Aluminum-scandium alloy, target blank and preparation method of target blank

Abstract

The invention provides an aluminum-scandium alloy, a target blank and a preparation method of the aluminum-scandium alloy, and the preparation method comprises the following steps: carrying out electron beam melting treatment on an aluminum-scandium alloy bar to form an aluminum-scandium alloy melt; carrying out seeding treatment on the aluminum-scandium alloy melt, and then carrying out vibration ingot pulling treatment to prepare an aluminum-scandium alloy target blank; the components of a seeding melt adopted in the seeding treatment are the same as those of the aluminum-scandium alloy melt; wherein the vibration frequency of the vibration ingot pulling treatment is 10 Hz to 50 Hz; the vibration amplitude of the vibration ingot pulling treatment ranges from 0.5 mm to 3 mm.

Description

Technical Field

[0001] The present application relates to the technical field of alloy material preparation, and in particular to an aluminum-scandium alloy and a target blank and a preparation method thereof. Background Art

[0002] ScAlN films prepared from aluminum-scandium alloy targets have properties such as high dielectric constant, high temperature resistance and high voltage dielectric coefficient. They have become the key core material of 5G RF filters and are widely used in the deposition of integrated circuits, memory devices and other semiconductor components in industries such as automobiles, aerospace, telecommunications and consumer electronics.

[0003] The traditional method of preparing aluminum-scandium alloy and target blank adopts the melting casting method, which is easily affected by the casting mold, introducing corresponding impurity elements into the target blank, and reducing the purity of the aluminum-scandium alloy product; in addition, since the melt-cast ingots are prone to defects such as pores and cold shuts, and the aluminum-scandium alloy has a large solidification range, in addition to the above defects, it is also prone to casting defects such as looseness, thermal cracks and segregation. These casting defects will have a negative impact on the quality of the final product.

[0004] Therefore, the traditional technology still needs to be improved. Summary of the Invention

[0005] Based on this, the present application provides an aluminum-scandium alloy and a target blank and a preparation method thereof. The preparation method of the aluminum-scandium alloy and the target blank can effectively reduce the inclusion content in the aluminum-scandium alloy, have a high product yield, good uniformity and low porosity, and a high target blank yield.

[0006] The technical solutions of this application to solve the above technical problems are as follows:

[0007] In one aspect of the present application, a method for preparing an aluminum-scandium alloy and a target blank is provided, comprising the following steps:

[0008] The aluminum-scandium alloy bar is subjected to electron beam melting treatment to form an aluminum-scandium alloy melt;

[0009] The aluminum-scandium alloy melt is subjected to a seeding treatment and then subjected to a vibration ingot pulling treatment to prepare an aluminum-scandium alloy target blank; the seeding melt used in the seeding treatment has the same composition as that of the aluminum-scandium alloy melt;

[0010] The vibration frequency of the vibration ingot pulling process is 10 Hz to 50 Hz; and the vibration amplitude of the vibration ingot pulling process is 0.5 mm to 3 mm.

[0011] In one embodiment, the pulling speed of the vibration pulling process is 1.5 mm / min to 5 mm / min.

[0012] In one embodiment, the aluminum-scandium alloy melt is subjected to seeding treatment and then subjected to vibration ingot pulling treatment to prepare the aluminum-scandium alloy target blank, which includes the following steps:

[0013] Placing the raw materials for preparing the seeding melt on a seeding head and performing electron beam melting to form the seeding melt;

[0014] The aluminum-scandium alloy melt is dripped into the seeding melt on the seeding head to perform the seeding process.

[0015] In one embodiment, the step of dripping the aluminum-scandium alloy melt into the seeding melt on the seeding head to perform the seeding treatment is performed in a crystallizer, the crystallizer includes a molten pool and the seeding head, and the seeding head is placed below the molten pool; the molten pool is used to place the aluminum-scandium alloy melt.

[0016] In one embodiment, the thickness of the seeding melt is 15 mm to 40 mm; and / or

[0017] During the vibration ingot pulling process, the vertical distance between the upper liquid surface of the melt in the molten pool and the top of the crystallizer is 15 mm to 25 mm.

[0018] In one embodiment, the power of the electron beam used in the electron beam melting process is 50kw~250kw.

