Substrate processing apparatus, gas supply system, substrate processing method, semiconductor device manufacturing method and program

Abstract

Provided is a technique capable of stably controlling the flow rate of a gas species, the flow rate of which is difficult to control in MFC. Thus, this substrate treatment device comprises: a treatment container for housing a substrate; a first gas pipe that supplies a treatment gas to the treatment container; a flow rate measurement unit that is provided to the first gas pipe, and that measures the flow rate of the treatment gas flowing inside the first gas pipe; a second gas pipe that is connected to the first gas pipe, and that supplies a first inert gas to a tank that retains a raw material for the treatment gas; a first flow rate adjustment unit that is provided to the second gas pipe, and that adjusts the flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; and a control unit that is configured to be capable of controlling the first flow rate adjustment unit and the first heating unit on the basis of flow rate data of the treatment gas measured by the flow rate measurement unit, so as to perform a process of supplying, to the substrate in the treatment container, the treatment gas for which at least one of the flow rate of the first inert gas and the temperature of the first inert gas is adjusted such that the flow rate of the treatment gas is a predetermined flow rate.

Description

[Technical Field]

[0001] The present disclosure relates to a substrate processing apparatus, a gas supply system, a substrate processing method, a method for manufacturing a semiconductor device, and a program. [Background technology]

[0002] A gas supply system using a mass flow controller (MFC) is used to control the flow rate of gas supplied to a reaction chamber of a substrate processing apparatus. An example of such a gas supply system is described in Patent Document 1, for example. [Prior art documents] [Patent documents]

[0003] [Patent Document 1] Japanese Patent Application Laid-Open No. 2017-045880 Summary of the Invention [Problem to be solved by the invention]

[0004] The present disclosure provides a technology that enables stable flow rate control even for gas species that are difficult to control in flow rate in an MFC. [Means for solving the problem]

[0005] According to one aspect of the present disclosure, there is provided a technology including: a processing vessel for accommodating a substrate; a first gas pipe for supplying a processing gas to the processing vessel; a flow rate measuring unit provided in the first gas pipe for measuring the flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe for supplying a first inert gas to a tank storing a raw material for the processing gas; a first flow rate adjusting unit provided in the second gas pipe for adjusting the flow rate of the first inert gas; a first heating unit for adjusting the temperature of the first inert gas; and a control unit configured to be capable of controlling the first flow rate adjusting unit and the first heating unit to perform a process of supplying a processing gas to a substrate in the processing vessel, the processing gas having at least one of the flow rate and the temperature of the first inert gas adjusted so that the flow rate of the processing gas becomes a predetermined flow rate based on flow rate data of the processing gas measured by the flow rate measuring unit. [Effects of the Invention]

[0006] According to the above configuration, it is possible to provide a technology that enables stable flow rate control even for gas species that are difficult to control the flow rate of in an MFC. [Brief explanation of the drawings]

[0007] [Figure 1] 1 is a longitudinal cross-sectional view showing an outline of a vertical processing furnace of a substrate processing apparatus according to an embodiment of the present disclosure. [Figure 2] FIG. 2 is a schematic cross-sectional view taken along the line AA in FIG. [Figure 3] 1 is a schematic configuration diagram of a gas supply system according to an embodiment of the present disclosure. [Figure 4] FIG. 2 is a schematic configuration diagram of a controller of a substrate processing apparatus according to an embodiment of the present disclosure, showing a control system of the controller in a block diagram. [Figure 5] 1 is a flowchart illustrating a substrate processing process according to an embodiment of the present disclosure. DETAILED DESCRIPTION OF THE INVENTION

[0008] The following description will be made with reference to Figures 1 to 5. Note that all drawings used in the following description are schematic, and the dimensional relationships, ratios, etc. of elements shown in the drawings do not necessarily match those of reality. Furthermore, the dimensional relationships, ratios, etc. of elements between multiple drawings do not necessarily match.

[0009] (1) Configuration of the substrate processing equipment The substrate processing apparatus 10 includes a processing furnace 202 provided with a heater 207 as a heating means (heating mechanism, heating system). The heater 207 has a cylindrical shape and is installed vertically by being supported by a heater base (not shown) as a holding plate.

[0010] [Outer tube (outer cylinder, outer pipe) 203] An outer tube (also referred to as an outer cylinder or outer tube) 203, which constitutes a reaction vessel (processing vessel), is disposed concentrically inside the heater 207. The outer tube 203 is made of a heat-resistant material such as quartz (SiO2) or silicon carbide (SiC) and has a cylindrical shape with a closed upper end and an open lower end. A manifold (inlet flange) 209 is disposed concentrically below the outer tube 203. The manifold 209 is made of a metal such as stainless steel (SUS) and has a cylindrical shape with open upper and lower ends. An O-ring 220a is provided as a sealing member between the upper end of the manifold 209 and the outer tube 203. The manifold 209 is supported by a heater base, so that the outer tube 203 is installed vertically.

[0011] [Inner tube (inner cylinder, inner pipe) 204] An inner tube (also called an inner cylinder or inner tube) 204 that constitutes a reaction vessel is disposed inside the outer tube 203. The inner tube 204 is made of a heat-resistant material such as quartz (SiO2) or silicon carbide (SiC), and is formed in a cylindrical shape with a closed upper end and an open lower end. The outer tube 203, the inner tube 204, and the manifold 209 mainly constitute a processing vessel (reaction vessel). A processing chamber 201 is formed in the cylindrical hollow portion of the processing vessel (inside the inner tube 204).

[0012] [Substrate support (boat) 217] The processing chamber 201 is configured to accommodate wafers 200 as substrates arranged in multiple vertical stages in a horizontal position using a boat 217 (described later). Nozzles 410 (first nozzle) and 420 (second nozzle) are provided in the processing chamber 201 so as to penetrate the sidewall of the manifold 209 and the inner tube 204. Gas supply pipes 310 and 320 serving as gas supply lines are connected to the nozzles 410 and 420, respectively. Thus, the substrate processing apparatus 10 is provided with two nozzles 410 and 420 and two gas supply pipes 310 and 320, and is configured to be able to supply multiple types of gases into the processing chamber 201. However, the processing furnace 202 of this embodiment is not limited to the above-described configuration.

[0013] [Gas supply section] The gas supply pipes 310 and 320 are connected to the gas supply system shown in Fig. 3. The gas supply system will be described in detail later.

[0014] Nozzles 410 and 420 are connected to the tips of the gas supply pipes 310 and 320, respectively. The nozzles 410 and 420 are configured as L-shaped nozzles, and their horizontal portions are provided so as to penetrate the side wall of the manifold 209 and the inner tube 204. The vertical portions of the nozzles 410 and 420 are provided inside the channel-shaped (groove-shaped) preliminary chamber 201a that protrudes radially outward from the inner tube 204 and extends vertically, and are provided in the preliminary chamber 201a facing upward (upward in the arrangement direction of the wafers 200) along the inner wall of the inner tube 204. The nozzles 410 and 420 are also arranged outside the opening 201b of the preliminary chamber 201a.

[0015] The nozzles 410 and 420 are provided to extend from a lower region of the processing chamber 201 to an upper region of the processing chamber 201, and are provided with a plurality of gas supply holes 410a and 420a, respectively, at positions facing the wafer 200. This allows processing gas to be supplied to the wafer 200 from the gas supply holes (openings) 410a and 420a of the nozzles 410 and 420, respectively.

