CN110218898B - Preparation method of copper-chromium-zirconium alloy wire - Google Patents
Preparation method of copper-chromium-zirconium alloy wire Download PDFInfo
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- CN110218898B CN110218898B CN201910477612.2A CN201910477612A CN110218898B CN 110218898 B CN110218898 B CN 110218898B CN 201910477612 A CN201910477612 A CN 201910477612A CN 110218898 B CN110218898 B CN 110218898B
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- B22D11/00—Continuous casting of metals, i.e. casting in indefinite lengths
- B22D11/001—Continuous casting of metals, i.e. casting in indefinite lengths of specific alloys
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention relates to a preparation method of a copper-chromium-zirconium alloy wire, which comprises the following steps: (1) preparing materials; (2) smelting; (3) continuous casting: when the temperature of the heat preservation furnace reaches the casting temperature, continuously casting by adopting a crystallizer with a chromium-added silicon nitride lining to obtain a casting blank, simultaneously adding a copper-zirconium alloy core wire into the heat preservation furnace by a wire feeding method according to the burning loss rule of zirconium, wherein the copper-zirconium alloy core wire is arranged on the outer layer and is a copper skin and the inner layer is a zirconium core; (4) carrying out plastic processing and defect removal treatment on the casting blank to obtain a wire rod; (5) and carrying out multistage step aging treatment on the wire rod. The method can stably control the contents of zirconium and chromium, and can produce the copper-chromium-zirconium alloy wire rod continuously in a short process.
Description
Technical Field
The invention relates to the technical field of copper alloy materials and processes, in particular to a preparation method of a copper-chromium-zirconium alloy wire.
Background
Compared with the common copper alloy, the copper-chromium-zirconium alloy has excellent conductivity, tensile strength, elasticity and high-temperature softening resistance, and can be used for manufacturing lead frame materials, elastic materials, aerospace cables, large-scale integrated circuit leads, spot welding electrodes and wire harnesses of automobiles and electronic control systems and the like. Has wide application prospect in the industrial fields of electronic products, aerospace, automobile parts, mechanical and electrical appliances and the like. The material takes copper as a base, and metal chromium and metal zirconium are added, because the chromium and the zirconium have extremely strong affinity with oxygen under the condition of high-temperature smelting and casting, and are very easy to oxidize and volatilize in the smelting and casting processes, the production difficulty is higher. Vacuum melting and casting methods are generally required to reduce oxidation and volatilization and ensure that the final product has satisfactory chemical compositions.
The existing smelting process of the copper-chromium-zirconium alloy mainly comprises two processes, one process is a vacuum smelting and extruding process, due to the inherent structure of the vacuum induction furnace, the production mode is only limited to products operated periodically, the weight or length of single casting is limited by the capacity of a crucible, products with larger weight or theoretically infinite length cannot be produced, and the production cost is higher; the other is a non-vacuum melting + continuous casting + extrusion process, which has the disadvantages that the components in the alloy are difficult to control and that products of larger weight or theoretically unlimited length cannot be produced as in the vacuum melting + extrusion process.
In addition, the crystallizer lining in the prior art adopts a graphite lining, and zirconium element in the copper-chromium-zirconium alloy reacts with the graphite lining to cause corrosion of the graphite lining, cracking and snapping of the surface of an ingot in the casting process, and loss of the zirconium element in the copper-chromium-zirconium alloy. Therefore, a short-flow continuous preparation method of the copper-chromium-zirconium alloy wire rod capable of stably controlling the contents of zirconium and chromium is needed.
Disclosure of Invention
The invention aims to solve the technical problem of providing a short-flow continuous preparation method of a copper-chromium-zirconium alloy wire rod, which can stably control the contents of zirconium and chromium, aiming at the current situation of the prior art.
