CN115069990B - Preparation method of anaerobic copper bar - Google Patents
Preparation method of anaerobic copper bar Download PDFInfo
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- CN115069990B CN115069990B CN202210905167.7A CN202210905167A CN115069990B CN 115069990 B CN115069990 B CN 115069990B CN 202210905167 A CN202210905167 A CN 202210905167A CN 115069990 B CN115069990 B CN 115069990B
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- copper
- filter cover
- crystallizer
- liquid inlet
- preparation
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- 239000010949 copper Substances 0.000 title claims abstract description 43
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 40
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 40
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 36
- 238000007664 blowing Methods 0.000 claims abstract description 19
- PTVDYARBVCBHSL-UHFFFAOYSA-N copper;hydrate Chemical compound O.[Cu] PTVDYARBVCBHSL-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000003723 Smelting Methods 0.000 claims abstract description 13
- 238000004321 preservation Methods 0.000 claims abstract description 13
- 239000012530 fluid Substances 0.000 claims abstract description 11
- 238000004891 communication Methods 0.000 claims abstract description 10
- 238000005266 casting Methods 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 239000012535 impurity Substances 0.000 claims abstract description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 4
- 239000003610 charcoal Substances 0.000 claims description 3
- 239000000498 cooling water Substances 0.000 claims description 3
- 229910052761 rare earth metal Inorganic materials 0.000 claims description 3
- 150000002910 rare earth metals Chemical class 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 8
- 229910052760 oxygen Inorganic materials 0.000 abstract description 8
- 239000001301 oxygen Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000011161 development Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910000881 Cu alloy Inorganic materials 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000013535 sea water Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/10—Supplying or treating molten metal
- B22D11/11—Treating the molten metal
- B22D11/116—Refining the metal
- B22D11/119—Refining the metal by filtering
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/04—Continuous casting of metals, i.e. casting in indefinite lengths into open-ended moulds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22D—CASTING OF METALS; CASTING OF OTHER SUBSTANCES BY THE SAME PROCESSES OR DEVICES
- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/14—Plants for continuous casting
- B22D11/145—Plants for continuous casting for upward casting
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a preparation method of an anaerobic red copper rod, which is characterized by comprising the following steps of: the oxygen-free red copper rod comprises the following components in percentage by mass of Cu more than or equal to 99.97 percent and the balance of unavoidable impurities; the preparation method comprises the following preparation steps: 1) Smelting: the bottom of the crystallizer is provided with a filter cover which is in fluid communication with the inner cavity of the crystallizer, and the bottom of the heat preservation furnace is provided with a bottom blowing device which is in fluid communication with the inner cavity of the crystallizer; the filter cover is tubular and comprises a bottom wall and a side wall arranged along the circumference of the bottom wall, the filter cover is positioned 50-100 mm below the liquid level of the molten copper, and a plurality of circles of liquid inlet holes are formed in the side wall of the filter cover from bottom to top; 2) And (5) continuously casting and leading out the copper rod. The bottom of the crystallizer is provided with the filter cover which is in fluid communication with the inner cavity of the crystallizer, the pressure of the copper water entering the mouth of the crystallizer can be uniformly distributed by the filter cover by adopting the siphon principle, the instantaneous suction force of the copper water inlet is reduced, the risk that impurities such as graphite flakes enter the guide rod is eliminated, the risk that bubbles brought by a bottom blowing process enter the guide rod is eliminated, and the oxygen content of the red copper guide rod and the air hole and hollow problems are reduced.
Description
Technical Field
The invention belongs to the technical field of copper alloy, and particularly relates to a preparation method of an anaerobic red copper rod.
Background
Red copper, also called red copper, is widely used in the chemical industry because of its excellent electrical conductivity, cold and hot workability, and because of its excellent corrosion resistance in the atmosphere, seawater and various acid and alkali environments, and is widely used in electrical and heat conductive equipment such as wires, cables, brushes and others.
