CN115178714A - Preparation device and method of high-purity copper and copper alloy cast ingot - Google Patents
Preparation device and method of high-purity copper and copper alloy cast ingot Download PDFInfo
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- CN115178714A CN115178714A CN202211112499.6A CN202211112499A CN115178714A CN 115178714 A CN115178714 A CN 115178714A CN 202211112499 A CN202211112499 A CN 202211112499A CN 115178714 A CN115178714 A CN 115178714A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D9/00—Machines or plants for casting ingots
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D27/00—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting
- B22D27/15—Treating the metal in the mould while it is molten or ductile ; Pressure or vacuum casting by using vacuum
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D7/00—Casting ingots, e.g. from ferrous metals
- B22D7/005—Casting ingots, e.g. from ferrous metals from non-ferrous metals
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Abstract
The invention belongs to the technical field of high-purity metal smelting and casting for integrated circuits, and particularly discloses a device and a method for preparing high-purity copper and copper alloy ingots, wherein the device comprises the following components: the smelting furnace chamber, and a smelting device and a casting device which are arranged in the smelting furnace chamber from top to bottom; the smelting device comprises a crucible, a spout assembly and a movable tray, wherein the spout assembly is inserted into a discharge hole formed in the bottom of the crucible, and the movable tray is arranged below the discharge hole of the crucible; the casting device comprises a casting mold and a bottom support, an opening at the upper end of the casting mold is right opposite to a discharge port of the crucible, and the bottom of the casting mold is inserted into the bottom support. The whole device has compact and simple structure and simple and reliable smelting and casting processes, is beneficial to eliminating or reducing metallurgical defects such as air holes, looseness, impurities and the like in the ingot casting tissues, effectively improves the yield and yield of ingot casting products, and obviously improves the production efficiency.
Description
Technical Field
The invention belongs to the technical field of high-purity metal smelting and casting for integrated circuits, and particularly relates to a device and a method for preparing high-purity copper and copper alloy ingots.
Background
The high-purity metal sputtering target is widely applied to industries such as information storage, integrated circuits, flat panel displays, solar cells and the like, and various film functional materials are mainly obtained by a magnetron sputtering technology. Currently, sputtering targets can be classified according to their chemical composition into: pure metal targets such as aluminum, copper, titanium, tantalum, cobalt, and the like; alloy target materials, such as aluminum copper, aluminum silicon, copper phosphorus, copper aluminum, copper manganese, tungsten titanium, nickel platinum, nickel cobalt, nickel vanadium and the like. According to moore's law, the chip manufacturing process is continuously advanced and continuously updated in an iterative manner. With the development of chip processes and manufacturing techniques, higher and higher requirements are also placed on the performance of various materials. As the material of the interconnection wire of the integrated circuit chip, aluminum and aluminum alloy materials are adopted in the processes of 90nm and above, high-purity copper materials are adopted in the processes of 90-45nm, ultra-pure copper-aluminum and copper-manganese alloy materials are mainly adopted in the processes of 45-7nm, and high-purity cobalt is adopted as the interconnection material in the processes below 7 nm. Thus, the importance of high purity copper and copper alloy sputtering targets is increasingly emerging.
As mentioned above, ultra-high purity copper alloy targets are key support materials for integrated circuit interconnects in processes of 45nm and below. Pure copper has a lower electrical resistivity and a higher thermal conductivity, and has two orders of magnitude higher electromigration resistance than Al. The copper is used as an excellent interconnection material, so that the delay can be reduced, the operation efficiency can be improved, and the reliability of an integrated circuit can be ensured. In addition, trace alloy elements such as Al and Mn are added into high-purity copper, and a spontaneous diffusion barrier layer or an interface barrier layer is formed by microalloying, so that the line width can be further reduced. Therefore, high purity copper and copper alloy sputtering targets are the main direction of market competition in the future.
