Casting method of aluminum target material
By adopting prestable and steady-state stage feeding and stirring treatments during the melting and casting of aluminum targets, the problems of difficult grain refinement and low nucleation rate in the melting and casting of high-purity aluminum targets are solved, and uniform grain refinement and optimization of structure are achieved.
Patent Information
- Application Number
- CN202411917270.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-24
- Publication Date
- 2025-03-14
AI Technical Summary
There are problems of grain refinement and low nucleation rate in the melting and casting process of high-purity aluminum targets.
A method of melting and casting of an aluminum target material includes melting the aluminum raw material into a liquid aluminum, and sequentially performing refining treatment, a first filtration treatment and a casting treatment. The specific steps include adding a first aluminum wire with a smaller diameter in the prestable stage of the casting process and performing a first stirring process, adding a second aluminum wire with a larger diameter in the steady state stage and performing a second stirring process, including ultrasonic and electromagnetic stirring processes.
Through this method, the grains of the aluminum target can be effectively refined, the grain uniformity and refinement effect can be improved, and the grain size of the tissue can be reduced.
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Figure CN119615081A_ABST
Abstract
Description
Technical Field
[0001] The present application relates to the technical field of target materials, and in particular to a method for melting and casting an aluminum target material. Background Art
[0002] Aluminum target is a kind of sputtering target used in vacuum coating industry. It is a product of high-purity aluminum material after a series of processing, with specific size and shape. With the increasing requirements for aluminum target, not only the purity of aluminum target is required to be high, but also the grain size, grain uniformity and texture orientation are strictly required. However, the nucleation rate of high-purity aluminum target (mass purity> 99.999%) is low, and there are problems such as difficulty in grain refinement. Summary of the invention
[0003] Based on this, an embodiment of the present application provides a method for melting and casting an aluminum target material with good grain refinement effect.
[0004] The present application provides a method for melting and casting an aluminum target material, and the method for melting and casting an aluminum target material comprises:
[0005] After melting the aluminum raw material to form aluminum liquid, the aluminum liquid is subjected to a refining process, a first filtering process and a casting process in sequence to prepare the aluminum target;
[0006] Wherein, a wire feeding treatment is performed on the aluminum liquid entering the casting process, and the casting process includes a pre-steady-state stage and a steady-state stage. The parameters of the casting process change in the pre-steady-state stage, and the parameters of the casting process do not change in the steady-state stage; when the casting process is in the pre-steady-state stage, the wire feeding treatment includes adding a first aluminum wire to the aluminum liquid, and performing a first stirring treatment on the aluminum liquid in the casting process; when the casting process is in the steady-state stage, the wire feeding treatment includes adding a second aluminum wire to the aluminum liquid, and performing a second stirring treatment on the aluminum liquid in the casting process; the diameter of the first aluminum wire is smaller than the diameter of the second aluminum wire, and the intensity of the first stirring treatment is smaller than the intensity of the second stirring treatment.
[0007] In some embodiments, the diameter of the first aluminum wire is 3 mm to 8 mm.
[0008] In some embodiments, the wire feeding process uses a wire feeding speed of the first aluminum wire of 80 cm / min to 120 cm / min.
[0009] In some embodiments, the diameter of the second aluminum wire is 8 mm to 12 mm.
[0010] In some embodiments, the wire feeding process uses a wire feeding speed of the second aluminum wire of 160 cm / min to 200 cm / min.
[0011] In some embodiments, the rate of change of the casting speed of the casting process during the pre-steady-state stage is >0.
[0012] In some embodiments, the rate of change of the cooling water flow rate of the casting process during the pre-steady-state stage is >0.
[0013] In some embodiments, the casting speed of the casting process in the steady state stage is 75 mm / min to 120 mm / min.
[0014] In some embodiments, the cooling water flow rate of the casting process in the steady state stage is 9m 3 / h~12m 3 / h.
[0015] In some embodiments, the first agitation treatment comprises a first ultrasonic treatment.
[0016] Optionally, the ultrasonic frequency of the first ultrasonic treatment is 5kHz~10kHz.
[0017] In some embodiments, the second stirring treatment includes a second electromagnetic stirring treatment and a second ultrasonic treatment.
[0018] Optionally, the frequency of the second electromagnetic stirring treatment is 4 Hz to 6 Hz, and the voltage is 7 V to 9 V.
[0019] Optionally, the ultrasonic frequency of the second ultrasonic treatment is 15kHz~25kHz.
[0020] In some embodiments, the aluminum outlet temperature of the casting process is 725°C to 750°C.
[0021] In some embodiments, the casting temperature of the casting process is 685°C to 705°C.
[0022] In some embodiments, the melting temperature is 700°C to 750°C.
[0023] In some embodiments, the mass purity of the aluminum raw material is ≥99.9995%.
[0024] In some embodiments, the aluminum target material melting and casting method further includes a second filtering treatment, wherein the second filtering treatment is used to filter the aluminum liquid after the wire feeding treatment, and the aluminum liquid after the second filtering treatment is cast.
[0025] In some embodiments, the mass purity of the aluminum target is ≥99.995%.
[0026] In some embodiments, the average grain size of the grains in the aluminum target is ≤1 mm.
