WO2021060084A1 - 原料供給装置及び原料供給方法 - Google Patents
原料供給装置及び原料供給方法 Download PDFInfo
- Publication number
- WO2021060084A1 WO2021060084A1 PCT/JP2020/034971 JP2020034971W WO2021060084A1 WO 2021060084 A1 WO2021060084 A1 WO 2021060084A1 JP 2020034971 W JP2020034971 W JP 2020034971W WO 2021060084 A1 WO2021060084 A1 WO 2021060084A1
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- Prior art keywords
- raw material
- container
- material supply
- solution
- solvent
- Prior art date
Links
- 239000002994 raw material Substances 0.000 title claims abstract description 193
- 238000000034 method Methods 0.000 title claims description 17
- 239000002904 solvent Substances 0.000 claims abstract description 64
- 239000007787 solid Substances 0.000 claims abstract description 57
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- 239000002612 dispersion medium Substances 0.000 claims abstract description 21
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 238000001514 detection method Methods 0.000 claims description 36
- 239000000243 solution Substances 0.000 description 90
- 239000002002 slurry Substances 0.000 description 80
- 239000012159 carrier gas Substances 0.000 description 35
- 239000007789 gas Substances 0.000 description 34
- 238000010586 diagram Methods 0.000 description 9
- 238000000926 separation method Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000001636 atomic emission spectroscopy Methods 0.000 description 3
- 238000002347 injection Methods 0.000 description 3
- 239000007924 injection Substances 0.000 description 3
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 239000010937 tungsten Substances 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000004696 coordination complex Chemical class 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- VSZWPYCFIRKVQL-UHFFFAOYSA-N selanylidenegallium;selenium Chemical compound [Se].[Se]=[Ga].[Se]=[Ga] VSZWPYCFIRKVQL-UHFFFAOYSA-N 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 230000008016 vaporization Effects 0.000 description 1
Images
Classifications
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67017—Apparatus for fluid treatment
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/4401—Means for minimising impurities, e.g. dust, moisture or residual gas, in the reaction chamber
- C23C16/4402—Reduction of impurities in the source gas
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/448—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials
- C23C16/4481—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for generating reactive gas streams, e.g. by evaporation or sublimation of precursor materials by evaporation using carrier gas in contact with the source material
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/44—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating
- C23C16/455—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the method of coating characterised by the method used for introducing gases into reaction chamber or for modifying gas flows in reaction chamber
- C23C16/45561—Gas plumbing upstream of the reaction chamber
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/02104—Forming layers
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
- H01L21/04—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer
- H01L21/18—Manufacture or treatment of semiconductor devices or of parts thereof the devices having potential barriers, e.g. a PN junction, depletion layer or carrier concentration layer the devices having semiconductor bodies comprising elements of Group IV of the Periodic Table or AIIIBV compounds with or without impurities, e.g. doping materials
- H01L21/30—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26
- H01L21/31—Treatment of semiconductor bodies using processes or apparatus not provided for in groups H01L21/20 - H01L21/26 to form insulating layers thereon, e.g. for masking or by using photolithographic techniques; After treatment of these layers; Selection of materials for these layers
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67011—Apparatus for manufacture or treatment
- H01L21/67098—Apparatus for thermal treatment
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
- H01L21/67—Apparatus specially adapted for handling semiconductor or electric solid state devices during manufacture or treatment thereof; Apparatus specially adapted for handling wafers during manufacture or treatment of semiconductor or electric solid state devices or components ; Apparatus not specifically provided for elsewhere
- H01L21/67005—Apparatus not specifically provided for elsewhere
- H01L21/67242—Apparatus for monitoring, sorting or marking
- H01L21/67253—Process monitoring, e.g. flow or thickness monitoring
Definitions
- This disclosure relates to a raw material supply device and a raw material supply method.
- the present disclosure provides a technique capable of detecting that the separation of the solvent or dispersion medium contained in the solution or dispersion system and the solid raw material is completed.
