JP5975747B2 - Vacuum chamber components - Google Patents

Description

  The present invention relates to a vacuum chamber component, and more particularly to a vacuum chamber component having a metal plating film.

  In a manufacturing process of a semiconductor device or the like, various thin films are formed on a base material in a vacuum chamber by a sputtering method, a vacuum deposition method, or the like. During this film forming process, unnecessary films adhere to the vacuum chamber components such as the inner wall of the chamber, the deposition plate, and the vacuum parts.

  The film adhering to the vacuum chamber components becomes a contamination source when depositing other types of films, so that components with unnecessary films adhering must be cleaned. The vacuum chamber components are often cleaned by physical cleaning by sandblasting or chemical cleaning using a cleaning solution. Since such a cleaning operation is expensive and takes time to complete the cleaning, a simpler method for removing dirt from vacuum chamber components has been studied. For example, Japanese Patent Application Laid-Open No. 2005-101435 discloses an adhesion preventing plate formed by laminating an aluminum sheet so as to be peelable with an adhesive. If this adherence plate is contaminated, an aluminum sheet of another layer that is not contaminated will appear from the lower layer only by peeling off the outermost aluminum sheet to which dirt has adhered. You can reuse the landing plate.

JP 2005-101435 A

  However, when an aluminum sheet is bonded with an adhesive, outgas is generated from the adhesive, and the deposition preventing plate itself becomes a contamination source. Many vacuum chamber components have complicated shapes, and it is difficult to attach an aluminum sheet to the components having such complicated shapes. As described above, it is difficult to apply the structure in which the aluminum sheet is bonded to other than the flat protection plate.

  Therefore, an object of the present invention is to provide a vacuum chamber component that can easily remove attached dirt. Other objects of the present invention will become apparent by referring to the entire specification.

  The inventor makes the surface roughness of the base material on which the passive film is formed on the surface layer below a predetermined value, and when the specific metal plating film is formed on the passive film, the metal plating film is peeled off from the base material. We paid attention to that it is easy to do. Then, by applying such a metal plating film to a vacuum chamber component, it was found that the dirt attached to the vacuum chamber component can be easily removed simply by peeling off the metal plating film. The present invention has been made based on such knowledge. Each embodiment of the present invention will be described in detail below.

  A vacuum chamber component according to an embodiment of the present invention includes a passive film having a film thickness of 1 nm or more mainly composed of chromium hydrated oxyoxide on the surface, and the surface roughness is an arithmetic average roughness Ra of 0. A stainless steel substrate of 7 μm or less, formed on the stainless steel substrate through the passive film, an electrolytic Ni plating film, an electrolytic Sn plating film, an electrolytic Cu plating film, an electrolytic Ag plating film, an electroless Ni-P And at least one metal plating film selected from the group consisting of a plating film and an electroless Cu plating film.

  A vacuum chamber component according to another embodiment of the present invention includes a passive film having a thickness of 1 nm or more mainly composed of titanium oxide on the surface, and the surface roughness is 0.7 μm or less in terms of arithmetic average roughness Ra. A titanium alloy base material, and at least one metal plating film formed on the titanium alloy base material through the passive film and selected from the group consisting of an electrolytic Ni plating film and an electrolytic Cu plating film.

  A vacuum chamber component according to another embodiment of the present invention is a base material and an electroless Ni plating film formed on the base material, and the surface layer thereof has a thickness of 1 nm or more mainly composed of nickel oxide. A Ni plating film having a Vickers hardness Hv of 900 or more and a surface roughness of 0.6 μm or less in arithmetic mean roughness Ra; And an electrolytic Ni plating film formed through a dynamic film.

  A vacuum chamber component according to another embodiment of the present invention is provided with a passive film having a film thickness of 1 nm or more mainly composed of aluminum oxide and / or aluminum hydroxide on the surface, and the surface roughness is an arithmetic average roughness. And an aluminum alloy base material having a thickness Ra of 0.3 μm or less, and an electrolytic Cu plating film formed on the aluminum alloy base material via the passive film.

  According to various embodiments of the present invention, a vacuum chamber component is provided that can easily remove attached dirt.

Schematic of a vacuum apparatus in which a vacuum chamber component according to an embodiment of the present invention is used. Schematic of vacuum chamber components according to one embodiment of the present invention

  Various embodiments of the present invention will be described with reference to the accompanying drawings. In each embodiment, similar constituent elements will be described with similar reference numerals, and detailed description of the similar constituent elements will be omitted as appropriate.

  The present invention can be applied to a vacuum chamber provided in various vacuum apparatuses, and can be applied, for example, to a vacuum chamber provided in various film forming apparatuses for forming a film on a substrate. The film forming apparatus to which the present invention can be applied includes various PVD apparatuses for forming a film on a substrate by various physical vapor deposition methods (PVD method), various CVD apparatuses for forming a film on a substrate by various chemical vapor deposition methods (CVD method), and various types. An etching apparatus for processing the substrate surface by an etching method is included. As an example, the PVD apparatus to which the present invention is applicable includes various sputtering apparatuses for forming a film on a substrate by a sputtering method.

  FIG. 1 shows a schematic view of a sputtering apparatus in which a vacuum chamber component according to an embodiment of the present invention is used. As illustrated, a vacuum apparatus 10 according to an embodiment of the present invention includes a vacuum chamber 11, and a substrate fixing jig 12 for fixing the substrate 13 and a target 14 are fixed inside the vacuum chamber 11. A target installation unit 15 is provided. The substrate fixing jig 12 and the target setting unit 15 may be configured to be rotatable in order to form a uniform thin film on the substrate 13.