The technical scheme adopted by the invention for solving the technical problems is as follows: a preparation method of a copper-chromium-zirconium alloy wire rod comprises the following steps:
(1) preparing materials: weighing the raw materials according to the component proportion of the copper-chromium-zirconium alloy;
(2) smelting; melting the raw materials of each component in several times, and transferring the raw materials into a heat preservation furnace filled with protective gas;
(3) continuous casting: when the temperature of the heat preservation furnace reaches the casting temperature, continuously casting by adopting a crystallizer with a chromium-added silicon nitride lining to obtain a casting blank, simultaneously adding a copper-zirconium alloy core wire into the heat preservation furnace by a wire feeding method according to the burning loss rule of zirconium, wherein the copper-zirconium alloy core wire is arranged on the outer layer and is a copper skin and the inner layer is a zirconium core;
(4) performing plastic processing on the casting blank, and performing or not performing surface defect removal treatment according to the requirement to obtain a wire rod;
(5) and carrying out multistage step aging treatment on the wire rod.
And (6) cleaning the surface of the wire rod, and grinding, polishing and straightening the surface of the wire rod for better wire rod quality.
Preferably, the raw materials comprise Cu, Cr and a Cu-Y intermediate alloy with 15-20% of Y content, and the fractional melting in the step (2) comprises the following steps: adding Cu into the solution to be melted, adding a covering agent to cover the solution, and adding a deoxidizing agent to perform deoxidation treatment; and (3) raising the temperature to 1250-1350 ℃, starting adding Cr, preserving the temperature for 15-45 minutes, adding the copper-yttrium intermediate alloy, and controlling the temperature to 1200-1400 ℃. The rare earth yttrium reacts with peritectic reaction generated in the casting process of the copper chromium zirconium alloy wire rod to prevent the enrichment and growth of Cr particles in the casting process, thereby improving the dispersion strengthening effect of the copper chromium zirconium alloy and ensuring excellent performance.
Preferably, the copper-chromium-zirconium alloy wire rod comprises the following components in percentage by mass: 0.7 to 1 percent of Cr0; zr0.05-0.15%; y0.02-0.1%; the balance being copper; the deoxidizer is 0.05-0.1% of Mg, and the added Mg can improve the high-temperature softening resistance. The casting temperature of the copper chromium zirconium alloy wire rod is 1250-1350 ℃.
In order to accurately control the zirconium content, the zirconium content of the copper-zirconium alloy core wire in the step (3) is 20-30 wt%, and the copper-zirconium alloy core wire is continuously added by adopting an automatic wire feeding machine according to the burn-out rule of 0.005-0.02 wt% of zirconium in 1 minute, so that the zirconium content is controlled within the range of 0.05-0.15 wt%.
Preferably, the mass fractions of the components of the covering agent are 30-40% of cryolite, 30-40% of sodium carbonate and 30-40% of calcium fluoride. Further preferably, the covering agent consists of cryolite, sodium carbonate and calcium fluoride in a ratio of 1:1: 1. The covering agent has the functions of covering, preventing element from burning and degassing. In addition, the covering agent mentioned in the Chinese invention of "a covering agent for chromium zirconium copper smelting and its preparation and use method", which is published under the publication number CN108977679A (application number CN201810814454.0), or other covering agents commonly used in the art can be used as the covering agent.
Preferably, the chromium element content of the lining is 0 to 0.5% (excluding 0). More preferably, the content of the chromium element is 0.1%.
In order to realize online solid solution, controlling the surface temperature of the casting blank out of the crystallizer to be 750-850 ℃ during the continuous casting in the step (3); and secondary strong cooling water is sprayed on the surface of the casting blank at the outlet of the crystallizer, the temperature of the cooling water is 15-30 ℃, and the water pressure is 0.2-0.5 MPa. In order to control the surface temperature of the casting blank, the specification of the casting bar blank is phi 12-50 mm, and the casting speed is controlled to be 0.6-2.0 m/min.
To further improve performance, the multistage ageing comprises the following steps: the aging temperature is increased to 500-550 ℃, the temperature is kept for 0.5-1 h, then the temperature is reduced to 400-450 ℃, and the temperature is kept for 2-3 h.
Preferably, the plastic working of the step (4) is sequentially cold rolling, drawing, and then scalping to remove surface defects.
