Preparation process and preparation device of high-strength and high-conductivity chromium-zirconium-copper alloy material

By using the down-induction method and the combination of inert gas and graphite phosphorus sheet cover agent in the casting process of copper-chromium zirconium alloy, the copper-chromium zirconium alloy in the prior art has solved the high cost, low efficiency and unstable composition during the smelting process in the prior art. The problem of this has achieved the improvement of the preparation of long-size or large-scale coils and the improvement of material performance.

CN119456968AInactive Publication Date: 2025-02-18HANGZHOU ZHONGHONG TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202411700230.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-26
Publication Date
2025-02-18
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing copper-chromium-zirconium alloys have problems of high production costs, low production efficiency and unstable composition during the smelting process, and it is difficult for traditional casting processes to prepare long-size or large-scale coils, which affects the performance of the material.

Method used

The casting process is improved by using the lower lead method, and the non-vacuum preparation technology is realized through the combination of inert gas and graphite phosphorus sheet covering agent, which solves the problems of rapid alloying and chromium-zirconium burning, ensures component stability, and refines the alloy solidification. To prepare a conglomerate crystal continuous casting billet.

Benefits of technology

The preparation of long-size or large-scale coils is realized, which improves the mechanical properties and quality of chromium-zirconium copper alloy materials, reduces production costs, and improves production efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention belongs to the technical field of non-ferrous metal heat treatment processing, and particularly relates to a high-strength and high-conductivity chromium-zirconium-copper alloy material preparation technology and a preparation device thereof.The high-strength and high-conductivity chromium-zirconium-copper alloy material preparation device comprises second supporting columns and a smelting furnace, the smelting furnace is fixedly arranged on the multiple second supporting columns in a supported mode, and a heat preservation casting furnace is arranged on one side of the smelting furnace; hydraulic liquid transfer devices are arranged in the heat-preservation casting furnace and the smelting furnace, an alloy bin is arranged on one side in the heat-preservation casting furnace, a casting guiding bin is arranged on one side of the alloy bin in the heat-preservation casting furnace, a crystallizer is arranged at the bottom of the casting guiding bin, and a combined traction device is arranged at the bottom of the crystallizer. According to the method, the defects of a traditional upper leading-out method and a traditional horizontal leading-out method are overcome through a lower leading-out method, the problems of rapid alloying and chromium-zirconium burning loss can be solved, the component stability of the chromium-zirconium-copper alloy can be ensured, large-scale continuous large-scale production can be achieved, the alloy solidification structure can be refined, a fully-equiaxed crystal continuous casting billet can be prepared, and the production efficiency is improved. And the mechanical property of the continuous casting billet is effectively improved.
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Description

Technical Field

[0001] The invention belongs to the technical field of heat treatment of nonferrous metals, and in particular relates to a preparation process and a preparation device of a high-strength and high-conductivity chromium-zirconium-copper alloy material. Background Art

[0002] Copper-chromium-zirconium alloy is an alloy composed of three metals: copper, chromium and zirconium. It has the characteristics of high hardness, good wear resistance and explosion resistance, and high softening temperature. It is widely used in many fields. Copper-chromium-zirconium alloy has a stable demand in the market due to its excellent performance, especially in applications that require high strength, high conductivity and high temperature resistance. The domestic research time for copper-chromium-zirconium product technology is relatively short, and some high-end chromium-zirconium copper is difficult to meet market demand. Enterprises and research institutions continue to optimize this alloy and explore new applications to meet the ever-changing industrial needs.

[0003] my country's patent CN200710047494.9 discloses a method and device for preparing a high-strength and high-conductivity copper-chromium-zirconium alloy material. The inventive method changes and controls the aging conditions of the copper-chromium-zirconium alloy, places the entire aging process in a steady magnetic field (0.1-12T), and simultaneously passes a direct current into the copper-chromium-zirconium alloy. The synergistic effect of the magnetic field and the electric field is used to change the organizational morphology, structure and properties of the copper alloy product, and prepare a copper-chromium-zirconium alloy material with uniform distribution of alloy elements, high strength and high conductivity.

[0004] The existing technology utilizes the synergistic effect of magnetic field and electric field to improve the performance of chromium-zirconium-copper alloy materials, but the existing technology as a whole still has certain shortcomings when used: First, most of the existing chromium-zirconium-copper alloys are often fused by vacuum melting or non-vacuum melting technology. However, in the production process, the first technology has the problem of high production cost and low production efficiency, while the second technology cannot solve the problem of rapid addition of multiple elements. The composition after melting is unstable, and the overall mechanical properties of the chromium-zirconium-copper alloy are seriously reduced. Secondly, when casting chromium-zirconium-copper alloy, existing enterprises all use the upper casting or horizontal casting technology in the continuous casting process. These two technologies cannot solve the problem of preparing long or large coils, which seriously affects the application scope of chromium-zirconium-copper alloy materials. At the same time, the alloy materials will be stretched or extruded to varying degrees, and there will be uneven organization or composition, which will affect the overall performance. Summary of the invention

