JPH1112763A - Surface-treated aluminum component of vacuum equipment and its production - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide the surface-treated aluminum components of a vacuum equipment with the corrosion resistance to plasma, etc., of the outer face improved, the gas discharge in an vacuum environment reduced and the corrosion resistance of the wall face of an internally provided cooling water conduit improved. SOLUTION: The component 20 (heater cover), component 22 (substrate cover) and component 23 (gas dispersing plate) to be provided to a vacuum equipment are formed with aluminum or aluminum alloy material, and a cooling water conduit is furnished in each of the components 20, 22 and 23. A nonporous anodic oxide film having 0.3-0.9 μm thickness and contg. <=10 wt.% water is formed at least on the outer face of the above components, and a boehmite film having 0.2-0.3 μm thickness is formed on the wall face of the conduit.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

The present invention relates to a chemical vapor deposition (C) process.
Surface-treated aluminum components such as a gas dispersion plate, a susceptor, and a heater cover provided in vacuum equipment such as a VD device, an ion plating device, a dry etching device, a plasma CVD device, and a physical vapor deposition (PVD) device, and a method of manufacturing the same. In this connection, the corrosion resistance of the outer surface against plasma and the like is improved, the amount of gas released in a vacuum environment is reduced, and the corrosion resistance of the wall of a cooling water channel provided inside is improved.

[0002]

2. Description of the Related Art Conventionally, semiconductor products have been deposited on a substrate by a method such as vacuum deposition, sputtering, or chemical vapor deposition in a processing vessel capable of evacuating vacuum equipment, such as Si ₃ N ₄ , W, and A.
It is produced by forming a thin film such as l. By the way, a gas dispersion plate provided in such a vacuum device,
Stainless steel is used for the components such as the susceptor and the heater cover.
Since the performance of thin films such as semiconductors may be reduced due to heavy weight or heavy metals such as chromium and nickel mixed into the system, the use of aluminum or aluminum alloy materials has been attempted. I have. However, when a film is formed or etched using the above-described vacuum equipment, the film is usually processed in a high temperature atmosphere of about 150 to 400 ° C., and aluminum or aluminum alloy used under such a high temperature is usually used. A component made of a material has a problem that it is strongly corroded by chlorine gas or fluorine plasma used for etching. This is because the decomposition of a reactive gas such as chlorine gas used for etching is promoted, and the reactivity between the reactive gas and aluminum or an aluminum alloy is promoted by heat. In addition, when a thin film is formed, the thin film may adhere to components other than the substrate in the processing container. In this case, the thin film attached to an unnecessary portion is removed with a halogen-containing etching gas. Therefore, there is a problem that the components are corroded by the etching gas.

[0003] Therefore, in order to suppress the above-mentioned problem caused by heat, a water channel is machined and provided inside a component made of aluminum or an aluminum alloy material.
Cooling is performed by passing water through the water channel. As a countermeasure against corrosion of the surface of the component, a method of forming a porous anodic oxide film by performing a sulfuric acid alumite treatment with a sulfuric acid electrolytic solution has been considered. However, since the porous anodic oxide film contains a large amount of moisture and sulfuric acid in the film, the film becomes a release gas and is released in a large amount into the processing vessel to cause contamination of the thin film, The purpose of achieving a high vacuum inside cannot be achieved sufficiently, and when used in a high-temperature atmosphere, the film is easily cracked by heat, and may be peeled off and adhere to the substrate. The quality of the resulting product deteriorated and was not practical. In addition, since the current cannot flow around a part provided inside, such as a water channel, because the current flows well, the porous anodized film is not formed on the wall surface of the water channel. However, there is a problem that it is corroded by cooling water.

[0004]

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and improves the corrosion resistance of the outer surface against plasma and the like, reduces the amount of gas released in a vacuum environment, and is provided inside. Another object of the present invention is to provide a surface-treated aluminum component part of a vacuum device having improved corrosion resistance of a wall of a cooling water channel.