  The inside of the vacuum chamber 11 is connected to the pressure control means 18 through the gas pipe 18a and the main valve 18b. The pressure control means 18 includes a vacuum pump, and the vacuum chamber 11 is evacuated by the vacuum pump until a predetermined ultimate pressure is reached. During film formation, sputtering gas is supplied from the gas supply unit 19 into the vacuum chamber 11 through the gas pipe 19a and the gas supply valve 19b, and a voltage is applied to the target 14 from the power supply unit 16. As a result, atoms jumping out of the target react with the sputtering gas, and the substance generated by this reaction reaches the surface of the substrate 13. The substance that has reached the surface of the substrate 13 is deposited on the surface of the substrate 13, and a thin film made of the substance is formed.

  The atoms ejected from the target and the products (hereinafter referred to as “film constituent materials”) generated by the reaction of the atoms and the sputtering gas are not only the substrate 13 but also the inner wall 11a of the vacuum chamber 11 and the vacuum chamber. 11 may adhere to various vacuum parts exposed in the interior. In order to prevent this film constituent material from reaching the inner wall 11a, a deposition preventing plate 17 is installed so as to cover the inner wall 11a. As described above, by performing the film forming process in the vacuum chamber 11, the film constituent material adheres to the deposition preventing plate 17 and various vacuum parts provided in the vacuum chamber 11, and an unnecessary film is formed on these surfaces. End up. Depending on the shape of the deposition preventing plate 17 and the installation method, an unnecessary film may be formed on the inner wall 11a.

  Such an unnecessary film formed on the components of the vacuum chamber 11 can cause various problems in the film forming process. For example, when a film different from the unnecessary film attached to the components of the vacuum chamber 11 is formed in the vacuum chamber 11, it becomes a contamination source. Further, the film attached to the components of the vacuum chamber 11 adsorbs moisture, so that the evacuation may take a long time. Furthermore, when an unnecessary film adhering to the components of the vacuum chamber 11 is insulative, formation of a desired electric field in the vacuum chamber 11 may be prevented.

  The present invention provides a vacuum chamber component that can easily remove dirt even when it is attached as described above. FIG. 2 is a view schematically showing a vacuum chamber component according to an embodiment of the present invention. As illustrated, a vacuum chamber component 20 according to an embodiment of the present invention includes a base material 21 and a metal plating film 22 formed on the base material 21. The substrate 21 includes a substrate body 21a and a passive film 21b formed on the surface layer of the substrate body 21a. The metal plating film 22 is provided on the base body 21a via the passive film 21b.

  The vacuum chamber component 20 is an arbitrary part or member exposed to the vacuum atmosphere in the vacuum chamber 11, for example, an inner wall 11a of the vacuum chamber 11, a vacuum valve (not shown), a vacuum gauge (not shown), And various vacuum parts. The inner wall 11a, the substrate fixing jig 12, the target installation portion 15, the deposition plate 17, the main valve 18b, and the gas supply valve 19b in the embodiment shown in FIG. 1 are all examples of the vacuum chamber component 20. Further, since the ends of the gas pipe 18a and the gas pipe 19a are exposed in the vacuum chamber 11, the gas pipe 18a and the gas pipe 19a can also be included in the vacuum chamber component 20.

  The vacuum chamber components to which the present invention is applied are not limited to those shown in the figure, but include, for example, a rotation mechanism for rotating the substrate fixing jig 12 and the target setting portion 15, a thermocouple for temperature measurement, and a shutter for the viewport. The rotating part of the vacuum pump, various bolts, nuts, bands, flanges and the like provided in the vacuum chamber 11 are also included in the vacuum chamber components to which the present invention is applied. In addition to those explicitly described in this specification, the vacuum chamber 11 can be provided with various components according to its use, and such components are also included in the vacuum chamber components to which the present invention is applied. obtain.

  The materials of the base body 21a, the passive film 21b, and the metal plating film 22 are appropriately determined so that the metal plating film 22 can be easily separated from the base material 21 in the completed component 20. For example, in one embodiment, the base material 21a is formed of stainless steel such as stainless steel (SUS304) in the shape of the component 20. FIG. 2 shows a plate-like base material 21, but the base material 21 a can take any shape according to the type of the component 20. For example, when the component 20 is a bolt, the shape is a bolt. When the substrate 21a is made of stainless steel, the passive film 21b is a film mainly composed of chromium hydrated oxyoxide CrOx (OH) 2-x · nH2O, and the metal plating film 22 is electrolytic Ni plating. It is at least one plating film selected from the group consisting of a film, an electrolytic Sn plating film, an electrolytic Cu plating film, an electrolytic Ag plating film, an electroless Ni plating film, and an electroless Cu plating film. The base material 21 made of stainless steel has an arithmetic mean roughness Ra of 0.7 μm or less, and the chromium hydrated oxyoxide passive film 21b has a thickness of 1 nm or more. Further, the film thickness of the metal plating film 22 is approximately 50 nm to 1000 μm, regardless of which type of plating is used. The thickness of the metal plating film 22 is preferably 20 μm to 100 μm in order to withstand the tensile stress at the time of peeling.

  In another embodiment, the base material 21a is formed by forming a titanium alloy such as a titanium alloy (TP340) into the shape of the component 20. In this case, the passive film 21b is a film having a thickness of 1 nm or more mainly composed of titanium oxide, and the metal plating film 22 is at least one selected from the group consisting of an electrolytic Ni plating film and an electrolytic Cu plating film. It is a plating film. The titanium alloy base material 21 has a surface roughness of 0.7 μm or less in terms of arithmetic average roughness Ra, and the thickness of the passive film 21b mainly composed of titanium oxide is 1 nm or more.