[0019] In one embodiment, the method for preparing the aluminum-scandium alloy bar comprises the following steps:

[0020] The raw materials are configured according to the stoichiometric composition of the aluminum-scandium alloy: metal scandium and metal aluminum;

[0021] Performing gradient suspension melting on the metal scandium and the metal aluminum to prepare an aluminum-scandium alloy;

[0022] The aluminum-scandium alloy is subjected to suspension melting and drawn into an ingot to prepare an aluminum-scandium alloy bar.

[0023] In one embodiment, based on the total amount of metal atoms contained in the raw material, the raw material includes: 5at%-53at% of metal scandium atoms and 47at%-95at% of metal aluminum atoms.

[0024] In some embodiments, the scandium content is 5 at% to 25 at%, the pulling speed is 3 mm / min to 5 mm / min, and the vibration amplitude is 1.5 mm to 3 mm; and / or

[0025] The content of the metal scandium is 25 at % to 53 at %, the ingot pulling speed is 1.5 mm / min to 3 mm / min, and the vibration amplitude is 0.5 mm to 1.5 mm.

[0026] In another aspect of the present application, an aluminum-scandium alloy and a target blank are provided, wherein the aluminum-scandium alloy and the target blank are prepared by the above-mentioned preparation method of the aluminum-scandium alloy and the target blank.

[0027] In the above-mentioned method for preparing an aluminum-scandium alloy target blank, an aluminum-scandium alloy bar is subjected to electron beam melting to form an aluminum-scandium alloy melt, and the aluminum-scandium alloy is melted and cast by electron beam vibration ingot pulling technology, and the melt is degassed and purified at the same time, thereby avoiding the pores and cold shut defects existing in the traditional melting and casting process; the aluminum-scandium alloy melt is subjected to a seeding treatment, and the composition of the seeding melt used in the seeding treatment is the same as that of the aluminum-scandium alloy melt, thereby avoiding the introduction of other impurity elements into the seeding melt during the seeding treatment, thereby reducing the content of inclusions in the obtained aluminum-scandium alloy and making the aluminum-scandium alloy melt more uniform; then a vibration ingot pulling treatment is performed to prepare an aluminum-scandium alloy target blank, and the probability of porosity and segregation of the ingot is reduced by controlling the specific vibration frequency and vibration amplitude of the vibration ingot pulling. Among them, if the amplitude is too small and the frequency is too high, it is easy to cause the prepared aluminum-scandium alloy target blank to crack. If the amplitude is too large and the frequency is too low, it is easy to cause the prepared aluminum-scandium alloy target blank to have defects such as pores and looseness. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a front view of the aluminum-scandium alloy melting device of Example 1;

[0029] Figure 2 is a tomographic image of a cross section of the aluminum-scandium alloy sample prepared in Example 1;

[0030] Figure 3 1 is the metallographic structure diagram of the aluminum-scandium alloy sample prepared in Example 1;

[0031] Figure 4 is a tomographic image of a cross section of the aluminum-scandium alloy sample prepared in Example 2;

[0032] Figure 5 This is a micrograph of the metallographic structure of the aluminum-scandium alloy sample prepared in Example 2.

[0033] Description of reference numerals:

[0034] 1. Aluminum-scandium alloy melting device; 10. Transport device; 11. Conveyor track; 12. Feed track; 13. Scandium alloy bar; 20. Electron beam melting furnace; 21. Electron beam emitter; 22. Crystallizer; 22A. Molten pool; 22B. Seeder; 23. Tension device. DETAILED DESCRIPTION

[0035] To facilitate understanding of the present application, a more comprehensive description of the present application will be provided below with reference to the accompanying drawings. The accompanying drawings illustrate preferred embodiments of the present application. However, the present application may be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a more thorough and comprehensive understanding of the disclosure of the present application.

[0036] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art to which this application pertains. The terms used herein in the specification of this application are for the purpose of describing specific embodiments only and are not intended to limit this application.

[0037] The term "comprises", "comprising" or any other variant thereof is intended to cover non-exclusive inclusion, so that the process, method, article or equipment comprising a series of elements includes not only those elements, but also includes other elements not clearly listed, or also includes elements inherent to such process, method, article or equipment. In the absence of more restrictions, the elements limited by the sentence "comprising a ..." do not exclude the presence of other identical elements in the process, method, article or equipment comprising the elements. The indefinite articles "a" and "an" before the elements or components of the present application have no restriction on the quantity requirements (i.e., the number of occurrences) of the elements or components. Therefore, "a" or "a" should be interpreted as including one or at least one, and the elements or components in the singular also include the plural form, unless the quantity obviously refers only to the singular form. The meaning of "plurality" is at least two, for example two, three, etc., unless otherwise clearly and specifically defined.

