CN111549251A - Cu-Cr-Zr alloy suitable for non-vacuum preparation and preparation method thereof - Google Patents
Cu-Cr-Zr alloy suitable for non-vacuum preparation and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a Cu-Cr-Zr alloy suitable for non-vacuum preparation and a preparation method thereof, and the Cu-Cr-Zr alloy comprises the following components: 0.2 to 0.8 weight percent of Cr, 0.02 to 0.2 weight percent of Zr, 0.05 to 0.2 weight percent of Mg, 0.03 to 0.06 weight percent of B, 0.03 to 0.2 weight percent of Ti, and the balance of Cu. The preparation method comprises the following steps: melting, melt degassing, alloying and casting. The Cu-Cr-Zr product obtained by the invention is suitable for non-vacuum casting such as up-drawing continuous casting, horizontal continuous casting, vertical continuous casting and the like, and in the continuous casting or semi-continuous casting process, Zr and Mg elements are compensated by Cu-Mg-Zr intermediate alloy, so that the operability of non-vacuum preparation is improved. The product is prepared by the conventional process, the tensile strength can be realized to be not less than 560MPa, and the electric conductivity is not less than 75% IACS.
Description
Technical Field
The invention relates to the technical field of copper alloy processing, in particular to a Cu-Cr-Zr alloy suitable for non-vacuum preparation and a preparation method thereof.
Background
The Cu-Cr-Zr alloy has excellent comprehensive performance, can be used for lead frames of very large-scale circuits, electrical connectors, resistance welding electrodes, high-speed rail contact wires, crystallizer linings and the like, and has wide development prospect.
As Zr element is easy to burn out, the ideal preparation method of the Cu-Cr-Zr alloy is vacuum casting. Because the vacuum casting mode has large equipment investment, lower production efficiency and high alloy preparation cost, in order to improve the production efficiency and reduce the cost in the existing industrial production, a non-vacuum continuous casting mode is usually adopted to produce cast ingots, and the cast ingots are processed into required products. Under the non-vacuum condition, Zr loss control in the Cu-Cr-Zr alloy continuous casting process and continuous casting material supplementing process, semi-continuous casting melt transfer and Zr loss control of melt in a crystallizer, and how to ensure the stability of Zr in the full length range of an ingot and improve the yield of Zr element are the technical problems faced at the present stage.
In the non-vacuum preparation method, in order to reduce the burning loss of Zr, it is a conventional practice to protect the melt with a covering agent or an inert gas, such as patents CN101531149B, CN101613808B, CN101618445B, CN106735003B, CN107586975B, CN108526422A, etc. The method has a certain protection effect, but because the continuous casting process is longer in duration and oxygen is introduced into raw materials in the continuous casting material-supplementing process, the oxygen content in the melt can be continuously increased, so that the yield of Zr is generally lower than 50%. Researchers have also replaced Zr with other elements or reduced Zr content to reduce the difficulty of preparation. The patents CN107287468B and CN108526422A replace or reduce Zr content by adding common elements such as Mg, Si and the like with low price, and CN103966475B and CN108277378B respectively adopt Ti and Ag elements to replace Zr elements. However, the excellent comprehensive performance of the Cu-Cr-Zr alloy is difficult to completely achieve by the alternative alloys, and the Cu-Cr-Zr alloy is still advocated although the preparation difficulty is high.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a Cu-Cr-Zr alloy suitable for non-vacuum preparation and a preparation method thereof.
The invention is realized by the following technical scheme.
A Cu-Cr-Zr alloy suitable for non-vacuum preparation, which is characterized by comprising the following components: 0.2 to 0.8 weight percent of Cr, 0.02 to 0.2 weight percent of Zr, 0.05 to 0.2 weight percent of Mg, 0.03 to 0.06 weight percent of B, 0.03to 0.2 weight percent of Ti, and the balance of Cu.