[0005] In order to overcome the deficiencies of the prior art, the present invention provides a preparation process and a preparation device for a high-strength and high-conductivity chromium-zirconium-copper alloy material. The present invention solves the defects of the traditional upper and horizontal lead-out methods by improving the process and corresponding equipment, and adopts a lower lead-out method, which can not only solve the problems of rapid alloying and chromium-zirconium burnout, ensure the composition stability of the chromium-zirconium-copper alloy, and realize large-scale continuous production, but also refine the alloy solidification structure, prepare a fully equiaxed crystal continuous casting billet, and effectively improve the mechanical properties of the continuous casting billet.

[0006] In order to achieve the above-mentioned object, the present invention provides the following technical solution: A preparation process of a high-strength and high-conductivity chromium-zirconium-copper alloy material, comprising the following preparation process: S1: Prepare cathode copper, copper-chromium alloy, and copper-zirconium alloy according to the proportion and process and dry each material; S2: Lay a 10-15 cm covering agent in the smelting furnace and the insulation casting furnace, put the prepared cathode copper into the smelting furnace, then increase the power to increase the temperature, remove oxygen during the melting process, and heat to 1300±30℃ after it is completely melted; S3: The cathode copper solution is transported to the insulation casting furnace through the dark current channel, and then the covering agent in the insulation casting furnace is replaced with a graphite phosphorus sheet covering agent with a thickness of 10-15 cm. Then the temperature of the insulation casting furnace is raised to 1300±50°C, and the copper-chromium alloy is added to the alloy bin and kept warm for 1 hour. After the temperature is kept constant at 1300±30°C, the copper-zirconium alloy is added and kept for 9-11 minutes; S4: Start the combined traction device, adjust the casting speed to 340-450 mm / min and start traction. At this time, a certain amount of copper-chromium-zirconium solution is water-cooled through the crystallizer and then non-contact water-cooled downward casting is performed; S5: The downwardly casted material will be formed into a chromium-zirconium-copper alloy rod with a diameter of φ25-φ30, and then pulled to the coiling machine 30 for coiling processing until it is coiled into a rod wire weighing 3-5 tons.

[0007] Preferably, the copper-chromium alloy is an intermediate alloy in the range of CuCr10-CuCr40, and the copper-zirconium alloy is an intermediate alloy in the range of CuZr15-CuZr40.

[0008] Preferably, when the chromium-zirconium-copper solution in S4 is crystallized, the current through electromagnetic induction is 10-50A and the frequency is 15-50HZ; during the water cooling process, the cooling water temperature is lower than 35°C, the water pressure is 3-5pa, and the water flow rate is 30-70 liters / min; the optimal moving speed of the chromium-zirconium-copper material downward through the crystallizer is 360mm / min.

[0009] Preferably, the chromium-zirconium copper rod and wire in S4 can be continuously solution treated in the smelting furnace 1 and the insulation casting furnace during the casting process; during the solution treatment process, a certain amount of cathode copper, copper-chromium alloy and copper-zirconium alloy needs to be added in a timed variable manner to meet the continuous casting.

[0010] Preferably, the process of conveying the cathode copper solution to the heat-insulating casting furnace and adding the alloy material in S3 needs to be carried out under the protection of inert gas.

[0011] Preferably, the inert gas is argon or nitrogen, and the protective pressure of the inert gas is 3-5 Pa.

[0012] A preparation device for a high-strength and high-conductivity chromium-zirconium-copper alloy material comprises a first support column and a smelting furnace, wherein the smelting furnace is rotatably supported on a plurality of the first support columns, an insulation casting furnace is arranged on one side of the smelting furnace, a hydraulic liquid transfer device is arranged in the insulation casting furnace and the smelting furnace, an alloy bin is arranged on one side inside the insulation casting furnace, a casting bin is arranged on one side of the alloy bin in the insulation casting furnace, a crystallizer is arranged at the bottom of the casting bin, and a combined traction device is arranged at the bottom of the crystallizer.

[0013] Preferably, the hydraulic fluid transfer device includes a first undercurrent channel arranged in the smelting furnace, a rotating axis is arranged on the first support column on one side of the first undercurrent channel, a transfer port is arranged on one side of the rotating axis, a guide groove is arranged on the heat-insulating casting furnace on one side of the transfer port, a second undercurrent channel is arranged in the guide groove, the first undercurrent channel and the transfer port, the guide groove and the second undercurrent channel are in communication with each other, a sealing cover plate is arranged on the top of the heat-insulating casting furnace, and an inert gas inlet pipe is arranged on the sealing cover plate.

[0014] Preferably, the combined traction device comprises an integrated traction machine arranged below the crystallizer, a wire take-up tension frame is arranged on one side of the integrated traction machine, and a wire coiling machine is arranged on one side of the wire take-up tension frame.

