Method for preparing copper target material through electron beam melting

Abstract

The invention provides a method for preparing a copper target material through electron beam smelting, which comprises the following steps: S1, preparation of a high-purity copper ingot: directly filling pretreated 4N cathode copper into a crystallizer of an electron beam smelting furnace, vacuumizing a furnace body of the electron beam furnace, and starting an electron gun to be aligned with the crystallizer for smelting and purifying to obtain purified 5N cathode copper liquid; and S2, crystal grain control is conducted, specifically, the electronic gun is shut down immediately, a vibrator is started, the vibration frequency is adjusted to be 2-10 times / 30 S, vibration is conducted for 3-10 min, the vibrator is shut down, the electronic gun is started again, the power is adjusted to be 10-40 KW, rotating disturbance is conducted towards the center along the inner edge of the crystallizer for 15-30 S, and a silver-copper alloy cast ingot is obtained after cooling. According to the method, the step of preparing the target material is simplified to be completed in one step in the electron beam furnace in the smelting process, and the grain size of the silver-copper alloy target material prepared through the steps of alloy preparation and grain control is smaller than or equal to 100 micrometers.

Description

Technical Field

[0001] The invention relates to the field of nonferrous metal purification, and in particular to a method for preparing a copper target material by electron beam melting. Background Art

[0002] In recent years, with the increasing development of sputtering target materials and technologies, the importance of sputtering target materials has become increasingly apparent in sputtering technology. The quality of the target material will directly affect the quality of the coating. During the sputtering process, the atoms on the surface of the target material are sputtered out in the form of ions and fall on the surface of the substrate to form a thin film. The material can be coated to improve the surface hardness, wear resistance, corrosion resistance, and heat resistance of the material to meet the different use requirements of the material. The key to vacuum magnetron sputtering coating lies in the target material used.

[0003] The main application areas of high-purity copper are the preparation of high-purity copper targets, advanced audio product conductors, fatigue-resistant cables and interconnect materials. High-purity copper is often used as interconnect material due to its high electromigration resistance and low resistance. As the characteristic dimensions of metal interconnects develop towards the nanoscale, the width of metal interconnects continues to decrease, and the number of layers of metal interconnects continues to increase. The original pure copper target process has problems with electromigration and oxidation and cannot meet current needs.

[0004] Therefore, it is necessary to provide a method for preparing copper target material by electron beam melting to solve the above technical problems. Summary of the invention

[0005] The invention provides a method for preparing a copper target material by electron beam melting, which solves the problems of electromigration and oxidation in the original pure copper target material process.

[0006] In order to solve the above technical problems, the present invention provides a method for preparing a copper target material by electron beam melting, comprising the following steps: S1. Preparation of high-purity copper ingot: directly load the pretreated 4N cathode copper into the crystallizer of the electron beam melting furnace, then evacuate the electron beam furnace body, and then turn on the electron gun to aim at the crystallizer for melting and purification to obtain the purified 5N cathode copper liquid; S2. Grain control: Immediately turn off the electron gun, turn on the vibrator, adjust the vibration frequency to 2-10 times / 30S, vibrate for 3-10min, turn off the vibrator, turn on the electron gun again, adjust the power to 10-40KW, rotate and disturb along the inner edge of the crystallizer toward the center for 15-30S, and obtain a silver-copper alloy ingot after cooling.

[0007] Preferably, the disturbance of the electron beam in S1 can play the role of stirring the mixed melt and refining the grains.

[0008] Preferably, the function of the vibrator in S2 is to break the grains and reduce the porosity of the matrix.

[0009] Preferably, the vacuum degree of the electron beam furnace chamber in S1 is 1.5×10-1Pa.

[0010] Preferably, the 4N cathode copper in S1 needs to be pretreated, and the pretreatment of the 4N cathode copper uses a 10% NaOH solution to clean oil stains, and then rinses it clean for use.

[0011] Preferably, the purification power of the electron gun in S1 is 20-25 kW, and the time is 20-30 minutes.