With the high-speed development of the technologies in the fields of household appliances, transportation, power engineering, renewable energy sources, smart grids and the like, the requirements for semiconductor devices with the characteristics of high input impedance, low voltage control power consumption, simple control circuit, high voltage resistance, high bearing current and the like are more and more obvious, the requirements for the semiconductor devices are more and more urgent, and the requirements for the characteristics of the semiconductor devices are well met by IGBT (insulated gate bipolar transistor).
The high-conductivity (more than 100% IACS) and high-temperature-resistant (more than 200 ℃) red copper bars are needed to be used for conducting and transmitting heat in IGBT production, and the upward red copper bars used for the red copper bars produced in the prior art have the problems of surface oxidation, slag inclusion, air holes, hollowness and the like, the oxygen content is higher than 10ppm, the requirements of the IGBT on the high conductivity and the high-temperature resistance of the red copper bars are difficult to meet, and the development and the production of the high-quality upward red copper bars are urgent in view of the development and the production.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of an oxygen-free red copper rod with high conductivity, high temperature resistance and other comprehensive properties.
The technical scheme adopted for solving the technical problems is as follows: a preparation method of an anaerobic copper bar is characterized in that: the oxygen-free red copper rod comprises the following components in percentage by mass of Cu more than or equal to 99.97 percent and the balance of unavoidable impurities; the preparation method comprises the following preparation steps:
1) Smelting: adding an electrolytic plate into a smelting furnace for smelting, keeping the temperature between 1140 and 1170 ℃ after electrolytic copper is completely smelted, covering the copper surface with charcoal, introducing copper water into a heat preservation furnace from the smelting furnace, covering the copper surface in the heat preservation furnace with graphite flakes, adding 0.03 to 0.04 weight percent of rare earth, arranging a crystallizer inserted into the copper water at the top of the heat preservation furnace, arranging a filter cover at the bottom of the crystallizer and in fluid communication with the inner cavity of the crystallizer, and arranging a bottom blowing device at the bottom of the heat preservation furnace and in fluid communication with the inner cavity of the crystallizer; the filter cover is tubular, comprises a bottom wall and side walls arranged along the circumference of the bottom wall, the filter cover is positioned 50-100 mm below the liquid level of the molten copper, a plurality of circles of liquid inlet holes are formed in the side walls of the filter cover from bottom to top, the inner diameter of the filter cover is R, and the hole spacing L 1 of each circle of adjacent liquid inlet holes is as follows: 6-10 mm, diameter R1 of each liquid inlet hole: 1-3 mm, and the number of open holes is an integer through R/6;
2) Leading up and continuously casting to lead out a copper bar: casting temperature 1140-1170 ℃, and copper water inflow speed V2 of a liquid inlet hole: 3.0-4.0 m/s, and the pulling speed V1: 300-360 mm/min, controlling the temperature difference between the inlet water and the outlet water of cooling water at 20-30 ℃, pulling for 10-40 min, starting a bottom blowing device, blowing nitrogen for 30-60 min, then introducing nitrogen mixed with carbon monoxide, wherein the bottom blowing pressure is 0.2-0.5 MPa, and the flow is 2-8L/min.
Diameter R1 of each liquid inlet hole: 1-3 mm, the diameter is larger than 3mm, the liquid suction force of the liquid inlet hole is larger, graphite flakes and oxidized scum are easy to suck into the guide rod, and bottom blowing bubbles are easy to suck, so that the hollow problem of the guide rod is caused, the diameter is smaller than 1mm, the liquid inlet of the liquid inlet hole is not easy to split and divide, the liquid supplementing is not timely caused directly, and the guide rod is pulled and interrupted; the hole spacing refers to the distance from the center of one hole to the center of the other hole, the hole spacing is 6-10 mm, the liquid inlet holes below 6mm are too dense, the liquid inlet is not beneficial to the liquid inlet split flow and the partial pressure, the liquid inlet holes above 10mm are not matched with the diameter of the liquid inlet holes of 1-3 mm, and the liquid supplementing amount of the copper water cannot follow up.
