Method of processing substrate, method of manufacturing semiconductor device, program and substrate processing apparatus

Abstract

The film characteristics of a metal-based film formed on a substrate are improved. (a) a process of supplying a second metal-containing gas to a substrate having a first metal film and an insulating film to form a first film containing a second metal on the first metal film, and (b) a process of supplying a second metal-containing gas to a substrate to form a second film containing a second metal on the first film and the insulating film.

Description

Technology Field

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

[0002] For example, a low-resistance tungsten (W) film is used as a word line of a NAND-type flash memory or DRAM having a three-dimensional structure. In addition, a titanium nitride (TiN) film is used as a barrier film between this W film and an insulating film (see, for example, Patent Documents 1 and 2). Prior art literature

[0003] Japanese Patent Publication No. 2011-66263, International Publication No. 2019 / 058608, Pamphlet The problem to be solved

[0004] However, as the stacking of three-dimensional NAND-type flash memory becomes more complex, etching becomes difficult, making the word line thinner is a challenge. To solve this problem, a method for forming a metal-based film with good film properties without forming a barrier film as described above is required.

[0005] The present disclosure aims to provide a technology capable of improving the film properties of a metal-based film. means of solving the problem

[0006] According to one aspect of the present disclosure,

[0007] (a) a process of supplying a second metal-containing gas to a substrate having a first metal film and an insulating film to form a first film containing a second metal on the first metal film, and (b) a process of supplying a second metal-containing gas to a substrate to form a second film containing a second metal on the first film and the insulating film. Effects of the invention

[0008] According to one aspect of the present disclosure, it is possible to improve the film properties of a metal-based film formed on a substrate. Brief explanation of the drawing

[0009] FIG. 1 is a cross-sectional view illustrating a schematic diagram of a vertical processing unit of a substrate processing apparatus in one embodiment of the present disclosure. Figure 2 is a schematic cross-sectional view of line AA in Figure 1. FIG. 3 is a schematic diagram of a controller of a substrate processing device in one embodiment of the present disclosure, and is a block diagram illustrating the control system of the controller. FIG. 4 is a drawing illustrating a substrate processing process in one embodiment of the present disclosure. Specific details for implementing the invention

[0010] The following description will be explained with reference to FIGS. 1 to 4. Furthermore, the drawings used in the following description are all 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 each other among multiple drawings.

[0011] (1) Configuration of the substrate processing device

[0012] The substrate processing device (10) is provided with a processing furnace (202) that has a heater (207) as a heating means (heating mechanism, heating system). The heater (207) is cylindrical in shape and is installed vertically by being supported by a heater base (not shown) as a holding support plate.

[0013] Inside the heater (207), an outer tube (203) is arranged concentrically with the heater (207) to form a reaction tube (reaction vessel, processing vessel). The outer tube (203) is made of a heat-resistant material, such as quartz (SiO2) or silicon carbide (SiC), and is formed in a cylindrical shape with the top closed and the bottom open. Below the outer tube (203), a manifold (inlet flange) (209) is arranged concentrically with the outer tube (203). The manifold (209) is made of a metal, such as stainless steel (SUS), and is formed in a cylindrical shape with the top and bottom open. An O-ring (220a) serving as a sealing member is provided between the top of the manifold (209) and the outer tube (203). As the manifold (209) is supported on the heater base, the outer tube (203) is installed vertically.

[0014] An inner tube (204) constituting a reaction vessel is disposed on the inner side of the outer tube (203). The inner tube (204) is composed of a heat-resistant material such as quartz or SiC, for example, and is formed in a cylindrical shape with the top closed and the bottom open. The processing vessel (reaction vessel) is mainly composed of the outer tube (203), the inner tube (204), and the manifold (209). A processing chamber (201) is formed in the hollow portion of the processing vessel (inside the inner tube (204)).

[0015] The processing chamber (201) is configured to accommodate a wafer (200) as a substrate arranged in multiple stages in a vertical direction in a horizontal position by a boat (217) as a support.

[0016] In the processing chamber (201), nozzles (410, 420, 430) are provided to penetrate the side wall of the manifold (209) and the inner tube (204). Gas supply pipes (310, 320, 330) are each connected to the nozzles (410, 420, 430). However, the processing furnace (202) of the present embodiment is not limited to the form described above.

[0017] In the gas supply pipes (310, 320, 330), a mass flow controller (MFC) (312, 322, 332), which is a flow controller (flow control unit), is provided in order from the upstream side. In addition, in the gas supply pipes (310, 320, 330), a valve (314, 324, 334), which is an opening and closing valve, is provided in each of the gas supply pipes (310, 320, 330). A gas supply pipe (510, 520, 530) that supplies inert gas is connected to the downstream side of the valve (314, 324, 334) of the gas supply pipes (310, 320, 330). In the gas supply pipes (510, 520, 530), MFCs (512, 522, 532), which are flow controllers (flow control units), and valves (514, 524, 534), which are open / close valves, are respectively provided in order from the upstream side.

[0018] A nozzle (410, 420, 430) is connected to the tip of each gas supply pipe (310, 320, 330). The nozzle (410, 420, 430) is configured as an L-shaped nozzle, and its horizontal portion is provided to penetrate the side wall of the manifold (209) and the inner tube (204). The vertical portion of the nozzle (410, 420, 430) is provided inside a channel-shaped (groove-shaped) pre-chamber (201a) that is formed to protrude outward in the diameter direction of the inner tube (204) and also extend in the vertical direction, and is provided within the pre-chamber (201a) in a direction upward along the inner wall of the inner tube (204) (upward in the arrangement direction of the wafer (200)).

[0019] The nozzles (410, 420, 430) are provided to extend from the lower region of the processing chamber (201) to the upper region of the processing chamber (201), and each has a plurality of gas supply holes (410a, 420a, 430a) provided at a position facing the wafer (200). Accordingly, processing gas is supplied to the wafer (200) from each of the gas supply holes (410a, 420a, 430a) of the nozzles (410, 420, 430). These gas supply holes (410a, 420a, 430a) are provided in plurality from the lower to the upper part of the inner tube (204), each have the same opening area, and are also provided with the same opening pitch. However, the gas supply holes (410a, 420a, 430a) are not limited to the shape described above. For example, the opening area of ​​the inner tube (204) may be gradually increased from the bottom to the top. By doing so, it becomes possible to make the flow rate of the gas supplied from the gas supply holes (410a, 420a, 430a) more uniform.

[0020] The gas supply holes (410a, 420a, 430a) of the nozzles (410, 420, 430) are provided in multiple locations at a height from the bottom to the top of the boat (217) described later. Accordingly, the processing gas supplied into the processing chamber (201) from the gas supply holes (410a, 420a, 430a) of the nozzles (410, 420, 430) is supplied to the entire area of ​​the wafer (200) accommodated from the bottom to the top of the boat (217). The nozzles (410, 420, 430) may be provided to extend from the lower area to the upper area of ​​the processing chamber (201), but it is preferable that they be provided to extend to the vicinity of the ceiling of the boat (217).