[0016] A plurality of gas supply holes 410a are provided from the bottom to the top of the inner tube 204, each having the same opening area and arranged at the same opening pitch. However, the gas supply holes 410a are not limited to the above-described form. For example, the opening area may gradually increase from the bottom to the top of the inner tube 204. This makes it possible to more uniform the flow rate of gas supplied from the gas supply holes 410a.

[0017] A plurality of gas supply holes 420a are provided from the bottom to the top of the inner tube 204, each having the same opening area and arranged at the same opening pitch. However, the gas supply holes 420a are not limited to the above-described form. For example, the opening area may gradually increase from the bottom to the top of the inner tube 204. This makes it possible to more uniform the flow rate of gas supplied from the gas supply holes 420a.

[0018] The gas supply holes 410a, 420a of the nozzles 410, 420 are provided at a plurality of positions at a height from the bottom to the top of the boat 217, which will be described later. Therefore, the process gas supplied from the gas supply holes 410a, 420a of the nozzles 410, 420 into the process chamber 201 is supplied to the wafers 200 accommodated from the bottom to the top of the boat 217, i.e., to the entire area of ​​the wafers 200 accommodated in the boat 217. The nozzles 410, 420 may be provided so as to extend from the bottom region to the top region of the process chamber 201, but are preferably provided so as to extend to near the ceiling of the boat 217.

[0019] From the gas supply pipe 310, a source gas containing a first metal element (first metal-containing gas, first source gas) is supplied as a processing gas into the processing chamber 201 via a nozzle 410.

[0020] A reactive gas serving as a processing gas is supplied from the gas supply pipe 320 into the processing chamber 201 via a nozzle 420 .

[0021] In this embodiment, a raw material gas, which is a metal-containing gas, is supplied into the processing chamber 201 through the gas supply hole 410a of the nozzle 410, and a reactive gas is supplied into the processing chamber 201 through the gas supply hole 420a of the nozzle 420, whereby the raw material gas (metal-containing gas) and the reactive gas are supplied to the surface of the wafer 200, and a metal-containing film is formed on the surface of the wafer 200.

[0022] Further, an inert gas can be supplied into the processing chamber 201 through the nozzles 410 and 420. Note that, although an example in which N2 gas is used as the inert gas will be described below, other than N2 gas, a rare gas such as argon (Ar) gas, helium (He) gas, neon (Ne) gas, or xenon (Xe) gas may also be used as the inert gas.

[0023] In the gas supply method of this embodiment, gas is transported via nozzles 410, 420 arranged in a vertically elongated annular space defined by the inner wall of the inner tube 204 and the ends of the multiple wafers 200, i.e., in a cylindrical space called a pre-chamber 201a. Gas is then ejected into the inner tube 204 from multiple gas supply holes 410a, 420a provided in the nozzles 410, 420 at positions facing the wafers. More specifically, source gas and the like are ejected from the gas supply hole 410a of the nozzle 410 and the gas supply hole 420a of the nozzle 420 in a direction parallel to the surface of the wafer 200, i.e., in the horizontal direction.

[0024] [Exhaust section] The exhaust hole (exhaust port) 204a is a through-hole formed in the sidewall of the inner tube 204 at a position facing the nozzles 410 and 420, i.e., at a position 180 degrees opposite the preliminary chamber 201a, and is, for example, a vertically elongated slit-shaped through-hole. Therefore, gas supplied from the gas supply holes 410a and 420a of the nozzles 410 and 420 into the processing chamber 201 and flowing over the surface of the wafer 200, i.e., remaining gas, flows through the exhaust hole 204a into the exhaust path 206 formed by the gap formed between the inner tube 204 and the outer tube 203. The gas flowing into the exhaust path 206 then flows into the exhaust pipe 231 and is discharged to the outside of the processing furnace 202. Note that the exhaust unit is composed of at least the exhaust pipe 231.

[0025] The exhaust hole 204a is provided at a position facing the plurality of wafers 200 (preferably at a position facing the upper and lower portions of the boat 217), and the gas supplied from the gas supply holes 410a and 420a to the vicinity of the wafers 200 in the processing chamber 201 flows horizontally, i.e., in a direction parallel to the surfaces of the wafers 200, and then flows into the exhaust path 206 through the exhaust hole 204a. That is, the gas remaining in the processing chamber 201 is exhausted parallel to the main surfaces of the wafers 200 through the exhaust hole 204a. Note that the exhaust hole 204a is not limited to being configured as a slit-shaped through-hole, and may be configured as a plurality of holes.

[0026] The manifold 209 is provided with an exhaust pipe 231 that exhausts the atmosphere inside the processing chamber 201. The exhaust pipe 231 is connected to, in order from upstream, a pressure sensor 245 serving as a pressure detector (pressure detection unit) that detects the pressure inside the processing chamber 201, an APC (Auto Pressure Controller) valve 243, and a vacuum pump 246 serving as a vacuum exhaust device. The APC valve 243 can evacuate and stop the evacuation of the processing chamber 201 by opening and closing the valve while the vacuum pump 246 is operating. Furthermore, the pressure inside the processing chamber 201 can be adjusted by adjusting the valve opening while the vacuum pump 246 is operating. An exhaust system, i.e., an exhaust line, is mainly composed of the exhaust hole 204a, the exhaust path 206, the exhaust pipe 231, the APC valve 243, and the pressure sensor 245. The vacuum pump 246 may be included in the exhaust system.

[0027] As shown in FIG. 1 , a seal cap 219 serving as a furnace port cover capable of airtightly closing the lower end opening of the manifold 209 may be provided below the manifold 209. The seal cap 219 is configured to abut against the lower end of the manifold 209 from below in the vertical direction. The seal cap 219 is made of a metal such as SUS and is formed in a disk shape. An O-ring 220b serving as a sealing member abutting against the lower end of the manifold 209 is provided on the upper surface of the seal cap 219. A rotation mechanism 267 is provided on the opposite side of the seal cap 219 from the processing chamber 201, rotating the boat 217 that accommodates the wafers 200. A rotation shaft 255 of the rotation mechanism 267 is connected to the boat 217 through the seal cap 219. The rotation mechanism 267 is configured to rotate the boat 217 to rotate the wafers 200. The seal cap 219 is configured to be raised and lowered in the vertical direction by a boat elevator 115 serving as an elevating mechanism installed vertically outside the outer tube 203. The boat elevator 115 is configured to be able to load and unload the boat 217 into and out of the processing chamber 201 by lifting and lowering the seal cap 219. The boat elevator 115 is configured as a transfer device (transfer mechanism) that transfers the boat 217 and the wafers 200 accommodated in the boat 217 into and out of the processing chamber 201.

[0028] The boat 217, which serves as a substrate support, is configured to support a plurality of wafers 200, for example, 25 to 200 wafers 200, in a horizontal position, aligned vertically with their centers aligned, and arranged in multiple stages, i.e., spaced apart. The boat 217 is made of a heat-resistant material such as quartz or SiC. A heat insulating section 218, also made of a heat-resistant material such as quartz or SiC, is provided at the bottom of the boat 217. This configuration makes it difficult for heat from the heater 207 to be transmitted to the seal cap 219.

[0029] 2, a temperature sensor 263 is installed in the inner tube 204 as a temperature detector, and the amount of power supplied to the heater 207 is adjusted based on temperature information detected by the temperature sensor 263, thereby achieving a desired temperature distribution within the processing chamber 201. The temperature sensor 263 is configured in an L-shape, similar to the nozzles 410 and 420, and is installed along the inner wall of the inner tube 204.

