Aluminum component for semiconductor manufacturing equipment and method for manufacturing the same

JP7914115B2Active Publication Date: 2026-09-01UACJ CORP
View PDF 9 Cites 0 Cited by

Patent Information

Application Number
JP2023545680
Authority / Receiving Office
JP · JP
Patent Type
Patents
Current Assignee / Owner
Priority Date
2021-09-06
Filing Date
2022-09-01
Publication Date
2026-09-01
Estimated Expiration
2042-09-01

AI Technical Summary

Benefits of technology

【0009】 前記半導体製造装置用アルミニウム部材(以下、「アルミニウム部材」という。)の母材上には陽極酸化皮膜が設けられている。また、陽極酸化皮膜中には、前記特定の異質粒子が存在している。このような異質粒子は、前記アルミニウム部材の温度が上昇し、陽極酸化皮膜にクラックが発生した場合に、クラックを陽極酸化皮膜の厚み方向とは異なる方向に誘導することができる。それ故、前記アルミニウム部材の陽極酸化皮膜にクラックが発生した場合であっても、異質粒子によってクラックが陽極酸化皮膜の厚み方向とは異なる方向に進展しやすい。その結果、クラックの進展が陽極酸化皮膜の内部で停止し、陽極酸化皮膜と母材との界面まで到達しにくくなる。

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure 0007914115000002
    Figure 0007914115000002
  • Figure 0007914115000003
    Figure 0007914115000003
  • Figure 0007914115000004
    Figure 0007914115000004
Patent Text Reader

Abstract

This aluminum member (1) for semiconductor manufacturing devices comprises: a base material (2) comprising aluminum or an aluminum alloy; and an anodic oxidation coating film (3) formed on the base material (2). Heterogeneous particles (31), which have a long-axis diameter from 0.1-15 µm, both inclusive, and contain a metal atom other than the Al atom, are present in the anodic oxidation coating film (3). The method for producing the aluminum member (1) for semiconductor manufacturing devices comprises an anodic oxidation treatment step for forming a heterogeneous particle (31)-containing anodic oxidation coating film (3) on a base material (2) by subjecting a base material (2) that has second-phase particles in an Al matrix to an anodic oxidation treatment using an acidic electrolyte solution.
Need to check novelty before this filing date? Find Prior Art

Description

[Technical Field]

[0001] The present invention relates to an aluminum component for semiconductor manufacturing equipment and a method for manufacturing the same. [Background technology]

[0002] In semiconductor manufacturing equipment such as CVD (chemical vapor deposition) equipment, PVD (physical vapor deposition) equipment, and dry etching equipment, the temperature of components such as chambers rises while the semiconductor placed inside the chamber is being processed. Furthermore, if impurities are released from the components inside the chamber while the semiconductor is being processed, it may cause defects in the semiconductor. To suppress the occurrence of these problems, aluminum alloys, which have high heat resistance and low impurity release, are used in the components of semiconductor manufacturing equipment.

[0003] For example, Patent Document 1 describes an Al alloy for semiconductor manufacturing equipment that has excellent gas corrosion resistance and plasma corrosion resistance, as well as excellent anodized film formation properties and heat resistance, characterized by containing Mn: 0.3~1.5% (mass%, the same applies hereinafter), Cu: 0.3~1.5%, Fe: 0.1~1.0% as alloy components, with the remainder being Al and unavoidable impurities, and having an average crystal grain size of 50 μm or less. The Al alloy for semiconductor manufacturing equipment described in Patent Document 1 is used as a material for semiconductor manufacturing equipment after an anodized film is formed on its surface. [Prior art documents] [Patent Documents]

[0004] [Patent Document 1] Japanese Patent Application Publication No. 11-043734 [Overview of the project] [Problems that the invention aims to solve]

[0005] However, the thermal expansion coefficients of the aluminum alloy and the anodized coating are different. Therefore, if the temperature of a semiconductor manufacturing equipment material with an anodized coating on an aluminum alloy rises, cracks may occur in the anodized coating. If these cracks propagate along the thickness direction of the anodized coating and reach the interface between the aluminum alloy and the anodized coating, the aluminum alloy may be exposed. As a result, this may lead to a decrease in corrosion resistance and an increase in outgassing.