- the raw material supply device includes a container for storing a solution in which a first solid raw material is dissolved in a solvent or a dispersion system in which a first solid raw material is dispersed in a dispersion medium, and a container stored in the container.
- the removal portion for forming the second solid raw material by removing the solvent or the dispersion medium from the solution or the dispersion system, and the removal of the solvent or the dispersion medium from the solution or the dispersion system are completed. It has a detection unit for detecting the above and a heating unit for heating the second solid raw material.
- FIG. 6 shows an example of the raw material supply system Diagram showing an example of raw material supply source Diagram showing an example of raw material supply source Diagram showing another example of a raw material source
- FIG. 6 shows an example of end point detection processing
- FIG. 1 is a diagram showing an example of a raw material supply system.
- the raw material supply system 1 includes a raw material supply source 10, a carrier gas supply source 20, raw material supply devices 30 and 40, a processing device 50, and a control device 90.
- the raw material supply source 10 supplies the raw material supply devices 30 and 40 with a solution in which the first solid raw material is dissolved in a solvent or a slurry in which the first solid raw material is dispersed in a solvent (dispersion medium).
- the raw material supply source 10 is not particularly limited as long as it can supply the solution or the slurry M to the raw material supply devices 30 and 40.
- FIG. 2A to 2C are diagrams showing an example of the raw material supply source 10, and is a configuration example in which the raw material supply source 10 supplies a solution obtained by dissolving the first solid raw material in a solvent to the raw material supply devices 30 and 40.
- the raw material supply source 10 includes, for example, as shown in FIG. 2A, a tank 11 filled with the solution LS, a pipe 12 inserted into the tank 11 from above, and a valve 13 interposed in the pipe 12. ..
- the solution LS is supplied from the pipe 12 by pressurizing the solution LS filled in the tank 11 by its own weight. Further, as shown in FIG.
- the raw material supply source 10 is interposed in the tank 11 filled with the solution LS, the pipes 12 and 14 inserted into the tank 11 from above, and the pipes 12 and 14. It may have valves 13, 15.
- the inside of the tank 11 is pressurized by supplying an inert gas such as nitrogen (N 2) into the tank 11 from the pipe 14, and the solution LS is supplied from the pipe 12.
- the raw material supply source 10 includes a tank 11 filled with the solution LS, a pipe 16 connected below the tank 11, and a valve 17 interposed in the pipe 16. May have.
- the solution LS is supplied from below the tank 11 via the pipe 16 by using free fall due to gravity.
- FIG. 3 is a diagram showing another example of the raw material supply source 10, and is a configuration example in which the raw material supply source 10 supplies the slurry in which the first solid raw material is dispersed in a solvent to the raw material supply devices 30 and 40.
- the raw material supply source 10 includes a tank 11 filled with slurry SL, a pipe 12 inserted into the tank 11 from above, a valve 13 interposed in the pipe 12, and a tank 11. It has a shaking table 18 and a shaking table 18 for vibrating.
- the tank 11 placed on the shaking table 18 is vibrated and pressurized by the weight of the slurry SL filled in the tank 11 to supply the slurry SL from the pipe 12. ..
- the raw material supply source 10 is connected to the raw material supply device 30 via the pipes L10 and L11, and the raw material supply device 30 is connected to the raw material supply device 30 via the pipes L10 and L11 with a solution obtained by dissolving the first solid raw material in a solvent or the first.
- a slurry in which a solid raw material is dispersed in a solvent is supplied.
- Valves V11a and V11b are interposed in the pipe L11. When the valves V11a and V11b are opened, the solution or slurry M is supplied from the raw material supply source 10 to the raw material supply device 30, and when the valves V11a and V11b are closed, the solution or slurry M is supplied from the raw material supply source 10 to the raw material supply device 30. It is blocked.
- the pipe L11 may be provided with a flow rate controller (not shown) for controlling the flow rate of the solution or slurry M flowing through the pipe L11, an additional valve, or the like.
