CN117677735A - Aluminum member for semiconductor manufacturing apparatus and method for manufacturing the same - Google Patents

Aluminum member for semiconductor manufacturing apparatus and method for manufacturing the same Download PDF

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Publication number
CN117677735A
CN117677735A CN202280050736.2A CN202280050736A CN117677735A CN 117677735 A CN117677735 A CN 117677735A CN 202280050736 A CN202280050736 A CN 202280050736A CN 117677735 A CN117677735 A CN 117677735A
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base material
manufacturing apparatus
semiconductor manufacturing
aluminum member
aluminum
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布村顺司
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UACJ Corp
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UACJ Corp
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/05—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys of the Al-Si-Mg type, i.e. containing silicon and magnesium in approximately equal proportions
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/02—Alloys based on aluminium with silicon as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C21/00—Alloys based on aluminium
    • C22C21/06—Alloys based on aluminium with magnesium as the next major constituent
    • C22C21/08—Alloys based on aluminium with magnesium as the next major constituent with silicon
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
    • C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
    • C22F1/04—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon
    • C22F1/047—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of aluminium or alloys based thereon of alloys with magnesium as the next major constituent
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02—Anodisation
    • C25D11/04—Anodisation of aluminium or alloys based thereon
    • C25D11/16—Pretreatment, e.g. desmutting
    • C—CHEMISTRY; METALLURGY
    • C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Electrochemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Other Surface Treatments For Metallic Materials (AREA)

Abstract

An aluminum member (1) for a semiconductor manufacturing apparatus has a base material (2) made of aluminum or an aluminum alloy, and an anodized film (3) formed on the base material (2). In the anodic oxidation coating (3), heterogeneous particles (31) having a long axis diameter of 0.1 [ mu ] m or more and 15 [ mu ] m or less and containing metal atoms other than Al atoms are present. The method for producing an aluminum member (1) for a semiconductor production device comprises the following anodic oxidation treatment steps: an anodic oxidation treatment is performed on a base material (2) having second phase particles in an Al matrix phase by using an acidic electrolyte, and an anodic oxidation coating (3) containing heterogeneous particles (31) is formed on the base material (2).

Description

Aluminum member for semiconductor manufacturing apparatus and method for manufacturing the same
Technical Field
The present invention relates to an aluminum member for a semiconductor manufacturing apparatus and a method for manufacturing the same.
Background
In a semiconductor manufacturing apparatus such as a CVD (chemical vapor deposition) apparatus, a PVD (physical vapor deposition) apparatus, and a dry etching apparatus, the temperature of a component such as a chamber increases during processing of a semiconductor disposed in the chamber. Further, if the impurity element or the like is separated from the constituent members in the chamber during the process of the semiconductor, the impurity element or the like may cause defects in the semiconductor. In order to suppress the occurrence of these problems, aluminum alloys having high heat resistance and less impurity removal are used as constituent members of semiconductor manufacturing apparatuses.
For example, patent document 1 describes an Al alloy for a semiconductor manufacturing apparatus having excellent gas corrosion resistance, plasma corrosion resistance, acid aluminum film formability, and heat resistance, which is characterized by containing, as an alloy component, mn:0.3 to 1.5% (mass%, same as the following), cu:0.3 to 1.5 percent of Fe:0.1 to 1.0%, the balance being Al and unavoidable impurities, and having an average crystal grain diameter of 50 μm or less. The Al alloy for semiconductor manufacturing apparatus of patent document 1 is used as a material for semiconductor manufacturing apparatus after forming an alumite coating film on the surface.
Prior art literature
Patent literature
Patent document 1: japanese patent laid-open No. 11-043734
Disclosure of Invention
Problems to be solved by the invention
However, the aluminum alloy and the alumite coating have different thermal expansion coefficients. Therefore, when the temperature of the material for semiconductor manufacturing equipment provided with the alumite coating film on the aluminum alloy increases, cracks may occur in the alumite coating film. If the crack progresses in the thickness direction of the alumite film and reaches the interface between the aluminum alloy and the alumite film, the aluminum alloy may be exposed. As a result, corrosion resistance may be reduced and exhaust gas may be increased.
The present invention has been made in view of the above-described background, and an object thereof is to provide an aluminum member for a semiconductor manufacturing apparatus and a manufacturing method thereof, in which a state in which a base material is covered with an anodized film is easily maintained even when a crack occurs in the anodized film.
