JP2024063360A - Method for manufacturing member having gas flow passage, and member having gas flow passage - Google Patents

Abstract

[Problem] To provide a method for manufacturing a member having a gas flow passage, which can be easily manufactured while maintaining high corrosion resistance of the surface of the gas flow passage, and a member having a gas flow passage. [Solution] The method for manufacturing a member having a gas flow passage includes a step of preparing a metal material having a gas flow passage formed therein, and a step of forming a corrosion-resistant film on the inner surface of the gas flow passage by ALD. [Selected Figure] Figure 5

Description

This disclosure relates to a method for manufacturing a component having a gas flow path, and a component having a gas flow path.

For example, in a film forming apparatus that performs a film forming process on a substrate by ALD (Atomic Layer Deposition), a member having a gas flow path is used to introduce gas into the processing chamber (for example, Patent Document 1).

JP 2020-158798 A

The present disclosure provides a method for manufacturing a component having a gas flow passage, which can be easily manufactured while maintaining high corrosion resistance of the surface of the gas flow passage, and a component having a gas flow passage.

A method for manufacturing a component having a gas flow path according to one embodiment of the present disclosure includes the steps of preparing a metal material having a gas flow path formed therein, and forming a corrosion-resistant film on the inner surface of the gas flow path by ALD.

The present disclosure provides a method for manufacturing a component having a gas flow passage, which can be easily manufactured while maintaining high corrosion resistance of the surface of the gas flow passage, and a component having a gas flow passage.

1 is a schematic diagram showing an example of a configuration of an ALD film formation apparatus having an inlet block and a fitting block as a gas introduction member that is a member having a gas flow path. FIG. 2 is a perspective view showing an inlet block and a fitting block as a gas introduction member that is a member having a gas flow path according to the embodiment. FIG. FIG. 4 is a cross-sectional view showing an inlet block and a fitting block. 1A to 1C are cross-sectional process diagrams illustrating an example of a method for manufacturing a gas introduction member that is a member having a gas flow path. FIG. 1 is a cross-sectional view showing an example of an apparatus for forming an aluminum oxide film on the inner surface of a gas flow passage formed inside a material by ALD. FIG. 11 is a cross-sectional view showing another example of an apparatus for forming an aluminum oxide film on the inner surface of a gas flow passage formed inside a material by ALD. 1 is a cross-sectional view illustrating a method of performing anodizing on an aluminum material having a gas flow path.

The following describes the embodiment with reference to the attached drawings.

<Background>
First, the background will be explained.
In a film forming apparatus for ALD film forming or the like, in order to introduce gas into a processing vessel, a member having a gas flow passage is used, as described in Patent Document 1. When a general aluminum material such as aluminum or an aluminum alloy is used as the member having such a gas flow passage, anodizing (alumite treatment) is often used as a countermeasure against corrosion of the surface of the gas flow passage caused by the gas flowing through the gas flow passage.

Anodizing is an immersion process in which a member is immersed in an electrolyte and electricity is passed through it. In order to anodize the entire gas flow path of a member having a gas flow path, an opening has been provided in the gas flow path, and the anodizing process has been performed. After the process, the opening has been closed with a plug or a lid. For example, as shown in FIG. 8(a), an opening 502 is first provided in a gas flow path 501 of an aluminum material 500. Next, as shown in FIG. 8(b), an anodized film 503 is formed by anodizing, and a lid 504 with an anodized film 504a formed on the inside is welded. The opening 502 can be closed by these processes.

When sealing openings in this way by welding plugs or lids, it takes time and money, and this increases especially when the flow path is long or complex. In addition, the plugs and lids are also anodized, but when they are attached, friction with the main body of the component or heat from the welding can damage the coating, exposing the aluminum parts, resulting in insufficient corrosion resistance.