[0038] The weights of the relevant components mentioned in the examples of this application may not only refer to the specific content of each component, but also represent the proportional relationship between the weights of the components. Therefore, as long as the content of the relevant components is proportionally enlarged or reduced according to the examples of this application, it is within the scope disclosed in the examples of this application. Specifically, at% in the description of this application is atomic percentage, which represents the ratio of the number of atoms of an element to the total number of atoms, that is, molar percentage; the weights described in the examples of this application may be mass units known in the chemical industry such as μg, mg, g, and kg.

[0039] Except as shown in the operating examples or otherwise indicated, all numbers used in the specification and claims to express the amount of ingredients, physicochemical properties, etc. are understood to be adjusted by the term "about" in all cases. For example, therefore, unless otherwise indicated, the numerical parameters listed in the above specification and the appended claims are approximate values, and those skilled in the art will be able to appropriately change these approximate values ​​using the teachings disclosed herein to seek to obtain the desired properties. The use of numerical ranges expressed as endpoints includes all numbers within the range and any range within the range, for example, 1 to 5 includes 1, 1.1, 1.3, 1.5, 2, 2.75, 3, 3.80, 4 and 5, etc.

[0040] An embodiment of the present application provides a method for preparing an aluminum-scandium alloy and a target blank, including the following steps S100 and S200.

[0041] Step S100: Electron beam melting is performed on the aluminum-scandium alloy bar to form an aluminum-scandium alloy melt.

[0042] In some embodiments, the power of the electron beam used in the electron beam melting process is 50 kW to 250 kW.

[0043] It is understood that when a numerical range is disclosed herein, the range is considered continuous and includes the minimum and maximum values ​​of the range, as well as every value between such minimum and maximum values. Further, when a range refers to an integer, every integer between the minimum and maximum values ​​of the range is included. In addition, when multiple ranges are provided to describe a feature or characteristic, the ranges can be combined. In other words, unless otherwise indicated, all ranges disclosed herein are understood to include any and all subranges subsumed therein.

[0044] It should be noted that the power range of the electron beam is "50kw~250kw", which means that the power can take the minimum and maximum values ​​of the range of 50kw~250kw, as well as every value between the minimum and maximum values. Specific examples include but are not limited to the point values ​​in the embodiments and the following point values: 50kw, 55kw, 60kw, 65kw, 70kw, 75kw, 80kw, 85kw, 90kw, 95kw, 100kw, 105kw, 110kw, 115kw, 120kw, 125kw, 130kw, 135kw, 140kw, 145kw, kW, 150 kW, 155 kW, 160 kW, 165 kW, 170 kW, 175 kW, 180 kW, 185 kW, 190 kW, 195 kW, 200 kW, 205 kW, 210 kW, 215 kW, 220 kW, 225 kW, 230 kW, 235 kW, 240 kW, 245 kW, or 250 kW, or a range consisting of any two of these values, including, for example, 50 kW to 100 kW.

[0045] In some embodiments, the vacuum degree of the electron beam melting is 1×10 -4 Pa and above.

[0046] In some embodiments, the method for preparing the aluminum-scandium alloy bar includes steps S110 to S130.

[0047] Step S110: configuring raw materials according to the stoichiometric composition of the aluminum-scandium alloy: metal scandium and metal aluminum.

[0048] In some embodiments, based on the total amount of metal atoms contained in the raw materials, the raw materials include: 5at%-53at% of metal scandium atoms and 47at%-95at% of metal aluminum atoms.

[0049] Step S120: preparing an aluminum-scandium alloy by subjecting the metal scandium and the metal aluminum to gradient suspension melting.

[0050] Specifically, in step S120, the metal scandium and part of the metal aluminum are subjected to gradient suspension melting to prepare an aluminum-scandium alloy melt, and then the remaining metal aluminum is added to the aluminum-scandium alloy melt to prepare an aluminum-scandium alloy.

[0051] In some embodiments, the remaining metal aluminum may be added to the aluminum-scandium alloy melt multiple times, specifically, 2 times, 3 times, 4 times, or 5 times.

[0052] Step S130: subjecting the aluminum-scandium alloy to cold crucible suspension melting, directionally solidifying and pulling an ingot to prepare an aluminum-scandium alloy bar.