Means for solving the problems
One embodiment of the present invention is an aluminum member for a semiconductor manufacturing apparatus, comprising:
a base material composed of aluminum or an aluminum alloy; and
an anodic oxide film formed on the base material,
in the anodic oxidation coating, heterogeneous particles having a long axis diameter of 0.1 μm or more and 15 μm or less and containing metal atoms other than Al (aluminum) atoms are present.
Another aspect of the present invention is a method for producing an aluminum member for a semiconductor manufacturing apparatus, wherein,
the method for manufacturing an aluminum member for a semiconductor manufacturing apparatus comprises the following anodic oxidation treatment steps: and (c) performing an anodic oxidation treatment on a base material having second phase particles in an Al matrix phase by using an acidic electrolyte, thereby forming the anodic oxidation coating containing the heterogeneous particles on the base material.
Effects of the invention
An anodized film is provided on a base material of an aluminum member for a semiconductor manufacturing apparatus (hereinafter referred to as an "aluminum member"). In addition, in the anodic oxidation coating, the specific heterogeneous particles are present. When the temperature of the aluminum member increases and cracks occur in the anodized film, such foreign particles can induce the cracks in a direction different from the thickness direction of the anodized film. Therefore, even when cracks occur in the anodized film of the aluminum member, the cracks tend to progress in a direction different from the thickness direction of the anodized film due to the foreign particles. As a result, the progress of the crack stops inside the anodized film, and it is difficult to reach the interface between the anodized film and the base material.
Therefore, in the aluminum member, even when cracks occur in the anodized film, the anodized film is easily maintained in a state of covering the base material.
The method for producing an aluminum member further includes an anodizing step of anodizing the base material containing the second-phase particles using an acidic electrolyte. In the anodizing treatment step, at least a part of the second phase particles in the base material are taken into the anodized film along with growth of the anodized film. This makes it possible to easily form an anodized film having the foreign particles on the base material.
As described above, according to the above aspect, it is possible to provide an aluminum member for a semiconductor manufacturing apparatus and a manufacturing method thereof, in which even when a crack occurs in an anodized film, the state in which a base material is covered with the anodized film is easily maintained.
Drawings
Fig. 1 is a partial cross-sectional view showing a main part of an aluminum member for a semiconductor manufacturing apparatus in an embodiment.
Fig. 2 is a secondary electron image of a cross section of the heated test material S3 in the example.
Fig. 3 is a secondary electron image of a cross section of the heated test material R1 in the example.
Detailed Description
(aluminum Member for semiconductor manufacturing apparatus)
The material of the base material in the aluminum member can be appropriately selected from the group consisting of aluminum and aluminum alloy according to the use of the aluminum member. For example, when it is desired to reduce the exhaust gas from the aluminum member, the base material is preferably composed of 1000-series aluminum or 3000-series aluminum alloy. As the 3000 series aluminum alloy, for example, an aluminum alloy having the following chemical composition can be used: contains Mn (manganese): 1.0 mass% or more and 1.5 mass% or less, and contains 1 or 2 or more elements selected from the group consisting of Si (silicon), fe (iron), cu (copper), mg, cr (chromium), zn (zinc) and Ti (titanium) as an arbitrary component, and the balance is made up of Al and unavoidable impurities.
In addition, when the strength of the aluminum member is to be improved, the base material is preferably composed of 5000 series aluminum alloy or 6000 series aluminum alloy. As the 5000 series aluminum alloy, for example, an aluminum alloy having the following chemical composition can be used: contains Mg (magnesium): 0.5 mass% or more and 5.0 mass% or less, and contains 1 or 2 or more elements selected from the group consisting of Si, fe, cu, mn, cr, zn and Ti as an optional component, the balance being made up of Al and unavoidable impurities. Further, as 6000 series aluminum alloy, for example, an aluminum alloy having the following chemical composition may be used: contains Mg:0.3 mass% or more and 1.5 mass% or less, si:0.2 mass% or more and 1.2 mass% or less, and contains 1 or 2 or more elements selected from the group consisting of Fe, cu, mn, cr, zn and Ti as an optional component, the balance being made up of Al and unavoidable impurities.
The base material of the aluminum member may contain second phase particles. As described later, when the base material including the second phase particles is anodized, at least a part of the second phase particles is taken into the anodized coating film, and the second phase particles become heterogeneous particles. As a result, the aluminum member can be easily manufactured.