[0027] In some embodiments, the structure of the aluminum target is equiaxed crystal.
[0028] Compared with the traditional technology, this application has at least the following beneficial effects:
[0029] The present application performs a wire feeding treatment on the aluminum liquid undergoing casting treatment. The wire feeding treatment is to add aluminum wire of the same material as the aluminum liquid into the aluminum liquid. The grain size of the aluminum wire formed by extrusion is relatively small. The aluminum wire melts after being added to the aluminum liquid, which reduces the temperature in the aluminum liquid and increases the nucleation rate of the aluminum liquid, thereby reducing the grain size of the ingot. Furthermore, in the pre-steady-state stage of the casting process, a first aluminum wire with a relatively small diameter is added and a first stirring treatment is performed, which not only allows the crystal nuclei to be initially formed and evenly distributed, but also effectively avoids the formation of feather crystals. In the steady-state stage, a second aluminum wire with a relatively large diameter is added and a second stirring treatment is performed, which can ensure that the grain size formed by the ingot is uniform and the grain refinement effect. BRIEF DESCRIPTION OF THE DRAWINGS
[0030] Figure 1 This is the sample tissue diagram of the aluminum target material prepared in Example 1 of the present application.
[0031] Figure 2 This is the sample microstructure diagram of the aluminum target material prepared in Example 7 of the present application.
[0032] Figure 3 This is the sample microstructure diagram of the aluminum target material prepared in Example 8 of the present application.
[0033] Figure 4 This is the sample tissue diagram of the aluminum target material prepared in Comparative Example 1 of the present application.
[0034] Figure 5 This is the sample tissue diagram of the aluminum target material prepared in Comparative Example 6 of the present application. DETAILED DESCRIPTION
[0035] Below in conjunction with the embodiments and examples, the present application is further described in detail. These embodiments and examples are only used to illustrate the present application and are not used to limit the scope of the present application. The purpose of providing these embodiments and examples is to make the understanding of the disclosure of the present application more thorough and comprehensive. It should also be understood that the present application can be implemented in many different forms, and is not limited to the embodiments and examples described herein. Those skilled in the art can make various changes or modifications without violating the connotation of the present application, and the equivalent form obtained also falls within the protection scope of the present application. In addition, in the description below, a large number of specific details are given in order to provide a more comprehensive understanding of the present application. It should be understood that the present application can be implemented without one or more of these details.
[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 belongs. The terms used herein in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application.
[0037] In this application, "optionally", "optional", and "optional" mean optional or dispensable, that is, any one of the two parallel schemes of "yes" or "no". If multiple "options" appear in a technical solution, unless otherwise specified and there is no contradiction or mutual restriction, each "optional" is independent.
[0038] In this application, the terms "first", "second", etc. in "the first aspect", "the second aspect", etc. are used only for descriptive purposes and cannot be understood as indicating or implying relative importance or quantity, nor can they be understood as implicitly indicating the importance or quantity of the indicated technical features. Moreover, "first", "second", etc. only serve the purpose of non-exhaustive enumeration and description, and it should be understood that they do not constitute a closed limitation on quantity.
[0039] In the present application, the technical features described in an open manner include closed technical solutions composed of the listed features, and also include open technical solutions containing the listed features.
[0040] In the present application, when it comes to a numerical interval (i.e., a numerical range), unless otherwise specified, the distribution of the optional numerical values in the numerical interval is considered to be continuous, and includes the two numerical endpoints (i.e., the minimum and maximum values) of the numerical interval, and each numerical value between the two numerical endpoints. Unless otherwise specified, when the numerical interval only refers to an integer in the numerical interval, it includes the two endpoint integers of the numerical range, and each integer between the two endpoints, which is equivalent to directly listing each integer. When multiple numerical ranges are provided to describe features or characteristics, these numerical ranges can be combined. In other words, unless otherwise specified, the numerical range disclosed in the present application should be understood to include any and all sub-ranges included therein. The "numerical value" in the numerical interval can be any quantitative value, such as a number, a percentage, a ratio, etc. "Numerical interval" allows for a broad range of quantitative intervals such as percentage intervals, ratio intervals, and ratio intervals.
[0041] All documents mentioned in this application are cited as references in this application, just as each document is cited as reference separately. Unless they conflict with the application purpose and / or technical solution of this application, the cited documents involved in this application are cited with all contents and all purposes. When the cited documents are involved in this application, the definitions of relevant technical features, terms, nouns, phrases, etc. in the cited documents are also cited. When the cited documents are involved in this application, the examples and preferred methods of the cited relevant technical features can also be incorporated into this application as references, but are limited to the implementation of this application. It should be understood that when the cited content conflicts with the description in this application, the present application shall prevail or be modified adaptively according to the description of this application.
[0042] In the traditional casting process, the aluminum liquid cools and solidifies in the crystallizer. During the cooling and solidification, the impurity elements in the aluminum liquid assist in nucleation, achieving the effect of grain refinement. However, due to the low impurity content in high-purity aluminum and the relatively regular arrangement of high-purity aluminum atoms, it is more inclined to nucleate and grow according to its own inherent lattice structure mode during crystallization, and is not easily disturbed by external impurities to produce more nucleation sites or change the grain growth path. Therefore, high-purity aluminum itself has difficulty in nucleation. During the cooling and solidification process, it starts to grow before enough nuclei are formed, and finally forms a relatively coarse grain structure.