[0053] As can be understood, the aluminum-scandium alloy is melted by adding aluminum to scandium, and multiple melting passes promote alloy homogenization. After homogenization, the alloy is continuously directional solidified and drawn in a cold crucible suspension melting directional furnace to produce alloy bars. The bars have diameters ranging from 50mm to 220mm and lengths greater than 1000mm.

[0054] In the above-mentioned preparation method of aluminum-scandium alloy, the raw materials are configured by mixing metal scandium and metal aluminum in the stoichiometric ratio of the components of the aluminum-scandium alloy, and then ultra-clean gradient suspension melting and alloying are carried out. Then, the cold crucible suspension melting and directional solidification ingot pulling technology is used to prepare the aluminum-scandium alloy rods, which effectively solves the problem of impurities introduced into the alloy rods caused by traditional melting and casting rods, pressing rods or bundling other materials into rods.

[0055] Step S200: performing a seeding treatment on the aluminum-scandium alloy melt, and then performing a vibration ingot pulling treatment to prepare an aluminum-scandium alloy target blank; the composition of the seeding melt used in the seeding treatment is the same as that of the aluminum-scandium alloy melt; wherein the vibration frequency of the vibration ingot pulling treatment is 10 Hz to 50 Hz; and the vibration amplitude of the vibration ingot pulling treatment is 0.5 mm to 3 mm.

[0056] In some embodiments, the vibration mode is "pull, push, pull", vibrating up and down.

[0057] It should be noted that the vibration frequency range of "10 Hz to 50 Hz" can be a minimum value and a maximum value within the range of 10 Hz to 50 Hz, as well as every value between the minimum value and the maximum value. Specific examples include, but are not limited to, the point values ​​in the embodiments and the following point values: 10 Hz, 11 Hz, 12 Hz, 13 Hz, 14 Hz, 15 Hz, 16 Hz, 17 Hz, 18 Hz, 19 Hz, 20 Hz, 21 Hz, 22 Hz, 23 Hz, 24 Hz, 25 Hz, 26 Hz, 27 Hz, 28 Hz, 29 Hz, 30 Hz, 31 Hz, 32 Hz, 33 Hz, 34 Hz, 35 Hz, 36 Hz, 37 Hz, 38 Hz, 39 Hz, 40 Hz, 41 Hz, 42 Hz, 43 Hz, 44 Hz, 45 Hz, 46 Hz, 47 Hz, 48 Hz, 49 Hz, or 50 Hz, or a range consisting of any two of these values, including, for example, 10 Hz to 30 Hz.

[0058] The vibration amplitude range is "0.5 mm to 3 mm", which means the minimum and maximum values ​​in the range of 0.5 mm to 3 mm, as well as every value between the minimum and maximum values. Specific examples include, but are not limited to, the point values ​​in the embodiments and the following point values: 0.5 mm, 0.6 mm, 0.7 mm, 0.8 mm, 0.9 mm, 1 mm, 1.1 mm, 1.2 mm, 1.3 mm, 1.4 mm, 1.5 mm, 1.6 mm, 1.7 mm, 1.8 mm, 1.9 mm, 2 mm, 2.1 mm, 2.2 mm, 2.3 mm, 2.4 mm, 2.5 mm, 2.6 mm, 2.7 mm, 2.8 mm, 2.9 mm, or 3 mm. Or a range consisting of any two of these values, as an example, including: 0.5 mm to 2 mm.

[0059] In some embodiments, the seeding melt is selected from aluminum-scandium alloy rods.

[0060] In some embodiments, the pulling speed of the vibration pulling process is 1.5 mm / min to 5 mm / min.

[0061] It should be noted that the value range of the ingot pulling speed is "1.5mm / min~5mm / min", which means the minimum and maximum values ​​in the range of 1.5mm / min~5mm / min, and every value between the minimum and maximum values. Specific examples include but are not limited to the point values ​​in the embodiments and the following point values: 1.5 mm / min, 1.6 mm / min, 1.7 mm / min, 1.8 mm / min, 1.9 mm / min, 2 mm / min, 2.1 mm / min, 2.2 mm / min, 2.3 mm / min, 2.4 mm / min, 2.5 mm / min, 2.6 mm / min, 2.7 mm / min, 2.8 mm / min, 2.9 mm / min, 3 mm / min, 3.1 mm / min, 3.2 mm / min, 3.3 mm / min, 3.4 mm / min, 3.5 mm / min, 3.6 mm / min, 3.7 mm / min, 3.8 mm / min, 3.9 mm / min, 7 mm / min, 4.1 mm / min, 4.2 mm / min, 4.3 mm / min, 4.4 mm / min, 4.5 mm / min, 4.6 mm / min, 4.7 mm / min, mm / min, 4.8 mm / min, 4.9 mm / min or 5 mm / min, or a range consisting of any two of these values, including, for example, 1.5 mm / min to 3 mm / min.