The second phase particles contained in the base material have various compositions according to the material of the base material. For example, the base material made of 1000-system aluminum contains second phase particles such as an al—fe-system intermetallic compound and an al—fe—si-system intermetallic compound. In a base material composed of 3000 aluminum alloy, comprising second phase particles such as Al-Mn intermetallic compound, al-Mn-Si intermetallic compound, al-Fe-Si intermetallic compound, and Al-Mn-Fe-Si intermetallic compound. The base material made of 5000-series aluminum alloy contains second phase particles such as Al-Mg-series intermetallic compounds. The base material composed of 6000 series aluminum alloy contains Al-Mg series intermetallic compound and Al-Mg-Si series intermetallic compoundCompound, si, mg 2 Second phase particles such as Si.
An anodic oxide film is provided on the base material. The anodic oxide coating is mainly composed of an oxide of aluminum. The anodic oxide film may be a porous anodic oxide film having a plurality of pores, or a barrier anodic oxide film having no pores. The thickness of the anodic oxide film is not particularly limited, and can be appropriately set from a range of 0.1 μm to 100 μm, for example.
The anodic oxide film contains heterogeneous particles having a long axis diameter of 0.1 μm or more and 15 μm or less, which contain metal atoms other than Al atoms. When the anodic oxide film has cracks, the hetero particles having the major axis diameter within the above specific range can induce the progress direction of the cracks to a direction inclined with respect to the thickness direction of the anodic oxide film. Therefore, when the anodic oxide film is cracked, the crack tends to progress in a direction inclined with respect to the thickness direction of the anodic oxide film. Even if the crack that proceeds in the direction inclined with respect to the thickness direction of the anodized film is the same length as the crack that proceeds in the thickness direction of the anodized film, the depth of the crack tip from the surface of the anodized film can be made shallow. In addition, by advancing the crack in a direction inclined with respect to the thickness direction of the anodized film, the length of the crack can be prolonged, and the stress generated in the anodized film due to the difference in thermal expansion can be reduced. As a result, the tip of the crack is likely to remain in the anodized film, and the crack is unlikely to reach the interface between the anodized film and the base material.
The long axis diameter of the hetero particles present in the anodized film is a value measured by the following method. First, the aluminum member was cut into an arbitrary section, and a sample was collected. After embedding the sample in a resin, the cross section of the sample was mirror polished to expose the cross section of the anodized film. Next, a cross section of the anodized film was observed by using an electron microscope, and an electron microscopic image including heterogeneous particles was obtained. A rectangle circumscribing the heterogeneous particles present in the electron microscopic image is drawn, and the length of the long side of the rectangle is set to be the long axis diameter of the heterogeneous particles.
In addition, in the anodic oxidation coating, hetero particles having a long axis diameter of less than 0.1 μm and hetero particles having a long axis diameter of more than 15 μm may be present. However, heterogeneous particles having a major axis diameter of less than 0.1 μm have a lower effect in inducing the progress direction of cracks than particles having a major axis diameter within the above-mentioned specific range. Further, if the number of hetero particles having a major axis diameter exceeding 15 μm is too large, the number of hetero particles contained in the anodized film becomes small, and there is a possibility that the effect of inducing the progress direction of cracks is reduced.
From the viewpoint of more effectively suppressing the progress of cracks in the thickness direction of the anodized film, the average value of the long axis diameters of the hetero particles contained in the anodized film is preferably 0.1 μm or more and 15 μm or less, more preferably 0.5 μm or more and 10 μm or less, and still more preferably 1.0 μm or more and 5.0 μm or less. If the average value of the major axis diameters of the hetero particles is too small, the proportion of hetero particles having a major axis diameter of less than 0.1 μm contained in the anodized film increases, and the effect of inducing the progress direction of cracks may be reduced. In addition, when the average value of the major axis diameters of the hetero particles is too large, the proportion of hetero particles having a major axis diameter exceeding 15 μm contained in the anodic oxide film becomes large, and there is a possibility that the number of hetero particles contained in the anodic oxide film decreases.
