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

Abstract

A technology is provided capable of suppressing the deterioration of either or both of the uniformity of film characteristics within a substrate plane and the uniformity of film characteristics between planes due to a shortage of supply of raw gas. The technology comprises: (a) a process of closing a first valve of a first gas pipe and supplying raw gas from the upstream side of the first gas pipe to store the raw gas within the first gas pipe; and (b) a process of opening the first valve of the first gas pipe and supplying a first inert gas from the upstream side of the first gas pipe to supply the raw gas and the first inert gas from the first gas pipe to a substrate.

Description

Technology Field

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

[0002] As a process of manufacturing a semiconductor device, a process of forming a metal film on a substrate may be performed (e.g., see Patent Document 1). Prior art literature

[0003] Patent Document 1: Japanese Patent Publication No. 2021-120472 The problem to be solved

[0004] Due to a shortage of source gas supply, there are cases where either or both of the uniformity of film characteristics within the substrate plane and between substrates (inter-plane) deteriorate.

[0005] The present disclosure provides a technology capable of suppressing the deterioration of either or both of the uniformity of film characteristics within a substrate plane and the uniformity of film characteristics between planes due to a shortage of source gas supply. means of solving the problem

[0006] According to one embodiment of the present disclosure, a technology is provided comprising: (a) a process of closing a first valve of a first gas pipe and supplying a raw gas from an upstream side of the first gas pipe to store the raw gas in the first gas pipe; and (b) a process of opening the first valve of the first gas pipe and supplying a first inert gas from an upstream side of the first gas pipe to supply the raw gas and the first inert gas from the first gas pipe to a substrate. Effects of the invention

[0007] According to the present disclosure, it is possible to suppress the deterioration of either or both of the uniformity of film characteristics within a substrate plane and the uniformity of film characteristics between planes due to a shortage of source gas supply. Brief explanation of the drawing

[0008] FIG. 1 is a longitudinal cross-sectional view illustrating a schematic of a longitudinal processing path of a substrate processing device in one form. FIG. 2 is a schematic configuration diagram of a controller of a substrate processing device in one form, and is a diagram illustrating the control system of the controller as a block diagram. Figure 3 (A) is a diagram illustrating the flow of exhausting raw material gas out of the processing room. Figure 3 (B) is a diagram illustrating the case where raw gas is stored in a gas supply pipe. Figure 3 (C) is a diagram illustrating the flow of supplying raw gas to the processing room. Specific details for implementing the invention

[0009] Hereinafter, one embodiment of the present disclosure will be described with reference mainly to FIGS. 1 to 3. Furthermore, all drawings used in the following description are schematic, and the dimensional relationships of each element and the ratios of each element shown in the drawings do not necessarily correspond to reality. Also, the dimensional relationships of each element and the ratios of each element do not necessarily correspond to one another among multiple drawings.

[0010] (1) Configuration of the substrate processing device

[0011] As illustrated in FIG. 1, the processing furnace (202) includes a heater (207) as a heating system (temperature control unit). The heater (207) is cylindrical in shape. The heater (207) also functions as an activation mechanism (excitation unit) that activates [excites] the gas with heat.

[0012] A reaction tube (203) is installed inside the heater (207) in a concentric shape with respect to the heater (207). The reaction tube (203) is made of a heat-resistant material, such as quartz or silicon carbide, and is formed in a cylindrical shape with the top closed and the bottom open. A manifold (209) [hereinafter referred to as MF (209)] is installed below the reaction tube (203) in a concentric shape with respect to the reaction tube (203). The MF (209) is made of a metal material, such as stainless steel, and is formed in a cylindrical shape with the top and bottom open. The top part of the MF (209) is connected to the bottom part of the reaction tube (203) and is configured to support the reaction tube (203). An O-ring (220a) serving as a sealing member is installed between the MF (209) and the reaction tube (203). The reaction tube (203) is installed vertically, similar to the heater (207). The processing vessel (reaction vessel) is primarily composed of the reaction tube (203) and the MF (209). A processing chamber (201) is formed in the hollow portion of the processing vessel. The processing chamber (201) is configured to accommodate a wafer (200) as a substrate.

[0013] Nozzles (249a, 249b) are installed in the processing chamber (201) to penetrate the side wall of the MF (209). Gas supply pipes (232a) and (232b) serving as first gas pipes are respectively connected to the nozzles (249a, 249b).

[0014] In the gas supply pipe (232a), a vaporizer (300) that vaporizes gas in order from the upstream side, a valve (302a) as a fourth valve that is an opening / closing valve, a valve (302b) as a third valve, a valve (302c) as a second valve, and a valve (243a) as a first valve are installed. A gas supply pipe (232e) that supplies inert gas is connected upstream of the valve (243a) of the gas supply pipe (232a) and between the valve (302a) and the valve (302b) of the gas supply pipe (232a). A gas supply pipe (232c) that supplies inert gas is connected downstream of the valve (243a) of the gas supply pipe (232a). In the gas supply pipes (232c, 232e), a mass flow controller (MFC) (241c, 241e), which is a flow controller (flow control unit), and a valve (243c, 243e) are respectively installed in order from the upstream side. An exhaust pipe (232f) is connected as a third gas pipe that exhausts gas within the gas supply pipe (232a) between the valve (243a) and the valve (302c), which is upstream of the valve (243a) of the gas supply pipe (232a). A valve (302d) is installed in the exhaust pipe (232f). The exhaust pipe (232f) is connected to the upstream side of the APC valve (244) of the exhaust pipe (231) described later.