[0006] This invention has been made in view of the above background, and aims to provide an aluminum component for semiconductor manufacturing equipment and a method for manufacturing the same that can easily maintain the state in which the base material is covered by the anodic oxide film even when cracks occur in the anodic oxide film. [Means for solving the problem]

[0007] One aspect of the present invention comprises a base material made of aluminum or an aluminum alloy, Having an anodic oxide film formed on the base material, The aluminum component for semiconductor manufacturing equipment contains heterogeneous particles in the anodic oxide film, which have a major axis diameter of 0.1 μm or more and 15 μm or less and include metal atoms other than Al (aluminum) atoms.

[0008] Another aspect of the present invention is a method for manufacturing an aluminum component for a semiconductor manufacturing apparatus according to the above aspect, The present invention relates to a method for manufacturing aluminum components for semiconductor manufacturing equipment, comprising an anodic oxidation step in which a base material having second-phase particles in an Al matrix is ​​subjected to an anodic oxidation treatment using an acidic electrolyte to form an anodic oxide film containing the heterogeneous particles on the base material. [Effects of the Invention]

[0009] An anodic oxide film is provided on the base material of the aluminum component for semiconductor manufacturing equipment (hereinafter referred to as "aluminum component"). Furthermore, specific heterogeneous particles are present in the anodic oxide film. When the temperature of the aluminum component rises and cracks occur in the anodic oxide film, these heterogeneous particles can induce the cracks in a direction different from the thickness direction of the anodic oxide film. Therefore, even if cracks occur in the anodic oxide film of the aluminum component, the heterogeneous particles make it easier for the cracks to propagate in a direction different from the thickness direction of the anodic oxide film. As a result, the crack propagation stops inside the anodic oxide film and is less likely to reach the interface between the anodic oxide film and the base material.

[0010] Therefore, in the aforementioned aluminum component, even if cracks occur in the anodic oxide film, the state in which the anodic oxide film covers the base material is easily maintained.

[0011] Furthermore, the method for manufacturing the aluminum member includes an anodic oxidation step in which a base material containing second-phase particles is subjected to an anodic oxidation treatment using an acidic electrolyte. In the anodic oxidation step, as the anodic oxide film grows, at least a portion of the second-phase particles in the base material are incorporated into the anodic oxide film. This makes it possible to easily form an anodic oxide film containing the heterogeneous particles on the base material.

[0012] As described above, according to the above embodiment, it is possible to provide an aluminum component for semiconductor manufacturing equipment and a method for manufacturing the same that can easily maintain the state in which the base material is covered by the anodic oxide film even if cracks occur in the anodic oxide film. [Brief explanation of the drawing]

[0013] [Figure 1] Figure 1 is a partial cross-sectional view showing the main parts of an aluminum component for semiconductor manufacturing equipment in an embodiment. [Figure 2] Figure 2 shows a secondary electron image of the cross-section of the test material S3 after heating in the example. [Figure 3]Figure 3 shows a secondary electron image of the cross-section of the test material R1 after heating in the example. [Modes for carrying out the invention]

[0014] (Aluminum components for semiconductor manufacturing equipment) The base material of the aluminum component can be appropriately selected from the group consisting of aluminum and aluminum alloys, depending on the application of the aluminum component. For example, when trying to reduce outgassing from the aluminum component, it is preferable that the base material is made of 1000 series aluminum or 3000 series aluminum alloy. As a 3000 series aluminum alloy, for example, an aluminum alloy can be used that contains Mn (manganese): 1.0% to 1.5% by mass, and also contains one or more elements selected from the group consisting of Si (silicon), Fe (iron), Cu (copper), Mg, Cr (chromium), Zn (zinc), and Ti (titanium) as optional components, with the remainder being Al and unavoidable impurities.