Every 1mm of anodic oxide film 2 The number of heterogeneous particles having a major axis of 0.1 μm or more and 15 μm or less contained in the surface area is preferably 1600 or more. In this case, the interval between the hetero particles in the anodic oxide film can be sufficiently shortened. Therefore, even when a crack is generated in any portion of the anodized film, the possibility that heterogeneous particles having a long axis diameter within the above-described specific range exist in the vicinity of the crack can be increased. Thus, by anodic oxidation of every 1mm of the film 2 The number of the foreign particles contained in the surface area is within the specific range, so that the effect of suppressing the exposure of the base material can be further improved, and the state in which the base material is covered with the anodic oxide coating can be more easily maintained.
From the same viewpoint, the distance between the hetero particle and the hetero particle closest to the hetero particle in an arbitrary cross section of the aluminum member is preferably 25 μm or less, more preferably 20 μm or less, and further preferably 15 μm or less.
The composition of the hetero particles is not particularly limited, and the hetero particles may contain Si atoms. Examples of such heterogeneous particles include Si and Mg as monomers 2 Si, al-Mn-Fe-Si intermetallic compounds, and the like. In the case of producing an aluminum member by the production method of the above-described embodiment, second phase particles, which are not dissolved during the anodic oxidation treatment, among the second phase particles in the base material are taken into the anodic oxidation coating 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, mg in the base material 2 Since Si dissolves out Mg atoms during the anodic oxidation treatment and Si atoms are taken into the coating film, fine hetero particles rich in Si atoms can be dispersed in the coating film.
The thickness of the aluminum member for the semiconductor manufacturing apparatus is not particularly limited. For example, the aluminum member for the semiconductor manufacturing apparatus may be a thick plate having a thickness of 6mm or more. The occurrence of cracks in the anodic oxide film is considered to be caused by the difference in thermal expansion between the anodic oxide film and the base material. If the base material is thick, the stress due to the difference in thermal expansion increases, and therefore cracks tend to occur in the anodized film. In contrast, since the anodized film of the aluminum member contains heterogeneous particles having a long axis diameter in the above-described specific range, as described above, even when cracks occur in the anodized film, the progress direction of the cracks can be induced in a direction different from the thickness direction of the anodized film. Therefore, even when the thickness of the aluminum member for a semiconductor manufacturing apparatus is large, the base material can be easily maintained in a state of being covered with the anodic oxide film by the effect of the heterogeneous particles.
The aluminum member is used as a component of a semiconductor manufacturing apparatus. More specifically, the aluminum member is used in, for example, a chamber of a film forming apparatus such as a CVD apparatus or PVD apparatus, an etching apparatus such as a dry etching apparatus, a member disposed in the chamber, or the like.
(method for manufacturing aluminum Member for semiconductor manufacturing apparatus)
The method for producing an aluminum member includes an anodizing step of anodizing a base material having second-phase particles in an Al base material phase with an acidic electrolyte to form the anodized film containing the heterogeneous particles on the base material.
In the anodizing step, the base material having the second phase particles is anodized using an acidic electrolyte. When an acidic electrolyte is used as the electrolyte in the anodic oxidation, the dissolution reaction of the base material and the aluminum oxide and the growth reaction of the aluminum oxide proceed in parallel in the anodic oxidation. Thus, a porous anodic oxide film having a plurality of pores can be formed on the base material. Further, as the anodic oxide film grows, second phase particles, which are not dissolved in the electrolyte solution, among the second phase particles in the base material are taken into the anodic oxide film, and become heterogeneous particles. Therefore, by performing the above-described anodic oxidation treatment on the base material, an anodic oxidation coating containing heterogeneous particles can be formed on the base material.
The electrolyte used in the anodic oxidation treatment step may contain, for example, 1 or 2 or more acids selected from the group consisting of organic acids such as oxalic acid, malonic acid, 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, the electrolyte preferably contains 1 or 2 acids of oxalic acid and sulfuric acid.
In the anodizing treatment step, the base material and the counter electrode are immersed in the electrolyte, and a direct current is passed between the base material and the counter electrode, whereby an anodized film can be formed on the surface of the base material. The current density of the direct current in the anodic oxidation treatment is preferably 100A/m 2 600A/m 2 The following is given. By setting the current density of the DC current in the anodic oxidation treatment to 100A/m 2 The above is more preferably 200A/m 2 The above can accelerate anodic oxidationAnd the growth speed of the coating film is changed, so that the productivity of the aluminum component is improved. In addition, by setting the current density of the direct current in the anodic oxidation treatment to 600A/m 2 Hereinafter, it is more preferably 500A/m 2 In the following, the anodic oxide film can be uniformly grown on the base material, and burning of the base material and uneven anodic oxide film can be avoided.
