CN112981170A - Chromium-zirconium-copper alloy for cold heading and preparation method thereof - Google Patents
Chromium-zirconium-copper alloy for cold heading and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a chromium-zirconium-copper alloy for cold heading, which is characterized in that: the average grain size of the chromium-zirconium-copper alloy is less than or equal to 4 mu m, and the standard deviation of the sizes of the grains is less than or equal to 1/2 average grain size. The average grain size of the chromium-zirconium-copper alloy is controlled to be less than or equal to 4 mu m, the standard deviation of the sizes of all grains is controlled to be less than or equal to 1/2 average grain size, and the fine grain size means that the chromium-zirconium-copper alloy has higher grain boundary volume fraction; in addition, the fine grain size and the more uniform grain size are beneficial to improving the smoothness of the cold heading product and avoiding the orange peel phenomenon.
Description
Technical Field
The invention relates to a copper alloy, in particular to a chromium-zirconium-copper alloy for cold heading and a preparation method thereof.
Background
The materials of electrode caps, contact tips and other parts applied to the field of resistance welding are in high-temperature and high-current environments, so that the materials have excellent high strength, high conductivity and high-temperature softening resistance. Meanwhile, since parts such as electrode caps are generally formed by cold heading, excellent cold heading property is required. The cold heading requires that the material has uniform structure and proper strength. At present, the Cu-Cr-Zr bar for preparing the electrode cap material adopts the preparation process of casting, ingot casting heating, extruding, solid solution, drawing, aging and finished product drawing, because crystal grains of the material grow after solid solution, the product has the phenomena of large central crystal grains and small and uneven structures of the edge crystal grains after the subsequent drawing processing, and if the sizes and the proportions of the large and small crystal grains are not properly controlled, the problems of large deformation resistance and irregular deformation easily occur in the cold heading process.
The invention discloses a copper-chromium-zirconium alloy, a preparation method and application thereof in patent application No. CN201910583012.4, and the patent states that the cast structure can be refined and the subsequent processing performance can be improved by adding a proper amount of graphene oxide. However, the density of the graphene oxide as a two-dimensional material is greatly different from that of copper water, and the graphene oxide is difficult to uniformly disperse in a copper matrix by adopting a traditional vacuum melting method, so that the graphene oxide is also uneven in refining a casting blank, and the structure and the performance of the obtained product are also difficult to ensure. Finally, the cold heading performance is poor, and the method is not suitable for large-scale popularization and production.
The invention has patent application number CN201811474100.2 and discloses a copper chromium zirconium alloy and a preparation method thereof, and the patent refines the structure and improves the performance by adding trace scandium element. Although the trace elements can refine grains to a certain degree, the growth of the grains in the solid solution process is still difficult to limit, and the subsequent cold deformation is difficult to refine the thick structure in the center of the bar to be consistent with the edge. Therefore, the process still cannot obtain the copper alloy bar for cold heading with uniform structure and performance.
Therefore, further improvements are needed for the microstructure of the existing chromium zirconium copper alloy.
Disclosure of Invention
The first technical problem to be solved by the invention is to provide a chromium-zirconium-copper alloy for cold heading with fine and uniform structure.
The technical scheme adopted by the invention for solving the first technical problem is as follows: the utility model provides a chromium zirconium copper alloy for cold-heading which characterized in that: the average grain size of the chromium-zirconium-copper alloy is less than or equal to 4 mu m, and the standard deviation of the sizes of the grains is less than or equal to 1/2 average grain size.
Preferably, the hardness of the chromium-zirconium-copper alloy is 75-85 HRB, the yield strength is 440-520 MPa, the tensile strength is 480-560 MPa, the difference value between the yield strength and the tensile strength is less than or equal to 40MPa, the elongation after fracture is more than or equal to 15%, and the electric conductivity is 75-90% IACS. In the process of processing a copper alloy bar into products such as an electrode cap and the like, the bar is usually cut and blanked firstly, then cold heading processing is carried out, and poor ports, such as uneven and inclined ports and the like, usually exist at two ends after the material is cut, so that the cold heading deformation is uneven. The inventor finds that the shearing quality is related to the mechanical property of the material besides the material structure, so that the material can reach the performance indexes, namely proper hardness, strength and plasticity, the shearing end face can be ensured to be flat, and the material can be uniformly deformed during cold heading.
