CN109136634B - High-performance copper alloy material and preparation method thereof - Google Patents
High-performance copper alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of metal materials, and particularly relates to a high-performance copper alloy and a preparation method thereof; the copper alloy contains Zr element with the mass fraction of 0.02-0.11%, and the balance of Cu and inevitable impurities; the copper alloy of the invention obtains 600-750 MPa tensile strength and 75-97% IACS conductivity, the Vickers hardness and conductivity of the copper alloy are improved by 10-40 HV compared with those of the copper alloy after low-temperature rolling, the conductivity is improved by 10-20% IACS, and the copper alloy has excellent strength and conductivity; the preparation method of the invention improves the thermal stability of the copper matrix, ensures the thermal stability of the copper alloy in a long-term high-temperature working environment, and is not easy to cause the condition of alloy softening failure.
Description
Technical Field
The invention belongs to the technical field of metal materials, and particularly relates to a high-performance copper alloy and a preparation method thereof.
Background
Copper, as a metal material with excellent thermal and electrical conductivity, has long been a common material in industrial and domestic applications. The alloy formed by taking pure copper metal as a matrix and adding one or more other elements is a copper alloy, and compared with pure copper, the performance of the alloy is greatly improved in the aspects of strength, thermal stability, ductility, corrosion resistance and the like. In particular, in an electronic component for a vehicle, it is required to be usable for a long time in an environment of higher temperature and stronger vibration.
However, the current copper alloy preparation method has the problem that the high strength and the high conductivity cannot coexist. For example, some conventionally heat treated high strength Cu-Cr-Zr alloys typically have an electrical conductivity of 78% IACS and a tensile strength of 480MPa, while pure copper, although annealed at 100% IACS, has only about 200MPa in strength. The copper alloy prepared in the current industrial production needs to be sacrificed to some extent on the other hand in order to obtain certain properties of strength or conductivity. Therefore, how to improve the excellent thermal stability and high strength characteristics of the copper alloy and improve the electrical conductivity becomes an obstacle to the development of the copper alloy.
In order to solve the problems of coarse grains and component segregation of copper alloy, the invention provides an environment-friendly copper-chromium-zirconium electrical alloy (patent number: 200510048661.2), an alloy ingot blank is prepared by adding trace metal elements such as magnesium, samarium and yttrium, and is subjected to spray deposition, then materials in various shapes are processed by extrusion, drawing and the like, and although the tensile strength and the conductivity respectively reach 730MPa and 76% IACS, the problems of multiple trace metal elements, accurate regulation of a production process, influence on the conductivity and the like exist in large-scale production. Aiming at copper-chromium, copper-zirconium and copper-chromium-zirconium age hardening alloys, the invention patent (patent number: 201510976079: A) prepares a high-strength and high-conductivity copper alloy material by a method of cold rolling, aging and solution treatment for multiple times. But has the disadvantages of excessive alloy elements, complicated process steps and further space for improvement in electrical conductivity and mechanical properties. Therefore, the content of the alloy elements in the copper alloy is not easy to be excessive, and the processing technology is not easy to be too complicated.
According to the Hall-Petch relationship, the finer the grain structure of the metal material is, the higher the yield strength thereof is. In recent years, it has become popular to refine the grain strengthening matrix by large plastic deformation (e.g., equal channel angular deformation ECAP, surface mechanical grinding SMGT) in the conventional method of obtaining fine grain strengthening copper alloy by rapid solidification or heat treatment. Especially, the research of Luokeji in the nano-layered structure shows the feasibility of improving the strength and the plasticity of the metal material by preparing the nano-layered structure.
