CN114182134A - Cu-Cr-Zr alloy material, heat treatment process and application - Google Patents
Cu-Cr-Zr alloy material, heat treatment process and application Download PDFInfo
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Abstract
The invention discloses a Cu-Cr-Zr alloy material, a heat treatment process and application, wherein an alloy casting with the chemical composition of Cu-0.22Cr-0.24Zr is smelted and poured, and is subjected to solution treatment for 2 hours at 980 ℃, and then water quenching and cooling are carried out; carrying out primary aging treatment for 15-20h at 450 ℃, and then carrying out air cooling; carrying out secondary aging treatment for 5h at 480-630 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material. Compared with the prior art, the average diameter of the nanometer-order second phase which plays a strengthening role in the Cu-Cr-Zr alloy material treated by the heat treatment process is basically unchanged, but the number of precipitated phases after secondary aging is increased, the obvious distance between particles is reduced, and the secondary aging second phase is more sufficiently precipitated from the morphology and diffraction spots of the precipitated phases; the tensile strength and the conductivity of the Cu-Cr-Zr alloy material after heat treatment are both greatly improved, the tensile strength can reach 380MPa, the conductivity reaches 86.18 percent IACS, and the performance index requirements of the alloy for the lead frame are met.
Description
Technical Field
The invention relates to the technical field of alloy heat treatment, in particular to a Cu-Cr-Zr alloy material, a heat treatment process and application.
Background
The Cu-Cr-Zr alloy has high strength and good electric and heat conductivity, and is widely applied to the field of high strength and high conductivity. The conductivity and the strength of the copper alloy are a pair of contradictory performance indexes, the coordination of the relationship between the conductivity and the strength is a main problem to be solved for developing and developing the high-strength and high-conductivity copper alloy, and the basic idea at present is to adopt alloy elements with low solid solubility to carry out solid solution strengthening and solid solution aging treatment. The copper alloy has higher strength while ensuring higher conductivity of the copper alloy. The strengthening mode of the Cu-Cr-Zr alloy research is mainly deformation strengthening, or the combined action of the deformation strengthening, the aging precipitation strengthening and the like. Since the crystal defects generated by cold working have little influence on the electrical conductivity of the material, the strengthening method can improve the strength and simultaneously ensure that the alloy has high electrical conductivity, and is a main strengthening method. Through deformation strengthening and combination with other strengthening modes, the tensile strength of the Cu-Cr-Zr alloy can reach more than 600MPa, and the electric conductivity can reach more than 80% IACS. However, for some products for specific applications, such as near net shape products of cast articles, the manufacturing process does not allow for deformation, resulting in poor mechanical properties and electrical conductivity.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provide a Cu-Cr-Zr alloy material, a heat treatment process and application thereof, and the Cu-Cr-Zr alloy material can achieve both high strength and high conductivity only by a heat treatment process of solid solution and secondary aging under the condition of no deformation.
In order to achieve the purpose, the invention is implemented according to the following technical scheme:
the first purpose of the invention is to provide a heat treatment process of a Cu-Cr-Zr alloy material, which comprises the following steps:
firstly, carrying out solution treatment on an alloy casting which is smelted and poured and contains the chemical components of Cu-0.22Cr-0.24Zr at 980 ℃ for 2h, and then carrying out water quenching and cooling;
step two, carrying out primary aging treatment for 15-20h at 450 ℃, and then carrying out air cooling;
and step three, carrying out secondary aging treatment for 5h at 480 ℃ and 630 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material.
In a further preferred embodiment of the present invention, the time for the primary aging treatment is 15 hours.
In a more preferred embodiment of the present invention, the temperature of the secondary aging treatment is 480 ℃.
The second purpose of the invention is to provide the Cu-Cr-Zr alloy material prepared by the heat treatment process of the Cu-Cr-Zr alloy material, and the chemical composition of the Cu-Cr-Zr alloy material is Cu-0.22Cr-0.24 Zr.