[0015] Furthermore, when aiming to increase the strength of the aluminum component, it is preferable that the base material be composed of a 5000 series aluminum alloy or a 6000 series aluminum alloy. As a 5000 series aluminum alloy, for example, an aluminum alloy can be used that contains Mg (magnesium): 0.5% to 5.0% by mass, and one or more elements selected from the group consisting of Si, Fe, Cu, Mn, Cr, Zn, and Ti as optional components, with the remainder being Al and unavoidable impurities. As a 6000 series aluminum alloy, for example, an aluminum alloy can be used that contains Mg: 0.3% to 1.5% by mass, Si: 0.2% to 1.2% by mass, and one or more elements selected from the group consisting of Fe, Cu, Mn, Cr, Zn, and Ti as optional components, with the remainder being Al and unavoidable impurities.

[0016] The base material of the aluminum member may optionally contain second-phase particles. As described later, when anodizing treatment is performed on a base material containing second-phase particles, at least a part of the second-phase particles are incorporated into the anodized film and become heterogeneous particles. As a result, the aluminum member can be easily produced.

[0017] The second-phase particles contained in the base material have various compositions depending on the material of the base material. For example, a base material made of 1000-series aluminum contains second-phase particles such as Al-Fe intermetallic compounds and Al-Fe-Si intermetallic compounds. A base material made of 3000-series aluminum alloy contains second-phase particles such as Al-Mn intermetallic compounds, Al-Mn-Si intermetallic compounds, Al-Fe-Si intermetallic compounds, and Al-Mn-Fe-Si intermetallic compounds. A base material made of 5000-series aluminum alloy contains second-phase particles such as Al-Mg intermetallic compounds. A base material made of 6000-series aluminum alloy contains second-phase particles such as Al-Mg intermetallic compounds, Al-Mg-Si intermetallic compounds, Si, and Mg₂Si.

[0018] An anodized film is provided on the base material. The anodized film is mainly composed of an oxide of aluminum. The anodized film may be, for example, a porous anodized film having a large number of pores, or a barrier-type anodized film having no pores. The thickness of the anodized film is not particularly limited, and can be appropriately set, for example, within a range of 0.1 µm or more and 100 µm or less.

[0019] The anodic oxide film contains heterogeneous particles that include metal atoms other than Al atoms and have a major axis diameter of 0.1 μm to 15 μm. Heterogeneous particles with a major axis diameter within the specified range can guide the direction of crack propagation in a direction inclined with respect to the thickness direction of the anodic oxide film when cracks occur in the anodic oxide film. Therefore, when cracks occur in the anodic oxide film, the cracks tend to propagate in a direction inclined with respect to the thickness direction of the anodic oxide film. Cracks propagating in a direction inclined with respect to the thickness direction of the anodic oxide film can have a shallower crack tip depth from the surface of the anodic oxide film, even if they are the same length as cracks propagating along the thickness direction of the anodic oxide film. Furthermore, by propagating cracks in a direction inclined with respect to the thickness direction of the anodic oxide film, the length of the crack can be increased, and the stress generated within the anodic oxide film due to the difference in thermal expansion can be reduced. As a result, the tip of the crack is more likely to remain inside the anodic oxide film, making it less likely for the crack to reach the interface between the anodic oxide film and the base material.

[0020] The major axis diameter of foreign particles present in an anodized film is measured by the following method. First, an aluminum component is cut at an arbitrary cross-section, and a sample is taken. After embedding this sample in resin, the cross-section of the sample is mirror-polished to expose the cross-section of the anodized film. Next, the cross-section of the anodized film is observed using an electron microscope, and an electron microscope image containing the foreign particles is obtained. A rectangle is drawn circumscribing the foreign particles present in this electron microscope image, and the length of the longer side of the rectangle is taken as the major axis diameter of the foreign particles.