Further, the Cu-Cr-Zr alloy suitable for non-vacuum preparation comprises the following preferred components in percentage by mass: 0.3 to 0.6 weight percent of Cr, 0.05 to 0.1 weight percent of Zr, 0.1 to 0.2 weight percent of Mg, 0.03to 0.05 weight percent of B0.03 to 0.1 weight percent of Ti, and the balance of Cu.
Further, Zr and Mg are added through a Cu-Mg-Zr intermediate alloy, and the content of the elements in the Cu-Mg-Zr intermediate alloy comprises the following components: 10 to 30 weight percent of Zr, 5 to 20 weight percent of Mg, and the balance of Cu. Cr is added through a Cu-Cr intermediate alloy, B is added through a Cu-B intermediate alloy, Ti is added through a Cu-Ti intermediate alloy, and Cu is cathode copper.
The Cu-Cr-Zr alloy suitable for non-vacuum preparation can be used for producing various products such as plates, strips, foils, rods, wires, profiles and the like.
The preparation method of the Cu-Cr-Zr alloy suitable for non-vacuum preparation comprises the following steps:
(1) melting: putting copper into an induction melting furnace, adding a covering agent, and melting in a protective atmosphere to obtain a copper melt;
(2) melt degassing: degassing the copper melt obtained in the step (1), wherein the degassing treatment mode is one or the combination of Cu-P degassing and inert gas degassing, the oxygen content in the copper melt is reduced to below 50ppm, and the treated melt is subjected to tight covering and inert gas protection;
(3) alloying: adding the intermediate alloy into the copper melt obtained in the step (2) to obtain a copper alloy melt;
(4) casting: and (4) casting the copper alloy melt obtained in the step (3) to obtain a casting blank. And in the casting process, detecting the content of the alloy elements in the melt at regular time, and compensating the alloy elements according to the requirement.
Further, in the step (4), during the casting process, the content of alloy elements in the melt is detected at regular time, Cu-Mg-Zr intermediate alloy is added at intervals of 30-120 minutes to compensate Zr and Mg elements, and other elements are compensated at irregular time according to needs.
Further, in the step (4), the copper alloy melt obtained in the step (3) is cast in a non-vacuum mode selected from the group consisting of upward continuous casting, horizontal continuous casting and vertical continuous casting.
The Cu-Cr-Zr product obtained by the invention is prepared into a product by a conventional process, and has the performance of not less than 560MPa of tensile strength and not less than 75% of IACS of electric conductivity.
The alloy of the invention adds a certain amount of Mg and B elements, and because the Mg and B elements are easier to combine with oxygen, the oxygen content in the melt is reduced, the melt is continuously kept at low oxygen content, and the burning loss of the Zr element is reduced. In the continuous casting or semi-continuous casting process, Zr and Mg elements are compensated by the Cu-Mg-Zr intermediate alloy, so that the operability of non-vacuum preparation is further improved. The prepared alloy can be used in the fields of very large scale circuit lead frames, electrical connectors, resistance welding electrodes, high-speed rail contact wires, crystallizer linings and the like.