The preparation of high-purity copper and copper alloy cast ingots is the basis for manufacturing high-purity copper and copper alloy sputtering targets. From the results obtained at the present stage, the quality of the high-purity copper and copper alloy cast ingots is an important link of product development, and the quality of the high-purity copper and copper alloy cast ingots is used as the upstream of target production, and directly influences the service performance of the target and the customer satisfaction degree. The preparation method of the high-purity copper and alloy cast ingot is generally to melt in a vacuum induction furnace and obtain the cast ingot with the target size by adopting a tilting crucible static mold casting method, and is characterized by high purity, short period and low cost. However, in the actual production process under the existing equipment conditions, the obtained cast ingot often has more internal metallurgical defects, the types of the defects mainly comprise air holes, looseness, inclusions, cracks and the like, and the defects are mainly generated due to the limitations of the traditional smelting and casting equipment and process method. Therefore, the development of novel high-purity metal smelting and casting equipment and a process method can improve the quality of high-purity metal cast ingots, and has important practical significance for cost reduction, efficiency improvement and product quality stability improvement in the high-purity copper and copper alloy sputtering target industry.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a device and a method for preparing high-purity copper and copper alloy cast ingots.
The invention is realized by the following technical scheme.
A preparation facilities of high-purity copper and copper alloy ingot casting, characterized by that, the apparatus includes: the smelting furnace chamber, and the smelting device and the casting device which are arranged in the smelting furnace chamber from top to bottom; the smelting device comprises a crucible, a flow nozzle assembly and a movable tray, wherein the flow nozzle assembly is inserted into a discharge hole formed in the bottom of the crucible, and the movable tray is arranged below the discharge hole of the crucible; the casting device comprises a casting mold and a bottom support, an opening in the upper end of the casting mold is right opposite to the crucible discharge port, and the casting mold is arranged on the bottom support.
Further, the spout assembly comprises an outer guide pipe and an inner pipe which is detachably sleeved in the outer guide pipe, and the outer wall of the outer guide pipe is fixedly sleeved with the inner wall of the discharge hole of the crucible; an induction coil is arranged outside the lower part of the outer guide pipe.
Further, the outer catheter is a tapered tube, and the inner tube is a hollow cylindrical tube.
Furthermore, the movable tray comprises an upper tray and a lower supporting rod, the upper tray is connected with one end rod body of the lower supporting rod through a four-bar mechanism, and the other end of the lower supporting rod is connected with an electric push rod arranged outside the smelting furnace chamber.
Furthermore, the casting mold is a water-cooling copper mold and comprises a cylindrical shell with an upper opening and a lower opening, the cylindrical shell is formed by two semicircular plates which are oppositely arranged and connected through a clamping hoop, and a circulating cooling water pipeline is arranged on the outer wall of the cylindrical shell.
Furthermore, a riser is arranged at the top of the casting mould.
Further, the collet is a water-cooling copper collet and comprises an upper closed hollow cylinder and a lower closed hollow cylinder, a water inlet is formed in the bottom of the hollow cylinder, a water outlet is formed in the upper portion of the side wall of the hollow cylinder, the collet is arranged at the bottom of the smelting furnace chamber, and the bottom of the collet is connected with a servo motor arranged outside the smelting furnace chamber.
Further, the crucible is an electromagnetic induction heating type crucible.
The method for preparing the high-purity copper and copper alloy ingot by adopting the device is characterized by comprising the following steps of:
(1) Placing the movable tray at the lower end of the discharge hole of the crucible, and sealing the discharge hole;
(2) Placing a high-purity copper raw material in a crucible, and carrying out primary melting, cooling, secondary melting and refining, wherein when a copper alloy ingot is prepared, the alloy raw material is added in the secondary melting process, and then high-purity copper or a copper alloy melt is obtained;
(3) And the movable tray is separated from a discharge hole of the crucible, the high-purity copper or copper alloy melt enters the casting mold through the flow nozzle assembly, and the high-purity copper or copper alloy cast ingot is obtained after cooling.
Further, the step (2) is to melt at one time: vacuumizing to the vacuum degree less than or equal to 1 × 10 -2 Pa, heating at 1200-1300 ℃, and heating for 30-60min; cooling for 1h; secondary melting: heating at 1200-1300 ℃ for 15-30min; refining: filling argon into the hearth at the temperature of 1300-1350 ℃ until the pressure in the furnace is-0.09-0.05 MPa.
Further, in the step (3), the bottom support is driven by the servo motor to rotate in a reciprocating mode along the horizontal direction.