The third purpose of the invention is to provide the application of the Cu-Cr-Zr alloy material, and the Cu-Cr-Zr alloy material is used for preparing the copper-based lead frame.
Compared with the prior art, the average diameter of the nanometer-order second phase which plays a strengthening role in the Cu-Cr-Zr alloy material treated by the heat treatment process is basically unchanged, but the number of precipitated phases after secondary aging is increased, the obvious distance between particles is reduced, and the secondary aging second phase is more sufficiently precipitated from the morphology and diffraction spots of the precipitated phases; the tensile strength and the conductivity of the Cu-Cr-Zr alloy material after heat treatment are both greatly improved, the tensile strength can reach 380MPa, the conductivity reaches 86.18 percent IACS, and the performance index requirements of the alloy for the lead frame are met.
Drawings
FIG. 1 shows the tensile strength and electrical conductivity of Cu-0.22Cr-0.24Zr alloy under different heat treatment conditions.
FIG. 2 is an SEM photograph of a Cu-0.22Cr-0.24Zr alloy under different heat treatment conditions for Cu-0.22Cr-0.24 Zr: (a) a, a sample rod; (b) b, a sample rod; (c) c, a sample rod; (d) d, a sample rod; (e) e, a sample rod; (f) f, a sample rod; (g) g, a sample rod; (h) h, a sample rod; (i) i, a sample rod; .
FIG. 3 is a TEM photograph and diffraction spots of the Cu-0.22Cr-0.24Zr alloy after secondary aging (a) TEM photograph; (b) diffraction spots.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. The specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
Example 1
Firstly, selecting electrolytic copper, a Cu-Cr intermediate alloy and high-purity zirconium as raw materials for a test material, and properly proportioning; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. Pouring the alloy liquid into a zirconium oxide filter screen on a pouring cup to filter out charcoal, pouring the alloy liquid into a cavity through the pouring cup to pour out an alloy casting with the chemical component of Cu-0.22Cr-0.24 Zr; carrying out solution treatment on an alloy casting which is smelted and poured and has the chemical composition of Cu-0.22Cr-0.24Zr (wt%) at 980 ℃ for 2h, and then carrying out water quenching and cooling;
step two, carrying out primary aging treatment for 15h at 450 ℃, and then carrying out air cooling;
and step three, carrying out secondary aging treatment for 5 hours at 480 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material D.
Example 2
Firstly, selecting electrolytic copper, a Cu-Cr intermediate alloy and high-purity zirconium as raw materials for a test material, and properly proportioning; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. Pouring the alloy liquid into a zirconium oxide filter screen on a pouring cup to filter out charcoal, pouring the alloy liquid into a cavity through the pouring cup to pour out an alloy casting with the chemical component of Cu-0.22Cr-0.24 Zr; carrying out solution treatment on an alloy casting which is smelted and poured and has the chemical composition of Cu-0.22Cr-0.24Zr (wt%) at 980 ℃ for 2h, and then carrying out water quenching and cooling;
step two, carrying out primary aging treatment for 15h at 450 ℃, and then carrying out air cooling;
and step three, carrying out secondary aging treatment for 5 hours at 510 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material E.
Example 3
Firstly, selecting electrolytic copper, a Cu-Cr intermediate alloy and high-purity zirconium as raw materials for a test material, and properly proportioning; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. Pouring the alloy liquid into a zirconium oxide filter screen on a pouring cup to filter out charcoal, pouring the alloy liquid into a cavity through the pouring cup to pour out an alloy casting with the chemical component of Cu-0.22Cr-0.24Zr (wt%); carrying out solution treatment on an alloy casting which is smelted and poured and has the chemical composition of Cu-0.22Cr-0.24Zr at 980 ℃ for 2h, and then carrying out water quenching and cooling;
step two, carrying out primary aging treatment for 15h at 450 ℃, and then carrying out air cooling;
and thirdly, carrying out secondary aging treatment for 5 hours at 540 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material F.