[0005]

According to the first aspect of the present invention,
A component made of an aluminum or aluminum alloy material provided in a vacuum device, wherein the component has a cooling channel provided therein, has a thickness of at least 0.3 to 0.9 μm on an outer surface, and has a water content Characterized in that a nonporous anodic oxide film having a thickness of not more than 10% by weight is formed, and a boehmite film having a thickness of 0.2 to 3.0 μm is formed on the wall of the water channel. The constituent parts are the means for solving the above problem. According to a second aspect of the present invention, there is provided a vacuum apparatus characterized in that at least a surface-treated aluminum component of the vacuum apparatus according to the first aspect is provided.

According to a third aspect of the present invention, there is provided a cooling water channel inside, and boric acid, borate, adipic acid, tartrate, citrate, Anodizing treatment is performed with an aqueous electrolyte solution of one or more selected from the group of malonates to form a non-porous anodized film having a water content of 10% by weight or less, and then a non-porous anodized surface is formed on the outer surface. The method for producing a surface-treated aluminum component of a vacuum device, which comprises at least a step of immersing the component having the film formed thereon in hot water at 80 to 100 ° C. to form a boehmite film in the channel. This was the solution to the problem.

[0007]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment in which a surface-treated aluminum component of the present invention is applied to a heater cover, a substrate cover, and a gas dispersion plate of a plasma CVD apparatus will be described below. FIG. 1 is a schematic configuration diagram showing an example of a continuous processing type plasma CVD apparatus provided with a heater cover, a substrate cover, and a gas dispersion plate according to an embodiment of the surface-treated aluminum component of the present invention. This plasma CVD apparatus collects a processing vessel 10 capable of vacuum evacuation, a delivery mechanism 12 for delivering a wafer (substrate) 11 into the processing vessel 10, and a wafer 11 on which a thin film such as a plasma silicon oxide film is formed. And a high-frequency applying mechanism 16 for applying high frequency (RF) to the reactive gas supplied into the processing container 10, and a heater 11 for heating the wafer 11 sent into the processing container 10. Heater 18 and the heater 1
8 and a substrate cover 22 disposed above the heater cover 20 with a gap 21 therebetween. When forming a film, the heater cover 20 and the substrate cover Wafer 1 between covers 22
1 is arranged. The processing container 10
Is an Al-Mg 5000 alloy, Al-Mg-Si
It is made of a high strength aluminum alloy such as a 6000 series alloy. Further, the processing container 10 includes:
An exhaust pipe 25 connected to a negative pressure source (not shown) for evacuating the processing vessel 10 and a supply pipe 26 for feeding a reaction gas into the processing vessel 10 are connected. Further, the processing container 10
The gas distribution plate 23 is connected to the tip of the supply pipe 26 in the inside.

The heater cover 20 and the substrate cover 22
Is an embodiment of the surface-treated aluminum component of the present invention, and is made of surface-treated aluminum. These heater cover 20 and substrate cover 22
This is to prevent the heat from the heater 18 from spreading and escaping, and to heat the wafer 11 efficiently and uniformly.
Aluminum or an aluminum alloy is used as a material of the heater cover 20 and the substrate cover 20. The aluminum or aluminum alloy material used here is not particularly limited, and is a pure aluminum-based 1000-based alloy, an Al-Cu-based alloy, an Al-Cu-Mg
2000-based alloy, Al-Mn-based 3000-based alloy,
Al-Si 4000 alloy, Al-Mg 500
0 alloy, Al-Mg-Si 6000 alloy, Al
-7000 of Zn-Mg-Cu system and Al-Zn-Mg system
Based alloy, 7N01 alloy, Al-Fe-Mn based 8000
For example, a forming alloy, a structural alloy, an electric alloy, and a casting alloy such as AC1A, AC2A, AC3A, and AC4B are used. Further, alloys subjected to various refining treatments such as solution treatment and aging treatment are also used. Further, a clad material clad on the surface of these aluminum alloys can also be used. In the present invention, among the above-mentioned alloys, the same Al-Mg-based 5000-based alloy as the material forming the processing vessel 10, Al-Mg-
A Si-based 6000 series alloy is preferred, and a pure aluminum-based 1000 series alloy is particularly preferred when strength is not required.