[0043] The present application provides a method for melting and casting an aluminum target material, and the method for melting and casting an aluminum target material comprises:
[0044] After melting the aluminum raw material to form aluminum liquid, the aluminum liquid is subjected to a refining process, a first filtering process and a casting process in sequence to prepare the aluminum target;
[0045] Wherein, a wire feeding treatment is performed on the aluminum liquid entering the casting process, and the casting process includes a pre-steady-state stage and a steady-state stage. The parameters of the casting process change in the pre-steady-state stage, and the parameters of the casting process do not change in the steady-state stage; when the casting process is in the pre-steady-state stage, the wire feeding treatment includes adding a first aluminum wire to the aluminum liquid, and performing a first stirring treatment on the aluminum liquid in the casting process; when the casting process is in the steady-state stage, the wire feeding treatment includes adding a second aluminum wire to the aluminum liquid, and performing a second stirring treatment on the aluminum liquid in the casting process; the diameter of the first aluminum wire is smaller than the diameter of the second aluminum wire, and the intensity of the first stirring treatment is smaller than the intensity of the second stirring treatment.
[0046] The present application performs a wire feeding treatment on the aluminum liquid undergoing casting treatment. The wire feeding treatment is to add aluminum wire of the same material as the aluminum liquid into the aluminum liquid. The grain size of the aluminum wire formed by extrusion is relatively small. The aluminum wire melts after being added to the aluminum liquid, which reduces the temperature in the aluminum liquid and increases the nucleation rate of the aluminum liquid, thereby reducing the grain size of the ingot. Furthermore, in the pre-steady-state stage of the casting process, a first aluminum wire with a relatively small diameter is added and a first stirring treatment is performed, which not only allows the crystal nuclei to be initially formed and evenly distributed, but also effectively avoids the formation of feather crystals. In the steady-state stage, a second aluminum wire with a relatively large diameter is added and a second stirring treatment is performed, which can ensure that the grain size formed by the ingot is uniform and the grain refinement effect.
[0047] In some embodiments, the diameter of the first aluminum wire is 3 mm to 8 mm, for example, it can be 3.0 mm, 3.5 mm, 4.0 mm, 4.5 mm, 5.0 mm, 5.5 mm, 6.0 mm, 6.5 mm, 7.0 mm, 7.5 mm or 8.0 mm.
[0048] In some embodiments, the wire feeding process uses a wire feeding speed of the first aluminum wire of 80 cm / min to 120 cm / min, for example, it can be 80 cm / min, 85 cm / min, 90 cm / min, 95 cm / min, 100 cm / min, 105 cm / min, 110 cm / min, 115 cm / min or 120 cm / min.
[0049] When the aluminum liquid is in the pre-steady-state stage during the casting process, the diameter of the first aluminum wire and the wire feeding speed are selected as above in the present application, which can not only refine the grains, but also reduce the temperature change of the aluminum liquid, effectively avoid the formation of coarse grains and feather crystals, and avoid the cold shut and shrinkage defects caused by the sudden temperature drop caused by the addition of aluminum wire.
[0050] In some embodiments, the diameter of the second aluminum wire is 8 mm to 12 mm, for example, 8.0 mm, 8.5 mm, 9.0 mm, 9.5 mm, 10.0 mm, 10.5 mm, 11.0 mm, 11.5 mm or 12.0 mm.
[0051] In some embodiments, the wire feeding process uses a wire feeding speed of the second aluminum wire of 160 cm / min to 200 cm / min, for example, it can be 160 cm / min, 165 cm / min, 170 cm / min, 175 cm / min, 180 cm / min, 185 cm / min, 190 cm / min, 195 cm / min or 200 cm / min.
[0052] When the aluminum liquid is in a steady state during the casting process, the diameter of the second aluminum wire and the wire feeding speed are selected as above in the present application, which can improve the aluminum yield and optimize the melting process, and can reduce the surface area of the aluminum wire, thereby avoiding problems such as premature melting or insufficient melting of the aluminum wire, and excessive inclusions.
[0053] In some embodiments, the rate of change of the casting speed of the casting process in the pre-steady-state stage is greater than 0. It is understood that when the casting speed does not reach the set casting speed, the casting speed will gradually increase to the set casting speed; when the casting speed reaches the set casting speed, the casting speed remains stable and does not change.
[0054] In some embodiments, the rate of change of the cooling water flow rate of the casting process in the pre-steady-state stage is greater than 0. It is understood that when the cooling water flow rate does not reach the set cooling water flow rate, the cooling water flow rate will gradually increase to the set cooling water flow rate; when the cooling water flow rate reaches the set cooling water flow rate, the cooling water flow rate remains stable and does not change.
[0055] The present application detects the casting speed and cooling water flow parameters in the semi-solid casting process to determine whether the semi-solid casting process has reached a steady state, thereby effectively ensuring the process stability of the semi-solid casting process, simplifying the detection difficulty, and further ensuring the grain refinement effect during the casting process.