[0015] Preferably, an electromagnetic stirrer is provided inside the crystallizer.

[0016] In summary, compared with the prior art, the beneficial effects of this solution are: (1) The present invention improves and utilizes the process and corresponding equipment, and adopts an air barrier method of inert gas, charcoal and graphite phosphorus sheets during the fusion process of chromium-zirconium-copper alloy, so that the non-vacuum preparation technology can realize the preparation of long-sized or large-roll chromium-zirconium-copper alloy wires, and can realize the preparation of rods and wires up to several thousand meters and weighing 3-5 tons. The mechanical properties of the chromium-zirconium-copper alloy rods are also greatly improved, which not only reduces the production cost, but also effectively improves the quality of the chromium-zirconium-copper alloy; (2) The present invention improves the lead-out method and changes the equipment structure. The new down-lead casting technology can not only refine the alloy solidification structure and prepare fully equiaxed crystal continuous casting billets, but also effectively improve the mechanical properties of the continuous casting billets and reduce the possibility of solute element segregation, thereby effectively improving the quality and effect of chromium-zirconium-copper alloy materials; (3) In the process of the present invention, by quickly switching between the charcoal covering agent and the graphite phosphorus sheet covering agent, not only the overall production cost is greatly reduced, but also the occurrence of alloy burning during the smelting process can be reduced, thereby ensuring the stability of the copper-chromium-zirconium alloy composition to achieve continuous large-scale production, and the overall air barrier effect can also be greatly improved, effectively ensuring the production efficiency and quality of the chromium-zirconium-copper alloy. BRIEF DESCRIPTION OF THE DRAWINGS

[0017] Figure 1 A general diagram of the apparatus for preparing the present invention; Figure 2 It is a top view of the interior of the heat preservation casting furnace; Figure 3 for Figure 1 A partial enlarged view of the middle A; Figure 4 is a flow chart of the preparation process of the present invention; Figure 5 This is a cross-sectional comparison diagram of the chromium-zirconium-copper alloy produced by the present invention; In the figure: smelting furnace 1, first support column 2, first thermocouple 3, first melting groove 4, first sensor 5, first undercurrent channel 6, rotating axis 7, transfer port 8, power control cabinet 9, guide groove 10, second undercurrent channel 11, sealing cover plate 12, insulation casting furnace 13, crystallizer 14, second support column 15, hydraulic rod 16, second sensor 17, second thermocouple 18, induction bin 24, alloy bin 26, traction operation cabinet 27, traction integrated machine 28, wire take-up tension frame 29, wire coiling machine 30. DETAILED DESCRIPTION

[0018] In order to enable those skilled in the art to better understand the solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention.

[0019] Embodiment one: Reference Figure 1 , Attachment Figure 2 and attached Figure 3, a preparation device of high-strength and high-conductivity chromium-zirconium-copper alloy material, comprising a second support column 2, a smelting furnace 1, and a plurality of first support columns 2 on which the smelting furnace 1 is rotatably arranged, a pushing cylinder is arranged on the outside of the smelting furnace 1, and the output end of the pushing cylinder is rotatably connected to the outside of the smelting furnace 1, which can push the smelting furnace 1 to rotate at an angle, and the smelting furnace 1 will melt the cathode copper, and a first melting groove 4 is arranged at the bottom of the smelting furnace 1, and the first melting groove 4 is U-shaped as a whole, and a plurality of electric heating wires are wound on the outside, which are used for heating to melt the cathode copper, which is the prior art, and this scheme will not be elaborated too much, and a first sensor 5 and a first thermocouple are arranged inside and outside the smelting furnace 1 respectively, and the first thermocouple is similar to a thermometer for temperature monitoring, and is used to ensure that the temperature inside the furnace can reach the qualified standard and ensure the quality of smelting. A power control cabinet 9 is arranged on one side of the smelting furnace 1, and the power control cabinet 9 is used to control the power supply of the entire set of equipment.

