Raw material supply device and raw material supply method

Abstract

To provide a technology capable of heightening a sublimation rate of a solid raw material.SOLUTION: A raw material feeding device in an embodiment has a container for storing solution formed by dissolving a solid raw material into a solvent, or a disperse system formed by dispersing a solid raw material into a disperse medium, an injection part for spraying the solution or the disperse system, and injecting it into the container, and a control part for controlling the spray condition so that a spray direction of the solution or the disperse system sprayed from the injection part is changed in time.SELECTED DRAWING: Figure 1

Description

[Technical field]

[0001] The present disclosure relates to a raw material supplying device and a raw material supplying method. [Background technology]

[0002] A technique is known in which a solid raw material is dissolved in a solvent and sprayed into a processing chamber, the processing chamber is heated to remove the solvent and leave the solid raw material, and then the processing chamber is heated again to sublimate the solid raw material and generate a corresponding gas (see, for example, Patent Document 1). [Prior art documents] [Patent documents]

[0003] [Patent Document 1] JP 2004-115831 A Summary of the Invention [Problem to be solved by the invention]

[0004] The present disclosure provides techniques that can increase the sublimation rate of a solid source material. [Means for solving the problem]

[0005] A raw material supplying device according to one aspect of the present disclosure includes a container for storing a solution in which a solid raw material is dissolved in a solvent or a dispersion in which a solid raw material is dispersed in a dispersion medium, an injection unit for spraying the solution or the dispersion into the container, and a control unit for controlling spray conditions so as to change the spray direction of the solution or the dispersion sprayed from the injection unit over time. death , The spray conditions include a spray pressure. . Effect of the Invention

[0006] According to the present disclosure, the sublimation rate of a solid source material can be increased. [Brief description of the drawings]

[0007] [Figure 1] FIG. 1 is a diagram showing an example of a raw material supply system according to an embodiment. [Diagram 2] FIG. 1 is a diagram for explaining the operation of the raw material supply system of FIG. [Diagram 3] FIG. 2 is a diagram for explaining the operation of the raw material supply system of FIG. 1. [Figure 4] Diagram to explain spray direction (1) [Diagram 5] Diagram to explain spray direction (2) [Figure 6] FIG. 13 is a diagram showing a modified raw material supply device. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0008] Hereinafter, non-limiting exemplary embodiments of the present disclosure will be described with reference to the accompanying drawings. In all of the accompanying drawings, the same or corresponding members or parts are designated by the same or corresponding reference numerals, and duplicated descriptions will be omitted.

[0009] (Raw material supply system) A raw material supply system according to an embodiment will be described with reference to Fig. 1. Fig. 1 is a diagram showing an example of a raw material supply system according to an embodiment.

[0010] The raw material supply system 1 is a system that generates a reactive gas by sublimating a second solid raw material formed by removing the solvent from a solution (hereinafter simply referred to as the "solution") in which a first solid raw material is dissolved in a solvent, and performs film formation in a processing device using the generated reactive gas.

[0011] The first solid source material is not particularly limited, and may be, for example, an organometallic complex containing a metal element such as strontium (Sr), molybdenum (Mo), ruthenium (Ru), zirconium (Zr), hafnium (Hf), tungsten (W), aluminum (Al), etc., or a chloride containing a metal element such as tungsten (W), aluminum (Al), etc. The solvent may be, for example, hexane, as long as it can dissolve the first solid source material to generate a solution.

[0012] The raw material supply system 1 includes a raw material supply source 10, raw material supply devices 30 and 40, a processing device 50, and a control device 90.

[0013] The raw material supply source 10 supplies the solution M1 to the raw material supply devices 30 and 40. The raw material supply source 10 is disposed in, for example, a sub-fab. In this embodiment, the raw material supply source 10 includes a tank 11 and a float sensor 12. The tank 11 is filled with the solution M1. The float sensor 12 detects the amount of the solution M1 filled in the tank 11.