The purity of the high-purity copper or copper alloy cast ingot prepared by the method is more than or equal to 99.9999 percent (6N), even can reach more than or equal to 99.99995 percent (6N 5) or more than or equal to 99.99999 percent (7N), the oxygen content is less than or equal to 1ppm, the carbon content is less than or equal to 1ppm, the nitrogen content is less than or equal to 1ppm, the alloy component fluctuation is less than 5 percent, the diameter is phi 200-phi 400 mm, and the ingot casting structure has no metallurgical defects of air holes, looseness, inclusion and the like.
The invention has the beneficial technical effects that:
(1) According to the invention, the casting is realized by adopting the bottom lost casting of the crucible, and the metal melt in the crucible is injected into the lower casting mold through the bottom flow nozzle assembly, so that the oxide or inclusion and the like floating on the top layer of the liquid surface of the metal melt in the crucible finally flow into the casting mold and are intensively distributed on the top of the ingot, and thus the oxide or inclusion and the like can be removed when a shrinkage cavity is sawed in the subsequent process, and the risk that the oxide inclusion and the like enter the interior of the ingot tissue to cause defects is reduced;
(2) The casting mold provided by the invention is a water-cooled copper casting mold, the bottom support is a water-cooled copper bottom support, and after a melt enters the casting mold, circulating water cooling is provided in the axial direction and the radial direction, so that a high-purity metal cast ingot with excellent surface quality and fine crystal grains can be obtained more easily, the yield can be effectively improved, the surface of the cast ingot is smooth, demolding is easier, the service life of the casting mold can be greatly prolonged, the cast ingot discharging time is greatly shortened at the strong cooling rate of circulating water, and the production efficiency is remarkably improved;
(3) In the casting process, a servo motor is started to drive a bottom support to vibrate in a left-right reciprocating mode along the horizontal direction, so that the components of the alloy melt are uniform, the component fluctuation is less than 5%, the grain size is refined, the filling capacity of the metal melt is improved, and the metallurgical defects such as looseness, pores and the like are reduced;
(4) The smelting mode adopts vacuum induction smelting, and the gas can be ensured to escape sufficiently by cooling in the smelting process, so that the metal melt with high cleanliness and low gas content can be obtained;
(5) The whole device has compact and simple structure and simple and reliable smelting and casting processes, is beneficial to eliminating or reducing metallurgical defects such as air holes, looseness, impurities and the like in the ingot casting structure, effectively improves the yield and yield of ingot casting products, and obviously improves the production efficiency.
Drawings
Fig. 1 is a schematic structural diagram of an apparatus according to an embodiment of the present invention.
FIG. 2 is a schematic view of a portion of the structure of the present invention.
FIG. 3 is a process flow diagram of a method in an embodiment of the invention.
FIG. 4 is a scan of the internal metallurgical defect C of a high purity copper ingot according to an embodiment of the present invention.
FIG. 5 is a scan of the internal metallurgical defect C of the high purity copper aluminum alloy ingot in the example of the invention.
FIG. 6 is a C scan of internal metallurgical defects of a high purity Cu-Mn alloy ingot in an embodiment of the present invention.
Detailed Description
The invention is described in detail below with reference to the drawings and the detailed description.