[0021] From the gas supply pipe (310), a raw material gas containing a metal element (also called a metal-containing gas or a second metal-containing gas) as a processing gas is supplied into the processing chamber (201) via the MFC (312), valve (314), and nozzle (410).

[0022] From the gas supply pipe (320), reducing gas is supplied as a processing gas into the processing chamber (201) via the MFC (322), valve (324), and nozzle (420).

[0023] From the gas supply pipe (330), reforming gas is supplied as a processing gas into the processing chamber (201) via the MFC (332), valve (334), and nozzle (430).

[0024] From the gas supply pipes (510, 520, 530), argon (Ar) gas, for example, as an inert gas, is supplied into the processing chamber (201) via the MFC (512, 522, 532), valve (514, 524, 534), and nozzle (410, 420, 430), respectively. Below, an example of using Ar gas as an inert gas will be described, but as an inert gas, in addition to Ar gas, noble gases such as helium (He) gas, neon (Ne) gas, and xenon (Xe) gas may be used.

[0025] In the case where raw gas is flowed from the gas supply pipe (310), the raw gas supply system is mainly formed by the gas supply pipe (310), MFC (312), and valve (314), but the nozzle (410) may be included in the raw gas supply system. The raw gas supply system may also be referred to as the metal-containing gas supply system (second metal-containing gas supply system). In addition, when reducing gas is flowed from the gas supply pipe (320), the reducing gas supply system is mainly formed by the gas supply pipe (320), MFC (322), and valve (324), but the nozzle (420) may be included in the reducing gas supply system. In addition, when reforming gas is flowed from the gas supply pipe (330), the reforming gas supply system is mainly formed by the gas supply pipe (330), MFC (332), and valve (334), but the nozzle (430) may be included in the reforming gas supply system. Additionally, the metal-containing gas supply system, the reducing gas supply system, and the reforming gas supply system may also be referred to as the processing gas supply system. Additionally, the nozzles (410, 420, 430) may be considered to be included in the processing gas supply system. Furthermore, the inert gas supply system is mainly composed of gas supply pipes (510, 520, 530), MFCs (512, 522, 532), and valves (514, 524, 534).

[0026] In the present embodiment, the method of gas supply involves conveying gas through nozzles (410, 420, 430) arranged in a pre-chamber (201a) within a circular, vertically elongated space defined by the inner wall of the inner tube (204) and the end of a plurality of wafers (200). Then, gas is ejected into the inner tube (204) from a plurality of gas supply holes (410a, 420a, 430a) provided at positions facing the wafers of the nozzles (410, 420, 430). More specifically, raw gas, etc., is ejected in a direction parallel to the surface of the wafer (200) through the gas supply hole (410a) of the nozzle (410), the gas supply hole (420a) of the nozzle (420), and the gas supply hole (430a) of the nozzle (430).

[0027] The exhaust hole (exhaust port) (204a) is a through hole formed in a position opposite to the nozzle (410, 420, 430) on the side wall of the inner tube (204), and is, for example, a slit-shaped through hole that is thin and long in the vertical direction. Gas supplied into the processing chamber (201) from the gas supply holes (410a, 420a, 430a) of the nozzle (410, 420, 430) and flowing over the surface of the wafer (200) flows through the exhaust hole (204a) into the gap (inside the exhaust passage (206)) formed between the inner tube (204) and the outer tube (203). Then, the gas flowing into the exhaust passage (206) flows into the exhaust pipe (231) and is discharged out of the processing chamber (202).

[0028] The exhaust hole (204a) is provided in a position facing the plurality of wafers (200), and the gas supplied from the gas supply holes (410a, 420a, 430a) to the vicinity of the wafers (200) in the processing room (201) flows in a horizontal direction and then flows into the exhaust passage (206) through the exhaust hole (204a). The exhaust hole (204a) is not limited to being configured as a through hole in the shape of a slit, but may be configured by a plurality of holes.

[0029] The manifold (209) is provided with an exhaust pipe (231) for exhausting the atmosphere inside the processing room (201). The exhaust pipe (231) is connected in order from the upstream side to the pressure sensor (245) as a pressure detector (pressure detection unit) for detecting the pressure inside the processing room (201), an APC (Auto Pressure Controller) valve (243), and a vacuum pump (246) as a vacuum exhaust device. The APC valve (243) can perform vacuum exhaust and vacuum exhaust stoppage inside the processing room (201) by opening and closing the valve while the vacuum pump (246) is operating, and can also adjust the pressure inside the processing room (201) by adjusting the degree of valve opening while the vacuum pump (246) is operating. The exhaust system is mainly composed of an exhaust hole (204a), an exhaust passage (206), an exhaust pipe (231), an APC valve (243), and a pressure sensor (245). The vacuum pump (246) may be considered to be included in the exhaust system.

[0030] Below the manifold (209), a seal cap (219) is provided as a cover capable of hermetically sealing the lower opening of the manifold (209). The seal cap (219) is configured to be in contact with the lower end of the manifold (209) from the vertical lower side. The seal cap (219) is made of a metal such as SUS, for example, and is formed in a disc shape. On the upper surface of the seal cap (219), an O-ring (220b) is provided as a sealing member that contacts the lower end of the manifold (209). On the side opposite the processing chamber (201) in the seal cap (219), a rotation mechanism (267) is installed to rotate a boat (217) that accommodates a wafer (200). The rotation axis (255) of the rotation mechanism (267) passes through the seal cap (219) and is connected to the boat (217). The rotating mechanism (267) is configured to rotate the wafer (200) by rotating the boat (217). The seal cap (219) is configured to be raised vertically by a boat elevator (115) which is a lifting mechanism installed vertically on the outside of the outer tube (203). The boat elevator (115) is configured to enable the boat (217) to be brought into and taken out of the processing room (201) by raising the seal cap (219). The boat elevator (115) is configured as a conveying device (conveying mechanism, conveying system) that conveys the boat (217) and the wafer (200) contained in the boat (217) into and out of the processing room (201).

[0031] The boat (217) is configured to arrange multiple wafers (200), for example 25 to 200 wafers, in a horizontal position and with their centers aligned with one another, spaced apart in the vertical direction. The boat (217) is composed of a heat-resistant material, for example, quartz or SiC. At the bottom of the boat (217), a dummy substrate (218), composed of a heat-resistant material, for example, quartz or SiC, is supported in a horizontal position in multiple stages. With this configuration, heat from the heater (207) is made difficult to transfer to the seal cap (219). However, this embodiment is not limited to the form described above. For example, instead of providing a dummy substrate (218) at the bottom of the boat (217), an insulating tube composed of a tube-shaped member made of a heat-resistant material, such as quartz or SiC, may be provided.