[0020] Reference Figure 1 , Attachment Figure 2 and attached Figure 3 A plurality of second support columns 15 are arranged on one side of the smelting furnace 1, a hydraulic rod 16 is arranged on one side of the second support column 15, an insulation casting furnace 13 is arranged at the output end of the hydraulic rod 16 and the top rotation support of the second support column 15, a second sensor 17 is arranged outside the insulation casting furnace 13 for controlling the heating power of the furnace body, the hydraulic rod 16 can control the angle of inclination of the insulation casting furnace 13 so that the liquid inside moves, a hydraulic liquid transfer device is arranged in the insulation casting furnace 13 and the smelting furnace 1, the hydraulic liquid transfer device can allow the molten copper in the smelting furnace 1 to enter the insulation casting furnace 13 under the protection of argon gas, an alloy bin 26 is arranged in the insulation casting furnace below the hydraulic liquid transfer device, the alloy bin 26 is used for adding and mixing various alloy materials, and one side of the alloy bin 26 is in the insulation casting furnace 13 A casting bin 24 is provided, and the casting bin 24 is used to cast the mixed smelted alloy copper liquid downward. A crystallizer 14 is provided at the bottom of the casting bin 24. A water cooling system is provided inside the crystallizer 14, so that when the crystallizer 14 discharges the metal liquid downward, the metal liquid can be quickly cooled down to complete the hardening treatment. In this scheme, the casting of the alloy uses an unconventional bottom lead-out process. Compared with the top lead-out method, this method will not cause tearing between the crystals inside the alloy, and the overall grain size is more uniform. Compared with the horizontal lead-out method, the crystals will not be compressed, so that the chromium and zirconium elements will not appear in some places inside the copper material. Too much and too little in other places will not occur, thereby improving the overall mechanical strength of the chromium-zirconium-copper alloy and improving the quality of the molding effect. Therefore, a combined traction device is provided at the bottom of the crystallizer 14 to coil the chromium-zirconium-copper alloy into bundles.

[0021] In the above scheme, an electromagnetic stirrer is arranged inside the crystallizer 14. In the gap where the metal liquid is led downward for rapid cooling and forming, the metal liquid is rapidly rotated and stirred through reactions such as magnetic field and electric current, so that various metal elements can be quickly stirred and evenly dispersed to various positions before cooling, thereby improving the quality of the chromium-zirconium-copper alloy rod. In this scheme, the stirring of the electromagnetic stirrer can also improve the flow efficiency and stability of the metal liquid, reduce the occurrence of problems such as accumulation of the metal liquid or excessive pressure that makes it difficult to discharge, and improve the preparation effect of the chromium-zirconium-copper alloy material.

[0022] Reference Figure 1 , Attachment Figure 2 and attached Figure 3 In order to ensure the safety of the copper liquid when it is transferred from the smelting furnace 1 to the insulation casting furnace 13 and to improve the molding effect, a hydraulic transfer device is provided, which includes a first dark flow channel 6 arranged in the smelting furnace 1, a rotating shaft 7 is arranged on the first support column 2 on one side of the first dark flow channel 6, a transfer port 8 is arranged on one side of the rotating shaft 7, a guide groove 10 is arranged on the insulation casting furnace 13 on one side of the transfer port 8, a second dark flow channel 11 is arranged in the guide groove 10, the first dark flow channel 6 and the transfer port 8, the guide groove 10 and the second dark flow channel 11 are mutually circulated, a sealing cover plate 12 is arranged on the top of the insulation casting furnace 13, and an inert gas input pipe is arranged on the sealing cover plate 12. When the copper liquid needs to be transferred, the smelting furnace 1 will rotate downward with the rotation axis 7 as the axis under the action of the push cylinder, and the heat-insulating casting furnace 13 will also rotate with the rotation axis 7 as the axis point under the action of the hydraulic rod 16, so that the first dark flow channel 6 and the transfer port 8 correspond to each other. At this time, the cathode copper liquid will pass through the first dark flow channel 6, the transfer port 8, the guide groove 10, the second dark flow channel 11, and finally reach the alloy bin 26 and the casting bin 24. In this process, the sealing cover plate 12 will inject the inert gas into each cavity that can circulate with each other at a certain pressure through the inert gas input pipe, so that the oxygen inside each cavity is squeezed out of the cavity, reducing the oxidation reaction between oxygen and the chromium-zirconium alloy element, and improving the quality of mutual fusion of various elements.

[0023] Reference Figure 1 , Attachment Figure 2 and attached Figure 3 In order to ensure the forming effect of the chromium-zirconium-copper alloy, a traction integrated machine 28 is set below the crystallizer 14 by utilizing the height difference, a wire winding tension frame 29 is set on one side of the traction integrated machine 28, and a wire winding machine 30 is set on one side of the wire winding tension frame 29, wherein the wire winding tension frame 29 is used for tensioning the copper wire when winding it, and the wire winding machine 30 is used for completing the winding process of the copper wire.

[0024] Embodiment 2: A preparation process of high-strength and high-conductivity chromium-zirconium-copper alloy material, see attached Figure 4 ; Step 1: Prepare materials. Prepare raw materials according to the mass ratio of cathode copper material, copper-chromium alloy and copper-zirconium alloy: 93.53:5.84:0.63. Weigh a certain amount of covering agent. The covering agent, copper-chromium alloy and copper-zirconium alloy can be placed beside the smelting furnace 1 in advance. When the smelting furnace 1 melts other materials, the residual temperature is used for drying and heating to remove excess moisture and improve the smelting quality.