[0014] One end of a pipe L1 is inserted into the raw material supply source 10 from above the tank 11. The other end of the pipe L1 is connected to a carrier gas supply source G1, and the carrier gas is supplied from the supply source G1 into the tank 11 through the pipe L1. The carrier gas may be an inert gas such as nitrogen (N2) or argon (Ar). A valve V1 is provided in the pipe L1. When the valve V1 is opened, the carrier gas is supplied from the supply source G1 to the raw material supply source 10, and when the valve V1 is closed, the supply of the carrier gas from the supply source G1 to the raw material supply source 10 is cut off. A pressure sensor P1 is provided in the pipe L1 to detect the pressure in the pipe L1. The detection value of the pressure sensor P1 is transmitted to the control device 90. In addition, a flow rate controller (not shown) for controlling the flow rate of the carrier gas flowing through the pipe L1, an additional valve, etc. may be provided in the pipe L1.

[0015] The raw material supply source 10 is connected to the raw material supply device 30 via pipes L2 and L3, and supplies the solution M1 to the raw material supply device 30 via the pipes L2 and L3. Valves V2 and V3 are provided in the pipes L2 and L3, respectively. When the valves V2 and V3 are opened, the solution M1 is supplied from the raw material supply source 10 to the raw material supply device 30, and when the valves V2 and V3 are closed, the supply of the solution M1 from the raw material supply source 10 to the raw material supply device 30 is blocked. In addition, a flow rate controller (not shown) for controlling the flow rate of the solution M1 flowing through the pipe L3, an additional valve, etc. may be provided in the pipe L3.

[0016] Furthermore, the raw material supply source 10 is connected to the raw material supply device 40 via pipes L2 and L4, and supplies the solution M1 to the raw material supply device 40 via the pipes L2 and L4. A valve V4 is provided in the pipe L4. When the valves V2 and V4 are opened, the solution M1 is supplied from the raw material supply source 10 to the raw material supply device 40, and when the valves V2 and V4 are closed, the supply of the solution M1 from the raw material supply source 10 to the raw material supply device 40 is blocked. Furthermore, a flow rate controller (not shown) for controlling the flow rate of the solution M1 flowing through the pipe L4, an additional valve, etc. may be provided in the pipe L4.

[0017] The raw material supplying device 30 stores the solution M1 transported from the raw material supply source 10. In this embodiment, the raw material supplying device 30 includes a container 31, an injection part 32, an exhaust port 33, a heating part , and a filter .

[0018] The container 31 stores the solution M1 transported from the raw material supply source 10.

[0019] The injection unit 32 sprays the solution M1 supplied from the raw material supply source 10 via the pipes L2 and L3 and injects it into the container 31. By spraying the solution M1, the injection unit 32 vaporizes the solvent before the solution M1 reaches the filter 35. The injection unit 32 may be, for example, a spray nozzle. The spray nozzle may be fixed to, for example, the ceiling of the container 31, or may be attached to the ceiling of the container 31 so that the direction of the nozzle central axis can be changed.

[0020] The exhaust port 33 is provided below the container 31 and exhausts the inside of the container 31. The processing device 50 is connected to the exhaust port 33 via pipes L10 and L12. In addition, the exhaust port 33 is connected to an exhaust device E1 via pipes L10 and L14.

[0021] The heating unit 34 heats a solid source material (hereinafter referred to as "second solid source material M2") formed by removing the solvent from the solution M1, thereby sublimating the second solid source material M2 to generate a reactive gas. The heating unit 34 may be, for example, a heater disposed to cover the outer periphery of the container 31. The heating unit 34 is configured to be able to heat the inside of the container 31 to a temperature at which the second solid source material M2 can be sublimated to generate a reactive gas.

[0022] The filter 35 is disposed substantially horizontally in the container 31, and divides the inside of the container 31 into a first region 31a and a second region 31b. The first region 31a is provided with an injection section 32. The second region 31b is a region located below the first region 31a. The second region 31b is provided with an exhaust port 33. The filter 35 may be formed of any material that allows the reactive gas to pass through and captures the second solid raw material M2 and impurities such as particles, and may be formed of, for example, a porous material. The porous material may be, for example, a porous metal material such as a sintered body of stainless steel, or a porous ceramic material.

