A 5052 aluminum alloy ultra-thick plate and its preparation method

Abstract

The present invention relates to the technical field of aluminum alloy materials, and specifically discloses a method for preparing a 5052 aluminum alloy ultra-thick plate, comprising the following steps: (1) batching; (2) smelting and casting; (3) homogenization heat treatment; (4) sawing and milling; (5) heating; (6) hot rolling; and (7) annealing. In step (6), large reduction rolling is adopted during the rolling process, with a single-pass reduction of 40 to 50 mm, and rapid cooling is performed by spraying after rolling. In step (7), the annealing temperature is 320 to 340° C., the temperature is kept for 3 to 6 hours, and the cooling method is furnace cooling. In the method for preparing the 5052 aluminum alloy ultra-thick plate of the present invention, by reasonably adjusting the rolling process and the annealing process, etc., the microstructure and properties of the surface and core of the 5052 aluminum alloy plate are made consistent, so that a uniform and dense oxide film layer is obtained after anodizing, the anodizing performance and corrosion resistance are improved, and the use requirements of semiconductor equipment components are met.

Description

Technical Field

[0001] The present invention relates to the technical field of aluminum alloy materials, and in particular to a 5052 aluminum alloy ultra-thick plate and a preparation method thereof. Background Art

[0002] Due to their high precision and specific application environments, semiconductor equipment components require aluminum materials with high cleanliness, high corrosion resistance, and excellent anodizing properties. Currently, aluminum alloys used in semiconductor equipment are primarily imported, and the supply has long been monopolized by foreign manufacturers, significantly hindering the development of China's semiconductor industry. Semiconductor equipment chambers, such as photolithography machines, etching machines, and ion implanters, are typically manufactured from ultra-thick (≥150mm) aluminum alloy sheet. 5052 aluminum alloy, with its excellent formability, corrosion resistance, and medium strength, is commonly used in the manufacture of semiconductor equipment components. The main process of preparing 5052 aluminum alloy ultra-thick plates using existing technology is: batching → smelting → casting → homogenization → machining → heating → rolling. The rolling process adopts multiple rolling passes, and the deformation of a single pass is small. The surface and core of the plate cannot deform synchronously, resulting in a large difference in the microstructure of the surface and core. This will cause the oxide film layer generated in the subsequent anodizing process to have problems such as poor density, uneven thickness, and color difference. Therefore, the corrosion resistance is poor during use and cannot meet the many stringent requirements of semiconductor equipment for aluminum alloys. Summary of the Invention

[0003] The purpose of the present invention is to provide a 5052 aluminum alloy ultra-thick plate and a preparation method thereof, which overcomes the problem of large microstructural differences between the surface and core of the existing 5052 aluminum alloy ultra-thick plate, greatly improves the problems of uneven thickness, poor density and anodic oxidation color difference of the anodic oxide film layer, and improves the anodic oxidation performance and corrosion resistance.

[0004] To achieve the above object, the present invention provides a method for preparing an ultra-thick 5052 aluminum alloy plate, comprising the following steps:

[0005] (1) Material preparation; (2) Melting and casting; (3) Homogenization heat treatment; (4) Sawing and milling; (5) Heating; (6) Hot rolling; (7) Annealing;

[0006] In the step (1), the alloy is prepared according to the following weight percentages: Si≤0.12%, Fe≤0.15%, Cu≤0.10%, Mn≤0.10%, Mg 2.3-2.7%, Cr 0.15-0.25%, Zn≤0.10%, and the balance is Al and unavoidable impurities;

[0007] In the step (6), a large reduction is used during the rolling process, and the reduction per pass is 40 to 50 mm, so that the deformation of the surface and the core of the plate tends to be consistent; after rolling, the plate is rapidly cooled by spraying to control the temperature of the hot-rolled plate off the line and increase the internal storage energy of the plate after deformation;

[0008] In the step (7), the annealing temperature is 320-340° C., the temperature is kept for 3-6 hours, and the cooling method is furnace cooling.

[0009] Preferably, the preparation method of the above-mentioned 5052 aluminum alloy ultra-thick plate is characterized in that the smelting and casting in step (2) are as follows: the raw materials prepared in step (1) are subjected to smelting, composition adjustment, converter, online refining, filtration, and standing processes to obtain a high-purity, high-uniform 5052 aluminum alloy flat ingot, and the H content of the melt is controlled to be ≤0.10ml / 100gAl.