[0015] In the gas supply pipe (232b), an MFC (241b) and a valve (243b) are installed in order from the upstream side. A gas supply pipe (232d) for supplying inert gas is connected downstream of the valve (243b) of the gas supply pipe (232b). In the gas supply pipe (232d), an MFC (241d) and a valve (243d) are installed in order from the upstream side.

[0016] Nozzles (249a, 249b) are each installed in the space between the inner wall of the reaction tube (203) and the wafer (200), rising upward along the inner wall of the reaction tube (203) from the bottom to the top, toward the loading direction of the wafer (200). Gas supply holes (250a, 250b) for supplying gas are each installed on the sides of the nozzles (249a, 249b). The gas supply holes (250a, 250b) are each opened toward the center of the reaction tube (203) and configured to enable the supply of gas toward the wafer (200). Multiple gas supply holes (250a, 250b) are installed extending from the bottom to the top of the reaction tube (203).

[0017] From the gas supply pipe (232a), raw gas is supplied into the processing chamber (201) via a vaporizer (300), valves (302a to 302c, 243a), and nozzle (249a). Also, from the gas supply pipe (232a), raw gas is not supplied into the processing chamber (201) via a vaporizer (300), valves (302a to 302c), exhaust pipe (232f), and valve (302d), but is exhausted to the exhaust pipe (231). Additionally, raw gas is stored in the gas supply pipe (232a) by switching the valves (302a to 302d, 243a, 243e).

[0018] From the gas supply pipe (232b), a reaction gas that reacts with the raw material gas is supplied into the processing chamber (201) via the MFC (241b), valve (243b), and nozzle (249b).

[0019] Inert gas is supplied into the processing chamber (201) from the gas supply pipes (232c, 232d) via the MFC (241c, 241d), valve (243c, 243d), gas supply pipe (232a) and gas supply pipe (232b), nozzle (249a) and nozzle (249b), respectively. In addition, inert gas is supplied into the processing chamber (201) from the gas supply pipe (232e) via the MFC (241e), valve (243e), gas supply pipe (232a), and nozzle (249a).

[0020] The raw gas supply system is mainly configured by a gas supply pipe (232a) and valves (302a to 302c, 243a). A vaporizer (300) may be included in the raw gas supply system. The raw gas exhaust system is mainly configured by an exhaust pipe (232f) and valves (302d). The raw gas exhaust system may be included in the raw gas supply system. The reaction gas supply system is mainly configured by a gas supply pipe (232b), an MFC (241b), and valves (243b). The raw gas supply system and the reaction gas supply system may be collectively referred to as the gas supply system. Additionally, the inert gas supply system is mainly configured by gas supply pipes (232c to 232e), an MFC (241c to 241e), and valves (243c to 243e). In addition, the inert gas supplied from the gas supply pipe (232e), MFC (241e), and valve (243e) may be referred to as the first inert gas. In this case, the gas supply pipe (232e), MFC (241e), and valve (243e) may be referred to as the first inert gas supply system (also called the first inert gas supply section). In addition, the inert gas supplied from the gas supply pipe (232c), MFC (241c), and valve (243c) may be referred to as the second inert gas. In this case, the gas supply pipe (232c), MFC (241c), and valve (243c) may be referred to as the second inert gas supply system (also called the second inert gas supply section). The inert gas supply system may be included in the gas supply system.

[0021] Any one or all of the aforementioned supply systems may be configured as a gas supply system (248) in which valves (243a to 243e, 302a to 302d) or MFCs (241a to 241e) are integrated. The gas supply system (248) is connected to each of the gas supply pipes (232a to 232e) and is configured so that the operation of supplying various gases into the gas supply pipes (232a to 232e), that is, the opening and closing operation of the valves (243a to 243e, 302a to 302d) or the flow rate adjustment operation by the MFCs (241a to 241e) is controlled by a controller (121) to be described later. The gas supply system (248) is configured as an integrated or divided unit, and can be detached from the gas supply pipes (232a to 232e), etc., on an integrated unit basis, and configured so that maintenance, exchange, expansion, etc. of the gas supply system (248) can be performed on an integrated unit basis.

[0022] An exhaust pipe (231) for exhausting the atmosphere inside the processing room (201) is installed in the reaction pipe (203). A vacuum pump (246) [hereinafter referred to as the pump (246)] as an exhaust device is connected to the exhaust pipe (231) via a pressure sensor (245) as a pressure detector (pressure detection unit) for detecting the pressure inside the processing room (201) and an APC (Auto Pressure Controller) valve (244) as a pressure regulator (pressure adjustment unit). The APC valve (244) is configured to perform vacuum exhaust and vacuum exhaust stoppage inside the processing room (201) by opening and closing the valve while the pump (246) is in operation, and to adjust the pressure inside the processing room (201) by adjusting the opening degree of the valve based on pressure information detected by the pressure sensor (245) while the pump (246) is in operation. The exhaust system is mainly composed of an exhaust pipe (231), an APC valve (244), and a pressure sensor (245). A pump (246) may also be included in the exhaust system.

