CN111411256B - Copper-zirconium alloy for electronic components and preparation method thereof - Google Patents
Copper-zirconium alloy for electronic components and preparation method thereof Download PDFInfo
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
- C22C1/03—Making non-ferrous alloys by melting using master alloys
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
Abstract
The invention discloses a copper-zirconium alloy for electronic components and a preparation method thereof, wherein the alloy comprises the following components: 0.05 to 0.4 weight percent of Zr, 0.05 to 0.2 weight percent of Mg, 0.03 to 0.15 weight percent of Si, 0.01 to 0.06 weight percent of rare earth, and the balance of Cu and inevitable impurity elements. The invention also discloses a preparation method of the alloy, which comprises the steps of melting, alloying, casting, hot rolling, rough rolling, aging, finish rolling, stress relief annealing and finished product treatment. The copper-zirconium alloy has the advantages of high strength, high conductivity and excellent bending processability under the influence of the comprehensive action of Mg, Si and rare earth elements, the preparation method is easy for engineering production, the cost is low, the tensile strength of a finished strip is not less than 560MPa, the conductivity is not less than 80% IACS, and the product can be used for a very large-scale integrated circuit, a large-current electronic element and a heat dissipation part.
Description
Technical Field
The invention relates to the technical field of nonferrous metal processing, in particular to a copper-zirconium alloy for electronic components and a preparation method thereof.
Background
The copper-zirconium alloy has the electrical conductivity of 90-95% IACS and high heat resistance, and is often used as a copper alloy for electronic components such as high-power lead frames, electronic connectors and the like. With the rapid development of high-tech fields such as microelectronics, communication, transportation, aerospace, aviation and the like, electronic components are also developed in the directions of high integration, miniaturization and thin wall thinning, the transmission quantity and the heat productivity of the electronic components are increased, which puts higher requirements on copper alloy materials, and besides high electric conduction, heat conduction and heat resistance, alloy materials with the strength of more than 550MPa and the electric conductivity of more than 80% IACS are also needed urgently. Copper-zirconium alloy has low strength, and tensile strength of about 450MPa, although it has high electrical, thermal, and heat resistance properties, which limits its application in increasingly miniaturized electronic components.
In the copper-zirconium alloy, copper and zirconium are easy to precipitate mesophase particles at grain boundaries or defect positions in crystals, and the copper-zirconium alloy has large size, loose distribution and little contribution to the alloy strength, so the strength is low. In order to improve the strength of the copper-zirconium alloy, other strengthening methods need to be introduced. The addition of solid solution strengthening elements or the creation of new particle strengthening phases by adding elements is the main approach currently used. The trace Ti element is selected for patent CN104718302B, the Co and B element is selected for patent CN103380221B, and the Si element modified alloy is selected for patent CN105452502B, but the patents mainly improve the stress relaxation, bending formability, shearing formability and yield strength of the alloy, the strength of the alloy is improved to a small extent, and the tensile strength is generally less than 550 MPa. CN105088010B patent selects Ni, Si, Ag and rare earth elements, Ni and Si can form Ni2The Si non-oxide reinforcing phase improves the strength of the alloy, the silver improves the conductivity and the elongation of the alloy, the rare earth element changes the manufacturability of the alloy, and the effects of refining, degassing and microalloying are achieved, the tensile strength and the conductivity respectively reach 660MPa and 80 percent IACS, and the strength of the alloy is greatly improved. However, the cost for adding the Ag element in the patent is too high, and the Ag element is prepared by adopting a vacuum melting mode, so that the industrial cost is higher, and the popularization is not facilitated. The market urgently needs to develop an alloy material which has low cost, is easy to engineer and produce, has the strength of more than 550MPa and the electric conductivity of more than 80 percent IACS.
Disclosure of Invention
In view of the above-mentioned disadvantages of the prior art, the present invention provides a copper-zirconium alloy which has high strength, high conductivity and excellent bending workability at the same time, and a method for producing the same, and the product thereof can be used for very large scale integrated circuits, large current electronic components and heat dissipation parts.
The invention is realized by the following technical scheme.