[0010] Preferably, in the above-mentioned method for preparing the 5052 aluminum alloy ultra-thick plate, in the step (3), a two-stage homogenization heat treatment process is adopted to heat treat the 5052 aluminum alloy flat ingot obtained in the step (2). In the first stage, the ingot enters the soaking furnace at room temperature and is heated to 410-430°C and kept warm for 2-6 hours; in the second stage, the ingot is heated to 500-520°C and kept warm for 10-15 hours, and then taken out of the furnace and air-cooled after the end of the insulation.

[0011] Preferably, in the above-mentioned method for preparing the ultra-thick 5052 aluminum alloy plate, the flat ingot obtained in step (3) is subjected to head and tail trimming and surface milling, with the head and tail of the flat ingot each being trimmed by 100 to 200 mm, and the upper and lower surfaces each being milled by 7 to 15 mm.

[0012] Preferably, in the above-mentioned method for preparing the 5052 aluminum alloy ultra-thick plate, the heating temperature is 430-500° C., and the insulation time is 3-15 hours.

[0013] Preferably, in the above-mentioned method for preparing the 5052 aluminum alloy ultra-thick plate, in the step (6), rapid cooling is performed by spraying to control the offline temperature of the hot-rolled plate to be below 100°C.

[0014] A 5052 aluminum alloy ultra-thick plate is prepared by the above-mentioned preparation method of the 5052 aluminum alloy ultra-thick plate.

[0015] The above-mentioned 5052 aluminum alloy ultra-thick plate is used in semiconductor equipment.

[0016] Compared with the prior art, the present invention has the following beneficial effects:

[0017] 1. In the preparation method of the 5052 aluminum alloy ultra-thick plate of the present invention, by rationally adjusting the rolling process and annealing process, etc., the microstructure and properties of the surface and core of the 5052 aluminum alloy plate are made consistent, thereby obtaining a uniform and dense oxide film layer after anodizing, improving the anodizing performance and corrosion resistance, and meeting the use requirements of semiconductor equipment components.

[0018] 2. In the preparation method of the 5052 aluminum alloy ultra-thick plate of the present invention, by adopting a large reduction rolling method and a rapid cooling method by spraying after hot rolling, the deformed plate can store more energy inside, thereby allowing the plate to recrystallize at a lower temperature. At the same time, due to the low annealing temperature adopted, the grain structure does not grow abnormally, and a plate with a uniform and fine recrystallized grain structure is obtained, thereby improving the comprehensive performance of the plate. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] To more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for describing the embodiments. Obviously, the drawings described below are some embodiments of the present invention, and those skilled in the art can derive other drawings based on these drawings without inventive effort.

[0020] Figure 1 Metallographic microstructure of the 5052 aluminum alloy plate prepared in Example 1 of the present invention: (a) surface; (b) core.

[0021] Figure 2 Metallographic microstructure of the 5052 aluminum alloy plate prepared in Example 2 of the present invention: (a) surface; (b) core.

[0022] Figure 3 Metallographic microstructure of the 5052 aluminum alloy plate prepared in Example 3 of the present invention: (a) surface; (b) core.

[0023] Figure 4 Metallographic microstructure of the 5052 aluminum alloy plate prepared in Comparative Example 1 of the present invention: (a) surface; (b) core.

[0024] Figure 5 This is a diagram showing the anodizing effect of the 5052 aluminum alloy plate prepared in Example 1 of the present invention.

[0025] Figure 6 This is a diagram showing the anodizing effect of the 5052 aluminum alloy plate prepared in Example 2 of the present invention.

[0026] Figure 7 This is a diagram showing the anodizing effect of the 5052 aluminum alloy plate prepared in Example 3 of the present invention.

[0027] Figure 8 This is a diagram showing the anodizing effect of the 5052 aluminum alloy plate prepared in Comparative Example 1 of the present invention. DETAILED DESCRIPTION

[0028] The specific embodiments of the present invention are described in detail below, but it should be understood that the scope of protection of the present invention is not limited by the specific embodiments. Unless otherwise defined, all technical terms used hereinafter have the same meaning as those generally understood by those skilled in the art. The technical terms used herein are only for the purpose of describing specific embodiments and are not intended to limit the scope of protection of the present invention. Unless otherwise specified, the various raw materials, reagents, instruments and equipment used in the present invention can be purchased from the market or can be prepared by existing methods.

