Sublimation gas supply system and sublimation gas supply method

Abstract

To provide a system and method for supplying sublimation gas without reducing the utilization ratio of the sublimation gas even when exchanging a solid material vessel.SOLUTION: A system for supplying sublimation gas 1 includes: a first vessel 11; a first heating part 12 for heating the first vessel 11; a first buffer tank 13 for storing the sublimation gas; a dilution gas passage 17 connected to a first connection part C1 in a second passage 16 and for introducing dilution gas into the second passage 16; a first flow control device 19 provided between the first connection part C1 and the first buffer tank 13 on the second passage and for controlling a flow; a second flow control device 21 provided on the dilution gas passage and for controlling a flow; and a mixer 22 provided on the second passage and for mixing the dilution gas and the first sublimation gas met in the first connection part C1.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present disclosure relates to a sublimation gas supply system and a sublimation gas supply method for supplying a sublimation gas of a solid material to a downstream process. [Background technology]

[0002] In order to manufacture microelectronic devices such as semiconductor integrated devices and liquid crystal panels, it is necessary to deposit films of various materials on substrates. In recent years, dry coating has been applied to various components to improve their strength and other properties. Well-known methods for depositing and coating films include PVD (physical vapor deposition), CVD (chemical vapor deposition), and ALD (atomic layer deposition).

[0003] With the progress of the semiconductor industry, the vapor pressure of precursors used for film formation tends to be lower in order to meet strict film requirements. Precursors for film formation include inorganic and organometallic compounds of aluminum, barium, bismuth, chromium, cobalt, copper, gold, hafnium, indium, iridium, iron, lanthanum, lead, magnesium, molybdenum, nickel, niobium, platinum, ruthenium, silver, strontium, tantalum, titanium, tungsten, yttrium, and zirconium. In addition, inorganic metal compounds are generally used as precursors for dry coating in order to form carbon-free films. Since these materials have low vapor pressure, they need to be sublimated and supplied to the film formation chamber in the case of solid materials. In the conventional method, in a vapor generation chamber containing raw material powder, the raw material powder is heated to generate saturated vapor and the carrier gas is brought into contact with the raw material vapor itself, thereby supplying the carrier gas containing the raw material powder to the film formation device (see, for example, Patent Document 1). [Prior art documents] [Patent documents]

[0004] [Patent Document 1] JP 3-141192 Summary of the Invention [Problem to be solved by the invention]

[0005] However, in the above-mentioned conventional device, when replacing the vapor generating chamber, it is necessary to once discharge the sublimation gas from the storage chamber, which reduces the utilization rate of the sublimation gas in the conventional device.

[0006] An object of the present disclosure is to provide a sublimation gas supply system and a supply method thereof that do not reduce the utilization rate of the sublimation gas even when the solid material container is replaced. [Means for solving the problem]

[0007] The present disclosure relates to A sublimation gas supply system for supplying a sublimation gas of a solid material to a downstream process, comprising: a first container containing a first solid material; a first heating unit that heats the first container so that the first solid material sublimes to generate a first sublimation gas; a first buffer tank for storing the sublimation gas; a first passage for introducing the first sublimation gas into the first buffer tank; a second passage for supplying the first sublimation gas led out from the first buffer tank to a subsequent process; a dilution gas path connected to a first connection portion of the second path for introducing a dilution gas into the second path; a first flow control device provided on the second path between the first connection portion and the first buffer tank for controlling a flow rate; A second flow rate control device provided on the dilution gas path for controlling a flow rate; The gas supply system further includes a mixer that is provided on the second path and mixes the dilution gas and the first sublimation gas that have joined at the first connection portion.

[0008] According to this configuration, when the first container is replaced with another container containing the first solid material, it is not necessary to discharge the first sublimation gas from the first buffer tank, and therefore the first sublimation gas can be supplied to the subsequent process without reducing the utilization rate of the sublimation gas.

[0009] The above configuration further includes a second buffer tank provided on the dilution gas path and configured to store the dilution gas; a first valve provided on the first path; a second valve provided on the second path between the first connection portion and the first buffer tank; The dilution gas supply system may further include a third valve provided on the dilution gas path between the first connection portion and the second buffer tank.

[0010] According to this configuration, the flow rates of the first sublimation gas and the diluent gas can be appropriately controlled.

[0011] The above configuration further includes a first exhaust path provided on the first path between the first valve and the first buffer tank for exhausting the first sublimation gas from the first buffer tank; a third flow control device provided on the second path between the mixer and the downstream process for controlling a flow rate; The present invention may also have a configuration including an exhaust gas path that is provided on the second path between the mixer and the third flow rate control device and that exhausts gas on the second path.