[0030] This configuration maintains a uniform temperature at least in the region of the boat 217 that supports the wafers 200. There is a difference in temperature between this uniform temperature region (uniform temperature region T1) and the region below T1. T1 is also referred to as the substrate processing region. The vertical length of the substrate processing region is configured to be equal to or shorter than the vertical length of the uniform temperature region. The substrate processing region refers to the position in the vertical direction of the boat 217 where the wafers 200 are placed. Here, the wafers 200 refer to at least one of product wafers, dummy wafers, and fill dummy wafers. The substrate processing region refers to the region of the boat 217 that holds the wafers 200. In other words, the substrate processing region is also referred to as the substrate holding region.

[0031] 4, the controller 121, which is a control unit (control means), is configured as a computer including a CPU (Central Processing Unit) 121a, a RAM (Random Access Memory) 121b, a storage device 121c, and an I / O port 121d. The RAM 121b, the storage device 121c, and the I / O port 121d are configured to be able to exchange data with the CPU 121a via an internal bus. An input / output device 122, which is configured as, for example, a touch panel, is connected to the controller 121.

[0032] The storage device 121c is composed of, for example, a flash memory, an HDD (Hard Disk Drive), etc. The storage device 121c readably stores a control program for controlling the operation of the substrate processing apparatus, a process recipe describing the procedures and conditions of a semiconductor device manufacturing method (described later), and the like. The process recipe is a combination of processes (steps) in a semiconductor device manufacturing method (described later) that are executed by the controller 121 to obtain a predetermined result, and functions as a program. Hereinafter, the process recipe, control program, etc. are collectively referred to simply as a program. In this specification, the term "program" may refer to a process recipe alone, a control program alone, or a combination of a process recipe and a control program. The RAM 121b is configured as a memory area (work area) for temporarily storing programs, data, etc. read by the CPU 121a.

[0033] The I / O port 121d is connected to the MFCs 315b, 315c, 315d, 325a, and 325b, the valves 314a, 314b, 314c, 314d, 316, 318, 320, 324a, and 324b, the pressure sensor 245, etc. The I / O port 121d is also connected to the APC valve 243, the vacuum pump 246, the heater 207, the temperature sensor 263, the rotation mechanism 267, the boat elevator 115, etc.

[0034] The CPU 121a is configured to read and execute a control program from the storage device 121c, and to read a recipe or the like from the storage device 121c in response to input of an operation command from the input / output device 122. The CPU 121a is configured to be able to control the flow rate adjustment of various gases by the MFCs 315b, 315c, 315d, 325a, and 325b, and the opening and closing operations of the valves 314a, 314b, 314c, 314d, 316, 318, 320, 324a, and 324b, in accordance with the contents of the read recipe. The CPU 121a is also configured to control the opening and closing operation of the APC valve 243, the pressure adjustment operation by the APC valve 243 based on the pressure sensor 245, the temperature adjustment operation of the heater 207 based on the temperature sensor 263, the start and stop of the vacuum pump 246, etc. The CPU 121a is also configured to control the rotation and rotation speed adjustment of the boat 217 by the rotation mechanism 267, the lifting and lowering of the boat 217 by the boat elevator 115, the storing of the wafers 200 in the boat 217, and the like.

[0035] The controller 121 can be configured by installing the above-mentioned program stored in an external storage device 123 (for example, a magnetic tape, a magnetic disk such as a flexible disk or a hard disk, an optical disk such as a CD or a DVD, a magneto-optical disk such as an MO, or a semiconductor memory such as a USB memory or a memory card) into a computer. The storage device 121c and the external storage device 123 are configured as computer-readable recording media. Hereinafter, these will be collectively referred to simply as recording media. In this specification, the recording medium may include only the storage device 121c, only the external storage device 123, or both. The program may be provided to the computer using a communication means such as the Internet or a dedicated line, without using the external storage device 123.

[0036] (2) Gas supply system configuration Next, the gas supply system (source gas supply system) according to this embodiment will be specifically described. As shown in Fig. 3, the gas supply system 12 includes a source gas supply system 300 and a reactive gas supply system 400. First, the source gas supply system 300 will be described.

[0037] [Raw gas supply system] (raw materials) In the present disclosure, the raw material is a material having vapor pressure characteristics such that the saturated vapor pressure is 0.01 to 100 KPa at 50°C to 200°C. More preferably, the raw material is a material having low vapor pressure characteristics such that the saturated vapor pressure is 0.01 to 5 KPa at 50°C to 200°C. A material having such relatively low vapor pressure characteristics is called a low vapor pressure material (low vapor pressure raw material). In the present disclosure, the raw material present in the tank 313 may be in a solid, liquid, or gaseous state. The raw material may be a material that is in a solid state at room temperature and pressure and also a low vapor pressure material.

[0038] The raw material may be, for example, a material containing a metal element and a halogen element. The metal element may be selected from Al, Mo, W, Hf, Zr, etc. The halogen element may be selected from F, Cl, Br, I, etc. Examples of raw materials that are solid at room temperature and atmospheric pressure include AlCl3, Al2Cl6, MoCl5, WCl6, HfCl4, ZrCl4, MoO2Cl2, and MoOCl4. Examples of raw materials that are liquid at room temperature and atmospheric pressure include metal element raw materials such as Ru and La.

[0039] When using such raw materials, a problem arises in that a normal mass flow controller cannot stably adjust the flow rate. The raw material supply system of the present disclosure makes it possible to stably adjust the flow rate, and even if the state of the raw material in the tank 313 (amount or surface state of the raw material) changes, it is possible to adjust the flow rate of the raw material and supply it stably. Details of the raw material supply system are described below.

[0040] (tank) The raw material is stored inside the tank 313. The tank 313 vaporizes or sublimates the raw material to generate a raw material gas. For convenience of explanation, the phase change of the raw material into a gas will be referred to simply as "vaporization" in this specification unless otherwise specified, without distinguishing between "vaporization or sublimation."

[0041] The tank 313 is provided with a heater 317b as a second heating unit, and the amount of vaporization of the raw material is controlled by adjusting the temperature of the tank 313. The temperature of the tank 313 can be changed for each substrate processing.

[0042] (First Gas Pipe) A gas supply pipe 310 (310a), which corresponds to the first gas pipe of the present disclosure, is connected between the tank 313 and the processing chamber 201. A flow rate measurement unit 312 and a valve 314a are provided in the first gas pipe, and a fourth gas pipe 310d (described later) is connected to the first gas pipe. A valve 318 may be provided between the tank and the connection point with the fourth gas pipe 310d. The flow rate measurement unit 312 measures the flow rate of the processing gas flowing through the first gas pipe 310a. Specific examples include a mass flow meter, a differential pressure measurement, an IR sensor, and a pressure gauge. Here, differential pressure measurement is a method of measurement based on the pressure difference between two points. When the flow rate measuring unit 312 is configured with a pressure diameter, the flow rate of the raw material gas in the processing gas is calculated based on the difference between the pressure when the gas is supplied through the route of the second gas pipe 310b → tank 313 → first gas pipe 310a and the pressure when the gas is supplied through the route of the second gas pipe 310b → bypass pipe 319 → first gas pipe 310a. When an IR sensor is used, the flow rate of the raw material gas is calculated by irradiating light adjusted to the absorption spectrum specific to the raw material and measuring the amount of light absorbed (reflected).

[0043] (Second Gas Pipe) The second gas pipe 310b is a pipe that supplies a carrier gas serving as a first inert gas to the tank 313. The second gas pipe 310b is connected to the tank 313. The second gas pipe 310b is provided with a first flow rate regulator 315b, a valve 314b, a first heating unit 317a, and a valve 316. The first inert gas is, for example, a rare gas such as Ar gas or N2 gas, and promotes vaporization of the raw material. The amount of vaporization of the raw material can be controlled by adjusting the supply amount of the first inert gas and the temperature of the first inert gas. Here, the first heating unit 317a is, for example, configured with a gas heating mechanism having a heater installed therein. In this disclosure, the first inert gas is also referred to as a heated carrier gas.