[0056] In some embodiments, the casting speed of the casting process in the steady state stage is 75 mm / min to 120 mm / min, for example, it can be 75 mm / min, 80 mm / min, 85 mm / min, 90 mm / min, 95 mm / min, 100 mm / min, 105 mm / min, 110 mm / min, 115 mm / min or 120 mm / min.
[0057] In some embodiments, the cooling water flow rate of the casting process in the steady state stage is 9m 3 / h~12m 3 / h, for example, it can be 9.0m 3 / h、9.5m 3 / h、10.0m 3 / h、10.5m 3 / h、11.0m 3 / h、11.5m 3 / h or 12.0m 3 / h.
[0058] In some embodiments, the first agitation treatment comprises a first ultrasonic treatment.
[0059] Optionally, the ultrasonic frequency of the first ultrasonic treatment is 5kHz~10kHz, for example, it can be 5.0kHz, 5.5kHz, 6.0kHz, 6.5kHz, 7.0kHz, 7.5kHz, 8.0kHz, 8.5kHz, 9.0kHz, 9.5kHz or 10.0kHz.
[0060] In the wire feeding process of the present application, when the first aluminum wire is added, ultrasonic vibration is performed on the aluminum liquid in the casting process. By further selecting the parameters of the ultrasonic vibration, the initial formation and uniform distribution of the crystal nuclei are improved, and the formation of feather crystals can be effectively avoided, thereby improving the quality of the ingot.
[0061] In some embodiments, the second stirring treatment includes a second electromagnetic stirring treatment and a second ultrasonic treatment.
[0062] Optionally, the frequency of the second electromagnetic stirring treatment is 4 Hz to 6 Hz, for example, 4 Hz, 5 Hz or 6 Hz, and can be 5 Hz.
[0063] Optionally, the voltage of the second electromagnetic stirring treatment is 7V to 9V, for example, 7V, 7.5V, 8V or 9V. The voltage of the electromagnetic stirring treatment selected in the present application as above can be coordinated with the frequency of the electromagnetic stirring treatment to effectively refine the grains and avoid affecting the casting quality due to the mixing and uneven temperature distribution inside the melt.
[0064] Optionally, the ultrasonic frequency of the second ultrasonic treatment is 15kHz~25kHz, for example, it can be 15kHz, 16kHz, 17kHz, 18kHz, 19kHz, 20kHz, 21kHz, 22kHz, 23kHz, 24kHz or 25kHz.
[0065] In the wire feeding process of the present application, when the second aluminum wire is added, the aluminum liquid in the casting process is subjected to electromagnetic stirring and ultrasonic vibration. Compared with the electromagnetic stirring and ultrasonic vibration when the first aluminum wire is added in the pre-steady state, the stirring effect is stronger, thereby enhancing the dendrite wall crushing effect, effectively reducing the grain size of the casting structure, and improving the uniformity of the grains.
[0066] In some embodiments, the aluminum outlet temperature of the casting process is 725°C to 750°C, for example, it can be 725°C, 730°C, 735°C, 740°C, 745°C or 750°C.
[0067] In some embodiments, the casting temperature of the casting process is 685°C to 705°C, for example, 685°C, 690°C, 695°C, 700°C or 705°C.
[0068] In some embodiments, the melting temperature is 700°C to 750°C, for example, 700°C, 705°C, 710°C, 715°C, 720°C, 725°C, 730°C, 735°C, 740°C, 745°C or 750°C.
[0069] In some embodiments, the mass purity of the aluminum raw material is ≥99.9995%.
[0070] In some embodiments, the aluminum target material melting and casting method further includes a second filtering treatment, wherein the second filtering treatment is used to filter the aluminum liquid after the wire feeding treatment, and perform a casting treatment on the aluminum liquid after the second filtering treatment.
[0071] The present application filters the aluminum liquid after wire feeding treatment, thereby effectively reducing the agglomerates generated during the wire feeding process, making the grain refinement effect of the casting more uniform, and improving the overall quality of the casting.
[0072] Optionally, the filter density of the second filtration treatment is 50 PPI to 60 PPI, for example, 50 PPI, 51 PPI, 52 PPI, 53 PPI, 54 PPI, 55 PPI, 56 PPI, 57 PPI, 58 PPI, 59 PPI or 60 PPI. PPI refers to the average number of pores per square inch.
[0073] In some embodiments, the refining process includes: introducing a refining gas into the aluminum liquid and stirring the liquid.
[0074] Optionally, the refining gas comprises at least one of argon and chlorine.
[0075] Optionally, the inlet flow rate of the refined gas is 10 L / min to 30 L / min, for example, it can be 10 L / min, 12 L / min, 14 L / min, 16 L / min, 18 L / min, 20 L / min, 22 L / min, 24 L / min, 26 L / min, 28 L / min or 30 L / min.
[0076] Optionally, the stirring speed is 300 rpm to 400 rpm, for example, it can be 300 rpm, 310 rpm, 320 rpm, 330 rpm, 340 rpm, 350 rpm, 360 rpm, 370 rpm, 380 rpm, 390 rpm or 400 rpm.
[0077] Optionally, the stirring time is ≥ 25 min.
[0078] In some embodiments, the first filtering treatment includes: sequentially performing first-stage filtering and second-stage filtering on the aluminum liquid after the refining treatment.