[0032] As shown in FIG. 2, a temperature sensor (263) as a temperature detector is installed inside the inner tube (204), and the amount of current supplied to the heater (207) is adjusted based on the temperature information detected by the temperature sensor (263), thereby configuring the temperature inside the processing chamber (201) to have a desired temperature distribution. The temperature sensor (263) is configured in an L-shape, similar to the nozzles (410, 420, 430), and is provided along the inner wall of the inner tube (204).

[0033] As illustrated in FIG. 3, 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. An input / output device (122), configured as, for example, a touch panel, is connected to the controller (121).

[0034] 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, and a process recipe containing the steps or conditions of the semiconductor device manufacturing method (substrate processing method) described later are stored in a readable manner. The process recipe is a combination that allows each process (each step) in the semiconductor device manufacturing method (substrate processing method) described later to be executed by the controller (121) to obtain a predetermined result, and functions as a program. Hereinafter, this process recipe, control program, etc. are collectively referred to simply as a program. In this specification, when the term "program" is used, it may include only the process recipe, only the control program, or a combination of the process recipe and the control program. The RAM (121b) is configured as a memory area (work area) where programs or data read by the CPU (121a) are temporarily maintained.

[0035] The I / O port (121d) is connected to the above-described MFC (312, 322, 332, 512, 522, 532), valve (314, 324, 334, 514, 524, 534), pressure sensor (245), APC valve (243), vacuum pump (246), heater (207), temperature sensor (263), rotating mechanism (267), boat elevator (115), etc.

[0036] The CPU (121a) is configured to read and execute a control program from a memory device (121c), and also to read a recipe, etc. 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 (312), 322, 332, 512, 522, 532), the opening and closing operation of the valve (314, 324, 334, 514, 524, 534), the opening and closing operation of the APC valve (243), the pressure adjustment operation based on the pressure sensor (245) by the APC valve (243), the temperature adjustment operation of the heater (207) based on the temperature sensor (263), the starting and stopping of the vacuum pump (246), the rotation and rotation speed adjustment operation of the boat (217) by the rotation mechanism (267), the lifting operation of the boat (217) by the boat elevator (115), and the receiving operation of the wafer (200) into the boat (217), according to the contents of the read recipe.

[0037] The controller (121) can be configured by installing the above-described program stored in an external storage device (e.g., magnetic tape, magnetic disk such as a flexible disk or hard disk, optical disk such as a CD or DVD, magneto-optical disk such as an MO, semiconductor memory such as a USB memory or memory card) (123) into a computer. The storage device (121c) and the external storage device (123) are configured as computer-readable recording media. Hereinafter, these are collectively referred to simply as recording media. In this specification, the recording media may include only the storage device (121c), only the external storage device (123), or both. Providing the program to the computer may be done using communication means such as the internet or a dedicated line, without using the external storage device (123).

[0038] (2) Substrate processing process

[0039] As a process of manufacturing a semiconductor device, an example of a process for forming a film containing a second metal (also referred to as a second metal-containing film) on a wafer (200), for example, used as a control gate electrode of a 3DNAND, is described using FIG. 4. The process of forming the second metal-containing film is carried out using the processing furnace (202) of the substrate processing device (10) described above. In the following description, the operation of each part constituting the substrate processing device (10) is controlled by a controller (121).

[0040] In the substrate processing process (semiconductor device manufacturing process) according to the present embodiment,

[0041] (a) a process of supplying a second metal-containing gas to a wafer (200) having a first metal film and an insulating film to form a first film containing the second metal on the first metal film, and

[0042] (b) A process of supplying the second metal-containing gas to the wafer (200) to form a second film containing the second metal on the first film and the insulating film.

[0043] Perform the above steps and form a first film and a second film containing a second metal on the wafer (200).

[0044] In this specification, the term "wafer" may be used to mean "the wafer itself" or "a laminate of a wafer and a predetermined layer or film, etc. formed on its surface." In this specification, the term "surface of a wafer" may be used to mean "the surface of the wafer itself" or "the surface of a predetermined layer or film, etc. formed on the wafer." In this specification, the term "substrate" is used in the same way as the term "wafer."

[0045] (Wafer import)

[0046] When multiple wafers (200) are loaded (wafer charged) into the boat (217), as shown in FIG. 1, the boat (217) supporting the multiple wafers (200) is lifted by the boat elevator (115), brought into the processing room (201) (boat loaded), and received into the processing container. In this state, the seal cap (219) closes the lower opening of the outer tube (203) through the O-ring (220).

[0047] Here, the wafer (200) has a first metal film and an insulating film.

[0048] As insulating films, there are oxide films, nitride films, oxynitride films, carbonate films, carbonate nitride films, etc., containing at least one element such as a Group 13 element, a Group 14 element, or a Group 3 element. Examples include aluminum oxide (AlO) films, silicon oxide (SiO) films, titanium oxide (TiO) films, zirconium oxide (ZrO) films, hafnium oxide (HfO) films, silicon nitride (SiN) films, silicon oxynitride (SiON) films, silicon carbonate (SiOC) films, silicon carbonate nitride (SiOCN) films, etc. Furthermore, they may be composite films of these materials or laminated films of these materials. Additionally, the Si in the SiN, SiON, SiOC, and SiOCN described herein may be a film in which Si is substituted with other Group 13 elements, Group 14 elements, Group 3 elements, etc.

[0049] Additionally, the first metal film and the insulating film of the wafer (200) may be formed on the same horizontal plane or on different planes. The other plane is, for example, a case where a plurality of concave portions are formed on the wafer (200), such that the first metal film is formed on the inner surface of the concave portion and the side wall of the concave portion is formed as an insulating film.

[0050] The first metal and the second metal are metals comprising, for example, at least one of tungsten (W), titanium (Ti), ruthenium (Ru), cobalt (Co), and molybdenum (Mo). The first metal and the second metal may be metal elements or compounds having the same element as the main element. Additionally, the first metal and the second metal may be metal elements or compounds having different elements as the main element. The gas containing the second metal comprises the second metal and at least one halogen element. The halogen element is, for example, fluorine (F), chlorine (Cl), bromine (Br), and iodine (I). Specific examples of the second metal-containing gas include, for instance, tungsten hexafluoride (WF6) gas, tungsten hexachloride (WCl6) gas, molybdenum trichloride (MoCl3) gas, molybdenum chloride (MoCl5) gas, molybdenum dioxide (MoO2Cl2) gas containing Mo, oxygen (O), and Cl, molybdenum tetrachloride (MoOCl4) gas, ruthenium hexafluoride (RuF6) gas, etc.

[0051] In a film formation using a compound containing such a halogen element (referred simply to as a halide in this disclosure), a reaction may occur in which the halide itself or a reaction by-product generated by using the halide etches (removes) a second metal-containing layer formed on the wafer (200). The amount of this etching reaction can be adjusted (controlled) by, for example, the configuration of the wafer (200) to be processed, the gas supply sequence of the substrate processing process, and various processing conditions.