Zirconium is an element for improving the strength of the alloy in aging strengthening, and can improve the recrystallization temperature and the thermal stability of the alloy, so that the alloy has high strength, high conductivity and high thermal stability. When the content of the zirconium element is less than 0.02%, the strength is not obviously improved, and the influence on the recrystallization temperature is small; when the content of zirconium element exceeds 0.11%, although the strength of the alloy is improved, the decrease in conductivity and plasticity is also significant. In order to obtain the best balance of strength, formability, plasticity and conductivity, the content of zirconium is controlled to be 0.02-0.11% by mass. In the published patent of 'a high-strength high-conductivity rare earth copper-zirconium alloy and a preparation method thereof' (patent number CN105088010B), zirconium element with the mass fraction of 0.35-0.45% is added, so that the softening temperature of the copper alloy after secondary rolling is increased to more than 500 ℃, the hardness value reaches about 200 HV and the conductivity is maintained to be more than 75% IACS, and the patent result fully shows the effectiveness of the zirconium element in improving the performance of the copper alloy.
Meanwhile, the reason why the zirconium element can effectively improve the thermal stability of the copper alloy is that the zirconium element segregates to grain boundaries or forms a precipitated phase in the grains during heat treatment, and the precipitate segregation reduces the mobility of the grains which can be inhibited by the grain boundaries, thereby hindering the recrystallization behavior of the grains. The thermal stability of the copper matrix is improved and the influence of the alloy elements on the conductivity is reduced through a very small amount of zirconium alloy elements, and the nano-scale grain structure improved strength is obtained by combining plastic deformation with high thermal stability, so that the method is expected to become a new idea for preparing the high-strength and high-conductivity copper alloy.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the defects in the prior art are overcome, the high-performance copper alloy with high conductivity, good mechanical property, good thermal stability and low production cost is provided, and the invention also aims to provide the copper alloy with high performance, wherein the copper alloy with high conductivity, good mechanical property, good thermal stability and low production cost comprises the following components: the preparation method of the high-performance copper alloy material is provided, and the copper alloy prepared by the method can meet the requirements of industrial application on the conductivity, thermal stability and mechanical property of the copper alloy.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a high-performance copper alloy contains 0.02 to 0.11 mass% of Zr element, and the balance of Cu and inevitable impurities.
Further, the copper alloy has a crystal grain size of 30 to 500 nm in the thickness direction and 90 to 25000 nm in the length direction as measured by transmission electron microscopy.
Furthermore, the copper alloy has a high-angle grain boundary fraction of more than 50% and a grain aspect ratio of 3:1-50:1 in an electron back scattering diffraction technology test.
Furthermore, the copper matrix grain structure in the copper alloy contains a twin crystal structure with the volume fraction of 5-85%, the lamella spacing of the twin crystal is 5-100 nm, and an included angle of about 2-40 degrees is formed between the lamella spacing and the long axis direction of the copper matrix grain.
Furthermore, in the test of the three-dimensional atom probe, 30-80% of Zr element in mass fraction is distributed on the crystal boundary of the copper matrix crystal grain.
Further, an appropriate amount of Zr or a Cu-Zr mother alloy is added to a copper melt whose remaining components are copper and irremovable impurities by melting, and solidified to obtain a solid copper alloy containing Zr element in a mass fraction of 0.02 to 0.11%.
A method of making a high performance copper alloy, the method comprising the steps of: sequentially carrying out smelting, solidification, solution treatment, equal-channel angular deformation (ECAP) or equal-channel angular deformation (ECAE), primary heat treatment, low-temperature rolling treatment and secondary heat treatment;
(1) the solution treatment is a heat treatment process of heating the copper alloy to 950 ℃ and 1000 ℃, preserving heat for 1-2 hours, and rapidly quenching and cooling;
(2) the isometric angular deformation is a plastic processing process for carrying out large plastic deformation on the copper alloy block after the solution treatment to realize the ultrafine grain;
(3) the primary heat treatment is a heat treatment process of heating the copper alloy block subjected to the equal-diameter angular deformation to 250-350 ℃ in a protective atmosphere, preserving the heat for 0.5-1.5 hours, and then rapidly quenching and cooling to room temperature;
(4) the low-temperature rolling treatment is a processing process of rolling deformation of the copper alloy subjected to primary heat treatment at a temperature lower than zero ℃ (for example, the copper alloy is quickly subjected to rolling deformation after being soaked in liquid nitrogen until the temperature is balanced);
(5) the secondary heat treatment is a heat treatment process that the copper alloy after low-temperature rolling is heated to 250-350 ℃ and is kept for 0.5-10 hours, and is rapidly quenched and cooled to room temperature.