In order to prevent the burning loss of chromium and zirconium from reducing, the protective gas is argon, and the positive pressure of the argon is maintained at 0.005-0.05 MPa.
The copper-chromium-zirconium alloy wire rod prepared by the method has good processing performance and casting performance, and meanwhile, the alloy has the advantages of high strength, good conductivity, excellent elasticity and good high-temperature stress relaxation resistance.
Compared with the prior art, the invention has the advantages that: according to the invention, the crystallizer with the lining made of the silicon nitride material added with the chromium element is selected, the silicon nitride material can not react with chromium and zirconium, and the further addition of the chromium element can improve the high-temperature oxidation resistance of the lining, prevent the loss of chromium and zirconium and realize the short-flow and continuous copper-chromium-zirconium alloy wire; according to the invention, in the continuous casting process, zirconium is supplemented in a wire feeding mode according to the burning loss rule of zirconium, so that the stability of the zirconium content can be controlled, and the performance of the obtained copper-chromium-zirconium alloy wire can be stably controlled.
Drawings
FIG. 1 is a metallographic photograph of example 2 of the present invention;
fig. 2 is a metallographic photograph of example 2 of the present invention.
Detailed Description
The following examples are given to further illustrate the embodiments of the present invention.
The composition ratios of the copper chromium zirconium alloy strip according to four examples of the invention are shown in table 1 below:
table 1: alloy chemical composition (wt%) of the embodiment of the invention
Material numbering | Cr | Zr | Mg (deoxidizer) | Y | Cu |
Example 1 | 1 | 0.15 | 0.03 | 0.02 | Balance of |
Example 2 | 1.2 | 0.1 | 0.04 | 0.03 | Balance of |
Example 3 | 0.9 | 0.07 | 0.02 | 0.1 | Balance of |
Example 4 | 0.7 | 0.12 | 0.02 | 0.1 | Balance of |
Example 1
1) Material preparation and smelting: weighing the components according to the component proportion of the copper-chromium-zirconium alloy wire rod in the table 1, and adding Cu into a smelting furnace to be heated and melted; after the Cu is melted, adding a covering agent for covering; 0.03% magnesium was added for deoxidation treatment. And (3) heating to 1300 ℃, adding Cr, keeping the temperature for 20 minutes, and then adding a copper-yttrium intermediate alloy, wherein the amount of the added copper-yttrium intermediate alloy is 0.07 percent of the weight of the raw materials, and the yttrium content in the copper-yttrium intermediate alloy is 15-20 percent. Controlling the temperature at 1250 ℃, transferring into a heat preservation furnace, wherein the heat preservation furnace adopts inert gas for protection, and the positive pressure of argon in the heat preservation furnace is maintained at 0.005-0.05 MPa, so that the burning loss of chromium and zirconium which are particularly easy to oxidize in the heat preservation furnace is reduced. The covering agent of the embodiment is composed of cryolite, sodium carbonate and calcium fluoride according to the mass fraction of 1:1: 1.
2) When the temperature of the holding furnace reaches 1300 ℃, a crystallizer with a silicon nitride lining added with 0.5 percent of chromium is adopted for continuous casting. The specification of the casting bar blank is phi 28mm, the casting speed is controlled to be 0.9m/min, and the surface temperature of the casting blank discharged from the crystallizer is controlled to be 800 ℃. The casting blank at the outlet of the crystallizer adopts strong cooling water, the water temperature of the cooling water is 15 ℃, and the water pressure is 0.2MPa, so that the online solid solution effect of the chromium-zirconium-copper casting blank is realized. Simultaneously, according to a zirconium burning loss rule and then according to a 0.006 percent zirconium burning loss rule in minutes, the copper-zirconium alloy cored wire is continuously added in the heat preservation furnace by adopting an automatic wire feeding machine, so that the stable control of zirconium is ensured.
3) Cold rolling the casting blank from phi 28mm to phi 20mm, and drawing to phi 19mm
4) Peeling until phi 19mm is 18.7 mm.
5) Drawing from phi 18.7mm to phi 12mm in multiple passes.
