Film deposition method and film deposition apparatus

Abstract

To provide a technology that can achieve both good step coverage and high productivity.SOLUTION: A deposition method according to one aspect of the present disclosure has the following processes: (a) preparing a substrate having a recess on its surface, (b) supplying an organic raw material gas to the surface and causing the organic raw material gas to be adsorbed in the recess, (c) supplying an oxygen-containing gas to the surface and oxidizing the organic raw material gas adsorbed in the recess, and (d) after the process (c), supplying a first gas containing a dehydrating agent to the surface.SELECTED DRAWING: Figure 7

Description

Technical Field

[0001] The present disclosure relates to a film forming method and a film forming apparatus.

Background Art

[0002] Before adsorbing the source gas, a film forming technique is known in which an additive gas capable of controlling the adsorbability of the source gas is supplied to adjust the amount of OH groups while performing film formation by atomic layer deposition (see, for example, Patent Document 1).

Prior Art Documents

Patent Documents

[0003]

Patent Document 1

Summary of the Invention

Problems to be Solved by the Invention

[0004] The present disclosure provides a technique capable of achieving both good step coverage and high productivity.

Means for Solving the Problems

[0005] A film forming method according to an aspect of the present disclosure includes: (a) a step of preparing a substrate having a recess on a surface; (b) a step of supplying an organic source gas to the surface and adsorbing the organic source gas in the recess; (c) a step of supplying an oxygen-containing gas to the surface and oxidizing the organic source gas adsorbed in the recess; and (d) a step of supplying a first gas containing a dehydrating agent to the surface after the step (c). death , The first gas contains an inert gas, and the flow rate of the inert gas is greater than the flow rate of the dehydrating agent. .

Effects of the Invention

[0006] According to the present disclosure, both good step coverage and high productivity can be achieved.

Brief Description of the Drawings

[0007] [Figure 1] Figure 1 is a cross-sectional view showing an example of the configuration of a film deposition apparatus according to an embodiment. [Figure 2] Figure 2 is a perspective view showing the internal configuration of the film deposition apparatus shown in Figure 1. [Figure 3] Figure 3 is a plan view showing the internal configuration of the film deposition apparatus shown in Figure 1. [Figure 4] Figure 4 is a cross-sectional view of the vacuum vessel along the circumferential direction of the rotary table. [Figure 5] Figure 5 is a cross-sectional view of the vacuum vessel along the radial direction of the rotating table. [Figure 6] Figure 6 is a plan view showing another example of the configuration of the film deposition apparatus according to the embodiment. [Figure 7] Figure 7 is a flowchart showing an example of a film deposition method according to the present invention. [Figure 8] Figure 8 is a schematic diagram showing an example of a film deposition method according to the embodiment. [Figure 9] Figure 9 is a schematic diagram showing a conventional film deposition method. [Figure 10] Figure 10 shows a method for evaluating the embedding characteristics of a silicon oxide film. [Figure 11] Figure 11 shows the evaluation results of the embedding characteristics of the silicon oxide film. [Modes for carrying out the invention]

[0008] Hereinafter, exemplary embodiments of the present disclosure, not limited to those described herein, will be described with reference to the attached drawings. In all attached drawings, the same or corresponding members or components are denoted by the same or corresponding reference numerals, and redundant descriptions are omitted.

[0009] [Film forming equipment] Referring to Figures 1 to 5, a film deposition apparatus according to an embodiment will be described. As shown in Figures 1 to 3, the film deposition apparatus comprises a flat vacuum vessel 1 having a substantially circular planar shape, and a rotary table 2 provided inside the vacuum vessel 1 and having a rotation center at the center of the vacuum vessel 1. The vacuum vessel 1 has a bottomed cylindrical container body 12, and a top plate 11 that is airtightly and detachably arranged on the upper surface of the container body 12 via a sealing member 13 (Figure 1), such as an O-ring.

[0010] The rotary table 2 is fixed at its center to a cylindrical core 21. The core 21 is fixed to the upper end of a vertically extending rotating shaft 22. The rotating shaft 22 penetrates the bottom 14 of the vacuum vessel 1, and its lower end is attached to a drive unit 23 that rotates the rotating shaft 22 (Figure 1) around a vertical axis. The rotating shaft 22 and the drive unit 23 are housed in a cylindrical case body 20 with an open top. The flange portion of the case body 20 is airtightly attached to the bottom surface of the bottom 14 of the vacuum vessel 1, maintaining an airtight seal between the internal atmosphere of the case body 20 and the external atmosphere.

[0011] As shown in Figures 2 and 3, the surface of the rotary table 2 is provided with circular recesses 24 for placing multiple substrates W (five in the illustrated example) along the rotation direction (circumferential direction). In Figure 3, for convenience, only one substrate W is shown in the recess 24. The substrate W may be, for example, a semiconductor wafer. The recess 24 has an inner diameter slightly larger than the diameter of the substrate W and a depth approximately equal to the thickness of the substrate W. When the substrate W is placed in the recess 24, the surface of the substrate W and the surface of the rotary table 2 (the area where the substrate W is not placed) are at the same height. Through holes (none shown) are formed in the bottom surface of the recess 24 through which, for example, three lifting pins pass to support the back surface of the substrate W and raise and lower the substrate W.

[0012] FIG. 2 and FIG. 3 are diagrams for explaining the structure inside the vacuum chamber 1. For the sake of convenience in explanation, the illustration of the top plate 11 is omitted. As shown in FIGS. 2 and 3, above the rotary table 2, reaction gas nozzles 31, 32, 33 and separation gas nozzles 41, 42 made of, for example, quartz are arranged at intervals in the circumferential direction of the vacuum chamber 1 (the rotation direction of the rotary table 2 indicated by the arrow A in FIG. 3). In the illustrated example, from the transfer port 15 described later in the clockwise direction (the rotation direction of the rotary table 2), the reaction gas nozzle 33, the separation gas nozzle 41, the reaction gas nozzle 31, the separation gas nozzle 42 and the reaction gas nozzle 32 are provided in this order. The reaction gas nozzles 31, 32, 33 and the separation gas nozzles 41, 42 have gas introduction ports 31a, 32a, 33a, 41a, 42a (FIG. 3) which are the base ends fixed to the outer peripheral wall of the container body 12, respectively. The reaction gas nozzles 31, 32, 33 and the separation gas nozzles 41, 42 are introduced into the vacuum chamber 1 from the outer peripheral wall of the vacuum chamber 1 and are attached so as to extend horizontally with respect to the rotary table 2 along the radial direction of the container body 12.