Preferably, the chromium-zirconium-copper alloy comprises the following components in percentage by mass: 0.4 to 1.2 wt% of Cr, 0.05 to 0.15 wt% of Zr, 0.01 to 0.1 wt% of Si, 0.01 to 0.08 wt% of Fe, 0.01 to 0.04 wt% of Ti, and the balance of Cu.
Si, Fe and Ti elements can further refine grains and improve the cold heading performance and the surface quality of products.
The second technical problem to be solved by the invention is to provide a preparation method of the chromium-zirconium-copper alloy for cold heading.
The technical scheme adopted by the invention for solving the second technical problem is as follows: a preparation method of chromium-zirconium-copper alloy for cold heading is characterized by comprising the following steps: the method comprises the following steps:
a) casting: preparing an alloy casting blank by an upward continuous casting method;
b) primary drawing: drawing the alloy casting blank by 30-80% of deformation;
c) solid solution: carrying out solid solution treatment on the wire blank subjected to drawing processing, wherein the solid solution temperature is 940-990 ℃;
d) continuous extrusion: carrying out continuous extrusion processing on the wire blank subjected to the solution treatment, wherein the extrusion ratio is 0.5-1.8, and the extrusion speed is 2-8 m/min;
e) secondary drawing: drawing the continuously extruded wire blank by 20-80% of deformation;
f) aging treatment: carrying out aging treatment on the cold-processed wire blank, controlling the temperature to be 400-500 ℃, and keeping the temperature for 1-5 h;
g) drawing a finished product: and (4) carrying out finished product drawing on the wire blank subjected to the aging treatment, wherein the deformation is 5-20%.
The average grain size of the casting blank prepared by upward casting is about 800 mu m, the grain size is large, the large grain size can be crushed by primary drawing, and then the c) solid solution is carried out, so that the fiber structure after drawing is recrystallized, the material hardened by drawing is softened, the hardness is reduced, and the subsequent continuous extrusion is convenient. The wire blank is subjected to strong shear deformation in the continuous extrusion process, crystal grains are further refined on the original basis, the blank and a tool generate heat through friction in the process, the extrusion ratio is 0.5-1.8, the extrusion speed is 2-8 m/min, the extruded blank can quickly pass through an extrusion cavity, the material is short in heating time, the crystal grains are prevented from growing, good surface quality is guaranteed, secondary drawing, aging and finished product drawing are carried out, and the process parameters are controlled within the range to finally realize a small and uniform microstructure of the crystal grains.
Preferably, the primary drawing deformation is 50-80%, the average grain size of the copper alloy wire blank after drawing is less than or equal to 80 microns, and the standard deviation of the grain size is less than or equal to 20 microns; the solid solution temperature is 950-990 ℃, the heat preservation time is 10-30 min, and the electric conductivity of the solid-dissolved wire blank is less than or equal to 46% IACS. The method is characterized in that Cr and Zr elements are dissolved in a Cu matrix as much as possible, the solid solubility of Cr and Zr in Cu is increased along with the increase of the solid solution temperature, the crystal grains grow due to too high solid solution temperature, the high solid solution temperature of 950-990 ℃ and the short heat preservation time of 10-30 min are adopted, the electric conductivity after solid solution is not more than 46% IACS (International Annealed copper standard temperature System), the good solid solution effect is achieved, meanwhile, the average crystal grain size is not more than 80 mu m, the standard deviation of the crystal grain size is not more than 20 mu m, the crystal grain growth is avoided, and the control of the final crystal grain structure is guaranteed.
Preferably, the average grain size of the wire rod after continuous extrusion is less than or equal to 9 μm, and the standard deviation of the grain size is less than or equal to 3 μm.