[0012] According to this configuration, when it is necessary to remove the sublimation gas (for example, the first sublimation gas) in the system in the control of the sublimation gas system, the sublimation gas can be appropriately discharged.

[0013] The above disclosure further includes a first buffer tank heating unit for heating the first buffer tank; and a mixer heating section for heating the mixer.

[0014] According to this configuration, when the dilution gas and the sublimation gas are mixed, solidification of the sublimation gas can be prevented.

[0015] The disclosure further includes a second container containing a second solid material; a second heating section for heating the second container so that the second solid material sublimes to generate a second sublimation gas; and a third path for introducing the second sublimation gas into the first buffer tank, wherein the first solid material and the second solid material are the same solid material. By the same material it is meant that they are made of substantially the same material.

[0016] According to this configuration, if the pressure of the first sublimation gas in the first container drops (i.e., the first solid material decreases to a predetermined amount or less), the first sublimation gas is not removed from the first buffer tank, and the second sublimation gas can be introduced from the second container into the first buffer tank. This is because the first sublimation gas and the second sublimation gas referred to here are composed of the same sublimation gas. "The first solid material and the second solid material are the same solid material" means that they are composed of substantially the same material.

[0017] The disclosure further includes a second container containing a second solid material; a second heating section for heating the second container so that the second solid material sublimes to generate a second sublimation gas; a third buffer tank for storing the second sublimation gas; a fourth passage for introducing the second sublimation gas into the third buffer tank; a fifth passage for supplying the second sublimation gas led out from the third buffer tank to the second passage between the mixer and the first buffer tank; a fourth flow control device provided on the fifth path for controlling a flow rate; and a valve provided on the fifth path. Here, the first solid material and the second solid material are different solid materials. "The first solid material and the second solid material are different solid materials" means that they are made of substantially different materials.

[0018] According to this configuration, the supply of the first sublimation gas from the first container can be stopped, and then the second sublimation gas can be supplied from the second container to a subsequent process.

[0019] The above disclosure further includes a second pressure gauge for measuring a pressure in the first buffer tank, and a controller, wherein: The controller may be configured to control the second valve to open so that the first sublimation gas flows through the first connection portion when the second pressure gauge reaches a predetermined pressure at startup. According to this configuration, the first sublimation gas can be appropriately supplied to the subsequent process. Here, the predetermined pressure is, for example, 1×10 -6 From 1×10 -1 The pressure is, for example, 1 kPa to 50 kPa when the first solid material is MoO2Cl2. The predetermined pressure value can be converted into the concentration of the predetermined first sublimation gas.

[0020] The disclosure further comprises a controller, wherein: The controller may be configured to control the second valve and the third valve to be closed in stop control.

[0021] According to this configuration, it is possible to prevent the dilution gas from flowing into the first buffer tank. Therefore, the sublimation gas supply system can be restarted without discharging the sublimation gas stored in the first buffer tank. As a specific control method, any of the following (1) to (3) may be used. (1) The second valve and the third valve are closed simultaneously. (2) Close the second valve and then close the third valve. (3) Close the third valve and then the second valve.

[0022] The above-mentioned device further includes a controller, The controller controls at least one selected from the group consisting of the first flow control device and the second flow control device so as to adjust the concentration of the first sublimation gas introduced to the downstream process during steady-state operation or depending on the status of the downstream process.

[0023] According to this configuration, if the downstream process changes the concentration of the first sublimation gas during steady operation, the concentration of the first sublimation gas can be appropriately changed.

[0024] Another disclosure is a sublimation gas supply method for supplying a sublimation gas of a solid material to a downstream process, comprising: a first heating step of heating a first container containing a first solid material to generate a first sublimation gas derived from the first solid material; a first introducing step of introducing the first sublimation gas into a first buffer tank; a first supply step of supplying the first sublimation gas led out from the first buffer tank to a subsequent process; a first dilution step of supplying a dilution gas to the first sublimation gas led out from the first buffer tank; a first flow rate control step of controlling a flow rate of the first sublimation gas led out from the first buffer tank; and a second flow rate control step of controlling the flow rate of the dilution gas supplied from the dilution gas path.

[0025] The other disclosure above includes a second heating step of heating a second container that contains a second solid material to generate a second sublimation gas derived from the second solid material; a second introducing step of introducing the second sublimation gas into a first buffer tank; and a first switching step of stopping the first introducing step and switching to the second introducing step, wherein the first solid material and the second solid material are the same solid material.

[0026] According to the above disclosure, if the pressure of the first sublimation gas in the first container decreases (i.e., the amount of the first solid material decreases below a predetermined amount), the first sublimation gas is not removed from the first buffer tank, and the second sublimation gas can be introduced from the second container into the first buffer tank.