  In another embodiment, the base material 21a is formed by forming an aluminum alloy such as an A2000 series aluminum alloy into the shape of the component 20. In this case, the passive film 21b is a film having a thickness of 1 nm or more mainly composed of aluminum oxide and / or aluminum hydroxide, and the metal plating film 22 is an electrolytic Cu plating film. The base material 21 of the aluminum alloy has an arithmetic average roughness Ra of 0.3 μm or less, and the thickness of the passive film 21b mainly composed of aluminum oxide and / or aluminum hydroxide is 1 nm or more. It is.

  In another embodiment, the base material 21a is formed by forming a base material made of an arbitrary material capable of electroless Ni plating into the shape of the component 20, for example, stainless steel, steel, Al, Al alloy, Ti , Ti alloy, Mg, Mg alloy, Cu, Cu alloy, glass, ceramics, Inconel, and brass. In this case, an electroless Ni plating layer (not shown) is formed on the surface of the base material 21a directly or indirectly with a base layer according to a conventional method. This electroless Ni plating film has a hardness of 900 or more in terms of Vickers hardness Hv and a surface roughness of 0.6 μm or less in terms of arithmetic average roughness Ra. A passive film 21b having a thickness of 1 nm or more mainly composed of nickel oxide is formed on the surface layer of the electroless Ni plating layer. An electrolytic Ni plating film is formed as a metal plating film 22 on the passive film 21b.

  A method of creating the vacuum chamber component 20 will be described by taking as an example the case of using a stainless steel base material 21. Even when another material such as a titanium alloy is used as the material of the base material 21, the component 20 can be produced by the same method. Therefore, the case of using the stainless steel base material 21 will be described as a representative example. First, a stainless steel substrate that is commonly used as a material for vacuum chamber components is prepared and processed into the shape of the component 20. When the surface roughness of the prepared stainless steel base material is larger than 0.7 μm in arithmetic average roughness Ra, the surface roughness of the stainless steel is set to 0. 0 in arithmetic average roughness Ra by lapping polishing or blasting. It adjusts so that it may become 7 micrometers or less. On the surface layer of stainless steel, a passive film mainly composed of chromium hydrated oxyoxide having a film thickness of 1 nm or more is usually formed. When there is no passive film mainly composed of chromium hydrated oxyoxide on the surface layer of stainless steel, or when the thickness of the passive film 21b is less than 1 nm, the substrate 21 is heated, The oxidation of the stainless steel in the surface layer of the base material 21 is promoted, and a passive film 21b mainly composed of chromium hydrated oxyoxide of 1 nm or more is formed on the surface layer of the base material 21.

  Next, it is selected from the group consisting of an electrolytic Ni plating film, an electrolytic Sn plating film, an electrolytic Cu plating film, an electrolytic Ag plating film, an electroless Ni plating film, and an electroless Cu plating film on the passive film 21b. At least one metal plating film 22 is formed. The metal plating film 22 is formed by appropriately using a well-known plating method that is commonly used.

  The type and thickness of the metal plating film 22 include the material of the base material 12, the surface roughness of the base material 21, the formation state of the passive film 21b, the oil film for promoting peeling applied to the surface of the base material 21 and the foreign material layer. Presence / absence and / or conditions of the vacuum equipment in which the component is used (initial vacuum level, time to reach initial vacuum level, vacuum during process, type of source gas, process temperature, pressure during process , And applied voltage, elements to be removed as contamination sources, etc.).

  Various pre-treatments can be performed on the base material 21 before the metal plating film 22 is formed. For example, an oil film, wax, wax, or graphite may be spray-coated on the surface of the base material 21 before the metal plating film 22 is formed, and a thin film of an amorphous carbon film is formed on the surface of the base material 21. Also good. By performing such pretreatment, the metal plating film 22 is more easily peeled off from the base material 21. A thin film formed by spray coating or an amorphous carbon film is formed to a thickness that does not substantially impair the conductivity required for plating, for example, to a thickness of 100 nm or less. The For pretreatments such as water washing, hot water purification, alkaline degreasing, electrolytic degreasing, alcohol cleaning, and organic solvent cleaning that are commonly used to improve the adhesion of the plating film to the substrate, the metal plating film 22 is removed from the substrate 21. It is desirable to omit this because it can be a factor that makes it difficult to peel off.

  Before forming the metal plating film 22, a part of the surface of the base material 21 on which the passive film 21b is formed is smoothed so that the surface roughness of the part becomes smaller than that of the other part. Also good. For example, as shown in FIG. 2, a mirror surface processing may be performed on a part of the surface of the base material 21 to provide a mirror surface portion 23. The mirror surface portion 23 can be provided at an arbitrary position on the surface of the base material 21 in consideration of ease of peeling of the metal plating film 22. For example, it is provided along the edge of the substrate 21. Thus, by providing a part of the surface of the base material 21 with a surface roughness smaller than that of the other part, the metal plating film 22 can be more easily peeled off starting from the part.

  Further, the metal plating film 22 may be formed in a state in which a part of the surface of the substrate 21 is masked with an adhesive tape or the like so that the plating film is not formed on the part. As a result, a step is formed between the portion where the plating film is not formed and the portion where the plating film is formed, so that the metal plating film 22 can be more easily peeled off starting from this step.

  The metal plating film 22 formed as described above can be easily peeled off from the base material 21 simply by the operator holding and pulling a part of the metal plating film 22 with a fingertip. Tools such as markings, tweezers, pliers, and pliers can be used to pick the metal plating film 22. Further, it is possible to make the metal plating film 22 more easily peeled off from the base material 21 by applying ultrasonic waves to the metal plating film 22 or applying vibration. Further, the metal plating film 22 can be easily peeled off from the substrate 21 by alternately raising the metal plating film 22 to a high temperature and a low temperature. Some of these peeling methods can be used in combination with other peeling methods.