Therefore, in one embodiment, a material made of an aluminum material having a gas flow path therein is prepared, and an aluminum oxide (alumina) film is formed by ALD on the entire inner surface of the gas flow path. This results in a member having a gas flow path, which has a main body made of an aluminum material, a gas flow path formed inside the main body, and an aluminum oxide film, which is an ALD film formed as a corrosion-resistant film on the entire inner surface of the gas flow path.

Because ALD is a gas-based process, the process gas is sufficiently supplied to the gas flow path without the need for openings. This eliminates the need for openings that were necessary during anodizing, and the effort required to seal openings by welding plugs or lids is almost eliminated, allowing a corrosion-resistant film to be formed over the entire surface of the gas flow path. Even if tiny plugs or lids are required, ALD can be performed after the plugs or lids are attached, and the aluminum oxide film formed as an ALD film will not peel off when the plugs or lids are attached. Moreover, gas also circulates in the tiny gaps between the plugs or lids and the main body, forming an ALD film.

This makes it possible to easily manufacture a component having a gas flow path in which the gas flow path surface is corrosion resistant while maintaining high corrosion resistance over the entire surface of the gas flow path.

<Specific embodiment>
[ALD Film Forming Apparatus Using a Member Having a Gas Flow Channel]
A typical example of a member having a gas flow path according to the embodiment is a gas introduction member that introduces a gas into a processing vessel containing a substrate in a film formation apparatus that performs film formation using a gas, such as ALD film formation. Examples of the gas introduction member include an inlet block and a fitting block.

Figure 1 shows a schematic diagram of an example of an ALD film formation device having an inlet block and a fitting block as gas introduction members, which are members having gas flow paths.

The film forming apparatus 1 has a processing vessel 10 that is configured to be depressurized and that contains a substrate W. A loading/unloading port (not shown) is provided on the side wall of the processing vessel 10 for loading and unloading the substrate W. An exhaust duct 51 is provided at the top of the processing vessel 10 so as to go around the wall. The top of the processing vessel 10 has an opening, and a lid 13 is attached via a sealing member so as to close the opening. A cap member 3 is attached to the bottom of the lid 13.

Below the cap member 3 in the processing vessel 10, a mounting table 2 on which a substrate W is placed is provided. Inside the mounting table 2, a heater (not shown) is provided for heating the substrate W. A support member 23 extending downward is connected to the center of the lower surface of the mounting table 2 through an opening 15 formed in the bottom wall of the processing vessel 10. The mounting table 2 is raised and lowered by a lifting mechanism 24 via the support member 23 between a processing position shown in FIG. 1 for processing a substrate and a transport position below that for transporting the substrate. A flange 25 is provided on the support member 23 at a position outside the processing vessel 10, and a bellows 26 is provided between the flange 25 and the bottom wall of the processing vessel 10 to surround the opening 15.

When the mounting table 2 is in the processing position, a processing space S is formed between the cap member 3 and the mounting table 2. An inverted cone-shaped recess 31 that forms the processing space S is formed on the underside of the cap member 3. A gas inlet passage 35 is formed in the center of the lid 13 and the cap member 3, penetrating them, to introduce gas into the processing space S.

The annular exhaust duct 51 has a gas passage 55 formed therein, and slits 56 connected to the gas passage 55 are formed around the entire circumference of the inner surface of the exhaust duct 51. An exhaust port 57 is provided on the outer wall of the exhaust duct 51, and one end of an exhaust pipe 52 is connected to the exhaust port 57. The other end of the exhaust pipe 52 is connected to an exhaust device 53, which is, for example, a vacuum pump. In addition, the exhaust pipe 52 is provided with an APC valve 54 for adjusting the pressure in the processing space S.

A gas introduction mechanism 4 is provided on the lid 13 to introduce gas into the processing space S in the processing vessel 10 via the gas introduction path 35. The gas introduction mechanism 4 has an inlet lock 41 and a fitting block 42 as gas introduction members, which are members having a gas flow path according to the embodiment. Raw material gases, reaction gases, purge gases, etc. for ALD film formation are supplied to the gas introduction mechanism 4 from multiple gas supply sources (not shown) of the gas supply unit 60 via piping 61.

