Te-cu alloy smelting furnace and application thereof
By employing a vacuum feeding system and optimized feeding method in a tellurium-copper alloy smelting furnace, combined with lanthanum-carbon-magnesium composite coating, the problems of high oxygen content and low conductivity in tellurium-copper alloys were solved, achieving the preparation of high-quality tellurium-copper alloys.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2025-12-18
- Publication Date
- 2026-03-17
AI Technical Summary
In existing tellurium-copper alloy smelting processes, the oxygen content is high, the conductivity is low, and the feeding process is complex, making it difficult to effectively control tellurium segregation and vapor volatilization.
A tellurium-copper alloy smelting furnace was designed, including a furnace lining, a furnace cover, a charging system, and a charging pipe. Through vacuum charging and an optimized charging method, combined with the coating of lanthanum-carbon-magnesium composite material, one-time charging is achieved, reducing oxygen content and improving tellurium segregation and vapor volatilization.
It significantly reduces the oxygen content in tellurium copper alloys, improves the alloy's electrical conductivity and mechanical properties, simplifies the feeding process, and reduces operational complexity.
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Figure CN121346513B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of smelting furnaces, and particularly to a tellurium-copper alloy smelting furnace and its applications. Background Technology
[0002] Tellurium copper alloys are copper-based alloys of tellurium and copper. During high-temperature smelting, tellurium copper alloys readily react with oxygen to form oxides such as cuprous oxide (Cu₂O). These oxides reduce the alloy's electrical conductivity, ductility, and mechanical properties.
[0003] The existing smelting process for tellurium-copper alloys involves adding high-purity copper (≥99.9%) to a furnace, covering it with a covering agent, and then heating and melting it under the protection of the covering agent (which forms a physical barrier on the surface of the melt, isolating it from air and reducing contact between the metal and oxygen). After complete melting, the covering agent is gently removed using a feeding tool to create a localized opening, and tellurium (≥99.5%) is slowly added into this opening. However, the tellurium-copper alloys prepared using the existing smelting process have a high oxygen content and low electrical conductivity.
[0004] To reduce oxygen content and improve conductivity, CN111809074A discloses a method for preparing tellurium-copper alloy. This method uses charcoal as a covering agent and adds a lanthanum-carbon-magnesium composite material in two stages for deoxidation, grain refinement, and impurity removal. Tellurium is added between the two additions (there are three additions during the smelting process). Although this reduces oxygen content and conductivity, the addition of both tellurium and the lanthanum-carbon-magnesium composite material requires removing the covering agent, which introduces air into the molten pool. Inert gas must be introduced to vent the air after each addition, but even then, the air entering the molten pool is difficult to expel, resulting in a still high oxygen content in the prepared tellurium-copper alloy material. The conductivity still needs improvement, and the long interval between the first and last additions complicates the operation.
[0005] The above background information is provided to facilitate understanding of the present invention and is not intended to be publicly known technology disclosed to the general public prior to the application of this invention. Summary of the Invention
[0006] To address the aforementioned deficiencies, the present invention provides a tellurium-copper alloy smelting furnace and its application, which aims to improve at least one of the problems mentioned in the background art.
[0007] The technical solution is as follows: A tellurium-copper alloy smelting furnace includes a furnace lining, a furnace cover covering the furnace lining, and a tellurium-copper alloy smelting charging system. The furnace lining and the furnace cover form a furnace cavity. An induction system is located around the furnace lining. The tellurium-copper alloy smelting charging system includes a hopper and a feeding pipe connected to the bottom of the hopper. A feeding valve is installed on the feeding pipe. An upwardly extending holding pipe is provided at the center of the furnace bottom of the furnace lining. A series of through holes are opened on a section of the holding pipe near the furnace bottom. The top of the holding pipe does not exceed the liquid level line of the molten pool formed after the copper is melted. The lower end of the feeding pipe is located inside the holding pipe. A branch pipe is also installed on the feeding pipe. A vacuum valve and a vacuum pump are installed on the branch pipe. The vacuum pump is connected to an vent pipe. The lower end face of the feeding pipe is located below the liquid level line of the molten pool when charging.
[0008] Furthermore, a filter device and a cold trap are also installed on the branch pipe. The filter device is installed between the vacuum valve and the vacuum pump, and the cold trap is installed between the filter device and the vacuum pump.