[0062] In some embodiments, the scandium content of the metal is 5 at % to 25 at %, the pulling speed is 3 mm / min to 5 mm / min, and the vibration amplitude is 1.5 mm to 3 mm.

[0063] In some embodiments, the scandium content of the metal is 25 at % to 53 at %, the pulling speed is 1.5 mm / min to 3 mm / min, and the vibration amplitude is 0.5 mm to 1.5 mm.

[0064] In some embodiments, the step of performing seeding treatment on the aluminum-scandium alloy melt and then performing vibration ingot pulling treatment to prepare the aluminum-scandium alloy target blank includes steps S210 to S220.

[0065] Step S210: placing the raw materials for preparing the seeding melt on a seeding head and performing electron beam melting to form the seeding melt.

[0066] Step S220: dripping the aluminum-scandium alloy melt into the seeding melt on the seeding head to perform the seeding process.

[0067] In some embodiments, the diameter of the seeding head is 100 mm to 500 mm.

[0068] It should be noted that the diameter of the seeding head ranges from 100 mm to 500 mm, which means that the diameter can take the minimum and maximum values ​​within the range of 100 mm to 500 mm, as well as every value between the minimum and maximum values. Specific examples include, but are not limited to, the point values ​​in the embodiments and the following point values: 100 mm, 110 mm, 120 mm, 130 mm, 140 mm, 150 mm, 160 mm, 170 mm, 180 mm, 190 mm, 200 mm, 210 mm, 220 mm, 230 mm, 240 mm, 250 mm, 260 mm, 270 mm, 280 mm, 290 mm, 300 mm, 310 mm, 320 mm, 330 mm, 340 mm, 350 mm, 360 mm, 370 mm, 380 mm, 390 mm, 400 mm, 410 mm, 420 mm, 430 mm, 440 mm, 450 mm, 460 mm, 470 mm, 480 mm, 490 mm, or 500 mm, or a range consisting of any two of these values, for example, including 100 mm to 300 mm.

[0069] In one specific example, the step of dripping the aluminum-scandium alloy melt into the seeding melt on the seeding head to perform the seeding treatment is carried out in a crystallizer, and the crystallizer includes a molten pool and a seeding head, and the seeding head is placed below the molten pool; the molten pool is used to place the aluminum-scandium alloy melt.

[0070] In some embodiments, the melt thickness of the seeding melt is 15 mm to 40 mm.

[0071] In some embodiments, during the vibration ingot pulling process, a vertical distance between an upper liquid surface of the melt in the molten pool and a top of the crystallizer is 15 mm to 25 mm.

[0072] It can be understood that, with the horizontal line of the upper liquid surface of the melt in the molten pool as the reference, the vertical distance from the top of the crystallizer is 15 mm ~ 25 mm.

[0073] In some embodiments, the vertical distance between the seeding head and the top of the crystallizer is maintained at 50 mm to 60 mm.

[0074] In the above-mentioned preparation method of aluminum-scandium alloy, the aluminum-scandium alloy bar is subjected to electron beam melting to form an aluminum-scandium alloy melt, and the electron beam vibration ingot pulling technology is used to melt and cast the aluminum-scandium alloy, thereby avoiding the pores and cold shut defects existing in the traditional melting and casting process; the aluminum-scandium alloy melt is subjected to a seeding treatment, and the composition of the seeding melt used in the seeding treatment is the same as that of the aluminum-scandium alloy melt, thereby avoiding the introduction of other impurity elements into the seeding melt during the seeding treatment, thereby reducing the content of inclusions in the obtained aluminum-scandium alloy and making the aluminum-scandium alloy melt more uniform; then, a vibration ingot pulling treatment is performed to prepare an aluminum-scandium alloy target blank, and the vibration frequency and amplitude of the specific vibration ingot pulling are controlled to reduce the probability of looseness and segregation of the ingot. Among them, if the amplitude is too small and the frequency is too high, it is easy to cause segregation of the prepared aluminum-scandium alloy target blank; if the amplitude is too large and the frequency is too low, it is easy to cause the prepared aluminum-scandium alloy target blank to have defects such as pores and looseness.