[0029] Example 1

[0030] A method for preparing an ultra-thick 5052 aluminum alloy plate comprises the following steps:

[0031] (1) Ingredients: The aluminum alloy raw material is prepared according to the following weight percentage components: Si 0.05%, Fe 0.10%, Cu 0.05%, Mn 0.05%, Mg 2.3%, Cr 0.25%, Zn 0.05%, and the balance is Al and unavoidable impurities;

[0032] (2) Melting and casting: The raw materials prepared in step (1) are subjected to the processes of melting, composition adjustment, converter, online refining, filtration, and standing to cast a 5052 aluminum alloy flat ingot. The H content of the melt is 0.092 ml / 100 g Al, and the specifications of the flat ingot are 580 mm × 1600 mm × 6000 mm;

[0033] (3) Homogenization heat treatment: The 5052 aluminum alloy flat ingot obtained in step (2) is subjected to homogenization heat treatment, and a two-stage homogenization heat treatment process is adopted. In the first stage, the ingot is placed in a soaking furnace at room temperature and heated to 410°C with the furnace and kept warm for 6 hours; in the second stage, the ingot is heated to 500°C and kept warm for 15 hours. After the end of the heat preservation, the ingot is taken out of the furnace and air-cooled;

[0034] (4) Sawing and milling: The slab obtained in step (3) is cut at the head and tail and the surface is milled. The head and tail of the slab are each cut off by 200 mm, and the upper and lower surfaces are each milled off by 7 mm;

[0035] (5) Heating: The flat ingot obtained in step (4) is placed in a heating furnace for heating at 500° C. for 3 h;

[0036] (6) Hot rolling: The flat ingot after heating and heat preservation in step (5) is taken out of the furnace and hot rolled. During the rolling process, a large reduction rolling is adopted. The number of rolling passes is 10, and the reduction of each pass is 40-50 mm. The ultra-thick plate with a thickness of 150 mm is rolled. After rolling, it is quickly cooled by spraying and the offline temperature of the hot-rolled plate is controlled to be 75°C.

[0037] (7) Annealing: The ultra-thick plate obtained in step (6) is annealed at a temperature of 320°C for 6 hours. The cooling method is furnace cooling. The annealed plate is cut with a precision saw to obtain a finished plate.

[0038] Example 2

[0039] A method for preparing an ultra-thick 5052 aluminum alloy plate comprises the following steps:

[0040] (1) Ingredients: The aluminum alloy raw material is prepared according to the weight percentage, namely: Si 0.12%, Fe 0.10%, Cu 0.05%, Mn 0.05%, Mg 2.7%, Cr 0.15%, Zn 0.10%, and the balance is Al and inevitable impurities;

[0041] (2) Melting and casting: The raw materials prepared in step (1) are subjected to the following processes: melting, composition adjustment, converter, online refining, filtration, and standing, and then cast into 5052 aluminum alloy flat ingots. The H content of the melt is 0.089 ml / 100 g Al, and the specifications of the flat ingots are 580 mm × 1600 mm × 6000 mm;

[0042] (3) Homogenization heat treatment: The 5052 aluminum alloy flat ingot obtained in step (2) is subjected to homogenization heat treatment, and a two-stage homogenization heat treatment process is adopted. In the first stage, the ingot is placed in a soaking furnace at room temperature and heated to 430°C and kept at that temperature for 2 hours; in the second stage, the ingot is heated to 520°C and kept at that temperature for 10 hours. After the end of the heat preservation, the ingot is taken out of the furnace and air-cooled;

[0043] (4) Sawing and milling: The slab obtained in step (3) is cut at the head and tail and the surface is milled. The head and tail of the slab are each cut off by 100 mm, and the upper and lower surfaces are each milled off by 15 mm;

[0044] (5) Heating: The flat ingot obtained in step (4) is placed in a heating furnace and heated at a temperature of 430° C. for 15 h;

[0045] (6) Hot rolling: The flat ingot after heating and heat preservation in step (5) is taken out of the furnace and hot rolled. During the rolling process, a large reduction rolling is adopted. The number of rolling passes is 8, and the reduction of each pass is 40-50 mm. The ultra-thick plate with a thickness of 190 mm is rolled. After rolling, it is quickly cooled by spraying and the offline temperature of the hot-rolled plate is controlled to be 86°C.

[0046] (7) Annealing: The ultra-thick plate obtained in step (6) is annealed at a temperature of 340°C for 3 hours. The cooling method is furnace cooling. The annealed plate is cut with a precision saw to obtain a finished plate.