6) And raising the aging temperature to 500 ℃, preserving the heat for 1h, then lowering the temperature to 430 ℃, and preserving the heat for 3 h.
7) And cleaning the surface of the finished product, and grinding, polishing and straightening the surface.
Example 2
1) Material preparation and smelting: weighing the components according to the component proportion of the copper-chromium-zirconium alloy wire rod in the table 1, and adding Cu into a smelting furnace to be heated and melted; after the Cu is melted, a covering agent is added for covering, 0.04 percent of magnesium is added for deoxidation treatment, and the effect of improving high-temperature softening resistance can be achieved. And (3) heating to 1320 ℃, adding Cr, keeping the temperature for 25 minutes, and then adding a copper-yttrium intermediate alloy, wherein the amount of the added copper-yttrium intermediate alloy is 0.08 percent of the weight of the raw materials, and the yttrium content in the copper-yttrium intermediate alloy is 15-20 percent. Controlling the temperature at 1300 ℃, transferring into a heat preservation furnace, preserving the heat of the heat preservation furnace by adopting inert gas argon, and maintaining the positive pressure of the argon in the heat preservation furnace at 0.005-0.05 MPa to ensure that the burning loss of chromium and zirconium which are particularly easy to oxidize in the heat preservation furnace is reduced. The covering agent of the embodiment is composed of cryolite, sodium carbonate and calcium fluoride according to the mass fraction of 30:30: 40.
2) When the temperature of the holding furnace reaches 1280 ℃, a crystallizer with a silicon nitride lining added with 0.1 percent of chromium is adopted for continuous casting. The specification of the casting bar blank is phi 30mm, the casting speed is controlled to be 1.1m/min, and the surface temperature of the casting blank out of the crystallizer is controlled to be 830 ℃. The casting blank at the outlet of the crystallizer adopts strong cooling water, the temperature of the cooling water is 30 ℃, and the water pressure is 0.5MPa, so that the online solid solution effect of the chromium-zirconium-copper casting blank is realized. Simultaneously, according to a zirconium burning loss rule and then according to a 0.006 percent zirconium burning loss rule in minutes, the copper-zirconium alloy cored wire is continuously added in the heat preservation furnace by adopting an automatic wire feeding machine, so that the stable control of zirconium is ensured.
3) Cold rolling the casting blank from phi 30mm to phi 22mm, and drawing to phi 20mm
4) Peeling with phi 20mm to phi 19.7 mm.
5) Drawing from phi 19.7mm to phi 12mm in multiple passes.
6) Raising the aging temperature to 550 ℃, preserving the heat for 0.5h, then lowering the temperature to 430 ℃ and preserving the heat for 3 h.
7) And cleaning the surface of the finished product, and grinding, polishing and straightening the surface.
Example 3
1) Material preparation and smelting: weighing the materials according to the component proportion of the copper-chromium-zirconium alloy wire, and adding Cu into a smelting furnace to be heated and melted; after the Cu is melted, a covering agent is added for covering, and 0.02 percent of magnesium is added for deoxidation treatment. And (3) heating to 1310 ℃, adding Cr, preserving the temperature for 30 minutes, and then adding a copper-yttrium intermediate alloy, wherein the amount of the added copper-yttrium intermediate alloy is 0.09% of the weight of the raw materials, and the yttrium content in the copper-yttrium intermediate alloy is 15-20%. Controlling the temperature to 1350 ℃, transferring into a heat preservation furnace, wherein the heat preservation furnace adopts inert gas argon for protection, and the positive pressure of argon in the heat preservation furnace is maintained at 0.005-0.05 MPa, so that the burning loss of chromium and zirconium which are particularly easy to oxidize in the heat preservation furnace is reduced. The covering agent of the embodiment is composed of cryolite, sodium carbonate and calcium fluoride according to the mass fraction of 30:40: 30.