As shown in FIG. 2, the heater cover 20 is provided with a cooling water passage 20a therein. Further, the heater cover 20 has a nonporous anodic oxide film having a thickness of 0.3 to 0.9 μm and a water content of 10% by weight or less formed on at least the outer surface thereof.
The surface treatment is performed by forming a boehmite film having a thickness of 0.2 to 3.0 μm on the wall surface of a. The substrate cover 22 is provided with a cooling water passage 22 a inside similarly to the heater cover 20. Further, the substrate cover 22 has a thickness of at least 0.3 to
A non-porous anodized film having a thickness of 0.9 μm and a water content of 10% by weight or less is formed, and a boehmite film having a thickness of 0.2 to 3.0 μm is formed on the wall surface of the water channel 22a. I have. The gas dispersion plate 23 is also one embodiment of the surface-treated aluminum component of the present invention, and is made of surface-treated aluminum. This gas dispersion plate 23
The same material as the above-mentioned aluminum or aluminum alloy is used as the material for the above. The gas dispersion plate 23 is provided with a cooling water channel (not shown) inside. Further, the gas dispersion plate 23 has a thickness of at least 0.3 to 0.9 μm on its outer surface and a water content of 1 μm.
0% by weight or less of non-porous anodized film is formed,
Further, a surface treatment is performed by forming a boehmite film having a thickness of 0.2 to 3.0 μm on the wall surface of the water channel.

Next, a method of manufacturing the heater cover 20 will be described in detail. The heater cover 20 is formed using the aluminum or aluminum alloy material as described above, and then a cooling water passage 20a is formed inside the heater cover 20 by post-processing. Thereafter, pre-processing is performed on the heater cover 20. The pre-treatment is not particularly limited, and it suffices that the pre-treatment is capable of removing fats and oils adhering to the surface of the material and removing a heterogeneous oxide film on the aluminum or aluminum alloy surface. For example,
After performing a degreasing treatment with a weak alkaline degreasing solution, a method of performing a desmut treatment in a nitric acid aqueous solution after performing an alkali etching with a sodium hydroxide aqueous solution, and a method of performing acid cleaning after the degreasing treatment are appropriately selected and used. Can be

Then, the pretreated heater cover 20 is immersed in an aqueous electrolyte solution,
Is connected to the anode and subjected to an anodic oxidation treatment using a DC power supply to form a nonporous anodized film on at least the outer surface of the heater cover 20. As the electrolyte aqueous solution, boric acid, borate, adipic acid, tartrate, citrate, malonate, which is an electrolyte that hardly dissolves the generated nonporous anodic oxide film and generates a nonporous anodic oxide film An electrolyte aqueous solution having low film solubility in which one or two or more selected from the group described above are dissolved is used. Among these electrolytes, boric acid, borate and adipic acid are preferred.

The concentration of the electrolyte in the aqueous electrolyte solution ranges from 1 to 20.
0 g / l is preferred. If the electrolyte concentration is lower than 1 g / l, the coating tends to be uneven, while if it exceeds 200 g / l, it is difficult to dissolve and a precipitate may be formed. The aqueous electrolyte solution has a pH of from 2 to 9, preferably from 3 to 9.
8 If the pH of the aqueous electrolyte solution is less than 3, the anodic oxide film tends to be porous, and if the ph exceeds 8, the film dissolves in the electrolyte and the production rate decreases. The temperature of the aqueous electrolyte solution (electrolysis bath temperature) is in the range of 30 to 95 ° C, preferably 40 to 60 ° C. If the bath temperature is lower than 30 ° C., the solubility of the electrolyte is low, and the voltage loss due to the liquid resistance increases. On the other hand, if the bath temperature exceeds 95 ° C., boiling may be involved and costs may be required for heating. When the bath temperature is 40 to 60 ° C., it is effective to reduce the water content of the nonporous anodic oxide film.

In this electrolytic bath, the aluminum or aluminum alloy material is connected to a power source and electrolyzed so as to be an anode even if it is continuous or intermittent. An insoluble conductive material is used for the cathode. As described above, a DC current is used, and a DC density of 0.2 to 5 is used in DC electrolysis.
It is about A / dm ² . If the current density is less than 0.2 A / dm ^2, it takes a long time to form a film. On the other hand, 5A /
If it exceeds dm ² , surface defects such as film and burn easily occur. The electrolysis time is a few seconds to about 30 minutes, and electrolysis is performed by selecting the desired film thickness and electrolysis conditions.