[0027] The above invention includes a second heating step of heating a second container that contains a second solid material to generate a second sublimation gas derived from the second solid material; a second introducing step of introducing the second sublimation gas into a third buffer tank; a second supply step of supplying the second sublimation gas led out from the third buffer tank to a subsequent process; a second dilution step of supplying the dilution gas to the second sublimation gas derived from the third buffer tank; and a second switching step of stopping the first introducing step and the first supplying step and switching to the second introducing step and the second supplying step, wherein the first solid material and the second solid material are different solid materials. [Brief description of the drawings]

[0028] [Figure 1] FIG. 1 shows an outline of a sublimation gas supply system according to the first embodiment. [Diagram 2] FIG. 2 shows an outline of a sublimation gas supply system according to the second embodiment. [Diagram 3] FIG. 3 shows an outline of a sublimation gas supply system according to the third embodiment. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0029] Several embodiments of the present invention will be described below. The embodiments described below are merely examples of the present invention. The present invention is not limited to the following embodiments, and includes various modified forms that are implemented within the scope of the present invention. It should be noted that not all of the configurations described below are necessarily essential configurations of the present invention.

[0030] (Embodiment 1) Figure 1 shows an outline of the sublimation gas supply system. The arrows in Figure 1 indicate the flow directions of various gases (e.g., sublimation gas, dilution gas). In this embodiment, there is one container and one buffer tank, which stores the sublimated gas produced from the container.

[0031] A first solid material S1 is stored in the first container 11. The first container 11 may be of a tray type or a trayless type. The tray type refers to a type in which one or more trays are built into the container and the solid material is placed on the tray. The trayless type refers to a type in which the solid material is placed directly in the container.

[0032] The first heating unit 12 can heat the first container 11. When the first container 11 is heated, a first sublimation gas is generated from the first solid material S1. In FIG. 1, the first heating unit 12 is a jacket type that covers the first container 11, but is not limited to this. For example, the first heating unit 12 may be an oven type that heats the entire surface of the first container 11. The first thermometer T1 measures the temperature of the first heating unit 12. Then, the first heating unit 12 is controlled based on the measured temperature. The first container 11 may be equipped with a first pressure gauge P1 that measures the pressure inside the first container 11.

[0033] The first sublimation gas generated from the first container 11 is introduced into the first buffer tank 13 through the first path 15. In other words, the first container 11 is connected to the first buffer tank 13 through the first path 15. As shown in FIG. 1, the first buffer tank 13 may be provided with a first buffer tank heater 14. For example, the first buffer tank heater 14 may be a jacket type that covers the first buffer tank heater 14. The first buffer tank 13 may be provided with a second pressure gauge P2. The second pressure gauge P2 measures the pressure inside the first buffer tank 13. The first path 15 has a third connection part C3 connected to the purge gas path 27. A purge gas flows through the purge gas path 27. The purge gas is, for example, oxygen, nitrogen, and hydrogen. The purge gas may also be an inert gas. For example, helium, argon, and neon can be mentioned. A valve (not shown) may be provided on the purge gas path 27. When the purge gas is supplied to the first path 15, the valve (not shown) on the purge gas path 27 may be open. The first path 15 has a second connection part C2 connected to a first discharge path 25 for discharging the sublimation gas stored in the first buffer tank 13. A pump 26 is provided on the first discharge path 25. A valve (not shown) may be provided on the first discharge path 25. The stored sublimation gas is then supplied to the subsequent process BP through a second path 16. A first connection part C1 is provided on the second path 16. The first connection part C1 is connected to a diluent gas path 17 for introducing a diluent gas.

[0034] A second buffer tank 18 may be provided on the dilution gas path 17. The second buffer tank 18 stores a dilution gas. Here, the dilution gas is, for example, an inert gas such as nitrogen gas, a rare gas such as argon gas, or hydrogen gas.

[0035] The dilution gas merges with the sublimation gas discharged from the first buffer tank 13 at the first connection part C1. Then, the dilution gas and the sublimation gas are mixed in the mixer 22 provided on the second path 16. Here, the mixer 22 may have any configuration when the sublimation gas and the dilution gas are mixed. For example, the mixer 22 may be an extension pipe, a gas mixer, or a Venturi tube. The mixer 22 may be provided with a mixer heating part 28. In this case, even if the temperature of the dilution gas is relatively lower than the temperature of the sublimation gas, the solidification of the sublimation gas can be prevented. Furthermore, in the second path 16, an exhaust gas connection part CE may be provided between the mixer 22 and the subsequent process BP. The exhaust gas connection part CE is connected to the exhaust gas path 23. A pump (not shown) and a valve (not shown) may be provided on the exhaust gas path 23 between the pump and the exhaust gas connection part CE. In addition, a heating unit (not shown) may be provided on the second path 16 to prevent the sublimation gas from solidifying.