As shown in fig. 1-2, a device for preparing high purity copper and copper alloy ingots comprises: the smelting furnace comprises a smelting furnace chamber 1, a smelting device and a casting device, wherein the smelting device and the casting device are arranged in the smelting furnace chamber from top to bottom;
the smelting furnace chamber 1 is a vacuum smelting chamber with the vacuum degree of 10 -3 Pa-10 -1 Within the Pa range;
the smelting device comprises a crucible 2, a spout assembly and a movable tray 3; the crucible 2 is an electromagnetic induction heating type crucible and comprises a cylindrical crucible, an insulating and heat-insulating layer 19 is lined between the outer wall of the crucible 2 and an electromagnetic induction coil 20, one surface of the insulating and heat-insulating layer 19, which is close to the electromagnetic induction coil 20, is a mica plate for insulating, one surface of the insulating and heat-insulating layer, which is close to the crucible 2, is an asbestos plate or an aluminum silicate felt for insulating and preserving heat, and the like, is positioned at the inner upper part of the smelting furnace chamber 1 and is supported by a support and used for containing metal melt, and the solid metal melt in the crucible 2 is converted into liquid metal melt by utilizing the electromagnetic induction heating principle; the flow nozzle assembly is inserted into a discharge port 4 formed in the bottom of the crucible 2, and specifically comprises an outer guide pipe 5 and an inner pipe 6 detachably sleeved in the outer guide pipe 5, the outer wall of the outer guide pipe 5 is fixedly sleeved with the inner wall of the crucible discharge port 4, the outer guide pipe 5 is a hollow conical pipe with an open upper end and a hollow lower end, specifically can be a graphite guide pipe, the inner pipe 6 is a hollow cylindrical pipe with an open upper end and a open lower end, the inner pipe 6 can be tightly and detachably inserted into the inner lower part of the outer guide pipe 5, and an induction coil 18 is arranged outside the lower part of the outer guide pipe 5 and used for heating a melt in the inner pipe 6; the movable tray 3 is arranged below the crucible discharge port 4, the movable tray 3 comprises an upper tray 7 and a lower supporting rod 8, the upper tray 7 is connected with one end rod body of the lower supporting rod 8 through a four-bar mechanism 9, concretely, the four-bar mechanism 9 comprises a front group of connecting rods and a rear group of connecting rods, each group comprises two connecting rods, the upper end and the lower end of each connecting rod are respectively provided with a connecting hole, the upper end of each connecting rod is connected with the upper tray 7 through a pin shaft, the lower end of each connecting rod is connected with an end rod body of the lower supporting rod 8 through a pin shaft, and the other end of the lower supporting rod 8 is connected with an electric push rod 10 arranged outside the smelting furnace chamber;
the casting device comprises a casting mold 11 and a bottom support 12, an opening at the upper end of the casting mold 11 is opposite to a crucible discharge port, the casting mold 11 is arranged on the bottom support 12, a riser 13 is arranged at the top of the casting mold 11, and the casting device plays a role in heat preservation and feeding after all melt is transferred from the crucible 2 to the casting mold 11, so that the shrinkage cavity depth of the cast ingot is reduced, and the yield of the cast ingot is improved; specifically, the casting mould 11 is water-cooling copper mold, specifically can be the copper product matter, including upper and lower open-ended cylindrical shell 14, open-top is as the runner, cylindrical shell 14 can be for two relative semicircle boards that set up that connect through two upper and lower clamps 15 constitute, prevent through clamp 15 that 11 parts of casting mould in the operation process produce the weeping, lead to the ingot casting can not shaping or geometric dimensions unusual, cylindrical shell 14's outer wall is equipped with recirculated cooling water pipeline 16, specifically can be corrugated metal pipe, be used for the ingot casting cooling with higher speed, and the production efficiency is improved.
Further, the bottom support 12 is a water-cooling copper support, specifically can be made of a red copper material, and comprises an upper closed hollow cylinder and a lower closed hollow cylinder, wherein the bottom of the hollow cylinder is provided with a water inlet, the upper part of the side wall is provided with a water outlet for being connected with a circulating cooling water pipeline, the bottom support 12 is arranged at the bottom of the smelting furnace chamber 1, the upper part of the bottom support is positioned in the smelting furnace chamber 1, and the bottom of the bottom support is connected with a servo motor 17 arranged outside the smelting furnace chamber. The bottom support is used for improving the cooling rate of the bottom of the cast ingot.