[0023] One end of the pipe L8 is connected to the downstream side of the valve V3 of the pipe L3. The other end of the pipe L8 is connected to a carrier gas supply source G7 via the pipe L7, and the carrier gas is supplied from the supply source G7 into the container 31 via the pipes L7, L8, and L3. The carrier gas may be an inert gas such as N2 or Ar. Valves V8a and V8b are interposed in the pipe L8 in this order from the supply source G7 side. When the valves V8a and V8b are opened, the carrier gas is supplied from the supply source G7 to the raw material supply device 30, and when the valves V8a and V8b are closed, the supply of the carrier gas from the supply source G7 to the raw material supply device 30 is cut off. A flow rate controller F7 that controls the flow rate of the carrier gas flowing through the pipe L7 is interposed in the pipe L7. In this embodiment, the flow rate controller F7 is a mass flow controller (MFC).

[0024] The raw material supplying device 30 is connected to the processing device 50 via pipes L10 and L12, and supplies reactive gas to the processing device 50 via the pipes L10 and L12. Valves V10a to V10c are installed in the pipe L10 in this order from the raw material supplying device 30 side. When the valves V10a to V10c are opened, reactive gas is supplied from the raw material supplying device 30 to the processing device 50, and when the valves V10a to V10c are closed, the supply of reactive gas from the raw material supplying device 30 to the processing device 50 is cut off. The pipe L10 is provided with a pressure sensor P10 that detects the pressure inside the pipe L10. The detection value of the pressure sensor P10 is transmitted to the control device 90.

[0025] One end of the pipe L13 is connected between the valve V10a and the valve V10b of the pipe L10. The other end of the pipe L13 is connected between the valve V8a and the valve V8b of the pipe L8. The pipe L13 functions as a bypass pipe that connects the pipe L8 and the pipe L10 without the raw material supply device 30. The valve V13 is interposed in the pipe L13. When the valve V13 is opened, the pipe L8 and the pipe L10 communicate with each other, and when the valve V13 is closed, the communication between the pipe L8 and the pipe L10 is blocked.

[0026] One end of the pipe L14 is connected between the valve V10b and the valve V10c of the pipe L10. The other end of the pipe L14 is connected to an exhaust device E1 such as a vacuum pump. A pressure control valve V14 is interposed in the pipe L14. When the pressure control valve V14 is opened while the valves V10a and V10b are open, the inside of the container 31 is exhausted and the solvent can be removed from the solution M1 stored in the container 31. When the pressure control valve V14 is closed, the removal of the solvent from the solution M1 stored in the container 31 can be stopped. In addition, the pressure in the container 41 can be controlled by adjusting the opening of the pressure control valve V14.

[0027] The raw material supplying device 40 stores the solution M1 transported from the raw material supply source 10. The raw material supplying device 40 is provided in parallel with the raw material supplying device 30. In this embodiment, the raw material supplying device 40 includes a container 41, an injection unit 42, an exhaust port 43, a heating unit 44, and a filter 45.

[0028] The container 41 stores the solution M1 transported from the raw material supply source 10.

[0029] The injection unit 42 sprays the solution M1 supplied from the raw material supply source 10 via the pipes L2 and L4 and injects it into the container 41. By spraying the solution M1, the injection unit 42 vaporizes the solvent before the solution M1 reaches the filter 45. The injection unit 42 may be, for example, a spray nozzle. The spray nozzle may be fixed to, for example, the ceiling of the container 41, or may be attached to the ceiling of the container 41 so that the direction of the nozzle central axis can be changed.

[0030] The exhaust port 43 is provided below the container 41 and exhausts the inside of the container 41. The processing device 50 is connected to the exhaust port 43 via pipes L11 and L12. In addition, the exhaust port 43 is connected to an exhaust device E2 via pipes L11 and L16.

[0031] The heating unit 44 heats the second solid source material M2 formed by removing the solvent from the solution M1, thereby sublimating the second solid source material M2 to generate a reactive gas. The heating unit 44 may be, for example, a heater arranged to cover the outer periphery of the container 41. The heating unit 44 is configured to be able to heat the inside of the container 41 to a temperature at which the second solid source material M2 can be sublimated to generate a reactive gas.