[0044] (Third Gas Pipe) The third gas pipe 310c is a pipe that supplies a carrier gas serving as a second inert gas to the tank 313. The third gas pipe 310c is connected to the tank 313. A second flow rate adjuster 315c and a valve 314c are provided in the third gas pipe 310c. The second inert gas is, for example, a rare gas such as Ar gas or N2 gas, and promotes vaporization of the raw material. The second inert gas is used to adjust the temperature and flow rate of the first inert gas. In the present disclosure, the second inert gas is also referred to as an auxiliary gas.

[0045] (4th Gas Pipe) The fourth gas pipe 310d is a pipe that supplies a dilution gas as a third inert gas to the first gas pipe 310a. The fourth gas pipe 310d is connected to the first gas pipe 310a. A third flow rate regulator 315d and a valve 314d are provided in the fourth gas pipe 310d.

[0046] In the present disclosure, the source gas supply system 300 includes at least a first gas pipe 310a, a flow rate measuring unit 312, a tank 313, a second gas pipe 310b, a first heating unit 317a, valves 314a and 314b, and a first flow rate adjusting unit 315b. The source gas supply system 300 may include other components shown in FIG.

[0047] (Bypass pipe) 3 may be provided. The bypass pipe 319 is a gas pipe that directly connects the first gas pipe 310a and the second gas pipe 310b. The bypass pipe 319 is provided with a valve 320. By opening and closing the valves 320, 316, and 318, a gas path from the second gas pipe 310b to the tank 313 to the first gas pipe 310a and a gas path from the second gas pipe 310b to the first gas pipe 310a can be formed.

[0048] [Reaction gas supply system] (reactive gas) The reactive gas of the present disclosure is a reactive gas (reactant) that reacts with the raw material gas. A hydrogen-containing gas (reducing gas) can be used as the reactive gas. Examples of the hydrogen-containing gas that can be used include hydrogen (H2) gas and deuterium gas. A nitrogen-containing gas (nitride gas) can be used as the reactive gas. Examples of the nitrogen-containing gas that can be used include ammonia (NH3) gas and hydrazine (N2H4) gas. An oxygen-containing gas (oxidizing gas) can be used as the reactive gas. Examples of the oxygen-containing gas that can be used include oxygen (O2) gas, ozone (O3) gas, water (H2O), and hydrogen peroxide (H2O2) gas. (5th Gas Pipe) The fifth gas pipe 320 (320a) is provided with a fourth flow rate regulator 325a and a valve 324a, and is connected to the processing chamber 201. (6th Gas Pipe) The sixth gas pipe 320b is a pipe that supplies a dilution gas as a fourth inert gas to the fifth gas pipe 320a. The sixth gas pipe 320b is provided with a fifth flow rate regulator 325b and a valve 324b.

[0049] In the present disclosure, the reactive gas supply system 400 is composed of at least a fifth gas pipe 320a, a fourth flow rate regulator 325a, and a valve 324a. The reactive gas supply system 400 may include other components shown in FIG.

[0050] In the present disclosure, each of the first flow rate adjustment unit 315b, the second flow rate adjustment unit 315c, the third flow rate adjustment unit 315d, the fourth flow rate adjustment unit 325a, and the fifth flow rate adjustment unit 325b is configured by, for example, a mass flow controller (MFC).

[0051] (Control unit) The controller 121, which corresponds to the control unit in the present disclosure, is configured to be able to calculate the flow rate of the source gas in the processing gas flowing through the first gas pipe 310a based on the measurement signal from the flow rate measurement unit 312, the setting value of the first flow rate adjustment unit 315b, the physical property data of the source gas, the physical property data of the inert gas, etc. In addition to these, the controller 121 may also calculate the flow rate of the source gas in the processing gas based on the setting value of the second flow rate adjustment unit 315c and the setting value of the third flow rate adjustment unit 315d.

[0052] (3) Substrate processing process Next, as a substrate processing step, a semiconductor device manufacturing process using the substrate processing apparatus 10 according to this embodiment will be described. Note that, below, an overview of the semiconductor device manufacturing process will be first described, and the part of the semiconductor device manufacturing process relating to the source gas supply method using the source gas supply system 300 will be described separately later in "(4) Source gas supply method."

[0053] As one step in the manufacturing process of a semiconductor device, an example of a step of forming a Mo-containing film containing molybdenum (Mo) to be used as a control gate electrode of 3D NAND on a wafer 200 will be described with reference to Fig. 5. In the following description, the operation of each part constituting the substrate processing apparatus 10 is controlled by a controller 121.

[0054] In this specification, the term "wafer" may mean "the wafer itself" or "a laminate of a wafer and a predetermined layer, film, etc. formed on its surface." In this specification, the term "surface of a wafer" may mean "the surface of the wafer itself" or "the surface of a predetermined layer, film, etc. formed on the wafer." In this specification, the term "substrate" is synonymous with the term "wafer."

[0055] (Wafer loading) 1, when a plurality of wafers 200 are loaded into the boat 217 (wafer charge), the boat 217 supporting the plurality of wafers 200 is lifted by the boat elevator 115, carried into the processing chamber 201 (boat load), and accommodated in the processing vessel. In this state, the seal cap 219 closes the lower end opening of the outer tube 203 via the O-ring 220.

[0056] (pressure and temperature regulation) The processing chamber 201, i.e., the space in which the wafer 200 is present, is evacuated by the vacuum pump 246 to a desired pressure (vacuum level). At this time, the pressure inside the processing chamber 201 is measured by the pressure sensor 245, and the APC valve 243 is feedback-controlled (pressure adjustment) based on this measured pressure information. The vacuum pump 246 is kept in a constantly operating state at least until the processing of the wafer 200 is completed.

[0057] The inside of the processing chamber 201 is heated by the heater 207 to a desired temperature. At this time, the amount of power supplied to the heater 207 is feedback-controlled (temperature adjustment) based on temperature information detected by the temperature sensor 263 so that the inside of the processing chamber 201 has a desired temperature distribution. Hereinafter, the temperature of the heater 207 is set to a temperature such that the temperature of the wafer 200 is in the range of, for example, 300° C. to 600° C. The inside of the processing chamber 201 is heated by the heater 207 continuously at least until the processing of the wafer 200 is completed.

[0058] [Step S10] (metal-containing gas supply)

[0059] The valve 314a is opened to allow an inert gas to flow into the tank 313. The valve 316 is also opened to allow a metal-containing gas, which is a source gas, to flow from the tank 313 into the gas supply pipe 310. The flow rate of the metal-containing gas is adjusted by the flow rate of the first inert gas adjusted by the MFC 315b, and the metal-containing gas is supplied into the processing chamber 201 through the gas supply holes 410a of the nozzle 410 and exhausted through the exhaust pipe 231. At this time, the metal-containing gas is supplied to the wafer 200. At this time, the valve 314d may be opened simultaneously to allow a third inert gas to flow into the gas supply pipe 310d. The third inert gas flowing through the gas supply pipe 310d has its flow rate adjusted by the MFC 315d, and is supplied into the processing chamber 201 together with the metal-containing gas and exhausted through the exhaust pipe 231. At this time, in order to prevent the metal-containing gas from entering the nozzle 420, the valve 324b is opened to allow the inert gas to flow into the gas supply pipes 320b and 320 (320a). The inert gas is supplied into the processing chamber 201 via the gas supply pipe 320 and the nozzle 420, and is exhausted from the exhaust pipe 231. The first inert gas mainly acts as a carrier gas, and the third inert gas mainly acts as a dilution gas that adjusts the concentration of the source gas in the processing gas. Although the first inert gas mainly acts as a carrier gas, it can also adjust the concentration of the source gas in the processing gas. By using both the first inert gas and the third inert gas, the transport of the source gas and the accuracy of concentration adjustment can be improved.

