CN114672689B - Rare earth copper alloy material with electromagnetic shielding function and preparation method thereof - Google Patents
Rare earth copper alloy material with electromagnetic shielding function and preparation method thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21D—MODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
- C21D8/00—Modifying the physical properties by deformation combined with, or followed by, heat treatment
- C21D8/02—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips
- C21D8/0247—Modifying the physical properties by deformation combined with, or followed by, heat treatment during manufacturing of plates or strips characterised by the heat treatment
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- 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
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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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
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
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- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
Abstract
The invention discloses a rare earth copper alloy material with an electromagnetic shielding function and a preparation method thereof, wherein the rare earth copper alloy material comprises the following components in percentage by mass: 5.0 to 15.0 weight percent of Fe, 0.4 to 1.2 weight percent of Si, 0.2 to 0.4 weight percent of X, 0.2 to 0.5 weight percent of Cr, 0.05 to 0.15 weight percent of Zr and the balance of Cu, wherein the sum of the components is 100 percent. According to the invention, si element with a specific proportion is added into the copper-iron alloy, so that an FeSi phase can be formed with Fe, and the combined addition of the rare earth Sc, Y, sr, ce, yb and La is more beneficial to the precipitation of the Fe phase in the copper-iron alloy compared with the precipitation of single rare earth on the basis of further degassing and deoxidation of pure alloy melt, so that the electromagnetic shielding composite rare earth copper alloy has more excellent electromagnetic shielding performance. Meanwhile, aiming at the defect that the increase of the content of the rare earth elements can embrittle the grain boundary, the zirconium element and the chromium element are added, the zirconium element and the chromium element and the jointly added rare earth elements can form a specific rare earth precipitation phase and a chromium phase, and the formation of an iron phase can strengthen a copper alloy matrix together, so that the reduction of the processing performance of the alloy is avoided.
Description
Technical Field
The invention belongs to the technical field of copper alloy processing, and particularly relates to a rare earth copper alloy material with an electromagnetic shielding function and a preparation method thereof.
Background
With the progress of industrial technology in China, copper and copper alloy with multiple functionalities are widely applied to more than two hundred fields of electronic communication, aerospace, ocean engineering and the like. Due to the excellent electric conduction and heat conduction performance, particularly in the production process of products such as large-scale integrated circuit lead frames, electromagnetic shielding systems and the like, the copper alloy has no substitutable position. In the last 80 th century, researchers in the united states developed Cu-Fe-P alloys such as C19400, C19500, C19700, and C19210 for lead frames, which had excellent conductivity, high strength, and good soldering and processing properties. However, the copper-iron alloy with excellent electromagnetic shielding performance, electrical and thermal conductivity and good mechanical properties is still needed to be further developed. After the rare earth elements are added into copper and copper alloy, the effects of deoxidation, degassing, tissue refinement and impurity form and distribution change can be achieved, so that the cold-hot deformation performance and the welding performance of the copper alloy are improved, the strength, the hardness and the plasticity of the copper alloy are improved, and the thermal stability, the corrosion resistance and the wear resistance of the copper alloy can be enhanced. For example, patent nos. CN111549253A and CN111636010A disclose methods for promoting Fe phase precipitation by using 0.1-1.00% of Ce, la and Y to improve the conductivity of Cu — Fe alloy. The invention patent CN103451575A discloses that the hardness of copper-iron alloys is greatly increased using 0.62-0.83wt% Sc and 0.45-0.51wt% Re. However, the rare earth elements with too high content can embrittle the grain boundary, so that the processing performance of the alloy is greatly reduced, and meanwhile, the research on the related performance of the copper-iron alloy by jointly adding two or more rare earth elements is very rare. Therefore, in the design process of the copper-iron alloy, the optimization of the combined addition of the rare earth elements becomes a research idea for developing a novel copper-iron alloy with multiple excellent performances.
Disclosure of Invention
The invention aims to provide a rare earth copper alloy material with an electromagnetic shielding function and a preparation method thereof, wherein the precipitation of an iron phase is further promoted by combining Si element and rare earth element in the alloy, so that the copper-iron alloy has a better electromagnetic shielding function.