The applied voltage is in the range of about 200 to 650 V, preferably about 350 to 500 V, since the thickness of the oxide film formed with respect to the voltage of 1 V is about 14 angstroms with respect to the DC current. . By performing electrolysis at a high voltage and setting the film thickness to 0.5 to 0.7 μm, high corrosion resistance is obtained, and the film is not deteriorated by boehmite treatment in a later step. By such an anodizing treatment, a nonporous anodized film having a uniform thickness is formed on at least the outer surface of the heater cover 20. The thickness of the nonporous anodized film is 0.3 μm to 0.9 μm, preferably 0.5 μm
About 0.7 μm. If the thickness is less than 0.3 μm, the thickness is too small and the corrosion resistance to a reactive gas, plasma or the like becomes insufficient. On the other hand, since a film thickness larger than 0.9 μm cannot be obtained by the electrolytic treatment, the upper limit of the film thickness is 0.9 μm.

The anodic oxide film thus obtained is nonporous, and its porosity is preferably at most about 5% and its water content is preferably at most 10% by weight. If the porosity of the anodic oxide film exceeds 5%, the surface area of the anodic oxide film increases, and the amount of adsorbed moisture and gas increases, which may have the same adverse effect as an increase in the water content. is there. On the other hand, if the porosity exceeds 5%, it cannot be said that the film is a nonporous film.

The water content of the nonporous anodized film is 10% by weight.
If the pressure exceeds 1, the amount of water (gas released from the film) volatilized from the film increases, so that the degree of vacuum in the processing vessel 10 cannot be sufficiently increased, resulting in poor vacuum characteristics. There is a problem that it reacts with gas, plasma, or the like, contaminates the thin film, and adversely affects the characteristics of the semiconductor substrate.

The porosity and water content (moisture content) are determined by the above-mentioned electrolysis conditions. The above-described anodizing treatment can be performed on an unprocessed aluminum or aluminum alloy material such as a coil. However, it is preferable to perform the anodization on a material that has been subjected to processing such as cutting.

The non-porous anodic oxide film formed by the above-described anodizing treatment is non-porous and does not pass an electric current. Therefore, unlike the porous anodizing treatment (sulfuric alumite treatment), the non-porous anodized film is formed in the water passage 20a. Although a nonporous anodic oxide film is also formed on the wall surface, depending on the shape of the heater cover 20, there may be a portion where the film thickness becomes as thin as about 1/5 to 1/10, or gas generated in the electrolytic treatment may stay. Since it is difficult to form a film in an easy part, a boehmite film is formed on the wall surface of the water channel 20a by performing a boehmite treatment (hydration treatment) in the bath water on the heater cover 20 on which the nonporous anodic oxide film is formed. I do. High-temperature water can be used as building bath water,
In particular, it is preferable to use ion-exchanged water having an electric conductivity of 0.1 μS or less in terms of preventing blackening of the surface of the aluminum or aluminum alloy material and easily forming a boehmite film.

The temperature of the construction bath water is from 80 ° C. to the boiling point (100
° C). The boehmite treatment in the present invention is 20
It is about 180 minutes. In the construction bath water, it is preferable to use pure water alone to prevent the adhesion of impurities, but it is also possible to add an alkali additive such as ammonia, amine, alcoholamine, amide, and triethanolamine, and use it. When the boehmite film formation rate is high, it is necessary to shorten the boehmite treatment time.

The water channel 20a made of aluminum or aluminum alloy material by such boehmite treatment
A boehmite film is formed on the wall surface of. The thickness of the boehmite film is 0.2 μm to 3.0 μm, preferably 1.
It is about 0 μm to 2.0 μm. If the thickness of the boehmite film is less than 0.2 μm, sufficient corrosion resistance to cooling water flowing through the water channel 20a cannot be obtained. On the other hand, even if the film thickness is increased beyond 3.0 μm, no significant increase in the effect can be expected anymore, and the processing time for forming the film becomes longer, which is disadvantageous in cost. During the boehmite treatment as described above, the hydration treatment does not proceed because a nonporous anodic oxide film is formed on the outer surface of the heater cover 20, while the inner water passage 20 a is formed by the nonporous anodic oxidation. Since the film is not formed sufficiently, a boehmite film (hydrated film) is formed. As described above, the heater cover 20 of the embodiment of the surface-treated aluminum component of the present invention
Is obtained.