[0032] The filter 45 is disposed substantially horizontally within the container 41, and divides the inside of the container 41 into a first region 41a and a second region 41b. The first region 41a is provided with an injection section 42. The second region 41b is a region located below the first region 41a. The second region 41b is provided with an exhaust port 43. The filter 45 is formed of the same material as the filter 35, for example.

[0033] One end of the pipe L9 is connected to the downstream side of the valve V4 of the pipe L4. The other end of the pipe L9 is connected to a carrier gas supply source G7 via the pipe L7, and the carrier gas is supplied from the supply source G7 into the container 41 via the pipes L7, L9, and L4. The carrier gas may be an inert gas such as N2 or Ar. The pipe L9 is provided with valves V9a and V9b in this order from the supply source G7 side. When the valves V9a and V9b are opened, the carrier gas is supplied from the supply source G7 to the raw material supply device 40, and when the valves V9a and V9b are closed, the supply of the carrier gas from the supply source G7 to the raw material supply device 40 is blocked.

[0034] The raw material supplying device 40 is connected to the processing device 50 via pipes L11 and L12, and supplies reactive gas to the processing device 50 via the pipes L11 and L12. Valves V11a to V11c are provided in the pipe L11 in this order from the raw material supplying device 40 side. When the valves V11a to V11c are opened, reactive gas is supplied from the raw material supplying device 40 to the processing device 50, and when the valves V11a to V11c are closed, the supply of reactive gas from the raw material supplying device 40 to the processing device 50 is cut off. The pipe L11 is provided with a pressure sensor P11 that detects the pressure inside the pipe L11. The detection value of the pressure sensor P11 is transmitted to the control device 90.

[0035] One end of the pipe L15 is connected between the valve V11a and the valve V11b of the pipe L11. The other end of the pipe L15 is connected between the valve V9a and the valve V9b of the pipe L9. The pipe L15 functions as a bypass pipe that connects the pipe L9 and the pipe L11 without the raw material supply device 40. The valve V15 is interposed in the pipe L15. When the valve V15 is opened, the pipe L9 and the pipe L11 communicate with each other, and when the valve V15 is closed, the communication between the pipe L9 and the pipe L11 is blocked.

[0036] One end of the pipe L16 is connected between the valve V11b and the valve V11c of the pipe L11. The other end of the pipe L16 is connected to an exhaust device E2 such as a vacuum pump. A pressure control valve V16 is interposed in the pipe L16. When the pressure control valve V16 is opened while the valves V11a and V11b are open, the inside of the container 41 is exhausted and the solvent can be removed from the solution M1 stored in the container 41. When the pressure control valve V16 is closed, the removal of the solvent from the solution M1 stored in the container 41 can be stopped. In addition, the pressure in the container 41 can be controlled by adjusting the opening of the pressure control valve V16.

[0037] The processing device 50 is connected to the raw material supply device 30 via pipes L10 and L12, and is supplied with a reactive gas generated by heating and sublimating the second solid raw material M2 in the raw material supply device 30. The processing device 50 is also connected to the raw material supply device 40 via pipes L11 and L12, and is supplied with a reactive gas generated by heating and sublimating the second solid raw material M2 in the raw material supply device 40.

[0038] The processing device 50 performs various processes such as film formation on substrates such as semiconductor wafers using reactive gas supplied from the raw material supply devices 30 and 40. In this embodiment, the processing device 50 includes a processing vessel 51, a flow meter 52, a storage tank 53, a pressure sensor 54, and a valve V12. The processing vessel 51 accommodates one or more substrates. In this embodiment, the flow meter 52 is a mass flow meter (MFM). The flow meter 52 is disposed in the pipe L12 and measures the flow rate of the reactive gas flowing through the pipe L12. The storage tank 53 temporarily stores the reactive gas. By providing the storage tank 53, a large flow rate of reactive gas can be supplied into the processing vessel 51 in a short time. The storage tank 53 is also called a buffer tank or a fill tank. The pressure sensor 54 detects the pressure in the storage tank 53. The pressure sensor 54 is, for example, a capacitance manometer. The valve V12 is disposed in the pipe L12. When the valve V12 is opened, reactive gas is supplied from the source supply devices 30 and 40 to the processing vessel 51, and when the valve V12 is closed, the supply of reactive gas from the source supply devices 30 and 40 to the processing vessel 51 is stopped.