  In each embodiment of the present invention, even if the metal plating film 22 is provided on the substrate 21, the metal plating film 22 itself does not become a contamination source. Further, since one surface of the metal plating film 22 is in close contact with the surface of the base material 21, the amount of moisture adsorbed does not increase and does not hinder evacuation. Further, the metal plating film 22 is peeled off from the base material 21 in the form of a sheet and does not remain on the base material 21. For this reason, the metal plating film 22 can be removed from the base material 21 only by performing a simple peeling operation. In addition, various substances attached to the metal plating film 22 peeled off in the form of a sheet can be easily recovered. In particular, when a noble metal such as gold, silver, platinum, or rhodium adheres to the metal plating film 22, the metal plating film 22 can be a film that is easily dissolved in a chemical solution such as an acid such as an Sn plating film. Since the Sn plating film is easily dissolved in acid, precious metals such as gold attached to the Sn plating film can be easily separated and recovered by immersing the peeled Sn plating film in an acid solution.

  Although FIG. 2 illustrates an example in which the metal plating film 22 is formed on one surface of the base material 21, the metal plating film 22 can be formed on any surface of the base material 21. Various coatings can be formed on the metal plating film 22 within the scope of the present invention. For example, by forming a Sn plating film on the metal plating film 22, it becomes possible to easily collect the precious metal adhering to the surface. Further, by forming an Ag plating film, a Cu plating film, an Au plating film, or an Rh plating film on the metal plating film 22, the conductivity of the finished product surface can be improved. Further, on the metal plating film 22, an amorphous carbon film or a film such as Au or ITO formed by a vacuum process may be formed.

Example 1-1 to Example 1-6
A plate material of 10 cm in length, 4 cm in width, and 0.5 mm in thickness, made of stainless steel (SUS304) with a surface roughness of 0.08 μm of chromium-hydrated oxyoxide formed on the surface layer and an arithmetic average roughness Ra of 0.08 μm. Got ready. Next, the surface layer of the plate was washed with diluted neutral detergent. An electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of this plate material by using a sulfamic acid Ni plating solution manufactured by Nippon Kagaku Sangyo Co., Ltd. according to a conventional method. A sample in which an electrolytic Ni plating film was formed on a stainless steel substrate provided with the passivated film of chromium hydrated oxyoxide thus obtained was named Example 1-1. The surface roughness (arithmetic mean roughness Ra) values described in this specification were measured using a Keyence ultra deep color 3D shape measurement microscope VK-9510, with a lens magnification of 150 times and a RUN MODE of over color. It was measured with depth, wavelength set to 408 nm, maximum output set to 0.9 mW, and pitch set to 0.1 μm.

  The same stainless steel plate as in Example 1-1 was prepared, and electrolytic Cu plating having a film thickness of about 25 μm was prepared on the surface of this plate using a pyrophosphoric acid Cu plating solution manufactured by Nippon Chemical Industry Co., Ltd. according to a conventional method. Formed. A sample in which the electrolytic Cu plating film was formed on the stainless steel substrate provided with the passive film of the chromium hydrated oxyoxide thus obtained was named Example 1-2.

  The same stainless steel plate as in Example 1-1 was prepared, and electrolytic Sn plating with a film thickness of about 25 μm was formed on the surface of this plate using a UTBSn plating solution manufactured by Ishihara Pharmaceutical Co., Ltd. according to a conventional method. . A sample in which an electrolytic Sn plating film was formed on a stainless steel substrate provided with a passivated film of chromium hydrated oxyoxide thus obtained was named Example 1-3.

  The same stainless steel plate as in Example 1-1 was prepared, and electrolytic Ag plating with a film thickness of about 25 μm was formed on the surface of this plate using a dine silver plating solution manufactured by Daiwa Kasei Co., Ltd. according to a conventional method. did. A sample in which an electrolytic Ag plating film was formed on a stainless steel substrate provided with the passivated film of chromium hydrated oxyoxide thus obtained was named Example 1-4.

  The same stainless steel plate material as in Example 1-1 was prepared, and Melplate NI-2280LF M1 plating solution and Melplate NI-2280LF M2 plating solution manufactured by Meltex Co., Ltd. were used on the surface of this plate material. Accordingly, an electroless Ni—P plating having a phosphorus concentration of about 12.8 wt% and a film thickness of about 25 μm was formed. A sample in which an electroless Ni—P plating film was formed on a stainless steel substrate provided with the thus obtained passive film of chromium hydrated oxyoxide was designated as Example 1-5.

  The same stainless steel plate as in Example 1-1 was prepared, and electroless Cu plating with a film thickness of about 25 μm was performed on the surface of the plate using Melplate Cu plating solution manufactured by Meltex Co., Ltd. according to a conventional method. Formed. A sample in which an electroless Cu plating film was formed on a stainless steel substrate provided with the thus obtained passive film of chromium hydrated oxyoxide was defined as Example 1-6.

Example 2-1 to Example 2-6
As in Example 1-1, chromium hydrated oxyoxide of 1 nm or more is formed on the surface layer, the surface roughness is made of stainless steel (SUS304) having an arithmetic average roughness Ra of 0.08 μm, 10 cm in length, A plate material having a width of 4 cm and a thickness of 0.5 mm was prepared. And this board | plate material was blasted and the surface roughness was 0.2 micrometer by arithmetic mean roughness Ra. Next, the surface layer of the plate was washed with diluted neutral detergent. Then, an electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the plate material by using a sulfamic acid Ni plating solution manufactured by Nippon Chemical Industry Co., Ltd. according to a conventional method. The sample thus obtained was named Example 2-1.