The method of manufacturing the substrate cover 22 is as follows.
Then, after forming a cooling water channel 22a inside the substrate cover 22 by post-processing, a thickness of 0.3 to 0.3 mm is formed on at least the outer surface of the substrate cover 22 in the same manner as in the method of manufacturing the heater cover 20 described above. 0.9 μm and water content of 1
0% by weight or less of a nonporous anodic oxide film
When a boehmite film having a thickness of 0.2 to 3.0 μm is formed on the wall surface a, the substrate cover 22 of the embodiment of the surface-treated aluminum component of the present invention is obtained. Further, the method of manufacturing the gas dispersion plate 23 includes forming the gas dispersion plate 23 using aluminum or an aluminum alloy, forming a cooling water passage inside the gas dispersion plate 23 by post-processing, and then forming the above-described heater. In the same manner as in the method of manufacturing the cover 20, at least the outer surface of the gas distribution plate 23 has a thickness of 0.3 to
A non-porous anodic oxide film having a thickness of 0.9 μm and a water content of 10% by weight or less is formed, and a thickness of 0.2 to 3.
When a 0 μm boehmite film is formed, the gas dispersion plate 23 of the embodiment of the surface-treated aluminum component of the present invention is obtained.

In order to form a thin film on the wafer 11 using such a plasma CVD apparatus, the inside of the processing chamber 10 is depressurized by operating a negative pressure source connected to the exhaust pipe 25,
The reactive gas is supplied from the supply pipe 26 and high frequency is applied to the reactive gas by the high frequency applying mechanism 16, and the wafer 11 sequentially sent from the sending mechanism 12 to the gap 21 between the heater cover 20 and the substrate cover 22 is heated by the heater. A thin film is formed while heating by 18, and the wafer 11 on which the thin film is formed is sequentially collected by the collecting mechanism 14. At this time, if necessary, the water channel 20a of the heater cover 20 and the substrate cover 22
This is performed while flowing cooling water through the water channel 22a.

At least the outer surface of the heater cover 20, the substrate cover 22, and the gas distribution plate 23 of the embodiment of the surface-treated aluminum component of the present invention has a thickness of 0.3 to 0.9 μm and a water content of Is less than 10% by weight, a small amount of gas is released from the film and the outer surface has excellent corrosion resistance to plasma and the like. In addition, the thickness of the wall
Due to the formation of the 3.0 μm boehmite film,
Excellent corrosion resistance to cooling water. In addition, in forming a nonporous anodic oxide film, no sealing treatment is required, and the electrolysis time can be shorter than in the case of forming a porous anodic oxide film. The productivity can be improved and the cost can be reduced. Further, when the porosity of the nonporous anodic oxide film is 5% or less, the effect of reducing water and gas adsorbed on the surface and the corrosion resistance are particularly excellent. Therefore, in the plasma CVD apparatus provided with the heater cover 20, the substrate cover 22, and the gas dispersion plate 23 of such an embodiment,
Even in a vacuum environment, the amount of gas released from the film due to the moisture is small, so that the vacuum characteristics are excellent, and the gas released from the film reacts with a reactive gas such as chlorine gas or plasma. When a thin film is formed using such a plasma CVD apparatus,
There is an advantage that contamination of the thin film is improved, and a semiconductor substrate having stable characteristics is easily obtained.

In the embodiment of the vacuum device, the case where the heater cover 20, the substrate cover 22, and the gas dispersion plate 23 are arranged in the processing container 10 has been described. However, in the vacuum device according to the present invention, One or two things may be provided.
Further, in the embodiment of the vacuum apparatus, the case where the surface-treated aluminum component of the present invention is provided in the plasma CVD apparatus has been described. However, the present invention is not necessarily limited thereto, and a CVD apparatus, an ion plating apparatus, a dry etching apparatus, It may be provided in a vacuum device such as a PVD device. Further, in the embodiment of the surface-treated aluminum component, the case where the invention is applied to the heater cover 20, the substrate cover 22, and the gas distribution plate 23 has been described. However, the present invention is not necessarily limited to this, and the surface-treated aluminum component according to the present invention is not limited thereto. Can also be applied to susceptors and the like.