Further, the rolling direction of the copper alloy in the low-temperature rolling treatment in the step (4) is consistent with the direction of the constant-diameter angular deformation, the pressing amount of each rolling is 0.5-1mm, the copper alloy needs to be soaked in liquid nitrogen again after each rolling, and the rolling work is repeated; the total rolling reduction of the sample was 60-99%.
The technical scheme adopted by the invention has the beneficial effects that:
1. the tensile strength and hardness of the copper alloy treated by the method are obviously improved compared with those of pure copper.
2. Compared with pure copper, the conductivity of the copper alloy treated by the method is reduced.
3. Compared with pure copper, the copper alloy treated by the method disclosed by the invention has the advantage that the thermal stability after plastic deformation is obviously improved.
4. The preparation method of the high-strength and high-conductivity copper alloy is simple to operate, low in equipment requirement and good in application prospect.
5. The invention provides reference for the subsequent preparation of the high-strength and high-conductivity copper alloy.
Drawings
The invention is further illustrated with reference to the following figures and examples.
Fig. 1 is a metallographic photograph of a copper alloy after solution treatment.
FIG. 2 is a grain structure image of the copper alloy after the isodiametric angular deformation.
Fig. 3 is a grain structure image of the copper alloy after the primary heat treatment.
FIG. 4 is a transmission electron microscope image of a copper alloy after cold rolling deformation.
Fig. 5 is a grain structure image of the copper alloy after the secondary heat treatment.
FIG. 6 is a tensile curve of a copper alloy after solution treatment, after 8 passes of equal-diameter angular deformation, and after completion of low-temperature rolling at 90% reduction.
Detailed Description
The following examples are intended to provide those skilled in the art with a more complete understanding of the present invention, and are not intended to limit the scope of the present invention. Reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
The copper alloy comprises 0.08% by mass of zirconium and the balance of copper and impurities which are difficult to remove, and the ingredients are fully mixed and then put into a smelting furnace to be melted, cooled and cut into block samples. Putting the copper alloy into a muffle furnace for solution treatment at 980 ℃ for 2 hours, and rapidly quenching and cooling to room temperature. And (3) carrying out equal-diameter angular deformation on the copper alloy, wherein the copper alloy is rotated by 90 degrees in the clockwise direction by each pass of extrusion, and the deformation direction is kept unchanged. The extrusion pass is to refine the grains of the copper alloy to an ultra-fine grain size, and the extrusion pass in this example is 8 passes. And then carrying out primary heat treatment on the copper alloy at the temperature of 300 ℃ for 1 hour, and rapidly quenching to room temperature. And then soaking the copper alloy in liquid nitrogen, carrying out one-pass rolling treatment on the copper alloy after the temperature of the copper alloy is completely the same as that of the liquid nitrogen, wherein the reduction in each-pass rolling is 0.5 mm, soaking the copper alloy in the liquid nitrogen again after one-pass rolling is finished, and repeating the rolling process again, wherein the final reduction is 90%. And (3) carrying out secondary heat treatment after rolling, wherein the heat treatment temperature is 300 ℃, the time is 1 hour, and rapidly quenching and cooling to room temperature after heating.