Preferably, the average grain size of the wire rod after the secondary drawing is less than or equal to 6 μm, and the standard deviation of the grain size is less than or equal to 2 μm.
Preferably, the hardness of the copper alloy wire blank after the aging treatment is 70-82 HRB, the yield strength is 400-460 MPa, the tensile strength is 460-520 MPa, and the electric conductivity is 78-90% IACS.
Compared with the prior art, the invention has the advantages that:
1) the average grain size of the chromium-zirconium-copper alloy is controlled to be less than or equal to 4 mu m, the standard deviation of the sizes of all grains is controlled to be less than or equal to 1/2 average grain size, and the fine grain size means that the crystal grain boundary volume fraction is higher, and the crystal grain structure is relatively loose, so that the movement of the crystal grains during cold heading is facilitated, and the cold heading performance is improved; in addition, the fine grain size and the more uniform grain size are beneficial to improving the smoothness of the cold heading product and avoiding the orange peel phenomenon.
2) According to the process, the casting blank is obtained by an upward continuous casting method and then is directly drawn, then the wire blank is obtained by adopting a solid solution and continuous extrusion mode, a more uniform and fine grain structure can be obtained, the problem of coarse grains caused in the hot extrusion and solid solution processes is avoided, the problem of uneven sizes of grains at the center and the edge caused by the subsequent drawing is further weakened, and the material has proper hardness, strength and plasticity by matching with proper drawing and heat treatment processes, so that the flatness of the sheared and blanked rear end face is ensured, the deformation resistance of the material is reduced, the uniform deformation performance capability of the material is increased, and the process has a positive effect on smooth cold heading forming.
3) The chromium-zirconium-copper alloy has the hardness of 75-85 HRB, the yield strength of 440-520 MPa, the tensile strength of 480-560 MPa, the difference between the yield strength and the tensile strength of less than or equal to 40MPa, the elongation after fracture of more than or equal to 15 percent and the electrical conductivity of 75-90 percent IACS. The cold heading compression ratio is more than 35%, the cold heading surface roughness is less than 3.5Ra, the surface is smooth and clean, no orange peel texture exists, and the cold heading deformation is uniform.
Drawings
FIG. 1 is a diagram of EBSD grains of a finished product of example 1 of the present invention.
Detailed Description
The invention is described in further detail below with reference to the accompanying examples.
Example 1
The copper, chromium and zirconium alloy comprises the following components: cr: 0.55 wt%, Zr: 0.9 wt%, the balance being Cu and unavoidable impurities; the process flow of the copper-chromium-zirconium bar comprises the following steps:
1) casting: preparing a copper-chromium-zirconium alloy wire blank with the diameter of 30mm by an upward continuous casting method;
2) primary drawing: drawing a wire blank with the diameter of 30mm to the diameter of 25mm, wherein the total deformation is 30.56%;
3) solid solution: carrying out solid solution on the wire blank after drawing at 960 ℃, preserving the heat for 30min, and quenching after finishing the heat preservation;
4) continuous extrusion: continuously extruding the wire blank subjected to solid solution at the extrusion speed of 3m/min to obtain a wire blank with the diameter of 30 mm; the extrusion ratio was 0.69;
5) secondary drawing: cold drawing the continuously extruded wire blank to 16mm, wherein the total deformation is 71.56%;
6) aging treatment: carrying out aging treatment on the wire blank after drawing, controlling the temperature at 485 ℃, keeping the temperature for 2h, and cooling the wire blank to room temperature after the heat preservation time is over;
7) acid washing: carrying out acid washing treatment on the wire blank subjected to the aging treatment for 10min to remove surface oxide skin;
8) drawing a finished product: the wire blank after acid washing was subjected to drawing processing to 15.5mm with a deformation of 6.15%.