[0009] Furthermore, the feed pipe is a telescopic sleeve. The upper end of the outer tube of the telescopic sleeve is connected to the hopper. The inner tube retracts into the outer tube when no material is being added. When material needs to be added, it extends out from the lower end of the outer tube. The feed valve and the branch pipe are installed on the outer tube, with the feed valve located above the branch pipe.
[0010] Furthermore, the length of the through-hole group in the material-filling tube is less than 1 / 5 of the total length of the through-hole group, and the diameter of the material-filling tube is not less than Y, where Y = (20V / (π*h))0.5, V is the total volume of the tellurium block with copper foil added, and h is the depth of the molten pool. The through-hole group includes several rings of through holes, each ring of through holes having the same diameter. The first ring of through holes is located at the bottom of the material-filling tube, and the diameter decreases as it gets further away from the furnace bottom.
[0011] Furthermore, the diameter of the first ring of through holes is 5 mm, the diameter of the second ring of through holes is 3 mm, and from the third ring of through holes onwards, the diameter decreases at a rate of 20%.
[0012] Furthermore, a baffle group is provided inside the material holding tube, and the baffle group is located above the through hole group; the baffle group is arranged from bottom to top inside the material holding tube, with only one baffle at each height. One end of the baffle is connected to the wall of the material holding tube, and the other end extends towards the middle. The projection surface of four adjacent baffles coincides with the horizontal section of the material holding tube. Each baffle is inclined downwards at an angle of 5° to 10°.
[0013] Furthermore, the furnace bottom of the furnace lining is higher in the middle and lower on both sides, with an inclination angle of 5°~10°. A stirring coil groove is provided below the furnace lining, and a stirring coil is installed in the stirring coil groove.
[0014] The present invention also provides applications of tellurium copper alloy smelting furnaces.
[0015] The technical solution is as follows: The aforementioned tellurium-copper alloy smelting furnace is used to prepare tellurium-copper alloys, including the following steps:
[0016] S1. Melting: Copper is added to the furnace cavity of the tellurium copper alloy material furnace and heated to melt.
[0017] S2. After the copper has completely melted, raise the temperature to 1000℃;
[0018] S3. After heat preservation and standing, open the furnace cover and slowly place the feeding pipe on the support ring of the holding pipe. Then turn on the vacuum valve and vacuum pump to evacuate the feeding pipe to 10 mbar. Turn off the vacuum valve and vacuum pump, open the feeding valve and feed the material. During the feeding process, turn on the vacuum valve and vacuum pump to a slight negative pressure of 500 mbar. After feeding is completed, immediately turn off the vacuum valve and vacuum pump.
[0019] S4. Increase the temperature to 1100℃;
[0020] S5. Casting;
[0021] S6. Bar extrusion;
[0022] S7. Cold processing and cold drawing to the finished product.
[0023] Compared with the prior art, the beneficial effects of the present invention are as follows:
[0024] This invention improves the feeding system and adds a material-holding pipe inside the furnace, sets the furnace bottom to be higher in the middle and lower on both sides, and uses lanthanum-carbon-magnesium cladding for tellurium. This also improves tellurium segregation, sublimation and reduces oxygen content, and only requires one feeding during the smelting process. Attached Figure Description
[0025] Figure 1 This is a schematic diagram of the overall structure of the tellurium-copper alloy material melting furnace of the present invention;
[0026] Figure 2 This is a schematic diagram of the charging system of the tellurium-copper alloy material furnace of the present invention;
[0027] Figure 3 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 1 ;
[0028] Figure 4 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 2 ;
[0029] Figure 5 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 3 ;
[0030] Figure 6 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 4 ;
[0031] In the diagram: 1. Furnace lining, 2. Furnace cover, 3. Furnace cavity, 4. Induction coil, 5. Induction cooling system, 6. Material holding pipe, 61. Through hole group, 62. Baffle group, 63. Support ring, 7. Stirring coil groove, 8. Induction yoke, 9. Bushing, 10. Feeding system, 101. Hopper, 102. Discharge pipe, 103. Material valve, 104. Branch pipe, 105. Vacuum valve, 106. Vacuum pump, 107. Exhaust pipe, 108. Filter device, 109. Cold trap. Detailed Implementation
[0032] The invention will now be further described with reference to the accompanying drawings.