[0021] Furthermore, the anodic oxide film may contain foreign particles with a major axis diameter of less than 0.1 μm, or foreign particles with a major axis diameter exceeding 15 μm. However, foreign particles with a major axis diameter of less than 0.1 μm have a lower effect in guiding the direction of crack propagation compared to particles with a major axis diameter within the specified range. Also, if the number of foreign particles with a major axis diameter exceeding 15 μm becomes excessively large, the number of foreign particles contained in the anodic oxide film will decrease, which may lead to a reduction in the effect of guiding the direction of crack propagation.

[0022] From the viewpoint of more effectively suppressing crack propagation in the thickness direction of the anodized film, it is preferable that the average value of the long axis diameter of the foreign particles contained in the anodized film is 0.1 μm or more and 15 μm or less, more preferably 0.5 μm or more and 10 μm or less, and even more preferably 1.0 μm or more and 5.0 μm or less. If the average value of the long axis diameter of the foreign particles is excessively small, the proportion of foreign particles with a long axis diameter of less than 0.1 μm contained in the anodized film will increase, which may lead to a decrease in the effect of inducing the direction of crack propagation. Also, if the average value of the long axis diameter of the foreign particles is excessively large, the proportion of foreign particles with a long axis diameter exceeding 15 μm contained in the anodized film will increase, which may lead to a decrease in the number of foreign particles contained in the anodized film.

[0023] Surface area of ​​anodic oxide film: 1 mm² 2 Preferably, the number of foreign particles with a major axis diameter of 0.1 μm to 15 μm contained in each particle is 1600 or more. In this case, the spacing between foreign particles within the anodic oxide film can be sufficiently short. Therefore, even if a crack occurs in any part of the anodic oxide film, the likelihood of foreign particles with the major axis diameter within the specified range being present near the crack can be increased. Accordingly, the surface area of ​​the anodic oxide film is 1 mm². 2 By keeping the number of foreign particles contained in each sample within the specified range, the effect of suppressing the exposure of the base material can be further enhanced, and the state in which the base material is covered by the anodic oxide film can be more easily maintained.

[0024] From a similar viewpoint, it is preferable that the distance between the foreign particle and the foreign particle closest to it in any cross-section of the aluminum member be 25 μm or less, more preferably 20 μm or less, and even more preferably 15 μm or less.

[0025] The composition of the heterogeneous particles is not particularly limited, but the heterogeneous particles may contain Si atoms. Examples of such heterogeneous particles include elemental Si, Mg2Si, and Al-Mn-Fe-Si intermetallic compounds. When an aluminum component is manufactured by the manufacturing method of the above embodiment, second-phase particles in the base material that did not dissolve during the anodizing treatment are incorporated into the anodized film and become heterogeneous particles. Therefore, the heterogeneous particles often have the same composition as the second-phase particles contained in the base material, or a composition derived from the second-phase particles. For example, in the case of Mg2Si in the base material, Mg atoms dissolve and Si atoms are incorporated into the film during the anodizing treatment, so fine heterogeneous particles rich in Si atoms can be dispersed in the film.

[0026] The thickness of the aluminum component for semiconductor manufacturing equipment is not particularly limited. For example, the aluminum component for semiconductor manufacturing equipment may be a thick plate with a thickness of 6 mm or more. The occurrence of cracks in the anodic oxide film is thought to be caused by the difference in thermal expansion between the anodic oxide film and the base material. When the thickness of the base material increases, the stress caused by the difference in thermal expansion increases, making it easier for cracks to occur in the anodic oxide film. In contrast, since the anodic oxide film of the aluminum component contains heterogeneous particles having a major axis diameter within the specific range, as mentioned above, even if cracks occur in the anodic oxide film, the direction of crack propagation can be guided in a direction different from the thickness direction of the anodic oxide film. Therefore, even when the aluminum component for semiconductor manufacturing equipment is thick, the effect of the heterogeneous particles makes it easy to maintain a state in which the base material is covered with the anodic oxide film.

[0027] The aforementioned aluminum member is used as a component of semiconductor manufacturing equipment. More specifically, the aluminum member is used, for example, in chambers and components placed inside chambers in film deposition equipment such as CVD equipment and PVD equipment, and etching equipment such as dry etching equipment.