Example 2
The copper, chromium and zirconium alloy comprises the following components: cr: 0.85 wt%, Zr: 0.12 wt%, Si: 0.04 wt%, Fe: 0.025 wt%, Ti: 0.03 wt%, the balance being Cu and unavoidable impurities; the process flow of the copper-chromium-zirconium bar comprises the following steps:
1) casting: preparing a copper-chromium-zirconium alloy wire blank with the diameter of 35mm by an upward continuous casting method;
2) primary drawing: drawing a wire blank with the diameter of 35mm to the diameter of 20mm, wherein the total deformation is 67.35%;
3) solid solution: carrying out solid solution on the wire blank after drawing at 940 ℃, preserving the heat for 60min, and quenching after finishing the heat preservation;
4) continuous extrusion: continuously extruding the solid-dissolved wire blank at the extrusion speed of 4.5m/min to obtain a wire blank with the diameter of 18 mm; the extrusion ratio was 1.23;
5) secondary drawing: cold drawing the continuously extruded wire blank to 16mm, wherein the total deformation is 20.99%;
6) aging treatment: carrying out aging treatment on the wire blank after drawing, controlling the temperature at 410 ℃, keeping the temperature for 4h, and air-cooling to room temperature after the heat preservation time is over;
7) acid washing: carrying out acid washing treatment on the wire blank subjected to the aging treatment for 10min to remove surface oxide skin;
8) drawing a finished product: the wire blank after acid washing was subjected to drawing processing to 15.5mm with a deformation of 6.15%.
Example 3
The copper, chromium and zirconium alloy comprises the following components: cr: 0.85 wt%, Zr: 0.12 wt%, Si: 0.04 wt%, Fe: 0.025 wt%, Ti: 0.03 wt%, the balance being Cu and unavoidable impurities; the process flow of the copper-chromium-zirconium bar comprises the following steps:
1) casting: preparing a copper-chromium-zirconium alloy wire blank with the diameter of 35mm by an upward continuous casting method;
2) primary drawing: drawing a wire blank with the diameter of 40mm to the diameter of 18mm, wherein the total deformation is 69.75%;
3) solid solution: carrying out solid solution on the wire blank after drawing at 950 ℃, preserving the heat for 60min, and quenching after finishing the heat preservation;
4) continuous extrusion: continuously extruding the solid-dissolved wire blank at the extrusion speed of 4.5m/min to obtain a wire blank with the diameter of 18 mm; the extrusion ratio is 1;
5) secondary drawing: cold drawing the continuously extruded wire blank until the thickness is 13mm and the total deformation is 47.83%;
6) aging treatment: carrying out aging treatment on the wire blank after drawing, controlling the temperature at 450 ℃, keeping the temperature for 3h, and cooling the wire blank to room temperature after the heat preservation time is over;
7) acid washing: carrying out acid washing treatment on the wire blank subjected to the aging treatment for 10min to remove surface oxide skin;
8) drawing a finished product: the wire blank after pickling was drawn to 12.5mm with a strain of 7.54%.
Comparative example 1
The copper, chromium and zirconium alloy comprises the following components: cr: 0.55 wt%, Zr: 0.9 wt%, the balance being Cu and unavoidable impurities; the process flow of the copper-chromium-zirconium bar comprises the following steps:
1) casting: preparing a copper-chromium-zirconium alloy wire blank with the diameter of 30mm by an upward continuous casting method;
2) drawing: drawing a wire blank with the diameter of 30mm to the diameter of 25mm, wherein the total deformation is 30.56%;
3) solid solution: carrying out solid solution on the wire blank after drawing at 960 ℃, preserving the heat for 30min, and quenching after finishing the heat preservation;
4) drawing: cold-drawing the wire blank subjected to the solution treatment until the wire blank is processed to be 16mm and the total deformation is 59.04%;
5) aging treatment: carrying out aging treatment on the wire blank after drawing, controlling the temperature at 485 ℃, keeping the temperature for 2h, and cooling the wire blank to room temperature after the heat preservation time is over;
6) acid washing: carrying out acid washing treatment on the wire blank subjected to the aging treatment for 10min to remove surface oxide skin;
7) drawing a finished product: the wire blank after acid washing was subjected to drawing processing to 15.5mm with a deformation of 6.15%.