[0033] In the description of this invention, it should be noted that, unless otherwise explicitly specified and limited, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to a fixed connection, an indirect connection via an intermediate medium, or the internal communication of two components or the interaction between two components. Those skilled in the art can understand the specific meaning of the above terms in this invention according to the specific circumstances.
[0034] In the description of this invention, it should be understood that the terms "upper," "lower," "front," "rear," "vertical," "horizontal," "top," "bottom," "inner," and "outer," etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, and are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation of this invention. In the description of this invention, "a plurality of" means two or more, unless otherwise precisely specified.
[0035] The terms “first,” “second,” “third,” “fourth,” etc. (if present) in the specification, claims, and accompanying drawings of this application are used to distinguish similar objects and are not necessarily used to describe a particular order or sequence. It should be understood that such data can be interchanged where appropriate so that the embodiments of this application described herein can be implemented, for example, in orders other than those illustrated or described herein. Furthermore, the terms “comprising” and “having,” and any variations thereof, are intended to cover a non-exclusive inclusion; for example, a process, method, system, product, or apparatus that comprises a series of steps or units is not necessarily limited to those steps or units explicitly listed, but may include other steps or units not explicitly listed or inherent to such processes, methods, products, or apparatus.
[0036] To make the objectives, technical solutions, and advantages of the embodiments of this application clearer, the technical solutions of the embodiments of this application will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of this application, not all embodiments. Based on the embodiments of this application, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of this application.
[0037] The technical solution of the present invention will be described in detail below with reference to specific embodiments. These specific embodiments can be combined with each other, and the same or similar concepts or processes may not be described again in some embodiments.
[0038] Please refer to Figures 1-5 , Figure 1 This is a schematic diagram of the overall structure of the tellurium-copper alloy material melting furnace of the present invention. Figure 2 This is a schematic diagram of the charging system of the tellurium-copper alloy material furnace of the present invention. Figure 3 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 1 , Figure 4 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 2 , Figure 5 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 3 , Figure 6 This is the axial cross-section of the tellurium sump tube of the present invention. Figure 4 .
[0039] like Figure 1 A tellurium copper alloy material melting furnace includes a furnace lining 1 and a furnace cover 2 covering the furnace lining 1. The furnace lining 1 and the furnace cover 2 form a furnace cavity 3. An induction system is located around the furnace lining 1, and an induction cooling system 5 is installed outside the induction system. The tellurium copper alloy material melting furnace also includes a feeding system 10.
[0040] The feeding system 10 of the present invention Figure 2 It includes a hopper 101 and a discharge pipe 102 connected to the bottom of the hopper 101. A material valve 103 is installed on the discharge pipe 102. A branch pipe 104 is also installed on the discharge pipe 102. A vacuum valve 105 and a vacuum pump 106 are installed on the branch pipe 104. The vacuum pump 106 is connected to an exhaust pipe 107. The lower end face of the discharge pipe 102 is below the liquid level line of the molten pool when the material is added.
[0041] With the addition of the feeding system 10, in the process of smelting tellurium-copper alloy materials, when adding tellurium or lanthanum-carbon-magnesium composite materials midway, after opening the furnace cover 2, the feeding pipe 102 is slowly placed into the molten pool. Then, the vacuum valve 105 and vacuum pump 106 are opened to evacuate the feeding pipe 102 to 10 mbar. The vacuum valve 105 and vacuum pump 106 are then closed, and the feeding valve 103 is opened for feeding. During the feeding process, the vacuum valve 105 and vacuum pump 106 are opened to a slight negative pressure of 500 mbar (the purpose is to extract the air brought in during the feeding process). After the feeding is completed, the vacuum valve 105 and vacuum pump 106 are immediately closed. When slowly placing the feeding pipe 102 into the molten pool, the covering agent should be prevented from entering the feeding pipe 102. With the feeding system 10 and vacuuming, the area of the covering agent displaced during the feeding process only needs to be the diameter of the feed pipe 102. During the feeding process, in addition to the feed pipe 102, the rest of the molten pool is also covered by the covering agent. No air is introduced into the molten pool during the entire feeding process. Compared with the existing methods, this greatly reduces the oxygen content in the tellurium copper alloy and improves the overall performance of the alloy.