[0013] The reaction gas nozzles 31, 32 are provided with a plurality of discharge holes 31h, 32h (FIG. 4) that open toward the rotary table 2 at intervals along the length direction of the reaction gas nozzles 31, 32. Similarly, the reaction gas nozzle 33 is also provided with a plurality of discharge holes (not shown) that open toward the rotary table 2 at intervals along the length direction of the reaction gas nozzle 33.

[0014] The separation gas nozzle 42 is provided with a plurality of discharge holes 42h (FIG. 4) that open toward the rotary table 2 at intervals along the length direction of the separation gas nozzle 42. Similarly, the separation gas nozzle 41 is also provided with a plurality of discharge holes (not shown) that open toward the rotary table 2 at intervals along the length direction of the separation gas nozzle 41.

[0015] The organic raw material gas is introduced from the organic raw material gas supply unit 111 into the reaction gas nozzle 31. The organic raw material gas supply unit 111 includes an organic raw material gas supply path 111a, an organic raw material gas source 111b, a flow controller 111c, and a valve 111d. The organic raw material gas supply path 111a is provided outside the vacuum vessel 1. The organic raw material gas supply path 111a is connected to the reaction gas nozzle 31. The organic raw material gas source 111b, the flow controller 111c, and the valve 111d are provided in the organic raw material gas supply path 111a in order from the upstream side to the downstream side in the gas flow direction. Thereby, the supply timing of the organic raw material gas from the organic raw material gas source 111b is controlled by the valve 111d, and the flow rate is adjusted to a predetermined value by the flow controller 111c. The organic raw material gas flows from the organic raw material gas supply path 111a into the reaction gas nozzle 31 and is discharged from the reaction gas nozzle 31 into the vacuum vessel 1. The flow controller 111c may be, for example, a mass flow controller.

[0016] The organic raw material gas may be, for example, a gas containing a metal element, a carbon element, and a hydrogen element. The metal element may be, for example, Al (aluminum), Ti (titanium), Sr (strontium), zirconium (Zr), or hafnium (Hf). The organic raw material gas may be, for example, tris(dimethylamino)cyclopentadienyl zirconium gas.

[0017] A plurality of reaction gas nozzles 31 may be provided at intervals in the circumferential direction of the vacuum vessel 1. In this case, the organic raw material gas supply unit 111 is configured to introduce the organic raw material gas into the plurality of reaction gas nozzles 31. The lower region of the reaction gas nozzle 31 becomes an adsorption region P1 for adsorbing the organic raw material gas to the substrate W.

[0018] Oxygen-containing gas is introduced into the reaction gas nozzle 32 from the oxygen-containing gas supply unit 112. The oxygen-containing gas supply unit 112 comprises an oxygen-containing gas supply path 112a, an oxygen-containing gas source 112b, a flow controller 112c, and a valve 112d. The oxygen-containing gas supply path 112a is located outside the vacuum vessel 1. The oxygen-containing gas supply path 112a is connected to the reaction gas nozzle 32. The oxygen-containing gas supply path 112a is equipped with the oxygen-containing gas source 112b, the flow controller 112c, and the valve 112d in order from the upstream side to the downstream side in the direction of gas flow. As a result, the supply timing of the oxygen-containing gas from the oxygen-containing gas source 112b is controlled by the valve 112d, and the flow rate is adjusted to a predetermined rate by the flow controller 112c. The oxygen-containing gas flows from the oxygen-containing gas supply path 112a into the reaction gas nozzle 32 and is discharged from the reaction gas nozzle 32 into the vacuum vessel 1. The flow controller 112c may be, for example, a mass flow controller.

[0019] Oxygen-containing gases are gases that oxidize organic raw material gases. Examples of oxygen-containing gases include a mixture of hydrogen (H2) and oxygen (O2), O2 gas, water vapor (H2O gas), ozone (O3) gas, a mixture of H2 and O3, nitric oxide (NO) gas, nitrous oxide (N2O) gas, nitrogen dioxide (NO2) gas, carbon monoxide (CO) gas, and carbon dioxide (CO2) gas.

[0020] Multiple reaction gas nozzles 32 may be provided around the vacuum vessel 1 at intervals from each other. In this case, the oxygen-containing gas supply unit 112 is configured to introduce oxygen-containing gas to the multiple reaction gas nozzles 32. The region below the reaction gas nozzles 32 becomes an oxidation region P2 for oxidizing the organic raw material gas adsorbed on the substrate W in the adsorption region P1.

[0021] Oxygen-containing gas is introduced into the reaction gas nozzle 33 from the oxygen-containing gas supply unit 113. The oxygen-containing gas supply unit 113 comprises an oxygen-containing gas supply path 113a, an oxygen-containing gas source 113b, a flow controller 113c, and a valve 113d. The oxygen-containing gas supply path 113a is located outside the vacuum vessel 1. The oxygen-containing gas supply path 113a is connected to the reaction gas nozzle 33. In the oxygen-containing gas supply path 113a, the oxygen-containing gas source 113b, the flow controller 113c, and the valve 113d are provided in order from the upstream side to the downstream side in the direction of gas flow. As a result, the supply timing of the oxygen-containing gas from the oxygen-containing gas source 113b is controlled by the valve 113d, and the flow rate is adjusted to a predetermined rate by the flow controller 113c. The oxygen-containing gas flows from the oxygen-containing gas supply path 113a into the reaction gas nozzle 33 and is discharged from the reaction gas nozzle 33 into the vacuum vessel 1. The flow controller 113c may be, for example, a mass flow controller.

[0022] The oxygen-containing gas may be the same as the oxygen-containing gas introduced from, for example, the oxygen-containing gas source 112b. In this case, the oxygen-containing gas source 113b may be a gas source common to both the oxygen-containing gas source 112b and the oxygen-containing gas source 113b.

[0023] A plasma source (not shown) may be provided above the reaction gas nozzle 33. In this case, plasma can be generated from the oxygen-containing gas introduced into the vacuum vessel 1 from the reaction gas nozzle 33, thereby increasing the oxidizing effect on the surface of the substrate W.

[0024] Multiple reaction gas nozzles 33 may be provided around the vacuum vessel 1 at intervals from each other. In this case, the oxygen-containing gas supply unit 113 is configured to introduce oxygen-containing gas to the multiple reaction gas nozzles 33. The region below the reaction gas nozzles 33 becomes an oxidation region P3 for oxidizing the organic raw material gas adsorbed on the substrate W in the adsorption region P1.