A copper-zirconium alloy for electronic components, characterized by comprising: 0.05 to 0.4 weight percent of Zr, 0.05 to 0.2 weight percent of Mg, 0.03 to 0.15 weight percent of Si, 0.01 to 0.06 weight percent of rare earth, and the balance of Cu and inevitable impurity elements; wherein the total content of the inevitable impurity elements is less than 0.1 wt%, the mass percentage of the Zr, Mg and Si elements meets the requirement that (Zr + Mg)/Si is more than 2, and excessive Si elements are prevented from being dissolved in a matrix in a solid solution mode.
Further, the inevitable impurity elements include Fe, P, Ti, Cr, Zn, Al, Ni.
Further, the copper-zirconium alloy for electronic components of the present invention preferably includes, by mass: 0.1 to 0.2 weight percent of Zr, 0.1 to 0.2 weight percent of Mg, 0.03 to 0.1 weight percent of Si, 0.03 to 0.06 weight percent of rare earth, and the balance of Cu and inevitable impurities.
Further, the rare earth element is one of La, Ce and Y.
Furthermore, the tensile strength of a copper-zirconium product prepared from the copper-zirconium alloy is not less than 560MPa, the elongation is more than 3%, and the conductivity is not less than 80% IACS.
The preparation method of the copper-zirconium alloy for the electronic component is characterized by comprising the following steps:
(1) melting: loading copper into an induction melting furnace, adding a covering agent, melting in a protective atmosphere, and degassing to obtain a copper melt;
(2) alloying: sequentially adding the intermediate alloy into the copper melt to obtain a copper alloy melt;
(3) casting: casting the copper alloy melt obtained in the step (2) to obtain a casting blank, wherein the casting temperature is 1180-1250 ℃;
(4) hot rolling: heating, hot rolling and online quenching are carried out on the casting blank obtained in the step (3), the hot rolling heating temperature is 880-960 ℃, the heat preservation is carried out for 4 hours, and the final rolling temperature is not lower than 700 ℃;
(5) rough rolling: performing cold rolling deformation on the copper alloy hot rolled blank obtained in the step (4), wherein the deformation amount is 70-95%;
(6) aging: carrying out aging treatment on the copper alloy cold-rolled copper strip obtained in the step (5), wherein the aging temperature is 380-450 ℃, and the heat preservation time is 2-6 h;
(7) finish rolling: cold rolling deformation with 50% -80% of deformation amount is carried out on the aging strip obtained in the step (6);
(8) and (3) finished product treatment: and (5) performing stress relief annealing, straightening and slitting treatment on the strip obtained in the step (7).
Further, the method adopts non-vacuum fusion casting to prepare the alloy ingot.
Further, in the step (2), the adding sequence of the master alloy is Cu-Mg, Cu-Si, Cu-rare earth and Cu-Zr.
Compared with the prior art, the invention has the remarkable technical effects that:
(1) in the alloy of the invention, Zr is formed by adding Mg and Si elements on the basis of the prior copper-zirconium alloyxSiyAnd a precipitate phase rich in Mg and Si for assisting CuaZrbThe phases further increase the strength of the alloy.
(2) In the alloy, a certain amount of Mg element is added, so that solid solution strengthening is realized, and simultaneously, because Mg is easier to combine with oxygen, the oxygen content in the melt is reduced, the melt continuously keeps low oxygen content, the oxidation loss of Zr is reduced, and the yield of the Zr element is improved;
(3) according to the invention, the rare earth elements can play roles in purifying a melt, refining ingot casting tissues and further strengthening alloy, the comprehensive performance of a finished product is improved, and the rare earth elements are easy to combine with O elements and are also beneficial to reducing the oxidation loss of Zr elements;
(4) the copper-zirconium alloy has the advantages of high strength, high conductivity and excellent bending processability under the influence of the comprehensive action of Mg, Si and rare earth elements, the preparation method is easy for engineering production, the cost is low, the tensile strength of the finished strip is more than 560MPa, and the conductivity of the finished strip is more than 80% IACS.
Detailed Description
The present invention will be described in detail with reference to the following embodiments.