[0023] A seal cap (219) [hereinafter referred to as the cap (219)] is installed below the MF (209) as a furnace mouth cover capable of hermetically sealing the lower opening of the MF (209). An O-ring (220b) is installed on the upper surface of the cap (219) as a sealing member that contacts the lower end of the MF (209). A rotation mechanism (267) for rotating the boat (217), which will be described later, is installed below the cap (219). The rotation axis (255) of the rotation mechanism (267) passes through the cap (219) and is connected to the boat (217). The rotation mechanism (267) is configured to rotate the wafer (200) by rotating the boat (217). The cap (219) is configured to be raised vertically by a boat elevator (115) [hereinafter referred to as the elevator (115)] which is a lifting mechanism installed outside the reaction tube (203). The elevator (115) is configured to enable the boat (217) to be brought into and taken out of the processing room (201) by raising the cap (219). The elevator (115) is configured as a conveying device (conveying mechanism) that conveys the boat (217), i.e., the wafer (200), into and out of the processing room (201).

[0024] The boat (217) serving as a substrate support is configured to support multiple wafers (200), for example, 25 to 200 wafers, in a horizontal position and aligned vertically with each other, in a multi-stage arrangement, that is, arranged at intervals. The boat (217) is made of a heat-resistant material, for example, quartz or SiC. At the bottom of the boat (217), an insulating plate (218), made of a heat-resistant material, for example, quartz or SiC, is supported in a multi-stage manner. Furthermore, the notation of a numerical range such as "25 to 200 wafers" in this specification implies that the lower and upper limits are included within that range. Therefore, for example, "25 to 200 wafers" means "25 wafers or more and 200 wafers or less." The same applies to other numerical ranges.

[0025] A temperature sensor (263) serving as a temperature detector is installed inside the reaction tube (203). By adjusting the energization state to the heater (207) based on the temperature information detected by the temperature sensor (263), the temperature inside the processing room (201) becomes a desired temperature distribution.

[0026] As illustrated in FIG. 2, the controller (121), which is a control unit (control means), is configured as a computer equipped with a CPU (Central Processing Unit) (121a), RAM (Random Access Memory) (121b), a memory device (121c), and an I / O port (121d). The RAM (121b), the memory device (121c), and the I / O port (121d) are configured to exchange data with the CPU (121a) via an internal bus (121e). An input / output device (122), configured such as a touch panel, is connected to the controller (121). Additionally, the substrate processing unit (100) may be configured to have one control unit or may be configured to have multiple control units. That is, control for performing the processing sequence described later may be performed using one control unit or may be performed using multiple control units. In addition, a plurality of control units may be configured as a control system connected to one another via a wired or wireless communication network, or the control for performing the processing sequence described below may be performed by the entire control system. In this specification, the term "control unit" may be used in cases including a plurality of control units in addition to a single control unit, or in cases including a control system configured by a plurality of control units. Furthermore, a control unit may be a physical controller, or it may exist in the controller's memory as a software program.

[0027] The memory device (121c) is composed of, for example, flash memory, HDD (Hard Disk Drive), etc. Within the memory device (121c), a control program that controls the operation of the substrate processing device (100), and a process recipe containing the sequence or conditions of the substrate processing described later are stored so as to be readable. The process recipe is a combination of each sequence in the substrate processing described later to be executed by the controller (121) to obtain a predetermined result, and functions as a program. Hereinafter, the process recipe and the control program are collectively referred to simply as a program. Also, the process recipe is referred to simply as a recipe. In this specification, when the term "program" is used, it may include only the recipe, only the control program, or both. The RAM (121b) is configured as a memory area (work area) where programs or data read by the CPU (121a) are temporarily stored.

[0028] The I / O port (121d) is connected to the aforementioned MFC (241a to 241e), valves (243a to 243e, 302a to 302d), pressure sensor (245), APC valve (244), pump (246), heater (207), temperature sensor (263), rotating mechanism (267), elevator (115), etc.

[0029] The CPU (121a) is configured to read and execute a control program from a memory device (121c), and also to read a recipe from the memory device (121c) in accordance with the input of an operation command from an input / output device (122). The CPU (121a) is configured to control the flow rate adjustment operation of various gases by the MFC (241a to 241e), the opening and closing operation of the valve (243a to 243e, 302a to 302d), the opening and closing operation of the APC valve (244), the pressure adjustment operation by the APC valve (244) based on the pressure sensor (245), the starting and stopping of the pump (246), the temperature adjustment operation of the heater (207) based on the temperature sensor (263), the rotation and rotation speed adjustment operation of the boat (217) by the rotating mechanism (267), and the lifting operation of the boat (217) by the elevator (115), etc., in accordance with the contents of the read recipe.

[0030] The controller (121) can be configured by installing the aforementioned program stored in an external storage device [e.g., a magnetic disk such as a hard disk, an optical disk such as a CD, a semiconductor memory such as a USB memory] (123) into a computer. The storage device (121c) or the external storage device (123) is configured as a computer-readable recording medium that records the program. Hereinafter, these are collectively referred to simply as recording media. In this specification, the term "recording medium" may be used to include only the storage device (121c), only the external storage device (123), or both. Additionally, the provision of the program to the computer may be performed using communication means such as the internet or a dedicated line, without using the external storage device (123).