The bottom blowing pressure is lower than 0.2MPa, bubbles are difficult to generate, the bottom blowing pressure is higher than 0.5MPa, the pressure is too large, huge bubbles are generated, oxygen removal is not facilitated, oxidized scum is also not facilitated to be carried out, meanwhile, potential safety hazards exist, the flow is lower than 2L/min, the amount of bubbles is small, a large amount of bubbles are generated higher than 8L/min, and the combination of carbon monoxide and oxygen and the removal of oxidized slag by the bubbles are not facilitated.
Preferably, the value of the inner diameter R of the filter cover, the hole spacing L 1, the diameter R1 of the liquid inlet hole, the diameter a/mm of the red copper rod, the drawing speed V1/mm/s and the copper water flowing speed V2/mm/s of the liquid inlet hole satisfy the following conditions: a 2V1L1/πV2R1 2 < [ R/6 ]. Times.R, wherein [ R/6] represents an integer of R/6. By establishing the relation that the liquid inlet amount is larger than the pulling amount, the R value meeting the safety requirement is obtained, the pulling interruption of the upper guide rod is avoided, the upper guide rod is easy to drop and hurt people at a high position, and the crystallizer is easy to burn.
Compared with the prior art, the invention has the advantages that: the bottom of the crystallizer is provided with a filter cover which is in fluid communication with the inner cavity of the crystallizer, the pressure of the copper water entering the mouth of the crystallizer can be uniformly distributed by the filter cover by adopting a siphon principle, the instant suction force of the copper water inlet is reduced, the risk that impurities such as graphite flakes enter a guide rod is eliminated, the risk that bubbles brought by a bottom blowing process enter the guide rod is eliminated, the oxygen content of the red copper guide rod and the air holes and the hollow problem are reduced, the oxygen content of the red copper rod is lower than 10ppm, the average grain size is lower than 50 mu m, the electric conductivity is higher than 100 percent IACS, the tensile strength is higher than 200MPa, the elongation is higher than 55 percent, and the high-temperature softening temperature is higher than 200 ℃.
Drawings
Fig. 1 is a schematic structural diagram of an insulation furnace according to an embodiment of the present invention, wherein 1 is a crystallizer, 2 is a filter cover, and 3 is a bottom blowing device.
Detailed Description
The invention is described in further detail below with reference to the embodiments of the drawings.
The invention provides 4 examples and 2 comparative examples, wherein the examples are prepared by the preparation method of the invention, and the specific preparation steps are as follows:
1) Smelting: adding an electrolytic plate into a 5t power frequency smelting furnace for smelting, keeping the temperature between 1140 and 1170 ℃ after electrolytic copper is completely smelted, covering the surface of copper with charcoal, introducing copper water into a heat preservation furnace from the smelting furnace, covering the surface of copper water in the heat preservation furnace with graphite flakes, adding 0.03 to 0.04 weight percent of rare earth at the same time, arranging a crystallizer inserted into the copper water at the top of the heat preservation furnace, arranging a filter cover at the bottom of the crystallizer and in fluid communication with the inner cavity of the crystallizer, and arranging a bottom blowing device at the bottom of the heat preservation furnace and in fluid communication with the inner cavity of the crystallizer; the filter cover is tubular, comprises a bottom wall and side walls arranged along the circumference of the bottom wall, the filter cover is positioned 50-100mm below the liquid level of the molten copper, a plurality of circles of liquid inlet holes are formed in the side walls of the filter cover from bottom to top, the inner diameter of the filter cover is R, and the hole spacing L 1 between each circle of liquid inlet holes is formed in each circle: 6-10 mm, diameter R1 of each liquid inlet hole: 1-3 mm, and the number of open holes is an integer through R/6;
2) Leading up and continuously casting to lead out a copper bar: casting temperature 1140-1170 ℃, and copper water inflow speed V2 of a liquid inlet hole: 3.0-4.0 m/s, and the pulling speed V1: 300-360 mm/min, controlling the temperature difference between the inlet water and the outlet water of cooling water at 15-20 ℃, pulling for 10-40 min, starting a bottom blowing device, blowing nitrogen for 30-60 min, then introducing nitrogen mixed with carbon monoxide, wherein the bottom blowing pressure is 0.2-0.5 MPa, and the flow is 2-8L/min.