[0028] (Method for manufacturing aluminum components for semiconductor manufacturing equipment) The method for manufacturing the aluminum member is as follows: The method includes an anodic oxidation step in which a base material having second-phase particles in an Al matrix is ​​subjected to an anodic oxidation treatment using an acidic electrolyte to form an anodic oxide film containing the heterogeneous particles on the base material.

[0029] In the anodizing process, an acidic electrolyte is used to anodize a base material containing second-phase particles. When an acidic electrolyte is used in the anodizing process, the dissolution reaction of the base material and aluminum oxide and the growth reaction of the aluminum oxide proceed in parallel during the anodizing process. As a result, a porous type anodic oxide film with numerous pores can be formed on the base material. Furthermore, as the anodic oxide film grows, second-phase particles in the base material that did not dissolve in the electrolyte are incorporated into the anodic oxide film, becoming heterogeneous particles. Therefore, by applying the aforementioned anodizing process to the base material, an anodic oxide film containing heterogeneous particles can be formed on the base material.

[0030] The electrolyte used in the anodizing process may contain one or more acids selected from the group consisting of organic acids such as oxalic acid, malonic acid, and tartaric acid, and inorganic acids such as sulfuric acid and phosphoric acid. From the viewpoint of further improving the heat resistance of the anodized film, it is preferable that the electrolyte contains one or two acids from among oxalic acid and sulfuric acid.

[0031] In the anodizing process, an anodic oxide film can be formed on the surface of the base material by immersing the base material and the counter electrode in an electrolyte solution and passing a direct current between them. The current density of the direct current in the anodizing process is 100 A / m². 2 More than 600A / m 2 Preferably, the current density of the DC current in the anodizing process is 100 A / m². 2 The above is a futuristic 200 A / m 2 By doing so, the growth rate of the anodic oxide film can be accelerated, and the productivity of aluminum components can be improved. In addition, the current density of the DC current in the anodic oxidation process can be set to 600 A / m². 2For a more precise rate, use 500 A / m. 2 By doing the following, it is possible to grow a uniform anodic oxide film on the base material and avoid burning of the base material and unevenness in the anodic oxide film.

[0032] In the anodizing process, the electrolyte temperature is preferably between 263K and 303K. By setting the electrolyte temperature to 263K or higher, more preferably 273K or higher, the solubility of the electrolyte can be appropriately increased, and the concentration of the electrolyte in the electrolyte can be sufficiently high. Furthermore, by setting the electrolyte temperature to 303K or lower, more preferably 293K or lower, an excessive increase in the dissolving power of the electrolyte can be avoided, and the growth rate of the anodized film can be accelerated.

[0033] The base material used in the anodizing process may be manufactured by any method. For example, the method for manufacturing the aluminum member further includes a casting step of producing an ingot made of aluminum or an aluminum alloy, A homogenization process is performed by holding the ingot at a temperature of 500°C to 560°C for 5 to 10 hours to perform a homogenization treatment. The process may also include a hot rolling step in which the homogenized ingot is subjected to hot rolling at a temperature of 500°C to 560°C to produce the base material.

[0034] As a casting method in the casting process, DC casting can be used, for example. The thickness of the ingot obtained in the casting process is not particularly limited, but the ingot may have a thickness of, for example, 600 mm or more.

[0035] In the homogenization process, the ingot obtained in the casting process is subjected to homogenization by holding it at a temperature of 500°C to 560°C for 5 to 10 hours. By setting the holding temperature and holding time in the homogenization process to the aforementioned specific ranges, the structure of the ingot can be sufficiently homogenized. Then, by subjecting such an ingot to hot rolling, a base material containing the desired second-phase particles can be obtained.

[0036] In the hot rolling process, the homogenized ingot is hot-rolled at a temperature between 500°C and 560°C. This allows the base material to be obtained. If the starting temperature for hot rolling is too low, the deformation resistance of the ingot will increase, which may cause cracking during rolling or lead to a decrease in productivity. On the other hand, if the starting temperature for hot rolling is too high, the ingot may melt locally due to the heat generated during processing during hot rolling.