The temperature of the electrolyte in the anodizing treatment step is preferably 263K or more and 303K or less. By setting the temperature of the electrolyte to 263K or more, more preferably 273K or more, the solubility of the electrolyte can be moderately increased, and the concentration of the electrolyte in the electrolyte can be sufficiently increased. Further, by setting the temperature of the electrolyte to 303K or less, more preferably 293K or less, an excessive increase in the dissolution force of the electrolyte can be avoided, and the growth rate of the anodic oxide film can be increased.
The base material used in the anodizing treatment step can be produced by any method.
For example, the method for manufacturing an aluminum member may further include:
a casting step of producing an ingot made of aluminum or an aluminum alloy;
a homogenizing step of homogenizing the ingot at a temperature of 500 to 560 ℃ for 5 to 10 hours; and
and a hot rolling step of hot rolling the ingot subjected to the homogenization treatment at a temperature of 500 ℃ or higher and 560 ℃ or lower to produce the base material.
As a casting method in the casting step, for example, DC casting can be employed. The thickness of the ingot obtained in the casting step is not particularly limited, and the ingot may have a thickness of 600mm or more, for example.
In the homogenizing step, the ingot obtained in the casting step is kept at a temperature of 500 ℃ to 560 ℃ for 5 hours to 10 hours. By setting the holding temperature and holding time in the homogenization treatment to the above specific ranges, the structure of the ingot can be sufficiently homogenized. Then, by hot rolling such an ingot, a base material containing desired second phase particles can be obtained.
In the hot rolling step, the homogenized ingot is hot rolled at a temperature of 500 ℃ or higher and 560 ℃ or lower. Thus, a base material can be obtained. If the initial temperature during hot rolling is too low, the deformation resistance of the ingot increases, and breakage may occur in the ingot during rolling, or the productivity may be deteriorated. On the other hand, if the starting temperature of the hot rolling is too high, the ingot may be locally melted due to heat generated during the hot rolling.
In the above-described production method, the base material obtained as described above may be directly subjected to the anodizing treatment step. The above production method may also include a heat treatment step of performing heat treatment such as annealing on the base material, if necessary, after the hot rolling step and before the anodic oxidation step.
The above-described production method may further include a pretreatment step of pretreating the base material after the hot rolling step and before the anodic oxidation step. Examples of the pretreatment of the base material include degreasing such as alkali degreasing, polishing such as mechanical polishing, chemical polishing, and electrolytic polishing. In the pretreatment step, 1 kind of pretreatment may be performed alone or 2 or more kinds of pretreatment may be performed in combination as appropriate, depending on the desired properties of the aluminum member.
When the alkali degreasing treatment is performed in the pretreatment step, the gloss of the anodized film obtained after the anodizing treatment can be reduced, and an aluminum member having a non-glossy appearance can be obtained. In addition, when polishing is performed in the pretreatment step, the gloss of the anodized film obtained after the anodizing treatment can be improved, and an aluminum member having a glossy appearance can be obtained. In the pretreatment step, it is preferable to perform electrolytic polishing treatment on the base material from the viewpoint of further improving the gloss of the aluminum member.
[ example ]
Examples of the aluminum member for semiconductor manufacturing apparatus and the manufacturing method thereof will be described below. As shown in fig. 1, the aluminum member 1 of this example has a base material 2 made of aluminum or an aluminum alloy, and an anodized film 3 formed on the base material 2. The anodized film 3 has heterogeneous particles 31 having a long axis diameter of 0.1 μm or more and 15 μm or less and containing metal atoms other than Al atoms.
The aluminum member 1 of this example can be obtained by the following method, for example. First, an ingot having a chemical composition represented by any one of alloy marks a5052, a5083, and a6063 is produced by DC casting (casting step). The thickness of the ingot was set to 600mm, for example. The ingot is kept at a temperature of 500 ℃ to 560 ℃ for 5 hours to 10 hours, and subjected to a homogenization treatment (a homogenization treatment step). After the homogenization treatment step, hot rolling was performed while the temperature of the ingot was 500 to 560 ℃ inclusive, to produce a sheet having a thickness of 300mm (hot rolling step).