The rare earth copper alloy material with the electromagnetic shielding function comprises the following components in percentage by mass: 5.0 to 15.0 weight percent of Fe, 0.4 to 1.2 weight percent of Si, 0.2 to 0.4 weight percent of X, 0.2 to 0.5 weight percent of Cr, 0.05 to 0.15 weight percent of Zr and the balance of Cu, wherein the sum of the components is 100 percent; wherein: x represents a combination of rare earth metals.
And X is formed by combining Sc and one or more rare earth elements of Y, sr, ce, yb and La.
Preferably, in the combination of rare earth elements, the respective rare earth elements are combined in equal proportion.
The preparation method of the rare earth copper alloy material with the electromagnetic shielding function comprises the following steps:
1) Smelting: preparing required elements according to the designed alloy component proportion, heating electrolytic copper, iron, silicon and chromium to a molten state, turning off a heating power supply of an induction furnace, adding copper-zirconium alloy, adding a rare earth combined element X, stirring uniformly under the protection of inert gas, and then fully slagging off until the melt is clean and limpid to obtain a rare earth-copper alloy melt;
2) Casting: performing semi-continuous casting on the rare earth copper alloy melt in the step 1) at a set temperature to obtain a copper alloy ingot;
3) Homogenizing: carrying out homogenization annealing treatment on the copper alloy ingot in the step 2) in inert gas to obtain a homogenized ingot;
4) And (3) combined forming heat treatment: and 3) carrying out cold working deformation and aging combination treatment on the homogenized ingot in the step 3) to obtain the rare earth copper alloy material with the electromagnetic shielding function.
In the step 1), the combined element X of iron, silicon, chromium and rare earth is added in a monomer form, zirconium is added in a copper-zirconium alloy form, and the mass percentage of zirconium in the copper-zirconium alloy is 40-60%; after the heating power supply of the induction furnace is closed, the temperature of the furnace still needs to be controlled between 1450 and 1600 ℃.
In the step 2), the temperature of the semi-continuous casting is 1250-1350 ℃.
In the step 3), the homogenization annealing treatment temperature is 950-980 ℃ and the time is 24-48 h.
In the step 4), the cold working deformation and aging combined treatment specifically comprises the following steps:
firstly, carrying out primary cold working deformation treatment on a homogenized cast ingot according to the total deformation of more than or equal to 80%, carrying out pre-aging treatment under an inert atmosphere after the treatment is finished, then carrying out secondary cold working deformation treatment according to the total deformation of more than or equal to 75%, carrying out aging treatment under the inert atmosphere after the treatment is finished, then carrying out tertiary cold working deformation treatment according to the total deformation of more than or equal to 50%, carrying out tertiary aging treatment under the inert atmosphere after the treatment is finished, finally carrying out fourth cold working deformation treatment on the cast ingot according to the total deformation of more than or equal to 50%, and annealing treatment after the treatment is finished to obtain the rare earth copper alloy material with the electromagnetic shielding function.
Preferably, the pre-aging treatment temperature is 400-550 ℃, and the treatment time is 1-2 h; the aging treatment temperature is 350-500 ℃, and the treatment time is 1-2 h; the temperature of the third-stage aging treatment is 320-380 ℃, and the treatment time is 16-32 h; the annealing temperature is 200-300 ℃, and the annealing time is 4-5 h.
The invention has the beneficial effects that:
1) According to the invention, si element with a specific proportion is added into the copper-iron alloy, so that FeSi phase can be formed with Fe, and the combined addition of the rare earth Sc, Y, sr, ce, yb and La is more beneficial to the precipitation of Fe phase in the copper-iron alloy compared with the precipitation of single rare earth on the basis of further degassing and deoxidation of pure alloy melt, so that the electromagnetic shielding composite rare earth copper alloy has more excellent electromagnetic shielding performance. Meanwhile, aiming at the defect that the increase of the content of the rare earth elements can embrittle the grain boundary, the zirconium element and the chromium element are added, the zirconium element and the chromium element and the jointly added rare earth elements can form a specific rare earth precipitated phase and a chromium phase together, and the formation of an iron phase can strengthen a copper alloy matrix together to avoid the reduction of the processing performance of the alloy.