[0060] At this time, the APC valve 243 is adjusted to set the pressure inside the processing chamber 201 to, for example, a pressure within a range of 1 to 3990 Pa, for example, 1000 Pa. The supply flow rate of the inert gas controlled by the MFC 310b is, for example, 0.1 to 1.0 slm, preferably 0.1 to 0.5 slm. The supply flow rate of the inert gas controlled by the MFC 310d is, for example, a flow rate within a range of 0.1 to 20 slm. Note that in this disclosure, the notation of a numerical range such as "1 to 3990 Pa" means that the lower limit and the upper limit are included in the range, so for example, "1 to 3990 Pa" means "1 Pa or more and 3990 Pa or less." The same applies to other numerical ranges.

[0061] At this time, only metal-containing gas and inert gas are flowing into the process chamber 201. Here, a molybdenum (Mo)-containing gas can be used as the metal-containing gas. Examples of Mo-containing gases that can be used include MoCl5 gas, MoO2Cl2 gas, and MoOCl4 gas. By supplying the metal-containing gas, a metal-containing layer is formed on the wafer 200 (the AlO film serving as the surface underlayer). Here, when either MoO2Cl2 gas or MoOCl4 gas is used as the metal-containing gas, the metal-containing layer is a Mo-containing layer. The Mo-containing layer may be a Mo layer containing Cl or O, or an adsorption layer of MoO2Cl2 (MoOCl4), or may contain both. The Mo-containing layer is a film primarily composed of Mo and may contain elements such as Cl, O, and H in addition to Mo.

[0062] Here, the source material in the tank 313 is preheated by the heater 317b to a temperature at which the source material vaporizes. However, for example, in the following cases (A) to (E), the temperature of the source material in the tank 313 changes, and the predetermined flow rate of the source material may not be obtained. (A) When the supply rate of the first inert gas is increased, (B) When the supply rate of the first inert gas is decreased, (C) When the amount of source material in the tank 313 becomes less than the predetermined amount, (D) When the particle size of the source material in the tank 313 becomes smaller, or (E) When the particle size of the source material in the tank 313 becomes larger. When such events occur, the amount of source material vaporized increases or decreases, the flow rate of the source material in the process gas changes, and the concentration of the source material changes, resulting in problems such as different film characteristics formed on the wafers 200 for each wafer 200 or each layer.

[0063] To reduce the occurrence of such problems, for example, the following adjustments are made. [Step S10A (Adjusting the Flow Rate of the First Inert Gas)] The flow rate of the first inert gas is adjusted. By adjusting the flow rate of the first inert gas, the amount of vaporization of the raw material can be adjusted, and the flow rate of the raw material gas can be adjusted. For example, the flow rate of the first inert gas is increased in response to a decrease in the flow rate of the raw material gas in the processing gas. This allows the flow rate of the raw material gas in the processing gas to be increased. Conversely, when the flow rate of the raw material gas increases, the flow rate of the first inert gas is decreased. Note that, by adjusting the flow rate of the first inert gas, fluctuations in the total flow rate of the processing gas can be suppressed, so it is preferable to adjust the flow rate of the third inert gas as a dilution gas. [Step S10B (Adjusting the Temperature of the First Inert Gas)] The temperature of the first inert gas is adjusted. Adjusting the temperature of the first inert gas allows the vaporization rate of the source gas and the flow rate of the source gas to be adjusted. For example, the temperature of the first inert gas is increased in response to a decrease in the flow rate of the source gas in the processing gas. This increases the vaporization rate of the source material and increases the flow rate of the source gas in the processing gas. Conversely, when the flow rate of the source gas increases, the temperature of the first inert gas is decreased. Here, the temperature of the first inert gas is adjusted using at least one of the first heating unit 317a and the second heating unit 317b. The first heating unit 317a is, for example, configured with a heat exchanger, and the second heating unit 317b is configured to heat the tank 313 with a resistance heater. The first heating unit 317a can directly heat the first inert gas, making it easier to adjust the temperature of the first inert gas compared to using the second heating unit 317b. Furthermore, the second heating unit 317b also changes the temperature of the tank 313, which may affect the temperature of the source material. Therefore, it is preferable to maintain the temperature of the second heating unit 317b constant and adjust the temperature of the first heating unit 317a. More preferably, the temperature of the first heating unit 317a is set to a temperature higher than the temperature of the second heating unit 317b. This temperature relationship makes it easier for the first inert gas heated by the first heating unit 317a to affect the temperature of the raw material in the tank 313, even if the temperature drops before it reaches the tank 313.

[0064] Another method for adjusting the temperature of the first inert gas is to supply a second inert gas. The first heating unit 317a is maintained at a predetermined temperature, and the heated first inert gas and the unheated second inert gas are mixed and supplied to the tank 313 to adjust the temperature of the first inert gas. Adjusting the temperature of the first inert gas in this manner shortens the temperature adjustment time. The temperature of the first inert gas can be adjusted by changing the temperature setting of the first heating unit 317a, but there is a time lag between changing the set temperature and the change in the temperature of the first inert gas. However, by supplying an unheated second inert gas to the heated first inert gas in this manner, the temperature of the first inert gas can be adjusted in a short time. The temperature adjustment of the first inert gas using the second inert gas is performed by adjusting the flow rate of the second inert gas or the flow rate ratio of the first inert gas to the second inert gas. For example, the temperature of the inert gas supplied to the tank 313 can be lowered by maintaining the flow rate of the first inert gas constant and increasing the flow rate of the second inert gas. Conversely, by keeping the flow rate of the first inert gas constant and decreasing the flow rate of the second inert gas, the temperature of the inert gas supplied to the tank 313 can be increased. Note that, if it is desired to keep the total amount of inert gas supplied to the tank 313 constant, the flow rate of the second inert gas can be increased while decreasing the flow rate of the first inert gas, or the flow rate of the second inert gas can be decreased while increasing the flow rate of the first inert gas. By keeping the total amount of inert gas supplied to the tank 313 constant, it is possible to suppress changes in the flow rate (concentration) of the source gas in the processing gas supplied to the processing chamber 201.

[0065] [Step S11 (first purge process)] (Residual gas removal) After a predetermined time has elapsed since the start of the supply of the metal-containing gas, e.g., 0.01 to 10 seconds, the valve 318 is closed to stop the supply of the metal-containing gas. That is, the time for supplying the metal-containing gas to the wafer 200 is set to, e.g., 0.01 to 10 seconds. At this time, the APC valve 243 of the exhaust pipe 231 remains open, and the vacuum pump 246 evacuates the processing chamber 201 to remove any unreacted metal-containing gas remaining in the processing chamber 201 or any metal-containing gas remaining after contributing to the formation of the metal-containing layer. That is, the processing chamber 201 is purged. At this time, the valves 314a and 324b remain open, and the supply of the inert gas into the processing chamber 201 is maintained. The inert gas acts as a purge gas, enhancing the effect of removing any unreacted metal-containing gas remaining in the processing chamber 201 or any metal-containing gas remaining after contributing to the formation of the metal-containing layer from the processing chamber 201.