- the raw material supply source 10 is connected to the raw material supply device 40 via the pipes L10 and L12, and is a solution obtained by dissolving the first solid raw material in a solvent in the raw material supply device 40 via the pipes L10 and L12. A slurry in which the solid raw material of 1 is dispersed in a solvent is supplied. Valves V12a and V12b are interposed in the pipe L12. When the valves V12a and V12b are opened, the solution or slurry M is supplied from the raw material supply source 10 to the raw material supply device 40, and when the valves V12a and V12b are closed, the solution or slurry M is supplied from the raw material supply source 10 to the raw material supply device 40. It is blocked. Further, the pipe L12 may be provided with a flow rate controller (not shown) for controlling the flow rate of the solution or slurry M flowing through the pipe L12, an additional valve, or the like.
- the first solid raw material is not particularly limited, but is a metal such as strontium (Sr), molybdenum (Mo), ruthenium (Ru), zirconium (Zr), hafnium (Hf), tungsten (W), aluminum (Al) and the like. It may be an organic metal complex containing an element, or a chloride containing a metal element such as tungsten (W) or aluminum (Al).
- a metal such as strontium (Sr), molybdenum (Mo), ruthenium (Ru), zirconium (Zr), hafnium (Hf), tungsten (W), aluminum (Al) and the like. It may be an organic metal complex containing an element, or a chloride containing a metal element such as tungsten (W) or aluminum (Al).
- the solvent may be hexane, for example, as long as it can dissolve or disperse the first solid raw material to produce a solution or slurry M.
- the carrier gas supply source 20 supplies the carrier gas to the raw material supply devices 30 and 40.
- the carrier gas supply source 20 is connected to the pipe L11 via the pipes L20 and L21, and supplies the carrier gas to the raw material supply device 30 via the pipes L20, L21 and L11.
- a valve V21 is interposed in the pipe L21. When the valves V21 and V11b are opened, the carrier gas is supplied from the carrier gas supply source 20 to the raw material supply device 30, and when the valves V21 and V11b are closed, the carrier gas supply from the carrier gas supply source 20 to the raw material supply device 30 is cut off.
- the pipe L21 may be provided with a flow rate controller (not shown) for controlling the flow rate of the carrier gas flowing through the pipe L21, an additional valve, or the like.
- the carrier gas supply source 20 is connected to the pipe L12 via the pipes L20 and L22, and supplies the carrier gas to the raw material supply device 40 via the pipes L20, L22 and L12.
- a valve V22 is interposed in the pipe L22. When the valves V22 and V12b are opened, the carrier gas is supplied from the carrier gas supply source 20 to the raw material supply device 40, and when the valves V22 and V12b are closed, the carrier gas supply from the carrier gas supply source 20 to the raw material supply device 40 is cut off.
- the pipe L22 may be provided with a flow rate controller (not shown) for controlling the flow rate of the carrier gas flowing through the pipe L22, an additional valve, or the like.
- the carrier gas is not particularly limited, but may be, for example , an inert gas such as nitrogen (N 2 ) or argon (Ar).
- the raw material supply device 30 stores a solution in which the first solid raw material is dissolved in a solvent or a slurry in which the first solid raw material is dispersed in the solvent, which is supplied from the raw material supply source 10.
- the raw material supply device 30 includes a container 31, a storage unit 33, a heating unit 35, an exhaust device 37, and a detection unit 39.
- Container 31 stores the solution or slurry M.
- the tip of the pipe L11 is inserted into the container 31 from above, and the solution or slurry M and the carrier gas are supplied through the pipe L11.
- a spray nozzle may be attached to the tip of the pipe L11.
- the tip of the pipe L51 is inserted into the container 31 from above, and the reactive gas generated in the container 31 is supplied to the processing device 50 via the pipe L51.
- the tip of the pipe L30 is inserted into the container 31 from above, and the inside of the container 31 is exhausted through the pipe L30 to remove the solvent from the solution or the slurry M in the container 31.