The invention has the following beneficial technical effects:
(1) in the invention, a certain amount of Mg and B elements are added into the alloy, so that the Mg and B elements are more easily combined with oxygen, the oxygen content in the melt is reduced, the low oxygen content of the melt is continuously kept, the Zr loss in the continuous casting process and the continuous casting material supplementing process of the Cu-Cr-Zr alloy can be reduced, or the Zr loss of the semi-continuous casting melt transfer and the melt in the crystallizer can be reduced, the Zr stability in the full length range of the ingot casting can be improved, and the yield of the Zr element can be improved;
(2) in the invention, in the continuous casting or semi-continuous casting process, Zr and Mg are compensated by the Cu-Mg-Zr intermediate alloy, so that the simultaneous addition of Mg and Zr is realized, and the Mg is easy to combine with oxygen, thereby effectively reducing the oxidation loss of Zr, ensuring that the yield of Zr reaches 70 percent, and further improving the operability of non-vacuum preparation;
(3) in the invention, the elements B and Ti can further strengthen the alloy and refine the ingot casting structure, and the comprehensive performance of the finished product is improved;
(4) the Cu-Cr-Zr alloy disclosed by the invention is suitable for non-vacuum preparation in up-drawing continuous casting, horizontal continuous casting, vertical continuous casting and the like, and can be used for producing various products such as plates, strips, foils, rods, wires, section bars and the like.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1
(1) Melting: adding cathode copper into a three-furnace induction smelting furnace with a middle transition bin, adding charcoal and graphite flakes for covering, and melting under the protection of argon to obtain a copper melt;
(2) degassing: introducing argon into the copper melt in the step (1) for twenty minutes, measuring that the oxygen content in the melt is 45ppm, covering charcoal and crystalline flake graphite on the treated melt, and filling argon for protection;
(3) alloying: adding a Cu-15 wt% Cr intermediate alloy into the melt for melting, after the Cu-15 wt% Cr intermediate alloy is completely melted, sequentially adding Cu-20 wt% Mg-10 wt% Zr, Cu-5 wt% B and Cu-20 wt% Ti intermediate alloy, stirring, standing, and adjusting the alloy components to be 0.2 wt% Cr, 0.02 wt% Zr, 0.15 wt% Mg, 0.06 wt% B, 0.2 wt% Ti and the balance of Cu;
(4) upward continuous casting: and starting up continuous casting when the temperature of the melt reaches 1200 ℃. In the process of drawing casting, the components of the melt are detected at regular time, and the compensation of Cu-5 wt% Mg-30 wt% Zr is carried out once every 120 minutes. Obtaining 2.5 tons of phi 20mm casting blanks;
(5) processing to a bar line: and (4) carrying out solid solution treatment on the copper alloy bar blank obtained in the step (4) at 900 ℃ for 1h, continuously extruding to phi 28mm, carrying out cold drawing to phi 20mm, carrying out aging treatment at 420 ℃ for 4h, and carrying out cold drawing to phi 10 mm.
The alloy has a tensile strength of 560MPa and an electrical conductivity of 85% IACS.
Example 2
(1) Melting: adding cathode copper into a three-furnace induction smelting furnace with a middle transition bin, adding charcoal and graphite flakes for covering, and melting under the protection of argon to obtain a copper melt;
(2) degassing: introducing argon into the copper melt in the step (1) for twenty minutes, measuring that the oxygen content in the melt is 30ppm, covering charcoal and crystalline flake graphite on the treated melt, and filling argon for protection;
(3) alloying: adding a Cu-15 wt% Cr intermediate alloy into the melt for melting, after the Cu-15 wt% Cr intermediate alloy is completely melted, sequentially adding Cu-10 wt% Mg-30 wt% Zr, Cu-5 wt% B and Cu-30 wt% Ti intermediate alloy, stirring, standing, and adjusting the alloy components to be 0.3 wt% Cr, 0.15 wt% Zr, 0.08 wt% Mg, 0.05 wt% B, 0.1 wt% Ti and the balance of Cu;
(4) upward continuous casting: and starting up continuous casting when the temperature of the melt reaches 1250 ℃. In the process of drawing casting, the components of the melt are detected at regular time, and the compensation of Cu-5 wt% Mg-30 wt% Zr is carried out once every 60 minutes. Obtaining 2 tons of phi 25mm casting blanks;
(5) processing to a bar line: and (4) carrying out solid solution treatment on the copper alloy bar blank obtained in the step (4) at 900 ℃ for 1h, continuously extruding to phi 35mm, carrying out cold drawing to phi 20mm, carrying out aging treatment at 450 ℃ for 4h, and carrying out cold drawing to phi 14 mm.
The alloy had a tensile strength of 572MPa and an electrical conductivity of 84% IACS.