[0025] Separation gas and dehydrating agent are introduced into the separation gas nozzle 41 from the separation gas supply unit 114. The separation gas supply unit 114 comprises a separation gas supply path 114a, a separation gas source 114b, a flow controller 114c, a valve 114d, a dehydrating agent supply path 114e, a dehydrating agent source 114f, a flow controller 114g, and a valve 114h. The separation gas supply path 114a is located outside the vacuum vessel 1. The separation gas supply path 114a is connected to the separation gas nozzle 41. In the separation gas supply path 114a, the separation gas source 114b, the flow controller 114c, and the valve 114d are provided in order from the upstream side to the downstream side in the direction of gas flow. As a result, the supply timing of the separation gas from the separation gas source 114b is controlled by the valve 114d, and the flow rate is adjusted to a predetermined level by the flow controller 114c. The separated gas flows from the separated gas supply path 114a into the separated gas nozzle 41 and is discharged from the separated gas nozzle 41 into the vacuum vessel 1. The flow controller 114c may be, for example, a mass flow controller.

[0026] The dehydrating agent supply path 114e is located outside the vacuum vessel 1. The dehydrating agent supply path 114e is connected to the separation gas supply path 114a downstream of the valve 114d. The dehydrating agent supply path 114e is equipped with a dehydrating agent source 114f, a flow rate controller 114g, and a valve 114h in order from upstream to downstream in the direction of gas flow. As a result, the supply timing of the dehydrating agent from the dehydrating agent source 114f is controlled by the valve 114h, and the flow rate is adjusted to a predetermined level by the flow rate controller 114g. The dehydrating agent flows from the dehydrating agent supply path 114e through the separation gas supply path 114a to the separation gas nozzle 41, and is discharged into the vacuum vessel 1 from the separation gas nozzle 41 together with the separation gas. The flow rate controller 114g may be, for example, a mass flow controller.

[0027] The separation gas may be, for example, an inert gas. The inert gas may be a noble gas such as helium (He), neon (Ne), or argon (Ar). The inert gas may also be nitrogen (N2).

[0028] The dehydrating agent is a gas used to remove moisture adsorbed on the surface of the substrate W. The dehydrating agent may be, for example, tetrahydrofuran (THF) gas or dimethylamine gas.

[0029] Multiple separation gas nozzles 41 may be provided around the vacuum vessel 1 at intervals from each other. In this case, the separation gas supply unit 114 is configured to introduce the separation gas and dehydrating agent to the multiple separation gas nozzles 41. The separation gas supply unit 114 may also be configured to introduce the separation gas and dehydrating agent to different separation gas nozzles 41. The area below the separation gas nozzles 41 becomes a separation region D1 for suppressing the mixing of the organic raw material gas and the oxygen-containing gas. The separation region D1 also functions as a dehydration region for removing H2O with the dehydrating agent.

[0030] Separation gas is introduced into the separation gas nozzle 42 from the separation gas supply unit 115. The separation gas supply unit 115 comprises a separation gas supply path 115a, a separation gas source 115b, a flow controller 115c, and a valve 115d. The separation gas supply path 115a is located outside the vacuum vessel 1. The separation gas supply path 115a is connected to the separation gas nozzle 42. The separation gas source 115b, the flow controller 115c, and the valve 115d are arranged in order from the upstream side to the downstream side in the direction of gas flow in the separation gas supply path 115a. As a result, the supply timing of the separation gas from the separation gas source 115b is controlled by the valve 115d, and the flow rate is adjusted to a predetermined rate by the flow controller 115c. The separation gas flows from the separation gas supply path 115a into the separation gas nozzle 42 and is discharged from the separation gas nozzle 42 into the vacuum vessel 1. The flow controller 115c may be, for example, a mass flow controller.

[0031] The separated gas may be the same as the separated gas introduced from, for example, the separated gas source 114b. In this case, the separated gas source 115b may be a gas source common to both the separated gas source 114b and the separated gas source 115b.

[0032] Multiple separation gas nozzles 42 may be provided around the vacuum vessel 1 at intervals from each other. In this case, the separation gas supply unit 115 is configured to introduce separation gas to multiple separation gas nozzles 42. The area below the separation gas nozzles 42 becomes a separation region D2 for suppressing the mixing of organic raw material gas and oxygen-containing gas.

[0033] Referring to Figures 2 and 3, two convex portions 4 are provided inside the vacuum vessel 1. The convex portions 4, together with the separation gas nozzles 41 and 42, constitute the separation regions D1 and D2, and are therefore attached to the underside of the top plate 11 so as to protrude toward the rotary table 2, as will be described later. The convex portions 4 have a fan-shaped planar form with their tops cut in an arc shape, with the inner arc connecting to the protruding portion 5 (described later) and the outer arc being positioned along the inner circumferential surface of the container body 12 of the vacuum vessel 1.

[0034] Figure 4 shows a cross-section of the vacuum vessel 1 along the concentric circles of the rotary table 2 from reaction gas nozzle 31 to reaction gas nozzle 32. As shown in Figure 4, a convex portion 4 is attached to the underside of the top plate 11. Therefore, inside the vacuum vessel 1, there is a flat, low ceiling surface (first ceiling surface 44) which is the underside of the convex portion 4, and two ceiling surfaces (second ceiling surface 45) that are higher than the first ceiling surface 44 and are located on both sides of the first ceiling surface 44 in the circumferential direction. The first ceiling surface 44 has a fan-shaped planar shape with its top cut in an arc shape. Also, as shown in the figure, a groove 43 is formed in the center of the convex portion 4 so as to extend radially, and the separation gas nozzle 42 is housed in the groove 43. Similarly, a groove 43 is formed in the other convex portion 4, and the separation gas nozzle 41 is housed in the groove 43. Reaction gas nozzles 31 and 32 are provided in the space below the second ceiling surface 45, respectively. The reaction gas nozzles 31 and 32 are positioned near the substrate W, spaced apart from the second ceiling surface 45. As shown in Figure 4, the reaction gas nozzle 31 is located in the space 48a below the second ceiling surface 45 on the right side of the convex portion 4, and the reaction gas nozzle 32 is located in the space 48b below the second ceiling surface 45 on the left side.