[0047] Example 3

[0048] A 5052 aluminum alloy ultra-thick plate and a preparation method thereof, comprising the following steps:

[0049] (1) Ingredients: The aluminum alloy raw material is prepared according to the weight percentage, namely: Si 0.08%, Fe 0.15%, Cu 0.10%, Mn 0.10%, Mg 2.5%, Cr 0.21%, Zn 0.03%, and the balance is Al and unavoidable impurities;

[0050] (2) Melting and casting: The raw materials prepared in step (1) are subjected to the following processes: melting, composition adjustment, converter, online refining, filtration, and standing, and then cast into 5052 aluminum alloy flat ingots. The H content of the melt is 0.089 ml / 100 g Al, and the specifications of the flat ingots are 580 mm × 1600 mm × 6000 mm;

[0051] (3) Homogenization heat treatment: The 5052 aluminum alloy flat ingot obtained in step (2) is subjected to homogenization heat treatment, and a two-stage homogenization heat treatment process is adopted. In the first stage, the ingot is placed in a soaking furnace at room temperature and heated to 420°C and kept at this temperature for 4 hours; in the second stage, the ingot is heated to 510°C and kept at this temperature for 12 hours. After the end of the heat preservation, the ingot is taken out of the furnace and air-cooled;

[0052] (4) Sawing and milling: The flat ingot obtained in step (3) is cut at the head and tail and the surface is milled. The head and tail of the flat ingot are each cut off by 150 mm, and the upper and lower surfaces are each milled off by 10 mm;

[0053] (5) Heating: The flat ingot obtained in step (4) is placed in a heating furnace and heated at a temperature of 480° C. for 6 h;

[0054] (6) Hot rolling: The flat ingot heated and kept in step (5) is taken out of the furnace and hot rolled. During the rolling process, a large reduction is adopted. The number of rolling passes is 8, and the reduction of each pass is 40-50 mm. The thick plate with a thickness of 230 mm is rolled. After rolling, it is quickly cooled by spraying, and the offline temperature of the hot-rolled plate is controlled to be 98°C.

[0055] (7) Annealing: The ultra-thick plate obtained in step (6) is annealed at a temperature of 330°C for 5 hours. The cooling method is furnace cooling. The annealed plate is cut with a precision saw to obtain a finished plate.

[0056] Comparative Example 1

[0057] A 5052 aluminum alloy plate for semiconductor equipment and a preparation method thereof, comprising the following steps:

[0058] (1) Ingredients: The aluminum alloy raw material is prepared according to the weight percentage, namely: Si 0.12%, Fe 0.10%, Cu 0.05%, Mn 0.05%, Mg 2.7%, Cr 0.15%, Zn 0.10%, and the balance is Al and inevitable impurities;

[0059] (2) Melting and casting: The alloy composition designed in step (1) is prepared, and after the processes of melting, composition adjustment, converter, online refining, filtration, and standing, a 5052 aluminum alloy flat ingot is cast. The melt H content is 0.095 ml / 100 gAl, and the specifications of the flat ingot are 580 mm × 1600 mm × 6000 mm;

[0060] (3) Homogenization heat treatment: The 5052 flat ingot obtained in step (2) was subjected to homogenization heat treatment at a homogenization temperature of 550°C for a holding time of 10 h. After the holding time was completed, the ingot was taken out of the furnace and air-cooled;

[0061] (4) Sawing and milling: The flat ingot obtained in step (3) is cut at the head and tail and the surface is milled. The head and tail of the flat ingot are each cut off by 150 mm, and the upper and lower surfaces are each milled off by 10 mm;

[0062] (5) Heating: The flat ingot obtained in step (4) is placed in a heating furnace for heating at 500° C. for 6 h;

[0063] (6) Hot rolling: The flat ingot heated and kept in step (5) is taken out of the furnace and subjected to multi-pass rolling. The number of rolling passes is 22, and the single pass is rolled with a small reduction of 10 to 20 mm to form an ultra-thick plate with a thickness of 190 mm. The final rolling temperature is controlled at 380°C, and air cooling is performed after the final rolling.

[0064] The metallographic microstructure and anodic oxidation performance of the 5052 aluminum alloy ultra-thick plates prepared in Examples 1-3 and Comparative Example 1 were tested. Figures 1 to 8 .