[0031] (2) Substrate processing process

[0032] An example of a processing sequence for forming a predetermined film on a wafer (200) as a step of substrate processing in a manufacturing process of a semiconductor device using the aforementioned substrate processing device (100) will be described. In the following description, the operation of each part constituting the substrate processing device (100) is controlled by a controller (121).

[0033] The term “wafer” as used in this specification may refer to the wafer itself or to a laminate of the wafer and a predetermined layer or film formed on its surface. The term “surface of the wafer” as used in this specification may refer to the surface of the wafer itself or to the surface of a predetermined layer formed on the wafer. When the phrase “form a predetermined layer on the wafer” is used in this specification, it may mean directly forming a predetermined layer on the surface of the wafer itself or forming a predetermined layer on a layer formed on the wafer. When the term “substrate” is used in this specification, it has the same meaning as when the term “wafer” is used.

[0034] (Wafer import)

[0035] When multiple wafers (200) are loaded into the boat (217), as shown in FIG. 1, the boat (217) supporting the multiple wafers (200) is lifted by the elevator (115) and brought into the processing room (201) and received into the processing container. In this state, the cap (219) closes the lower opening of the MF (209) through the O-ring (220b).

[0036] (Pressure adjustment and temperature adjustment)

[0037] The space within the processing room (201), i.e., the space where the wafer (200) exists, is vacuum-exhausted by a pump (246) so that the desired pressure (vacuum level) is achieved. At this time, the pressure within the processing room (201) is measured by a pressure sensor (245), and based on this measured pressure information, the APC valve (244) is feedback-controlled (pressure adjustment). The pump (246) is kept in a constantly operating state for at least until the processing of the wafer (200) is completed. Additionally, the processing room (201) is heated by a heater (207) so that the temperature within it is desired. At this time, the amount of current supplied to the heater (207) is feedback-controlled (temperature adjustment) based on temperature information detected by a temperature sensor (263) so that the temperature distribution within the processing room (201) is desired. Heating within the processing room (201) by the heater (207) is continuously performed for at least until the processing of the wafer (200) is completed.

[0038] The raw gas used here is a gas with a vapor pressure of, for example, 100 Torr or less, and is a gas that has a lower vapor pressure than other gases supplied to the wafer (200) and cannot be supplied to the MFC. When a gas with a low vapor pressure of 100 Torr or less is used as the raw gas, the amount of raw gas supplied from the upper part of the nozzle (249a) is reduced compared to the lower part of the nozzle (249a) in the processing chamber (201), and the uniformity of film characteristics between the surfaces of the wafer (200) may deteriorate. Also, because the gas is supplied from the side of the wafer (200), the amount of raw gas supplied from the center side of the wafer (200) is reduced compared to the side side of the wafer (200), and the uniformity of film characteristics within the surface of the wafer (200) may deteriorate. Additionally, when a gas with a low vapor pressure of 100 Torr or less is used as the raw gas, the raw gas may not be supplied to the wafer (200) and may flow back out of the processing chamber (201). In the present disclosure, a raw gas with a low vapor pressure of, for example, 100 Torr or less is supplied by the raw gas supply process described below. Here, film characteristics refer to, for example, the film thickness, electrical characteristics, composition, etc. of a film formed on a wafer (200).

[0039] [Raw Gas Supply Process, Step (S1)]

[0040] In this process, the cycle of performing the next steps A through D in order is performed a predetermined number of times (m times, where m is an integer of 1 or 2 or more).

[0041] [Step A]

[0042] In this step, the atmosphere inside the gas supply pipe (232a) is exhausted from the exhaust pipe (232f) to exhaust the gas remaining inside the gas supply pipe (232a). Specifically, with valves (302a, 243a, 243e) closed, valves (302b to 302d) are opened, and the atmosphere inside the gas supply pipe (232a) is vacuum exhausted by the APC valve (244) and pump (246) of the exhaust pipe (231) through the gas supply pipe (232a) and exhaust pipe (232f). At this time, valve (243c) may be opened simultaneously to allow inert gas to flow into the gas supply pipe (232c). The inert gas is flow-regulated by the MFC (241c), supplied into the processing chamber (201) through the nozzle (249a), and exhausted from the exhaust pipe (231). In addition, at this time, the valve (243d) may be opened and an inert gas may be flowed into the gas supply pipe (232b, 232d).

[0043] By exhausting the atmosphere inside the gas supply pipe (232a), the amount of gas remaining inside the gas supply pipe (232a) can be reduced. Additionally, the dilution of the raw material gas stored in Step C, which will be described later, by the remaining gas can be suppressed. Furthermore, the amount of raw material gas stored in Step C can be increased. In addition, the efficiency of storing the raw material gas can be improved by exhausting so that the inside of the gas supply pipe (232a) becomes a vacuum atmosphere. Furthermore, the amount of raw material gas stored or the concentration of the raw material gas can be kept constant for each cycle.