2) When the temperature of the holding furnace reaches 1310 ℃, a crystallizer with a silicon nitride lining added with 0.3 percent of chromium is adopted for continuous casting. The specification of the casting bar blank is phi 26mm, the casting speed is controlled to be 1.3m/min, and the surface temperature of the casting blank out of the crystallizer is controlled to be 790 ℃. The casting blank at the outlet of the crystallizer adopts strong cooling water, the water temperature of the cooling water is 20 ℃, and the water pressure is 0.3MPa, so that the online solid solution effect of the chromium-zirconium-copper casting blank is realized. Meanwhile, according to the zirconium burning loss rule and then according to the 0.005% zirconium burning loss rule in minutes, the copper-zirconium alloy cored wire is continuously added in the heat preservation furnace by adopting an automatic wire feeding machine, so that the stable control of zirconium is ensured.
3) Cold rolling the casting blank from phi 26mm to phi 19mm, and then drawing to phi 18mm
4) Peeling until phi 18mm to phi 17.8 mm.
5) Drawing from phi 17.8mm to phi 12mm in multiple passes.
6) The aging temperature is increased to 500 ℃, the temperature is kept for 0.7h, then the temperature is reduced to 420 ℃, and the temperature is kept for 3 h.
7) And cleaning the surface of the finished product, and grinding, polishing and straightening the surface.
Example 4
1) Material preparation and smelting: weighing the materials according to the component proportion of the copper-chromium-zirconium alloy wire, and adding Cu into a smelting furnace to be heated and melted; and after the Cu is melted, adding a covering agent for covering. 0.02% magnesium was added for deoxidation treatment. And (3) heating to 1350 ℃, adding Cr, keeping the temperature for 15 minutes, and then adding a copper-yttrium intermediate alloy, wherein the amount of the added copper-yttrium intermediate alloy is 0.05 percent of the weight of the raw materials, and the yttrium content in the copper-yttrium intermediate alloy is 15-20 percent. Controlling the temperature at 1320 ℃, transferring into a holding furnace, wherein the holding furnace adopts inert gas argon for protection, and the positive pressure of argon in the holding furnace is maintained at 0.005-0.05 MPa, so that the burning loss of chromium and zirconium which are particularly easy to oxidize in the holding furnace is reduced. The covering agent of the embodiment is composed of cryolite, sodium carbonate and calcium fluoride according to the mass fraction of 40:30: 30.
2) When the temperature of the holding furnace reaches 1350 ℃, a crystallizer with a silicon nitride lining added with 0.2 percent of chromium is adopted for continuous casting. The specification of the casting bar blank is phi 24mm, the casting speed is controlled to be 1.5m/min, and the surface temperature of the casting blank discharged from the crystallizer is controlled to be 820 ℃. The casting blank at the outlet of the crystallizer adopts strong cooling water, the water temperature of the cooling water is 18 ℃, and the water pressure is 0.4MPa, so that the online solid solution effect of the chromium-zirconium-copper casting blank is realized. Simultaneously, according to a zirconium burning loss rule and then according to a 0.006 percent zirconium burning loss rule in minutes, the copper-zirconium alloy cored wire is continuously added in the heat preservation furnace by adopting an automatic wire feeding machine, so that the stable control of zirconium is ensured.
3) Cold rolling the casting blank from phi 24mm to phi 18mm, and drawing to phi 17mm
4) Peeling until phi 17mm to phi 16.8 mm.
5) Drawing from phi 16.8mm to phi 10mm in multiple passes.
6) Raising the aging temperature to 500 ℃, preserving the heat for 0.5h, then lowering the temperature to 400 ℃, and preserving the heat for 3 h.
7) And cleaning the surface of the finished product, and grinding, polishing and straightening the surface.
The performance test results of the copper-chromium-zirconium alloy wires prepared in the four examples are shown in table 2:
TABLE 2 product Performance parameters
As can be seen from Table 2, the Cu-Cr-Zr alloy strip prepared by the method has the characteristics of high strength, good conductivity, excellent elasticity, good high-temperature stress relaxation resistance and the like.
The technical means disclosed in the invention scheme are not limited to the technical means disclosed in the above embodiments, but also include the technical scheme formed by any combination of the above technical features. It should be noted that those skilled in the art can make various improvements and modifications without departing from the principle of the present invention, and such improvements and modifications are also considered to be within the scope of the present invention.