Example 1
As shown in fig. 3, a method for preparing a high-purity copper ingot by using the device comprises the following steps:
(1) The movable tray 3 is driven by the electric push rod 10 to move to the lower end of the crucible discharge port 4, and the discharge port 4 is sealed;
(2) Placing high-purity copper raw materials in a crucible 2 according to a certain stacking sequence, closing a furnace door arranged in a smelting furnace chamber 1, and vacuumizing the furnace until the vacuum degree is less than or equal to 1 multiplied by 10 -2 Pa, starting a heating power supply connected with the electromagnetic induction heating type crucible 2 to heat the raw material for one-time melting, melting the metal solid in the crucible 2 by using the principle of electromagnetic induction heating when current flows through an induction coil, stopping heating until the raw material is completely melted into a liquid melt, and heating for 60min at the temperature from room temperature to 1300 ℃; turning off a power supply to naturally cool the melt for 1h, and fully escaping nitrogen, oxygen, carbon and other impurity elements with vapor pressure higher than that of the molten metal, so as to achieve the purposes of degassing, removing impurities and purifying the melt; starting a power supply again for heating, carrying out secondary melting, heating at 1300 ℃, heating for 15min, raising the temperature to 1350 ℃ for refining the copper melt, simultaneously filling argon into a hearth until the pressure in the furnace is-0.09 to-0.05 MPa, further degassing and removing impurities, and improving the surface quality of the cast ingot; there are mainly two positions for monitoring the temperature of the metal melt, one of which is the temperature of the crucible 2: fixing a temperature measuring protection tube on the outer wall of the crucible, and monitoring the temperature of the crucible in real time by using a thermocouple; second is the temperature of the outer catheter 5:inserting a temperature measuring protection tube on the outer wall of the outer guide tube 5, and monitoring and controlling the temperature of induction heating in the outer guide tube 5 in real time by using an armored tungsten-rhenium thermocouple;
(3) After smelting, the casting stage is carried out, before casting, an induction coil 18 outside an outer guide pipe 5 is electrified, so that condensed metal melt entering a nozzle assembly is heated and melted, a movable tray 3 is moved to be separated from a crucible discharge port 4, the prepared high-purity copper melt enters a casting mold 11 through the nozzle assembly to be molded, a bottom support 12 is driven by a servo motor 17 to rotate in a reciprocating mode along the horizontal direction, an internal structure with fine grains and few metallurgical defects is obtained, and a high-purity copper ingot is obtained after the melt is condensed under the action of circulating cooling water.
In whole casting process, the recirculated cooling water pipeline that mould 11 and collet 12 were equipped with is in the running state all the time, make the fuse-element in mould 11 all can realize quick cooling in axial and footpath, both can guarantee the surface quality and the inside microstructure of ingot casting, the adhesion of outer wall and 11 inner walls of mould when can avoiding the metal fuse-element to solidify again, do benefit to the life who prolongs the mould, in addition still can shorten the time of drawing a furnace, greatly improve production efficiency. The red copper casting mould is adopted, so that the phenomenon that the metal melt reacts with the casting mould material in the casting process to cause the surface of the cast ingot to generate impurities to be polluted is avoided, and the quality of the cast ingot is reduced.
By the embodiment of the invention, the high-purity copper ingot with the size of 400 mm multiplied by 700mm, the purity of more than or equal to 99.99999 percent (7N), the oxygen content of less than or equal to 1ppm, the carbon content of less than or equal to 1ppm, the nitrogen content of less than or equal to 1ppm, and clean and defect-free interior can be obtained. Fig. 4 is a scan of internal metallurgical defects C of a high purity copper ingot according to an embodiment of the invention. Table 1 shows the purity test results of the high-purity copper ingots according to the examples of the present invention.