Example 2
The copper alloy comprises 0.02 mass percent of zirconium, the balance of copper and impurities which are difficult to remove, the ingredients are fully mixed and then put into a smelting furnace to be melted, and the mixture is cut into a block sample after being cooled. Putting the copper alloy into a muffle furnace for solution treatment at 950 ℃ for 2 hours, and rapidly quenching and cooling to room temperature. And (3) carrying out equal-diameter angular deformation on the copper alloy, wherein the copper alloy is rotated by 90 degrees in the clockwise direction by each pass of extrusion, and the deformation direction is kept unchanged. The extrusion pass is to refine the grains of the copper alloy to an ultra-fine grain size, and the extrusion pass in this example is 10 passes. And then carrying out primary heat treatment on the copper alloy at the temperature of 250 ℃ for 0.5 hour, and rapidly quenching to room temperature. And then soaking the copper alloy in liquid nitrogen, carrying out one-pass rolling treatment on the copper alloy after the temperature of the copper alloy is completely the same as that of the liquid nitrogen, wherein the reduction in each-pass rolling is 0.5 mm, soaking the copper alloy in the liquid nitrogen again after one-pass rolling is finished, and repeating the rolling process again, wherein the final reduction is 60%. And (3) carrying out secondary heat treatment after rolling is finished, wherein the temperature is 250 ℃, the time is 0.5 hour, and rapidly quenching and cooling to room temperature after heating is finished.
Example 3
The copper alloy comprises 0.11 mass percent of zirconium, the balance of copper and impurities which are difficult to remove, the ingredients are fully mixed and then put into a smelting furnace to be melted, and the mixture is cut into a block sample after being cooled. Putting the copper alloy into a muffle furnace for solution treatment at 1000 ℃ for 2 hours, and rapidly quenching and cooling to room temperature. And (3) carrying out equal-diameter angular deformation on the copper alloy, wherein the copper alloy is rotated by 90 degrees in the clockwise direction by each pass of extrusion, and the deformation direction is kept unchanged. The extrusion pass is to refine the grains of the copper alloy to an ultra-fine grain size, and the extrusion pass in this example is 10 passes. And then carrying out primary heat treatment on the copper alloy at 350 ℃ for 1 hour, and rapidly quenching to room temperature. And then soaking the copper alloy in liquid nitrogen, carrying out one-pass rolling treatment on the copper alloy after the temperature of the copper alloy is completely the same as that of the liquid nitrogen, wherein the rolling reduction in each pass is 1mm, soaking the copper alloy in the liquid nitrogen again after one-pass rolling is finished, and repeating the rolling process again, wherein the final rolling reduction is 60%. And (3) carrying out secondary heat treatment after rolling is finished, wherein the temperature is 350 ℃, the time is 5 hours, and rapidly quenching and cooling to room temperature after heating is finished.
Example 4
The copper alloy comprises 0.02 mass percent of zirconium, the balance of copper and impurities which are difficult to remove, the ingredients are fully mixed and then put into a smelting furnace to be melted, and the mixture is cut into a block sample after being cooled. Putting the copper alloy into a muffle furnace for solution treatment at 1000 ℃ for 2 hours, and rapidly quenching and cooling to room temperature. And (3) carrying out equal-diameter angular deformation on the copper alloy, wherein the copper alloy is rotated by 180 degrees in the clockwise direction by each pass of extrusion, and the deformation direction is kept unchanged. The extrusion pass is to refine the grains of the copper alloy to an ultra-fine grain size, and the extrusion pass in this example is 12 passes. And then carrying out primary heat treatment on the copper alloy at the temperature of 300 ℃ for 0.5 hour, and rapidly quenching to room temperature. And then soaking the copper alloy in liquid nitrogen, carrying out one-pass rolling treatment on the copper alloy after the temperature of the copper alloy is completely the same as that of the liquid nitrogen, wherein the reduction in each-pass rolling is 0.7mm, soaking the copper alloy in the liquid nitrogen again after one-pass rolling is finished, and repeating the rolling process again, wherein the final reduction is 99%. And (3) carrying out secondary heat treatment after rolling is finished, wherein the temperature is 250 ℃, the time is 3 hours, and rapidly quenching and cooling to room temperature after heating is finished.