[0025] Step 2: Melting. Evenly lay a charcoal covering agent of about 15 cm in the melting furnace 1 and the insulation casting furnace 13, then put the prepared cathode copper into the melting furnace 1, and then increase the power and temperature to melt the material. The overall melting process must be operated in accordance with the process specifications to achieve accurate degassing treatment, and remove gases such as oxygen and hydrogen that affect the molding effect. When the liquid in the melting furnace 1 reaches a certain liquid level, the first thermocouple 3 detects the temperature to 1200±10℃ and takes a sample to detect the composition and oxygen content of the original copper liquid. The oxygen content must be less than or equal to 10PPM. After the component content is measured to be qualified, the melting furnace 1 must be continued. Increase the power and heat up to 1320±10℃ before waiting for liquid transfer. In this step, the cathode copper will gradually turn into metal liquid during the melting process, and the charcoal covering agent is initially laid on the bottom. However, in the process of melting the cathode copper, the charcoal itself is light in weight, so it will float up with the metal liquid and cover the cathode copper liquid, thereby forming an isolation zone on the top of the copper liquid, isolating oxygen, reducing the oxidation reaction between the copper liquid and oxygen, and improving the molding quality. At the same time, the charcoal covering agent is affordable and can effectively reduce production costs. In this step, the charcoal covering agent can also be placed on the cathode copper after the cathode copper is placed, which will not affect the molding quality.

[0026] Step three: Fill with inert gas, seal the insulation casting furnace 13 with a sealing cover plate 12, and use 5pa argon gas to flow it into the first undercurrent channel 6, the transfer port 8, the guide groove 10 and other cavities that need to be passed through during the liquid transfer. In this step, the argon gas will squeeze out the oxygen in each cavity, so that the copper liquid will flow in an oxygen-free environment, reducing the possibility of oxidation; the argon gas itself will not react with elements such as chromium, zirconium and copper, and the molding quality will also be improved.

[0027] Step 4: liquid transfer. After the argon gas is filled for about 10 minutes, use the power control cabinet 9 to turn off the power of the smelting furnace 1, start the hydraulic liquid transfer device, and transfer the liquid with the rotating axis 7 as the axis. The cathode copper liquid will pass through the first dark current channel 6, the transfer port 8, the guide groove 10, and the second dark current channel 11 to reach the alloy bin 26 and the induction casting bin 24. When the standard liquid level is reached in the furnace cavity of the insulation casting furnace, start the power of the smelting furnace 1 in the power control cabinet 9, increase the power of the second sensor 17 in the insulation casting furnace 13, open the sealing cover 12 to replace the graphite phosphorus sheet covering agent, the thickness of the graphite phosphorus sheet covering agent is about 15 cm, and then continue to heat the alloy bin 26 and the induction casting bin 24 to 1300±10℃. In this step, the copper liquid is poured into the insulation casting furnace 13. In the process, due to the previous Charcoal covering agent is filled, so the charcoal covering agent will float up and cover the surface of the molten copper during the continuous injection of molten copper, so that under the protection of argon gas, a secondary air isolation effect can be formed. However, the charcoal covering agent is easy to penetrate impurities into the alloy in the further high-temperature alloy process, resulting in burning, which affects the quality of the chromium-zirconium alloy. Therefore, the graphite phosphorus flake covering agent is replaced. The graphite phosphorus flake covering agent has a better air isolation effect than the charcoal covering agent, and it will not react with the chromium-zirconium alloy. However, it is heavy and cannot effectively float upward during the melting of the molten copper. Therefore, in the subsequent addition, the quality of the alloy forming can be improved by replacing the covering agent. This explanation shows that this replacement step is only used when the equipment is started for the first time. When the subsequent casting is continued, only graphite phosphorus flakes need to be continuously added without too many steps.

[0028] Step 5: Adding materials. When the temperature in the alloy bin 26 and the casting bin 24 reaches 1300±10℃, add the heated and dried CuCr10 alloy into the alloy bin 26 in proportion, then heat it to 1300±10℃ and keep it warm to allow it to fully dissolve. Take samples after 20 minutes, and adjust the temperature after testing until the chromium content in the copper liquid reaches the target value. Keep warm for 40 minutes, then add the heated and dried CuZr40 alloy into the alloy bin 26 in succession, take samples after 5 minutes, and adjust the temperature after testing until the copper, chromium and zirconium content in the copper liquid reaches the target value.

[0029] Step 6: Casting. After about 10 minutes of copper-zirconium alloy being added into the alloy bin 26, operate the button of the traction operation cabinet 27 to start the traction integrated machine 28. The casting speed is adjusted from low to high according to the casting conditions according to the process standards to 360 mm / min. During this process, the water cooling system is quickly adjusted, wherein the inlet temperature of the cooling water needs to be lower than 35°C, and the flow rate is adjusted to 30 L / min. The electromagnetic stirring function of the crystallizer 14 is started, and the current is set to 15 A and the frequency is 25 Hz. The downward casting begins, and the chromium-zirconium-copper liquid will form a chromium-zirconium-copper casting rod of φ25-φ30. During the casting process, the chromium-zirconium copper rod and wire can be continuously solution treated in the smelting furnace 1 and the insulation casting furnace. During the solution process, a certain amount of cathode copper, copper-chromium alloy and copper-zirconium alloy needs to be added in a timed variable manner to meet the continuous casting.