[0044] [Step B]

[0045] Next, in this step, as shown in (A) of FIG. 3, raw gas is flowed from the upstream side of the gas supply pipe (232a) to the exhaust pipe (232f). Specifically, with valves (243a, 243e) closed, valves (302a to 302d) are opened, and raw gas is flowed from the upstream side of the gas supply pipe (232a) to the exhaust pipe (232f). At the same time, valve (243c) is opened, and inert gas is flowed into the gas supply pipe (232c). This prevents the atmosphere inside the processing chamber (201) from flowing back into the gas supply pipe (232a). The flow rate of the inert gas is adjusted by the MFC (241c), supplied into the processing chamber (201) through the nozzle (249a), and exhausted from the exhaust pipe (231). In addition, at this time, the valve (243d) may be opened and an inert gas may be flowed into the gas supply pipe (232b, 232d).

[0046] By flowing raw gas into the exhaust pipe (232f) from the upstream side of the gas supply pipe (232a), the gas remaining in the gas supply pipe (232a) is extruded by the raw gas and exhausted. Therefore, in the next step, the raw gas is diluted by the residual gas, so that the concentration of the raw gas can be suppressed and the concentration of the stored raw gas can be kept constant in each cycle.

[0047] [Step C]

[0048] Next, in this step, as shown in (B) of FIG. 3, raw gas is stored in the gas supply pipe (232a). Specifically, with valves (243a, 243e) closed, valves (302a, 302d) are closed, and raw gas is stored in the gas supply pipe (232a). At this time, with valve (243c) open, inert gas is flowed into the gas supply pipe (232c). That is, while raw gas is stored in the gas supply pipe (232a), inert gas is supplied from the gas supply pipe (232c) through the gas supply pipe (232a) to the space where the wafer (200) is present. By doing so, the atmosphere inside the processing room (201) can be suppressed from flowing back into the gas supply pipe (232a). The inert gas is flow-regulated by the MFC (241c) and supplied into the processing chamber (201) through the nozzle (249a), and exhausted from the exhaust pipe (231). At this time, the valve (243d) may also be opened to allow the inert gas to flow into the gas supply pipes (232b, 232d).

[0049] Here, the length of the gas supply pipe (232a) between the valve (243a) and the valve (302a) is configured to be longer than the length of the gas supply pipe (232a) between the valve (243a) and the reaction pipe (203), which is a processing vessel accommodating the wafer (200). By doing so, the amount of raw material gas stored can be increased, and the amount of residual gas that has flowed back from the processing chamber (201) to the gas supply pipe (232a) can be reduced. Additionally, the amount of inert gas supplied into the processing chamber (201) simultaneously with the raw material gas from the gas supply pipe (232e) can be reduced.

[0050] In this step, instead of valve (302a), valve (302c) or valve (302b) may be closed and raw gas may be stored downstream of valve (302c) or valve (302b). Additionally, either valve (302c) or valve (302b) may be closed based on predetermined data, and raw gas may be stored downstream of the closed valve. Furthermore, as predetermined data, data on the amount of stored gas based on the thickness of the gas supply pipe (232a) and the pipe length between each valve when each of valves (302a to 302c) is closed is stored in a memory device (121c), etc.

[0051] That is, the gas supply pipe (232a) can be used as a storage section for storing gas between the valve (243a) and the valve (302a), valve (302b), or valve (302c) of the gas supply pipe (232a) by closing any one of the valve (243a), valve (302a), valve (302b), or valve (302c). By doing so, the amount of raw gas stored in the gas supply pipe (232a) can be adjusted while suppressing backflow from the reaction pipe (203).

[0052] Specifically, for example, by closing valve (243a) and valve (302a), the amount of liquid stored in the gas supply pipe (232a) can be increased compared to valves (302b, 302c), and the amount of liquid remaining when it flows back from the processing room (201) to the gas supply pipe (232a) can be reduced. In addition, the amount of inert gas supplied from the gas supply pipe (232e) supplied to the processing room (201) can be reduced. In addition, for example, by closing valve (243a) and valve (302b), the amount of liquid stored in the gas supply pipe (232a) can be reduced compared to valve (302a). In addition, for example, by closing valve (243a) and valve (302c), the amount of liquid stored in the gas supply pipe (232a) can be reduced compared to valves (302a, 302b).

[0053] [Step D]

[0054] Next, in this step, raw gas is flowed into the processing chamber (201) as shown in (C) of FIG. 3. Specifically, with valves (302a, 302d) closed, valves (243a, 243e) are opened, and raw gas stored in the gas supply pipe (232a) is flowed into the processing chamber (201). At this time, the raw gas stored in the gas supply pipe (232a) is extruded by the inert gas supplied from the gas supply pipe (232e), supplied into the processing chamber (201) through the nozzle (249a), and exhausted from the exhaust pipe (231). At this time, with valve (243c) open, the flow rate of the inert gas supplied to the gas supply pipe (232c) by the MFC (241c) is made greater than the flow rate of the inert gas supplied to the gas supply pipe (232c) in the aforementioned steps A to C. The flow-controlled inert gas is supplied into the processing chamber (201) along with the raw gas and exhausted from the exhaust pipe (231). That is, the raw gas and inert gas are supplied to the space where the wafer (200) is present through the gas supply pipe (232a). In addition, to prevent the raw gas from entering the nozzle (249b), the valve (243d) is opened and the inert gas is flowed into the gas supply pipe (232d). The inert gas is supplied into the processing chamber (201) through the gas supply pipe (232d) and the nozzle (249b) and exhausted from the exhaust pipe (231).

