging of liquid material. On the other hand, the charge gas is supplied into the bellows 322 through a pipe 327 and a pipe 328 formed in the lower plate 323C. Piping 327 is upper plate 3
23A and the moving plate 323B, and is fixed to the lower plate 323C. The pipes 326, 327
Is connected to the three-valve four-way switching valve 10A described above.

When the charge gas is further supplied into the bellows 322 in the state shown in FIG. 18, the bellows 322 extends up and down, and the moving plate 323B is pushed upward. As a result, the bellows 321 is contracted up and down, and the liquid material inside is sent to the transfer line via the pipe 326 and the switching valve (see FIG. 17). At this time, the amount of the liquid material in the bellows 322 can be displayed by the vertical position of the moving plate 323B.

The material of the bellows 321 is SU
A metal having excellent corrosion resistance such as S, a synthetic resin such as PTFE, or the like is used. In the example shown in FIG. 18, the bellows 321 for liquid material is contracted by supplying a charge gas into the bellows 322. However, the bellows 321 may be contracted upward using an air cylinder or a pantograph mechanism. good.

In correspondence between the embodiment described above and the elements of the claims, the ports P1 to P3 are
Are connected to the diaphragms 152A and 152A.
52B connects the first and second valve bodies of claim 1 with the port P
Reference numerals 11 to P14 denote first to fourth conduits of the second aspect, diaphragms 112A to 112C denote the first to third valve elements of the second aspect, bag 304 a flexible bag, and bellows 311 a bellows. The pressure-sensitive bag 301, the pressure gauge 301 and the remaining amount measuring device 302 are measuring means, the light receiving element 163 is a photoelectric sensor, the monitoring device 1
6 and the control unit 164 are detection means, the mass flow meters 8A to 8D are thermal mass flow meters, and the bellows 321 is a first mass flow meter.
, The bellows 322 constitutes a second bellows-like bag, and the moving plate 323B constitutes a pointing member.

[0070]

As described above, according to the first and second aspects of the present invention, the dead volume in the liquid material transfer line can be reduced, and the generation of deposits due to the stagnation of the liquid material can be achieved. Can be reduced, and the malfunction of the valve and the generation of the residue in the vaporizer can be prevented. In addition, gas purge,
Washing, liquid replacement and the like can be sufficiently performed. In particular,
According to the second aspect of the present invention, when the material container is replaced, after the line cleaning is performed, the material container and the three-way four-way switching valve are integrally removed to thereby prevent metal deposition due to atmospheric contact before and after the material container replacement. Can be reduced. According to the third aspect of the present invention, since the liquid material does not come into contact with the supply gas, it is possible to prevent the gas from being dissolved into the liquid material, and to suppress generation of bubbles in the liquid material transfer line. The stability of flow control is improved. In particular, liquid feeding by a mass flow controller is effective because liquid feeding is generally performed by gas pressurization. According to the invention of claim 4, since the measuring means does not come into direct contact with the liquid material, it is possible to prevent problems of the measuring means due to corrosion or the like. According to the invention of claim 5, since the liquid material in the first bellows-like bag does not come into contact with the supply gas, it is possible to prevent the gas from being dissolved into the liquid material, and to prevent the liquid material from being introduced into the liquid material transfer line. The generation of air bubbles is suppressed, and the stability of flow control is improved. Further, since the indicating member moves with the expansion and contraction of the first bellows-like bag, the amount of the liquid material in the first bellows-like bag can be confirmed by the position of the indicating member. According to the sixth aspect of the present invention, since the pressure in the drain tank is reduced, the fluid in the liquid material transfer line is easily discharged to the drain tank. In addition, since the drain tank is connected to the liquid material transfer line immediately before the vaporizer, the liquid material transfer line can be cleaned and replaced more smoothly, and can be reliably replaced and cleaned in the pipe. . According to the invention of claim 7, since bubbles generated in the liquid material transfer line can be detected, it is possible to supply the liquid material to the vaporizer under conditions that do not generate bubbles, Stable material supply can be performed. According to the invention of claim 8,
The thermal influence from the vaporizer to the thermal mass flowmeter can be reduced, and the measurement error can be reduced. According to the eighth and ninth aspects of the present invention, the capacity of the pipe between the flow control valve and the carburetor can be reduced, and the responsiveness of the flow control can be improved. According to the invention of claim 10, corrosion resistance and chemical resistance to a liquid material are improved,
The life of the resin member can be improved. Claim 11
According to the twelfth aspect of the present invention, it is possible to reduce the generation of bubbles due to the filter, and to improve the strength of the filter by adding a mesh having a large wire diameter. In particular, according to the twelfth aspect of the invention, the corrosion resistance and chemical resistance of the filter to the liquid material are improved.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram of an entire vaporizer.