  An electrolytic Cu plating having a film thickness of about 25 μm is formed on a stainless steel plate material (Ra is 0.2 μm) blasted as in Example 2-1 in the same manner as in Example 1-2. -2 sample was obtained. Also, electrolytic Sn plating having a film thickness of about 25 μm was formed on a stainless steel plate (Ra: 0.2 μm) blasted in the same manner as in Example 2-1 in the same manner as in Example 2-1. The sample of Example 2-3 was obtained. Further, electrolytic Ag plating having a film thickness of about 25 μm was formed on a stainless steel plate material (Ra: 0.2 μm) blasted in the same manner as in Example 2-1 in the same manner as in Example 2-1, and then performed. The sample of Example 2-4 was obtained. Further, electroless Ni-P plating having a film thickness of about 25 μm is formed on the stainless steel plate material (Ra is 0.2 μm) as in Example 2-1 by the same method as in Example 1-5. Thus, a sample of Example 2-5 was obtained. Further, an electroless Cu plating having a film thickness of about 25 μm is formed on the stainless steel plate material (Ra is 0.2 μm) blasted in the same manner as in Example 2-1 by the same method as in Example 1-6. A sample of Example 2-6 was obtained.

Example 3-1 to Example 3-6
As in Example 1-1, chromium hydrated oxyoxide of 1 nm or more is formed on the surface layer, and the surface roughness is made of stainless steel (SUS304) having an arithmetic average roughness Ra of 0.08 μm, 10 cm in length, A plate material having a width of 4 cm and a thickness of 0.5 mm was prepared. And this board | plate material was blasted and the surface roughness was 0.7 micrometer by arithmetic mean roughness Ra. Next, the surface layer of the plate was washed with diluted neutral detergent. Then, an electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the plate material by using a sulfamic acid Ni plating solution manufactured by Nippon Chemical Industry Co., Ltd. according to a conventional method. A sample in which the electrolytic Ni plating film was formed on the stainless steel substrate provided with the passivated film of chromium hydrated oxyoxide thus obtained was named Example 3-1.

  An electrolytic Cu plating having a film thickness of about 25 μm is formed on a stainless steel plate material (Ra is 0.7 μm) blasted in the same manner as in Example 3-1 in the same manner as in Example 3-1, -2 sample was obtained. Also, electrolytic Sn plating having a film thickness of about 25 μm was formed on a stainless steel plate (Ra: 0.7 μm) blasted in the same manner as in Example 3-1 in the same manner as in Example 3-1. A sample of Example 3-3 was obtained. Also, electrolytic Ag plating with a film thickness of about 25 μm was formed on the stainless steel plate material (Ra is 0.7 μm) blasted in the same manner as in Example 3-1 in the same manner as in Example 3-1. The sample of Example 3-4 was obtained. Also, electroless Ni-P plating having a film thickness of about 25 μm is formed on the stainless steel plate material (Ra is 0.7 μm) blasted in the same manner as in Example 3-1, in the same manner as in Example 1-5. Thus, a sample of Example 3-5 was obtained. Further, electroless Cu plating having a film thickness of about 25 μm is formed on a stainless steel plate material (Ra is 0.7 μm) blasted in the same manner as in Example 3-1, in the same manner as in Example 1-6. A sample of Example 3-6 was obtained.

  About each sample of Example 1-1 to Example 1-6, Example 2-1 to Example 2-6, and Example 3-1 to Example 3-6 prepared as described above, Pull the edge of the surface of the stainless steel substrate on which the metal plating film is formed with one finger of the tester in the direction away from the substrate body (generally in the direction of the arrow shown in FIG. 2). Whether or not peeled off from the stainless steel base body. As a result, for each sample of Example 1-1 to Example 1-6, Example 2-1 to Example 2-6, and Example 3-1 to Example 3-6, the metal plating film was formed into a sheet shape. It was possible to peel off. In this specification, “peeling into a sheet” means that the metal plating film is formed on the surface of the substrate without leaving a part of the film on the substrate. The state peeled in the sheet form, maintaining the integrity as the film. FIG. 2 schematically shows a state in which the metal plating film 22 is peeled from the base material 21 in a sheet shape. For the samples of Example 3-1 to Example 3-6, the surface roughness Ra is 0.08 μm at the end of the stainless steel substrate of the sample (the position corresponding to the position of the mirror surface portion 23 in FIG. 2). A smoothed part was created, and the part was picked with a finger and peeled off.

  Thus, the surface layer is provided with a passive film mainly composed of chromium hydrated oxyoxide and having a film thickness of 1 nm or more, and the surface roughness is 0.08 μm, 0.2 μm, and 0.7 μm in arithmetic mean roughness Ra. Electrolytic Ni plating film, electrolytic Sn plating film, electrolytic Cu plating film, electrolytic Ag plating film, electroless Ni-P plating film, and electroless Cu plating through the passive film on the surface of stainless steel It was confirmed that when at least one metal plating film selected from the group consisting of the films was prepared, the metal plating film could be easily peeled off from the stainless steel substrate. As the surface roughness of the base material is smaller, the metal plating film is more easily peeled off. From the above experimental results, the surface roughness of the surface of the stainless steel base material with an arithmetic average roughness Ra of 0.7 μm or less is as follows. It was confirmed that the metal plating film can be easily peeled from the substrate by forming the metal plating film through a passive film.