[0066] [Step S12] (reaction gas supply) After removing the residual gas from the processing chamber 201, the valve 324a is opened to allow the reactive gas to flow into the gas supply pipe 320 (320a). The flow rate of the reactive gas is adjusted by the MFC 325a, and the reactive gas is supplied into the processing chamber 201 through the gas supply holes 420a of the nozzle 420 and exhausted through the exhaust pipe 231. At this time, the reactive gas is supplied to the wafer 200. At this time, the valve 324b may be opened at the same time to allow the inert gas to flow into the gas supply pipe 320b. The flow rate of the inert gas flowing through the gas supply pipe 320b is adjusted by the MFC 325b. The inert gas is supplied into the processing chamber 201 together with the reactive gas and exhausted through the exhaust pipe 231. At this time, in order to prevent the reactive gas from entering the nozzle 410, the valves 314a and 314d are opened to allow the inert gas to flow into the gas supply pipe 310a. The inert gas is supplied into the processing chamber 201 through the gas supply pipe 310 and the nozzle 410, and is exhausted from the exhaust pipe 231. Here, the reactive gas is, for example, a reducing gas.

[0067] At this time, the APC valve 243 is adjusted to set the pressure inside the processing chamber 201 within a range of, for example, 1 to 3990 Pa, for example, 2000 Pa. The supply flow rate of the reducing gas controlled by the MFC 325a is set within a range of, for example, 1 to 50 slm, preferably 15 to 30 slm. The supply flow rates of the inert gas controlled by the MFCs 325b and 315d are each set within a range of, for example, 0.1 to 30 slm. The time for which the reducing gas is supplied to the wafer 200 is set within a range of, for example, 0.01 to 120 seconds.

[0068] At this time, the gas flowing into the process chamber 201 may be a reducing gas alone or a reducing gas and an inert gas. Examples of the reducing gas include hydrogen (H) gas, deuterium (D) gas, and gas containing activated hydrogen. When H gas is used as the reducing gas, the H gas undergoes a substitution reaction with at least a portion of the Mo-containing layer formed on the wafer 200 in step S10. That is, O and chlorine (Cl) in the Mo-containing layer react with H and are desorbed from the Mo layer. These are exhausted from the process chamber 201 as reaction by-products such as water vapor (H O), hydrogen chloride (HCl), and chlorine (Cl). As a result, a metal layer (Mo layer) containing Mo but substantially free of Cl and O is formed on the wafer 200.

[0069] [Step S13 (second purge process)] (Residual gas removal) After the metal layer is formed, the valve 324a is closed to stop the supply of the reaction gas.

[0070] Then, by performing a process similar to that of step S11 (first purging process) described above, the reaction gas and reaction by-products remaining in the process chamber 201, which have not reacted or have contributed to the formation of the metal layer, are removed from the process chamber 201. That is, the inside of the process chamber 201 is purged.

[0071] (Performed a specified number of times) By performing the cycle of steps S10 to S13 in order one or more times (a predetermined number of times (n times, where n is an integer of 1 or more)), a metal-containing film of a predetermined thickness (for example, 0.5 to 20.0 nm) is formed on wafer 200. The above cycle is preferably repeated multiple times. Furthermore, each of steps S10 to S13 may be performed at least once or more.

[0072] The above-described step S10A (adjusting the flow rate of the first inert gas) and step S10B (adjusting the temperature of the first inert gas) are performed before the above-described step S10. Alternatively, they may be performed between steps S10 to S13. Steps S10A and S10B may be performed while a predetermined number of processes are performed. By performing these steps during the processing of the wafer 200, the characteristics of each layer of the film formed on the wafer 200 can be made uniform.

[0073] (After purging and atmospheric pressure recovery) An inert gas is supplied into the processing chamber 201 through each of the gas supply pipes 310a and 320a and exhausted through the exhaust pipe 231. The inert gas acts as a purge gas, thereby purging the processing chamber 201 with the inert gas, and gases and reaction by-products remaining in the processing chamber 201 are removed from the processing chamber 201 (after-purge). Thereafter, the atmosphere in the processing chamber 201 is replaced with the inert gas (inert gas replacement), and the pressure in the processing chamber 201 is returned to normal pressure (return to atmospheric pressure).

[0074] (Wafer removal) Thereafter, the seal cap 219 is lowered by the boat elevator 115 to open the lower end of the outer tube 203. Then, the processed wafers 200 supported by the boat 217 are unloaded from the lower end of the outer tube 203 to the outside of the outer tube 203 (boat unloading). Thereafter, the processed wafers 200 are removed from the boat 217 (wafer discharging).

[0075] (4) Raw material gas supply method Next, a source gas supply method performed using the source gas supply system 300 according to this embodiment will be specifically described with reference to Fig. 3. The source gas supply method is performed during a step of supplying a metal-containing gas as a source gas into the processing chamber 201, which is a reaction chamber.

[0076] First, a first raw material gas is generated by vaporizing the raw material in the tank 313. Next, a first inert gas is supplied to the tank 313 to promote the vaporization of the raw material. That is, a second raw material gas is generated by mixing the first raw material gas and the first inert gas. Then, the second raw material gas is caused to flow downstream of the tank 313.

[0077] Next, a third inert gas is supplied to the gas supply pipe 310d to dilute the second source gas. In this embodiment, the same type of gas, such as Ar gas or N2 gas, is used as the first and third inert gases. That is, a third source gas is generated by mixing the second source gas and the third inert gas. The generated third source gas flows to the flow rate measuring unit 312. Here, the third inert gas does not necessarily have to be used.

[0078] Next, the flow rate is measured by the flow rate measuring unit 312. The measured flow rate value (flow rate data) is input to the controller 121. The controller 121 calculates data on the source gas from the measured flow rate value, at least the set flow rate of the first flow rate adjusting unit 315b, the physical property values ​​of the source gas, the physical property values ​​of the first inert gas, etc. Here, the source gas data refers to, for example, at least one of the flow rate of the source gas among the third source gases flowing through the first gas pipe 310a, the concentration of the source gas, etc.

[0079] Next, based on the calculated raw material gas data, at least one of the following feedback controls (A) to (E) is performed so that the raw material gas flow rate data becomes a predetermined value (target value). Note that the raw material gas flow rate data may be controlled to fall within a predetermined range, rather than a predetermined value. Also, a combination of two or more of (A) to (E) may be performed.

[0080] (A) Flow rate adjustment of the first inert gas The flow rate of the first inert gas is adjusted by the first flow rate adjuster 315b. The flow rate of the first inert gas is adjusted by adjusting the flow rate setting value of the first flow rate adjuster 315b. For example, by increasing the flow rate of the first inert gas, the amount of vaporization of the raw material in the tank 313 can be increased. By increasing the vaporization amount, the flow rate of the raw material can be increased. Conversely, by decreasing the flow rate of the first inert gas, the amount of vaporization of the raw material in the tank 313 can be decreased. By decreasing the vaporization amount, the flow rate of the raw material can be decreased.

[0081] (B) Temperature adjustment of the first inert gas The temperature of the first inert gas is adjusted by the first heating unit 317a. By increasing the temperature of the first heating unit 317a, the temperature of the first inert gas is increased. By increasing the temperature of the first inert gas, the temperature of the raw material in the tank 313 can be increased. As a result, the amount of raw material vaporized can be increased. Furthermore, by decreasing the temperature of the first inert gas, the temperature of the first inert gas is lowered. By decreasing the temperature of the first inert gas, the amount of raw material vaporized in the tank 313 can be reduced. Because the first inert gas directly contacts the raw material in the tank 313, the amount of raw material vaporized can be adjusted in a relatively short time by adjusting the temperature of the first inert gas.