[0055] As described above, after Step C, the valve (243a) is opened to supply inert gas from the upstream side of the gas supply pipe (232a), and the raw gas and inert gas stored in the gas supply pipe (232a) are supplied to the wafer (200). At this time, by simultaneously making the flow rate of the inert gas supplied from the gas supply pipe (232c) greater than the flow rate of the inert gas supplied from the gas supply pipe (232c) in Steps A to C described above, the inert gas supplied from the gas supply pipe (232c) acts to suppress the backflow of the atmosphere inside the processing room (201) in Steps A to C, and to dilute the raw gas in Step D. In addition, the flow rate of the inert gas supplied from the gas supply pipe (232c) is adjusted according to the concentration of the raw gas diluted in Step D.

[0056] By opening the valve (243a) and increasing the flow rate of the inert gas supplied from the gas supply pipe (232c), the concentration of the raw material gas supplied from the nozzle (249a) can be kept constant. Alternatively, the valve (243a) may be opened after increasing the flow rate of the inert gas supplied from the gas supply pipe (232c). In this case, the concentration of the raw material gas supplied from the nozzle (249a) can be lowered. Alternatively, the flow rate of the inert gas supplied from the gas supply pipe (232c) may be increased after opening the valve (243a). In this case, the concentration of the raw material gas supplied from the nozzle (249a) can be increased. That is, the opening and closing timing of the valve (243a) and the flow rate control of the inert gas by the MFC (241c) are performed according to the concentration of the raw material gas to be diluted.

[0057] In addition, in this step, by adjusting the MFC (241e, 241c), the flow rate of the inert gas supplied from the gas supply pipe (232e) is made greater than the flow rate of the inert gas supplied from the gas supply pipe (232c). By supplying the inert gas in this way, even when using a raw gas with low vapor pressure, the raw gas is extruded by the inert gas, and the supply amount of the raw gas between wafers (200) and within the wafer (200) surface can be equalized. Therefore, it is possible to suppress the deterioration of either or both of the film characteristic uniformity within the wafer (200) surface and the film characteristic uniformity between surfaces due to a lack of raw gas supply. In particular, it is possible to suppress the deterioration of the film characteristic uniformity between surfaces.

[0058] At this time, the main gas flowing into the processing room (201) is the raw material gas. That is, the raw material gas is supplied to the wafer (200).

[0059] As a source gas, a gas containing metal elements and halogen elements may be used. Here, as the metal element, in addition to transition metals from Group 3 to Group 12, elements including Group 13 elements may be used.

[0060] As a gas containing a metal element and a halogen element, a gas containing at least one element among, for example, molybdenum (Mo), zirconium (Zr), hafnium (Hf), aluminum (Al), indium (In), gallium (Ga), etc., and a halogen element may be used. In addition, as a gas containing a metal element and a halogen element, a gas containing a metal element and at least one element among, for example, fluorine (F), chlorine (Cl), bromine (Br), iodine (I), etc. may be used. As a gas containing a metal element and a halogen element, it is preferable to use a gas containing a metal element and Cl. One or more of these may be used as a source gas.

[0061] That is, as gases containing metal elements and halogen elements, zirconium chloride (ZrCl4) gas, hafnium chloride (HfCl4) gas, aluminum chloride (AlCl3) gas, gallium chloride (GaCl3) gas, indium chloride (InCl3) gas, molybdenum pentachloride (MoCl5) gas, molybdenum dioxide dichloride (MoO2Cl2) gas, molybdenum tetrachloride (MoOCl4) gas, etc., can be used. One or more of these can be used as raw materials.

[0062] As an inert gas, for example, in addition to nitrogen (N2) gas, noble gases such as argon (Ar) gas, helium (He) gas, neon (Ne) gas, and xenon (Xe) gas can be used. It is preferable to use Ar gas as an inert gas. In addition, one or more of these can be used as inert gases.

[0063] [Residual gas removal, Step (S2)]

[0064] After a first layer containing a metal element and a halogen element is formed on at least a portion of the wafer (200), valves (243a, 243b) are closed and valves (243c, 243d) are opened, and inert gas as a purge gas is supplied into the gas supply pipes (232a, 232b) through the gas supply pipes (232c, 232d), and the APC valve (244) of the exhaust pipe (231) is opened so that the processing chamber (201) is vacuum exhausted by the pump (246) and the processing chamber (201) is purged.

[0065] [Reaction gas supply process, step (S3)]

[0066] Next, a reaction gas is supplied to the wafer (200) inside the processing chamber (201) to exhaust it. Specifically, the valve (243b) is opened and the reaction gas is flowed into the gas supply pipe (232b). The reaction gas is flow-regulated by the MFC (241b), supplied into the processing chamber (201) via the nozzle (249b), and exhausted from the exhaust pipe (231). At the same time, the valve (243d) is opened and an inert gas is flowed into the gas supply pipe (232d). The inert gas is flow-regulated by the MFC (241d), supplied into the processing chamber (201) together with the reaction gas, and exhausted from the exhaust pipe (231). Additionally, to prevent the reaction gas from entering the nozzle (249a), the valve (243c) is opened and an inert gas is flowed into the gas supply pipe (232c). Inert gas is supplied into the processing chamber (201) via the gas supply pipe (232c) and nozzle (249a), and is exhausted from the exhaust pipe (231).