Example 3
(1) Melting: adding cathode copper into a three-furnace induction smelting furnace with a middle transition bin, adding charcoal and graphite flakes for covering, and melting under the protection of argon to obtain a copper melt;
(2) degassing: introducing argon into the copper melt in the step (1) for twenty minutes, measuring that the oxygen content in the melt is 35ppm, covering charcoal and crystalline flake graphite on the treated melt, and filling argon for protection;
(3) alloying: adding a Cu-15 wt% Cr intermediate alloy into the melt for melting, adding Cu-20 wt% Mg-20 wt% Zr, Cu-5 wt% B and Cu-30 wt% Ti intermediate alloy after the Cu-15 wt% Cr intermediate alloy is completely melted, stirring, standing, and adjusting the alloy components to be 0.45 wt% of Cr, 0.1 wt% of Zr, 0.2 wt% of Mg, 0.04 wt% of B, 0.05 wt% of Ti and the balance of Cu;
(4) horizontal continuous casting: when the temperature of the melt reaches 1225 ℃, horizontal continuous casting is started. In the process of drawing casting, the components of the melt are detected at regular time, and the compensation of Cu-5 wt% Mg-30 wt% Zr is carried out once every 60 minutes. Obtaining 1.6 tons of phi 150mm casting blanks;
(5) processing to a bar line: and (4) sawing the copper alloy bar blank obtained in the step (4) at-940 ℃ for 3h to extrude phi 28mm, cold drawing to phi 16mm, cold drawing at 450 ℃ for 4h to age, and cold drawing to phi 8 mm.
The tensile strength of the alloy is 590MPa, and the conductivity is 81% IACS.
Example 4
(1) Melting: adding copper into an induction smelting furnace, adding charcoal and graphite flakes to cover, and melting under the protection of argon to obtain a copper melt;
(2) degassing: introducing argon into the copper melt in the step (1) for twenty minutes, adding Cu-P, stirring, standing, measuring the oxygen content in the melt to be 23ppm, covering charcoal and crystalline flake graphite on the treated melt, and filling argon for protection;
(3) alloying: adding a Cu-15 wt% Cr intermediate alloy into the melt for melting, adding Cu-5 wt% Mg-10 wt% Zr, Cu-5 wt% B and Cu-30 wt% Ti intermediate alloy after the Cu-15 wt% Cr intermediate alloy is completely melted, stirring, standing, and adjusting the alloy components to be 0.6 wt% Cr, 0.05 wt% Zr, 0.05 wt% Mg, 0.03 wt% B, 0.09 wt% Ti and the balance of Cu;
(4) vertical continuous casting: and starting vertical continuous casting when the temperature of the melt reaches 1300 ℃, and performing compensation of Cu-5 wt% Mg-30 wt% Zr once every 90 minutes by detecting the components of the melt at regular time in the process of drawing casting. 3.8 tons of 150 multiplied by 330mm casting blanks are obtained;
(5) processing the strip: and (4) heating the copper alloy ingot obtained in the step (4) at 960 ℃ for 4h, hot rolling to 16mm, cold rolling to 2.7mm, ageing at 480 ℃ for 4h, and cold rolling to 0.5 mm.
The alloy has a tensile strength of 605MPa and an electrical conductivity of 79% IACS.