Example 1:
(1) melting: loading copper into an induction smelting furnace, adding charcoal and crystalline flake graphite, melting under the protection of argon, and degassing to obtain a copper melt;
(2) alloying: sequentially adding the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of La and Cu-15 wt% of Zr into a furnace, and preserving heat until the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of La and Cu-15 wt% of Zr are completely melted to obtain a copper alloy melt;
(3) casting: casting the copper alloy melt obtained in the step (2) at 1180 ℃ to obtain a casting blank with the specification of 200 x 600mm, wherein the casting blank comprises 0.05 wt% of Zr, 0.17 wt% of Mg, 0.06 wt% of Si, 0.06 wt% of La, and the balance of Cu and inevitable impurities;
(4) hot rolling: carrying out heating hot rolling and on-line quenching on the copper alloy casting blank obtained in the step (3), wherein the hot rolling heating temperature is 880 ℃, the heat preservation time is 4 hours, the final rolling temperature is 700 ℃, and the thickness of the hot rolled blank is 16 mm;
(5) rough rolling: performing cold rolling deformation on the copper alloy hot rolled blank obtained in the step (4), wherein the deformation amount is 75%;
(6) aging: carrying out aging treatment on the copper alloy cold-rolled copper strip obtained in the step (5) at the temperature of 420 ℃ for 4 h;
(7) finish rolling: cold rolling deformation of the aged strip with 80% of deformation;
(8) stress relief and finished product treatment: and (3) preserving heat at 550 ℃ for 30s for stress relief annealing and straightening and slitting treatment.
The obtained product has the properties of tensile strength of 571MPa, elongation of 4.5%, electric conductivity of 85.2% IACS and Vickers hardness of 172.
Example 2:
(1) melting: loading copper into an induction smelting furnace, adding charcoal and crystalline flake graphite, melting in a nitrogen protective atmosphere, and degassing to obtain a copper melt;
(2) alloying: sequentially adding the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of Ce and Cu-15 wt% of Zr into a furnace, and preserving heat until the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of Ce and Cu-15 wt% of Zr are completely melted to obtain a copper alloy melt;
(3) casting: casting the copper alloy melt obtained in the step (2) at 1200 ℃ to obtain a casting blank with the specification of 200 multiplied by 600mm, wherein the casting blank comprises 0.11 wt% of Zr, 0.1 wt% of Mg, 0.03 wt% of Si, 0.05 wt% of Ce, and the balance of Cu and inevitable impurities;
(4) hot rolling: carrying out heating hot rolling and on-line quenching on the copper alloy casting blank obtained in the step (3), wherein the hot rolling heating temperature is 900 ℃, the heat preservation time is 4 hours, the final rolling temperature is 720 ℃, and the thickness of the hot rolled blank is 16 mm;
(5) rough rolling: performing cold rolling deformation on the copper alloy hot rolled blank obtained in the step (4), wherein the deformation is 80%;
(6) aging: carrying out aging treatment on the copper alloy cold-rolled copper strip obtained in the step (5) at 380 ℃ for 6 h;
(7) finish rolling: cold rolling the aged strip with 75% of deformation;
(8) stress relief and finished product treatment: and (3) preserving heat at 550 ℃ for 30s for stress relief annealing and straightening and slitting treatment.
The obtained product has the properties of 565MPa of tensile strength, 5 percent of elongation, 87.1 percent of electrical conductivity IACS and 168 Vickers hardness.