[0035] The first ceiling surface 44 forms a narrow separation space H relative to the rotating table 2. When separation gas is supplied from the discharge hole 42h of the separation gas nozzle 42, the separation gas flows through separation space H toward spaces 48a and 48b. Since the volume of separation space H is smaller than the volume of spaces 48a and 48b, the separation gas can raise the pressure in separation space H to a higher level than the pressure in spaces 48a and 48b. That is, a high-pressure separation space H is formed between spaces 48a and 48b. The separation gas flowing out of separation space H into spaces 48a and 48b acts as a counterflow to the organic raw material gas from the adsorption region P1 and the oxygen-containing gas from the oxidation region P2. Therefore, the organic raw material gas from the adsorption region P1 and the oxygen-containing gas from the oxidation region P2 are separated by separation space H. Thus, mixing and reaction between the organic raw material gas and the oxygen-containing gas within the vacuum container 1 can be suppressed.

[0036] The height h1 of the first ceiling surface 44 relative to the upper surface of the rotating table 2 is set to a height suitable for making the pressure in the separation space H higher than the pressure in spaces 48a and 48b, taking into consideration the pressure inside the vacuum chamber 1 during film deposition, the rotation speed of the rotating table 2, the flow rate of the separation gas, etc.

[0037] On the other hand, a projection 5 (Figures 2 and 3) is provided on the underside of the top plate 11, surrounding the outer circumference of the core portion 21 that fixes the rotating table 2. The projection 5 is continuous with the part of the convex portion 4 on the side of the rotation center, and its underside is formed at the same height as the first ceiling surface 44.

[0038] Figure 1, which was referred to earlier, is a cross-sectional view along the line I-I' in Figure 3, showing the region where the second ceiling surface 45 is provided. On the other hand, Figure 5 is a cross-sectional view showing the region where the first ceiling surface 44 is provided. As shown in Figure 5, a bent portion 46 is formed on the periphery of the fan-shaped convex portion 4 (the outer edge side of the vacuum vessel 1), bending in an L-shape so as to face the outer end surface of the rotary table 2. Similar to the convex portion 4, the bent portion 46 suppresses the intrusion of reaction gas from both sides of the separation regions D1 and D2, and suppresses the mixing of the organic raw material gas and the oxygen-containing gas. The fan-shaped convex portion 4 is provided on the top plate 11, and since the top plate 11 can be removed from the container body 12, there is a small gap between the outer surface of the bent portion 46 and the container body 12. The gap between the inner circumferential surface of the bent portion 46 and the outer end surface of the rotary table 2, and the gap between the outer circumferential surface of the bent portion 46 and the container body 12 are set to dimensions similar to, for example, the height of the first ceiling surface 44 relative to the upper surface of the rotary table 2.

[0039] In the separation regions D1 and D2, the inner circumferential wall of the container body 12 is formed as a vertical surface close to the outer circumferential surface of the bent portion 46 (Figure 5). On the other hand, in areas other than the separation regions D1 and D2, the inner circumferential wall of the container body 12 is recessed outward from, for example, the part facing the outer end surface of the rotary table 2 to the bottom portion 14 (Figure 1). For the sake of explanation, the recessed portion having a roughly rectangular cross-sectional shape will be referred to as the exhaust region E. Specifically, the exhaust region communicating with the adsorption region P1 will be designated as the first exhaust region E1, and the region communicating with the oxidation region P2 will be designated as the second exhaust region E2. At the bottom of the first exhaust region E1 and the second exhaust region E2, a first exhaust port 61 and a second exhaust port 62 are formed, respectively, as shown in Figures 1 to 3. The first exhaust port 61 and the second exhaust port 62 are connected to the vacuum pump 64 via an exhaust pipe 63, as shown in Figure 1. A pressure controller 65 is provided in the exhaust pipe 63.

[0040] As shown in Figures 1 and 5, a heater unit 7 is provided in the space between the rotary table 2 and the bottom 14 of the vacuum vessel 1, and the substrate W on the rotary table 2 is heated to the temperature determined by the process recipe via the rotary table 2. An annular cover member 71 is provided below the periphery of the rotary table 2 (Figure 5). The cover member 71 separates the atmosphere from the space above the rotary table 2 to the first exhaust region E1 and the second exhaust region E2 from the atmosphere where the heater unit 7 is located, thereby suppressing the intrusion of gas into the area below the rotary table 2. The cover member 71 comprises an inner member 71a provided so as to view the outer edge of the rotary table 2 and the outer circumference of the outer edge from below, and an outer member 71b provided between the inner member 71a and the inner circumferential surface of the vacuum vessel 1. The outer member 71b is provided below the bent portion 46 formed on the outer edge of the convex portion 4 in the separation regions D1 and D2, and close to the bent portion 46. The inner member 71a surrounds the heater unit 7 all around, below the outer edge of the rotary table 2 (and below the portion slightly outside the outer edge).

[0041] The bottom portion 14 on the side of the rotation center that is closer to the space where the heater unit 7 is located protrudes upward to form a projection 12a, approaching the core portion 21 near the center of the lower surface of the rotary table 2. There is a narrow space between the projection 12a and the core portion 21, and the gap between the inner circumferential surface of the through hole for the rotating shaft 22 that penetrates the bottom portion 14 and the rotating shaft 22 is also narrow. These narrow spaces are in communication with the case body 20. The case body 20 is provided with a purge gas supply pipe 72 for supplying purge gas into these narrow spaces for purging. The bottom portion 14 of the vacuum vessel 1 is provided with a plurality of purge gas supply pipes 73 at predetermined angular intervals in the circumferential direction below the heater unit 7 for purging the space where the heater unit 7 is located. Figure 5 shows one purge gas supply pipe 73. Between the heater unit 7 and the rotary table 2, a cover member 7a is provided to cover the area from the inner circumferential wall of the outer member 71b (the upper surface of the inner member 71a) to the upper end of the protrusion 12a in the circumferential direction, in order to suppress the intrusion of gas into the area where the heater unit 7 is installed. The cover member 7a is made of, for example, quartz.

[0042] A separation gas supply pipe 51 is connected to the center of the top plate 11 of the vacuum vessel 1. The separation gas supply pipe 51 supplies separation gas to the space 52 between the top plate 11 and the core 21. The separation gas supplied to space 52 is discharged towards the periphery along the surface on the side of the substrate mounting area of ​​the rotary table 2 through a narrow gap 50 between the protrusion 5 and the rotary table 2. The gap 50 can be maintained at a higher pressure than spaces 48a and 48b by the separation gas. Therefore, the gap 50 prevents the mixing of the organic raw material gas supplied to the adsorption region P1 and the oxygen-containing gas supplied to the oxidation region P2 through the central region C. In other words, the gap 50 (or central region C) functions similarly to the separation space H (or separation regions D1 and D2).