Example 5
(1) Melting: adding copper into a belt induction smelting furnace, adding charcoal and graphite flakes for covering, and melting under the protection of argon to obtain a copper melt;
(2) degassing: introducing argon into the copper melt in the step (1) for twenty minutes, adding Cu-P, stirring, standing, measuring the oxygen content in the melt to be 20ppm, covering charcoal and crystalline flake graphite on the treated melt, and filling argon for protection;
(3) alloying: adding a Cu-15 wt% Cr intermediate alloy into the melt for melting, adding Cu-5 wt% Mg-15 wt% Zr, Cu-5 wt% B and Cu-30 wt% Ti intermediate alloy after the Cu-15 wt% Cr intermediate alloy is completely melted, stirring, standing, and adjusting the alloy components to be 0.8 wt% of Cr, 0.2 wt% of Zr, 0.1 wt% of Mg, 0.06 wt% of B, 0.03 wt% of Ti and the balance of Cu;
(4) vertical continuous casting: and starting vertical continuous casting when the temperature of the melt reaches 1250 ℃, and performing compensation of Cu-5 wt% Mg-30 wt% Zr once every 30 minutes by detecting the components of the melt at regular time in the process of drawing casting. 2.7 tons of 150 multiplied by 330mm casting blanks are obtained;
(5) processing the strip: and (4) heating the copper alloy ingot obtained in the step (4) at 960 ℃ for 4h, hot rolling to 14mm, cold rolling to 2 mm-480 ℃ for 4h, aging, and cold rolling to 0.3 mm.
The tensile strength of the alloy is 613MPa, and the conductivity is 80% IACS.
The compositions of the alloys of the examples are shown in Table 1, and their properties are shown in Table 2:
table 1 example alloy compositions
TABLE 2 properties of the alloys of the examples
| Alloy (I) | Tensile strength/MPa | Conductivity/% IACS |
| Example 1 | 560 | 85 |
| Example 2 | 572 | 84 |
| Example 3 | 590 | 81 |
| Example 4 | 605 | 79 |
| Example 5 | 613 | 75 |
| Comparative example 1 | 565 | 80 |
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 (6)
1. A Cu-Cr-Zr alloy suitable for non-vacuum preparation, which is characterized by comprising the following components: 0.2 to 0.8 weight percent of Cr, 0.02 to 0.2 weight percent of Zr, 0.05 to 0.2 weight percent of Mg, 0.03 to 0.06 weight percent of B, 0.03to 0.2 weight percent of Ti, and the balance of Cu.
2. The alloy of claim 1, wherein the composition comprises, in mass percent: 0.3 to 0.6 weight percent of Cr, 0.05 to 0.1 weight percent of Zr, 0.1 to 0.2 weight percent of Mg, 0.03 to 0.05 weight percent of B, 0.03to 0.1 weight percent of Ti, and the balance of Cu.
3. The alloy of claim 1, wherein both Zr and Mg are added via a Cu-Mg-Zr master alloy, the element content of the Cu-Mg-Zr master alloy comprising: 10 to 30 weight percent of Zr, 5 to 20 weight percent of Mg, and the balance of Cu.
4. A method for preparing a Cu-Cr-Zr alloy suitable for non-vacuum preparation according to any of claims 1-3, characterized in that it comprises the following steps:
(1) melting: putting copper into an induction melting furnace, adding a covering agent, and melting in a protective atmosphere to obtain a copper melt;
(2) melt degassing: degassing the copper melt obtained in the step (1), wherein the degassing treatment mode is one or the combination of Cu-P degassing and inert gas degassing, the oxygen content in the copper melt is reduced to below 50ppm, and the treated melt is subjected to tight covering and inert gas protection;
(3) alloying: adding the intermediate alloy into the copper melt obtained in the step (2) to obtain a copper alloy melt;
(4) casting: and (4) casting the copper alloy melt obtained in the step (3) to obtain a casting blank.
5. The method according to claim 4, wherein in the step (4), the content of the alloy elements in the melt is detected periodically during the casting process, and the Cu-Mg-Zr intermediate alloy is added for compensating Zr and Mg elements at intervals of 30-120 minutes.
6. The method of claim 4, wherein in the step (4), the copper alloy melt obtained in the step (3) is cast by one of upward continuous casting, horizontal continuous casting and vertical continuous casting.
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Cited By (1)
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| CN113278829A (en) * | 2021-04-13 | 2021-08-20 | 太原晋西春雷铜业有限公司 | Semi-continuous preparation process of large-size C70250 copper alloy ingot |
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