2) The preparation process of the invention uses a combined process of large deformation and aging heat treatment, so that the ferrosilicon phase and the chromium phase formed by a specific proportion accumulate deformation energy through large deformation and are separated out through aging treatment. The process further improves the mechanical property of the alloy on the basis of improving the electrical conductivity of the alloy.
3) The electromagnetic shielding composite rare earth copper alloy prepared by the method has good electromagnetic shielding performance, high strength and high electric conductivity, the tensile strength of the alloy prepared by the method is more than 800MPa, the electric conductivity is more than 50% IACS, and the electromagnetic shielding effectiveness is more than 90dB.
Drawings
FIG. 1 as-cast microstructure map prepared in example 1.
Detailed Description
Example 1
Electrolytic copper, pure iron, pure silicon, pure chromium, pure yttrium, pure scandium and Cu-50Zr intermediate alloy are used as raw materials, and the weight ratio of Fe:5.0wt%, si:0.5wt%, Y:0.2wt%, sc:0.2wt%, cr:0.3wt%, zr:0.05wt% and the balance of Cu.
Firstly, heating and melting copper, iron, silicon and chromium in a graphite crucible by using an induction furnace, closing a heating power supply of the induction furnace, then adding a Cu-50Zr intermediate alloy, then adding rare earth elements of yttrium and scandium, then controlling the furnace temperature at 1450-1500 ℃ under the protection of nitrogen, fully stirring, and then slagging off again to obtain a pure melt.
And (3) cooling the pure melt to 1250 ℃, performing semi-continuous casting to obtain a copper alloy ingot, wherein the structure photograph of the obtained ingot is shown in figure 1, the as-cast alloy has uniform structure, a small amount of primary iron phase dendritic crystals exist, and the growth of crystal grains can be inhibited by the intermetallic compounds enriched at the grain boundary.
And carrying out homogenization annealing treatment on the copper alloy ingot for 24 hours at the temperature of 950 ℃ in a protective atmosphere to obtain a homogenized ingot.
Carrying out primary cold-working deformation treatment on the homogenized cast ingot according to 80% deformation; after the treatment is finished, pre-aging for 1h under the condition of protective atmosphere and 500 ℃, and after the treatment is finished, performing secondary cold deformation processing according to the deformation amount of 80%; after the treatment is finished, carrying out secondary aging treatment for 2h under the protective atmosphere and the temperature of 400 ℃; after the treatment is finished, performing third cold deformation processing according to 50% deformation, and after the treatment is finished, performing third-stage aging treatment for 32 hours at 350 ℃ in a protective atmosphere; and after the treatment is finished, performing cold working deformation treatment according to the deformation of 50%, and after the treatment is finished, performing annealing treatment at 200 ℃ for 4h to obtain the rare earth copper alloy plate with the electromagnetic shielding function.
The alloy prepared in this example had a tensile strength of 853MPa, an elongation of 2.9%, an electrical conductivity of 53.2% IACS, an electromagnetic shielding effectiveness of 93dB (test frequency range 10KHz-18 GHz), and a thermal conductivity of 212W/m.K.
Comparative example 1
Compared with the embodiment 1, si is not added in the elements; according to the weight ratio of Fe:5.0wt%, Y:0.2wt%, sc:0.2wt%, cr:0.3wt%, zr:0.05wt% and the balance of Cu.
The alloy prepared in this comparative example had a tensile strength of 762MPa, an elongation of 1.9%, an electric conductivity of 45% IACS, an electromagnetic shielding effectiveness of 84dB (test frequency range 10KHz-18 GHz), and a thermal conductivity of 178W/m.K.
Compared with example 1, the mechanical property, the electric conductivity and the electromagnetic shielding effectiveness are all reduced.
Comparative example 2
In comparison with example 1, no Cr and Zr were added to the elements, according to Fe:5.0wt%, si:0.5wt%, Y:0.2wt%, sc:0.2wt% and the balance of Cu.
The alloy prepared in this comparative example had a tensile strength of 531MPa, an elongation of 2.1%, an electric conductivity of 51% by volume of IACS, and an electromagnetic shielding effectiveness of 91dB (test frequency range 10KHz-18 GHz); the thermal conductivity was 203W/m.K.
The mechanical properties are significantly reduced compared to example 1.