[0030] Step 7: Forming, when casting downward, the appearance and element content of the chromium-zirconium copper casting rod must be tested online in a timely manner. The appearance test includes the diameter, surface finish, color, cracks, etc. The element content refers to whether the copper, chromium and zirconium meet the standard range. The copper-chromium-zirconium casting rod passes through the corresponding components such as the take-up tension frame and the winding machine until it is coiled into a large rod and wire coil weighing 3-5 tons.

[0031] Embodiment three: A preparation process of high-strength and high-conductivity chromium-zirconium-copper alloy material, see attached Figure 4 : Step 1: Prepare materials. Prepare raw materials according to the mass ratio of cathode copper material, copper-chromium alloy and copper-zirconium alloy: 92.52:4.65:2.83. Weigh a certain amount of covering agent. The covering agent, copper-chromium alloy and copper-zirconium alloy can be placed beside the smelting furnace 1 in advance. When the smelting furnace 1 melts other materials, the residual temperature is used for drying and heating to remove excess moisture and improve the smelting quality.

[0032] Step 2: Melting, put the prepared cathode copper into the smelting furnace 1, then lay a 15 cm graphite phosphorus sheet covering agent on the cathode copper, and evenly lay a 10 cm charcoal covering agent in the insulation casting furnace 13, and then increase the power to heat the material to melt the material. The overall melting process must be operated in accordance with the process specifications to achieve accurate degassing treatment, and remove gases such as oxygen and hydrogen that affect the molding effect. When the liquid in the smelting furnace 1 reaches a certain liquid level, the first thermocouple 3 detects the temperature to 1200±10℃ and takes a sample to detect the composition and oxygen content of the original copper liquid, where the oxygen content must be less than Or equal to 10PPM. After the content of the component is measured to be qualified, the smelting furnace 1 needs to be powered up and heated to 1320±10℃ before liquid transfer. In this step, the cathode copper will gradually turn into metal liquid during the melting process, and the graphite phosphor sheet covering agent is laid on the cathode copper at the beginning. Therefore, in the process of melting the cathode copper, the graphite phosphor sheet covering agent will always cover the top of the copper liquid, thereby forming an isolation zone on the top of the copper liquid, completing the role of isolating oxygen, reducing the oxidation reaction between the copper liquid and oxygen, and improving the molding quality. At the same time, the graphite phosphor sheet covering agent will not react with the copper liquid, which can effectively improve the molding quality.

[0033] Step three: Fill with inert gas, seal the insulation casting furnace 13 with a sealing cover plate 12, and use 5pa nitrogen to flow it into the first undercurrent channel 6, the transfer port 8, the guide groove 10 and other cavities that need to pass through when transferring liquid. In this step, the nitrogen will squeeze out the oxygen in each cavity, so that the copper liquid will flow in an oxygen-free environment, reducing the possibility of oxidation; although nitrogen will produce trace reactions with elements such as chromium, zirconium and copper compared to argon, the covering agent previously used graphite phosphorus flakes, so the isolation effect is not too reduced. At the same time, the overall cost of nitrogen is much lower than that of argon, which can effectively reduce the cost of production.

[0034] Step 4: liquid transfer. After the nitrogen is filled for about 10 minutes, use the power control cabinet 9 to turn off the power of the smelting furnace 1, start the hydraulic liquid transfer device, and transfer the liquid with the rotating axis 7 as the axis. The cathode copper liquid will pass through the first dark current channel 6, the transfer port 8, the guide groove 10, and the second dark current channel 11 to reach the alloy bin 26 and the induction bin 24. When the standard liquid level is reached in the furnace cavity of the insulation casting furnace, start the power of the smelting furnace 1 in the power control cabinet 9, increase the power of the second sensor 17 in the insulation casting furnace 13, open the sealing cover 12 to replace the graphite phosphorus sheet covering agent, and then continue to heat the alloy bin 26 and the induction bin 24 to 1300±10℃. In this step, when the copper liquid is poured into the insulation casting furnace 13, since the charcoal covering agent has been filled inside, the charcoal The covering agent will also float up and cover the surface of the molten copper during the continuous injection of the molten copper, thereby forming a secondary air isolation effect under the protection of nitrogen. However, the charcoal covering agent is prone to infiltrate impurities into the alloy during the further high-temperature alloy process, resulting in burnout and affecting the quality of the chromium-zirconium alloy. Therefore, the graphite phosphorus flake covering agent is replaced. The graphite phosphorus flake covering agent is better than the charcoal covering agent in isolating air and will not react with the chromium-zirconium alloy. However, it is more expensive and heavier, and cannot effectively float upward during the melting of the molten copper. Therefore, subsequent additions can only be made to improve the quality of alloy forming by replacing the covering agent. This indicates that this replacement step is only used when the equipment is started for the first time. When the subsequent casting is continued, only graphite phosphorus flakes need to be continuously added without too many steps.