Example 5
The copper alloy comprises 0.04% of zirconium by mass, the balance of copper and impurities which are difficult to remove, the ingredients are fully mixed and then put into a smelting furnace to be melted, and the mixture is cut into a block sample after being cooled. Putting the copper alloy into a muffle furnace for solution treatment at 980 ℃ for 2 hours, and rapidly quenching and cooling to room temperature. And (3) carrying out equal-diameter angular deformation on the copper alloy, wherein the deformation direction of the alloy is kept unchanged in each pass of extrusion. The extrusion pass is to refine the grains of the copper alloy to an ultra-fine grain size, and the extrusion pass in this example is 8 passes. And then carrying out primary heat treatment on the copper alloy, wherein the aging temperature is 300 ℃, the time is 0.5 hour, and the copper alloy is rapidly quenched to the room temperature. And then soaking the copper alloy in liquid nitrogen, carrying out one-pass rolling treatment on the copper alloy after the temperature of the copper alloy is completely the same as that of the liquid nitrogen, wherein the reduction in each-pass rolling is 0.5 mm, soaking the copper alloy in the liquid nitrogen again after one-pass rolling is finished, and repeating the rolling process again, wherein the final reduction is 95%. And (3) carrying out secondary heat treatment after rolling is finished, wherein the aging temperature is 300 ℃, the time is 10 hours, and after heating is finished, rapidly quenching and cooling to room temperature.
Table 1 shows the tensile strength, microhardness and electrical conductivity of the copper alloy after aging strengthening treatment
The present inventors have conducted extensive studies and found that the balance of the Zr element is 0.02 to 0.11 mass%, and the Cu element and inevitable impurities constitute the balance. The size of the crystal grains in the thickness direction was 30-500 nm and the size in the length direction was 100-25000 nm as measured by transmission electron microscopy. In the test of the electron back scattering diffraction technology, the high-angle grain boundary fraction exceeds 50 percent, and the aspect ratio of the grains reaches 3:1-50: 1. The copper matrix grain structure contains twin crystal structure with volume fraction of 5-85%, the lamella spacing of the twin crystal is 5-100 nm, and an included angle of about 2-40 degrees is formed with the long axis direction of the copper matrix grain. In the test of the three-dimensional atom probe, 30-80% of Zr element exists on the crystal boundary of the copper alloy crystal grains, and is uniformly distributed. The copper alloy has the beneficial effects that the copper alloy achieves the tensile strength of 600-750 MPa and the electric conductivity of 75-97% IACS, and has excellent strength and electric conductivity.
In the embodiment of the invention, Zr with the mass fraction of 0.02-0.11% is added into a copper matrix with the balance of copper and impurities which cannot be removed through smelting, and a bulk copper alloy is obtained after solidification. In an annealing test of the copper alloy at 500 ℃ for 1 hour and 300 ℃ after the equal-diameter angular deformation, the matrix grain size of the copper alloy is maintained at an ultra-fine grain size, the grain size is maintained at 2000 nm and 200 ℃ without obvious grain growth. In the annealing test of the copper alloy at the temperature of 300-500 ℃ for 1 hour after low-temperature rolling, the grain size of the copper alloy matrix in the rolling normal direction (grain thickness) is maintained at 2000 nm, and the grain large-angle grain boundary fraction is more than 50%. The method has the advantages of improving the thermal stability of the copper matrix and ensuring that the alloy is not easy to lose efficacy and soften under the long-term high-temperature working environment.
The method for producing a copper alloy comprises subjecting a molten copper alloy base material to solution treatment at 950-. And performing secondary heat treatment at the temperature of 250-350 ℃ for 0.5-10 hours again, and quenching and cooling, so that the Vickers hardness and the conductivity of the copper alloy after the secondary heat treatment are improved by 10-40 HV compared with the Vickers hardness of the copper alloy after low-temperature rolling, and the conductivity is improved by 10-20% IACS.