[0067] At this time, the main gas flowing into the processing room (201) is a reaction gas. That is, the reaction gas is supplied to the wafer (200).

[0068] A reducing gas may be used as the reaction gas. For example, a gas containing the element hydrogen (H) may be used as the reducing gas. As a gas containing H, gases such as hydrogen (H2) gas, monosilane (SiH4) gas, disilane (Si2H6) gas, trisilane (Si3H8) gas, ammonia (NH3) gas, hydrazine (N2H4) gas, and phosphine (PH3) gas may be used. One or more of these may be used as the reaction gas.

[0069] Specifically, when, for example, MoCl5 gas is used as the raw material gas and, for example, H2 gas is used as the reaction gas, the Cl in the MoCl5 gas is reduced by the H2 gas as the MoCl5 gas reacts with the MoCl5 gas, and the first layer containing metal elements and halogen elements on the wafer (200) is modified into a second layer containing metal elements.

[0070] [Residual gas removal, Step (S4)]

[0071] After a second layer containing a metal element is formed on the wafer (200), an inert gas as a purge gas is supplied in the same processing order as the aforementioned step (S2), and the APC valve (244) of the exhaust pipe (231) is opened so that the inside of the processing chamber (201) is vacuum exhausted by the pump (246) and the inside of the processing chamber (201) is purged.

[0072] [Perform a set number of times, Step (S5)]

[0073] A predetermined film of a predetermined thickness is formed on a wafer (200) by performing a cycle of performing the aforementioned steps (S1) to (S4) in sequence a predetermined number of times (n times, where n is an integer of 1 or 2 or more). Specifically, for example, a molybdenum (Mo) containing film, which is a metal containing film, is formed. If the number of cycles of performing steps (S1) to (S4) in sequence is less than the predetermined number, the process returns to step (S1).

[0074] (After purge and return to atmospheric pressure)

[0075] Inert gas is supplied into the treatment chamber (201) from each of the gas supply pipes (232c, 232d) and exhausted from the exhaust pipe (231). The inert gas acts as a purge gas. By doing so, the treatment chamber (201) is purged, and any residual gas or reaction byproducts remaining in the treatment chamber (201) are removed from the treatment chamber (201). Afterward, the atmosphere inside the treatment chamber (201) is replaced with inert gas, and the pressure inside the treatment chamber (201) returns to normal pressure.

[0076] (Wafer Export)

[0077] The cap (219) is lowered by the elevator (115) and the bottom of the MF (209) is opened. Then, the processed wafer (200) is supported on the boat (217) and is removed from the bottom of the MF (209) to the outside of the reaction tube (203). The processed wafer (200) is removed from the boat (217).

[0078] (3) Other forms

[0079] Next, a modified example of the substrate processing device (100) in the aforementioned form will be described in detail. In the following modified example, only the differences from the aforementioned form will be described in detail.

[0080] (Variation Example)

[0081] In this modified example, as shown by the dashed line in FIG. 1, a gas supply pipe (232c) that supplies inert gas is installed upstream of the valve (243a) of the gas supply pipe (232a). Even when the gas supply pipe (232c) is installed upstream of the valve (243) of the gas supply pipe (232a), the raw material gas can be diluted and supplied to the wafer (200), and the supply amount of raw material gas can be increased. That is, in this modified example, the same effect as the aforementioned form can be obtained.

[0082] In addition, the above-described form was explained by citing an example in which a cycle of performing steps A through D in sequence as a raw gas supply process [step (S1)] is performed a predetermined number of times (m times, where m is an integer of 1 or 2 or more). The present disclosure is not limited to the above-described form, and a cycle of performing steps B through D in sequence may be performed a predetermined number of times (m times, where m is an integer of 1 or 2 or more) without performing step A. In this form, the same effect as in the above-described form can be obtained, and in this modified example, the processing time can be further shortened.

[0083] In addition, the above-described embodiment described an example of forming a film using a batch-type substrate processing apparatus that processes multiple wafers at once. The present disclosure is not limited to the above-described embodiment and can preferably be applied to cases where a film is formed using, for example, a single-wafer type substrate processing apparatus that processes one or multiple wafers at once. In addition, the above-described embodiment described an example of forming a film using a substrate processing apparatus that includes a hot wall type processing furnace. The present disclosure is not limited to the above-described embodiment and can preferably be applied to cases where a film is formed using a substrate processing apparatus that includes a cold wall type processing furnace.

[0084] Even when using such a substrate processing device, each process can be performed with the same processing sequence and processing conditions as the aforementioned forms or variations, and the same effects as the aforementioned forms or variations can be obtained.

[0085] The aforementioned forms or variations may be used in appropriate combination. In this case, the processing order and processing conditions may be the same as, for example, the processing order and processing conditions of the aforementioned forms or variations.