[0042] In one or more embodiments of the present invention, in order to protect the vacuum pump 106, a filter device 108 and a cold trap 109 are also installed on the branch pipe 104. The filter device 108 is installed between the vacuum valve 105 and the vacuum pump 106, and the cold trap 109 is installed between the filter device 108 and the vacuum pump 106. Those skilled in the art should understand that the feed valve 103, filter device 108, cold trap 109, vacuum pump 106, and vacuum valve 105 are all prior art, and those skilled in the art can select them according to specific needs.
[0043] To ensure that the lower end of the feed pipe 102 is below the molten pool level during feeding and on the furnace cover 2 when not feeding, the feed pipe 102 is a retractable sleeve. The upper end of the outer tube of this retractable sleeve is connected to the hopper 101, and the inner tube retracts into the outer tube when not feeding. When feeding is required, it extends from the lower end of the outer tube. The feed valve 103 and the branch pipe 104 are installed on the outer tube, with the feed valve 103 located above the branch pipe 104. Those skilled in the art should understand that retractable sleeves are existing mature technology, and can be selected according to needs.
[0044] Although the aforementioned feeding system 10 and vacuuming method greatly reduce the oxygen content in the tellurium copper alloy and improve the overall performance of the alloy, due to the special characteristics of tellurium (not only are its melting and boiling points low, but the density of tellurium powder is also lower than that of copper), the tellurium segregation phenomenon and tellurium vapor volatilization phenomenon in the smelting of tellurium copper alloy are very serious. On the one hand, this affects the performance of tellurium copper alloy materials, and on the other hand, more tellurium needs to be added to achieve the total tellurium content in the tellurium copper alloy material. To reduce tellurium segregation, various methods have been adopted in the industry. When adding tellurium, 3mm-5mm tellurium blocks are used, and a layer of copper foil is wrapped around the tellurium blocks. In induction furnaces, in addition to electromagnetic stirring on the sides and bottom, slow mechanical stirring is also installed (e.g., CN111809074A). While this reduces tellurium segregation to some extent, electromagnetic stirring increases tellurium vapor volatilization to some extent, and mechanical stirring significantly increases tellurium vapor volatilization. Furthermore, the slow addition of tellurium increases the risk of exposed molten pool, leading to increased oxygen content. Therefore, in one or more embodiments of this invention, an upwardly extending charging pipe 6 is provided at the center of the furnace bottom of the furnace lining 1. A series of through holes 61 are opened on a section of the charging pipe 6 near the furnace bottom, and the top of the charging pipe 6 does not exceed the liquid level line of the molten pool formed after the copper melts.
[0045] By installing an upward-extending charging pipe 6 at the center of the furnace bottom, when adding tellurium after the copper has completely melted, the covering agent is gently removed with a charging tool, and the lower end of the discharge pipe 102 is inserted into the charging pipe 6. During the charging process, 3mm~5mm tellurium blocks wrapped with copper foil first enter the discharge pipe 102 from the hopper 101, and then enter the charging pipe 6 to deposit downwards. As can be seen from the temperature field distribution of the furnace, the temperature is lower in the section near the bottom of the charging pipe 6, and the tellurium blocks are wrapped with copper foil. Therefore, the tellurium blocks melt gradually in the charging pipe 6 first, and then diffuse outwards. Due to the presence of the charging pipe 6 and the discharge pipe 102, there is no need to worry about molten pool splashing during the tellurium block deposition process, allowing for rapid charging, increasing charging time, reducing the exposed area and time of the molten pool, reducing the oxygen content of the product, and improving product quality.
[0046] In one or more embodiments of the present invention, in order to further improve tellurium segregation and reduce tellurium vapor volatilization, the length of the through hole group 61 in the material holding pipe 6 is less than 1 / 5 of the total length of the through hole group 61, and the diameter of the material holding pipe 6 is not less than Y, where Y = (20V / (π*h)). 0.5 Where V is the total volume of the tellurium ingot with copper foil added, and h is the depth of the molten pool. At this pipe diameter, before the tellurium ingot melts after being added, it is located in the low-temperature zone, which can delay the melting time of the tellurium ingot, improve segregation, and also reduce tellurium vapor.