[0035] Step 5: Adding materials. When the temperature in the alloy bin 26 and the casting bin 24 reaches 1320±10℃, add the heated and dried CuCr40 alloy into the alloy bin 26 in proportion, then heat it to 1320±10℃ and keep it warm to allow it to fully dissolve. Take samples after 20 minutes, and adjust them continuously after testing until the chromium content in the copper liquid reaches the target value. Keep warm for 40 minutes, then add the heated and dried CuZr15 alloy into the alloy bin 26 in succession, take samples after 5 minutes, and adjust them continuously after testing until the copper, chromium and zirconium content in the copper liquid reaches the target value.

[0036] Step 6: Casting. After about 10 minutes of copper-zirconium alloy being added into the alloy bin 26, operate the button of the traction operation cabinet 27 to start the traction integrated machine 28. The casting speed is adjusted from low to high according to the casting conditions according to the process standards to 360 mm / min. During this process, the water cooling system is quickly adjusted, wherein the inlet temperature of the cooling water needs to be lower than 35°C, and the flow rate is adjusted to 40 L / min. The electromagnetic stirring function of the crystallizer 14 is started, and the current is set to 30 A and the frequency is 45 Hz. The downward casting begins, and the chromium-zirconium-copper liquid will form a φ30 chromium-zirconium-copper casting rod. During the casting process, the chromium-zirconium copper rod and wire can be continuously solution treated in the smelting furnace 1 and the insulation casting furnace. During the solution process, a certain amount of cathode copper, copper-chromium alloy and copper-zirconium alloy needs to be added in a timed variable manner to meet the continuous casting.

[0037] Step 7: Forming, when casting downward, the appearance and element content of the chromium-zirconium copper casting rod must be tested online in a timely manner. The appearance test includes the diameter, surface finish, color, cracks, etc. The element content refers to whether the copper, chromium and zirconium meet the standard range. The copper-chromium-zirconium casting rod passes through the corresponding components such as the take-up tension frame and the wire coiling machine until it is coiled into a large rod and wire coil weighing 3-4 tons.

[0038] In summary, through the process and device of the present invention, rods and wires can be continuously produced through multiple liquid transfers, alloy addition and other methods, which solves the problem of continuous casting of long or large rods and wires of chromium-zirconium-copper alloy, and can prepare advanced rods and wires that are several thousand meters long and weigh 3-4 tons.

[0039] Comparative Example 1: The present invention adopts non-vacuum melting and casting to realize the preparation of long-size / large-volume heavy copper-chromium-zirconium alloy ingots, and the grain size reaches micron level! Figure 5 .

[0040] The present invention prepares: The ingot structure morphology and the grain size are micron level (9 levels).

[0041] A certain enterprise (non-vacuum): The grain size of the ingot microstructure is at the centimeter level (0-1 level).

[0042] Comparative Example 2: United States, Japan, Germany, China [Φ6-Φ120]: Rm≥450MPa, HRB55-86, IACS%75-83; This project [Φ0.5-Φ40] was tested by relevant instruments: Rm≥650MPa, HRB80-90, IACS%75-88.

[0043] Comparative Example 3: Through the continuous production of copper-chromium-zirconium alloy materials through non-vacuum preparation technology, the unit processing cost is reduced by 52.98% compared with vacuum smelting preparation, and the comprehensive material is increased by 30%, which can obtain cost and efficiency advantages.

[0044] For example, certain words are used in the specification and claims to refer to specific components. Those skilled in the art should understand that hardware manufacturers may use different terms to refer to the same component. This specification and claims do not use differences in names as a way to distinguish components, but use differences in the functions of components as the criteria for distinction. For example, "including" mentioned throughout the specification and claims is an open term, so it should be interpreted as "including but not limited to". "Approximately" means that within an acceptable error range, those skilled in the art can solve the technical problem within a certain error range and basically achieve the technical effect.

[0045] It should be noted that the terms "include", "comprises" or any other variations thereof are intended to cover non-exclusive inclusion, so that a product or system including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such product or system. In the absence of more restrictions, the elements defined by the sentence "comprises a ..." do not exclude the existence of other identical elements in the product or system including the elements.

[0046] The above description shows and describes several preferred embodiments of the present application, but as mentioned above, it should be understood that the present application is not limited to the form disclosed herein, and should not be regarded as excluding other embodiments, but can be used in various other combinations, modifications and environments, and can be modified within the scope of the application concept described herein through the above teachings or the technology or knowledge of the relevant field. The changes and modifications made by those skilled in the art do not deviate from the spirit and scope of the present application, and should be within the scope of protection of the claims attached to the present application.