[0039] The control device 90 is an example of a control unit, and controls each part of the raw material supply system 1. For example, the control device 90 controls the operation of the raw material supply source 10, the raw material supply devices 30 and 40, the processing device 50, etc. The control device 90 also controls the opening and closing of various valves. The control device 90 may be, for example, a computer.

[0040] The control device 90 controls the spray conditions so as to change over time the spray direction of the solution M1 sprayed from the injection parts 32, 42. For example, the control device 90 changes the spray conditions continuously to change over time the spray direction of the solution M1 sprayed from the injection parts 32, 42. Also, for example, the control device 90 changes the spray conditions in a stepwise manner to change over time the spray direction of the solution M1 sprayed from the injection parts 32, 42.

[0041] The spray conditions include, for example, the spray pressure, the pressure in the containers 31 and 41, the temperature in the containers 31 and 41, and the direction of the nozzle central axis. For example, the control device 90 controls the spray pressure by adjusting the flow rate of the carrier gas supplied from the supply source G1 into the tank 11 based on the detection value of the pressure sensor P1. For example, the control device 90 controls the pressure in the container 31 by adjusting the aperture of the pressure control valve V14 based on the detection value of the pressure sensor P10. For example, the control device 90 controls the pressure in the container 41 by adjusting the aperture of the pressure control valve V16 based on the detection value of the pressure sensor P11. For example, the control device 90 controls the temperature in the container 31 by adjusting the set temperature of the heating unit 34. For example, the control device 90 controls the temperature in the container 41 by adjusting the set temperature of the heating unit 44. For example, the control device 90 controls the direction of the nozzle central axis of the spray nozzle.

[0042] The spray direction is the direction in which the amount of spray per unit time and unit solid angle is maximum. The spray direction includes, for example, the spray pattern and the spray angle. The spray pattern is the cross-sectional shape of the solution sprayed from the spray nozzle when it spreads. The spray angle is the angle at which the solution sprayed from the spray nozzle spreads.

[0043] (Operation of raw material supply system) 2 and 3, an example of the operation (raw material supplying method) of the raw material supplying system 1 will be described. In the raw material supplying system 1, a control device 90 controls the opening and closing of various valves, so that one of two raw material supplying devices 30, 40 provided in parallel supplies reactive gas to a processing device 50, and the other charges a solid raw material. An example of the operation of the raw material supplying system 1 will be specifically described below.

[0044] First, referring to FIG. 2, a case where the raw material supplying device 30 supplies reactive gas to the processing device 50 and the raw material supplying device 40 fills the solid raw material will be described. FIG. 2 is a diagram for explaining the operation of the raw material supplying system 1 of FIG. 1. In FIG. 2, the pipes through which the carrier gas, the solution M1, and the reactive gas flow are shown by thick solid lines, and the pipes through which the carrier gas, the solution M1, and the reactive gas do not flow are shown by thin solid lines. In FIG. 2, the open state of the valves is shown by outlined symbols, and the closed state of the valves is shown by filled symbols. Note that the raw material supplying system 1 will be described assuming that, in the initial state, all the valves are closed as shown in FIG. 1, and the second solid raw material M2 is stored in the raw material supplying device 30.

[0045] The control device 90 controls the heating unit 34 of the raw material supply device 30 to heat and sublimate the second solid raw material M2 in the container 31 to generate reactive gas (sublimation process). The control device 90 also opens the valves V8a, V8b, V10a to V10c, and V12. This allows a carrier gas to be injected from the supply source G7 through the pipes L7 and L8 into the container 31 of the raw material supply device 30, and the reactive gas generated in the container 31 together with the carrier gas is supplied to the processing container 51 through the pipes L10 and L12. In the sublimation process, the second solid raw material M2 is deposited over a wide area on the inner wall of the container 31 and the filter 35 in the filling and drying process described later, so that the specific surface area of ​​the second solid raw material M2 is large. This allows the sublimation rate of the second solid raw material M2 to be increased.