Example 3:
(1) melting: loading copper into an induction smelting furnace, adding charcoal and crystalline flake graphite, melting under the protection of argon, and degassing to obtain a copper melt;
(2) alloying: sequentially adding the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si and Cu-10 wt% of Y, Cu-15 wt% of Zr into a furnace, and preserving heat until the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si and Cu-10 wt% of Y, Cu-15 wt% of Zr are completely melted to obtain a copper alloy melt;
(3) casting: casting the copper alloy melt obtained in the step (2) at 1250 ℃ to obtain a casting blank with the specification of 200 multiplied by 600mm, wherein the casting blank comprises 0.2 wt% of Zr, 0.2 wt% of Mg, 0.08 wt% of Si, 0.05 wt% of Y, and the balance of Cu and inevitable impurities;
(4) hot rolling: carrying out heating hot rolling and on-line quenching on the copper alloy casting blank obtained in the step (3), wherein the hot rolling heating temperature is 920 ℃, the heat preservation time is 4 hours, the final rolling temperature is 700 ℃, and the thickness of the hot rolled blank is 16 mm;
(5) rough rolling: performing cold rolling deformation on the copper alloy hot rolled blank obtained in the step (4), wherein the deformation amount is 85%;
(6) aging: carrying out aging treatment on the copper alloy cold-rolled copper strip obtained in the step (5) at 450 ℃ for 2 h;
(7) finish rolling: cold rolling the aged strip with 65% deformation;
(8) stress relief and finished product treatment: and (3) preserving heat at 550 ℃ for 30s for stress relief annealing and straightening and slitting treatment.
The obtained product has the properties of 596MPa of tensile strength, 4 percent of elongation, 84.5 percent of IACS of electric conductivity and 176 of Vickers hardness.
Example 4:
(1) melting: loading copper into an induction smelting furnace, adding charcoal and crystalline flake graphite, melting under the protection of argon, and degassing to obtain a copper melt;
(2) alloying: sequentially adding the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of La and Cu-15 wt% of Zr into a furnace, and preserving heat until the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of La and Cu-15 wt% of Zr are completely melted to obtain a copper alloy melt;
(3) casting: casting the copper alloy melt obtained in the step (2) at the casting temperature of 1230 ℃ to obtain a casting blank with the specification of 200 multiplied by 600mm, and the casting blank comprises 0.3 wt% of Zr, 0.05 wt% of Mg, 0.1 wt% of Si, 0.01 wt% of La, and the balance of Cu and inevitable impurities;
(4) hot rolling: carrying out heating hot rolling and on-line quenching on the copper alloy casting blank obtained in the step (3), wherein the hot rolling heating temperature is 940 ℃, the heat preservation time is 4 hours, the final rolling temperature is 700 ℃, and the thickness of the hot rolled blank is 16 mm;
(5) rough rolling: performing cold rolling deformation on the copper alloy hot rolled blank obtained in the step (4), wherein the deformation amount is 90%;
(6) aging: carrying out aging treatment on the copper alloy cold-rolled copper strip obtained in the step (5) at the temperature of 420 ℃ for 4 h;
(7) finish rolling: cold rolling deformation of 60% of deformation amount is carried out on the aged strip;
(8) stress relief and finished product treatment: and (3) preserving heat at 550 ℃ for 30s for stress relief annealing and straightening and slitting treatment.
The obtained product has the properties of tensile strength of 610MPa, elongation of 3.5 percent, electric conductivity of 82.7 percent IACS and Vickers hardness of 181.
Example 5:
(1) melting: loading copper into an induction smelting furnace, adding charcoal and crystalline flake graphite, melting in a nitrogen protective atmosphere, and degassing to obtain a copper melt;
(2) alloying: sequentially adding the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of Ce and Cu-15 wt% of Zr into a furnace, and preserving heat until the master alloy Cu-10 wt% of Mg, Cu-15 wt% of Si, Cu-10 wt% of Ce and Cu-15 wt% of Zr are completely melted to obtain a copper alloy melt;
(3) casting: casting the copper alloy melt obtained in the step (2) at 1250 ℃ to obtain a casting blank with the specification of 200 multiplied by 600mm, wherein the components of the casting blank are Zr 0.4 wt%, Mg 0.1 wt%, Si 0.15 wt%, Ce 0.03 wt%, and the balance of Cu and inevitable impurities;
(4) hot rolling: carrying out heating hot rolling and on-line quenching on the copper alloy casting blank obtained in the step (3), wherein the hot rolling heating temperature is 960 ℃, the heat preservation time is 4 hours, the final rolling temperature is 700 ℃, and the thickness of the hot rolled blank is 16 mm;
(5) rough rolling: performing cold rolling deformation on the copper alloy hot rolled blank obtained in the step (4), wherein the deformation amount is 95%;
(6) aging: carrying out aging treatment on the copper alloy cold-rolled copper strip obtained in the step (5) at the temperature of 420 ℃ for 4 h;
(7) finish rolling: cold rolling deformation of 50% of deformation amount is carried out on the aged strip;
(8) stress relief and finished product treatment: and (3) preserving heat at 550 ℃ for 30s for stress relief annealing and straightening and slitting treatment.