[0079] Optionally, the filter density of the first stage filtration is 30PPI~50PPI, for example, it can be 30PPI, 32PPI, 34PPI, 36PPI, 38PPI, 40PPI, 42PPI, 44PPI, 46PPI, 48PPI or 50PPI.
[0080] Optionally, the filter density of the second stage filtration is 50PPI~60PPI, for example, it can be 50PPI, 51PPI, 52PPI, 53PPI, 54PPI, 55PPI, 56PPI, 57PPI, 58PPI, 59PPI or 60PPI.
[0081] In some embodiments, the mass purity of the aluminum target is ≥99.9995%.
[0082] In some embodiments, the average grain size of the aluminum target is ≤1 mm, for example, 0.5 mm to 1 mm.
[0083] In some embodiments, the structure of the aluminum target is equiaxed crystal.
[0084] Exemplarily, a method for melting and casting the above-mentioned aluminum target material is provided, comprising the following steps:
[0085] S1. Melting aluminum raw materials with a mass purity of ≥99.9995% at 700°C~750°C to form aluminum liquid;
[0086] S2, introducing refining gas into the aluminum liquid in S1 and stirring, the refining gas flow rate is 10L / min~30L / min, the stirring speed is 300rpm~400rpm, and the time is ≥25min;
[0087] S3, performing first-stage filtration and second-stage filtration on the aluminum liquid refined in S2, wherein the filter density of the first-stage filtration is 30PPI~50PPI, and the filter density of the second-stage filtration is 50PPI~60PPI;
[0088] S4, feeding wire treatment to the aluminum liquid filtered in S3, when it is detected that the aluminum liquid is in the pre-steady-state stage during the casting process, adding a first aluminum wire to the aluminum liquid, the diameter of the first aluminum wire is 3mm~8mm, the wire feeding speed is 80cm / min~120cm / min, and at the same time, a first ultrasonic treatment of 5kHz~10kHz is applied to the aluminum liquid during the casting process; when it is detected that the aluminum liquid is in the steady-state stage during the casting process, adding a second aluminum wire to the aluminum liquid, the diameter of the second aluminum wire is 8mm~12mm, the wire feeding speed is 160cm / min~200cm / min, and at the same time, a second electromagnetic stirring treatment of 4Hz~6Hz and a voltage of 7V~9V and a second ultrasonic treatment of 15kHz~25kHz are applied to the aluminum liquid during the casting process;
[0089] S5, filtering the aluminum liquid after the wire feeding treatment in S4, and the filter density used in the filtering treatment is 30PPI~50PPI;
[0090] S6: Cast the aluminum liquid after filtering in S5. The outlet temperature of the casting process is 725℃~750℃, the casting temperature is 685℃~705℃, the casting speed is 75mm / min~120mm / min, and the cooling water flow rate is 9m 3 / h~12m 3 / h, and an aluminum target is prepared.
[0091] The embodiments of the present application will be described in detail below in conjunction with examples. It should be understood that these examples are only used to illustrate the present application and are not intended to limit the scope of the present application. The experimental methods for which specific conditions are not specified in the following examples are preferably referred to the guidance provided in the present application, and can also be based on the experimental manual or normal conditions in this area, can also be based on the conditions recommended by the manufacturer, or refer to experimental methods known in the art.
[0092] Example 1
[0093] S1. Melting aluminum raw material with a mass purity of 99.9995% at 730° C. to form aluminum liquid;
[0094] S2, introducing argon and chlorine in a volume ratio of 20:1 into the aluminum liquid in S1 and stirring, the gas flow rate is 20L / min, the stirring speed is 350rpm, and the time is 30min;
[0095] S3, performing first-stage filtration and second-stage filtration on the aluminum liquid refined in S2, wherein the filter density of the first-stage filtration is 40PPI, and the filter density of the second-stage filtration is 50PPI;
[0096] S4: Feed the aluminum liquid filtered in S3 with wire. When it is detected that the aluminum liquid is in the pre-steady-state stage during the casting process, that is, the casting speed during the casting process does not reach 100 mm / min, and the cooling water flow rate does not reach 11 m 3 / h, add a first aluminum wire into the aluminum liquid, the diameter of the first aluminum wire is 5mm, the wire feeding speed is 100cm / min, and at the same time, apply a first ultrasonic treatment of 10kHz to the aluminum liquid in the casting process; when it is detected that the aluminum liquid in the casting process is in a steady state stage, that is, the casting speed in the casting process reaches 100mm / min and remains stable, and the cooling water flow rate reaches 11m 3 / h and remain stable, add a second aluminum wire into the aluminum liquid, the diameter of the second aluminum wire is 10mm, the wire feeding speed is 180cm / min, and at the same time, apply a second electromagnetic stirring treatment of 5Hz and 8V voltage and a second ultrasonic treatment of 20kHz to the aluminum liquid in the casting process;
[0097] S5, filtering the aluminum liquid after the wire feeding treatment in S4, and the filter density used in the filtering treatment is 50PPI;
[0098] S6: Cast the aluminum liquid after filtering in S5. The outlet temperature of the casting treatment is 730℃, the casting temperature is 695℃, the casting speed is 100mm / min, and the cooling water flow rate is 11m 3 / h, and an aluminum target is prepared.