[0052] The composition of the wafer (200) is, for example, the type of film existing on the surface of the wafer (200) and the structure existing on the surface of the wafer (200). For example, regarding the type of film, the etching reaction is more likely to occur on the insulating film than on the metal film. That is, the removal reaction of the second metal-containing layer during the formation of the second metal-containing layer is more likely to occur on the insulating film.

[0053] Conditions for forming the second metal-containing layer include, for example, a gas supply sequence, the temperature of the wafer (200), and the supply amount of the second metal-containing gas. By increasing the temperature of the wafer (200) to increase the reactivity of the second metal-containing gas, it is possible to facilitate the occurrence of an etching reaction. Additionally, it is effective to set the temperature of the wafer (200) to a temperature at which a decomposition reaction of the second metal-containing gas can occur. Furthermore, as a condition, increasing the supply amount of the second metal-containing gas can facilitate the occurrence of an etching reaction. Here, the supply amount refers to at least one of the supply flow rate of the second metal-containing gas, the supply time, and the pressure inside the processing room (201). Additionally, the supply amount of the second metal-containing gas may be increased by combining these. For example, the supply amount can be increased by adjusting the product of the supply flow rate and the supply time. Furthermore, adjusting the product of the supply flow rate and the supply time means increasing at least one of the supply flow rate and the supply time to increase the supply amount.

[0054] In addition, methods to reduce the amount of etching reaction, or to increase the amount of film formation reaction more than the amount of etching reaction, include, for example, controlling the reverse of these or modifying the surface condition of the wafer (200).

[0055] As a method for modifying the surface condition of the wafer (200), for example, there is a method of supplying a modification gas to the wafer (200) that promotes or inhibits the adsorption of a second metal-containing gas on the surface of the wafer (200). By supplying such a modification gas to the wafer (200), at least one part of the modification gas can be adsorbed on the wafer (200). By adjusting the ease of combination between at least one part of the adsorbed modification gas and the second metal-containing gas, the amount of the etching reaction can be adjusted (controlled). Examples of controlling the amount of the second metal-containing layer (second metal-containing film) and the amount of etching will be described later.

[0056] Here, the adjustment of the amount of the second metal-containing layer and the amount of etching is effective, in particular, when the following structure is formed on the wafer (200). As for the structure formed on the wafer (200), for example, there is a structure in which a plurality of concave portions are formed, a first metal film is exposed on the innermost surface of the concave portions, and an insulating film is exposed on the side wall surface of the concave portions.

[0057] In addition, reaction by-products generated by using halides include, for example, at least one of the following. The reaction by-products generated may vary depending on the gas supply sequence of the substrate processing process or various conditions.

[0058] A) Halogen generated by the decomposition of halides. Such generation occurs, for example, when the temperature of the wafer (200) at the time of supplying the halides is at a decomposition temperature, or when a gas that decomposes the halides is present in the processing room (201) or on the surface of the wafer (200).

[0059] B) Halogen generated when the halogen comes into contact with the surface of the wafer (200). This generation occurs, for example, when the halogen comes into contact with the surface of the wafer (200), and the halogen contained in the halogen is detached.

[0060] C) Halogen generated by the reaction between a halide and a reaction gas (reducing gas). Such generation occurs when the reaction gas is supplied to a halide adsorbed on the surface of the wafer (200), causing the halide to react with the reaction gas. Additionally, it may also occur when the halide reacts with the reaction gas in the gas phase within the processing room (201).

[0061] (Pressure adjustment and temperature adjustment)

[0062] The space within the processing room (201), that is, the space where the wafer (200) exists, is vacuumed by a vacuum pump (246) so that the pressure (vacuum level) is reached. 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 (243) is feedback controlled (pressure adjustment). The vacuum 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 the processing room (201) is reached. At this time, the amount of current supplied to the heater (207) is feedback controlled (temperature adjustment) based on the temperature information detected by the temperature sensor (263) so that the temperature distribution within the processing room (201) is reached. The heating of the processing room (201) by the heater (207) is continued for at least until the processing of the wafer (200) is completed.

[0063] [Formation process of the first layer (first film)]

[0064] [Second metal-containing gas supply, Step S11]

[0065] The valve (314) is opened to flow the second metal-containing gas, which is the raw material gas, into the gas supply pipe (310). The second metal-containing gas is flow-regulated by the MFC (312), supplied into the processing chamber (201) from the gas supply hole (410a) of the nozzle (410), and exhausted from the exhaust pipe (231). At this time, the second metal-containing gas is supplied to the wafer (200). At the same time, the valve (514) is opened to flow an inert gas, such as Ar gas, into the gas supply pipe (510). The Ar gas flowing into the gas supply pipe (510) is flow-regulated by the MFC (512), supplied into the processing chamber (201) together with the second metal-containing gas, and exhausted from the exhaust pipe (231). At this time, in order to prevent the second metal-containing gas from entering the nozzle (420), the valve (524) may be opened to allow Ar gas to flow into the gas supply pipe (520). The Ar gas is supplied into the processing chamber (201) through the gas supply pipe (320) and the nozzle (420) and is exhausted from the exhaust pipe (231).

[0066] At this time, the APC valve (243) is adjusted so that the pressure inside the processing chamber (201) is set to, for example, 1000 Pa, within the range of 1 to 3990 Pa. The supply flow rate of the second metal-containing gas controlled by the MFC (312) is set to, for example, within the range of 0.1 to 3.0 slm, preferably 0.4 to 2.5 slm. The supply flow rate of the Ar gas controlled by the MFCs (512, 522) is set to, for example, within the range of 0.1 to 20 slm. The time for supplying the second metal-containing gas to the wafer (200) is set to, for example, 1 to 60 seconds, preferably 1 to 10 seconds. The temperature of the wafer (200) is set to a temperature of 300 to 700°C. Preferably, it is 500 to 700°C. In addition, in the present disclosure, a numerical range notation such as “1 to 3990 Pa” means that the lower and upper limits are included in that range. Accordingly, for example, “1 to 3990 Pa” means “1 Pa or more and 3990 Pa or less.” The same applies to other numerical ranges.

[0067] At this time, the gas flowing into the processing room (201) is only the second metal-containing gas and Ar gas. By supplying the second metal-containing gas, a second metal-containing layer is formed on the wafer (200).

[0068] Here, by making the supply amount of the second metal-containing gas greater than that of Step S21 described later, a first second metal-containing layer can be preferentially formed on the first metal film having the wafer (200). Here, the supply amount of the second metal-containing gas refers to at least one of the supply flow rate of the second metal-containing gas, the supply time of the second metal-containing gas, and the pressure within the processing room (201) as the space where the wafer (200) exists. At least one of these is made greater than that of Step S21 described later. In addition, the supply amount of the second metal-containing gas may be adjusted by a combination of these.