[0043] As shown in Figures 2 and 3, a transfer port 15 is formed in the side wall of the vacuum container 1 for transferring the substrate W between the external transfer arm 10 and the rotary table 2. The transfer port 15 is opened and closed by a gate valve (not shown). Below the rotary table 2, a transfer lifting pin and its lifting mechanism (neither shown) are provided at a location corresponding to the transfer position of the substrate W, passing through a recess 24 to lift the substrate W from the back side.

[0044] The film deposition apparatus is equipped with a control unit 100. As shown in Figure 1, the control unit 100 includes a computer for controlling the operation of the entire apparatus. The memory of the control unit 100 stores a program that causes the film deposition apparatus to perform the film deposition method described later under the control of the control unit 100. The program is structured into a group of steps to execute the film deposition method described later. The program is stored on a medium 102 such as a hard disk, compact disk, magneto-optical disk, memory card, or flexible disk, and is read into the storage unit 101 by a predetermined reading device and installed in the control unit 100.

[0045] Referring to Figure 6, another example of the configuration of the film deposition apparatus according to the embodiment will be described. Figure 6 is a plan view showing another example of the configuration of the film deposition apparatus according to the embodiment.

[0046] The film deposition apparatus shown in Figure 6 differs from the film deposition apparatuses shown in Figures 1 to 5 in that a dehydrating agent nozzle 34 is provided between the separation gas nozzle 41 and the reaction gas nozzle 31 in the circumferential direction of the vacuum chamber 1. The following explanation will focus on the differences from the film deposition apparatuses shown in Figures 1 to 5.

[0047] The dehydrating agent nozzle 34 has its base end, the gas introduction port 34a, fixed to the outer circumferential wall of the container body 12. The dehydrating agent nozzle 34 is introduced into the vacuum container 1 from the outer circumferential wall of the vacuum container 1 and is mounted so as to extend horizontally to the rotary table 2 along the radial direction of the container body 12.

[0048] Dehydrating agent is introduced into the dehydrating agent nozzle 34 from the dehydrating agent supply unit 116. The dehydrating agent supply unit 116 comprises a dehydrating agent supply path 116a, a dehydrating agent source 116b, a flow rate controller 116c, and a valve 116d. The dehydrating agent supply path 116a is located outside the vacuum container 1. The dehydrating agent supply path 116a is connected to the dehydrating agent nozzle 34. The dehydrating agent supply path 116a is provided with the dehydrating agent source 116b, the flow rate controller 116c, and the valve 116d in order from the upstream side to the downstream side in the direction of gas flow. As a result, the supply timing of the dehydrating agent from the dehydrating agent source 116b is controlled by the valve 116d, and the flow rate is adjusted to a predetermined flow rate by the flow rate controller 116c. The dehydrating agent flows from the dehydrating agent supply path 116a into the dehydrating agent nozzle 34 and is discharged from the dehydrating agent nozzle 34 into the vacuum container 1. The flow controller 116c may be, for example, a mass flow controller.

[0049] Multiple dehydrating agent nozzles 34 may be provided around the vacuum container 1 at intervals from each other. In this case, the dehydrating agent supply unit 116 is configured to introduce the dehydrating agent to the multiple dehydrating agent nozzles 34.

[0050] The film deposition apparatus shown in Figure 6 is configured such that the dehydrating agent is introduced into the dehydrating agent nozzle 34, but not into the separation gas nozzle 41. However, similar to the film deposition apparatus shown in Figures 1 to 5, the dehydrating agent may be introduced into both the dehydrating agent nozzle 34 and the separation gas nozzle 41. In this case, since the dehydrating agent can be supplied from both the dehydrating agent nozzle 34 and the separation gas nozzle 41, the effect of desorbing H2O adsorbed on the surface of the substrate W is enhanced.

[0051] [Film formation method] The film deposition method according to the embodiment will be described with reference to Figures 7 and 8. Figure 7 is a flowchart showing an example of the film deposition method according to the embodiment. Figure 8 is a schematic diagram showing an example of the film deposition method according to the embodiment. The film deposition method according to the embodiment includes steps S1 to S5 shown in Figure 7.

[0052] In step S1, a substrate W having recesses on its surface is prepared. The substrate W may be, for example, a semiconductor wafer. The recesses may be, for example, trenches or holes.

[0053] Step S2 is performed after step S1. In step S2, an organic raw material gas is supplied to the surface of the substrate W, and the organic raw material gas is adsorbed into the depressions. The organic raw material gas may be a gas containing, for example, a metal element, a carbon element, and a hydrogen element. The metal element may be, for example, Al, Ti, Sr, Zr, or Hf. The organic raw material gas may be, for example, tris(dimethylamino)cyclopentadienylzirconium gas. After step S2, a step of supplying an inert gas to the surface of the substrate W may be performed. In this case, the organic raw material gas that is not adsorbed into the depressions is easily exhausted.

[0054] Step S3 is performed after step S2. In step S3, an oxygen-containing gas is supplied to the surface of the substrate W to oxidize the organic raw material gas adsorbed in the recesses. As a result, a silicon oxide film is formed on the upper and inner surfaces of the recesses of the substrate W. The oxygen-containing gas is a gas that oxidizes the organic raw material gas. The oxygen-containing gas may be, for example, a mixture of H2 and O2, O2 gas, H2O gas, O3 gas, a mixture of H2 and O3, NO gas, N2O gas, NO2 gas, CO gas, or CO2 gas. In step S3, carbon dioxide (CO2), water (H2O), etc., are generated by the reaction between the organic raw material gas adsorbed in the recesses and the oxygen-containing gas. CO2 is easily exhausted and hardly remains on the upper and inner surfaces of the recesses. In contrast, H2O is not easily exhausted, so some of the H2O remains on the upper and inner surfaces of the recesses and is adsorbed. For example, as shown in Figure 8(a), H2O remains on the surface of the substrate W and is adsorbed.