Example 4
Firstly, selecting electrolytic copper, a Cu-Cr intermediate alloy and high-purity zirconium as raw materials for a test material, and properly proportioning; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. Pouring the alloy liquid into a zirconium oxide filter screen on a pouring cup to filter out charcoal, pouring the alloy liquid into a cavity through the pouring cup to pour out an alloy casting with the chemical component of Cu-0.22Cr-0.24Zr (wt%); carrying out solution treatment on an alloy casting which is smelted and poured and has the chemical composition of Cu-0.22Cr-0.24Zr at 980 ℃ for 2h, and then carrying out water quenching and cooling;
step two, carrying out primary aging treatment for 15h at 450 ℃, and then carrying out air cooling;
and step three, carrying out secondary aging treatment for 5 hours at 570 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material G.
Example 5
Firstly, selecting electrolytic copper, a Cu-Cr intermediate alloy and high-purity zirconium as raw materials for a test material, and properly proportioning; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. Pouring the alloy liquid into a zirconium oxide filter screen on a pouring cup to filter out charcoal, pouring the alloy liquid into a cavity through the pouring cup to pour out an alloy casting with the chemical component of Cu-0.22Cr-0.24Zr (wt%); carrying out solution treatment on an alloy casting which is smelted and poured and has the chemical composition of Cu-0.22Cr-0.24Zr at 980 ℃ for 2h, and then carrying out water quenching and cooling;
step two, carrying out primary aging treatment for 15h at 450 ℃, and then carrying out air cooling;
and step three, carrying out secondary aging treatment for 5 hours at the temperature of 600 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material H.
Example 6
Firstly, selecting electrolytic copper, a Cu-Cr intermediate alloy and high-purity zirconium as raw materials for a test material, and properly proportioning; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. Pouring the alloy liquid into a zirconium oxide filter screen on a pouring cup to filter out charcoal, pouring the alloy liquid into a cavity through the pouring cup to pour out an alloy casting with the chemical component of Cu-0.22Cr-0.24Zr (wt%); carrying out solution treatment on an alloy casting which is smelted and poured and has the chemical composition of Cu-0.22Cr-0.24Zr at 980 ℃ for 2h, and then carrying out water quenching and cooling;
step two, carrying out primary aging treatment for 15h at 450 ℃, and then carrying out air cooling;
and step three, carrying out secondary aging treatment for 5 hours at 630 ℃, and then carrying out air cooling to obtain the Cu-Cr-Zr alloy material I.
Comparative example 1
The test material adopts electrolytic copper, Cu-Cr intermediate alloy and high-purity zirconium as raw materials in a proper proportion; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. The alloy liquid is poured into a zirconium oxide filter screen on the pouring cup to filter charcoal, and the alloy liquid is poured into the cavity through the pouring cup to pour out an alloy casting A with the chemical component of Cu-0.22Cr-0.24Zr (wt%).
Comparative example 2
The test material adopts electrolytic copper, Cu-Cr intermediate alloy and high-purity zirconium as raw materials in a proper proportion; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. Pouring the alloy liquid into a zirconium oxide filter screen on a pouring cup to filter out charcoal, pouring the alloy liquid into a cavity through the pouring cup to pour out an alloy casting with the chemical component of Cu-0.22Cr-0.24Zr (wt%); the alloy casting with the chemical composition of Cu-0.22Cr-0.24Zr is smelted and poured, and is subjected to solution treatment for 2 hours at the temperature of 980 ℃, and then water quenching and cooling are carried out.