Example 4-1 to Example 4-2
A passive film mainly composed of titanium oxide of 1 nm or more is formed on the surface layer, and the surface roughness is made of a titanium alloy (TP340) with an arithmetic average roughness Ra of 0.38 μm, 10 cm long, 4 cm wide, thickness A 0.5 mm plate was prepared. And this board | plate material was blasted and surface roughness was set to 0.28 micrometer by arithmetic mean roughness Ra. Next, the surface layer of the plate was washed with diluted neutral detergent. An electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of this plate material by using a sulfamic acid Ni plating solution manufactured by Nippon Kagaku Sangyo Co., Ltd. according to a conventional method. The sample thus obtained was named Example 4-1. Further, electrolytic Cu plating having a film thickness of about 25 μm was formed on the same titanium alloy plate (Ra: 0.28 μm) as in Example 4-1 by the same method as in Example 1-2, and Example 4-2. Samples were obtained.

Example 5-1 to Example 5-2
As in Example 4-1, a passive film mainly composed of titanium oxide of 1 nm or more is formed on the surface layer, and the surface roughness is made of a titanium alloy (TP340) having an arithmetic average roughness Ra of 0.38 μm. A plate material having a length of 10 cm, a width of 4 cm, and a thickness of 0.5 mm was prepared. Next, the surface layer of the plate was washed with diluted neutral detergent. Then, an electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the plate material in the same manner as in Example 1-1. The sample thus obtained was named Example 5-1. Further, an electrolytic Cu plating having a film thickness of about 25 μm was formed on a titanium alloy plate material (Ra is 0.38 μm) blasted in the same manner as in Example 5-1 and performed. The sample of Example 5-2 was obtained.

Example 6-1 to Example 6-2
As in Example 5-1, a passive film mainly composed of titanium oxide of 1 nm or more is formed on the surface layer, and the surface roughness is made of a titanium alloy (TP340) having an arithmetic average roughness Ra of 0.38 μm. A plate material having a length of 10 cm, a width of 4 cm, and a thickness of 0.5 mm was prepared. And this board | plate material was blasted and the surface roughness was 0.7 micrometer by arithmetic mean roughness Ra. Next, the surface layer of the plate was washed with diluted neutral detergent. Then, an electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the plate material in the same manner as in Example 1-1. The sample thus obtained was named Example 6-1. An electrolytic Cu plating having a film thickness of about 25 μm was formed on a titanium alloy plate material (Ra: 0.7 μm) blasted as in Example 6-1 by the same method as in Example 1-2. -2 sample was obtained.

  About each sample of Example 4-1 to Example 4-2, Example 5-1 to Example 5-2, and Example 6-1 to Example 6-2 prepared as described above, With the finger of one hand of the tester, pull the edge of the surface of the titanium alloy substrate on which each metal plating film is formed in the direction away from the substrate body (generally in the direction of the arrow shown in FIG. 2). It was confirmed whether or not peeled off from the titanium alloy base body. As a result, for each sample of Example 4-1 to Example 4-2, Example 5-1 to Example 5-2, and Example 6-1 to Example 6-2, the metal plating film was formed into a sheet shape. It was possible to peel off. In addition, for the samples of Example 6-1 to Example 6-2, the surface roughness Ra is 0.08 μm at the end of the stainless steel substrate of the sample (the position corresponding to the position of the mirror surface portion 23 in FIG. 2). A smoothed part was created, and the part was picked with a finger and peeled off.

  In this way, a titanium alloy mainly composed of titanium oxide and having a passive film having a thickness of 1 nm or more on the surface, titanium alloys whose surface roughness is 0.28 μm, 0.38 μm, and 0.7 μm in arithmetic mean roughness Ra. When at least one metal plating film selected from the group consisting of an electrolytic Ni plating film and an electrolytic Cu plating film is formed on the surface of the substrate via the passive film, the metal plating film is formed of the titanium alloy. It was confirmed that it can be easily peeled off from the substrate. As the surface roughness of the base material is small, the metal plating film is considered to be easily peeled off. From the above experimental results, the surface roughness of the surface of the titanium alloy base material having an arithmetic average roughness Ra of 0.7 μm or less It was confirmed that the metal plating film can be easily peeled from the substrate by forming the metal plating film through a passive film.

Example 7-1
A passive film mainly composed of aluminum oxide and aluminum hydroxide of 1 nm or more is formed on the surface layer, and the surface roughness is made of an A2000 series aluminum alloy having an arithmetic average roughness Ra of 0.3 μm, 10 cm in length, A plate material having a width of 4 cm and a thickness of 0.6 mm was prepared. Next, the surface layer of the plate was washed with diluted neutral detergent. An electrolytic Cu plating film having a film thickness of about 25 μm was formed on the surface of this plate material in the same manner as in Example 1-2. The sample thus obtained was named Example 7-1.

  For the sample of Example 7-1 prepared as described above, the edge of the surface on which the metal plating film of the aluminum alloy base material is formed is separated from the base material body with the finger of one palm of the tester. It was pulled (generally in the direction of the arrow shown in FIG. 2) to confirm whether or not the metal plating film was peeled off from the aluminum alloy base body. As a result, for the sample of Example 7-1, the metal plating film could be peeled off in a sheet form. As described above, the surface of the aluminum alloy substrate having a surface roughness of 0.3 μm in terms of arithmetic mean roughness Ra is provided on the surface layer with a passive film mainly composed of aluminum oxide and aluminum hydroxide and having a film thickness of 1 nm or more. In addition, it was confirmed that when an electrolytic Cu plating film was prepared via the passive film, the electrolytic Cu plating film could be easily peeled from the aluminum alloy substrate. As the surface roughness of the base material is small, the metal plating film is considered to be more easily peeled off. From the above experimental results, the surface roughness of the surface of the aluminum alloy base material with an arithmetic average roughness Ra of 0.3 μm or less is as follows. It was confirmed that the electrolytic Cu plating film can be easily peeled from the substrate by creating the electrolytic Cu plating film through the passive film.