[0055] Step S4 is performed after step S3. In step S4, a first gas containing a dehydrating agent is supplied to the surface of the substrate W. The dehydrating agent is a gas used to remove moisture adsorbed on the surface of the substrate W. The dehydrating agent may be, for example, THF gas or dimethylamine gas. In step S4, H2O adsorbed on the upper and inner surfaces of the recesses is removed by the dehydrating agent. For example, when THF gas is supplied to the surface of the substrate W as shown in Figure 8(a), the THF gas acts on the H2O adsorbed on the surface of the substrate W as shown in Figure 8(b), and the H2O adsorbed on the surface of the substrate W is removed and exhausted along with the THF gas as shown in Figure 8(c). As a result, a surface from which H2O has been removed is formed on the substrate W as shown in Figure 8(d). The first gas may also contain an inert gas. In this case, the H2O removed by the dehydrating agent is more easily exhausted from the upper and inner surfaces of the recesses. The flow rate of the inert gas may be greater than, for example, the flow rate of the dehydrating agent. In this case, the H2O removed by the dehydrating agent is more easily exhausted from the top and inner surfaces of the recesses.

[0056] Process S5 is performed after process S4. Process S5 determines whether processes S2 to S4 have been performed the set number of times. If the number of executions has not reached the set number, processes S2 to S4 are performed again. On the other hand, if the number of executions has reached the set number, the process is terminated. The set number of executions for process S5 may be, for example, one time or two or more times. Hereinafter, the cycle including processes S2 to S4 will be referred to as the ALD cycle.

[0057] Incidentally, organic raw material gases have the property of adsorbing more H2O on surfaces where H2O is adsorbed. Therefore, in step S2 of the second and subsequent ALD cycles, if the amount of H2O adsorbed differs between the upper and inner surfaces of the recesses, variations will occur in the amount of organic raw material gas adsorbed according to the amount of H2O adsorbed, resulting in poor step coverage. The reason why the amount of organic raw material gas adsorbed is greater on surfaces where H2O is adsorbed is thought to be as follows.

[0058] Figure 9 is a schematic diagram showing a conventional film deposition method. The conventional film deposition method does not have the aforementioned step S4. In the conventional film deposition method, steps S2 and S3 are repeated until a set number of times is reached. Below, the conventional film deposition method will be explained using the example of a case where the organic raw material gas is a Zr-based raw material gas containing Zr as a metal element, the oxygen-containing gas is O3 gas, and the inert gas is N2 gas.

[0059] First, a Zr-based raw material gas is supplied to the surface of the substrate W, and the Zr-based raw material gas is adsorbed onto the surface of the substrate W. Next, as shown in Figure 9(a), O3 gas is supplied to the surface of the substrate W on which the Zr-based raw material gas has been adsorbed. At this time, the Zr-based raw material gas adsorbed on the surface of the substrate W reacts with the O3 gas to generate H2O, CO2, NO, etc. Next, as shown in Figure 9(b), N2 gas is supplied to the surface of the substrate W. This causes the H2O, CO2, NO, etc. generated by the reaction between the Zr-based raw material gas and the O3 gas to be exhausted. At this time, since H2O is less easily exhausted than CO2 and NO, some of the H2O remains on the surface of the substrate W and is adsorbed. Next, as shown in Figure 9(c), a Zr-based raw material gas is supplied to the substrate W on which H2O remains. Organic raw material gases such as Zr-based raw material gas have the property of adsorbing onto surfaces that have OH groups. Therefore, when a Zr-based raw material gas is supplied to the surface on which H2O containing OH groups is adsorbed, the H2O on the surface of the substrate W reacts with the Zr-based raw material gas, causing the Zr-based raw material gas to be adsorbed and OH groups to be generated in the Zr-based raw material gas. The OH groups generated in the Zr-based raw material gas react with another Zr-based raw material gas, causing further adsorption of the Zr-based raw material gas on the surface. In this way, in one ALD cycle, the surface on which H2O is adsorbed is adsorbed with Zr-based raw material gas equivalent to two ALD cycles. For this reason, the film thickness is expected to be thicker on the surface where H2O is adsorbed than on the surface where H2O is not adsorbed. Next, as shown in Figure 9(d), N2 gas, an example of an inert gas, is supplied to the surface of the substrate W. This exhausts the by-products generated by the reaction on the surface of the substrate W.

[0060] In the film formation method according to this embodiment, after oxidizing the organic raw material gas, a dehydrating agent is supplied to the surface of the substrate W to remove H2O adsorbed on the upper and inner surfaces of the recesses. Therefore, variations in the amount of organic raw material gas adsorbed on the upper and inner surfaces of the recesses can be suppressed in the second and subsequent ALD cycles. As a result, good step-level coating can be obtained.

[0061] Furthermore, in the film formation method according to this embodiment, a first gas containing a dehydrating agent is used as the gas supplied when purging the oxygen-containing gas, instead of the conventional inert gas. This makes it possible to suppress variations in the amount of organic raw material gas adsorbed on the upper and inner surfaces of the recesses without extending the time of a single ALD cycle. As a result, good step coverage and high productivity can be achieved simultaneously.

[0062] In contrast, when only an inert gas is used as the gas supplied during purging of oxygen-containing gas, the H2O desorbed from the lower inner surface of the recess by the inert gas may be re-adsorbed onto the upper inner surface or top surface of the recess when it is exhausted from the recess. As a result, the amount of H2O adsorbed on the upper inner surface or top surface of the recess becomes greater than that adsorbed on the lower inner surface. Consequently, the amount of organic raw material gas adsorbed onto the upper inner surface or top surface of the recess becomes greater than the amount adsorbed onto the lower inner surface of the recess. As a result, good step coverage cannot be obtained. Since it takes a long time to desorb the H2O re-adsorbed onto the upper inner surface or top surface of the recess, productivity decreases.

[0063] Another method involves applying thermal energy to the substrate W to desorb H2O adsorbed on the upper and inner surfaces of the recesses. In this case, it is not easy to selectively apply thermal energy to the regions where H2O is adsorbed, and differences in film quality may occur between regions where thermal energy is applied and regions where it is not. Also, when thermal energy is applied, the temperature of the substrate W increases. Therefore, the substrate W must be cooled after the thermal energy is applied. This reduces productivity.

[0064] Next, we will describe the case in which a film deposition method according to the embodiment is carried out using the film deposition apparatus shown in Figures 1 to 5, and a silicon oxide film is deposited in the recesses formed on the surface of the substrate W.