Comparative example 1 a continuous extrusion process was absent compared to example 1.
Comparative example 2
The copper, chromium and zirconium alloy comprises the following components: cr: 0.85 wt%, Zr: 0.12 wt%, the balance being Cu and unavoidable impurities; the process flow of the copper-chromium-zirconium bar comprises the following steps:
1) casting: preparing a copper-chromium-zirconium alloy ingot with the diameter of 240mm by a horizontal continuous casting method;
2) ingot casting and heating: heating an ingot with the diameter of 240mm to 920 ℃;
3) extruding: putting the heated cast ingot into an extruder for extrusion, wherein the extrusion specification is 30 mm;
4) solid solution: carrying out solid solution on the extruded wire blank at 940 ℃, preserving heat for 60min, and quenching after finishing the heat preservation;
5) drawing: carrying out cold drawing on the continuously extruded wire blank, and processing to 16 mm;
6) aging treatment: carrying out aging treatment on the wire blank after drawing, controlling the temperature at 410 ℃, keeping the temperature for 4h, and air-cooling to room temperature after the heat preservation time is over;
7) acid washing: carrying out acid washing treatment on the wire blank subjected to the aging treatment for 10min to remove surface oxide skin;
8) drawing a finished product: the wire blank after acid washing was subjected to drawing processing to 15.5mm with a deformation of 6.15%.
The microstructures, mechanical properties and cold heading properties of examples and comparative examples were examined.
Average grain size and standard deviation of grain size: and taking a section vertical to the drawing direction, grinding and polishing, imaging and processing by a scanning electron microscope with an EBSD system, and counting the sizes of the grains in the picture by Channel 5 software. For the purposes of the present invention, the average value of the respective grain sizes determined with 10 segments is considered as the average grain size (mGS), and the standard deviation of these grain sizes is considered as the grain size standard deviation.
Cold heading performance:
the cold heading compression ratio is used as an index for evaluating the deformation resistance of the material, the larger the numerical value of the cold heading compression ratio is, the better the cold heading performance is, the method is used for measuring the cold heading compression ratio, for samples with the same specification, the same force is applied along the axial direction of the samples at room temperature, the samples are compressed, the compression is stopped when the specified force value is reached, and the ratio of the deformation length of the samples to the original length of the samples is the cold heading compression ratio.
And testing the roughness of the surface after cold heading by a roughness meter to judge the smoothness of the surface of the sample after cold heading. And (4) judging whether the deformation is uniform or not by observing the shape of the sample after cold heading.
As can be seen from Table 1, the average grain size of the chromium-zirconium-copper alloy is less than or equal to 4 μm, the standard deviation of the sizes of all grains is less than or equal to 1/2 average grain size, the grains are fine and uniform, and the grain size is obviously superior to that of comparative example 1 and comparative example 2; the difference between the yield strength and the tensile strength is controlled within 40MPa, and after cold heading, the compressibility, the cold heading surface smoothness and the cold heading deformation uniformity are superior to those of comparative example 1 and comparative example 2.
TABLE 1 microstructure, mechanical properties and Cold heading Properties of examples and comparative examples
Claims (8)
1. The utility model provides a chromium zirconium copper alloy for cold-heading which characterized in that: the average grain size of the chromium-zirconium-copper alloy is less than or equal to 4 mu m, and the standard deviation of the sizes of the grains is less than or equal to 1/2 average grain size.
2. The chromium zirconium copper alloy for cold heading as claimed in claim 1, wherein: the chromium-zirconium-copper alloy has the hardness of 75-85 HRB, the yield strength of 440-520 MPa, the tensile strength of 480-560 MPa, the difference between the yield strength and the tensile strength of less than or equal to 40MPa, the elongation after fracture of more than or equal to 15 percent and the electrical conductivity of 75-90 percent IACS.
3. The chromium zirconium copper alloy for cold heading as claimed in claim 1, wherein: the chromium-zirconium-copper alloy comprises the following components in percentage by mass: 0.4 to 1.2 wt% of Cr, 0.05 to 0.15 wt% of Zr, 0.01 to 0.1 wt% of Si, 0.01 to 0.08 wt% of Fe, 0.01 to 0.04 wt% of Ti, and the balance of Cu.