[0012] Preferably, the number and sequence of the grain control steps in S1 and S2 can be adjusted according to the grain size to be achieved and the porosity requirements of the target material. Each time after the electron gun is turned on for the second time, the power of the electron gun needs to be adjusted to 50-100KW, and the disturbance is controlled within 10S. The purpose of adjusting the high power is to quickly melt and control the matrix loss rate.

[0013] Preferably, the 4N cathode copper pretreatment in S1 comprises the following steps: S11. Preparation: S112. Ensure that the operating environment is well ventilated; S113. Prepare the necessary equipment and materials, including alkali-resistant containers, stirrers, personal protective equipment such as protective gloves and goggles, and accurately prepared 10% NaOH solution; S12, soaking treatment: S121. Place the cathode copper in an alkali-resistant container and pour in a sufficient amount of 10% NaOH solution to ensure that the cathode copper is completely immersed in the solution; S122, determining the soaking time according to the degree of oil pollution and the size of cathode copper; S13, stirring and cleaning: S131. During the soaking process, a stirrer may be used to stir slowly to accelerate the reaction between the oil stain and the NaOH solution and improve the cleaning effect; S132, after the immersion is completed, the cathode copper is taken out from the solution and rinsed with clean water to remove the residual NaOH solution and reaction products; S14, Inspection and Drying: S141, check whether the oil stains on the surface of the cathode copper are completely removed. If there are still residual oil stains, repeat the above steps to clean again; S142. After cleaning, place the cathode copper in a well-ventilated place to dry naturally or use drying equipment to dry it, ensuring that there is no moisture remaining on the surface of the cathode copper.

[0014] Preferably, a processing device is required for stirring and cleaning the cathode copper in S13, and the processing device includes a workbench, the surface of the workbench is connected to a box body, the bottom of the inner wall of the box body is connected to a circular limit seat, a container is arranged inside the circular limit seat, a base is connected to the center position of one end of the workbench, a stirring device is arranged on the surface of the base, the stirring device includes a telescopic frame, a motor is installed on one side of the surface of the telescopic frame, and one end of the motor output shaft is fixedly connected to a stirring member through a coupling.

[0015] Preferably, a shielding assembly is provided on the surface of the container, and the shielding assembly includes a shielding plate, one side of the shielding plate is connected to a first magnetic block, the bottom of the first magnetic block is magnetically connected to a second magnetic block, and the second magnetic block is connected to the surface of the container.

[0016] Compared with the related art, the method for preparing copper target by electron beam melting provided by the present invention has the following beneficial effects: Electron beam melting to prepare high-purity metals has the characteristics of high production efficiency and good purification effect. The present invention simplifies the steps of preparing the target material to complete the melting process in one step in the electron beam furnace. The silver-copper alloy target material prepared by the alloy preparation and grain control steps has fine grains ≤100μm, uniform, free of pores and inclusions, and the purity meets the 5N standard; It only needs to install a vibrator on the cooling bed in the three-gun electron beam furnace to interfere with the growth of dendrites during the cooling process and play a role in refining the grains. It requires little modification to the existing equipment, is easy to implement, and is suitable for industrial promotion. During the process of electron beam melting, purification and grain control, the loss rate in the melting and grain control process is controlled within 10% by controlling the electron beam power and melting time. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 A schematic structural diagram of a first embodiment of a method for preparing a copper target material by electron beam melting provided by the present invention; Figure 2 This is the metallographic structure diagram of the silver-copper alloy target; Figure 3 A schematic structural diagram of a second embodiment of a method for preparing a copper target material by electron beam melting provided by the present invention; Figure 4 for Figure 3 An enlarged schematic diagram of part A is shown; Figure 5 for Figure 3 The three-dimensional structural schematic diagram of the entire device is shown.