Example 8-1 to Example 8-2 A base material having an electroless Ni plating film formed on the surface of a stainless steel (SUS304) plate having a length of 10 cm, a width of 4 cm, and a thickness of 0.5 mm was prepared. The surface roughness of the substrate (electroless nickel plating film) was 0.6 μm in terms of arithmetic average roughness Ra. Next, the substrate was heated at 400 ° C. for 1 hour. On the surface layer of the substrate after heating (surface layer of electroless nickel plating film), a passive film with a thickness of 1 nm or more mainly composed of nickel oxide is formed. The hardness of the substrate surface after heating is as follows: The Vickers hardness Hv was 900. An electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the heated substrate in the same manner as in Example 1-1. The sample thus obtained was named Example 8-1.

Comparative Example 1
A base material having an electroless Ni plating film formed on the surface of a stainless steel (SUS304) plate having a length of 10 cm, a width of 4 cm, and a thickness of 0.5 mm was prepared. The surface roughness of this substrate was 0.13 μm in terms of arithmetic average roughness Ra. Next, an electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the substrate in the same manner as in Example 1-1. The sample thus obtained was designated as Comparative Example 1.

  For the samples of Example 8-1 and Comparative Example 1 prepared as described above, the edge of the surface on which the metal plating film of the base material was formed was removed from the base material body with the finger of one palm of the tester. Pulling in a direction away (generally in the direction of the arrow shown in FIG. 2), it was confirmed whether or not the electrolytic Ni plating film was peeled off from the substrate body. As a result, for the sample of Example 8-1, the electrolytic Ni plating film could be peeled off in a sheet form. On the other hand, when the electrolytic Ni plating film was peeled off, a part of the sample of Comparative Example 1 remained on the substrate surface and could not be peeled off into a sheet shape. As described above, the surface layer of the passive film mainly composed of nickel oxide and having a film thickness of 1 nm or more is provided, and the surface roughness of the base material is provided with an electroless Ni plating film having an arithmetic average roughness Ra of 0.6 μm. When an electrolytic Ni plating film was formed on the surface via the passive film, it was confirmed that the electrolytic Ni plating film can be easily peeled from the substrate. As the surface roughness of the base material is smaller, it is considered that the metal plating film is more easily peeled off. From the above experimental results, an electroless Ni plating film having an arithmetic average roughness Ra of 0.6 μm or less is provided. It was confirmed that the electrolytic Ni plating film was easily peeled from the base material on which the electroless Ni plating film was formed by preparing an electrolytic Ni plating film on the surface of the base material through a passive film.

Comparative Example 2-1 to Comparative Example 2-4
A plate material having a surface roughness of arithmetic average roughness Ra of 0.65 μm of iron (SPCC) and having a length of 10 cm, a width of 4 cm and a thickness of 0.5 mm was prepared. Then, an electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the plate material in the same manner as in Example 1-1. The sample thus obtained was designated as Comparative Example 2-1. Further, electrolytic Cu plating having a film thickness of about 25 μm was formed on the same iron plate material (Ra is 0.65 μm) as in Comparative Example 2-1 by the same method as in Example 1-2. A sample was obtained. In addition, electrolytic Sn plating having a film thickness of about 25 μm was formed on the same iron plate material (Ra is 0.65 μm) as in Comparative Example 2-1 by the same method as in Example 1-3. A sample was obtained. Further, electrolytic Ag plating having a film thickness of about 25 μm was formed on the same iron plate material (Ra is 0.65 μm) as in Comparative Example 2-1 by the same method as in Example 1-4, and Comparative Example 2-4. A sample was obtained.

Comparative Example 3-1 to Comparative Example 3-4
A plate material having a surface roughness of arithmetic mean roughness Ra of 0.05 μm of iron (SPCC) and having a length of 10 cm, a width of 4 cm, and a thickness of 0.5 mm was prepared. Then, an electrolytic Ni plating film having a film thickness of about 25 μm was formed on the surface of the plate material in the same manner as in Example 1-1. The sample thus obtained was designated as Comparative Example 3-1. Further, electrolytic Cu plating having a film thickness of about 25 μm was formed on the same iron plate material (Ra is 0.05 μm) as in Comparative Example 3-1 by the same method as in Example 1-2, and Comparative Example 3-2. A sample was obtained. In addition, electrolytic Sn plating having a film thickness of about 25 μm was formed on the same iron plate material (Ra is 0.65 μm) as in Comparative Example 3-1 by the same method as in Example 1-3, and Comparative Example 3-3. A sample was obtained. Further, electrolytic Ag plating having a film thickness of about 25 μm was formed on the same iron plate material (Ra is 0.65 μm) as in Comparative Example 3-1 by the same method as in Example 1-4, and Comparative Example 3-4 A sample was obtained.

  About each sample of Comparative Example 2-1 to Comparative Example 2-4 and Comparative Example 3-1 to Comparative Example 3-4 prepared as described above, the tester's palm finger is used to form the base metal. The edge of the surface on which the plating film was formed was pulled away from the base body (generally in the direction of the arrow shown in FIG. 2) to confirm whether each metal plating film was peeled off from the base body. As a result, a part of the samples of Comparative Example 2-1 to Comparative Example 2-4 and Comparative Example 3-1 to Comparative Example 3-4 remained on the substrate surface when the electrolytic Ni plating film was peeled off. ， It could not be peeled into a sheet. In this way, it was confirmed that a passive film was difficult to form, and even if a metal plating film was formed on an iron substrate, it could not be peeled into a sheet.