The value of the inner diameter R of the filter cover, the hole spacing L 1, the diameter R1 of the liquid inlet hole, the diameter a/mm of the red copper rod, the drawing speed V1/mm/s and the copper water flowing speed V2/mm/s of the liquid inlet hole satisfy the following conditions: a 2V1L1/πV2R1 2 < [ R/6 ]. Times.R, wherein [ R/6] represents an integer of R/6.
Comparative example 1 differs from the example in that: there is no filter housing.
Comparative example 2 differs from the example in that: r does not correspond to: a 2V1L1/πV2R1 2 < [ R/6 ]. Times.R, R is 14mm, which results in that the fluid infusion is not timely and is easy to form a hollow.
The following tests were carried out on the examples and comparative examples obtained:
Average grain size detection: GBT 6394-2017 metal average grain size determination method.
Oxygen content detection: the GBT5158.1-2011 metal powder reduction method is used for measuring the oxygen content.
Tensile strength: and testing by a conventional tension machine.
Conductivity of: and (5) conducting the test by a conductivity meter.
High temperature softening temperature: GB/T33370-2016 copper and copper alloy softening temperature measuring method.
TABLE 1 composition and key process parameter control for embodiments of the invention
TABLE 2 Key process parameter control for embodiments of the invention
TABLE 3 microstructure and Properties of examples and comparative examples of the invention
Claims (1)
1. A preparation method of an anaerobic copper bar is characterized in that: the oxygen-free red copper rod comprises the following components in percentage by mass of Cu more than or equal to 99.97 percent and the balance of unavoidable impurities; the preparation method comprises the following preparation steps:
1) Smelting: adding an electrolytic plate into a smelting furnace for smelting, keeping the temperature between 1140 and 1170 ℃ after electrolytic copper is completely smelted, covering the copper surface with charcoal, introducing copper water into a heat preservation furnace from the smelting furnace, covering the copper surface in the heat preservation furnace with graphite flakes, adding 0.03 to 0.04 weight percent of rare earth, arranging a crystallizer inserted into the copper water at the top of the heat preservation furnace, arranging a filter cover at the bottom of the crystallizer and in fluid communication with the inner cavity of the crystallizer, and arranging a bottom blowing device at the bottom of the heat preservation furnace and in fluid communication with the inner cavity of the crystallizer; the filter cover is tubular, comprises a bottom wall and side walls arranged along the circumference of the bottom wall, the filter cover is positioned 50-100 mm below the liquid level of the molten copper, a plurality of circles of liquid inlet holes are formed in the side walls of the filter cover from bottom to top, the inner diameter of the filter cover is R, and the hole spacing L 1 of each circle of adjacent liquid inlet holes is as follows: 6-10 mm, diameter R1 of each liquid inlet hole: 1-3 mm, and the number of open holes is an integer through R/6;
2) Leading up and continuously casting to lead out a copper bar: casting temperature 1140-1170 ℃, and copper water inflow speed V2 of a liquid inlet hole: 3.0-4.0 m/s, and the pulling speed V1: 300-360 mm/min, controlling the temperature difference between the inlet water and the outlet water of cooling water at 20-30 ℃, pulling for 10-40 min, starting a bottom blowing device, firstly blowing nitrogen for 30-60 min, then introducing nitrogen mixed with carbon monoxide, wherein the bottom blowing pressure is 0.2-0.5 MPa, and the flow is 2-8L/min;
The value of the inner diameter R of the filter cover is equal to the hole spacing L 1, the diameter R1 of the liquid inlet hole and the diameter a/mm of the red copper rod, the drawing speed V1/mm/s and the copper water flowing speed V2/mm/s of the liquid inlet hole are as follows: a 2V1L1/πV2R1 2 < [ R/6 ]. Times.R, wherein [ R/6] represents an integer of R/6.
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