[0046] 2, the control device 90 opens the valves V1, V2, and V4. This allows the carrier gas to be supplied from the supply source G1 to the raw material supply source 10, and the solution M1 is transported from the raw material supply source 10 to the raw material supply device 40 via the pipes L2 and L4. The solution M1 transported to the raw material supply device 40 is sprayed into the container 41 from the injection part 42. The solution M1 sprayed into the container 41 is deposited on the inner wall of the container 41 and the filter 45 as the second solid raw material M2 due to the evaporation of the solvent. This causes the second solid raw material M2 to be filled into the container 41 of the raw material supply device 40 (filling and drying process).

[0047] In the filling and drying process, the control device 90 controls the spray conditions so that the spray direction of the solution M1 sprayed from the injection part 42 is changed over time.

[0048] 4 and 5 are diagrams for explaining the spray direction. For example, the control device 90 executes a step of spraying the solution M1 under spraying conditions (see FIG. 4) where a large amount of the solution M1 is sprayed onto the upper part of the inner wall of the container 31, and a step of spraying the solution M1 under spraying conditions (see FIG. 5) where a large amount of the solution M1 is sprayed onto the lower part of the inner wall of the container 31. As a result, the solution M1 is sprayed from the injection part 42 over a wide area of ​​the inner wall of the container 41 and the filter 45, so that the second solid raw material M2 is deposited over a wide area of ​​the inner wall of the container 41 and the filter 45.

[0049] In addition, the control device 90 opens the valves V11a, V11b and the pressure control valve V16. As a result, the inside of the container 41 of the raw material supplying device 40 is evacuated by the exhaust device E2, so that the solvent vaporized by spraying the solution M1 into the container 41 is removed.

[0050] Next, referring to FIG. 3, a case where the raw material supplying device 40 supplies reactive gas to the processing device 50 and the raw material supplying device 30 fills the solid raw material will be described. FIG. 3 is a diagram for explaining the operation of the raw material supplying system 1 of FIG. 1. In FIG. 3, the pipes through which the carrier gas, the solution M1, and the reactive gas flow are indicated by thick solid lines, and the pipes through which the carrier gas, the solution M1, and the reactive gas do not flow are indicated by thin solid lines. In addition, in FIG. 3, the open state of the valves is indicated by outlined symbols, and the closed state of the valves is indicated by filled symbols. Note that in the raw material supplying system 1, all the valves are closed in the initial state as shown in FIG. 1. Also, as shown in FIG. 3, the description will be given assuming that the second solid raw material M2 is stored in the raw material supplying device 40.

[0051] The control device 90 controls the heating unit 44 of the raw material supply device 40 to heat and sublimate the second solid raw material M2 in the container 41 to generate reactive gas (sublimation process). The control device 90 also opens the valves V9a, V9b, V11a to V11c, and V12. This allows a carrier gas to be injected from the supply source G7 through the pipes L7 and L9 into the container 41 of the raw material supply device 40, and the reactive gas generated in the container 41 together with the carrier gas is supplied to the processing container 51 through the pipes L11 and L12. In the sublimation process, the second solid raw material M2 is deposited over a wide area on the inner wall of the container 41 and the filter 45 in the filling and drying process described later, so that the specific surface area of ​​the second solid raw material M2 is large. This allows the sublimation rate of the second solid raw material M2 to be increased.

[0052] 3, the control device 90 opens the valves V1, V2, and V3. As a result, a carrier gas is supplied from the supply source G1 to the raw material supply source 10, and the solution M1 is transported from the raw material supply source 10 to the raw material supply device 30 via the pipes L2 and L3. The solution M1 transported to the raw material supply device 30 is sprayed into the container 31 from the injection part 32. The solution M1 sprayed into the container 31 is deposited on the inner wall of the container 31 and the filter 35 as the second solid raw material M2 due to the evaporation of the solvent. As a result, the second solid raw material M2 is filled into the container 31 of the raw material supply device 30 (filling and drying process).

[0053] In the filling and drying process, the control device 90 controls the spraying conditions so as to change over time the spraying direction of the solution M1 sprayed from the injection part 32. As a result, the solution M1 is sprayed from the injection part 32 over a wide area of ​​the inner wall of the container 31 and the filter 35, so that the second solid raw material M2 is deposited over a wide area of ​​the inner wall of the container 31 and the filter 35.