- the solid raw material M2 of 2 is formed.
- a plurality of storage units 33 are provided in the container 31 to store the solution or the slurry M.
- the storage unit 33 has, for example, a tray shape with an open upper side.
- the heating unit 35 heats the second solid raw material M2 formed by removing the solvent from the solution or the slurry M to sublimate the second solid raw material M2 to generate a reactive gas.
- the heating unit 35 may be, for example, a heater arranged so as to cover the bottom portion and the outer periphery of the container 31.
- the heating unit 35 is configured to be able to heat the inside of the container 31 to a temperature at which the second solid raw material M2 can be sublimated to generate a reactive gas.
- the exhaust device 37 is connected to the container 31 via the pipe L30, and exhausts the inside of the container 31.
- the solvent is removed from the solution or slurry M in the container 31 to form the second solid raw material M2.
- a valve V30 is interposed in the pipe L30. When the valve V30 is opened, the inside of the container 31 is exhausted, and when the valve V30 is closed, the exhaust inside the container 31 is shut off.
- the exhaust device 37 is an example of a removing unit, and includes a pressure regulating valve, a vacuum pump, and the like.
- the detection unit 39 is interposed in the pipe L30, and by analyzing the components contained in the fluid flowing through the pipe L30, whether or not the removal of the solvent from the solution or the slurry M stored in the container 31 is completed. Is detected.
- the detection unit 39 includes at least one of a quadrupole mass spectrometer (QMS: Quadrupole Mass Spectrometer), a quantum cascade laser (QCL: Quantum Cascade Laser), an emission spectroscopic analysis (OES: Optical Emission Spectroscopy), and a pressure gauge. ..
- the pipe L21 for supplying the carrier gas is connected to the pipe L11 for supplying the solution or the slurry M
- the present disclosure is not limited to this.
- the tip of the pipe L21 for supplying the carrier gas may be directly inserted into the container 31.
- the pipe L30 for exhausting the inside of the container 31 is inserted into the container 31 separately from the pipe L51 for supplying the reactive gas to the processing device 50 has been described.
- the present disclosure is not limited to this.
- the pipe L30 for exhausting the inside of the container 31 may be connected to the pipe L51 for supplying the reactive gas to the processing device 50.
- the raw material supply device 40 is provided in parallel with the raw material supply device 30.
- the raw material supply device 40 stores a solution in which the first solid raw material is dissolved in a solvent or a slurry in which the first solid raw material is dispersed in the solvent, which is supplied from the raw material supply source 10.
- the raw material supply device 40 includes a container 41, a storage unit 43, a heating unit 45, an exhaust device 47, and a detection unit 49.
- Container 41 stores the solution or slurry M.
- the tip of the pipe L12 is inserted into the container 41 from above, and the solution or slurry M and the carrier gas are supplied via the pipe L12.
- a spray nozzle may be attached to the tip of the pipe L12.
- the tip of the pipe L52 is inserted into the container 41 from above, and the reactive gas generated in the container 41 is supplied to the processing device 50 via the pipe L52.
- the tip of the pipe L40 is inserted into the container 41 from above, and the inside of the container 41 is exhausted through the pipe L40 to remove the solvent from the solution or the slurry M in the container 41.
- the solid raw material M2 of 2 is formed.
- a plurality of storage units 43 are provided in the container 41 to store the solution or the slurry M.
- the storage unit 43 has, for example, a tray shape with an open upper side.
- the heating unit 45 heats the second solid raw material M2 formed by removing the solvent from the solution or the slurry M to sublimate the second solid raw material M2 to generate a reactive gas.
- the heating unit 45 may be, for example, a heater arranged so as to cover the bottom portion and the outer periphery of the container 41.
- the heating unit 45 is configured to be able to heat the inside of the container 41 to a temperature at which the second solid raw material M2 can be sublimated to generate a reactive gas.