In the film formation apparatus 1 configured as described above, the substrate W is carried into the processing vessel 10 and placed on the mounting table 2 at the transfer position, and then the mounting table 2 is raised to the processing position to form the processing space S. The processing space S is then evacuated by the exhaust device 53 to adjust the processing space S to the desired vacuum level, and the substrate W is heated to the desired temperature by the heater. In this state, the source gas, reaction gas, and purge gas are sequentially supplied from the gas supply unit 60 via the gas introduction mechanism 4 and the gas introduction path 35 to the processing space S, and an ALD film is formed on the substrate W by ALD.

[Gas introduction member]
Next, the gas introduction member, which is a member having a gas flow passage according to the embodiment, will be described in detail.
FIG. 2 is a perspective view showing an inlet block 41 and a fitting block 42 as gas introduction members, which are members having a gas flow path according to the embodiment. FIG. 3 is a plan view showing the inlet block 41. FIG. 4 is a cross-sectional view showing the inlet block 41 and the fitting block 42.

The inlet block 41 has a main body 411 made of an aluminum material such as aluminum or an aluminum alloy, and three gas flow paths 414a, 414b, and 414c formed inside the main body 411. As shown in FIG. 4, the inlet block 41 further has an aluminum oxide film 415, which is an ALD film, as a corrosion-resistant film on the entire inner surface of the gas flow paths 414a, 414b, and 414c of the main body 411. The tip of the main body 411 is a first connection part 412 connected to the gas introduction path 35, and the base end of the main body 411 is a second connection part 413 connected to the fitting block 42. The first connection part 412 is cylindrical, and a space 412a is formed in the lower part. The gas flow paths 414a, 414b, and 414c are formed so that one end faces the space 412a.

The fitting block 42 has a main body 421 made of aluminum or an aluminum alloy, and three gas flow paths 424a, 424b, and 424c formed inside the main body 421. As shown in FIG. 4, the fitting block 42 further has an aluminum oxide film 425, which is an ALD film, as a corrosion-resistant film on the entire inner surface of the gas flow paths 424a, 424b, and 424c of the main body 421. The part of the main body 421 directly below the inlet block 41 is a first connection part 422 connected to the second connection part 413 of the fitting block 41, and the part of the main body 421 protruding from the inlet block 41 is a second connection part 423 to which the pipe 61 of the gas supply part 60 is connected. The second connection part 423 has three gas introduction ports 423a, 423b, and 423c, to which the pipes 61 are respectively connected.

The second connection part 413 of the inlet block 41 and the first connection part 422 of the fitting block 42 are connected so that the gas flow paths 414a, 414b, and 414c are connected to the gas flow paths 424a, 424b, and 424c, respectively.

In this embodiment, the inlet block 41 and the fitting block 42 have three gas flow paths connected to three pipes 61, but the number of gas flow paths is not limited.

[Method of manufacturing gas introduction member]
Next, an example of a method for manufacturing a gas introduction member, which is a member having a gas flow passage, will be described. Here, an example will be shown in which an inlet block is used as the gas introduction member.

Figure 5 is a cross-sectional view illustrating an example of a manufacturing method for a gas introduction member, which is a member having a gas flow path.

First, a material 41' is prepared, which is made of an aluminum material such as aluminum or an aluminum alloy and has a gas flow path 414 formed therein (Figure 5(a)).

The gas flow passage 414 is formed, for example, by a drill. When the gas flow passage 414 is formed by a drill, the hole is drilled from the end of the material 41', so holes are also formed in parts other than the gas flow passage 414, but these parts can be blocked with plugs.

Next, an aluminum oxide film 415 is formed as a corrosion-resistant film on the entire inner surface of the gas flow path 414 by ALD (Figure 5 (b)).