[0047] In one or more embodiments of the present invention, in order to further improve tellurium segregation and reduce tellurium vapor volatilization, the through-hole group 61 includes several rings of through-holes, each ring having the same diameter. The first ring of through-holes is located at the bottom of the feeding tube 6, and the diameter of the first ring of through-holes is 5 mm. The diameter of the second ring of through-holes is 3 mm. From the third ring of through-holes onwards, the diameter decreases at a rate of 20% (the diameter of the third ring of through-holes is 2.4 mm). With this arrangement, after feeding, a portion of the tellurium blocks directly leaves the feeding tube 6 through the first ring of through-holes and melts in the bottom molten pool outside the feeding tube 6. A portion is melted until it can leave the feeding tube 6 through the through-hole group 61 of each ring before being melted.
[0048] In one or more embodiments of the present invention, in order to further improve tellurium segregation and reduce tellurium vapor volatilization, the furnace bottom of the furnace lining 1 is high in the middle and low on both sides, with an inclination angle of 5° to 10°. Under this structure, on the one hand, the liquid at the bottom of the molten pool flows from the middle to both sides under the action of weight, which is conducive to the horizontal flow of the melt, improving tellurium segregation and reducing tellurium vapor volatilization. On the other hand, the tellurium blocks coming out of the charging pipe 6 are dispersed to both sides under the action of gravity, further improving tellurium segregation and reducing tellurium vapor volatilization.
[0049] In one or more embodiments of the present invention, in order to further improve tellurium segregation and reduce tellurium vapor volatilization, a baffle assembly 62 is provided inside the material receiving pipe 6. The baffle assembly 62 is located above the through-hole assembly 61. The purpose of the baffle assembly 62 is to block the upward flow of the melt in the material receiving pipe 6, providing resistance to the upward flow of the molten tellurium. The baffle assembly 62, on the one hand, prevents the upward flow of the melt with high tellurium concentration, and on the other hand, because there is no opening in the upper part of the material receiving pipe 6, it also prevents the horizontal diffusion of the melt in the material receiving pipe 6 in the area near the surface of the molten pool.
[0050] In one or more embodiments of the present invention, in order to effectively block the flow, the baffle assembly 62 is arranged from bottom to top along the inside of the material receiving pipe 6, with only one baffle at each height, such as... Figure 3-6 As shown, one end of the baffle is connected to the wall of the material holding pipe 6, and the other end extends towards the middle. The projection surfaces of the four adjacent baffles coincide with the horizontal cross-section of the material holding pipe 6.
[0051] In one or more embodiments of the present invention, in order to prevent the tellurium block from staying on the baffle during feeding, each baffle is tilted downward at an angle of 5° to 10°.
[0052] In one or more embodiments of the present invention, in order to avoid introducing new impurities, the material of the material-holding pipe 6 and the material-feeding tool is the same as the material of the furnace lining 1.
[0053] In one or more embodiments of the present invention, in order to reduce the difficulty of operation, a support ring 63 is provided on the inner wall of the inner baffle group 62 above the pipe opening, and the inner extension of the support ring 63 is not less than the wall thickness of the lower end of the feed pipe 102.
[0054] In one or more embodiments of the present invention, for safe feeding, the lower section of the feeding tool (not shown in the figure) is a lower pipe with a diameter smaller than that of the material holding pipe 6, and the upper section is a funnel-shaped opening.
[0055] In one or more embodiments of the present invention, in order to improve the horizontal diffusion at the bottom of the molten pool, a stirring coil groove 7 is provided below the furnace lining 1, and a stirring coil is installed in the stirring coil groove 7. During operation, the stirring coil provides electromagnetic stirring. For those skilled in the art, the installation and operation of electromagnetic stirring are conventional techniques, and no creative effort is required for their installation and use. In the present invention, the electromagnetic stirring at the bottom not only provides diffusion force for the melt at the bottom of the molten pool, but also provides power for the movement of the tellurium block.