[0037] In the above manufacturing method, the base material obtained as described above may be subjected directly to the anodizing process. Alternatively, the above manufacturing method may include a heat treatment step, after the hot rolling process and before the anodizing process, in which the base material may be subjected to heat treatment such as annealing as needed.

[0038] Furthermore, the manufacturing method may include a pretreatment step in which the base material is pretreated after the hot rolling step and before the anodizing step. Examples of pretreatment of the base material include degreasing treatments such as alkaline degreasing, and polishing treatments such as mechanical polishing, chemical polishing, and electrolytic polishing. In the pretreatment step, one of the above-mentioned pretreatments may be performed alone depending on the desired properties of the aluminum component, or two or more pretreatments may be performed in appropriate combinations.

[0039] If alkaline degreasing is performed in the pretreatment step, the gloss of the anodic oxide film obtained after anodizing can be reduced, resulting in an aluminum component with a dull appearance. Conversely, if polishing is performed in the pretreatment step, the gloss of the anodic oxide film obtained after anodizing can be increased, resulting in an aluminum component with a glossy appearance. From the viewpoint of further increasing the gloss of the aluminum component, it is preferable to perform electrolytic polishing on the base material in the pretreatment step. [Examples]

[0040] Examples of the aluminum component for semiconductor manufacturing equipment and its manufacturing method are described below. As shown in Figure 1, the aluminum component 1 in this example has a base material 2 made of aluminum or an aluminum alloy and an anodic oxide film 3 formed on the base material 2. The anodic oxide film 3 contains heterogeneous particles 31 having a major axis diameter of 0.1 μm or more and 15 μm or less, and containing metal atoms other than Al atoms.

[0041] The aluminum component 1 in this example can be obtained, for example, by the following method. First, an ingot having a chemical composition represented by one of the alloy symbols A5052, A5083, or A6063 is produced by DC casting (casting process). The thickness of the ingot is, for example, 600 mm. This ingot is subjected to a homogenization treatment by holding it at a temperature of 500°C to 560°C for 5 to 10 hours (homogenization treatment process). After the homogenization treatment process, hot rolling is performed on the ingot while its temperature is between 500°C and 560°C to produce a plate material with a thickness of 300 mm (hot rolling process).

[0042] For sheet metal having the chemical composition represented by alloy symbol A5052, the sheet metal after hot rolling is used as base material 2. This sheet metal is tempered to the temper represented by temper symbol H112. For sheet metal having the chemical composition represented by alloy symbol A5083, the sheet metal is heated and annealed after hot rolling to temper it to the temper represented by temper symbol O. The sheet metal after annealing is then used as base material 2. For sheet metal having the chemical composition represented by alloy symbol A6063, the sheet metal is subjected to solution treatment after hot rolling, followed by artificial aging treatment to temper it to the temper represented by temper symbol T6. The sheet metal after artificial aging treatment is then used as base material 2.

[0043] These three types of base materials 2 are subjected to anodizing treatment under the conditions shown in Table 1 to form an anodic oxide film 3 on the base materials 2. This allows for the production of test materials S1 to S6 shown in Table 1. Note that test material R1 shown in Table 1 is a test material for comparison with test materials S1 to S6. The manufacturing method for test material R1 is the same as that for test materials S1 to S6, except that the holding temperature in the homogenization process is 480°C, the holding time is 4 hours, and the rolling start temperature in the hot rolling process is 450°C.

[0044] Next, we will explain the evaluation method for the structure and heat resistance of the anodic oxide coating 3 in test materials S1 to S6 and test material R1.