[0099] Example 2
[0100] S1. Melting aluminum raw material with a mass purity of 99.9995% at 750° C. to form aluminum liquid;
[0101] S2, introducing argon and chlorine in a volume ratio of 20:1 into the aluminum liquid in S1 and stirring, the gas flow rate is 20L / min, the stirring speed is 350rpm, and the time is 30min;
[0102] S3, performing first-stage filtration and second-stage filtration on the aluminum liquid refined in S2, wherein the filter density of the first-stage filtration is 40PPI, and the filter density of the second-stage filtration is 50PPI;
[0103] S4: Feed the aluminum liquid filtered in S3 with wire. When it is detected that the aluminum liquid is in the pre-steady-state stage during the casting process, that is, the casting speed during the casting process does not reach 75 mm / min, and the cooling water flow rate does not reach 9 m 3 / h, add a first aluminum wire into the aluminum liquid, the diameter of the first aluminum wire is 3mm, the wire feeding speed is 120cm / min, and at the same time, apply a first ultrasonic treatment of 5kHz to the aluminum liquid in the casting process; when it is detected that the aluminum liquid in the casting process is in a steady state stage, that is, the casting speed in the casting process reaches 75mm / min and remains stable, and the cooling water flow rate reaches 9m 3 / h and remain stable, add a second aluminum wire into the aluminum liquid, the diameter of the second aluminum wire is 8mm, the wire feeding speed is 200cm / min, and at the same time, apply a second electromagnetic stirring treatment of 5Hz and 7V voltage and a second ultrasonic treatment of 15kHz to the aluminum liquid in the casting process;
[0104] S5, filtering the aluminum liquid after the wire feeding treatment in S4, and the filter density used in the filtering treatment is 30PPI;
[0105] S6: Cast the aluminum liquid after filtering in S5. The outlet temperature of the casting treatment is 750℃, the casting temperature is 705℃, the casting speed is 75mm / min, and the cooling water flow rate is 9m 3 / h, and an aluminum target is prepared.
[0106] Example 3
[0107] S1. Melting aluminum raw material with a mass purity of 99.9995% at 730° C. to form aluminum liquid;
[0108] S2, introducing argon and chlorine in a volume ratio of 20:1 into the aluminum liquid in S1 and stirring, the gas flow rate is 20L / min, the stirring speed is 350rpm, and the time is 30min;
[0109] S3, performing first-stage filtration and second-stage filtration on the aluminum liquid refined in S2, wherein the filter density of the first-stage filtration is 40PPI, and the filter density of the second-stage filtration is 50PPI;
[0110] S4: Feed the aluminum liquid filtered in S3 with wire. When it is detected that the aluminum liquid is in the pre-steady-state stage during the casting process, that is, the casting speed during the casting process does not reach 120 mm / min, and the cooling water flow rate does not reach 12 m 3 / h, add a first aluminum wire into the aluminum liquid, the diameter of the first aluminum wire is 8mm, the wire feeding speed is 80cm / min, and at the same time, a first ultrasonic treatment of 10kHz is applied to the aluminum liquid in the casting process; when it is detected that the aluminum liquid in the casting process is in a steady state stage, that is, the casting speed in the casting process reaches 120mm / min and remains stable, and the cooling water flow rate reaches 12m 3 / h and remain stable, add a second aluminum wire into the aluminum liquid, the diameter of the second aluminum wire is 12mm, the wire feeding speed is 160cm / min, and at the same time, apply a second electromagnetic stirring treatment of 5Hz and 9V voltage and a second ultrasonic treatment of 25kHz to the aluminum liquid in the casting process;
[0111] S5, filtering the aluminum liquid after the wire feeding treatment in S4, and the filter density used in the filtering treatment is 40PPI;
[0112] S6: Cast the aluminum liquid after filtering in S5. The outlet temperature of the aluminum casting treatment is 725℃, the casting temperature is 685℃, the casting speed is 120mm / min, and the cooling water flow rate is 12m 3 / h, and an aluminum target is prepared.
[0113] Example 4
[0114] An aluminum target material was prepared according to the method of Example 1, except that the diameter of the first aluminum wire was 9 mm.
[0115] Example 5
[0116] An aluminum target material was prepared according to the method of Example 1, except that the diameter of the second aluminum wire was 6 mm.
[0117] Example 6
[0118] An aluminum target material was prepared according to the method of Example 1, except that the diameter of the second aluminum wire was 14 mm.
[0119] Example 7
[0120] An aluminum target material is prepared according to the method of Example 1, except that during the casting process, the aluminum liquid is not subjected to the first ultrasonic treatment and the second ultrasonic treatment.
[0121] Example 8
[0122] An aluminum target material is prepared according to the method of Example 1, except that during the casting process, the aluminum liquid is not subjected to the second electromagnetic stirring process.
[0123] Example 9
[0124] An aluminum target material is prepared according to the method of Example 1, except that the aluminum liquid is not filtered after the wire feeding process.
[0125] Comparative Example 1
[0126] An aluminum target material is prepared according to the method of Example 1, except that the wire feeding process in step S4 is not performed.