[0075] Please refer to the Figure 1 , Figure 1 The invention discloses an aluminum-scandium alloy smelting device 1, comprising a transport device 10 for transporting aluminum-scandium alloy bars into an electron beam melting furnace for smelting; and an electron beam melting furnace 20 for electron beam melting the aluminum-scandium alloy bars.

[0076] Please continue to refer to Figure 1 In some embodiments, the transport device 10 includes a transfer track 11 and a feed track 12, and the direction indicated by the horizontal arrow is the track transmission direction.

[0077] In some embodiments, the electron beam melting furnace 20 includes, from top to bottom, an electron beam emitter 21 , a crystallizer 22 , and a tensioning device 23 .

[0078] In some embodiments, the crystallizer 22 includes a molten pool 22A and a seeding head 22B, and the seeding head 22B is placed below the molten pool 22A; the molten pool is used to place the aluminum-scandium alloy melt.

[0079] When preparing aluminum-scandium alloy, part of the aluminum-scandium alloy rod is placed on the seeding head 22A as the raw material for preparing the seeding melt and electron beam melting is performed to form the seeding melt; the remaining aluminum-scandium alloy rod is heated in the electron beam heating zone, so that it drips onto the seeding melt on the seeding head for seeding treatment, and the aluminum-scandium alloy rod is continuously transported by the transportation device 10 to be heated in the electron beam heating zone, dripped into the molten pool, and accumulated to form a certain melt; when the vertical distance between the upper liquid surface of the melt in the molten pool and the top of the crystallizer is 15 mm ~ 25 mm, the ingot is vibrated and pulled by the pulling device 23.

[0080] It can be understood that the composition of the seeding melt is the same as that of the aluminum-scandium alloy melt, that is, the composition of the seeding melt is the same as the raw material for preparing the aluminum-scandium alloy melt. In other words, the composition of the seeding melt and the aluminum-scandium alloy melt can use the same aluminum-scandium alloy rod.

[0081] In some embodiments, the pulling device 23 is used to control the vibration frequency, vibration amplitude and ingot pulling speed during the vibration ingot pulling process, wherein the vertical downward arrow represents the ingot pulling direction.

[0082] The above-mentioned aluminum-scandium alloy smelting device can realize the engineering preparation of aluminum-scandium alloy and target blank through continuous feeding and ingot pulling, greatly reducing energy consumption, increasing production capacity and shortening production cycle.

[0083] Another embodiment of the present application provides an aluminum-scandium alloy and a target blank, which are prepared by the above-mentioned preparation method of the aluminum-scandium alloy and the target blank.

[0084] The aluminum-scandium alloy and target blank prepared by the preparation method have low inclusion content, and after removing defective parts, the product yield is 85% to 95%, the uniformity is good, and the porosity is less than 0.01%.

[0085] The present application will be described below in conjunction with specific embodiments, but the present application is not limited to the following embodiments. It should be understood that the attached claims summarize the scope of the present application. Under the guidance of the concept of the present application, those skilled in the art should realize that certain changes made to the various embodiments of the present application will be covered by the spirit and scope of the claims of the present application.

[0086] Example 1

[0087] (1) Place metal scandium and metal aluminum with a purity greater than 4N in a suspension furnace for multi-pass smelting, wherein the first pass: scandium 5kg, aluminum 3kg;

[0088] Second pass: add 3kg of additional aluminum;

[0089] The third pass: add an additional 3kg of aluminum;

[0090] The fourth pass: add 3kg of additional aluminum;

[0091] The fifth pass: pull the ingot into a round rod to form an aluminum-scandium alloy bar, cut part of the bar, and then crush it for later use.

[0092] (2) The aluminum-scandium alloy round bar prepared in step (1) is divided into a first aluminum-scandium alloy and a second aluminum-scandium alloy. The first aluminum-scandium alloy is placed on the feed track, and the second aluminum-scandium alloy is placed on the seeding head (using a φ200mm seeding head) after being crushed. The distance between the seeding head and the top of the crystallizer is kept at 55mm. Then, the furnace cover is covered and vacuum is drawn to a vacuum degree of 10 -4 Pa and above.