[0045] • Method for evaluating the structure of anodic oxide film 3 Each test material is cut, for example, by a plane perpendicular to the rolling direction, to expose the cross-section of the anodic oxide film 3. The cross-section of the anodic oxide film 3 is observed using a field emission scanning secondary electron microscope (FE-SEM) equipped with an energy-dispersive X-ray spectrometer (EDX), and a secondary electron image is obtained, as well as an elemental mapping image of the same field of view as the secondary electron image. Based on the secondary electron image and elemental mapping image, the position and size of the foreign particles 31 present in the anodic oxide film 3 are then determined. For example, the "SU-8230" manufactured by Hitachi High-Technologies Corporation can be used as the FE-SEM. For example, the "QUANTAX FlatQUAD" manufactured by Bruker can be used as the EDX.

[0046] Next, for each heterogeneous particle 31 that appears in the secondary electron image, a rectangle circumscribing the heterogeneous particle 31 is determined. The length of the longer side of this rectangle is defined as the major axis diameter of the heterogeneous particle 31. Table 1 shows the maximum major axis diameter of the heterogeneous particles 31 in each test material. In addition, the distance between each heterogeneous particle 31 that appears in the secondary electron image and the nearest heterogeneous particle 31 is measured. Table 1 shows the maximum distance between heterogeneous particles 31.

[0047] ·Heat resistance The heat resistance evaluation is performed based on the results of polarization measurement of the test material. Specifically, first, a plurality of test pieces for polarization measurement are produced by masking the surface of the test material such that a part of the anodized film 3 on the test material is exposed. The area of the measurement portion of the test piece, that is, the portion where the anodized film 3 is exposed, is 1 cm 2 . Next, some of the plurality of test pieces are heated in the atmosphere at a temperature of 200°C for 8 hours.

[0048] Next, a measurement solution is prepared by adding acetic acid to a 5% NaCl aqueous solution such that the acetic acid concentration is 1 mL / L. The test piece electrically connected to a potentiostat, a counter electrode, and a reference electrode are immersed in this solution, and left standing for a while to stabilize the potential of the measurement portion. For example, an Ag / AgCl electrode can be used as the reference electrode.

[0049] After the potential of the measurement portion is stabilized, a voltage is applied between the test piece and the counter electrode using the potentiostat, and the current density flowing to the measurement portion is measured while sweeping the potential of the measurement portion at a sweep rate of 20 mV / min. The potential sweeping is terminated when the potential of the measurement portion reaches -2000 mV relative to the reference electrode. A polarization curve is obtained through the above steps.

[0050] Next, in the polarization curve, the center of the potential region indicating the hydrogen diffusion limiting current is determined. Then, the current density at the center of the potential region is calculated. The current density obtained in this way can be used as an index of defects in the anodized film on the test piece. A larger current density value indicates that there are more defects in the anodized film 3, and a larger contact area between the base material 2 and the measurement solution.

[0051] Therefore, the ratio of the current density value calculated using the heated test piece to the current density value calculated using the unheated test piece indicates the rate of increase in defects due to heating. The rate of increase in defects due to heating for each test material is shown below.

[0052]

Table 1

[0053] As shown in Table 1, heterogeneous particles 31 having a major axis diameter within the specified range are present in the anodic oxide film 3 of test materials S1 to S6. Therefore, when the temperature of the test material rises and cracks occur in the anodic oxide film 3, the cracks tend to propagate in a direction different from the thickness direction of the anodic oxide film 3 due to the heterogeneous particles 31.

[0054] As an example, a secondary electron image of the cross-section of test material S3 after heating at 200°C for 8 hours is shown. In test material S3, the cracks 4 that have formed on the surface of the anodic oxide film 3 are induced in a direction inclined with respect to the thickness direction of the anodic oxide film 3 due to the presence of heterogeneous particles 31. As the cracks 4 propagate in a direction inclined with respect to the thickness direction of the anodic oxide film 3, the tips of the cracks 4 remain inside the anodic oxide film 3. Although not shown in the figure, in test materials S1-S2 and S4-S6, similar to test material S3, the cracks 4 that have formed on the surface of the anodic oxide film 3 are easily induced in a direction inclined with respect to the thickness direction of the anodic oxide film 3 due to the presence of heterogeneous particles 31.