Comparative example 3
The test material adopts electrolytic copper, Cu-Cr intermediate alloy and high-purity zirconium as raw materials in a proper proportion; the main technological parameters of the smelting process are as follows: when the vacuum degree is 4 multiplied by 10 < -1 > Pa (about half an hour), starting to electrify and heat to smelt the alloy, and in order to fully remove the absorbed air, firstly electrifying with low power, setting the power as 1kw/kg alloy, obviously deflating at 300-1000 ℃ in the experimental process, beginning to melt the alloy near 1150 ℃, continuing to heat, and then adding a proper amount of Zr through a charging hole. Since the melting points of Cr and Zr are high, Cr and Zr enter the copper matrix by dissolution, and therefore, a certain isothermal time is required to homogenize the alloying elements. And (3) preserving the heat when the temperature reaches 1250-1300 ℃ after the alloy is completely melted, and standing for 10-15 min. Argon is filled into the casting mould under 0.08MPa before casting, and the casting temperature is about 1250 ℃. The zirconium oxide filter screen that the alloy liquid pours into the pouring basin filters out the charcoal, the alloy liquid pours into the die cavity through the pouring basin and pours out the chemical composition of the alloy and is Cu-0.22Cr-0.24Zr (wt%); carrying out solution treatment on an alloy casting which is smelted and poured and has the chemical composition of Cu-0.22Cr-0.24Zr at 980 ℃ for 2h, and then carrying out water quenching and cooling; then carrying out primary aging treatment for 15h at 450 ℃, and then carrying out air cooling.
The alloy materials of the above examples 1-6 and the comparative examples 1-3 are respectively cast into sample bars with the size of phi 20mm multiplied by 120mm, and the sample bars are processed according to the regulation of GB6397-86 metal tensile test sample after solution treatment and aging treatment, and the specification of phi 5mm is selected; testing on a CMT electronic tensile testing machine at a loading speed of 2mm/min, measuring the conductivity by using an FQR-7501A eddy current conductivity meter, and obtaining a test result shown in figure 1; as can be seen from FIG. 1: the properties of the test bars under the different heat treatment processes (A-I) are shown in FIG. 1. As can be seen, the mechanical properties and the electric conductivity of the Cu-0.22Cr-0.24Zr alloy in the as-cast state are 198MPa and 45.75 percent IACS respectively. After the solid solution aging heat treatment, the tensile strength and the electric conductivity of the casting are both greatly improved. After primary aging, the tensile strength is improved from 198MPa to 330MPa, and the electrical conductivity is improved from 45.75 percent IACS to 81.5 percent IACS. The highest tensile strength of the sample after different secondary aging processes can reach 380MPa, and the highest electrical conductivity is 90.54% IACS. The comprehensive performance of tensile strength and conductivity is considered, and the secondary aging heat treatment process recommends that 980 ℃ is multiplied by 2h, water quenching is multiplied by 15h, air cooling is multiplied by 480 ℃ and multiplied by 5h, and air cooling is adopted. Under the heat treatment condition, the tensile strength and the electric conductivity of the Cu-0.22Cr-0.24Zr alloy are respectively 380MPa and 86.18 percent IACS. SEM photographs of the sample bars under different heat treatment process (A-I) conditions are shown in FIG. 2.
After secondary aging, the Cu-0.22Cr-0.24Zr alloy is subjected to ion thinning, the appearance and the structure of the Cu-0.22Cr-0.24Zr alloy are observed under a common H-800 transmission electron microscope and a JEM-2010 high-resolution electron microscope, and meanwhile, selective area electron diffraction analysis is carried out; the TEM photograph and diffraction spots of the Cu-0.22Cr-0.24Zr alloy after secondary aging are shown in FIG. 3, and it can be seen from FIG. 3 that: after secondary aging heat treatment, the average diameter of the nano-order second phase playing a strengthening role is basically unchanged, but the number of precipitated phases after secondary aging is increased, the obvious distance between particles is reduced, and the secondary aging second phase is more sufficiently precipitated from the morphology and diffraction spots of the precipitated phases.
The embodiments show that the alloy for the lead frame after heat treatment meets the performance index requirements of the alloy for the lead frame, and can be used for preparing the copper-based lead frame.
The technical solution of the present invention is not limited to the limitations of the above specific embodiments, and all technical modifications made according to the technical solution of the present invention fall within the protection scope of the present invention.
Claims (5)
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| CN115283774B (en) * | 2022-07-29 | 2023-11-24 | 中国电子科技集团公司第五十五研究所 | Treatment process of Cu-Cr-Zr alloy lead wire for packaging shell |
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Application publication date: 20220315 |