FIG. 2 is a view showing one embodiment of a liquid material supply device according to the present invention.

FIG. 3 is a view showing the appearance of flow control valves 9A to 9D.

FIG. 4 is a diagram illustrating details of a filter 18A;
(A) is sectional drawing of a filter, (b) is a figure which shows flow volume stability.

FIG. 5 is a diagram showing an open / closed state of each valve when supplying a liquid material to the vaporizer 2;

6A and 6B are diagrams showing an example of a two-valve three-way switching valve 15, wherein FIG. 6A is a front view, FIG.
(C) is a flow diagram.

FIG. 7 is a view for explaining a two-valve three-way switching valve 15;
6A is a cross-sectional view taken along the line BB of FIG. 6B, and FIG.
It is CC sectional drawing of.

FIG. 8 is an external view of a three-valve four-way switching valve 10,
(A) is a plan view, (b) is a view on arrow D of (a).

FIG. 9 is a view for explaining a three-valve four-way switching valve 10;
(A) is a flow diagram, (b) is a diagram schematically showing the internal structure.

10A and 10B are diagrams illustrating cleaning and gas purging at the time of material container replacement, wherein FIG. 10A illustrates a valve open / close state during cleaning, and FIG. 10B illustrates a valve open / close state during gas purging.

FIG. 11 is a view showing a valve opening / closing state during evacuation.

FIG. 12 is a view showing a valve opening / closing state during gas purging.

FIG. 13 is a diagram showing a valve opening / closing state during solvent cleaning.

FIG. 14 is a view showing a valve opening / closing state at the time of liquid replacement.

15 is a conceptual diagram of the monitoring device 16. FIG.

FIG. 16 is an enlarged view of a material container 3A of FIG. 2;

17A and 17B are diagrams showing a modification of the material container, FIG. 17A is a cross-sectional view showing a first modification, and FIG. 17B is a cross-sectional view showing a second modification.

FIG. 18 is a sectional view showing a third modification of the material container.

[Explanation of symbols]

 DESCRIPTION OF SYMBOLS 1 Liquid material supply apparatus 2 Vaporizer 3A-3C Material container 3D Solvent container 4A-4C Liquid material 4D Solvent 5 Charge gas line 6A-6E Transfer line 8A-8D Mass flow meter 9A-9D Flow control valve 10,10A, 10B 2 valve Three-way switching valve 13 Drain tank 15, 15A, 15D Three-valve four-way switching valve 16 Monitoring device 18A, 18D Filter

──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. ⁷ Identification FI FI Theme Court II (Reference) H01L 21/205 F16K 7/17 A // F16K 7/17 F04B 9/12 H (72) Inventor Tatsushi Kawamoto No. 1, Nishinokyo Kuwabaracho, Nakagyo-ku, Kyoto-shi, Kyoto (72) Inventor: Masashi Kawao 1) Nishi-no-Kyowaharacho, Nakagyo-ku, Kyoto-shi, Kyoto: Shimadzu Corporation (72) Inventor: Shigeru Matsuno Chiyoda-ku, Tokyo 2-3-2 Marunouchi, Mitsubishi Electric Corporation (72) Inventor Akira Yamada 2-3-2, Marunouchi, Chiyoda-ku, Tokyo Inside Mitsubishi Electric Corporation (72) Inventor Shoji Miyashita, Marunouchi, Chiyoda-ku, Tokyo 2-3-2, Mitsubishi Electric Corporation (72) Inventor Hideko Uchikawa 2-3-2, Marunouchi, Chiyoda-ku, Tokyo Mitsubishi Electric Corporation Term (Reference) 3H075 BB14 3H077 AA01 BB03 CC03 DD09 DD14 EE05 EE11 EE15 EE21 EE22 EE29 EE31 FF03 FF06 FF12 FF14 FF22 FF55 4G068 AA03 AB15 AC04 AC05 AD25 AE03 AF31 4K030 AA11 EA01 KA39 KA41 KA46 LA15 5F045 AA04 AC07 EE02 EE04 GB04 GB06

Claims (12)