[0086] The forms and variations of the present disclosure have been specifically described above. However, the forms and variations of the present disclosure are not limited to the aforementioned forms and variations, and various modifications are possible within the scope of not departing from the gist thereof. Explanation of the symbols

[0087] 200: Wafer (substrate) 232a: Gas supply pipe (1st gas pipe) 243a: Valve (First Valve)

Claims

Claim 1 (a) a process of closing a first valve of a first gas pipe and supplying a raw gas from the upstream side of the first gas pipe to store the raw gas in the first gas pipe; and (b) a process of opening the first valve of the first gas pipe and supplying a first inert gas from the upstream side of the first gas pipe to supply the raw gas and the first inert gas from the first gas pipe to a substrate, comprising a substrate processing method. Claim 2 In claim 1, (b) a substrate processing method in which a second inert gas is supplied to the first gas pipe from a second gas pipe connected to the first gas pipe. Claim 3 In paragraph 2, the substrate processing method wherein the second gas pipe is installed downstream of the first valve. Claim 4 In paragraph 2, the substrate processing method wherein the second gas pipe is installed upstream of the first valve. Claim 5 A substrate processing method according to paragraph 3, comprising the process of supplying the second inert gas from the second gas pipe through the first gas pipe between (a) to the space where the substrate exists. Claim 6 A substrate processing method according to claim 5, wherein the flow rate of the second inert gas in (b) is greater than the flow rate of the second inert gas in (c). Claim 7 In paragraph 2, (b) a substrate processing method in which the flow rate of the first inert gas is greater than the flow rate of the second inert gas. Claim 8 In claim 1, the method comprises a third gas pipe connected upstream of the first gas pipe and the first valve, (d) a process of flowing the raw material gas into the third gas pipe from upstream of the first gas pipe, and (a) a substrate processing method performed after (d). Claim 9 A substrate processing method according to claim 1, comprising a third gas pipe connected upstream of the first valve of the first gas pipe, and (e) a process of exhausting the atmosphere in the first gas pipe from the third gas pipe before (a). Claim 10 A substrate processing method according to claim 8, comprising a process of exhausting the atmosphere in the first gas pipe from the third gas pipe before (f) (d). Claim 11 A substrate processing method according to claim 1, comprising a second valve installed upstream of the first valve of the first gas pipe, and (a) closing the second valve and storing the raw gas downstream of the second valve. Claim 12 A substrate processing method according to claim 11, comprising a third valve installed upstream of the second valve of the first gas pipe, and (a) closing either the second valve or the third valve based on predetermined data, and storing the raw gas downstream of the closed valve. Claim 13 A substrate processing method according to claim 1, comprising a fourth valve installed upstream of the first valve of the first gas pipe, wherein the length of the first gas pipe between the first valve and the fourth valve is longer than the length of the first gas pipe between the first valve and the processing vessel accommodating the substrate. Claim 14 A substrate processing method according to claim 1, wherein the vapor pressure of the raw material gas is lower than the vapor pressure of another gas supplied to the substrate. Claim 15 A substrate treatment method according to claim 1, wherein the raw material gas comprises at least one element among Mo, Zr, Hf, Al, In, and Ga, and a gas containing a halogen element. Claim 16 (a) a process of closing a first valve of a first gas pipe and supplying a raw gas from the upstream side of the first gas pipe to store the raw gas in the first gas pipe; and (b) a process of opening the first valve of the first gas pipe and supplying a first inert gas from the upstream side of the first gas pipe to supply the raw gas and the first inert gas from the first gas pipe to a substrate. A method for manufacturing a semiconductor device comprising: (a) a process of closing a first valve of a first gas pipe and supplying a raw gas from the upstream side of the first gas pipe to store the raw gas and the first inert gas. Claim 17 (a) closing the first valve of the first gas pipe and supplying a raw gas from the upstream side of the first gas pipe to store the raw gas in the first gas pipe; and (b) opening the first valve of the first gas pipe and supplying a first inert gas from the upstream side of the first gas pipe to supply the raw gas and the first inert gas from the first gas pipe to a substrate, a program for executing the steps of the first valve of the first gas pipe and supplying the raw gas and the first inert gas from the first gas pipe to a substrate processing device by a computer. Claim 18 A substrate processing apparatus comprising: a first gas pipe for supplying raw gas to a substrate; a first valve installed in the first gas pipe; a first inert gas supply unit for supplying a first inert gas from the upstream side of the first gas pipe; and a control unit configured to control the first valve and the first inert gas supply unit so as to perform the following processes: (a) closing the first valve of the first gas pipe and supplying the raw gas from the upstream side of the first gas pipe and storing the raw gas within the first gas pipe; and (b) opening the first valve of the first gas pipe and supplying the first inert gas from the upstream side of the first gas pipe and supplying the raw gas and the first inert gas from the first gas pipe to the substrate. Claim 19 A gas supply system comprising a first gas pipe for supplying raw gas to a substrate, a first valve installed in the first gas pipe, and a first inert gas supply unit for supplying a first inert gas from the upstream side of the first gas pipe, and configured to enable controlling the first valve and the first inert gas supply unit to perform the following processes: (a) closing the first valve of the first gas pipe and supplying the raw gas from the upstream side of the first gas pipe and storing the raw gas in the first gas pipe; and (b) opening the first valve of the first gas pipe and supplying the first inert gas from the upstream side of the first gas pipe and supplying the raw gas and the first inert gas from the first gas pipe to the substrate.

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