[0069] In addition, by making the temperature of the wafer (200) in the process of forming the first layer (first film) (the temperature in the processing room (201) where the wafer (200) exists) higher than the temperature of the wafer (200) in the process of forming the second layer (second film), it is possible to promote the preferential formation of the first second metal-containing layer on the first metal film.

[0070] (Removal of residual gas, Step S12)

[0071] After the supply of the second metal-containing gas is started, the valve (314) of the gas supply pipe (310) is closed after a predetermined time has elapsed, for example, 1 to 60 seconds, to stop the supply of the second metal-containing gas. At this time, the APC valve (243) of the exhaust pipe (231) is left open so that the inside of the processing chamber (201) is vacuum-exhausted by the vacuum pump (246), and any unreacted gas remaining in the processing chamber (201) or the second metal-containing gas that contributed to the formation of the first second metal-containing layer is removed from the processing chamber (201). That is, the inside of the processing chamber (201) is purged. At this time, the valves (514, 524) are left open so that the supply of Ar gas into the processing chamber (201) is maintained. Ar gas acts as a purge gas and can enhance the effect of excluding unreacted gas remaining in the treatment chamber (201) or second metal-containing gas after contributing to the formation of the first second metal-containing layer from the treatment chamber (201).

[0072] (1st reduction gas supply, Step S13)

[0073] After removing residual gas from the processing chamber (201), the valve (324) is opened, and the first reducing gas is flowed into the gas supply pipe (320). The flow rate of the first reducing gas is controlled by the MFC (322), supplied into the processing chamber (201) from the gas supply hole (420a) of the nozzle (420), and exhausted from the exhaust pipe (231). At this time, the first reducing gas is supplied to the wafer (200). At the same time, the valve (524) is opened, and Ar gas is flowed into the gas supply pipe (520). The flow rate of the Ar gas flowing into the gas supply pipe (520) is controlled by the MFC (522). The Ar gas is supplied into the processing chamber (201) together with the first reducing gas and exhausted from the exhaust pipe (231). At this time, in order to prevent the first reducing gas from entering the nozzle (410), the valve (514) is opened to allow Ar gas to flow into the gas supply pipe (510). The Ar 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).

[0074] At this time, the APC valve (243) is adjusted so that the pressure inside the processing chamber (201) is set to a pressure within the range of, for example, 1 to 13,000 Pa, for example, 10,000 Pa. The supply flow rate of the first reducing gas controlled by the MFC (322) is set to a flow rate within the range of, for example, 1 to 50 slm, preferably 15 to 30 slm. The supply flow rate of the Ar gas controlled by the MFC (512, 522) is set to a flow rate within the range of, for example, 0.1 to 30 slm. At this time, the time for supplying the first reducing gas to the wafer (200) is set to a time within the range of 5 minutes or more and 30 minutes or less, for example, 20 minutes. By supplying the first reducing gas to the wafer (200) for a time of 5 minutes or more, the second metal-containing gas adsorbed on the wafer (200) can be reduced, and by making the time 30 minutes or less, the throughput can be improved and productivity can be secured.

[0075] At this time, the gas flowing into the processing chamber (201) is only the first reducing gas and Ar gas. The first reducing gas reacts with at least a portion of the first second metal-containing layer formed in step S11. Then, a second metal layer (second metal film) as a first film is preferentially formed on the first metal film.

[0076] Here, the first reducing gas is, for example, a gas composed of hydrogen (H). Preferably, it is a gas composed of hydrogen alone. Specifically, hydrogen (H2) gas or deuterium (D2) can be used.

[0077] (Residual gas removal, Step S14)

[0078] After forming the second metal layer, the valve (324) is closed to stop the supply of the first reducing gas. Then, by a processing procedure similar to the above-described step S12, any unreacted gas remaining in the processing chamber (201) or any first reducing gas or reaction by-products that contributed to the formation of the second metal layer are removed from the processing chamber (201). That is, the processing chamber (201) is purged.

[0079] (Perform a prescribed number of times)

[0080] By performing the cycle of sequentially performing the steps S11 to S14 described above a predetermined number of times (X times, where X is an integer of 1 or 2 or more), a first film (second metal film) of a predetermined thickness is preferentially formed on the first metal film. It is preferable to repeat the above-described cycle multiple times.

[0081] In addition, if a structure as described above is formed on the wafer (200), a first film is formed from the inner surface of the concave portion.

[0082] [Process of forming the modified layer]

[0083] Between the process of forming the first film and the process of forming the second film, a process of forming a modified layer may be performed. While it is possible to make the first film and the second film different simply by making the conditions of the first film formation process and the conditions of the second film formation process different, it is also easy to make the first film and the second film different by performing a process of forming a modified layer. Furthermore, when performing the process of forming a modified layer, the conditions of the first film formation process and the conditions of the second film formation process do not need to be significantly different. For example, there is a condition in which substrate processing is performed without making the temperature setting of the process wafer (200) for forming the first film different from the temperature setting of the process wafer (200) for forming the second film different.

[0084] An example of the process for forming a modified layer is explained.

[0085] (Supply of reforming gas, Step S31)

[0086] The valve (334) is opened to allow reforming gas to flow into the gas supply pipe (330). The reforming gas is flow-regulated by the MFC (332), supplied into the processing chamber (201) through the gas supply hole (430a) of the nozzle (430), and exhausted through the exhaust pipe (231). At this time, reforming gas is supplied to the wafer (200). At the same time, the valve (534) may be opened to allow an inert gas, such as Ar gas, to flow into the gas supply pipe (530). The Ar gas flowing through the gas supply pipe (530) is flow-regulated by the MFC (532), supplied into the processing chamber (201) together with the reforming gas, and exhausted through the exhaust pipe (231). At this time, in order to prevent the reforming gas from entering the nozzle (410, 420), the valve (514, 524) may be opened to allow Ar gas to flow into the gas supply pipe (510, 520). The Ar gas is supplied into the processing chamber (201) through the gas supply pipe (310, 320) and the nozzle (410, 420), and is exhausted from the exhaust pipe (231).

[0087] At this time, the APC valve (243) is adjusted so that the pressure inside the processing chamber (201) is, for example, set to 1000 Pa, within the range of 1 to 3990 Pa. The supply amount of reforming gas controlled by the MFC (332) is set to a flow rate within the range of 0.01 to 5.0 slm, for example. The time for supplying the reforming gas to the wafer (200) is set to a time within the range of 1 to 600 seconds, for example.

[0088] At this time, the gas flowing into the processing room (201) consists only of the reformed gas, or the reformed gas and an inert gas. By supplying the reformed gas, an adsorption layer (third layer) of the reformed gas is formed on the wafer (200).