TABLE 1 purity test results of high-purity copper ingots
Example 2
As shown in FIG. 3, the method for preparing the high-purity copper-aluminum ingot by adopting the device comprises the following steps:
(1) The movable tray 3 is driven by the electric push rod 10 to move to the lower end of the crucible discharge port 4, and the discharge port 4 is sealed;
(2) Placing high-purity copper raw materials in a crucible 2 according to a certain stacking sequence, closing a furnace door arranged on a smelting furnace chamber 1, and vacuumizing the furnace until the vacuum degree is less than or equal to 1 multiplied by 10 -2 Pa, starting a heating power supply connected with the electromagnetic induction heating type crucible 2 to heat the raw material for one-time melting, melting the metal solid in the crucible 2 by using the principle of electromagnetic induction heating when current flows through an induction coil, stopping heating until the raw material is completely melted into a liquid melt, and heating for 45min at the temperature of 1250 ℃ from room temperature; turning off a power supply to naturally cool the melt for 1h, and fully escaping nitrogen, oxygen, carbon and other impurity elements with vapor pressure higher than that of the molten metal, so as to achieve the purposes of degassing, removing impurities and purifying the melt; starting a power supply again for heating, carrying out secondary melting, wherein the heating temperature is 1250 ℃, the heating time is 20min, adding the high-purity aluminum serving as the alloy raw material, and then obtaining a high-purity copper-aluminum alloy melt; raising the temperature to 1320 ℃, refining the copper-aluminum alloy melt, and simultaneously filling argon into a hearth until the pressure in the furnace is-0.09 to-0.05 MPa, further degassing and removing impurities, and improving the surface quality of the cast ingot; there are two main positions for monitoring the temperature of the metal melt, one of which is the temperature of the crucible 2: fixing a temperature measuring protection tube on the outer wall of the crucible 2, and monitoring the temperature of the crucible 2 in real time by using a thermocouple; secondly the temperature of the outer catheter 5: inserting a temperature measuring protection tube on the outer wall of the outer guide tube 5, and monitoring and controlling the temperature of induction heating in the outer guide tube 5 in real time by using an armored tungsten-rhenium thermocouple;
(3) After smelting is finished, a casting stage is carried out, before casting, an induction coil 18 outside an outer guide pipe 5 is electrified, so that condensed metal melt entering a flow nozzle assembly is heated and melted, a movable tray 3 is moved to be separated from a crucible discharge port 4, the prepared high-purity copper-aluminum alloy melt enters a casting mold 11 through the flow nozzle assembly to be filled, a bottom support 12 is driven by a servo motor 17 to rotate in a reciprocating mode along the horizontal direction, the components of the alloy melt are uniform, an internal structure with fine grains and few metallurgical defects is obtained, and the melt is condensed under the action of circulating cooling water to obtain the high-purity copper-aluminum alloy cast ingot.
In whole casting process, the recirculated cooling water pipeline that mould 11 and collet 12 set up is the cooling circulation water in the metal bellows all the time and is in the running state, make the fuse-element in mould 11 all can realize quick cooling in axial and footpath, both can guarantee the surface quality and the inside microstructure of ingot casting, the adhesion of outer wall and 11 inner walls of mould when can avoiding the metal fuse-element to solidify again, do benefit to the life who prolongs the mould, in addition still can shorten the time of drawing a furnace, greatly improve production efficiency. The red copper casting mould is adopted, so that the phenomenon that the metal melt reacts with the casting mould material in the casting process to cause the surface of the cast ingot to generate impurities to be polluted is avoided, and the quality of the cast ingot is reduced.
By the embodiment of the invention, the high-purity copper-aluminum alloy ingot with the size of phi 300 multiplied by 700mm, the purity of more than or equal to 99.99995 percent (6N 5), the oxygen content of less than or equal to 1ppm, the carbon content of less than or equal to 1ppm, the nitrogen content of less than or equal to 1ppm, the Al alloy component fluctuation of less than 5 percent, and clean and defect-free interior can be obtained. FIG. 5 is a C scan of the internal metallurgical defects of the high purity copper aluminum alloy ingot of the embodiment of the invention. Table 2 shows the purity test results of the high-purity copper-aluminum alloy ingot according to the embodiment of the present invention.