[0018] Numbers in the figure: 1. crystallizer; 2. vibrator; 3. workbench; 4. box body; 5. circular limit seat; 6. placement container; 7. base; 8. stirring device; 81. telescopic frame; 82. motor; 83. stirring element; 9. shielding assembly; 91. shielding plate; 92. first magnetic block; 93. second magnetic block. DETAILED DESCRIPTION

[0019] The present invention will be further described below in conjunction with the accompanying drawings and implementation modes.

[0020] First embodiment Please refer to Figure 1 and Figure 2 ,in, Figure 1 A schematic structural diagram of a first embodiment of a method for preparing a copper target material by electron beam melting provided by the present invention; Figure 2 A method for preparing a copper target material by electron beam melting comprises the following steps: S1. Preparation of high-purity copper ingot: directly load the pretreated 4N cathode copper into the crystallizer 1 of the electron beam melting furnace, then evacuate the electron beam furnace body, and then turn on the electron gun to aim at the crystallizer 1 for melting and purification to obtain the purified 5N cathode copper liquid; S2. Grain control: Immediately turn off the electron gun, turn on vibrator 2, adjust the vibration frequency to 2-10 times / 30S, vibrate for 3-10min, turn off vibrator 2, turn on the electron gun again, adjust the power to 10-40KW, rotate and disturb along the inner edge of the crystallizer toward the center for 15-30S, and obtain a silver-copper alloy ingot after cooling.

[0021] The disturbance of the electron beam in S1 can stir the mixed melt and refine the grains.

[0022] The function of the vibrator in S2 is to break up the grains and reduce the porosity of the matrix.

[0023] The vacuum degree of the electron beam furnace chamber in S1 is 1.5×10 -1 Pa.

[0024] The 4N cathode copper in S1 needs to be pretreated. The 4N cathode copper is pretreated by using a 10% NaOH solution to clean the oil stains and then rinsed clean for later use.

[0025] The purification power of the electron gun in S1 is 20-25 kW, and the purification time is 20-30 minutes.

[0026] The grain control steps in S1 and S2 can be adjusted in number and order according to the grain size to be achieved and the porosity of the target material. Each time after the second electron gun is turned on, the power of the electron gun needs to be adjusted to 50-100KW, and the disturbance is controlled within 10S. The purpose of adjusting the high power is to quickly melt and control the matrix loss rate.

[0027] Compared with the related art, the method for preparing copper target by electron beam melting provided by the present invention has the following beneficial effects: The present invention provides a method for preparing a copper target material by electron beam melting. The preparation of high-purity metal by electron beam melting has the characteristics of high production efficiency and good purification effect. The present invention simplifies the steps of preparing the target material to complete the melting process in one step in an electron beam furnace. The silver-copper alloy target material prepared by the alloy preparation and grain control steps has fine grains of ≤100 μm, uniform, free of pores and inclusions, and the purity meets the 5N standard. It only needs to install a vibrator on the cooling bed in the three-gun electron beam furnace to interfere with the growth of dendrites during the cooling process and play a role in refining the grains. It requires little modification to the existing equipment, is easy to implement, and is suitable for industrial promotion. During the process of electron beam melting, purification and grain control, the loss rate in the melting and grain control process is controlled within 10% by controlling the electron beam power and melting time.

[0028] Second embodiment Please refer to Figure 3 , Figure 4 and Figure 5 Based on the method for preparing a copper target material by electron beam melting provided in the first embodiment of the present application, the second embodiment of the present application proposes another method for preparing a copper target material by electron beam melting. The second embodiment is only a preferred embodiment of the first embodiment, and the implementation of the second embodiment will not affect the independent implementation of the first embodiment.