- the exhaust device 47 is connected to the container 41 via the pipe L40, and exhausts the inside of the container 41.
- the solvent is removed from the solution or slurry M in the container 41 to form the second solid raw material M2.
- a valve V40 is interposed in the pipe L40. When the valve V40 is opened, the inside of the container 41 is exhausted, and when the valve V40 is closed, the exhaust inside the container 41 is shut off.
- the exhaust device 47 is an example of a removing unit, and includes a pressure regulating valve, a vacuum pump, and the like.
- the detection unit 49 is interposed in the pipe L40, and by analyzing the components contained in the fluid flowing through the pipe L40, whether or not the removal of the solvent from the solution or the slurry M injected into the container 41 is completed. Is detected.
- the detection unit 49 like the detection unit 39, includes at least one of a QMS, a QCL, an OES, and a pressure gauge.
- the pipe L22 for supplying the carrier gas is connected to the pipe L12 for supplying the solution or the slurry M, but the present disclosure is not limited to this.
- the tip of the pipe L22 for supplying the carrier gas may be directly inserted into the container 41.
- the pipe L40 for exhausting the inside of the container 41 is inserted into the container 41 separately from the pipe L52 for supplying the reactive gas to the processing device 50 has been described.
- the present disclosure is not limited to this.
- the pipe L40 for exhausting the inside of the container 41 may be connected to the pipe L52 for supplying the reactive gas to the processing device 50.
- the processing device 50 is connected to the raw material supply device 30 via the pipes L51 and L50, and the processing device 50 is a reaction generated by heating and sublimating the second solid raw material M2 in the raw material supply device 30. Sex gas is supplied.
- a valve V51 is interposed in the pipe L51. When the valve V51 is opened, the reactive gas is supplied from the raw material supply device 30 to the processing device 50, and when the valve V51 is closed, the supply of the reactive gas from the raw material supply device 30 to the processing device 50 is cut off.
- the processing device 50 is connected to the raw material supply device 40 via the pipes L52 and L50, and the processing device 50 is generated by heating and sublimating the second solid raw material M2 in the raw material supply device 40. Reactive gas is supplied.
- a valve V52 is interposed in the pipe L52. When the valve V52 is opened, the reactive gas is supplied from the raw material supply device 40 to the processing device 50, and when the valve V52 is closed, the supply of the reactive gas from the raw material supply device 40 to the processing device 50 is cut off.
- the processing device 50 executes various processes such as a film forming process on a substrate such as a semiconductor wafer by using the reactive gas supplied from the raw material supply devices 30 and 40.
- the processing device 50 includes a processing container 51, a mass flow meter 52, and a valve 53.
- the processing container 51 accommodates one or more substrates.
- the mass flow meter 52 is interposed in the pipe L50 and measures the flow rate of the reactive gas flowing through the pipe L50.
- the valve 53 is interposed in the pipe L50. When the valves V53 are opened, the reactive gas is supplied from the raw material supply devices 30 and 40 to the processing container 51, and when the valve V53 is closed, the supply of the reactive gas from the raw material supply devices 30 and 40 to the processing container 51 is cut off.
- the control device 90 controls each part of the raw material supply system 1.
- the control device 90 controls the operations of the raw material supply source 10, the carrier gas supply source 20, the raw material supply devices 30, 40, the processing device 50, the exhaust devices 37, 47, the detection units 39, 49, and the like. Further, the control device 90 controls the opening and closing of various valves.
- the control device 90 is an example of a control unit, and may be, for example, a computer.
- End point detection process a process for detecting that the removal of the solvent from the solution or slurry M stored in the containers 31 and 41 of the raw material supply devices 30 and 40 is completed (hereinafter referred to as “end point detection process”). An example will be described.
- FIG. 4 is a flowchart showing an example of the end point detection process.
- the end point detection process in the raw material supply device 30 will be described as an example.
- the end point detection process in the raw material supply device 40 may be the same as the end point detection process in the raw material supply device 30.