TABLE 2 purity test results of high-purity copper-aluminum alloy ingot
Example 3
As shown in fig. 3, a method for preparing a high-purity copper-manganese ingot by using the device comprises the following steps:
(1) The movable tray 3 is driven by the electric push rod 10 to move to the lower end of the crucible discharge port 4, and the discharge port 4 is sealed;
(2) Placing high-purity copper raw materials in a crucible 2 according to a certain stacking sequence, closing a furnace door arranged in a smelting furnace chamber 1, and vacuumizing the furnace until the vacuum degree is less than or equal to 1 multiplied by 10 -2 Pa, starting a heating power supply connected with the electromagnetic induction heating type crucible 2 to heat the raw material for melting for one time, and when current flows through the induction coil, utilizing the principle of electromagnetic induction heating to ensure that the raw material in the crucible 2 is meltedMelting the metal solid, stopping heating until the raw material is completely melted into a liquid melt, wherein the heating temperature is from room temperature to 1200 ℃, and the heating time is 30min; turning off the power supply to naturally cool the melt for 1h, and fully escaping nitrogen, oxygen, carbon and other impurity elements with vapor pressure higher than that of the molten metal, so as to achieve the purposes of degassing, removing impurities and purifying the melt; starting a power supply again for heating, carrying out secondary melting at the heating temperature of 1200 ℃ for 30min, adding high-purity manganese serving as an alloy raw material, and then obtaining a high-purity copper-manganese alloy melt; raising the temperature to 1300 ℃ for refining the copper-manganese alloy melt, and simultaneously filling argon into a hearth until the pressure in the furnace is-0.09 to-0.05 MPa, further degassing and removing impurities, and improving the surface quality of the cast ingot; there are mainly two positions for monitoring the temperature of the metal melt, one of which is the temperature of the crucible 2: fixing a temperature measuring protection tube on the outer wall of the crucible 2, and monitoring the temperature of the crucible in real time by using a thermocouple; second is the temperature of the outer catheter 5: inserting a temperature measuring protection tube on the outer wall of the outer guide tube 5, and monitoring and controlling the temperature of induction heating in the outer guide tube 5 in real time by using an armored tungsten-rhenium thermocouple;
(3) After smelting, the casting stage is carried out, before casting, an induction coil 18 outside an outer guide pipe 5 is electrified, so that condensed metal melt entering a nozzle assembly is heated and melted, a movable tray 3 is moved to separate from a crucible discharge port 4, the prepared high-purity copper-manganese alloy melt enters a casting mold 11 through the nozzle assembly to be molded, a bottom support 12 is driven by a servo motor 17 to rotate in a reciprocating mode along the horizontal direction, the components of the alloy melt are uniform, an internal structure with fine grains and few metallurgical defects is obtained, and the melt is condensed under the action of circulating cooling water to obtain the high-purity copper-manganese alloy cast ingot.
In whole casting process, the recirculated cooling water pipeline that mould 11 and collet 12 were equipped with is in the running state all the time, make the fuse-element in mould 11 all can realize quick cooling in axial and footpath, both can guarantee the surface quality and the inside microstructure of ingot casting, the adhesion of outer wall and 11 inner walls of mould when can avoiding the metal fuse-element to solidify again, do benefit to the life who prolongs the mould, in addition still can shorten the time of drawing a furnace, greatly improve production efficiency. The red copper casting mould is adopted, so that the phenomenon that the metal melt reacts with the casting mould material in the casting process to cause the surface of the cast ingot to generate impurities to be polluted is avoided, and the quality of the cast ingot is reduced.
By the embodiment of the invention, the high-purity copper-manganese alloy ingot with the size of phi 200 multiplied by 700mm, the purity of more than or equal to 99.9999 percent (6N), the oxygen content of less than or equal to 1ppm, the carbon content of less than or equal to 1ppm, the nitrogen content of less than or equal to 1ppm, the Mn alloy component fluctuation of less than 5 percent, and clean and defect-free interior can be obtained. FIG. 6 is a C-scan of internal metallurgical defects of a high purity Cu-Mn alloy ingot according to an embodiment of the present invention. Table 3 shows the purity test results of the high-purity copper-manganese alloy ingots according to the examples of the present invention.
TABLE 3 purity test results of high-purity Cu-Mn alloy ingots
Compared with the traditional smelting process, the liquid metal material in the crucible 2 can be fully stirred under the action of electromagnetic force, and the components of the metal melt are more uniform during casting. Meanwhile, in the smelting process, the smelting temperature can be adjusted by controlling the vacuum degree and the heating power, so that nitrogen, oxygen, carbon and other impurity elements with vapor pressure higher than that of the smelted metal in the metal melt can fully escape, and the purposes of degassing, removing impurities and purifying the melt are achieved. Compared with the traditional casting process, the bottom of the crucible 2 is adopted for casting, the metal melt in the crucible 2 is injected into the lower casting mold 11 through the bottom flow nozzle, so that the oxide or inclusion and the like floating on the top layer of the liquid surface of the metal melt in the crucible 2 finally flow into the casting mold 11 and are intensively distributed on the top of the cast ingot, so that the oxide or inclusion and the like can be removed when a shrinkage cavity is sawed in the subsequent process, the risk that the oxide inclusion and the like enter the interior of the cast ingot tissue to cause defects is reduced, and the method is favorable for obtaining the high-purity copper and copper alloy cast ingot with clean and defect-free interior.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention. It should be noted that other equivalent modifications can be made by those skilled in the art in light of the teachings of the present invention, and all such modifications can be made as are within the scope of the present invention.