[0065] Figures 1 to 4The metallographic microstructures of the 5052 aluminum alloy sheets prepared in Examples 1-3 and Comparative Example 1 are shown. As can be seen from the figures, the surface and core metallographic microstructures of the 5052 aluminum alloy sheets prepared in Examples 1-3 show little difference. This is because the sheets produced in Examples 1-3 were rolled using high reductions, resulting in consistent deformation of the surface and core, reducing differences in microstructure and performance between the two. Rapid cooling by spraying after hot rolling increases internal energy storage in the deformed sheets, allowing recrystallization at lower temperatures. Furthermore, due to the low annealing temperature, the grain structure does not grow abnormally, resulting in a sheet with a uniform, fine recrystallized grain structure. In contrast, the sheet produced in Comparative Example 1 was rolled using multiple passes of low reductions, resulting in inconsistent deformation of the surface and core, leading to significant differences in microstructure between the two.

[0066] Figures 5 to 8 The following images show the anodizing results of 5052 aluminum alloy plates prepared in Examples 1-3 and Comparative Example 1. The images show that the plates prepared in Examples 1-3 exhibit no significant color difference, and the resulting oxide films are relatively uniform and dense, demonstrating excellent anodizing performance. The plate prepared in Comparative Example 1 exhibits significant microstructural differences between the surface and core, which compromises the continuity and density of the oxide film and results in distinct color bands.

[0067] The foregoing descriptions of specific exemplary embodiments of the present invention are for purposes of illustration and description. These descriptions are not intended to limit the invention to the precise forms disclosed, and it is apparent that many variations and modifications are possible in light of the foregoing teachings. The exemplary embodiments have been selected and described for the purpose of explaining the specific principles of the invention and their practical application, thereby enabling those skilled in the art to realize and utilize a variety of exemplary embodiments of the invention and various options and modifications. The scope of the invention is intended to be defined by the claims and their equivalents.

Claims

1. A method for preparing an ultra-thick 5052 aluminum alloy plate, characterized in that: The following steps are involved: (1) Material preparation; (2) Melting and casting; (3) Homogenization heat treatment; (4) Sawing and milling; (5) Heating; (6) Hot rolling; (7) Annealing; In the step (1), the alloy is prepared according to the following weight percentages: Si≤0.12%, Fe≤0.15%, Cu≤0.10%, Mn≤0.10%, Mg 2.3-2.7%, Cr 0.15-0.25%, Zn≤0.10%, and the balance is Al and unavoidable impurities; In the step (6), a large reduction rolling method is used during the rolling process, with a single-pass reduction of 40 to 50 mm, and rapid cooling is performed by spraying after rolling; In the step (7), the annealing temperature is 320-340°C, the temperature is kept for 3-6 hours, and the cooling method is furnace cooling.

2. The method for preparing the 5052 aluminum alloy ultra-thick plate according to claim 1, wherein: The smelting and casting in step (2) are as follows: the raw materials prepared in step (1) are subjected to smelting, composition adjustment, converter, online refining, filtration, and standing processes to obtain a 5052 aluminum alloy flat ingot, and the H content of the melt is controlled to be ≤0.10 ml / 100 g Al.

3. The method for preparing the 5052 aluminum alloy ultra-thick plate according to claim 2, characterized in that: In the step (3), the 5052 aluminum alloy flat ingot obtained in the step (2) is heat treated by a two-stage homogenization heat treatment process. In the first stage, the ingot is placed in a soaking furnace at room temperature and heated to 410-430°C with the furnace and kept warm for 2-6 hours. In the second stage, the temperature is raised to 500~520℃ and kept warm for 10~15h. After the insulation is completed, the furnace is taken out of the furnace and air-cooled.

4. The method for preparing the 5052 aluminum alloy ultra-thick plate according to claim 3, wherein: The flat ingot obtained in step (3) is cut at the head and tail and the surface is milled. The head and tail of the flat ingot are cut off by 100 to 200 mm respectively, and the upper and lower surfaces are milled off by 7 to 15 mm respectively.

5. The method for preparing the 5052 aluminum alloy ultra-thick plate according to claim 1, wherein: In the step (5), the heating temperature is 430-500° C. and the insulation time is 3-15 h.

6. The method for preparing the 5052 aluminum alloy ultra-thick plate according to claim 1, characterized in that: In the step (6), the hot-rolled plate is rapidly cooled by spraying to control the offline temperature of the hot-rolled plate to be below 100°C.

7. A 5052 aluminum alloy ultra-thick plate produced by the method for producing the 5052 aluminum alloy ultra-thick plate according to any one of claims 1 to 6.

8. Use of the 5052 aluminum alloy ultra-thick plate as claimed in claim 7 in semiconductor equipment.

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