4. A method for producing a chromium zirconium copper alloy for cold heading as claimed in any one of claims 1 to 3, characterized in that: the method comprises the following steps:
a) casting: preparing an alloy casting blank by an upward continuous casting method;
b) primary drawing: drawing the alloy casting blank by 30-80% of deformation;
c) solid solution: carrying out solid solution treatment on the wire blank subjected to drawing processing, wherein the solid solution temperature is 940-990 ℃;
d) continuous extrusion: carrying out continuous extrusion processing on the wire blank subjected to the solution treatment, wherein the extrusion ratio is 0.5-1.8, and the extrusion speed is 2-8 m/min;
e) secondary drawing: drawing the continuously extruded wire blank by 20-80% of deformation;
f) aging treatment: carrying out aging treatment on the cold-processed wire blank, controlling the temperature to be 400-500 ℃, and keeping the temperature for 1-5 h;
g) drawing a finished product: and (4) carrying out finished product drawing on the wire blank subjected to the aging treatment, wherein the deformation is 5-20%.
5. The method for producing a chromium-zirconium-copper alloy for cold heading as claimed in claim 4, wherein: the primary drawing deformation is 50-80%, the average grain size of the copper alloy wire blank after drawing is less than or equal to 80 microns, and the standard deviation of the grain size is less than or equal to 20 microns; the solid solution temperature is 950-990 ℃, the heat preservation time is 10-30 min, and the electric conductivity of the solid-dissolved wire blank is less than or equal to 46% IACS.
6. The method for producing a chromium-zirconium-copper alloy for cold heading as claimed in claim 4, wherein: the average grain size of the continuously extruded wire blank is less than or equal to 9 mu m, and the standard deviation of the grain size is less than or equal to 3 mu m.
7. The method for producing a chromium-zirconium-copper alloy for cold heading as claimed in claim 4, wherein: the average grain size of the wire blank after the secondary drawing is less than or equal to 6 mu m, and the standard deviation of the grain size is less than or equal to 2 mu m.
8. The method for producing a chromium-zirconium-copper alloy for cold heading as claimed in claim 4, wherein: the hardness of the copper alloy wire blank after the aging treatment is 70-82 HRB, the yield strength is 400-460 MPa, the tensile strength is 460-520 MPa, and the electric conductivity is 78-90% IACS.
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| CN113718129A (en) * | 2021-08-30 | 2021-11-30 | 宁波金田铜业(集团)股份有限公司 | Chromium-zirconium-copper alloy and preparation method thereof |
| CN113718128A (en) * | 2021-08-30 | 2021-11-30 | 宁波金田铜业(集团)股份有限公司 | Copper-chromium-zirconium alloy and preparation method thereof |
| CN114309119A (en) * | 2021-12-29 | 2022-04-12 | 常州大学 | Graphene/copper composite deformed copper-chromium-zirconium alloy laminated strip and preparation method thereof |
| CN115074564A (en) * | 2022-07-04 | 2022-09-20 | 江西理工大学 | Preparation method of high-strength high-conductivity copper-chromium-zirconium alloy |
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| CN113718129A (en) * | 2021-08-30 | 2021-11-30 | 宁波金田铜业(集团)股份有限公司 | Chromium-zirconium-copper alloy and preparation method thereof |
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| CN113718128B (en) * | 2021-08-30 | 2022-06-28 | 宁波金田铜业(集团)股份有限公司 | Copper-chromium-zirconium alloy and preparation method thereof |
| CN114309119A (en) * | 2021-12-29 | 2022-04-12 | 常州大学 | Graphene/copper composite deformed copper-chromium-zirconium alloy laminated strip and preparation method thereof |
| CN114309119B (en) * | 2021-12-29 | 2023-10-20 | 常州大学 | Graphene/copper composite deformed copper-chromium-zirconium alloy layered strip and preparation method thereof |
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