The aluminum oxide film 415 may be formed by ALD using appropriate source gas, reactive gas, and purge gas in a conventional manner. For example, the material 41' is heated to about 180 to 200° C., and trimethylaluminum (TMA) as a source gas and O ₃ gas as a reactive gas are sequentially supplied with a purge of the residual gas between them, to form the aluminum oxide film 415 as an ALD film. That is, the material 41' heated to an appropriate temperature of about 180 to 200° C. is repeatedly supplied with TMA gas, purged with the residual gas, supplied with O ₃ gas, and purged with the residual gas, to form the aluminum oxide film 415 as an ALD film. In addition to O ₃ gas, H ₂ O gas, O ₂ gas, etc. may be used as the reactive gas. In addition, an inert gas such as Ar gas may be used as the purge gas when purging the residual gas. The purge gas may also be supplied when the source gas and reactive gas are supplied.

Such formation of an aluminum oxide film on the inner surface of the gas flow path 414 by ALD can be performed using the following device.

Figure 6 is a cross-sectional view showing an example of an apparatus for actually forming an aluminum oxide film on the inner surface of a gas flow path formed inside a material by ALD. The apparatus 200 of this example has a gas supply unit 120 provided at the inlet side of the gas flow path 414 of a material 41' having a gas flow path 414 formed therein, an exhaust unit 130 provided at the outlet side of the gas flow path 414, and a heating mechanism 140 for heating the material 41'.

The inlet of the gas flow path 414 is sealed by a gas introduction jig 111 having a gas introduction path therein, and gas is supplied from the gas supply unit 120 to the gas flow path 414 via the gas introduction jig 111.

The gas supply unit 120 includes a TMA gas supply source 121, an _O3 gas supply source 122, an Ar gas supply source 123, and gas pipes 124, 125, and 126, one end of which is connected to each of these sources. The other ends of the gas pipes 124, 125, and 126 are connected to a gas introduction jig 111, and the TMA gas, _O3 gas, and Ar gas as a purge gas are introduced into a gas flow path 414 through these pipes 124, 125, and 126 and the gas introduction jig 111. The gas pipes 124, 125, and 126 are provided with opening and closing valves 127, 128, and 129, respectively. Although not shown, these gas pipes are provided with flow rate controllers such as mass flow controllers.

The outlet of the gas flow path 414 is sealed by a gas exhaust jig 112 having a gas exhaust path inside, and the gas flow path 414 is configured to be exhausted by an exhaust unit 130 through the gas exhaust jig 112.

The exhaust section 130 has an exhaust pipe 131, one end of which is connected to the gas exhaust path of the gas exhaust jig 112, and an exhaust device 132 connected to the exhaust pipe 131. The exhaust device 132 has a vacuum pump and a pressure control valve.

In the apparatus 200 thus configured, the material 41' having the gas flow passage 414 formed therein is heated to 180 to 200° C. by the heating mechanism 140. In this state, first, Ar gas is supplied from the gas supply unit 120 to the gas flow passage 414, while the exhaust unit 130 exhausts the gas flow passage 414 to a predetermined reduced pressure state. Then, while controlling the pressure in the gas flow passage 414 by the exhaust unit 130, the gas supply unit 120 and the exhaust unit 130 perform ALD, which repeats the supply of TMA gas, purging with Ar gas, supply of _O3 gas, and purging with Ar gas to the gas flow passage 414. As a result, an aluminum oxide film, which is an ALD film, is formed to a desired thickness on the entire inner surface of the gas flow passage 414.

Figure 7 is a cross-sectional view showing another example of an apparatus for actually forming an aluminum oxide film on the inner surface of a gas flow path formed inside a material by ALD. The apparatus 300 of this example has a processing vessel 210 that contains a material 41' with a gas flow path 414 formed therein, a gas supply unit 220 that supplies gas to the processing vessel 210, an exhaust unit 230 that exhausts the inside of the processing vessel 210, and a heating mechanism 240 that heats the material 41'.