[0036] The sublimation gas supply system of this embodiment includes a flow control device that controls the flow rate of the sublimation gas and the flow rate of the dilution gas. Specifically, in the second path 16, a first flow control device 19 is provided between the first connection part C1 and the first buffer tank 13. In the dilution gas path 17, a second flow control device 21 is provided between the first connection part C1 and the second buffer tank 18. For example, a controller 100 (details will be described later) controls the first flow control device 19 and the second flow control device 21. As a result, the concentration of the sublimation gas can be appropriately changed. Therefore, a sublimation gas of an appropriate concentration can be supplied to the subsequent process BP. In addition, in the second path 16, a third flow control device 24 may be provided between the exhaust gas connection part CE and the subsequent process BP. A valve (not shown) may be provided between the third flow control device 24 and the exhaust gas connection part CE. As the flow control device, for example, a mass flow meter can be given. Another example of the flow control device is a device that combines a flow control valve and a flow meter. Another example of the flow control device is a device that controls the pressure before and after the path and controls the flow adjustment valve by using the differential pressure.

[0037] The sublimation gas supply system of this embodiment includes various valves. The first valve V1 is provided on the first path 15. As shown in FIG. 1, the first valve V1 may be provided between the third connection part C3 and the first container 11. The second valve V2 is provided on the second path 16. Specifically, the second valve V2 is provided between the first connection part C1 and the first buffer tank 13. The third valve V3 is provided on the dilution gas path 17. It is provided on the dilution gas path 17 between the first connection part C1 and the second flow control device 21. Furthermore, a fourth valve V4 may be provided. The fourth valve V4 is provided on the first path 15 between the second connection part C2 and the third connection part C3. Here, "on the path" includes piping connecting elements, and the inlet and outlet parts of each container and each buffer tank. Instead of the "valves" on the pathways, valves at the inlet and outlet of each vessel and each buffer tank may be used.

[0038] Furthermore, the sublimation gas supply system of this embodiment includes a controller 100. The controller 100 may be connected to various valves, various flow rate control devices, various pressure gauges, various pumps, and downstream processes. For example, the sublimation gas supply system of this embodiment can execute the following control. The following operations may be performed, for example, by the arithmetic circuit of the controller 100 reading a control program from the memory circuit of the controller 100. The controller 100 may include an arithmetic processing unit and a memory unit that stores the control program. Examples of the arithmetic processing unit include an MPU and a CPU. Examples of the memory unit include a memory. However, it is not necessarily required that the controller 100 performs the following operations. An operator may perform some of the operations.

[0039] (First heating step) The controller 100 controls the first heating unit 12 to heat the first container 11 that contains the first solid material S1. Then, a first sublimation gas derived from the first solid material S1 is generated.

[0040] (First supply process) The method includes a first introducing step of introducing a first sublimation gas into a first buffer tank 13. Specifically, the controller 100 controls the first valve V1 and the fourth valve V4 to open. Then, the first sublimation gas is introduced into the first container 11 through a first path 15. Next, the first sublimation gas derived from the first buffer tank 13 is supplied to the subsequent process BP. At this time, the controller 100 controls the second valve V2 to open.

[0041] (First dilution step) In this first supply step, a dilution gas is supplied midway. In the first dilution step, the controller 100 controls the third valve V3 to open the third valve V3.

[0042] (First flow rate control step and second flow rate control step) The controller 100 controls the first flow rate controller and the second flow rate controller so that the concentration of the first sublimation gas reaches a concentration required by the downstream process BP.

[0043] Furthermore, for example, the sublimation gas supply system of this embodiment can execute the following control at startup.