The obtained product has the properties of 627MPa of tensile strength, 3.1 percent of elongation, 80.6 percent of IACS of electric conductivity and 187 Vickers hardness.
TABLE 1 alloy composition Table for examples and comparative examples
TABLE 2 alloy Performance tables for examples and comparative examples
| Alloy (I) | Tensile strength (MPa) | Elongation (%) | Electrical conductivity (% IACS) | Hardness HV |
| Example 1 | 571 | 4.5 | 85.2 | 172 |
| Example 2 | 565 | 5 | 87.1 | 168 |
| Example 3 | 596 | 4 | 84.5 | 176 |
| Example 4 | 610 | 3.5 | 82.7 | 181 |
| Example 5 | 627 | 3.1 | 80.6 | 187 |
| Comparative example | 530 | 9.2 | 93.8 | 155 |
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 (3)
1. A preparation method of a copper-zirconium alloy for electronic components is characterized in that the copper-zirconium alloy comprises the following components: 0.05 to 0.4 weight percent of Zr, 0.05 to 0.2 weight percent of Mg, 0.03 to 0.15 weight percent of Si, 0.01 to 0.06 weight percent of rare earth, and the balance of Cu and inevitable impurity elements; wherein the total content of the inevitable impurity elements is less than 0.1 wt%, and the mass percentage of Zr, Mg and Si elements satisfies (Zr + Mg)/Si > 2; the preparation method specifically comprises the following steps:
(1) melting: loading copper into an induction melting furnace, adding a covering agent, melting under the protection of inert gas, and degassing to obtain a copper melt;
(2) alloying: sequentially adding the intermediate alloy into the copper melt to obtain a copper alloy melt;
(3) casting: casting the copper alloy melt obtained in the step (2) to obtain a casting blank, wherein the casting temperature is 1180-1250 ℃;
(4) hot rolling: heating, hot rolling and online quenching are carried out on the casting blank obtained in the step (3), the hot rolling heating temperature is 880-960 ℃, the heat preservation is carried out for 4 hours, and the final rolling temperature is not lower than 700 ℃;
(5) rough rolling: performing cold rolling deformation on the copper alloy hot rolled blank obtained in the step (4), wherein the deformation amount is 70-95%;
(6) aging: carrying out aging treatment on the copper alloy cold-rolled copper strip obtained in the step (5), wherein the aging temperature is 380-450 ℃, and the heat preservation time is 2-6 h;
(7) finish rolling: cold rolling deformation with 50% -80% of deformation amount is carried out on the aging strip obtained in the step (6);
(8) and (3) finished product treatment: and (5) performing stress relief annealing, straightening and slitting treatment on the strip obtained in the step (7).
2. The method of claim 1, wherein the method comprises non-vacuum casting to produce alloy ingots.
3. The method according to claim 1, wherein in the step (2), the master alloy is added in the order of Cu-Mg, Cu-Si, Cu-rare earth, Cu-Zr.
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| CN105452502A (en) * | 2013-08-12 | 2016-03-30 | 三菱综合材料株式会社 | Copper alloy for electronic/electrical devices, copper alloy thin plate for electronic/electrical devices, component for electronic/electrical devices, terminal and bus bar |
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| CN105452502A (en) * | 2013-08-12 | 2016-03-30 | 三菱综合材料株式会社 | Copper alloy for electronic/electrical devices, copper alloy thin plate for electronic/electrical devices, component for electronic/electrical devices, terminal and bus bar |
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| Title |
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| 高强高导Cu-Zr(-RE)合金时效和热变形行为研究;孙慧丽;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20170115;第B022-151页 * |
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