[0056] In one or more embodiments of the present invention, the induction system includes an induction coil 4, an induction yoke 8, a first electrode, and a second electrode. The first electrode introduces current from an external power source into the molten pool, and the second electrode draws current out of the molten pool and back to the external power source, forming a closed loop. The induction yoke 8 is disposed around the induction coil 4, and a current or voltage sensor is installed in the circuit of the second electrode. The induction yoke 8 prevents magnetic flux leakage, reduces energy consumption, and achieves energy saving. On the other hand, it provides strong support for the coil from the outside of the induction coil 4, thereby stabilizing the lifespan of the furnace lining 1. During smelting, the current or voltage sensor detects whether there is a furnace leakage by detecting whether the current or voltage is abnormal.
[0057] In one or more embodiments of the present invention, in order to protect the induction coil 4, isolate it from the high-temperature molten metal and resist its corrosion, provide structural support for the furnace lining 1, maintain the stability of the furnace lining 1, achieve electrical insulation, prevent short circuits, optimize the electromagnetic field distribution, and ensure the efficient and safe operation of the equipment, a bushing 9 is provided between the furnace lining 1 and the induction system.
[0058] In one or more embodiments of the present invention, in order to further improve tellurium segregation, reduce tellurium vapor volatilization and reduce oxygen content, the existing three-stage feeding process in the smelting process is changed to a single feeding. The feeding method is also changed from feeding lanthanum-carbon-magnesium mixed powder separately and copper foil-wrapped tellurium blocks separately to feeding a portion of the tellurium blocks with lanthanum-carbon-magnesium mixed powder by electrostatic coating and another portion of the tellurium blocks with copper foil, and then adding the coated tellurium blocks into the molten pool. When the electrostatically coated tellurium block and the copper foil-coated tellurium block enter the material collection tube 6 for deposition, a portion of the tellurium block comes out from the first ring of through holes and disperses to both sides. The other portion is melted until it can leave through the through hole group 61 of each ring, and then leaves the material collection tube 6 for further melting. Since the thermal conductivity of the lanthanum-carbon-magnesium mixed powder coated on the tellurium block is much lower than that of the copper foil, the tellurium block coating is dispersed throughout the molten pool (under the combined effects of the molten pool flow law, the molten pool temperature field distribution law, gravity, and the heat absorbed by the melting of lanthanum, magnesium, and copper). When lanthanum and magnesium melt and react with tellurium to form MgTe and LaTe, the final alloy is basically free of free Te. Since the tellurium block coating of this invention is dispersed throughout the molten pool, the carbon powder, lanthanum, and magnesium outside the tellurium block are also dispersed, resulting in better homogeneity of the alloy, lower oxygen content, and significantly improved electrical conductivity and mechanical properties.
[0059] In this invention, the copper foil-coated tellurium block (hereinafter referred to as copper-coated tellurium) coating process is an existing process, and the tellurium size is 3mm~5mm.
[0060] In this invention, the tellurium block coated with lanthanum-carbon-magnesium mixed powder (hereinafter referred to as lanthanum-carbon-magnesium coated tellurium) has a tellurium size of 3mm to 5mm.
[0061] Example 1: Obtaining Lanthanum-Coated Tellurium Carbon Magnesium
[0062] M1. Take dry lanthanum powder, carbon powder and magnesium powder, mix them evenly to form a mixed powder, wherein lanthanum is 25wt%, carbon is 50wt% and magnesium is 25%; the moisture content of each of the dry lanthanum powder, carbon powder and magnesium powder is <2wt% to avoid charge leakage.
[0063] M2, charging treatment, makes the mixed powder positively charged and the tellurium negatively charged. Charging treatment is an existing process that can be achieved through friction or corona treatment.
[0064] M3, mixing and adsorption, causing the mixed powder to be directionally adsorbed onto the tellurium surface (mixing and adsorption can be carried out in a rotating drum in an electrostatic field), forming lanthanum-carbon-magnesium tellurium-coated tellurium, for 25 minutes.
[0065] M4, cold-pressed, pressure <10 MPa.
[0066] Example 2
[0067] A method for preparing a tellurium-copper alloy material includes the following steps:
[0068] S1. Smelting: High-purity copper is added to the furnace cavity 3 of the above-mentioned tellurium copper alloy material furnace and heated to melt under the protection of charcoal covering agent.
[0069] S2. After the high-purity copper has completely melted, raise the temperature to 1000℃.