[0044] (Startup mode) (1) In response to a command from the controller 100, the pump 26 is operated to create a vacuum state (i.e., a substantial vacuum state) in the first buffer tank 13. (2) The second pressure gauge P2 measures the pressure inside the first buffer tank 13. (3) A determination unit (not shown) of the controller 100 may determine whether or not the inside of the first buffer tank 13 has become a vacuum state based on the measurement value of the second pressure gauge P2. (4) When the pump 26 is operated, only the first discharge path 25 is opened. (5) If the first exhaust path 25 is equipped with a valve, the controller 100 controls the valve to open. (6) The various valves (V2, V3, and V4) of the other paths connected to the first buffer tank 13 are controlled by the controller 100 to be in a closed state. At this time, the first heating unit 12 may heat the first container 11. In this case, a first sublimation gas is generated in the first container 11 from the first solid material S1. (7) When it is determined that the inside of the first buffer tank 13 is in a vacuum state, the controller 100 controls the first valve V1 and the fourth valve V4 to open. At this time, the valves of the first exhaust path 25 and the purge gas path 27 (not shown) are closed. Then, the first sublimation gas stored in the first container 11 is supplied to the first buffer tank 13 through the first path 15. (8) When the pressure measured by the second pressure gauge P2 exceeds a predetermined pressure, the controller 100 controls the second valve V2 to open and the third valve V3 to open so that the dilution gas can be supplied to the second path 16. (9) The controller 100 can appropriately control the first flow rate controller 19 and the second flow rate controller 21 so that the concentration of the first sublimation gas becomes a predetermined concentration (for example, a concentration required by a subsequent process BP). Here, the mixer heater 28 provided in the mixer 22 may be controlled according to the temperature of the dilution gas. For example, if the temperature of the dilution gas is lower than that of the first sublimation gas, it is expected that the temperature of the first sublimation gas will decrease. As a result, the first sublimation gas may solidify. By heating the mixer 22 with the mixer heater 28, it is possible to prevent the first sublimation gas from solidifying.

[0045] Also, even if the first container 11 continues to be heated, the first pressure gauge P1 may not reach a predetermined pressure. Here, for example, the pressure value measured by the first pressure gauge P1 can be converted into the concentration of the first sublimation gas based on a pressure concentration conversion value table provided in the controller. Not reaching the predetermined pressure means that the amount of the first solid material S1 in the first container 11 is insufficient. At that time, for example, the controller 100 controls to close the first valve V1. Then, the first container 11 can be removed and another container containing the first solid material can be attached. In this case, since the first buffer tank 13 contains the first sublimation gas derived from the first solid material, the first sublimation gas from the other container can be introduced into the first buffer tank 13 by opening the first valve V1 after attaching the other container. In other words, when replacing the first container 11 with another container, the sublimation gas supply system can be operated without returning the first buffer tank 13 to a vacuum state (i.e., without discharging the first sublimation gas remaining in the first buffer tank 13). Therefore, the utilization rate of the sublimation gas can be improved compared to the conventional system.

[0046] Next, the sublimation gas supply system of this embodiment can execute the following control during steady operation. The steady operation here means a state in which the sublimation gas is continuously supplied to the downstream process BP.

[0047] The controller 100 controls at least one selected from the group consisting of the first flow rate control device 19 and the second flow rate control device 21 so that the concentration of the first sublimation gas is the concentration required by the subsequent process BP. If the subsequent process is a film formation device, even if the film formation conditions are changed during steady operation, the first sublimation gas can be continuously supplied while changing its concentration. In other words, even if the subsequent process BP requires a different concentration of sublimation gas, the sublimation gas can be supplied to the subsequent process BP without stopping the sublimation gas supply system once.

[0048] Next, the sublimation gas supply system of this embodiment can execute the following control in the stop control. The controller 100 may control the second valve V2 and the third valve V3 so as to close the second valve V2 and the third valve V3 simultaneously. This control can prevent the dilution gas from flowing into the first buffer tank 13. It can also prevent the sublimation gas from flowing into the second buffer tank 18. Therefore, the sublimation gas supply system can be restarted without discharging the sublimation gas stored in the first buffer tank 13 and the dilution gas stored in the second buffer tank 18.

[0049] Second Embodiment As shown in Fig. 2, the sublimation gas supply system shown in the second embodiment further includes a second container 31 in which a second solid material S2 is stored, in addition to the sublimation gas supply system shown in the first embodiment. The second sublimation gas generated from the second container 31 is configured to be supplied to the first buffer tank 13. Here, in this embodiment, the first solid material S1 and the second solid material S2 are configured of the same solid material. The following mainly describes the differences from the first embodiment.

[0050] The second container 31 may be of a tray type or a trayless type. The second heating unit 32 can heat the second container 31. The second sublimation gas is generated from the second solid material S2 by heating the first container 31. The second heating unit 32 may be of a jacket type or an oven type. The second thermometer T2 measures the temperature of the second heating unit 32. Then, the second heating unit 32 is controlled based on the measured temperature. The second container 31 may be equipped with a third pressure gauge P3 that measures the pressure inside the second container 31. The second sublimation gas generated from the second container 31 is introduced into the first buffer tank 13 through the third path 33 and the first path 15. Here, the third path 33 is connected to the first path 15 at the fourth connection part C4. In FIG. 2, the fourth connection part C4 is provided between the first valve V1 and the third connection part C3, but is not particularly limited as long as it is between the first valve V1 and the fourth valve V4. Here, a sublimation gas supply method in this embodiment will be described.