For a plate having a chemical composition represented by alloy symbol a5052, a plate after hot rolling was directly used as the base material 2. The sheet material was tempered to a quality indicated by quality mark H112. For a sheet material having a chemical composition represented by alloy mark a5083, the sheet material after hot rolling is heated and annealed to temper the sheet material into a quality represented by quality mark O. Then, the annealed sheet material is used as the base material 2. The plate material having the chemical composition indicated by the alloy mark a6063 is subjected to solution treatment after hot rolling, and then subjected to artificial aging treatment, whereby the plate material is quenched and tempered to a quality indicated by the quality mark T6. Then, the artificially aged plate material was used as the base material 2.
The 3 base materials 2 were subjected to an anodic oxidation treatment under the conditions shown in table 1, whereby an anodic oxide film 3 was formed on the base materials 2. Thus, test materials S1 to S6 shown in table 1 were obtained. The test materials R1 shown in table 1 are test materials for comparison with the test materials S1 to S6. The production method of the test material R1 was the same as that of the test materials S1 to S6, except that the holding temperature in the homogenization treatment step was 480 ℃, the holding time was 4 hours, and the rolling start temperature in the hot rolling step was 450 ℃.
Next, the structure and the method of evaluating the heat resistance of the anodized coating 3 in the test materials S1 to S6 and the test material R1 will be described.
Method for evaluating structure of anodized film 3
Each test material is cut with a surface perpendicular to the rolling direction, for example, to expose the cross section of the anodized film 3. The cross section of the anodized film 3 was observed using a field emission scanning secondary electron microscope (FE-SEM) equipped with an energy dispersive X-ray spectroscopy device (EDX), to obtain a secondary electron image, and to obtain an elemental mapping image of the same field of view as the secondary electron image. Then, the position and size of the hetero particles 31 existing in the anodized film 3 are determined based on the secondary electron image and the element map. As the FE-SEM, for example, "SU-8230" manufactured by Hitachi Kagaku Kogyo Co., ltd. Further, as EDX, for example, "quanthax flutquad" manufactured by Bruker corporation may be used.
Next, for each of the hetero particles 31 appearing in the secondary electron image, a rectangle circumscribing the hetero particle 31 is determined. The length of the long side of the rectangle is set to the major axis of the hetero particle 31. Table 1 shows the maximum value of the major axis of the hetero particle 31 in each test material. Further, the interval between each hetero particle 31 appearing in the secondary electron image and the hetero particle 31 closest to the hetero particle 31 is measured. The maximum value of the interval between the hetero particles 31 is shown in table 1.
Heat resistance
The evaluation of heat resistance was performed based on the result 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 so as to expose a part of the anodic oxide film 3 in the test material. The area of the measurement portion in the test piece, i.e., the exposed portion of the anodized coating 3 was 1cm 2 . Next, a part of the test pieces was heated in the atmosphere at a temperature of 200 ℃ for 8 hours.
Then, acetic acid was added to a 5% NaCl aqueous solution so that the acetic acid concentration became 1mL/L to prepare a measurement solution. The solution was immersed in the test piece, the counter electrode and the reference electrode, which were electrically connected to the potentiostat, and allowed to stand for a while to stabilize the potential of the measurement section. As the reference electrode, for example, an Ag/AgCl electrode can be used.
After the potential of the measurement section was stabilized, a voltage was applied between the test piece and the counter electrode using a potentiostat, and the current density flowing in the measurement section was measured while scanning the potential of the measurement section at a scanning speed of 20 mV/min. Then, the scanning of the potential was ended at the point in time when the potential of the measuring section reached-2000 mV with respect to the reference electrode. Thereby, a polarization curve is obtained.
Next, in the polarization curve, the center of the potential region representing the diffusion limit current of hydrogen 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 of the anodic oxide film in the test piece, and a larger value of the current density indicates a larger number of defects in the anodic oxide film 3, and a larger contact area between the base material 2 and the measurement solution.
Therefore, the ratio of the value of the current density calculated using the test piece after heating to the value of the current density calculated using the test piece before heating represents the increase rate of the defect caused by heating. The increase rate of defects caused by heating in each test material is shown.
[ Table 1 ]
As shown in table 1, the anodized films 3 of the test materials S1 to S6 have heterogeneous particles 31 having long axis diameters within the above-described specific range. Therefore, when the temperature of the test material increases and a crack is generated in the anodized film 3, the crack tends to progress in a direction different from the thickness direction of the anodized film 3 due to the heterogeneous particles 31.