[0070] S3. After keeping it warm and standing for 15 minutes, open the furnace cover 2 and slowly place the feeding pipe 102 on the support ring 63 of the holding pipe 6. Then open the vacuum valve 105 and the vacuum pump 106 to evacuate the feeding pipe 102 to 10 mbar. Close the vacuum valve 105 and the vacuum pump 106, open the material valve 103, and feed the material. During the feeding process, open the vacuum valve 105 and the vacuum pump 106 to a slight negative pressure of 500 mbar. After feeding is completed, immediately close the vacuum valve 105 and the vacuum pump 106.
[0071] In this step, the total amount of tellurium is 0.3 wt% of copper, and the total amount of lanthanum powder, carbon powder, and magnesium powder is 0.04 wt% of copper. All the powders (lanthanum 25 wt%, carbon 50 wt%, magnesium 25 wt%) are used to coat the tellurium in the manner described in Example 1. The amount of tellurium coated with the mixed powder is 10.5 wt% of the total tellurium, and the remaining tellurium is coated with copper foil. During feeding, copper is added first to coat the tellurium, and then immediately lanthanum, carbon, and magnesium are added to coat the tellurium (meaning the total feeding is done in one step).
[0072] S4. Increase the temperature to 1100℃.
[0073] S5. Casting.
[0074] S6. Bar extrusion: The obtained copper alloy is heated to 800℃ by industrial frequency and hot extruded. The extruded billet is water-cooled.
[0075] S7. Cold working: The product is cold-drawn to the finished product using a hydraulic drawing machine.
[0076] In this embodiment, the molten pool adopts the molten pool of the present invention, that is, the bottom of the furnace of the feeding system 10, the material holding pipe 6, the bottom electromagnetic stirrer, and the furnace lining 1 is high in the middle and low on both sides, with an inclination angle of 5°~10°.
[0077] Comparative Example 1
[0078] Compared with Example 2, the molten pool is the same, the only difference is that the feeding is divided into three feedings. The first feeding is in S2, when the temperature is raised to 1000°C, the added material is a lanthanum-carbon-magnesium mixed powder (25wt% lanthanum, 50wt% carbon, 25% magnesium), and the amount added is 0.04wt% of the copper. The second feeding is in S3, the added material is copper-coated tellurium, and the total amount of tellurium is 0.3wt% of the copper. The third feeding is in S4, when the temperature is raised to 1100°C, the added material is a lanthanum-carbon-magnesium mixed powder (25wt% lanthanum, 50wt% carbon, 25% magnesium), and the amount added is 0.01wt% of the copper.
[0079] In this comparative example, the feeding operation is the same as the feeding operation in S3 of Example 2 (i.e., before feeding, the vacuum is drawn to 10 mbar, the vacuum valve 105 and the vacuum pump 106 are closed, the material valve 103 is opened, and the material is fed. During the feeding process, the vacuum valve 105 and the vacuum pump 106 are opened to a slight negative pressure of 500 mbar. After the feeding is completed, the vacuum valve 105 and the vacuum pump 106 are immediately closed).
[0080] In Example 2 and Comparative Example 1, after the furnace cover 2 was closed after the material was added, inert gas was not introduced for exhaust.
[0081] The tellurium copper alloy material prepared in Example 2 and the tellurium copper alloy material prepared in Comparative Example 1 were subjected to XRD to confirm the final phase. MgTe and LaTe were detected in Example 2, but no free Te peak was observed, while free Te peak was present in Comparative Example 1.
[0082] The oxygen content of the tellurium-copper alloy material prepared in Example 2 and the tellurium-copper alloy material prepared in Comparative Example 1 was tested. The oxygen content of Comparative Example 1 was higher than that of Example 2.
[0083] The above description is merely a preferred embodiment of the present invention and is not intended to limit the invention. Various modifications and variations can be made to the present invention by those skilled in the art. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.