[0051] (Second heating step) The controller 100 controls the fifth valve V5 to close. Then, the controller 100 controls the second container 31 containing the second solid material S2 to heat the second container 31. Then, the second sublimation gas derived from the second solid material S2 is generated.

[0052] (Second introduction step) The controller 100 controls the fifth valve V5 and the fourth valve V4 to open. Then, the second sublimation gas is introduced into the first buffer tank.

[0053] (First switching process) The first introduction step described in the first embodiment is stopped. In other words, the controller 100 controls the first valve V1 to close. In this way, the first introduction step is switched to the second introduction step.

[0054] (Container replacement process) Also, after the first switching step, the first container 11 may be replaced with another container containing the first solid material. Therefore, if the first sublimation gas generated from the first container 11 decreases, the second sublimation gas can be supplied from the second container to the first buffer tank 13. Here, the first sublimation gas and the second sublimation gas in this embodiment are derived from the same solid material. Therefore, when switching from the first introduction step to the second introduction step, it is not necessary to remove the sublimation gas stored in the first buffer tank 13. Therefore, the utilization rate of the sublimation gas can be increased compared to the conventional supply method.

[0055] (Third embodiment) 3, the sublimation gas supply system shown in the third embodiment further includes a second container 31 in which a second solid material S2 is stored in addition to the sublimation gas supply system shown in the first embodiment. The second sublimation gas generated from the second container 31 is configured to be supplied to a third buffer tank 43. Here, in this embodiment, the first solid material S1 and the second solid material S2 are configured of different solid materials.

[0056] The second sublimation gas generated from the second container 31 is introduced into the third buffer tank 43 through the fourth path 45. In other words, the second container 31 and the third buffer tank 43 are connected via the fourth path 45. As shown in FIG. 3, the third buffer tank 43 may be provided with a third buffer tank heating unit 44. For example, the third buffer tank heating unit 44 may be a jacket type that covers the first buffer tank heating unit 44. The third buffer tank 43 may be provided with a fourth pressure gauge P4. The fourth pressure gauge P4 measures the pressure inside the third buffer tank 43. Next, the stored second sublimation gas is supplied to the subsequent process BP through a fifth path 46. Specifically, as shown in Fig. 3, the fifth path 46 is connected to a fifth connection part C5 provided between the first connection part C1 and the first flow control device 19. The fifth connection part C5 may be provided between the first connection part C1 and the mixer 22. Various paths in this embodiment will be described, focusing on differences from the first and second embodiments.

[0057] The path through which the purge gas flows is composed of a sixth path 47 and an eighth path 49. The sixth path 47 is connected to the third connection part C3 on the first path 15 and the sixth connection part C6 of the fourth path 45. Furthermore, a seventh connection part C7 is provided on the sixth path 47. This seventh connection part C7 is connected to the eighth path 49. A sixth valve V6, a seventh valve V7, and an eighth valve V8 are provided on the eighth path 49 between the third connection part C3 and the seventh connection part C7, and between the sixth connection part C6 and the seventh connection part C7, respectively. For example, when it is desired to purge the first buffer tank 13 and the first path 15, the controller 100 controls the eighth valve V8 and the second valve V2 to close. The controller 100 also controls the fourth valve V4, the sixth valve V6, and the seventh valve V7 to open. In this manner, the purge gas can be introduced into the first buffer tank 13 and the first path 15.

[0058] Next, the path through which the exhaust gas (e.g., sublimation gas) flows will be described. The path through which the exhaust gas flows is composed of a seventh path 48 and a ninth path 50. The seventh path 48 is connected to the second connection part C2 on the first path 15 and the eighth connection part C8 of the fourth path 45. Furthermore, a ninth connection part C9 is provided on the seventh path 48. This ninth connection part C9 is connected to the ninth path 50. On the ninth path 50, a sixteenth valve V16, a ninth valve V9, and a tenth valve V10 are provided between the second connection part C2 and the ninth connection part C9, and between the eighth connection part C8 and the ninth connection part C9, respectively. For example, when it is desired to discharge the sublimation gas stored in the first buffer tank 13 and the first path 15, the controller 100 controls the fourth valve V4 and the tenth valve V10 to close. The controller 100 also controls the ninth valve V9 and the sixteenth valve V16 to open. Then, the pump 26 is driven to discharge the exhaust gas (here, the sublimated gas).