[0054] In addition, the control device 90 opens the valves V10a, V10b and the pressure control valve V14. As a result, the inside of the container 31 of the raw material supplying device 30 is evacuated by the exhaust device E1, so that the solvent vaporized by spraying the solution M1 into the container 31 is removed.

[0055] As described above, according to the embodiment, the control device 90 controls the opening and closing of the valves, so that one of the two raw material supply devices 30, 40 supplies reactive gas to the processing device 50, and the other charges the solid raw material. This enables the raw material supply devices 30, 40 to be automatically replenished with raw material, thereby improving the continuous operation capability of the processing device 50 and improving the availability of the processing device 50.

[0056] Furthermore, according to the embodiment, the control device 90 controls the spray conditions so as to change the spray direction of the solution M1 sprayed from the injection parts 32, 42 over time. As a result, the solution M1 is sprayed from the injection parts 32, 42 over a wide range of the inner walls of the containers 31, 41 and the filters 35, 45, so that the second solid source material M2 is deposited over a wide range of the inner walls of the containers 31, 41 and the filters 35, 45. As a result, the specific surface area of ​​the second solid source material M2 is increased, so that the sublimation rate when the second solid source material M2 is sublimated can be increased.

[0057] Next, a description will be given of a modified example of the raw material supplying device 30. Fig. 6 is a diagram showing the modified raw material supplying device.

[0058] Raw material supplying apparatus 30A of the modified example differs from raw material supplying apparatus 30 in that it further includes a gas discharge unit 36. Note that, since the other points are the same as raw material supplying apparatus 30, the following description will focus on the points that are different from raw material supplying apparatus 30.

[0059] The raw material supplying device 30A includes a container 31, an injection section 32, an exhaust port 33, a heating section , a filter 35, and a gas discharge section .

[0060] The gas discharge part 36 is provided on the ceiling of the container 31. The gas discharge part 36 discharges a counter gas toward the solution M1 sprayed into the container 31. This causes the spray direction of the solution M1 sprayed into the container 31 to change due to the counter gas. In this embodiment, the gas discharge part 36 is provided around the injection part 32. The counter gas may be, for example, the same gas as the carrier gas, for example, an inert gas such as N2 or Ar.

[0061] The control device 90 adjusts conditions such as the flow rate of the counter gas discharged from the gas discharge unit 36, thereby changing the spray direction of the solution M1 sprayed from the injection unit 32 over time. As a result, the solution M1 is sprayed from the injection unit 32 over a wide area of ​​the inner wall of the container 31 and the filter 35, and the second solid source material M2 is deposited over a wide area of ​​the inner wall of the container 31 and the filter 35. As a result, the specific surface area of ​​the second solid source material M2 is increased, and the sublimation rate when the second solid source material M2 is sublimated can be increased.

[0062] In the modified example, the raw material supplying device 30A has been described as a modified example of the raw material supplying device 30, but the same may be true for the modified example of the raw material supplying device 40.

[0063] The embodiments disclosed herein should be considered to be illustrative and not restrictive in all respects. The above-described embodiments may be omitted, substituted, or modified in various forms without departing from the scope and spirit of the appended claims.

[0064] In the above embodiment, the raw material supply system 1 has two raw material supply devices 30, 40 arranged in parallel, but the present disclosure is not limited thereto. For example, the raw material supply device may be one, or three or more raw material supply devices may be arranged in parallel. However, from the viewpoint of eliminating downtime associated with filling the solution M1, it is preferable that the raw material supply device is two or more.