[0093] (3) Start the electron beam emitter for heating, with an electron beam emission power of 60-62 kW, to melt the second aluminum-scandium alloy on the seeding head to form a seeding melt. When the melt thickness of the seeding melt is 20 mm, push the first aluminum-scandium alloy on the transmission track into the electron beam heating zone for heating, so that it melts and drips onto the seeding melt on the seeding head in the molten pool. Continue dripping the melt so that the molten pool liquid level is about 20 mm away from the top of the crystallizer, and start pulling the ingot. The pulling speed is 3-3.3 mm / min. At the same time, start the pull rod to vibrate up and down in "pull, push, pull", with a vibration frequency of 20 Hz and a vibration amplitude of 1.6-1.9 mm.

[0094] (4) After the vibration pulling process is completed, the seeding head and the ingot are taken out together, and then the seeding head is cut open to prepare the aluminum-scandium alloy target blank.

[0095] test:

[0096] 1. The cross section of the aluminum-scandium alloy sample prepared in Example 1 was subjected to electronic computed tomography (CT) to detect the porosity. The cross section tomography image is as follows: Figure 2 shown.

[0097] 2. The purity of the aluminum-scandium alloy sample prepared in Example 1 was tested by glow discharge mass spectrometry (GDMS).

[0098] 3. The aluminum-scandium alloy sample prepared in Example 1 was observed under an electron microscope and then subjected to a uniformity test. Specifically, SEM+EDS testing was used, which combined a scanning electron microscope (SEM) and an energy dispersive spectrometer (EDS). The microstructure of the aluminum-scandium alloy sample was as follows: Figure 3 The element detection results are shown in Table 1 (theoretical scandium content is 20at%).

[0099] Table 1

[0100]

[0101] The results show that the aluminum-scandium alloy target blank prepared in Example 1 of the present application has a yield of 87% after removing defective parts, a porosity of <0.01%, a purity of >4N, no large amount of impurities are introduced, and a uniformity of ±0.5at% (theoretical scandium content is 20at%).

[0102] Example 2

[0103] (1) Place metal scandium with a purity greater than 4N and metal aluminum in a suspension furnace for multi-pass smelting, wherein the first pass: scandium 8kg, aluminum 4kg;

[0104] Second pass: add an additional 3.2 kg of aluminum;

[0105] The third pass: pull the ingot into a round rod to form an aluminum-scandium alloy bar, cut part of the bar, and then crush it for later use.

[0106] (2) Place the first aluminum-scandium alloy and the second aluminum-scandium alloy prepared in step (1) on the feed track, and place the second aluminum-scandium alloy on the seeding head (using a φ200mm seeding head) after crushing. Keep a distance of 60mm between the seeding head and the top of the crystallizer, then cover the furnace and evacuate the vacuum to 10 -4 Pa and above.

[0107] (3) Start the electron beam emitter for heating, with an electron beam emission power of 72-74 kW, to melt the second aluminum-scandium alloy on the seeding head to form a seeding melt. When the melt thickness of the seeding melt is 30 mm, push the first aluminum-scandium alloy on the transmission track into the electron beam heating zone for heating, so that it melts and drips onto the seeding melt on the seeding head in the molten pool. Continue to drip the melt so that the molten pool liquid level is about 20 mm away from the top of the crystallizer, and start pulling the ingot. The ingot pulling speed is 1.5-1.8 mm / min. At the same time, start the pull rod to vibrate up and down in a "pull, push, pull" manner, with a vibration frequency of 20 Hz and a vibration amplitude of 0.8-1.2 mm.

[0108] (3) After the vibration pulling process is completed, the seeding head and the ingot are taken out together, and then the seeding head is cut open to prepare the aluminum-scandium alloy target blank.

[0109] test:

[0110] 1. The cross section of the aluminum-scandium alloy sample prepared in Example 2 was subjected to electronic computed tomography (CT) to detect the porosity. The cross section tomography image is as follows: Figure 4 shown.

[0111] 2. The purity of the aluminum-scandium alloy sample prepared in Example 2 was tested, specifically using GDSM testing.

[0112] 3. The aluminum-scandium alloy sample prepared in Example 2 was observed under an electron microscope and then subjected to a uniformity test. Specifically, SEM+EDS testing was used, which combined a scanning electron microscope (SEM) and an energy dispersive spectrometer (EDS). The metallographic structure of the aluminum-scandium alloy sample was as follows: Figure 5 The element detection results are shown in Table 2 (theoretical scandium content is 40at%).