[Claims] 1. A liquid material supply device for supplying a liquid material comprising a liquid organic metal or an organic metal solution contained in a material container to a vaporizer via a liquid material transfer line. 2 between the first and second pipelines.
A first valve body for turning on / off fluid transfer between the second pipeline and the second pipeline, and a first valve body provided between the second pipeline and the third pipeline, A second valve body for turning on / off fluid transfer between a second pipe line and the third pipe line, and a second valve body between the first valve body and the second valve body. A liquid material supply device, wherein an integrated two-valve three-way switching valve provided with the second conduit is disposed at a branch point where the liquid material transfer line branches into three directions. 2. A gas is supplied to a material container containing a liquid material composed of a liquid organic metal or an organic metal solution through a gas supply line, and the liquid material is sent out to a liquid material transfer line by gas pressure. In a liquid material supply device for supplying the liquid material to a vaporizer via a liquid material transfer line, the liquid material supply device is provided between a first pipe and a second pipe, and
A first valve body for turning on and off the transfer of fluid between the first pipeline and the second pipeline, and a first valve body provided between the first pipeline and the third pipeline, A second valve body for turning on / off the transfer of fluid between the first pipe and the third pipe, and provided between the second pipe and the fourth pipe. And a third valve element for turning on and off the transfer of fluid between the second pipe line and the fourth pipe line, and the first valve body, the second valve body, A three-way four-way switching valve having an integral structure in which the first pipe is provided between the second valve body and the second pipe is provided between the second valve body and the third valve body. Provided between the material container and the liquid material transfer line and gas supply line, connecting the first conduit and the gas supply line, the second conduit and the gas region of the material container, Connect the 3 and the liquid material transfer line, and the fourth line and the liquid region of the material container are connected, and the material container is connected to the gas supply line and the liquid material transfer line. A liquid material supply device, wherein the switching valve is integrally detachable. 3. A gas is supplied to a material container containing a liquid material composed of a liquid organic metal or an organic metal solution through a gas supply line, and the liquid material is sent out to a liquid material transfer line by gas pressure. In a liquid material supply device that supplies the liquid material to a vaporizer through a liquid material transfer line, the material container includes a casing to which gas from the gas supply line is supplied, and a casing that is housed in the casing. A flexible bag or a bellows-like bag in which a liquid material is stored, and when the gas is supplied into the casing,
The liquid material supply device, wherein the liquid material in the bag is delivered from the material container to the liquid material transfer line. 4. The liquid material supply device according to claim 3, further comprising a measuring unit that measures a liquid amount of the liquid material in the bag based on a change in pressure of the gas supplied into the casing. A liquid material supply device characterized by the above-mentioned. 5. A gas is supplied to a material container containing a liquid material composed of a liquid organic metal or an organic metal solution through a gas supply line, and the liquid material is sent out to a liquid material transfer line by gas pressure. In a liquid material supply device for supplying the liquid material to a vaporizer via a liquid material transfer line, a first bellows-shaped bag filled with the liquid material, and a serial connection in the direction of expansion and contraction of the first bellows-shaped bag. Connected,
A second bellows-like bag for contracting the first bellows-like bag by gas supply from the gas supply line; and a connecting portion between the first bellows-like bag and the second bellows-like bag, An indicator for indicating the position of the connection portion, wherein the first bellows-like bag is contracted by the second bellows-like bag to transfer the liquid material in the first bellows-like bag to the liquid material transfer line. A liquid material supply device, wherein the liquid material is supplied to the liquid material supply device. 6. The liquid material supply device according to claim 1, wherein the inside of the liquid material supply line is depressurized, and the liquid material supply line is replaced with a liquid or when the pipeline is cleaned. A liquid material supply device, wherein a drain tank for storing discharged waste liquid is connected via a valve immediately before the vaporizer in the liquid material transfer line. 7. The liquid material supply device according to claim 1, wherein the presence or absence of the liquid material in the liquid material transfer line and the presence or absence of bubbles generated from the liquid material are determined by a photoelectric sensor. A liquid material supply device, wherein a detecting means for detecting using the liquid material is provided in the liquid material transfer line. 8. A liquid material contained in a material container is transferred through a liquid material transfer line while controlling a flow rate by a thermal mass flow meter utilizing heat dissipation from a heating element and a flow control device having a flow control valve. In a liquid material supply device that supplies to the vaporizer, the flow meter and the flow control valve are separated, and the flow meter is disposed on the material container side of the liquid material transfer line,
The liquid material supply device, wherein the flow control valve is disposed on a vaporizer side of the liquid material transfer line. 9. The liquid material supply device according to claim 7, wherein the flow control valve is provided with a shutoff mechanism that can shut off the supply of the liquid material. 10. The liquid material supply device according to claim 1, wherein a resin member provided in the liquid material transfer line and in contact with the liquid material is provided with a PEEK (polyether ether keto).
ne), PTFE (polytetrafluoroethylene), PI (p
A liquid material supply device characterized by using any one of polyimide) and PBI (polybenzimidazole). 11. A liquid material supply device for supplying a liquid material contained in a material container to a vaporizer via a liquid material transfer line, wherein a filter provided in the liquid material transfer line is:
A liquid material supply device comprising a plurality of stacked first SUS meshes having a small wire diameter and a plurality of second SUS meshes having a large wire diameter. 12. The liquid material supply device according to claim 11, wherein a PTFE mesh is used instead of the SUS mesh.