[0059] The fifth path 46 will be described. The fifth path 46 connects the third buffer tank 43 and the fifth connection part C5. A third flow rate controller 51 is provided on the fifth path 46. An example of the fourth flow rate controller 51 is a mass flow meter. The fourth flow rate controller 51 controls the flow rate of the second sublimation gas.

[0060] Furthermore, a valve may be provided on the fifth path 46. As shown in Fig. 3, the valve may be provided between the third buffer tank 43 and the fourth flow control device 51 (a thirteenth valve shown in Fig. 3). Also, the valve may be provided between the fourth flow control device 51 and the fifth connection part C5 (a fourteenth valve shown in Fig. 3).

[0061] Further, a fifteenth valve V15 is provided on the second path 16. Specifically, as shown in FIG.

[0062] Here, a sublimation gas supply method in this embodiment will be described.

[0063] (Second heating step) The controller 100 controls the eleventh valve V11 to close. Then, the controller 100 controls the second container 31 that contains the second solid material S2 to heat the second container 31. Then, a second sublimation gas derived from the second solid material S2 is generated.

[0064] (Second introduction step) The controller 100 controls the eleventh valve V11 and the twelfth valve V12 to open. Then, the second sublimation gas is introduced into the third buffer tank 43.

[0065] (Second switching process) At this time, the first introduction step is stopped. In other words, the controller 100 controls the first valve V1 to close. In this manner, the first introduction step is switched to the second introduction step.

[0066] (Vacuum purge process) The second switching step may include a vacuum purging step, which includes the following steps: Also, the following steps may be repeated: (1) The third valve V3, the fourteenth valve V14, and the fifteenth valve V15 are controlled to be closed. (2) A pump (not shown) provided in the exhaust gas passage 23 is driven. At this time, a valve (not shown) provided between the pump and the exhaust gas connection part CE is opened. Then, a part of the second passage 16 is put into a vacuum state. (3) Close a valve (not shown) provided in the exhaust gas path 23. Next, open the third valve V3 to allow the dilution gas to flow. (4) The third valve V3 is closed. Then, a valve (not shown) provided in the exhaust gas path 23 is opened. In this manner, the dilution gas is discharged from the exhaust gas path.

[0067] Therefore, if the subsequent process BP requires a sublimation gas derived from a solid material different from the first sublimation gas generated from the first container 11, the second sublimation gas can be supplied from the second container to the subsequent process. Therefore, even when the type of sublimation gas to be supplied to the subsequent process is changed in the sublimation gas supply system, the sublimation gas can be continuously supplied without stopping the system. When switching between the various types of gases, some of the gas may be discharged before being sent to the subsequent process BP in order to clean the piping and mixer. Also, for example, the first sublimation gas and the second sublimation gas may be mixed and supplied to the subsequent process BP by controlling both the 14th valve V14 and the 15th valve V15 to be opened.

[0068] From the above description, many improvements and other embodiments of the present disclosure will be apparent to those skilled in the art. Therefore, the above description should be construed as merely illustrative and is provided for the purpose of teaching those skilled in the art the best mode for carrying out the present disclosure. Details of the structure and / or function thereof may be substantially modified without departing from the spirit of the present disclosure. [Industrial Applicability]

[0069] One aspect of the present disclosure is applicable to a sublimation gas supply system. [Explanation of symbols]

[0070] 1 Sublimation gas supply system 11 First Container 12 First heating section 13 First Buffer Tank 14 Heating section for first buffer tank 15 First Route 16 Second Path 17 Dilution gas path C1 First connection C2 Second connection C3 Third connection 18 Second Buffer Tank 19 First flow control device 21 Second flow control device 22 Mixer V1 First valve V2 Second valve V3 Third valve 23 Exhaust gas route 24 Third flow control device 25 First emission route 26 Pump 27 Purge gas path 28 Heating section for mixer P1 First pressure gauge P2 Second pressure gauge T1 First thermometer 100 Controller S1 First solid material BP later process P3 Third pressure gauge S2 Second solid material T2 Secondary thermometer C4 Fourth Connection 31 Second Container 32 Second heating section 33 The third route V5 Fifth valve 43 Third Buffer Tank 44 Third heating section 45 The Fourth Path 46 The fifth route 47 6th Route 48 7th Route 49 8th Route 50 9th Route 51 Fourth flow control device

Claims

1. A sublimation gas supply system for supplying a sublimation gas of a solid material to a downstream process, comprising: a first container containing a first solid material; a first heating unit that heats the first container so that the first solid material sublimes to generate a first sublimation gas; a first buffer tank for storing the sublimation gas; a first passage for introducing the first sublimation gas into the first buffer tank; a second passage for supplying the first sublimation gas led out from the first buffer tank to a downstream process; a dilution gas path connected to a first connection portion of the second path for introducing a dilution gas into the second path; a first flow control device provided on the second path between the first connection portion and the first buffer tank for controlling a flow rate; a second flow rate control device provided on the dilution gas path for controlling a flow rate; a first valve provided on the first path; a mixer provided on the second path for mixing the dilution gas and the first sublimation gas joined at the first connection portion, Sublimation gas supply system.