Example 2
Electrolytic copper, pure iron, pure silicon, pure chromium, pure yttrium, pure scandium and Cu-50Zr intermediate alloy are used as raw materials, and the weight ratio of Fe:10.0wt%, si:0.7wt%, Y:0.1wt%, sc:0.1wt%, sr 0.1wt%, cr:0.4wt%, zr:0.1wt% and the balance of Cu.
Firstly, heating and melting copper, iron, silicon and chromium in a graphite crucible by using an induction furnace, turning off a heating power supply of the induction furnace, then adding a Cu-60Zr intermediate alloy, then adding rare earth elements of yttrium and scandium, then controlling the furnace temperature at 1500-1550 ℃ under the protection of nitrogen, fully stirring, and slagging off again to obtain a pure melt.
And cooling the pure melt to 1300 ℃ for semi-continuous casting to obtain the copper alloy ingot.
And carrying out homogenization annealing treatment on the copper alloy ingot for 36h at the temperature of 980 ℃ in the protective atmosphere to obtain a homogenized ingot.
Carrying out primary cold machining deformation treatment on the homogenized cast ingot according to 85% deformation; after the treatment is finished, pre-aging for 1.5h under the condition of protective atmosphere and 550 ℃, and after the treatment is finished, performing secondary cold deformation processing according to the deformation amount of 80%; after the treatment is finished, carrying out aging treatment for 2h under the protective atmosphere and at the temperature of 400 ℃; after the treatment is finished, performing third cold deformation processing according to 65% deformation, and after the treatment is finished, performing three-stage aging treatment for 28 hours at the temperature of 370 ℃ in a protective atmosphere; and after the treatment is finished, performing cold working deformation treatment according to the deformation of 50%, and after the treatment is finished, performing annealing treatment at 250 ℃ for 4.5h to obtain the rare earth copper alloy plate with the electromagnetic shielding function.
The alloy prepared in this example had a tensile strength of 822MPa, an elongation of 3.1%, an electrical conductivity of 51.7% IACS, an electromagnetic shielding effectiveness of 98dB (test frequency range 10KHz-18 GHz), and a thermal conductivity of 206W/m.K.
Example 3
Electrolytic copper, pure iron, pure silicon, pure chromium, pure yttrium, pure scandium and Cu-50Zr intermediate alloy are used as raw materials, and the weight ratio of Fe:15.0wt%, si:1.0wt%, sc:0.15wt%, sr 0.15wt%, cr:0.2wt%, zr:0.15wt% and the balance of Cu.
Firstly, heating and melting copper, iron, silicon and chromium in a graphite crucible by using an induction furnace, turning off a heating power supply of the induction furnace, then adding a Cu-60Zr intermediate alloy, then adding rare earth elements of yttrium and scandium, then controlling the furnace temperature at 1550-1600 ℃ under the protection of nitrogen, fully stirring, and then slagging off again to obtain a pure melt.
And cooling the pure melt to 1350 ℃ for semi-continuous casting to obtain the copper alloy ingot.
And carrying out homogenization annealing treatment on the copper alloy ingot for 48 hours at the temperature of 950 ℃ in a protective atmosphere to obtain a homogenized ingot.
Carrying out primary cold-working deformation treatment on the homogenized cast ingot according to 80% deformation; after the treatment is finished, pre-aging for 1.5h under the condition of protective atmosphere and 500 ℃, and after the treatment is finished, performing secondary cold deformation processing according to the deformation amount of 75%; after the treatment is finished, carrying out aging treatment for 2h under the protective atmosphere and the temperature of 450 ℃; after the treatment is finished, performing third cold deformation processing according to 60% deformation, and after the treatment is finished, performing three-stage aging treatment for 28 hours at the temperature of 380 ℃ in a protective atmosphere; and after the treatment, performing cold working deformation treatment according to the deformation of 50%, and after the treatment is finished, performing annealing treatment at 200 ℃ for 4.5 hours to obtain the rare earth copper alloy plate with the electromagnetic shielding function.
The alloy prepared in this example had tensile strength of 818MPa, elongation of 2.9%, electrical conductivity of 52.6% IACS, electromagnetic shielding effectiveness of 94dB (test frequency range 10KHz-18 GHz), and thermal conductivity of 205W/m.K.