[0065] First, the gate valve is opened, and the substrate W is transferred from the outside via the transfer opening 15 by the transfer arm 10 into the recess 24 of the rotary table 2. The transfer of the substrate W is performed by raising and lowering a lifting pin from the bottom side of the vacuum container 1 through a through hole in the bottom surface of the recess 24 when the recess 24 stops in a position facing the transfer opening 15. This transfer of substrate W is performed by intermittently rotating the rotary table 2, and a substrate W is placed in each of the five recesses 24 of the rotary table 2.

[0066] Next, the gate valve is closed, and the vacuum chamber 1 is evacuated by the vacuum pump 64 to the achievable vacuum level. Then, separation gas is discharged at a predetermined flow rate from separation gas nozzles 41 and 42, separation gas is discharged at a predetermined flow rate from separation gas supply pipe 51, and purge gas is discharged at a predetermined flow rate from purge gas supply pipe 72. Dehydrating agent may also be discharged at a predetermined flow rate along with the separation gas from separation gas nozzle 41. In addition, the pressure controller 65 controls the pressure inside the vacuum chamber 1 to a preset processing pressure. Next, the substrate W is heated by the heater unit 7 while the rotary table 2 is rotated clockwise. The rotation speed of the rotary table 2 may be, for example, 1 rpm to 5 rpm, and in one example it is 3 rpm. The temperature of the substrate W may be, for example, 200°C to 300°C, and in one example it is 275°C.

[0067] Next, organic raw material gas is supplied from reaction gas nozzle 31, and oxygen-containing gas is supplied from reaction gas nozzle 33. If only separation gas is supplied from separation gas nozzle 41, a dehydrating agent is supplied from separation gas nozzle 41 along with the separation gas.

[0068] As the rotary table 2 rotates, the substrate W repeatedly passes through the adsorption region P1, separation region D2, oxidation region P3, and separation region D1 in this order.

[0069] In the adsorption region P1, the organic raw material gas supplied from the reaction gas nozzle 31 is adsorbed onto the upper and inner surfaces of the recesses in the substrate W. In the separation region D2, the organic raw material gas that is not adsorbed onto the recesses in the substrate W is exhausted. In the oxidation region P3, the organic raw material gas adsorbed onto the upper and inner surfaces of the recesses in the substrate W is oxidized by the oxygen-containing gas supplied from the reaction gas nozzle 33. As a result, a silicon oxide film is formed on the upper and inner surfaces of the recesses in the substrate W. When the organic raw material gas is oxidized, H2O is produced as a by-product, and the produced H2O can be adsorbed onto the surface of the silicon oxide film. In the separation region D1, the H2O adsorbed onto the surface of the silicon oxide film is desorbed by the dehydrating agent supplied from the separation gas nozzle 41.

[0070] As the rotating table 2 rotates, the substrate W reaches the adsorption region P1 again, and the organic raw material gas supplied from the reaction gas nozzle 31 is adsorbed onto the upper and inner surfaces of the recesses in the substrate W. At this time, since the H2O adsorbed onto the upper and inner surfaces of the recesses in the substrate W is desorbed, the variation in the amount of organic raw material gas adsorbed onto the upper and inner surfaces of the recesses in the substrate W becomes smaller.

[0071] Subsequently, as the substrate W passes through the oxidation region P3, the oxygen-containing gas supplied from the reaction gas nozzle 33 oxidizes the organic raw material gas adsorbed on the upper and inner surfaces of the recesses in the substrate W, further forming a silicon oxide film. At this time, the thickness distribution of the silicon oxide film reflects the density of the organic raw material gas adsorbed on the upper and inner surfaces of the recesses in the substrate W. Therefore, good step coverage is obtained.

[0072] Next, when the substrate W reaches the separation region D1 again, the H2O adsorbed on the surface of the silicon oxide film is detached by the dehydrating agent supplied from the separation gas nozzle 41.

[0073] After this, the above process is repeated, and a silicon oxide film with good step-level coverage is formed on the upper and inner surfaces of the recesses.

[0074] In the above example, the case in which oxygen-containing gas is supplied from reaction gas nozzle 33 and not from reaction gas nozzle 32 was described, but the invention is not limited to this. For example, oxygen-containing gas may be supplied from both reaction gas nozzle 32 and reaction gas nozzle 33. In this case, the oxidizing effect on the surface of the substrate W is increased, so a silicon oxide film with a low impurity concentration can be formed. Alternatively, for example, oxygen-containing gas may be supplied from reaction gas nozzle 32 instead of reaction gas nozzle 33.

[0075] As described above, according to the film formation method of the embodiment, after oxidizing the organic raw material gas, a dehydrating agent is supplied to the surface of the substrate W to remove H2O adsorbed on the upper and inner surfaces of the recesses. Therefore, variations in the amount of organic raw material gas adsorbed on the upper and inner surfaces of the recesses can be suppressed in the second and subsequent ALD cycles. As a result, good step-level coating can be obtained.

[0076] Furthermore, according to the film formation method of this embodiment, a first gas containing a dehydrating agent is used as the gas supplied when purging with an oxygen-containing gas, instead of the conventional inert gas. This makes it possible to suppress variations in the amount of organic raw material gas adsorbed on the upper and inner surfaces of the recesses without extending the time of a single ALD cycle. As a result, good step coverage and high productivity can be achieved simultaneously.

[0077] Furthermore, according to the film deposition method of the embodiment, the rotary table 2 is rotated at a constant speed, and the substrate W is passed through the adsorption region P1, the oxidation region P3, and the separation region D1, thereby performing steps S2 to S4 on the substrate W. For this reason, it is not easy to make the time of one step, for example, step S4, longer than the time of the other steps S2 and S3. According to the film deposition method of the embodiment, H2O adsorbed on the upper and inner surfaces of the recesses can be desorbed without extending the time of step S4. For this reason, the film deposition method of the embodiment is particularly effective in the film deposition apparatus of the embodiment described above. However, the film deposition method of the embodiment can also be applied to single-wafer apparatuses that process substrates W one at a time, and batch apparatuses that process multiple substrates W at once.

[0078] [Examples] An example is described in which good step coverage was confirmed when a silicon oxide film was deposited in a recess formed on the surface of a substrate using a film deposition apparatus according to the embodiment. In the example, a silicon oxide film was deposited in the recess under the conditions 1 to 4 shown below, and the step coverage and overhang of the silicon oxide film were evaluated.

[0079] Figure 10 shows a method for evaluating the embedding characteristics of a silicon oxide film. Figure 10 illustrates the overhang and step coverage properties of the silicon oxide film F formed in a recess R.