[0029] Specifically, the difference of the method for preparing a copper target material by electron beam melting provided in the second embodiment of the present application is that, in the method for preparing a copper target material by electron beam melting, the 4N cathode copper pretreatment in S1 comprises the following steps: S11. Preparation: S112. Ensure that the operating environment is well ventilated; S113. Prepare the necessary equipment and materials, including alkali-resistant containers, stirrers, personal protective equipment such as protective gloves and goggles, and accurately prepared 10% NaOH solution; S12, soaking treatment: S121. Place the cathode copper in an alkali-resistant container and pour in a sufficient amount of 10% NaOH solution to ensure that the cathode copper is completely immersed in the solution; S122, determining the soaking time according to the degree of oil pollution and the size of cathode copper; S13, stirring and cleaning: S131. During the soaking process, a stirrer may be used to stir slowly to accelerate the reaction between the oil stain and the NaOH solution and improve the cleaning effect; S132, after the immersion is completed, the cathode copper is taken out from the solution and rinsed with clean water to remove the residual NaOH solution and reaction products; S14, Inspection and Drying: S141, check whether the oil stains on the surface of the cathode copper are completely removed. If there are still residual oil stains, repeat the above steps to clean again; S142. After cleaning, place the cathode copper in a well-ventilated place to dry naturally or use drying equipment to dry it, ensuring that there is no moisture remaining on the surface of the cathode copper.

[0030] When the cathode copper is stirred and cleaned in S13, a processing device is required, and the processing device includes a workbench 3, the surface of the workbench 3 is connected to a box body 4, the bottom of the inner wall of the box body 4 is connected to a circular limit seat 5, and a container 6 is arranged inside the circular limit seat 5, a base 7 is connected to the center position of one end of the workbench 3, and a stirring device 8 is arranged on the surface of the base 7, and the stirring device 8 includes a telescopic frame 81, a motor 82 is installed on one side of the surface of the telescopic frame 81, and one end of the output shaft of the motor 82 is fixedly connected to a stirring member 83 through a coupling.

[0031] A shielding assembly 9 is provided on the surface of the placement container 6, and the shielding assembly 9 includes a shielding plate 91, and a first magnetic block 92 is connected to one side of the shielding plate 91, and the bottom of the first magnetic block 92 is magnetically connected to a second magnetic block 93, and the second magnetic block 93 is connected to the surface of the placement container 6.

[0032] A placement container 5 is arranged on the surface of the base 3 for use with a stirring device 8 and a blocking assembly 9, so that when the 4N cathode copper is placed in the container for immersion, it can be automatically and slowly processed.

[0033] The first magnetic block 92 and the second magnetic block 93 are circular, and a mounting through hole adapted to the stirring member 83 is provided at the center of one side of the shielding plate 91 .

[0034] The box body 4 can be used to store the solution dripping from the stirring member 83 when the placement container 6 is taken out from the box body 4 , and the circular limiting seat 5 is used to fix the placement container 6 .

[0035] During use, when immersing and stirring the 4N cathode copper, first place the 4N cathode copper inside the placement container 6 and add the treatment solution. After adding the treatment solution and 4N cathode copper inside the placement container 6, place the placement container 6 inside the circular limit seat 5 inside the box body 4, and then move the motor 82 with the stirring member 83 to the inside of the placement container 6 through the telescopic frame 81, and then install the baffle plate 91 with the first magnetic block 92 on the top of the placement container 6 and connect it to the second magnetic block 93, and then start the motor 82 to slowly drive the stirring member 83 to drive the 4N cathode copper to stir inside the placement container 6.

[0036] Compared with the related art, the method for preparing copper target by electron beam melting provided by the present invention has the following beneficial effects: The present invention provides a method for preparing a copper target material by electron beam melting. During the pretreatment of 4N cathode copper, the 4N cathode copper can be treated in a more refined manner through soaking treatment, stirring and cleaning, and inspection and drying operations, thereby preventing problems from occurring during the pretreatment of the 4N cathode copper and affecting subsequent operations.

[0037] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.