2. 2. The sublimation gas supply system of claim 1, wherein: a second buffer tank provided on the dilution gas path and configured to store the dilution gas; a second valve provided on the second path between the first connection portion and the first buffer tank; a third valve provided on the dilution gas path between the first connection part and the second buffer tank; Sublimation gas supply system.

3. 3. The sublimation gas supply system of claim 2, wherein: a first exhaust path provided on the first path between the first valve and the first buffer tank for exhausting the first sublimation gas from the first buffer tank; a third flow control device provided on the second path between the mixer and the downstream process for controlling a flow rate; An exhaust gas path is provided on the second path between the mixer and the third flow control device, and exhausts gas on the second path. Sublimation gas supply system.

4. 4. A sublimation gas supply system according to any one of claims 1 to 3, wherein a first buffer tank heating unit for heating the first buffer tank; A mixer heating unit for heating the mixer, Sublimation gas supply system.

5. 5. A sublimation gas supply system according to claim 2, further comprising: a second container containing a second solid material; a second heating unit configured to heat the second container so that the second solid material sublimes to generate a second sublimation gas; a third passage for introducing the second sublimation gas into the first buffer tank; Here, the first solid material and the second solid material are the same solid material. Sublimation gas supply system.

6. 5. A sublimation gas supply system according to claim 2, further comprising: a second container containing a second solid material; a second heating unit configured to heat the second container so that the second solid material sublimes to generate a second sublimation gas; a third buffer tank for storing the second sublimation gas; a fourth passage for introducing the second sublimation gas into the third buffer tank; a fifth passage for supplying the second sublimation gas led out from the third buffer tank to the second passage between the mixer and the first buffer tank; a fourth flow control device provided on the fifth path for controlling a flow rate; and a valve provided on the fifth path, wherein the first solid material and the second solid material are different solid materials. Sublimation gas supply system.

7. 7. A sublimation gas supply system according to claim 2, further comprising: a second pressure gauge for measuring a pressure in the first buffer tank; and a controller, wherein: the controller controls, at startup, to open the second valve so that the first sublimation gas flows through the first connection portion when the second pressure gauge reaches a predetermined pressure. Sublimation gas supply system.

8. 7. A sublimation gas supply system according to claim 2, further comprising: and a controller, wherein: The controller controls the second valve and the third valve to be closed in a stop control. Sublimation gas supply system.

9. 7. A sublimation gas supply system according to claim 2, further comprising: and a controller, wherein: The controller controls at least one selected from the group consisting of the first flow rate control device and the second flow rate control device so as to adjust the concentration of the first sublimation gas introduced into the downstream process during steady operation or according to the state of the downstream process. Sublimation gas supply system.

10. A sublimation gas supply method for supplying a sublimation gas of a solid material to a subsequent process, comprising the steps of: a first heating step of heating a first container containing a first solid material to generate a first sublimation gas derived from the first solid material; a first introducing step of introducing the first sublimation gas into a first buffer tank; a first supply step of supplying the first sublimation gas led out from the first buffer tank to a subsequent process; a first dilution step of supplying a dilution gas to the first sublimation gas led out from the first buffer tank; a first flow rate control step of controlling a flow rate of the first sublimation gas led out from the first buffer tank; A second flow rate control step of controlling the flow rate of the dilution gas supplied from the dilution gas path. Sublimation gas supply method.

11. The sublimation gas supply method according to claim 10, a second heating step of heating a second container containing a second solid material to generate a second sublimated gas derived from the second solid material; a second introducing step of introducing the second sublimation gas into a first buffer tank; A first switching step of stopping the first introduction step and switching to the second introduction step, Here, the first solid material and the second solid material are the same solid material. Sublimation gas supply method.

12. The sublimation gas supply method according to claim 10, a second heating step of heating a second container containing a second solid material to generate a second sublimated gas derived from the second solid material; a second introducing step of introducing the second sublimation gas into a third buffer tank; a second supply step of supplying the second sublimation gas led out from the third buffer tank to a subsequent process; a second dilution step of supplying the dilution gas to the second sublimation gas led out from the third buffer tank; a second switching step of stopping the first introduction step and the first supply step and switching to the second introduction step and the second supply step, wherein the first solid material and the second solid material are different solid materials. Sublimation gas supply method.

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