- the control device 90 controls the opening and closing of the raw material supply source 10 and various valves to inject the solution or slurry M into the container 31 (step S1).
- the control device 90 controls the opening and closing of the raw material supply source 10 and various valves, for example, after a lapse of a predetermined time, and ends the injection of the solution or the slurry M into the container 31.
- the control device 90 controls the raw material supply source 10 and various valves after, for example, a predetermined amount of solution or slurry M is supplied into the container 31, and the solution into the container 31.
- the injection of the slurry M may be completed.
- the timing at which the injection of the solution or the slurry M into the container 31 is completed in step S1 can be determined based on various conditions.
- control device 90 controls the opening and closing of the exhaust device 37 and various valves to exhaust the inside of the container 31 to start removing the solvent from the solution or the slurry M stored in the container 31. (Step S2).
- the control device 90 acquires the detection result of the detection unit 39, and determines whether or not the removal of the solvent from the solution or the slurry M stored in the container 31 is completed based on the detection result. (Step S3).
- the detection unit 39 is a pressure gauge
- the control device 90 determines that the removal of the solvent from the solution or slurry M stored in the container 31 is completed when the pressure gauge detects a pressure equal to or lower than a predetermined pressure. ..
- the predetermined pressure is determined by, for example, a preliminary experiment.
- step S3 When it is determined in step S3 that the removal of the solvent from the solution or slurry M is completed, the control device 90 controls the opening and closing of the exhaust device 37 and various valves to remove the solvent from the solution or slurry M in the container 31. The removal of the solvent is completed (step S4), and the treatment is completed. On the other hand, if it is determined in step S3 that the removal of the solvent from the solution or slurry M is not completed, the control device 90 returns the process to step S2. That is, step S2 is repeated until the removal of the solvent from the solution or slurry M is completed.
- the control device 90 is stored in the container 31 based on the detection result of the detection unit 39 interposed in the pipe L30 connecting the container 31 and the exhaust device 37. Detects that the removal of the solvent from the solution or slurry M is complete. Thereby, it is possible to detect that the separation of the solvent contained in the solution or slurry M stored in the container 31 and the solid raw material is completed.
- FIG. 5 is a diagram for explaining the operation of the raw material supply system 1.
- the pipe through which the carrier gas, the solution or the slurry M and the reactive gas are flowing is shown by a thick solid line
- the pipe in which the carrier gas, the solution or the slurry M and the reactive gas are not flowing is shown by a thin solid line.
- the valves V11a, V11b, V12a, V12b, V21, V22, V30, V40, V51, and V52 are all closed in the initial state. .. Further, it is assumed that the second solid raw material M2 is stored in the raw material supply device 30.
- the control device 90 controls the heating unit 35 of the raw material supply device 30 to heat and sublimate the second solid raw material M2 stored in the storage unit 33 in the container 31 to generate a reactive gas. Further, the control device 90 opens the valves V21, V11b, and V51. As a result, the carrier gas is injected from the carrier gas supply source 20 into the container 31 of the raw material supply device 30 via the pipes L20, L21, and L11, and the reactive gas generated in the container 31 together with the carrier gas is discharged from the pipe L51. It is supplied to the processing device 50 via L50. Further, the control device 90 opens the valves V12a and V12b.
- the solution or slurry M is injected from the raw material supply source 10 into the raw material supply device 40 via the pipes L10 and L12, and the solution or slurry M is stored in the storage unit 43 in the container 41 of the raw material supply device 40.
- the control device 90 closes the valves V12a and V12b and opens the valve V40.
- the inside of the container 41 is exhausted by the exhaust device 47, and the solvent is removed from the solution or slurry M stored in the container 41.
- the control device 90 acquires the detection result of the detection unit 49, and determines whether or not the removal of the solvent from the solution or the slurry M stored in the container 41 is completed based on the detection result. ..
- the control device 90 closes the valve V40. As a result, the exhaust in the container 41 by the exhaust device 47 is cut off.