Claims

1. A preparation process of a high-strength and high-conductivity chromium-zirconium-copper alloy material, characterized in that: The preparation process includes the following: S1: Prepare cathode copper, copper-chromium alloy, and copper-zirconium alloy according to the proportion and process and dry each material; S2: Lay a 10-15 cm covering agent in the smelting furnace and the insulation casting furnace, put the prepared cathode copper into the smelting furnace, then increase the power to increase the temperature, perform degassing during the melting process, and heat to 1300±30℃ after it is completely melted; S3: The cathode copper solution is transported to the insulation casting furnace through the dark current channel, and then the covering agent in the insulation casting furnace is replaced with a graphite phosphorus sheet covering agent with a thickness of 10-15 cm. Then the temperature of the insulation casting furnace is raised to 1300±50°C, and the copper-chromium alloy is added to the alloy bin and kept warm for 1 hour. After the temperature is kept constant at 1300±30°C, the copper-zirconium alloy is added and kept for 9-11 minutes; S4: Start the traction integrated machine, adjust the casting speed to 340-450 mm / min and start traction. At this time, a certain amount of copper-chromium-zirconium solution is water-cooled through the crystallizer, and then non-contact water-cooled molding and downward casting are performed; S5: The downwardly casted material will be formed into a chromium-zirconium-copper alloy rod with a diameter of φ25-φ30, and then pulled to the coiling machine 30 for coiling processing until it is coiled into a rod wire weighing 3-5 tons.

2. The preparation process of a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 1, characterized in that: The copper-chromium alloy is a master alloy in the range of CuCr10-CuCr40, and the copper-zirconium alloy is a master alloy in the range of CuZr15-CuZr40.

3. The preparation process of a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 1, characterized in that: When the chromium-zirconium-copper solution in S4 is crystallized, the current through electromagnetic induction is 10-50A and the frequency is 15-50HZ; during the water cooling process, the cooling water temperature is lower than 35°C, the water pressure is 3-5pa, and the water flow rate is 30-70 liters / min; the optimal moving speed of the chromium-zirconium-copper material downward through the crystallizer is 360mm / min.

4. The preparation process of a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 3, characterized in that: During the casting process of the chromium-zirconium copper rod and wire in S4, solution treatment can be continuously performed in the smelting furnace 1 and the insulation casting furnace; during the solution treatment process, a certain amount of cathode copper, copper-chromium alloy and copper-zirconium alloy needs to be added in a timed variable manner to meet the continuous casting.

5. The preparation process of a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 1, characterized in that: The process of conveying the cathode copper solution to the heat-insulating casting furnace and adding the alloy material in S3 needs to be carried out under the protection of inert gas.

6. The preparation process of a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 5, characterized in that: The inert gas is argon or nitrogen, and the protective pressure of the inert gas is 3-5 Pa.

7. A device for preparing a high-strength and high-conductivity chromium-zirconium-copper alloy material, comprising a first support column (2), a smelting furnace (1), characterized in that: A smelting furnace (1) is rotatably supported on the plurality of first support columns (2); a heat-insulating casting furnace (13) is arranged on one side of the smelting furnace (1); a hydraulic fluid transfer device is arranged inside the heat-insulating casting furnace (13) and the smelting furnace (1); an alloy bin (26) is arranged on one side inside the heat-insulating casting furnace (13); a casting bin (24) is arranged on one side of the alloy bin (26) in the heat-insulating casting furnace (13); a crystallizer (14) is arranged at the bottom of the casting bin (24); and a combined traction device is arranged at the bottom of the crystallizer (14).

8. The device for preparing a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 7, characterized in that: The hydraulic fluid transfer device comprises a first undercurrent channel (6) arranged in a smelting furnace (1), a rotating shaft (7) is arranged on one side of the first undercurrent channel (6) on a first support column (2), a flow transfer port (8) is arranged on one side of the rotating shaft (7), a guide groove (10) is arranged on one side of the flow transfer port (8) on an insulation casting furnace (13), a second undercurrent channel (11) is arranged in the guide groove (10), the first undercurrent channel (6) and the flow transfer port (8) as well as the guide groove (10) and the second undercurrent channel (11) are in communication with each other, a sealing cover plate (12) is arranged on the top of the insulation casting furnace (13), and an inert gas input pipe is arranged on the sealing cover plate (12).

9. The device for preparing a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 7, characterized in that: The combined traction device comprises an integrated traction machine (28) arranged below the crystallizer (14), a wire take-up tension frame (29) being arranged on one side of the integrated traction machine (28), and a wire coiling machine (30) being arranged on one side of the wire take-up tension frame (29).

10. The device for preparing a high-strength and high-conductivity chromium-zirconium-copper alloy material according to claim 1, characterized in that: An electromagnetic stirrer is arranged inside the crystallizer (14).

Citation Information

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