[0089] Here, the reforming gas is a gas containing, for example, at least one of a Group 13 element, a Group 14 element, or a Group 15 element. Examples of these elements include boron (B), silicon (Si), and phosphorus (P). More preferably, the reforming gas is a hydrogen compound. Examples of hydrogen compounds containing a Group 13 element include boron hydrides such as monoborane (BH3) and diborane (B2H6). Examples of hydrogen compounds containing a Group 14 element include silicon hydrides such as monosilane (SiH4), disilane (Si2H6), and trisilane (Si3H8). Examples of hydrogen compounds containing a Group 15 element include phosphorus hydrides such as phosphine (PH3) and diphosphine (P2H4). In addition, as a reforming gas containing a Group 15 element, in addition to hydrides, alkylphosphine gases such as trimethylphosphine ((CH3)3P) gas, triethylphosphine ((C2H5)3P) gas, trinormalpropylphosphine ((n-C3H7)3P) gas, triisopropylphosphine ((i-C3H7)3P) gas, trinormalbutylphosphine ((n-C4H9)3P) gas, triisobutylphosphine ((i-C4H9)3P) gas, tritertiarybutylphosphine ((t-C4H9)3P) gas, and tertiarybutylphosphine (t-C4H9PH2) gas, aminophosphine (NH2PH2) gas, tris(dimethylamino)phosphine ([(CH3)2N)]3P) gas, and bis(dimethylamino)phosphine (PH[N(CH3)2]2) gas, In some cases, aminophosphine-based gases such as bis(dimethylamino)chlorophosphine ([(CH3)2N]2PCl) gas, or phosphinasamide-based gases such as bis(dimethylamino)methylphosphine (CH3P[N(CH3)2]2) gas, dimethylaminodimethylphosphine ((CH3)2PN(CH3)2) gas, or diethylaminodiethylphosphine ((C2H5)2PN(C2H5)2) gas may be used.

[0090] Preferably, a gas containing P and hydrogen (H) is used as the reforming gas. By supplying this gas to the wafer (200), a reforming layer containing at least P is formed on the surface of the wafer (200). Preferably, the reforming layer is a layer containing P and H. More preferably, the reforming layer is a layer containing molecules of a Group 15 element-containing material or a material in which molecules of a Group 15 element-containing material have partially decomposed. For example, when PH3 is used as the Group 15 element-containing material, the first layer formed is P, H, PH x It may include. Here, X is an integer less than or equal to 3, and PH x The material is, for example, at least one of PH, PH2, and PH3. In addition, in order to form a modified layer containing such a material, it is preferable that the temperature in the treatment chamber (201) be at a temperature at which a portion of the material containing the group 15 element can decompose. For example, when PH3 is used as the material containing the group 15 element, the temperature in the treatment chamber (201) is set to a temperature in the range of 300°C to 650°C.

[0091] (Residual gas removal, Step S32)

[0092] After a predetermined amount of time has elapsed since the supply of reforming gas began, the valve (334) of the gas supply pipe (330) is closed to stop the supply of reforming gas. At this time, the APC valve (243) of the exhaust pipe (231) is left open so that the inside of the processing chamber (201) is vacuum-exhausted by the vacuum pump (246), and any unreacted or reforming gas remaining in the processing chamber (201) or that contributed to the formation of the reforming layer is removed from the processing chamber (201). That is, the atmosphere inside the processing chamber (201) is exhausted. By lowering the pressure inside the processing chamber (201), the reforming gas remaining in the gas supply pipe (330) or the nozzle (430) can be exhausted. By exhausting the reforming gas remaining in the gas supply pipe (330) or nozzle (430), the reforming gas remaining in the gas supply pipe (330) or nozzle (430) can be suppressed from being supplied into the treatment chamber (201) during the next second film formation process. Additionally, at this time, the valves (514, 524, 534) may be kept open to maintain the supply of Ar gas into the treatment chamber (201). In addition to acting as a gas to suppress gas entry into each nozzle, Ar gas can be used as a purge gas. When Ar gas is supplied as a purge gas, the effect of excluding unreacted or reforming gas remaining in the treatment chamber (201) or that contributed to the formation of the reforming layer from the treatment chamber (201) can be enhanced.

[0093] [Process of forming the second layer (second film)]

[0094] (Second metal-containing gas supply, Step S21)

[0095] The valve (314) is opened to flow the second metal-containing gas, which is the raw material gas, into the gas supply pipe (310). Additionally, the second metal-containing gas used in the second film formation process may be the same gas as the second metal-containing gas used in the first film formation process described above, or it may be a different type of second metal-containing gas. Here, the use of the same gas as the second metal-containing gas used in the first film formation process is described as an example. The flow rate of the second metal-containing gas is controlled by the MFC (312), supplied into the processing chamber (201) from the gas supply hole (410a) of the nozzle (410), and exhausted from the exhaust pipe (231). At this time, the second metal-containing gas is supplied to the wafer (200). At the same time, the valve (514) is opened to flow an inert gas, such as Ar gas, into the gas supply pipe (510). The Ar gas flowing through the gas supply pipe (510) has its flow rate adjusted by the MFC (512) and is supplied into the processing chamber (201) along with the second metal-containing gas, and is exhausted from the exhaust pipe (231). At this time, in order to prevent the second metal-containing gas from entering the nozzle (420), the valve (524) is opened to allow the Ar gas to flow into the gas supply pipe (520). The Ar 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).

[0096] At this time, the APC valve (243) is adjusted to set the pressure inside the processing chamber (201) to, for example, 1000 Pa, within the range of 1 to 3990 Pa. The supply amount of the second metal-containing gas controlled by the MFC (312) is set to a smaller supply amount than during the first film formation process. Here, the supply amount is adjusted, for example, by the supply flow rate. The supply flow rate of the second metal-containing gas is set to a flow rate within the range of, for example, 0.1 to 1.0 slm, preferably 0.1 to 0.3 slm. In this way, it is preferable to make it smaller than the flow rate supplied in step S11. The supply flow rate of the Ar gas controlled by the MFC (512, 522) is set to a flow rate within the range of, for example, 0.1 to 20 slm. The time for supplying the second metal-containing gas to the wafer (200) is set to, for example, 1 to 60 seconds, preferably 5 to 20 seconds. The temperature of the wafer (200) is set to a temperature of 300 to 700°C. Preferably, it is 300 to 600°C. Here, when the second metal-containing layer is formed on each of the first film and the insulating film, it is preferable to reduce the supply amount of the second metal-containing gas compared to the first film formation process. That is, at least one of the second metal-containing gas supply flow rate, supply time, and pressure inside the processing room (201) is reduced compared to step S11. If the formation of the modified layer is performed after the first film formation process, the supply amount of the second metal-containing gas may be the same as that of the first film formation process.

[0097] In addition, by making the temperature of the wafer (200) in the process of forming the second layer (second film) lower than the temperature of the wafer (200) in the process of forming the first layer (first film), the formation of the second film can be promoted on both the first film and the insulating film.