[0025]

The present invention will now be described by way of Examples and Comparative Examples.
Although specifically described, the present invention is not limited to only these examples. JIS as aluminum alloy
After a test piece made of a 5052 alloy material was formed, a water channel was formed inside the test piece by post-processing. Then, after degreasing this test piece with a weak etching degreasing agent,
Electrolyte at 140 to 640 V, current density of 1 A / dm ² and 45 ° C. with an aqueous electrolyte solution in which 80 g / l boric acid and 0.5 g / l ammonium borate are dissolved to form a nonporous anodic oxide film on at least the outer surface did. Here, the film thickness of the nonporous anodic oxide film was adjusted by changing the electrolytic voltage. After the electrolysis, the alloy was washed with water and dried at 80 ° C. Then, the test piece on which the non-porous anodic oxide film was formed was subjected to boehmite treatment in boiling water (ion-exchanged water) to form a boehmite film on the wall of the water channel, thereby performing various tests for surface treatment. (Sample No. 1)
To 8). Here, the thickness of the boehmite film was adjusted by changing the boehmite treatment time.

Further, as a comparative example, a test piece having a water channel therein was degreased using a JIS5052 alloy material in the same manner as described above, and then was subjected to a 50 ° C., 10% aqueous sodium hydroxide solution for 2 minutes. It was etched and washed with water. Then, after being immersed in 10% nitric acid at room temperature for 1 minute and desmutted, 1.3 A / dm3 with 15% to 20% sulfuric acid.
² , electrolysis was performed at 5 to 20 ° C. for 20 minutes to form a porous anodic oxide film on the outer surface of the test piece, thereby obtaining a surface-treated test piece (Sample Nos. 9 to 1).
1). Further, the test piece of Sample No. 11 was subjected to boehmite treatment in boiling water (ion-exchanged water) to form a boehmite film on the wall of the water channel.
The porous anodic oxide films of the test pieces of Sample Nos. 9 to 10 were not subjected to sealing treatment. The alumite sulfate treatment at the time of preparing the test piece of Sample No. 9 was performed using 15% sulfuric acid at 20 ° C. The alumite sulfate treatment at the time of preparing the test pieces of Sample Nos. 10 to 11 was performed using 20% sulfuric acid at 5 ° C.

The water content of the anodic oxide films of the test pieces of Sample Nos. 1 to 11 was measured by thermogravimetric analysis. The results are shown in Table 1 below. In addition, sample No.
The test pieces 1 to 11 were evaluated for corrosion resistance on the outer surface side, gas release property, and corrosion resistance of water channels. The results are shown in Table 1 below. Here, the corrosion resistance of the outer surface side was evaluated by irradiating a test piece with CF ₄ plasma of ₄₀ eV for 30 minutes in an atmosphere sucked in a vacuum of 10 ⁻⁶ Torr or less, and measuring a change in film thickness. The evaluation criterion is that the decrease in film thickness is 10%.
The following were rated as (○), and those with a decrease in film thickness of more than 10% were rated (x). In addition, the corrosion resistance of the outer surface side was set at 300 ° C. in an atmosphere sucked in a vacuum of 10 ⁻⁶ Torr or less.
Was evaluated by analyzing the amount of gas released upon heating to gas mass. The evaluation criteria were as follows: (○) when the gas was hardly released, (△) when the gas was released a little, (X) when the amount of gas released was large, and (XX) when very large amount of gas was released. The corrosion resistance of the waterway is
The evaluation was made by observing the state of the wall surface when tap water at 40 ° C. was flowed through the channel of the test piece for 30 days.
The results are shown in Table 1 below. The evaluation criteria were as follows: (の も の) when the area of the corroded portion was less than 10%, (△) when the area of the corroded portion was 10 to 30%, and (×) when the area of the corroded portion exceeded 30%.