As described below, a deposition plate is produced according to an embodiment of the present invention, a film formation process is performed using a vacuum chamber in which the produced deposition plate is installed, and a metal plating film is formed from the deposition plate after the film formation process. Whether or not can be peeled was confirmed. First, electrolysis with a thickness of 25 μm is carried out on the surface of a disk type stainless steel (SUS304) having a diameter of 110 mm, a thickness of 1 mm, and an arithmetic average roughness Ra of 0.08 μm via a passive film mainly composed of chromium hydrated oxyoxide. A test piece of an adhesion-preventing plate on which a Ni plating film was formed was prepared. Next, this test piece was placed in a vacuum chamber for a high-pressure DC micropulse plasma CVD apparatus. In addition, a cylindrical stainless steel (SUS304) work (diameter: 110 mm, height: 300 m) serving as a counter electrode of the cylindrical stainless steel deposition plate is prepared, and the work has a circular bottom at the bottom. It arrange | positioned in the position which opposes one circular surface of the test piece of an adhesion prevention board. In such an arrangement, a voltage was applied so that the workpiece side was the anode, and the test piece of the deposition plate was the cathode, and an amorphous carbon film was formed on the workpiece. The time required for the vacuum chamber to be evacuated to 3 × 10 ⁻⁴ Pa was almost the same as in the case of a normal deposition preventing plate.

  Next, argon gas plasma was introduced into the vacuum chamber, and the workpiece was cleaned for about 1 minute. Cleaning with argon gas plasma was performed under the conditions of an argon gas flow rate of 30 SCCM, a gas pressure of 2 Pa, an applied voltage of −2 kV, a pulse frequency of 10 kHz, and a pulse width of 10 μs. After cleaning, the argon gas is evacuated, and then acetylene at a flow rate of 30 SCCM is introduced into the vacuum chamber so that the gas pressure in the reaction vessel is 2 Pa, and the maximum applied voltage is −6 kV, the pulse frequency is 10 kHz, and the pulse width is 10 μs. Under conditions, an amorphous carbon film was formed on the workpiece for 30 minutes. Next, nitrogen gas was used as a leak gas, and the vacuum chamber was returned to normal pressure (atmospheric pressure) over 25 minutes. Thereafter, the vacuum chamber was opened, and the deposition plate was taken out from the vacuum chamber.

  Next, it was visually confirmed that the carbon component diffused in the process of forming the amorphous carbon film was adhered on the Ni plating film of the deposition plate taken out from the vacuum chamber. Next, when the edge of the surface of the deposition preventive plate was picked with a finger and pulled away from the surface of the deposition preventive plate, the Ni plating film on the surface of the deposition preventing plate remained carbon component adhered to the Ni plating coating. The sheet could be peeled off in the state.

  Next, an electrolytic Ni plating film was formed on the deposition plate from which the Ni plating film was peeled and the stainless steel was exposed. Next, when the edge of the surface of the adhesion-preventing plate was picked with a finger and pulled away from the surface of the adhesion-preventing plate, the Ni plating film on the surface of the adhesion-preventing plate could be peeled off into a sheet.

DESCRIPTION OF SYMBOLS 10: Vacuum apparatus 11: Vacuum chamber 11a: Inner wall 12: Board | substrate fixing jig 13: Board | substrate 14: Target 15: Target installation part 16: Power supply part 17: Deposit board 18: Pressure control means 18a: Gas pipe 18b: Main valve 19: Gas supply part 19a: Gas pipe 19b: Gas supply valve 20: Vacuum chamber components 21: Base material 21a: Base material body 21b: Passive film 22: Metal plating film 23: Mirror surface part

Claims (4)

A surface layer of a passive film mainly composed of chromium hydrated oxyoxide with a film thickness of 1 nm or more, and a surface roughness of 0.7 μm or less in terms of arithmetic mean roughness Ra;
Formed on the stainless steel substrate through the passive film, electrolytic Ni plating film, electrolytic Sn plating film, electrolytic Cu plating film, electrolytic Ag plating film, electroless Ni-P plating film, and electroless Cu plating film At least one metal plating film selected from the group consisting of:
A vacuum chamber component comprising: A titanium alloy base material having a surface layer of a passive film mainly composed of titanium oxide and having a film thickness of 1 nm or more, the surface roughness of which is 0.7 μm or less in arithmetic mean roughness Ra;
At least one metal plating film formed on the titanium alloy substrate through the passive film and selected from the group consisting of an electrolytic Ni plating film and an electrolytic Cu plating film;
A vacuum chamber component comprising: A substrate,
An electroless Ni plating film formed on the substrate, the surface layer having a passive film having a film thickness of 1 nm or more mainly composed of nickel oxide, and having a Vickers hardness Hv of 900 or more And an Ni plating film whose surface roughness is an arithmetic average roughness Ra of 0.6 μm or less,
An electrolytic Ni plating film formed on the Ni plating film via the passive film;
A vacuum chamber component comprising: An aluminum alloy substrate having a surface layer of a passive film having a thickness of 1 nm or more mainly composed of aluminum oxide and / or aluminum hydroxide, the surface roughness of which is an arithmetic average roughness Ra of 0.3 μm or less;
An electrolytic Cu plating film formed on the aluminum alloy substrate via the passive film;
A vacuum chamber component comprising:

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