- the raw material supply device 40 supplies the reactive gas to the processing device 50.
- the case of supplying and switching to the state of filling the solid raw material with the raw material supply device 30 will be described.
- the switching for example, the removal of the solvent from the solution or slurry M stored in the container 31 of the raw material supply device 30 is completed, and the second solid raw material M2 stored in the container 41 of the raw material supply device 40 is completed. Is executed when the remaining amount of is less than a predetermined value.
- FIG. 6 is a diagram for explaining the operation of the raw material supply system 1.
- the pipe through which the carrier gas, the solution or the slurry M and the reactive gas are flowing is shown by a thick solid line
- the pipe in which the carrier gas, the solution or the slurry M and the reactive gas are not flowing is shown by a thin solid line.
- the raw material supply system 1 will be described as assuming that the valves V11b, V21, and V51 are open and the valves V11a, V12a, V12b, V22, V30, V40, and V52 are closed before switching.
- control device 90 turns off the heating unit 35 of the raw material supply device 30 and closes the valves V11b, V21, and V51. As a result, the supply of the reactive gas from the raw material supply device 30 to the processing device 50 is stopped.
- the control device 90 subsequently controls the heating unit 45 of the raw material supply device 40 to heat and sublimate the second solid raw material M2 stored in the storage unit 43 in the container 41 to produce the reactive gas. Generate. Further, the control device 90 opens the valves V22, V12b, and V52. As a result, the carrier gas is injected from the carrier gas supply source 20 into the container 41 of the raw material supply device 40 via the pipes L20, L22, L12, and the reactive gas generated in the container 41 together with the carrier gas is discharged into the pipe L52, It is supplied to the processing device 50 via L50. Further, the control device 90 opens the valves V11a and V11b.
- the solution or slurry M is injected from the raw material supply source 10 into the raw material supply device 30 via the pipes L10 and L11, and the solution or slurry M is stored in the storage unit 33 in the container 31 of the raw material supply device 30.
- the control device 90 closes the valves V11a and V11b and opens the valve V30.
- the inside of the container 31 is exhausted by the exhaust device 37, and the solvent is removed from the solution or slurry M stored in the container 31.
- the control device 90 acquires the detection result of the detection unit 39, and determines whether or not the removal of the solvent from the solution or the slurry M stored in the container 31 is completed based on the detection result. ..
- the control device 90 closes the valve V30. As a result, the exhaust in the container 31 by the exhaust device 37 is cut off.
- the control device 90 controls the opening and closing of various valves to supply the reactive gas to the processing device 50 from one of the two raw material supply devices 30 and 40.
- the solid raw material is filled.
- the raw material supply devices 30 and 40 can be automatically replenished with raw materials, the continuous operation capacity of the processing device 50 can be improved, and the operating rate of the processing device 50 can be improved.
- the control device 90 is a solution stored in the container 31 based on the detection result of the detection unit 39 interposed in the pipe L30 connecting the container 31 and the exhaust device 37. Alternatively, it is detected that the removal of the solvent from the slurry M is completed. Thereby, it is possible to detect that the separation of the solvent contained in the solution or slurry M stored in the container 31 and the solid raw material is completed.
- the control device 90 is a solution stored in the container 41 based on the detection result of the detection unit 49 interposed in the pipe L40 connecting the container 41 and the exhaust device 47. Alternatively, it is detected that the removal of the solvent from the slurry M is completed. Thereby, it can be detected that the separation of the solvent contained in the solution or slurry M stored in the container 41 and the solid raw material is completed.
- a solution in which the first solid raw material is dissolved in a solvent or a slurry in which the first solid raw material is dispersed in a dispersion medium has been described as an example.
- a dispersion system such as a colloidal solution in which the first solid raw material is dispersed in a dispersion medium
- Dispersions include slurries and colloids as subordinate concepts.
- the slurry is also referred to as a suspension.
- Colloid includes a colloidal solution as a subordinate concept.
- Colloidal solutions are also referred to as sol.