[0028]

[Table 1]

As is evident from the results shown in Table 1, the sample No. 9 (comparative example) in which the porous anodic oxide film was formed by the alumite sulfate treatment had poor corrosion resistance on the outer surface side. This is because a corrosive gas or plasma invades from the holes and the corrosion resistance is reduced. Further, in the sample No. 11, a large amount of gas was released, because the hydration reaction proceeded more through the pores of the anodic oxide film during the boehmite treatment, and the water content of the film was 30 to 30%.
This is because it will be about 60% by weight. On the other hand, it was found that in the case where the nonporous anodic oxide film was formed, the above-mentioned hydration reaction did not proceed slightly. Also,
The water content is 10% by weight or less and the thickness is 0.3 to 0.9.
Samples Nos. 1 to 5 in which a non-porous anodic oxide film of μm is formed on the outer surface have a low water content and prevent the invasion of corrosive gas or plasma from the holes, so that the corrosion resistance on the outer surface side is reduced. It is clear that the gas emission is small and the gas emission amount is small. Further, even when the non-porous anodic oxide film is formed on the outer surface, the non-porous anodic oxide film has a water content of more than 10% by weight or the sample N having a thickness of less than 0.3 μm.
It can be seen that those with o.7 to 8 have poor corrosion resistance on the outer surface and a large amount of gas release. The sample No. 6 having a thin boehmite film thickness of 0.15 μm is
It can be seen that the corrosion resistance of the waterway is poor.

[0030]

As described above, in the surface-treated aluminum component of the vacuum device of the present invention, at least the outer surface has a thickness of 0.3 to 0.9 μm and a water content of 10 to 10 μm.
% By weight of a non-porous anodic oxide film having a thickness of 0.2 to 3.0 μm on the wall of a water channel provided therein. In addition, the corrosion resistance to plasma and the like on the outer surface is excellent, and the corrosion resistance to cooling water in the internal water passage is excellent. In addition, in the formation of the nonporous anodic oxide film, no sealing treatment is required, and the electrolysis time can be shorter than in the case of forming a porous anodic oxide film. In addition, productivity can be improved and costs can be reduced. Further, in a vacuum device provided with a surface-treated aluminum component of the vacuum device of the present invention,
Even in a vacuum environment, the amount of gas released from the film due to the moisture in the film is small, so the vacuum characteristics are excellent, and the gas released from the film is reactive gas such as chlorine gas or plasma. Because there is almost no reaction,
When etching or thin film formation is performed using such a vacuum device, the occurrence of poor etching or contamination of the thin film is improved, and there is an advantage that a semiconductor substrate or the like having stable characteristics is easily obtained.

[Brief description of the drawings]

FIG. 1 is a schematic configuration diagram showing an example of a continuous processing type plasma CVD apparatus provided with a heater cover, a substrate cover, and a gas dispersion plate according to an embodiment of a surface-treated aluminum component of the present invention.

FIG. 2 is a diagram of a heater cover provided in the plasma CVD apparatus of FIG. 1 as viewed from a substrate side.

[Explanation of symbols]

20: heater cover, 20a: water channel, 22: substrate cover, 22a: water channel, 23: gas dispersion plate.

Claims (3)

[Claims] 1. A component made of aluminum or an aluminum alloy material provided in a vacuum device, wherein said component has a cooling water channel provided therein and has a thickness of at least 0.3 to 0.9 μm on an outer surface. And a non-porous anodic oxide film having a water content of 10% by weight or less is formed, and a boehmite film having a thickness of 0.2 to 3.0 μm is formed on the wall of the water channel. Surface treated aluminum components of equipment. 2. A vacuum device comprising at least a surface-treated aluminum component of the vacuum device according to claim 1. 3. A component having a cooling water passage therein, and boric acid, borate, adipic acid, tartrate,
One or two selected from the group consisting of citrate and malonate
After performing anodizing treatment with an aqueous electrolyte solution comprising at least one or more species to form a nonporous anodized film having a water content of 10% or less, the component having the nonporous anodized film formed on the outer surface is heated to 80 to 100 ° C. At least a step of forming a boehmite film in the water channel by immersion in hot water.