The high-strength high-conductivity copper alloy according to the present invention is a solid copper alloy containing 0.02 to 0.11 mass% of Zr element obtained by adding an appropriate amount of Zr or a Cu — Zr master alloy to a copper melt containing copper and unremovable impurities as the remaining components by melting and solidifying the mixture.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (6)
1. A high-performance copper alloy is characterized in that: the copper alloy contains Zr element with the mass fraction of 0.02-0.11%, and the balance of Cu and inevitable impurities;
the preparation method of the high-performance copper alloy comprises the following steps: sequentially carrying out smelting, solidification, solid solution treatment, equal-diameter angular deformation ECAP or ECAE, primary heat treatment, low-temperature rolling treatment and secondary heat treatment;
(1) the solid solution treatment is a heat treatment process of heating the copper alloy block to 950 ℃ and 1000 ℃, preserving heat for 1-2 hours and rapidly quenching and cooling;
(2) the isometric angular deformation is a plastic processing process for carrying out large plastic deformation on the copper alloy block after the solution treatment to realize the ultrafine grain;
(3) the primary heat treatment is a heat treatment process of heating the copper alloy block subjected to the equal-diameter angular deformation to 250-350 ℃ in a protective atmosphere, preserving the heat for 0.5-1.5 hours, and then rapidly quenching and cooling to room temperature;
(4) the low-temperature rolling treatment is a processing process of rapidly performing rolling deformation after soaking the copper alloy subjected to primary heat treatment in liquid nitrogen at a temperature lower than zero DEG C until the temperature is balanced;
the rolling direction of the copper alloy in the low-temperature rolling treatment is consistent with the direction of the equal-diameter angular deformation, the rolling reduction of each rolling is 0.5-1mm, and after each rolling pass is finished, the copper alloy needs to be soaked in liquid nitrogen again for cooling treatment and then is repeatedly rolled; the total rolling reduction of the sample is 60-99%;
(5) the secondary heat treatment is a heat treatment process that the copper alloy after low-temperature rolling is heated to 250-350 ℃ and is kept for 0.5-10 hours, and is rapidly quenched and cooled to room temperature.
2. The high performance copper alloy of claim 1, wherein: in the test of the electron back scattering diffraction technology, the high-angle grain boundary fraction of the copper alloy exceeds 50 percent, and the aspect ratio of grains reaches 3:1-50: 1.
3. The high performance copper alloy of claim 1, wherein: the copper alloy contains a copper matrix grain structure with a volume fraction of 5-85% of a twin crystal structure, the lamella spacing of the twin crystal is 5-100 nm, and an included angle of about 2-40 degrees is formed between the twin crystal structure and the long axis direction of the copper matrix grain.
4. The high performance copper alloy of claim 1, wherein: the size of the crystal grain in the thickness direction of the copper alloy is 30-500 nm and the size in the length direction of the copper alloy is 90-25000 nm measured by a transmission electron microscope technology.
5. The high performance copper alloy of claim 1, wherein: in the test of the three-dimensional atom probe, 30-80% of Zr element by mass fraction is distributed on the crystal boundary of the copper matrix crystal grain.
6. The high performance copper alloy of claim 1, wherein: adding a proper amount of Zr or Cu-Zr mother alloy into a copper melt with the balance of copper and irremovable impurities by smelting, and solidifying to obtain the solid copper alloy containing Zr element with the mass fraction of 0.02-0.11%.
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| CN102108451A (en) * | 2011-02-15 | 2011-06-29 | 常州大学 | Preparation method of copper alloys with high strength and high electric conductivity |
| CN103380221A (en) * | 2011-02-18 | 2013-10-30 | 三菱伸铜株式会社 | Cu-zr-based copper alloy plate and process for manufacturing same |
| CN105039758A (en) * | 2015-06-11 | 2015-11-11 | 大连理工大学 | Precipitation strengthening type high-strength and high-conductivity CuZr alloy and preparing method thereof |
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| CN103380221A (en) * | 2011-02-18 | 2013-10-30 | 三菱伸铜株式会社 | Cu-zr-based copper alloy plate and process for manufacturing same |
| CN105039758A (en) * | 2015-06-11 | 2015-11-11 | 大连理工大学 | Precipitation strengthening type high-strength and high-conductivity CuZr alloy and preparing method thereof |
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