[0127] Comparative Example 2
[0128] An aluminum target material is prepared according to the method of Example 1, except that the first aluminum wire is not used for wire feeding treatment in the pre-steady-state stage of the casting process.
[0129] Comparative Example 3
[0130] An aluminum target material is prepared according to the method of Example 1, except that the second aluminum wire is not used for wire feeding treatment in the steady-state stage of the casting process.
[0131] Comparative Example 4
[0132] An aluminum target material was prepared according to the method of Example 1, except that the diameters of the first aluminum wire and the second aluminum wire were both 5 mm.
[0133] Comparative Example 5
[0134] An aluminum target material was prepared according to the method of Example 1, except that the diameters of the first aluminum wire and the second aluminum wire were both 10 mm.
[0135] Comparative Example 6
[0136] An aluminum target material is prepared according to the method of Example 1, except that when the first aluminum wire is added, the aluminum liquid in the casting process is not subjected to the first ultrasonic treatment; and when the second aluminum wire is added, the aluminum liquid in the casting process is not subjected to the second ultrasonic treatment and the second electromagnetic stirring treatment.
[0137] Comparative Example 7
[0138] An aluminum target material is prepared according to the method of Example 1, except that when the first aluminum wire is added, the aluminum liquid in the casting process is not subjected to the first ultrasonic treatment.
[0139] Comparative Example 8
[0140] An aluminum target material is prepared according to the method of Example 1, except that when the second aluminum wire is added, the aluminum liquid in the casting process is not subjected to the second ultrasonic treatment and the second electromagnetic stirring treatment.
[0141] The aluminum target materials prepared in the above embodiments and comparative examples are subjected to sample sawing and macroscopic etching, including:
[0142] The φ142 cast rod was sawn into a suitable length and then sawn into a 20 mm thick sample along the longitudinal direction. The large surface of the sample was milled on one side and then macro-etched with 10% sodium hydroxide. The sample structure after corrosion was observed, and the test results are shown in Table 1. Among them, the sample structure of Example 1 is as follows Figure 1 As shown, the sample tissue of Example 7 is as follows Figure 2 As shown, the sample tissue of Example 8 is as follows Figure 3 As shown, the sample tissue of Comparative Example 1 is as follows Figure 4 As shown, the sample tissue of Comparative Example 6 is as follows Figure 5 shown.
[0143] Table 1
[0144]
[0145] Note: The target material contains columnar crystals, stable columnar crystals, pre-stable equiaxed crystals and pre-stable inclusions, which will affect the thermal stability and organizational structure of the ingot, and the corrosion resistance will deteriorate.
[0146] From the above table we can see that:
[0147] (1) Compared with Examples 4-6, it can be seen that the present invention controls the diameter of the aluminum wire in the wire feeding process, which can effectively improve the grain refinement effect and form a more uniform microstructure.
[0148] (2) Compared with Examples 7-8, it can be seen that the present application can effectively achieve microstructure refinement and improve casting quality through the coordinated cooperation of ultrasonic treatment and electromagnetic stirring treatment.
[0149] (3) Compared with Example 9, it can be seen that the present application filters the aluminum liquid after the wire feeding process, effectively reducing inclusions and thus improving the purity of the aluminum liquid.
[0150] (4) Compared with Comparative Examples 1-8, it can be seen that the present application performs a wire feeding treatment on the aluminum liquid undergoing the casting treatment. The wire feeding treatment is to add aluminum wire of the same material as the aluminum liquid into the aluminum liquid. The grain size of the aluminum wire formed by extrusion is relatively small. The aluminum wire melts after being added to the aluminum liquid, which reduces the temperature in the aluminum liquid and increases the nucleation rate of the aluminum liquid, thereby reducing the grain size of the ingot. Furthermore, adding a first aluminum wire with a relatively small diameter and performing a first stirring treatment in the pre-steady-state stage of the casting treatment can not only allow the crystal nuclei to be initially formed and evenly distributed, but also effectively avoid the formation of feather crystals. Adding a second aluminum wire with a relatively large diameter and performing a second stirring treatment in the steady-state stage can ensure that the grain size formed by the ingot is uniform and the grain refinement effect.
[0151] In summary, the melting and casting method of the aluminum target material of the present application includes the following characteristics:
[0152] (1) The present application performs wire feeding processing on the aluminum liquid entering the casting process by adding aluminum wire of the same material as the aluminum liquid, wherein the grain size of the aluminum wire formed by the extruded wire is smaller, and the aluminum wire is partially melted to reduce the temperature of the aluminum liquid inside the crystallizer. At the same time, the melted aluminum wire increases the nucleation rate of the aluminum liquid in the crystallizer, thereby reducing the grain size of the cast structure.
[0153] (2) This application divides the wire feeding treatment liquid into two stages according to the pre-steady-state stage and the steady-state stage of the aluminum liquid in the casting process. In the pre-steady-state stage, a first aluminum wire with a smaller diameter is added, assisted by relatively weak ultrasonic vibration, so that the crystal nuclei are initially formed and distributed. In the steady-state stage, a second aluminum wire with an increased diameter is added, electromagnetic stirring is added, and the ultrasonic frequency is enhanced to strengthen the dendrite wall crushing effect and effectively reduce the grain size of the casting structure.