- Raw material supply system 30 Raw material supply device 31 Container 33 Storage unit 35 Heating unit 40 Raw material supply device 41 Container 43 Storage unit 45 Heating unit
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Abstract
Description
図1は、原料供給システムの一例を示す図である。図1に示されるように、原料供給システム1は、原料供給源10と、キャリアガス供給源20と、原料供給装置30,40と、処理装置50と、制御装置90と、を備える。
図4を参照し、原料供給装置30,40の容器31,41内に貯留された溶液又はスラリーMからの溶媒の除去が完了したことを検知する処理(以下「終点検知処理」という。)の一例について説明する。図4は、終点検知処理の一例を示すフローチャートである。以下、原料供給装置30における終点検知処理を例示して説明する。ただし、原料供給装置40における終点検知処理についても原料供給装置30における終点検知処理と同様であってよい。
原料供給システム1の動作(原料供給方法)の一例について説明する。原料供給システム1では、制御装置90が各種のバルブの開閉を制御することで、並列に設けられた2つの原料供給装置30,40のうちの一方で処理装置50への反応性ガスの供給を行い、他方で固体原料の充填を行う。以下、原料供給システム1の動作の一例について具体的に説明する。
30 原料供給装置
31 容器
33 貯留部
35 加熱部
40 原料供給装置
41 容器
43 貯留部
45 加熱部
Claims (6)
- 第1の固体原料を溶媒に溶解した溶液又は第1の固体原料を分散媒に分散させた分散系を貯留する容器と、
前記容器内に貯留された前記溶液又は前記分散系から前記溶媒又は前記分散媒を除去することにより第2の固体原料を形成する除去部と、
前記溶液又は前記分散系からの前記溶媒又は前記分散媒の除去が完了したことを検知する検知部と、
前記第2の固体原料を加熱する加熱部と、
を有する、原料供給装置。 - 前記除去部は、前記容器内を排気する排気装置を含み、
前記検知部は、前記容器と前記排気装置とを接続する配管に介設されている、
請求項1に記載の原料供給装置。 - 前記検知部は、QMS、QCL、OES、圧力ゲージの少なくともいずれかを含む、
請求項1又は2に記載の原料供給装置。 - 前記容器内に設けられ、前記溶液又は前記分散系を貯留する複数の貯留部を更に有する、
請求項1乃至3のいずれか一項に記載の原料供給装置。 - 制御部を更に有し、
前記制御部は、
前記溶液又は前記分散系を前記容器に注入するステップと、
前記容器内に注入された前記溶液又は前記分散系から前記溶媒又は前記分散媒を除去するステップと、
前記溶液又は前記分散系からの前記溶媒又は前記分散媒の除去が完了したか否かを判定するステップと、
を実行するように、前記除去部及び前記検知部を制御するように構成される、
請求項1乃至4のいずれか一項に記載の原料供給装置。 - 第1の固体原料を溶媒に溶解した溶液又は第1の固体原料を分散媒に分散させた分散系を容器に注入するステップと、
前記容器内に注入された前記溶液又は前記分散系から前記溶媒又は前記分散媒を除去するステップと、
前記溶液又は前記分散系からの前記溶媒又は前記分散媒の除去が完了したか否かを判定するステップと、
前記判定するステップにおいて前記溶媒又は前記分散媒の除去が完了したと判定された場合、前記溶液又は前記分散系から前記溶媒又は前記分散媒を除去することにより形成された第2の固体原料を加熱するステップと、
を有する、原料供給方法。
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US17/761,067 US11965242B2 (en) | 2019-09-24 | 2020-09-15 | Raw material supply apparatus and raw material supply method |
JP2021548839A JP7282188B2 (ja) | 2019-09-24 | 2020-09-15 | 原料供給装置及び原料供給方法 |
CN202080064398.9A CN114402092A (zh) | 2019-09-24 | 2020-09-15 | 原料供给装置和原料供给方法 |
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