[0080] Overhang is a value calculated as T1 / T2, where T1 is the thickness of the silicon oxide film F deposited on the upper surface of the recess R, and T2 is the thickness of the silicon oxide film F deposited on the upper inner surface of the recess R. The closer the overhang is to 100%, the smaller the difference between the thickness of the silicon oxide film F T1 deposited on the upper surface of the recess R and the thickness of the silicon oxide film F T2 deposited on the upper inner surface of the recess R, indicating a good overhang.

[0081] Step coverage is calculated as T3 / T2, where T2 is the thickness of the silicon oxide film F deposited on the upper inner surface of the recess R, and T3 is the thickness of the silicon oxide film F deposited on the lower inner surface of the recess R. The closer the step coverage is to 100%, the smaller the difference between the thickness T2 of the silicon oxide film F deposited on the upper inner surface of the recess R and the thickness T3 of the silicon oxide film F deposited on the lower inner surface of the recess R, indicating good step coverage.

[0082] (Condition 1) Under condition 1, a silicon oxide film was deposited in the recesses by supplying gas from each nozzle while rotating the rotary table 2 on which the substrate was placed. Specifically, a zirconium-containing gas, an example of an organic raw material gas, was supplied from reaction gas nozzle 31, ozone gas, an example of an oxygen-containing gas, was supplied from reaction gas nozzle 33, and nitrogen gas, an example of a separation gas, was supplied from separation gas nozzle 42. In addition, THF gas, an example of a dehydrating agent, was supplied from separation gas nozzle 41 at a flow rate of 1 slm, and nitrogen gas, an example of a separation gas, was supplied from separation gas nozzle 41 at a flow rate of 3 slm. Furthermore, the cross-section of the substrate was observed using a transmission electron microscope (TEM), and the overhang and step coverage of the silicon oxide film were calculated based on the cross-sectional image.

[0083] (Condition 2) In Condition 2, the flow rate of nitrogen gas supplied from the separation gas nozzle 41 was changed from 3 slm to 5 slm compared to Condition 1, and a silicon oxide film was deposited in the recessed area. All other conditions were the same as in Condition 1. Also, as in Condition 1, the cross-section of the substrate was observed using a TEM, and the overhang and step coverage of the silicon oxide film were calculated based on the cross-sectional image.

[0084] (Condition 3) In Condition 3, the flow rate of nitrogen gas supplied from the separation gas nozzle 41 was changed from 3 slm to 10 slm compared to Condition 1, and a silicon oxide film was deposited in the recessed area. All other conditions were the same as in Condition 1. Also, as in Condition 1, the cross-section of the substrate was observed using a TEM, and the overhang and step coverage of the silicon oxide film were calculated based on the cross-sectional image.

[0085] (Condition 4) In Condition 4, unlike Condition 1, only nitrogen gas was supplied from the separation gas nozzle 41 without supplying THF gas, and a silicon oxide film was deposited in the recessed area. All other conditions were the same as in Condition 1. Also, as in Condition 1, the cross-section of the substrate was observed using a TEM, and the overhang and step coverage of the silicon oxide film were calculated based on the cross-sectional image.

[0086] Figure 11 shows the evaluation results of the embedding characteristics of the silicon oxide film. Figure 11 shows the calculation results of the overhang and step coverage of the silicon oxide film deposited in the recesses under conditions 1 to 4.

[0087] As shown in Figure 11, conditions 1 to 3 show overhang and step coverage values ​​closer to 100% compared to condition 4. This result indicates that good overhang and good step coverage can be obtained by supplying THF gas and nitrogen gas from the separation gas nozzle 41.

[0088] Furthermore, as shown in Figure 11, under condition 3, the overhang and step coverage values ​​are closer to 100% than under conditions 1 and 2. This result indicates that increasing the flow rate of nitrogen gas supplied from the separation gas nozzle 41 further improves the overhang and step coverage.

[0089] The embodiments disclosed herein should be considered in all respects to be illustrative and not restrictive. The above embodiments may be omitted, replaced, or modified in various ways without departing from the scope and spirit of the appended claims. [Explanation of Symbols]

[0090] 1 Vacuum container 2 Rotating Tables 100 Control Unit P1 Adsorption area P2 oxidation region P3 oxidation region D1 Dehydration area W board

Claims

1. (a) A step of preparing a substrate having a recess on its surface, (b) A step of supplying an organic raw material gas to the surface and adsorbing the organic raw material gas in the recess, (c) A step of supplying an oxygen-containing gas to the surface and oxidizing the organic raw material gas adsorbed in the recess, (d) After step (c), a step of supplying a first gas containing a dehydrating agent to the surface, It has, The first gas contains an inert gas, and the flow rate of the inert gas is greater than the flow rate of the dehydrating agent. Film formation method.

2. The above steps (b), (c), and (d) are repeated multiple times in this order. The method for forming a film according to claim 1.

3. Step (c) is to apply H to the surface. ２ This includes the adsorption of O, Step (d) is to remove H adsorbed on the surface ２ Including the removal of O, The method for forming a film according to claim 1.

4. (e) The process includes a step of supplying an inert gas to the surface between step (c) and step (d), The method for forming a film according to claim 1.

5. The dehydrating agent is THF gas. The method for forming a film according to claim 1.

6. The substrate is arranged circumferentially on a rotating table provided inside a vacuum chamber. The vacuum container is provided above the rotating table, along the direction of rotation of the rotating table, with an adsorption region for carrying out step (b), an oxidation region for carrying out step (c), and a dehydration region for carrying out step (d). Steps (b), (c), and (d) are carried out by the rotation of the rotary table while the organic raw material gas is supplied to the adsorption region, the oxygen-containing gas is supplied to the oxidation region, and the first gas is supplied to the dehydration region. The method for forming a film according to claim 1.

7. Vacuum container and A gas supply unit that supplies gas into the vacuum container, Control unit and Equipped with, The control unit, (a) A step of preparing a substrate having a recess on its surface, (b) A step of supplying an organic raw material gas to the surface and adsorbing the organic raw material gas in the recess, (c) A step of supplying an oxygen-containing gas to the surface and oxidizing the organic raw material gas adsorbed in the recess, (d) After step (c), a step of supplying a first gas containing a dehydrating agent to the surface, The gas supply unit is configured to control the gas supply unit to perform the following actions: The first gas contains an inert gas, and the flow rate of the inert gas is greater than the flow rate of the dehydrating agent. Film deposition equipment.

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