[0098] At this time, the gas flowing into the processing chamber (201) is only the second metal-containing gas and Ar gas. By supplying the second metal-containing gas, a second second metal-containing layer is formed on the wafer (200). Here, when the first film and the insulating film are exposed on the wafer (200), the second second metal-containing layer is formed on the first film and on the insulating film, respectively.

[0099] If a process for forming a modified layer is performed after the process for forming a first film, the modified layer formed on the first film and the insulating film reacts with the second metal-containing gas, causing molecules containing the second metal to be deposited on the first film and the insulating film. Additionally, the modified layer reacts with the second metal-containing gas, causing elements or molecules contained in the modified layer to detach from the modified layer. During this detachment process, elements or molecules constituting the modified layer can be introduced into the second metal-containing layer.

[0100] (Removal of residual gas, Step S22)

[0101] After forming the second second metal-containing layer, the valve (314) is closed to stop the supply of the second metal-containing gas. Then, by a processing procedure similar to the above-described step S12, any unreacted gas or reaction by-products remaining in the processing chamber (201) or those that contributed to the formation of the second second metal-containing layer are removed from the processing chamber (201). That is, the processing chamber (201) is purged.

[0102] (2nd reduction gas supply, Step S23)

[0103] After removing residual gas from the processing chamber (201), the valve (324) is opened to flow a second reducing gas into the gas supply pipe (320). The second reducing gas is flow-regulated by the MFC (322), supplied into the processing chamber (201) from the gas supply hole (420a) of the nozzle (420), and exhausted from the exhaust pipe (231). At this time, the second reducing gas is supplied to the wafer (200). At the same time, the valve (524) is opened to flow Ar gas into the gas supply pipe (520). The Ar gas flowing into the gas supply pipe (520) is flow-regulated by the MFC (522). The Ar gas is supplied into the processing chamber (201) together with the second reducing gas and exhausted from the exhaust pipe (231). At this time, to prevent the second reducing gas from entering the nozzle (410), the valve (514) is opened to allow Ar gas to flow into the gas supply pipe (510). The Ar 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). Additionally, the second reducing gas may be configured to use the same type of gas as the first reducing gas, or a different type of reducing gas.

[0104] At this time, the APC valve (243) is adjusted so that the pressure inside the processing chamber (201) is set to a pressure within the range of, for example, 1 to 13,000 Pa, for example, 10,000 Pa. The supply flow rate of the reducing gas controlled by the MFC (322) is set to a flow rate within the range of, for example, 1 to 50 slm, preferably 15 to 30 slm. The supply flow rate of the Ar gas controlled by the MFC (512, 522) is set to a flow rate within the range of, for example, 0.1 to 30 slm.

[0105] At this time, the gas flowing into the processing room (201) is only the second reducing gas and Ar gas. The second reducing gas reacts with at least a portion of the second metal-containing layer formed on the wafer (200) in step S21. Then, a second metal layer is formed as a second film on the wafer (200).

[0106] (Residual gas removal, Step S24)

[0107] After forming the second metal layer, the valve (324) is closed to stop the supply of the second reducing gas. Then, by the same processing procedure as described above in step S14, any unreacted gas remaining in the processing chamber (201) or any second reducing gas or reaction by-products that contributed to the formation of the second metal layer are removed from the processing chamber (201). That is, the processing chamber (201) is purged.

[0108] (Perform a prescribed number of times)

[0109] By performing the cycle of sequentially performing the steps S21 to S24 described above a predetermined number of times (Y times, where Y is an integer of 1 or 2 or more), a second film of a predetermined thickness is formed on a wafer (200) on which a first film is formed. It is preferable to repeat the above-described cycle multiple times.

[0110] Additionally, when the wafer (200) has a first metal film and an insulating film, the second film is formed on the first film and on the insulating film. That is, unlike the first film, the second film is formed over the entire wafer (200).

[0111] (After purge and return to atmospheric pressure)

[0112] Ar gas is supplied into the treatment chamber (201) from each of the gas supply pipes (510, 520) and exhausted from the exhaust pipe (231). The Ar gas acts as a purge gas, thereby purging the treatment chamber (201) with an inert gas, and removing any remaining gas or reaction by-products from the treatment chamber (201) (after-purge). Afterward, the atmosphere inside the treatment chamber (201) is replaced with an inert gas (inert gas replacement), and the pressure inside the treatment chamber (201) is returned to normal pressure (atmospheric pressure return).

[0113] (Wafer Export)

[0114] After that, the seal cap (219) is lowered by the boat elevator (115), and the bottom of the outer tube (203) is opened. Then, the processed wafer (200) is discharged (boat unloaded) from the bottom of the outer tube (203) to the outside of the outer tube (203) while being supported by the boat (217). After that, the processed wafer (200) is discharged from the boat (217).

[0115] (3) Effects of this embodiment

[0116] According to the present embodiment, one or more of the effects shown below can be obtained.

[0117] (a) A second metal-containing film with different properties can be laminated.

[0118] (b) When irregularities are formed on the wafer (200), a metal film is exposed on the inner surface of the concave portion, and an insulating film is exposed on the side of the concave portion, a second metal-containing film can be formed from the inner surface of the wafer (200). That is, the inside of the concave portion can be uniformly filled with the second metal-containing film. In addition, by filling the second metal-containing film from the inner surface of the concave portion, the collapse of the convex portion (side wall of the concave portion) can be suppressed. That is, the collapse of the pattern formed on the wafer (200) can be suppressed.

[0119] (c) By making the supply amount of the second metal-containing gas in the first film formation process greater than the supply amount of the second metal-containing gas in the second film formation process, the amount of film formed on the bottom surface (first metal film) side of the concave portion in the first film formation process can be greater than the amount of etching, and the amount of film formed on the sidewall (insulating film) side of the concave portion can be less than the amount of etching. That is, the first film can be formed preferentially on the first metal film. In other words, the first film can be formed selectively on the first metal film. In addition, the selectivity of the first film formation can be improved.

[0120] (d) By making the temperature of the wafer (200) in the first film formation process higher than the temperature of the wafer (200) in the second film formation process, the amount of film formed on the bottom surface (first metal film) side of the concave portion in the first film formation process can be greater than the amount of etching, and the amount of film formed on the sidewall (insulating film) side of the concave portion can be less than the amount of etching. That is, the first film can be formed preferentially on the first metal film. In other words, the first film can be formed selectively on the first metal film. In addition, the selectivity of the first film formation can be improved.