[0082] (C) Temperature control of tank 313 (raw material) The second heating unit 317b adjusts the temperature of the tank 313 (raw material). By increasing the temperature of the second heating unit 317b, the temperature of the raw material in the tank 313 can be increased. As a result, the evaporation of the raw material can be promoted. Conversely, by decreasing the temperature of the second heating unit 317b, the temperature of the raw material in the tank 313 can be decreased, and the amount of evaporated raw material can be reduced. Note that, because the heat of the second heating unit 317b is transferred to the raw material via the tank 313, it takes a relatively long time for the amount of evaporated raw material to change after the temperature of the second heating unit 317b is changed. For this reason, it is preferable to adjust the temperature of the tank 313 while wafers 200 are not being processed.

[0083] (D) Flow rate adjustment of the second inert gas The flow rate of the second inert gas is adjusted by the second flow rate adjuster 315c. The flow rate of the second inert gas is adjusted by adjusting the setting value of the second flow rate adjuster 315c. By supplying the second inert gas, the temperature of the inert gas supplied to the tank 313 can be adjusted. In particular, the temperature of the inert gas supplied to the tank 313 is adjusted by supplying a heated first inert gas and an unheated second inert gas to the tank 313. The temperature of the inert gas supplied to the tank 313 can be adjusted by adjusting the temperature of the first inert gas, the flow rate of the first inert gas, and the flow rate of the second inert gas. The temperature of the first inert gas can be adjusted by the first heating unit 317a, but the temperature of the first heating unit 317a may not be changed instantaneously. For example, if the temperature of the first inert gas rises too much due to an increase in the temperature of the first heating unit 317a, it may be necessary to instantly lower the temperature. In this case, even if the temperature setting of the first heating unit 317a is lowered, it takes time for the temperature to decrease. In such a case, by supplying the second inert gas, the first inert gas, whose temperature has increased, is mixed with the second inert gas at room temperature, for example. This makes it possible to adjust the temperature of the inert gas supplied to the tank 313.

[0084] (E) Flow rate adjustment of the third inert gas Due to the above (A) to (D), the ratio of the flow rate of the source gas to the flow rate of the inert gas flowing through the first gas pipe 310a (source gas concentration) may deviate from the range used for processing the wafer 200. Here, by adjusting the flow rate of the third inert gas, the source gas flow rate (source gas concentration) used for processing the wafer 200 can be adjusted. For example, when the flow rate of the first inert gas is increased, the concentration of the source gas may decrease. In this case, by decreasing the flow rate of the third inert gas, the concentration of the source gas can be adjusted to fall within the predetermined range.

[0085] (5) Other embodiments Although the embodiments of the present disclosure have been specifically described above, the present disclosure is not limited to the above-described embodiments and can be modified in various ways without departing from the spirit and scope of the present disclosure.

[0086] For example, although the above embodiment has been described using a Mo-containing gas as an example, the present disclosure is not limited to this example and may be a gas containing at least one of the above-mentioned elements such as Al, Mo, W, Hf, and Zr.

[0087] Furthermore, in the above embodiment, the case where H2 gas is used as the reducing gas has been described as an example, but the present disclosure is not limited to this.

[0088] In the above embodiment, an example of film formation using a substrate processing apparatus that is a batch-type vertical apparatus that processes multiple substrates at a time has been described, but the present disclosure is not limited to this. The present disclosure can also be suitably applied to film formation using a single-wafer substrate processing apparatus that processes one or several substrates at a time. In addition, in the above aspect, an example of film formation using a substrate processing apparatus having a hot-wall type processing furnace has been described, but the present disclosure is not limited to the above aspect and can also be suitably applied to film formation using a substrate processing apparatus having a cold-wall type processing furnace.

[0089] When using these substrate processing apparatuses, each process can be performed using the same processing procedures and conditions as in the above-described embodiments and modifications, and the same effects as in the above-described embodiments and modifications can be obtained.

[0090] The above-described embodiments and modifications may be used in combination as appropriate. The processing procedures and processing conditions in such a case may be the same as those of the above-described embodiments and modifications, for example. [Explanation of symbols]

[0091] 10. Substrate processing equipment 12 Gas supply system 313 Tank 121 Controller (control unit) 200 wafers (substrates) 201 Processing chamber (reaction chamber) 310 First Gas Pipe

Claims

1. a processing vessel for accommodating a substrate; a first gas pipe for supplying a processing gas to the processing vessel; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be capable of controlling the first flow rate adjusting unit and the first heating unit to perform a process of supplying a process gas, in which at least one of a flow rate of the first inert gas and a temperature of the first inert gas is adjusted based on flow rate data of the process gas measured by the flow rate measuring unit so that the flow rate of the process gas becomes a predetermined flow rate, to the substrate in the process vessel; The control unit When the flow rate of the raw material in the processing gas is higher than a target value, The substrate processing apparatus is configured to be able to control a flow rate setting value of the second flow rate adjusting unit so as to increase the flow rate of the second inert gas.

2. The control unit When the flow rate of the raw material in the processing gas is lower than a target value, The substrate processing apparatus according to claim 1 , wherein the first heating unit is controllable so as to increase the temperature of the first inert gas.

3. A processing vessel that accommodates a substrate; a first gas pipe for supplying a processing gas to the processing vessel; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be capable of controlling the first flow rate adjusting unit and the first heating unit to perform a process of supplying a process gas, in which at least one of a flow rate of the first inert gas and a temperature of the first inert gas is adjusted based on flow rate data of the process gas measured by the flow rate measuring unit so that the flow rate of the process gas becomes a predetermined flow rate, to the substrate in the process vessel; The control unit When the flow rate of the raw material in the processing gas is lower than a target value, a first flow rate adjusting unit that adjusts a flow rate of the first inert gas and a second flow rate adjusting unit that adjusts a flow rate of the second inert gas;

4. A processing vessel for accommodating a substrate; a first gas pipe for supplying a processing gas to the processing vessel; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be capable of controlling the first flow rate adjusting unit and the first heating unit to perform a process of supplying a process gas, in which at least one of a flow rate of the first inert gas and a temperature of the first inert gas is adjusted based on flow rate data of the process gas measured by the flow rate measuring unit so that the flow rate of the process gas becomes a predetermined flow rate, to the substrate in the process vessel; The control unit When the flow rate of the raw material in the processing gas is lower than a target value, A substrate processing apparatus configured to be capable of controlling the first heating unit to increase the temperature of the first inert gas in the tank and controlling the second flow rate adjustment unit to reduce the flow rate of the second inert gas.

5. The control unit When the flow rate of the raw material in the processing gas is higher than a target value, The substrate processing apparatus according to claim 1 , wherein the first flow rate adjusting unit is capable of controlling the flow rate of the first inert gas supplied to the tank to be reduced.

6. The control unit When the flow rate of the raw material in the processing gas is higher than a target value, The substrate processing apparatus according to claim 1 , wherein the first heating unit is controllable so as to lower the temperature of the inert gas in the tank.

7. The control unit 2. The substrate processing apparatus according to claim 1, wherein the temperature of the first heating unit can be adjusted while the substrate is being processed in the processing chamber.