[0113] Table 2

[0114]

[0115] The results show that in Example 2 of the present application, after removing the defective parts, the yield of the obtained aluminum-scandium alloy target blank is 87%, the porosity is less than 0.01%, the purity is greater than 4N, no large amount of impurities are introduced, and the uniformity reaches ±0.5at% (theoretical scandium content is 40at%).

[0116] In summary, the aluminum-scandium alloy and target blank prepared in the embodiments of the present application have low inclusion content, high product yield, good uniformity and low porosity.

[0117] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0118] The above-described embodiments merely represent several implementation methods of the present application. While the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent application. It should be noted that a person skilled in the art could make various modifications and improvements without departing from the spirit of the present application, all of which fall within the scope of protection of the present application. Therefore, the scope of protection of the present patent application shall be determined by the appended claims.

Claims

1. A method for preparing an aluminum-scandium alloy and a target blank, characterized in that: The following steps are involved: The aluminum-scandium alloy bar is subjected to electron beam melting treatment to form an aluminum-scandium alloy melt; The aluminum-scandium alloy melt is subjected to a seeding treatment and then subjected to a vibration ingot pulling treatment to prepare an aluminum-scandium alloy target blank; the seeding melt used in the seeding treatment has the same composition as that of the aluminum-scandium alloy melt; The vibration frequency of the vibration ingot pulling process is 10 Hz to 50 Hz; and the vibration amplitude of the vibration ingot pulling process is 0.5 mm to 3 mm.

2. The method for preparing the aluminum-scandium alloy and the target blank according to claim 1, wherein: The pulling speed of the vibration pulling process is 1.5 mm / min to 5 mm / min.

3. The method for preparing the aluminum-scandium alloy and the target blank according to any one of claims 1 to 2, characterized in that: The steps of performing seeding treatment on the aluminum-scandium alloy melt and then performing vibration ingot pulling treatment to prepare the aluminum-scandium alloy target blank include the following steps: Placing the raw materials for preparing the seeding melt on a seeding head and performing electron beam melting to form the seeding melt; The aluminum-scandium alloy melt is dripped into the seeding melt on the seeding head to perform the seeding process.

4. The method for preparing the aluminum-scandium alloy and the target blank according to claim 3, wherein: The step of dripping the aluminum-scandium alloy melt into the seeding melt on the seeding head to perform the seeding treatment is carried out in a crystallizer, the crystallizer includes a molten pool and the seeding head, and the seeding head is placed below the molten pool; the molten pool is used to place the aluminum-scandium alloy melt.

5. The method for preparing the aluminum-scandium alloy and the target blank according to claim 4, wherein: The thickness of the seeding melt is 15 mm to 40 mm; and / or During the vibration ingot pulling process, the vertical distance between the upper liquid surface of the melt in the molten pool and the top of the crystallizer is 15 mm to 25 mm.

6. The method for preparing the aluminum-scandium alloy and the target blank according to any one of claims 1 to 2 and 4 to 5, characterized in that: The power of the electron beam used in the electron beam melting process is 50kw~250kw.

7. The method for preparing the aluminum-scandium alloy and the target blank according to any one of claims 1 to 2 and 4 to 5, characterized in that: The preparation method of the aluminum-scandium alloy bar comprises the following steps: The raw materials are configured according to the stoichiometric composition of the aluminum-scandium alloy: metal scandium and metal aluminum; preparing an aluminum-scandium alloy by subjecting the metal scandium and the metal aluminum to gradient suspension melting; The aluminum-scandium alloy is subjected to suspension melting and drawn into an ingot to prepare an aluminum-scandium alloy bar.

8. The method for preparing the aluminum-scandium alloy and the target blank according to claim 7, wherein: Based on the total amount of metal atoms contained in the raw material, the raw material includes: 5at% to 53at% of metal scandium atoms and 47at% to 95at% of metal aluminum atoms.

9. The method for preparing the aluminum-scandium alloy and the target blank according to claim 8, wherein: The metal scandium content is 5 at% to 25 at%, the ingot pulling speed is 3 mm / min to 5 mm / min, and the vibration amplitude is 1.5 mm to 3 mm; and / or The content of the metal scandium is 25 at % to 53 at %, the ingot pulling speed is 1.5 mm / min to 3 mm / min, and the vibration amplitude is 0.5 mm to 1.5 mm.

10. An aluminum-scandium alloy and a target blank, characterized in that: The aluminum-scandium alloy and target blank are prepared by the preparation method of the aluminum-scandium alloy and target blank according to any one of claims 1 to 9.

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