[0055] As a result of the above, the propagation of crack 4 stops inside the anodic oxide film 3, making it difficult for it to reach the interface between the anodic oxide film 3 and the base material 2.

[0056] On the other hand, the anodized coating 3 of test material R1 does not contain heterogeneous particles 31 having a major axis diameter within the specified range. Therefore, as shown in Figure 3, cracks 4 that occur on the surface of the anodized coating 3 propagate along the thickness direction of the anodized coating 3 and easily reach the interface between the anodized coating 3 and the base material 2. Consequently, the defect increase rate of test material R1 is higher than that of test materials S1 to S6.

[0057] Based on the above results, it can be understood that the aluminum member 1 having heterogeneous particles 31 with a long axis diameter within a specific range inside the anodic oxide film 3 has excellent heat resistance, and even if cracks 4 occur in the anodic oxide film 3, it is easy to maintain the state in which the base material 2 is covered by the anodic oxide film 3.

[0058] Furthermore, the specific embodiments of the aluminum component for semiconductor manufacturing equipment and the method for manufacturing the same according to the present invention are not limited to the embodiments shown in the examples, and the configuration can be appropriately modified without impairing the spirit of the present invention.

Claims

1. A base material made of aluminum or an aluminum alloy, Having an anodic oxide film formed on the base material, An aluminum component for semiconductor manufacturing equipment, wherein the anodic oxide film contains heterogeneous particles having a major axis diameter of 0.1 μm or more and 15 μm or less, and containing metal atoms other than Al atoms.

2. The aluminum member for semiconductor manufacturing apparatus according to claim 1, wherein the average of the major axis diameters of the heterogeneous particles is 0.1 μm or more and 15 μm or less.

3. Surface area of ​​the anodized film: 1 mm² 2 The aluminum component for semiconductor manufacturing apparatus according to claim 1, wherein the number of heterogeneous particles contained in each component is 1,600 or more.

4. The aluminum member for semiconductor manufacturing equipment according to claim 1, wherein the distance between the heterogeneous particle and the heterogeneous particle closest to the said heterogeneous particle in any cross-section of the aluminum member for semiconductor manufacturing equipment is 25 μm or less.

5. The aluminum member for semiconductor manufacturing apparatus according to claim 1, wherein the heterogeneous particles contain Si atoms.

6. The aluminum component for semiconductor manufacturing equipment according to claim 1, wherein the base material is made of a 5000 series aluminum alloy or a 6000 series aluminum alloy.

7. A method for manufacturing an aluminum member for semiconductor manufacturing equipment according to any one of claims 1 to 6, A method for manufacturing aluminum components for semiconductor manufacturing equipment, comprising an anodic oxidation step of applying an anodic oxidation treatment to a base material having second-phase particles in an Al matrix using an acidic electrolyte, thereby forming an anodic oxide film containing the heterogeneous particles on the base material.

8. The method for manufacturing aluminum components for semiconductor manufacturing equipment further includes a casting step of producing an ingot made of aluminum or an aluminum alloy, A homogenization process is performed by holding the ingot at a temperature of 500°C to 560°C for 5 to 10 hours, A method for manufacturing an aluminum component for semiconductor manufacturing equipment according to claim 7, comprising a hot rolling step of hot rolling the ingot that has been subjected to the homogenization treatment at a temperature of 500°C or higher and 560°C or lower to produce the base material.

Citation Information

Patent Citations

  • Aluminum alloy material for reddish beige-colored anodic oxidation coating and its production

    JP1996311589A

  • Aluminum alloy for semiconductor producing device excellent in formability of alumite coating excellent in gas corrosion resistance and plasma corrosion resistance and heat resistance and material for semiconductor producing device

    JP1999043734A

  • Parts for surface treatment apparatus having excellent voltage resistance

    JP2002241992A

  • Method for forming ceramic film on aluminum substrate surface

    JP2003171794A

  • Method for producing aluminum alloy thick plate

    JP2005074453A