Claims
1. A tellurium-copper alloy smelting furnace, comprising a furnace lining (1), a furnace cover (2) covering the top of the furnace lining (1), and a tellurium-copper alloy smelting feeding system, the furnace lining (1) and the furnace cover (2) forming a furnace cavity (3), and the furnace lining (1) being provided with an induction system on the periphery, wherein the tellurium-copper alloy smelting feeding system comprises a hopper (101) and a feeding pipe (102) connected to the bottom of the hopper (101), and a feeding valve (103) is installed on the feeding pipe (102), characterized in that, The furnace lining (1) is provided with a upwardly extending holding tube (6) at the center of the furnace bottom, a group of through holes (61) are formed on the tube adjacent to a section of the furnace bottom, the top end of the holding tube (6) does not exceed the liquid level line of the molten pool formed after the copper is melted, the lower end of the downcomer (102) is located in the holding tube (6), a branch pipe (104) is further installed on the downcomer (102), a vacuum valve (105) and a vacuum pump (106) are installed on the branch pipe (104), the vacuum pump (106) is connected with an exhaust pipe (107), and the lower end surface of the downcomer (102) is located below the liquid level line of the molten pool during charging.
2. The tellurium-copper alloy melting furnace according to claim 1, characterized by The branch pipe (104) is further provided with a filtering device (108) and a cold trap (109), the filtering device (108) is installed between the vacuum valve (105) and the vacuum pump (106), and the cold trap (109) is installed between the filtering device (108) and the vacuum pump (106).
3. The tellurium-copper alloy melting furnace according to claim 1, characterized by The downcomer (102) is a telescopic sleeve, the upper end of the outer tube of the telescopic sleeve is connected with the hopper (101), the inner tube is retracted into the outer tube when no charging is needed, and the inner tube is extended from the lower end of the outer tube when charging is needed, the material valve (103) and the branch pipe (104) are installed on the outer tube, and the material valve (103) is located above the branch pipe (104).
4. The tellurium-copper alloy melting furnace according to claim 1, characterized by The length of the through hole group (61) is less than 1 / 5 of the total length of the through hole group (61), the pipe diameter of the material containing tube (6) is not less than Y, Y=(20V / (pi*h)) 0.5 Wherein V is the total volume of the copper foil clad tellurium block, h is the depth of the molten pool, the through hole group (61) includes several circles of through holes, the hole diameter of each circle of through holes is the same, the first circle of through holes is located at the bottom of the material containing tube (6), and the farther from the furnace bottom, the smaller the hole diameter.
5. The tellurium-copper alloy melting furnace according to claim 4, characterized by The first group of through holes has a hole diameter of 5 mm, the second group of through holes has a hole diameter of 3 mm, and the hole diameter decreases at a rate of 20% from the third group of through holes.
6. The tellurium-copper alloy melting furnace according to claim 5, characterized by The holding tube (6) is provided with a baffle group (62) located above the group of through holes (61); the baffle group (62) is arranged from bottom to top in the holding tube (6), only one baffle is arranged at each height, one end of the baffle is connected to the wall of the holding tube (6), and the other end extends to the middle, the projection planes of the four adjacent baffles coincide with the horizontal section of the holding tube (6), and each baffle is inclined downward at an angle of 5°-10°.
7. The tellurium-copper alloy melting furnace according to claim 3, characterized by The furnace bottom of the furnace lining (1) is high in the middle and low on both sides, and the inclination angle is 5°-10°, and a stirring coil groove (7) is arranged below the furnace lining (1), and a stirring coil is arranged in the stirring coil groove (7).
8. The tellurium-copper alloy melting furnace according to any one of claims 1 to 7, which is used for producing a tellurium-copper alloy, characterized in that, The method comprises the following steps: S1. Melting: copper is added to the furnace cavity of the tellurium-copper alloy material furnace, and the copper is melted by heating; S2. After the copper is completely melted, the temperature is raised to 1000℃; S3. After heat preservation and standing, the furnace cover (2) is opened, the downcomer (102) is slowly placed on the supporting ring (63) of the holding tube (6), then the vacuum valve (105) and the vacuum pump (106) are opened, the inside of the downcomer (102) is vacuumized to 10 mbar, the vacuum valve (105) and the vacuum pump (106) are closed, the material valve (103) is opened, and charging is performed; during the charging process, the vacuum valve (105) and the vacuum pump (106) are opened to a micro negative pressure of 500 mbar, and immediately after the charging is completed, the vacuum valve (105) and the vacuum pump (106) are closed; S4. The temperature is raised to 1100℃; S5. Casting; S6. Rod extrusion; S7. Cold working and cold drawing to finished product.
Citation Information
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