[0121] (e) By performing a modification layer formation process after the first film formation process, the amount of film formed in the second film formation process can be made greater than the amount of etching in each part. That is, in the second film formation process after the modification layer formation process, it becomes possible to form the second film uniformly on the wafer (200). In other words, the selectivity of the second film formation can be reduced. Specifically, by using PH3 gas as the modification gas, PH3 is used as the modification layer. x A layer containing is formed. This pH xThe halides are prone to chemical reactions, and a layer containing a second metal is formed on the wafer (200), and molecules containing P are detached from the modified layer. Examples of molecules containing P include phosphoryl chloride (POCl3). Because such a reaction occurs, the deposition rate of the second metal-containing film can be improved. That is, the deposition rate can be made to exceed the etching rate. In addition, through this chemical reaction, an element (e.g., P) contained in the modified layer is introduced into the second metal-containing film (it is also said that the element contained in the modified layer diffuses into the second metal-containing film).

[0122] (4) Other embodiments

[0123] In the above-described embodiment, an example of forming a film using a batch-type substrate processing apparatus that processes multiple substrates at once was described. The present disclosure is not limited to the above-described embodiment and can be suitably applied to cases where a film is formed using, for example, a single-wafer type substrate processing apparatus that processes one or several substrates at once. Furthermore, in the above-described embodiment, an example of forming a film using a substrate processing apparatus having a hot-wall type processing furnace was described. The present disclosure is not limited to the above-described embodiment and can be suitably applied to cases where a film is formed using a substrate processing apparatus having a cold-wall type processing furnace.

[0124] Even when using these substrate processing devices, each process can be performed with the same processing procedure and processing conditions as the embodiments or variations described above, and the same effects as the embodiments or variations described above are obtained.

[0125] It is preferable to prepare (prepare multiple) process recipes (programs containing processing steps, processing conditions, etc.) used for forming these various thin films individually, according to the content of the substrate processing (film type, composition ratio, film quality, film thickness, processing steps, processing conditions, etc. of the thin film to be formed). Furthermore, when starting the substrate processing, it is preferable to appropriately select a suitable process recipe from among the multiple process recipes according to the content of the substrate processing. Specifically, it is preferable to store (install) in advance the multiple process recipes prepared individually according to the content of the substrate processing in a memory device (121c) equipped by the substrate processing device, via an electrical communication line or a recording medium (external storage device (123)) on which the said process recipes are recorded. Furthermore, when starting the substrate processing, it is preferable for the CPU (121a) equipped by the substrate processing device to appropriately select a suitable process recipe from among the multiple process recipes stored in the memory device (121c) according to the content of the substrate processing. By configuring it in this way, it becomes possible to universally and reproducibly form thin films of various types, composition ratios, film qualities, and film thicknesses with a single substrate processing device. In addition, the operator's operational burden (such as input burdens like processing procedures or processing conditions) can be reduced, and substrate processing can be started quickly while avoiding operational errors.

[0126] In addition, the present disclosure can also be realized, for example, by changing the process recipe of an existing substrate processing device. When changing the process recipe, it is possible to install the process recipe according to the present disclosure into an existing substrate processing device by interposing a telecommunication line or a recording medium on which the process recipe is recorded, or to change the process recipe itself to the process recipe according to the present disclosure by operating the input / output device of the existing substrate processing device.

[0127] The embodiments of the present disclosure have been described in detail above. However, the present disclosure is not limited to the embodiments described above, and various modifications are possible within the scope of not departing from the gist thereof. Explanation of the symbols

[0128] 10: Substrate processing device 121: Controller 200: Wafer (substrate) 201: Processing Room

Claims

Claim 1 (a) a process of supplying a second metal-containing gas containing a second metal halide to a substrate in which a first metal film and an insulating film are exposed, to form a first film containing the second metal on the first metal film, and (b) a process of supplying the second metal-containing gas to the substrate to form a second film containing the second metal on the first film and the insulating film, wherein the supply time of the second metal-containing gas in (a) is greater than the supply time of the second metal-containing gas in (b). Claim 2 A substrate processing method according to claim 1, wherein the supply amount of the second metal-containing gas in (a) is greater than the supply amount of the second metal-containing gas in (b). Claim 3 A substrate processing method according to claim 1, wherein the supply flow rate of the second metal-containing gas in (a) is greater than the supply flow rate of the second metal-containing gas in (b). Claim 4 delete Claim 5 A substrate processing method according to claim 1, wherein the pressure in the space where the substrate exists in (a) is greater than the pressure in the space where the substrate exists in (b). Claim 6 A substrate treatment method according to claim 1, having a process of supplying a reforming gas before (b). Claim 7 A substrate treatment method according to claim 6, wherein in (a) and (b), a reducing gas is supplied, and the reforming gas is a compound different from the reducing gas. Claim 8 A substrate treatment method according to claim 6, wherein the reforming gas is a hydrogen compound comprising at least one of a Group 13 element, a Group 14 element, and a Group 15 element. Claim 9 In claim 6, the substrate processing method wherein the reforming gas comprises at least one of boron, silicon, and phosphorus. Claim 10 A substrate treatment method according to claim 6, wherein the reforming gas comprises at least one of BH3, B2H6, SiH4, Si2H6, Si3H8, and PH3. Claim 11 A substrate treatment method according to any one of claims 1 to 3 and claims 5 to 10, wherein the first metal and the second metal comprise at least one of W, Ti, Ru, Co, and Mo. Claim 12 A substrate treatment method according to any one of claims 1 to 3 and 5 to 10, wherein (a) comprises: (a1) a process of supplying the second metal-containing gas to the substrate; and (a2) a process of supplying the first reducing gas to the substrate. Claim 13 In claim 12, (b) is a substrate processing method having (b1) a process of supplying the second metal-containing gas to the substrate and (b2) a process of supplying the second reducing gas to the substrate. Claim 14 (a) a process of supplying a second metal-containing gas containing a second metal halide to a substrate in which a first metal and an insulating film are exposed, to form a first film containing the second metal on the first metal, and (b) a process of supplying the second metal-containing gas to the substrate to form a second film containing the second metal on the first film and the insulating film, wherein the supply time of the second metal-containing gas in (a) is greater than the supply time of the second metal-containing gas in (b). Claim 15 (a) a step of supplying a second metal-containing gas containing a second metal halide to a substrate in which a first metal and an insulating film are exposed, thereby forming a first film containing the second metal on the first metal, and (b) a step of supplying the second metal-containing gas to the substrate to form a second film containing the second metal on the first film and the insulating film, and a step of making the supply time of the second metal-containing gas in (a) greater than the supply time of the second metal-containing gas in (b), a program recorded on a computer-readable recording medium. Claim 16 A substrate processing apparatus having a gas supply system for supplying a second metal-containing gas containing a second metal halide to a substrate having a first metal film and an insulating film exposed thereto, (a) a process of supplying the second metal-containing gas to a substrate having the first metal film and an insulating film to form a first film containing the second metal on the first metal film, (b) a process of supplying the second metal-containing gas to the substrate to form a second film containing the second metal on the first film and the insulating film, and a control unit configured to control the gas supply system to perform a process in which the supply time of the second metal-containing gas in (a) is greater than the supply time of the second metal-containing gas in (b).

Images