Claims (11)
1. The device for preparing the high-purity copper and copper alloy cast ingot is characterized by comprising the following components: the smelting furnace chamber, and a smelting device and a casting device which are arranged in the smelting furnace chamber from top to bottom; the smelting device comprises a crucible, a spout assembly and a movable tray, wherein the spout assembly is inserted into a discharge hole formed in the bottom of the crucible, and the movable tray is arranged below the discharge hole of the crucible; the casting device comprises a casting mold and a bottom support, an opening at the upper end of the casting mold is opposite to the crucible discharge port, and the casting mold is arranged on the bottom support.
2. The apparatus for preparing the high-purity copper and copper alloy ingot according to claim 1, wherein the nozzle assembly comprises an outer guide pipe and an inner pipe which is detachably sleeved in the outer guide pipe, and the outer wall of the outer guide pipe is fixedly sleeved with the inner wall of the discharge hole of the crucible; and an induction coil is arranged outside the lower part of the outer conduit.
3. The apparatus of claim 2, wherein the outer conduit is a tapered tube and the inner conduit is a hollow cylindrical tube.
4. The apparatus for preparing high-purity copper and copper alloy ingots according to claim 1, wherein the movable tray comprises an upper tray and a lower supporting rod, the upper tray is connected with a rod body at one end of the lower supporting rod through a four-bar linkage mechanism, and the other end of the lower supporting rod is connected with an electric push rod arranged outside a smelting furnace chamber.
5. The apparatus according to claim 1, wherein the casting mold is a water-cooled copper mold comprising a cylindrical shell with an upper opening and a lower opening, the cylindrical shell is composed of two opposite semicircular plates connected by a clamping band, and the outer wall of the cylindrical shell is provided with a circulating cooling water pipeline.
6. The apparatus for preparing the high purity copper and copper alloy ingot according to claim 5, wherein the casting mold is provided with a riser at the top thereof.
7. The apparatus for preparing the high-purity copper and copper alloy ingots according to claim 1, wherein the base is a water-cooled copper base comprising a hollow cylinder which is closed up and down, the bottom of the hollow cylinder is provided with a water inlet, the upper part of the side wall is provided with a water outlet, the base is arranged at the bottom of the smelting furnace chamber, and the bottom of the base is connected with a servo motor arranged outside the smelting furnace chamber.
8. The apparatus according to claim 1, wherein the crucible is an electromagnetic induction heating type crucible.
9. A method for producing high purity copper and copper alloy ingots using the apparatus of any of claims 1 to 8, comprising:
(1) Placing the movable tray at the lower end of the discharge port of the crucible, and sealing the discharge port;
(2) Placing a high-purity copper raw material in a crucible, and carrying out primary melting, cooling, secondary melting and refining, wherein when a copper alloy ingot is prepared, the alloy raw material is added in the secondary melting process, and then high-purity copper or a copper alloy melt is obtained;
(3) And the movable tray is separated from a discharge hole of the crucible, the high-purity copper or copper alloy melt enters the casting mold through the flow nozzle assembly, and a high-purity copper or copper alloy cast ingot is obtained after cooling.
10. The method according to claim 9, wherein the primary melting in step (2): vacuumizing to the vacuum degree less than or equal to 1 × 10 -2 Pa, heating at 1200-1300 ℃ for 30-60min; cooling for 1h; secondary melting: heating at 1200 to 1300 deg.CHeating at 15-30min; refining: filling argon into the hearth at the temperature of 1300-1350 ℃ until the pressure in the furnace is-0.09-0.05 MPa.
11. The method of claim 9, wherein in step (3), the collet is rotated back and forth in a horizontal direction by a servo motor.
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| CN202211112499.6A CN115178714B (en) | 2022-09-14 | 2022-09-14 | Preparation device and method of high-purity copper and copper alloy cast ingot |
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| CN115178714B (en) | 2022-12-09 |
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