[0065] In the above embodiment, a system has been described in which a reactive gas is generated by sublimating a second solid raw material M2 formed by removing a solvent from a solution M1, and a film is formed in a processing device 50 using the generated reactive gas, but the present disclosure is not limited thereto. For example, instead of the solution M1, a dispersion such as a slurry in which a first solid raw material is dispersed in a dispersion medium, or a colloidal solution in which a first solid raw material is dispersed in a dispersion medium can be used. For example, by using a colloidal solution, a precursor with a higher concentration can be filled than when the solution M1 or a slurry is used. The dispersion includes a slurry and a colloid as subordinate concepts. A slurry is also called a suspension. A colloid includes a colloidal solution as a subordinate concept. A colloidal solution is also called a sol. [Explanation of symbols]

[0066] 30,40 Raw material supply equipment 31,41 container 31a, 41a First Area 31b, 41b Second Area 32,42 Injection part 35,45 Filter 36 Gas outlet 90 Control device 50 Processing equipment E1, E2 exhaust system

Claims

1. a container for storing a solution in which a solid raw material is dissolved in a solvent or a dispersion in which a solid raw material is dispersed in a dispersion medium; an injection unit that sprays the solution or the dispersion into the container; a control unit that controls spray conditions so as to change the spray direction of the solution or the dispersion sprayed from the injection unit over time; having The spray conditions include a spray pressure. Raw material supply equipment.

2. a container for storing a solution in which a solid raw material is dissolved in a solvent or a dispersion in which a solid raw material is dispersed in a dispersion medium; an injection unit that sprays the solution or the dispersion into the container; a control unit that controls spray conditions so as to change the spray direction of the solution or the dispersion sprayed from the injection unit over time; having The spray conditions include a pressure in the container; Raw material supply equipment.

3. a container for storing a solution in which a solid raw material is dissolved in a solvent or a dispersion in which a solid raw material is dispersed in a dispersion medium; an injection unit that sprays the solution or the dispersion into the container; a control unit that controls spray conditions so as to change the spray direction of the solution or the dispersion sprayed from the injection unit over time; having The spray conditions include a temperature in the container. Raw material supply equipment.

4. The control unit continuously changes the spray conditions. The raw material supplying device according to any one of claims 1 to 3.

5. The control unit changes the spray conditions in a stepwise manner. The raw material supplying device according to any one of claims 1 to 3.

6. Further comprising a gas ejection unit that ejects a gas toward the solution or the dispersion system being sprayed in the container. The raw material supplying device according to any one of claims 1 to 5.

7. an exhaust port for exhausting the inside of the container; a filter that divides the inside of the container into a first region including the injection portion and a second region including the exhaust port; Further comprising The raw material supplying device according to any one of claims 1 to 6.

8. The filter is disposed substantially horizontally within the container. The raw material supplying device according to claim 7.

9. The filter is formed of a porous material. The raw material supplying device according to claim 7 or 8.

10. The second region is located below the first region. The raw material supplying device according to any one of claims 7 to 9.

11. The injection section evaporates the solvent or the dispersion medium before the solution or the dispersion reaches the filter. The raw material supplying device according to any one of claims 7 to 10.

12. The exhaust port is connected to a processing device. The raw material supplying device according to any one of claims 7 to 11.

13. The exhaust port is connected to an exhaust device that exhausts the inside of the container. The raw material supplying device according to any one of claims 7 to 12.

14. The dispersion is a slurry or a colloidal solution. A raw material supplying device according to any one of claims 1 to 13.

15. a step of spraying a solution in which a solid raw material is dissolved in a solvent or a dispersion in which a solid raw material is dispersed in a dispersion medium into a container, thereby vaporizing and removing the solvent or the dispersion medium from the solution or the dispersion medium, In the removing step, the spraying conditions including the spraying pressure are controlled so as to change the spraying direction of the solution or the dispersion system over time. Raw material supply method.

16. a step of spraying a solution in which a solid raw material is dissolved in a solvent or a dispersion in which a solid raw material is dispersed in a dispersion medium into a container, thereby vaporizing and removing the solvent or the dispersion medium from the solution or the dispersion medium, In the removing step, spraying conditions including the pressure in the container are controlled so as to change the spray direction of the solution or the dispersion over time. Raw material supply method.

17. a step of spraying a solution in which a solid raw material is dissolved in a solvent or a dispersion in which a solid raw material is dispersed in a dispersion medium into a container, thereby vaporizing and removing the solvent or the dispersion medium from the solution or the dispersion medium, In the removing step, spraying conditions including a temperature in the container are controlled so as to change a spraying direction of the solution or the dispersion system over time. Raw material supply method.

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