8. A processing vessel for accommodating a substrate; a first gas pipe for supplying a processing gas to the processing vessel; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be capable of controlling the first flow rate adjusting unit and the first heating unit to perform a process of supplying a process gas, in which at least one of a flow rate of the first inert gas and a temperature of the first inert gas is adjusted based on flow rate data of the process gas measured by the flow rate measuring unit so that the flow rate of the process gas becomes a predetermined flow rate, to the substrate in the process vessel; The control unit A substrate processing apparatus configured to be able to control the second flow rate adjustment unit to adjust the temperature of the inert gas in the tank by the flow rate of the second inert gas without changing the temperature setting of the first heating unit while the substrate is being processed in the processing container.

9. a second heating unit that heats the tank; The substrate processing apparatus according to claim 1 , wherein the control unit is configured to be able to set the temperature of the first heating unit to a temperature higher than the temperature of the second heating unit.

10. The control unit The substrate processing apparatus according to claim 9 , wherein the temperature of the second heating unit can be adjusted while the substrate is not being processed in the processing vessel.

11. The control unit The substrate processing apparatus according to claim 9 , wherein the temperature of the first heating section can be controlled in accordance with the temperature of the second heating section.

12. a first gas pipe for supplying a processing gas to a processing chamber for processing a substrate; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be able to control the first flow rate adjusting unit and the first heating unit based on flow rate data of the processing gas measured by the flow rate measuring unit so that the flow rate of the processing gas becomes a predetermined flow rate; and The control unit When the flow rate of the raw material in the processing gas is higher than a target value, A gas supply system configured to be able to control a flow rate setting value of the second flow rate adjusting unit so as to increase the flow rate of the second inert gas.

13. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel through a first gas pipe; and increasing the flow rate of the second inert gas supplied to the tank through a third gas pipe when the flow rate of the source material in the processing gas is higher than a target value.

14. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel through a first gas pipe; and increasing the flow rate of the second inert gas supplied to the tank from a third gas pipe when the flow rate of the raw material in the processing gas is higher than a target value.

15. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; a step of supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit, measuring a flow rate of the process gas, and generating flow rate data; a step of adjusting at least one of the flow rate and the temperature of the first inert gas based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, and supplying the processing gas to the substrate in the processing vessel through a first gas pipe; and a procedure for increasing the flow rate of the second inert gas supplied to the tank from a third gas pipe when the flow rate of the raw material in the processing gas is higher than a target value.

16. A first gas pipe for supplying a processing gas to a processing vessel for processing a substrate; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be able to control the first flow rate adjusting unit and the first heating unit based on flow rate data of the processing gas measured by the flow rate measuring unit so that the flow rate of the processing gas becomes a predetermined flow rate; and The control unit When the flow rate of the raw material in the processing gas is lower than a target value, A gas supply system configured to be able to control the first flow rate adjustment unit and the second flow rate adjustment unit so as to increase both the flow rate of the first inert gas and the flow rate of the second inert gas.

17. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel via a first gas pipe; and increasing both the flow rate of the first inert gas and the flow rate of the second inert gas supplied from a third gas pipe to the tank when the flow rate of the raw material in the processing gas is lower than a target value.

18. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel via a first gas pipe; and when the flow rate of the raw material in the processing gas is lower than a target value, increasing both the flow rate of the first inert gas and the flow rate of the second inert gas supplied to the tank from a third gas pipe.

19. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; a step of supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit, measuring a flow rate of the process gas, and generating flow rate data; a step of adjusting at least one of the flow rate and the temperature of the first inert gas based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, and supplying the processing gas to the substrate in the processing vessel through a first gas pipe; and a procedure for increasing both the flow rate of the first inert gas and the flow rate of the second inert gas supplied to the tank from a third gas pipe when the flow rate of the raw material in the processing gas is lower than a target value.

20. A first gas pipe for supplying a processing gas to a processing chamber for processing a substrate; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be able to control the first flow rate adjusting unit and the first heating unit based on flow rate data of the processing gas measured by the flow rate measuring unit so that the flow rate of the processing gas becomes a predetermined flow rate; and The control unit When the flow rate of the raw material in the processing gas is lower than a target value, A gas supply system configured to be able to control the first heating unit to increase the temperature of the first inert gas in the tank and to control the second flow rate adjustment unit to reduce the flow rate of the second inert gas.

21. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel through a first gas pipe; and when the flow rate of the raw material in the processing gas is lower than a target value, adjusting the temperature of the first inert gas in the tank so as to increase the temperature of the first inert gas, and reducing the flow rate of the second inert gas supplied to the tank from a third gas pipe.

22. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel through a first gas pipe; and when the flow rate of the raw material in the processing gas is lower than a target value, adjusting the temperature of the first inert gas in the tank so as to increase the temperature of the first inert gas, and reducing the flow rate of the second inert gas supplied to the tank from a third gas pipe.

23. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; a step of supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit, measuring a flow rate of the process gas, and generating flow rate data; a step of adjusting at least one of the flow rate and the temperature of the first inert gas based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, and supplying the processing gas to the substrate in the processing vessel through a first gas pipe; and a procedure for adjusting the temperature of the first inert gas in the tank so as to increase the temperature of the first inert gas when the flow rate of the raw material in the processing gas is lower than a target value, and for reducing the flow rate of the second inert gas supplied to the tank from a third gas pipe.

24. A first gas pipe for supplying a processing gas to a processing vessel for processing a substrate; a flow rate measuring unit provided in the first gas pipe and configured to measure a flow rate of the processing gas flowing through the first gas pipe; a second gas pipe connected to the first gas pipe and supplying a first inert gas to a tank storing a raw material of the processing gas; a first flow rate adjusting unit provided in the second gas pipe and configured to adjust a flow rate of the first inert gas; a first heating unit that adjusts the temperature of the first inert gas; a third gas pipe for supplying a second inert gas to the tank; a second flow rate adjusting unit provided in the third gas pipe and configured to adjust the flow rate of the second inert gas; a control unit configured to be able to control the first flow rate adjusting unit and the first heating unit based on flow rate data of the processing gas measured by the flow rate measuring unit so that the flow rate of the processing gas becomes a predetermined flow rate; and The control unit A gas supply system configured to be able to control the second flow rate adjustment unit to adjust the temperature of the inert gas in the tank by the flow rate of the second inert gas without changing the temperature setting of the first heating unit while the substrate is being processed in the processing vessel.

25. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel through a first gas pipe; and adjusting the temperature of the inert gas in the tank by the flow rate of a second inert gas supplied to the tank from a third gas pipe without changing the temperature setting of the first heating unit while the substrate is being processed in the processing vessel.

26. A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit to measure the flow rate of the process gas and generate flow rate data; supplying the processing gas, in which at least one of the flow rate and the temperature of the first inert gas is adjusted based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, to the substrate in the processing vessel through a first gas pipe; and adjusting the temperature of the inert gas in the tank by adjusting the flow rate of the second inert gas supplied to the tank from a third gas pipe while the substrate is being processed in the processing vessel, without changing the temperature setting of the first heating unit.

27. ​​A step of supplying a first inert gas from a second gas pipe having a first heating section to a tank storing a raw material to vaporize the raw material; a step of supplying a process gas containing the vaporized raw material from the tank to a flow rate measuring unit, measuring a flow rate of the process gas, and generating flow rate data; a step of adjusting at least one of the flow rate and the temperature of the first inert gas based on the flow rate data so that the flow rate of the processing gas becomes a predetermined flow rate, and supplying the processing gas to the substrate in the processing vessel through a first gas pipe; and a procedure for adjusting the temperature of the inert gas in the tank by the flow rate of the second inert gas supplied to the tank from a third gas pipe without changing the temperature setting of the first heating unit while the substrate is being processed in the processing vessel.

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