As an example, a secondary electron image of a cross section of the test material S3 after heating at a temperature of 200 ℃ for 8 hours is shown. In the test material S3, the crack 4 generated on the surface of the anodized film 3 is induced to a direction inclined with respect to the thickness direction of the anodized film 3 by the presence of the hetero particles 31. Then, the crack 4 progresses in a direction inclined with respect to the thickness direction of the anodized film 3, whereby the tip of the crack 4 stays inside the anodized film 3. In the test materials S1 to S2 and the test materials S4 to S6, too, similarly to the test material S3, the crack 4 generated on the surface of the anodized film 3 is easily induced to a direction inclined with respect to the thickness direction of the anodized film 3 due to the presence of the hetero particles 31, although not shown.
As a result, the progress of the crack 4 stops inside the anodized film 3, and it is difficult to reach the interface between the anodized film 3 and the base material 2.
On the other hand, in the anodized film 3 of the test material R1, the hetero particles 31 having the long axis diameter in the above-described specific range were not present. Therefore, as shown in fig. 3, the crack 4 generated on the surface of the anodized film 3 progresses in the thickness direction of the anodized film 3, and easily reaches the interface between the anodized film 3 and the base material 2. Therefore, the defect increase rate of the test material R1 is higher than that of the test materials S1 to S6.
From the above results, it can be understood that the aluminum member 1 including the hetero particles 31 having the long axis diameters in the above-described specific range in the inside of the anodized film 3 is excellent in heat resistance, and even when the anodized film 3 has the crack 4, the state in which the base material 2 is covered with the anodized film 3 is easily maintained.
The specific embodiment of the aluminum member for a semiconductor manufacturing apparatus and the manufacturing method thereof according to the present invention is not limited to the embodiment shown in the examples, and the configuration may be appropriately changed within a range not impairing the gist of the present invention.

Claims (8)

1. An aluminum member for a semiconductor manufacturing apparatus, comprising:
a base material composed of aluminum or an aluminum alloy; and
an anodic oxide film formed on the base material,
the anodic oxide film has heterogeneous particles having a long 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 a semiconductor manufacturing apparatus according to claim 1, wherein,
the average value of the long axis diameters of the heterogeneous particles is 0.1 μm or more and 15 μm or less.
3. The aluminum member for a semiconductor manufacturing apparatus according to claim 1 or 2, wherein,
every 1mm of the anodic oxidation coating 2 The number of the heterogeneous particles contained in the surface area is 1600 or more.
4. The aluminum member for a semiconductor manufacturing apparatus according to any one of claims 1 to 3, wherein,
in the arbitrary cross section of the aluminum member for a semiconductor manufacturing apparatus, the distance between the hetero particle and the hetero particle closest to the hetero particle is 25 μm or less.
5. The aluminum member for a semiconductor manufacturing apparatus according to any one of claims 1 to 4, wherein,
the heterogeneous particles contain Si atoms therein.
6. The aluminum member for a semiconductor manufacturing apparatus according to any one of claims 1 to 5, wherein,
the base material is composed of 5000 series aluminum alloy or 6000 series aluminum alloy.
7. A method for producing an aluminum member for a semiconductor manufacturing apparatus according to any one of claims 1 to 6, wherein,
the method for manufacturing an aluminum member for a semiconductor manufacturing apparatus comprises the following anodic oxidation treatment steps: and (c) performing an anodic oxidation treatment on a base material having second phase particles in an Al matrix phase by using an acidic electrolyte, thereby forming the anodic oxidation coating containing the heterogeneous particles on the base material.
8. The method for manufacturing an aluminum member for a semiconductor manufacturing apparatus according to claim 7, wherein,
the method for manufacturing an aluminum member for a semiconductor manufacturing apparatus further comprises:
a casting step of producing an ingot made of aluminum or an aluminum alloy;
a homogenization treatment step in which the ingot is kept at a temperature of 500 ℃ to 560 ℃ for 5 hours to 10 hours; and
and a hot rolling step of hot rolling the ingot subjected to the homogenization treatment at a temperature of 500 ℃ or higher and 560 ℃ or lower to produce the base material.
CN202280050736.2A 2021-09-06 2022-09-01 Aluminum member for semiconductor manufacturing apparatus and method for manufacturing the same Pending CN117677735A (en)

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