The gas supply unit 220 includes a TMA gas supply source 221, an _O3 gas supply source 222, an Ar gas supply source 223, and gas pipes 224, 225, and 226, one end of which is connected to each of the gas supply sources 221, 225, and 226. The other end of the gas pipes 224, 225, and 226 is connected to a gas introduction nozzle 250, and the TMA gas, _O3 gas, and Ar gas as a purge gas are introduced into the processing vessel 210 through the pipes 224, 225, and 226 and the gas introduction nozzle 250. The gas pipes 224, 225, and 226 are provided with opening and closing valves 227, 228, and 229, respectively. Although not shown, the gas pipes are provided with flow rate controllers such as mass flow controllers.

The exhaust section 230 has an exhaust pipe 231, one end of which is connected to the exhaust port 211 of the processing vessel 210, and an exhaust device 232 connected to the exhaust pipe 231. The exhaust device 232 has a vacuum pump and a pressure control valve.

In the apparatus 300 thus configured, the material 41' having the gas flow passage 414 formed therein is carried into the processing vessel 210 through a carry-in port (not shown) of the processing vessel 210. Next, the heating mechanism 240 heats the material 41' having the gas flow passage 414 formed therein to 180 to 200. In this state, first, Ar gas is supplied from the gas supply unit 220 through the gas introduction nozzle 250 into the processing vessel 210, while the exhaust unit 230 exhausts the processing vessel 210 to a predetermined reduced pressure state. Then, while controlling the pressure inside the processing vessel 210 by the exhaust unit 230, the gas supply unit 220 and the exhaust unit 230 perform ALD, which repeats the supply of TMA gas, purging with Ar gas, supply of _O3 gas, and purging with Ar gas to the processing vessel 210. As a result, an aluminum oxide film, which is an ALD film, is formed on the inner surface of the gas flow passage 414 to a desired thickness.

In addition, the formation of an aluminum oxide film on the inner surface of the gas flow passage 414 by ALD can also be performed using a film formation apparatus in which a material 41' having a gas flow passage formed therein is mounted instead of the inlet block 41 in the film formation apparatus 1 shown in FIG. 1. Specifically, a material 41' having a gas flow passage formed therein is mounted instead of the inlet block 41 of the film formation apparatus 1, the gas supply unit 60 is made capable of supplying TMA gas and _O3 gas, and a heating mechanism for heating the material 41' is provided. In such a film formation apparatus, prior to ALD on the substrate W, an aluminum oxide film is formed on the inner surface of the gas flow passage 414 of the material 41' by ALD of TMA gas and _O3 gas while heating the material 41' by the heating mechanism, thereby forming the inlet block 41. Then, ALD film formation on the substrate W is repeatedly performed thereafter.

With such an apparatus configuration, when the aluminum oxide film on the inner surface of the gas flow passage inside the inlet block 41 becomes worn due to repeated ALD on the substrate W, the aluminum oxide film can be repaired by ALD of TMA gas and _O3 gas.

As described above, according to this embodiment, a material 41' made of an aluminum material having a gas flow path inside is prepared, and an aluminum oxide film 415 is formed by ALD on the entire inner surface of the gas flow path to form a gas introduction member (inlet block 41, fitting block 42). Since ALD is a gas-based process, the process gas can be sufficiently distributed throughout the entire gas flow path without the need for openings, which were necessary during anodization. Therefore, a corrosion-resistant film can be formed on the entire surface of the gas flow path, with almost no effort required to close the openings by welding plugs or lids. In addition, even if the excess part is blocked with a plug after drilling to form a gas flow path, ALD can be performed after the plug is attached, and the aluminum oxide film formed as an ALD film will not peel off. Moreover, gas can be introduced into the minute gaps between the plug or lid and the main body, forming an ALD film.

This makes it possible to easily manufacture a gas introduction member whose gas flow path surface is corrosion-resistant while maintaining high corrosion resistance by forming an aluminum oxide film over the entire surface of the gas flow path.