Claims (7)
1. The preparation method of the copper-chromium-zirconium alloy wire is characterized by comprising the following steps of:
(1) preparing materials: weighing the raw materials according to the component proportion of the copper-chromium-zirconium alloy wire;
(2) smelting; melting the raw materials of each component in several times, and transferring the raw materials into a heat preservation furnace filled with protective gas;
(3) continuous casting: when the temperature of the heat preservation furnace reaches the casting temperature, continuously casting by adopting a crystallizer with a chromium-added silicon nitride lining to obtain a casting blank, simultaneously adding a copper-zirconium alloy core wire into the heat preservation furnace by a wire feeding method according to the burning loss rule of zirconium, wherein the copper-zirconium alloy core wire is arranged on the outer layer and is a copper skin and the inner layer is a zirconium core; the specification of the casting bar blank is phi 12-50 mm, the casting speed is controlled to be 0.6-2.0 m/min, and the surface temperature of the casting blank out of the crystallizer is controlled to be 750-850 ℃; secondary strong cooling water is sprayed on the surface of the casting blank at the outlet of the crystallizer, the temperature of the cooling water is 15-30 ℃, and the water pressure is 0.2-0.5 MPa, so that online solid solution is realized; the zirconium content of the copper-zirconium alloy core wire is 20-30 wt%, and the copper-zirconium alloy core wire is continuously added by adopting an automatic wire feeding machine according to the burn-out rule of 0.005-0.02 wt% of zirconium in 1 minute, so that the zirconium content is controlled within the range of 0.05-0.15 wt%;
(4) performing plastic processing on the casting blank, and performing or not performing surface defect removal treatment according to the requirement to obtain a wire rod;
(5) and carrying out multistage step aging treatment on the wire rod.
2. The method for producing a copper-chromium-zirconium alloy wire rod according to claim 1, characterized in that: the raw materials comprise metal Cu, metal Cr and a copper-yttrium intermediate alloy with yttrium content of 15-20%, and the step (2) of fractional melting comprises the following steps: adding Cu into the solution to be melted, adding a covering agent to cover the solution, and adding a deoxidizing agent to perform deoxidation treatment; and (3) raising the temperature to 1250-1350 ℃, starting adding Cr, preserving the temperature for 15-45 minutes, adding the copper-yttrium intermediate alloy, and controlling the temperature to 1200-1400 ℃.
3. The method for producing a copper-chromium-zirconium alloy wire rod according to claim 2, characterized in that: the copper-chromium-zirconium alloy wire comprises the following components in percentage by mass: 0.7 to 1 percent of Cr0; zr0.05-0.15%; y0.02-0.1%; the balance being copper; the deoxidizer is 0.05-0.1% of Mg.
4. The method for producing a copper-chromium-zirconium alloy wire rod according to claim 2, characterized in that: the covering agent comprises 30-40% of cryolite, 30-40% of sodium carbonate and 30-40% of calcium fluoride by mass.
5. The method for producing a copper-chromium-zirconium alloy wire rod according to claim 1, characterized in that: the content of chromium element in the lining is 0-0.5%, excluding 0.
6. The method for producing a copper-chromium-zirconium alloy wire rod according to claim 1, characterized in that: the multistage aging comprises the following steps: the aging temperature is increased to 500-550 ℃, the temperature is kept for 0.5-1 h, then the temperature is reduced to 400-450 ℃, and the temperature is kept for 2-3 h.
7. The method for producing a copper-chromium-zirconium alloy wire rod according to claim 1, characterized in that: and (4) performing cold rolling, drawing and peeling to remove surface defects.
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CN103290252A (en) * | 2012-05-17 | 2013-09-11 | 常熟明辉焊接器材有限公司 | High-strength and high-conductivity chromium zirconium copper alloy and processing technology thereof |
CN108179305A (en) * | 2017-12-25 | 2018-06-19 | 浙江力博实业股份有限公司 | A kind of continuously extruded method for preparing Cu-Cr-Zr alloy bar |
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