Claims

1. A method for preparing a copper target by electron beam melting, characterized in that: The following steps are involved: S1. Preparation of high-purity copper ingot: directly load the pretreated 4N cathode copper into the crystallizer of the electron beam melting furnace, then evacuate the electron beam furnace body, and then turn on the electron gun to aim at the crystallizer for melting and purification to obtain the purified 5N cathode copper liquid; S2. Grain control: Immediately turn off the electron gun, turn on the vibrator, adjust the vibration frequency to 2-10 times / 30S, vibrate for 3-10min, turn off the vibrator, turn on the electron gun again, adjust the power to 10-40KW, rotate and disturb along the inner edge of the crystallizer toward the center for 15-30S, and obtain a silver-copper alloy ingot after cooling.

2. The method for preparing a copper target by electron beam melting according to claim 1, characterized in that: The disturbance of the electron beam in S1 can stir the mixed melt and refine the grains.

3. The method for preparing a copper target by electron beam melting according to claim 1, characterized in that: The function of the vibrator in S2 is to break up the grains and reduce the porosity of the matrix.

4. The method for preparing a copper target by electron beam melting according to claim 1, characterized in that: The vacuum degree of the electron beam furnace chamber in S1 is 1.5×10-1Pa.

5. The method for preparing a copper target by electron beam melting according to claim 1, characterized in that: The 4N cathode copper in S1 needs to be pretreated. The 4N cathode copper is pretreated by using a 10% NaOH solution to clean the oil stains and then rinsed clean for later use.

6. The method for preparing a copper target by electron beam melting according to claim 1, characterized in that: The purification power of the electron gun in S1 is 20-25 kW, and the purification time is 20-30 minutes.

7. The method for preparing a copper target by electron beam melting according to claim 1, characterized in that: The grain control steps in S1 and S2 can be adjusted in number and order according to the grain size to be achieved and the porosity of the target material. Each time after the second electron gun is turned on, the power of the electron gun needs to be adjusted to 50-100KW, and the disturbance is controlled within 10S. The purpose of adjusting the high power is to quickly melt and control the matrix loss rate.

8. The method for preparing a copper target by electron beam melting according to claim 2, characterized in that: The 4N cathode copper pretreatment in S1 comprises the following steps: S11. Preparation: S112. Ensure that the operating environment is well ventilated; S113. Prepare the necessary equipment and materials, including alkali-resistant containers, stirrers, personal protective equipment such as protective gloves and goggles, and accurately prepared 10% NaOH solution; S12, soaking treatment: S121. Place the cathode copper in an alkali-resistant container and pour in a sufficient amount of 10% NaOH solution to ensure that the cathode copper is completely immersed in the solution; S122, determining the soaking time according to the degree of oil pollution and the size of cathode copper; S13, stirring and cleaning: S131. During the soaking process, a stirrer may be used to stir slowly to accelerate the reaction between the oil stain and the NaOH solution and improve the cleaning effect; S132, after the immersion is completed, the cathode copper is taken out from the solution and rinsed with clean water to remove the residual NaOH solution and reaction products; S14, Inspection and Drying: S141, check whether the oil stains on the surface of the cathode copper are completely removed. If there are still residual oil stains, repeat the above steps to clean again; S142. After cleaning, place the cathode copper in a well-ventilated place to dry naturally or use drying equipment to dry it, ensuring that there is no moisture remaining on the surface of the cathode copper.

9. The method for preparing a copper target by electron beam melting according to claim 8, characterized in that: When stirring and cleaning the cathode copper in S13, a processing device is required, and the processing device includes a workbench, the surface of the workbench is connected to a box body, the bottom of the inner wall of the box body is connected to a circular limit seat, and a container is placed inside the circular limit seat, and a base is connected to the center position of one end of the workbench, and a stirring device is provided on the surface of the base. The stirring device includes a telescopic frame, a motor is installed on one side of the surface of the telescopic frame, and one end of the motor output shaft is fixedly connected to a stirring member through a coupling.

10. The method for preparing a copper target by electron beam melting according to claim 9, characterized in that: A shielding assembly is provided on the surface of the container, and the shielding assembly includes a shielding plate, one side of the shielding plate is connected to a first magnetic block, the bottom of the first magnetic block is magnetically connected to a second magnetic block, and the second magnetic block is connected to the surface of the container.

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