Claims (6)
1. The rare earth copper alloy material with the electromagnetic shielding function is characterized by comprising the following components in percentage by mass: 5.0 to 15.0wt% of Fe, 0.4 to 1.2wt% of Si, 0.2 to 0.4wt% of X, 0.2 to 0.5wt% of Cr, 0.05 to 0.15wt% of Zr and the balance of Cu, wherein the sum of the components is 100%; wherein X represents a rare earth metal combination;
the preparation method of the rare earth copper alloy material with the electromagnetic shielding function comprises the following steps:
1) Smelting: preparing required elements according to the designed alloy component proportion, heating electrolytic copper, iron, silicon and chromium to a molten state, turning off a heating power supply of an induction furnace, adding copper-zirconium alloy, adding a rare earth combined element X, stirring uniformly under the protection of inert gas, and then fully slagging off until the melt is clean and limpid to obtain a rare earth-copper alloy melt;
2) Casting: performing semi-continuous casting on the rare earth copper alloy melt in the step 1) at a set temperature to obtain a copper alloy ingot;
3) Homogenizing: carrying out homogenization annealing treatment on the copper alloy ingot in the step 2) in inert gas to obtain a homogenized ingot;
4) Performing combined forming heat treatment: carrying out cold working deformation and aging combination treatment on the cast ingot homogenized in the step 3) to obtain a rare earth copper alloy material with an electromagnetic shielding function;
in the step 4), the cold working deformation and aging combined treatment comprises the following specific steps:
firstly, carrying out primary cold-processing deformation treatment on a homogenized cast ingot according to the total deformation of more than or equal to 80%, carrying out pre-aging treatment in an inert atmosphere after the treatment is finished, then carrying out secondary cold-processing deformation treatment according to the total deformation of more than or equal to 75%, carrying out aging treatment in the inert atmosphere after the treatment is finished, then carrying out tertiary cold-processing deformation treatment according to the total deformation of more than or equal to 60%, carrying out tertiary aging treatment in the inert atmosphere after the treatment is finished, finally carrying out fourth cold-processing deformation treatment on the cast ingot according to the total deformation of more than or equal to 50%, and carrying out annealing treatment after the treatment is finished to obtain the rare earth copper alloy material with the electromagnetic shielding function;
the pre-aging treatment temperature is 400-550 ℃, and the treatment time is 1-2h; the aging treatment temperature is 350 to 500 ℃, and the treatment time is 1 to 2h; the temperature of the third-stage aging treatment is 320-380 ℃, and the treatment time is 16-32h; the annealing temperature is 200 to 300 ℃, and the annealing time is 4 to 5 hours.
2. The rare earth copper alloy material with the electromagnetic shielding function as claimed in claim 1, wherein X is a combination of Sc and one or more rare earth elements selected from Y, ce, yb and La.
3. The rare earth copper alloy material with electromagnetic shielding function as claimed in claim 2, wherein the rare earth elements are combined in such a manner that the rare earth elements are combined in equal proportion.
4. The rare earth copper alloy material with the electromagnetic shielding function as claimed in claim 1, wherein in the step 1), the combined element X of iron, silicon, chromium and rare earth is added in a monomer form, zirconium is added in a copper-zirconium alloy form, and the mass percentage of zirconium in the copper-zirconium alloy is 40 to 60 percent; after the heating power supply of the induction furnace is closed, the furnace temperature still needs to be controlled at 1450-1600 ℃.
5. The rare earth copper alloy material with the electromagnetic shielding function as claimed in claim 1, wherein the temperature of the semi-continuous casting in step 2) is 1250 to 1350 ℃.
6. The rare earth copper alloy material with the electromagnetic shielding function as claimed in claim 1, wherein in the step 3), the homogenizing annealing temperature is 950 to 980 ℃ and the time is 24 to 48h.
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| JP5975604B2 (en) * | 2011-03-29 | 2016-08-23 | 株式会社神戸製鋼所 | Method for producing copper alloy for electromagnetic shielding material |
| CN108456799B (en) * | 2018-04-17 | 2019-10-11 | 沈阳赛美特新材料科技有限公司 | A kind of high-performance copper ferroalloy materials and its electroslag remelting preparation method |
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