[0154] (3) After the wire feeding process, the aluminum liquid is filtered to effectively reduce the agglomerates generated during the wire feeding process, making the grain refinement effect of the casting more uniform and improving the overall quality of the casting.
[0155] (4) The present application introduces ultrasonic and electromagnetic stirring while feeding the wire, which can not only improve the dispersion of the aluminum wire, but also can secondary crush the dendrites after nucleation, form more nucleation points, and obtain an ingot with a grain size of less than 1 mm.
[0156] (5) The present application adds homogeneous aluminum wire to the aluminum liquid solution, which can accurately control the added elements, avoiding the uncertainty of traditional casting while ensuring the consistency and repeatability of the results.
[0157] (6) The aluminum target material melting and casting method of the present application is suitable for industrial mass production.
[0158] The technical features of the above-described embodiments may be arbitrarily combined. To make the description concise, not all possible combinations of the technical features in the above-described 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.
[0159] The above-described embodiments only express several implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be construed as limiting the scope of the application. It should be noted that, for a person of ordinary skill in the art, several modifications and improvements can be made without departing from the concept of the present application, and these all belong to the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the attached claims.
Claims
1. A method for melting and casting an aluminum target, characterized in that: The melting and casting method of the aluminum target material comprises: After melting the aluminum raw material to form aluminum liquid, the aluminum liquid is subjected to a refining process, a first filtering process and a casting process in sequence to prepare the aluminum target; Wherein, a wire feeding treatment is performed on the aluminum liquid entering the casting process, and the casting process includes a pre-steady-state stage and a steady-state stage. The parameters of the casting process change in the pre-steady-state stage, and the parameters of the casting process do not change in the steady-state stage; when the casting process is in the pre-steady-state stage, the wire feeding treatment includes adding a first aluminum wire to the aluminum liquid, and performing a first stirring treatment on the aluminum liquid in the casting process; when the casting process is in the steady-state stage, the wire feeding treatment includes adding a second aluminum wire to the aluminum liquid, and performing a second stirring treatment on the aluminum liquid in the casting process; the diameter of the first aluminum wire is smaller than the diameter of the second aluminum wire, and the intensity of the first stirring treatment is smaller than the intensity of the second stirring treatment.
2. The method for melting and casting an aluminum target according to claim 1, characterized in that: The wire feeding process satisfies at least one of the following conditions: (1) The diameter of the first aluminum wire is 3 mm to 8 mm; (2) The wire feeding process uses a wire feeding speed of the first aluminum wire of 80 cm / min to 120 cm / min.
3. The method for melting and casting an aluminum target according to claim 1, wherein: The wire feeding process also satisfies at least one of the following conditions: (1) The diameter of the second aluminum wire is 8 mm to 12 mm; (2) The wire feeding process uses a wire feeding speed of the second aluminum wire of 160 cm / min to 200 cm / min.
4. The method for melting and casting an aluminum target according to claim 1, wherein: The parameters of the casting process in the pre-steady-state stage satisfy at least one of the following conditions: (1) the rate of change of the casting speed of the casting process in the pre-steady-state stage is greater than 0; (2) The rate of change of the cooling water flow rate of the casting process in the pre-steady-state stage is greater than 0.
5. The method for melting and casting an aluminum target according to claim 1, wherein: The parameters of the casting process in the steady state stage satisfy at least one of the following conditions: (1) The casting speed of the casting process in the steady state stage is 75 mm / min to 120 mm / min; (2) The cooling water flow rate of the casting process in the steady state stage is 9m 3 / h~12m 3 / h.
6. The method for melting and casting an aluminum target according to claim 1, wherein: The first stirring treatment comprises a first ultrasonic treatment; Optionally, the ultrasonic frequency of the first ultrasonic treatment is 5kHz~10kHz.
7. The method for melting and casting an aluminum target according to claim 1, wherein: The second stirring treatment includes a second electromagnetic stirring treatment and a second ultrasonic treatment; Optionally, the frequency of the second electromagnetic stirring treatment is 4 Hz to 6 Hz, and the voltage is 7 V to 9 V; Optionally, the ultrasonic frequency of the second ultrasonic treatment is 15kHz~25kHz.
8. The method for melting and casting an aluminum target according to any one of claims 1 to 7, characterized in that: The aluminum target material melting and casting method also satisfies at least one of the following conditions: (1) The aluminum outlet temperature of the casting process is 725°C to 750°C; (2) The casting temperature of the casting process is 685°C to 705°C; (3) The melting temperature is 700°C to 750°C; (4) The mass purity of the aluminum raw material is ≥99.9995%.
9. The method for melting and casting an aluminum target according to any one of claims 1 to 7, characterized in that: The smelting and casting method of the aluminum target material also includes a second filtering treatment, wherein the second filtering treatment is used to filter the aluminum liquid after the wire feeding treatment, and to perform a casting treatment on the aluminum liquid after the second filtering treatment.
10. The method for melting and casting an aluminum target according to any one of claims 1 to 7, characterized in that: The aluminum target material satisfies at least one of the following conditions: (1) The mass purity of the aluminum target is ≥99.9995%; (2) The average grain size of the aluminum target is ≤1 mm; (3) The structure of the aluminum target is equiaxed crystal.