<Other applications>
Although the embodiments have been described above, the embodiments disclosed herein should be considered to be illustrative and not restrictive in all respects. The above-described embodiments may be omitted, substituted, or modified in various forms without departing from the scope and spirit of the appended claims.

For example, in the above embodiment, the main body is made of an aluminum material such as aluminum or an aluminum alloy, and an aluminum oxide film is used as the corrosion-resistant film formed on the inner surface of the gas flow path by ALD. However, the present invention is not limited to this. In addition to aluminum, stainless steel and nickel alloys can also be used as the main body. In addition to aluminum oxide, the corrosion-resistant film formed by ALD can also be aluminum nitride, silicon oxide, silicon nitride, zirconia, yttrium oxide (yttria), niobium oxide, zinc oxide, titanium oxide, titanium nitride, etc. The metal constituting the material and the metal contained in the corrosion-resistant film may be different. In this way, the high degree of freedom in the combination of the metal material and the corrosion-resistant film is also a major advantage compared to the case of forming an anodized film on the inner surface of the gas flow path of a material made of an aluminum material.

In the above embodiment, an example was shown in which an inlet block or fitting block, which is a gas introduction member of an ALD film formation device, was used as a member having a gas flow path, but the gas introduction part of a film formation device that uses gas, not limited to ALD, can be used. Also, the gas introduction part can be applied to any member that requires corrosion resistance on the inner surface of the gas flow path, not limited to gas introduction parts.

1: Film forming apparatus 4: Gas introduction mechanism 41: Inlet block (gas introduction member)
41': Material 42: Fitting block (gas introduction member)
411, 421: Main body 414, 414a, 414b, 414c, 424a, 424b, 424c: Gas flow passage 415, 425: Aluminum oxide film (corrosion-resistant film, ALD film)

Claims (9)

Providing a metal material having a gas flow passage formed therein;
forming a corrosion-resistant film on an inner surface of the gas flow passage by ALD;
The method for producing a member having a gas flow passage comprising the steps of: The method for manufacturing a member having a gas flow path according to claim 1, wherein the metal material is aluminum or an aluminum alloy, and the corrosion-resistant film is an aluminum oxide film. The method for manufacturing a member having a gas flow path according to claim 2, wherein the aluminum oxide film is formed by ALD at 180 to 200°C using trimethylaluminum gas as a raw material gas and any one of _O3 gas, _H2O gas, and _O2 gas as a reactive gas. The method for manufacturing a member having a gas flow path according to claim 1, wherein the member having the gas flow path is a gas introduction member used for introducing gas into a film forming apparatus. The method for manufacturing a member having a gas flow passage according to claim 4, wherein a gas is supplied to the gas flow passage of the metal material while the metal material is mounted in the film forming device, and a corrosion-resistant film is formed on the inner surface of the gas flow passage by the ALD. The method for manufacturing a member having a gas flow path according to any one of claims 1 to 4, comprising providing a gas inlet at one end of the gas flow path formed inside the metal material, providing an exhaust at the other end, and supplying gas from the gas inlet to the gas flow path while exhausting the gas flow path with the exhaust, thereby forming a corrosion-resistant film on the inner surface of the gas flow path by the ALD. The method for manufacturing a member having a gas flow path according to any one of claims 1 to 4, comprising the steps of: placing a metal material having a gas flow path formed therein in a processing vessel; and supplying gas into the processing vessel while exhausting the inside of the processing vessel, thereby forming a corrosion-resistant film on the inner surface of the gas flow path by the ALD. A main body made of metal;
A gas flow path formed in the main body portion;
an ALD film formed as a corrosion-resistant film on the inner surface of the gas flow passage;
A member having a gas flow path. The member having a gas flow path according to claim 8, wherein the main body is aluminum or an aluminum alloy, and the ALD film is an aluminum oxide film.

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