CN115464406A - High-strength high-conductivity CuCr copper intermediate alloy and preparation method thereof - Google Patents
High-strength high-conductivity CuCr copper intermediate alloy and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of copper-chromium alloy, and particularly relates to a high-strength high-conductivity CuCr copper intermediate alloy and a preparation method thereof. The method comprises the following steps: step (1): selecting cathode electrolytic pure copper and chromium as raw materials, wherein the mass percent of the chromium is 15wt% +/-1%; step (2): smelting by adopting a vacuum intermediate frequency induction furnace, and preparing as-cast copper-chromium alloy in a vacuum environment; and (3): carrying out solid solution treatment and turning on the as-cast copper-chromium alloy to prepare a copper-chromium alloy bar; and (4): and (3) performing rotary forging and intermediate aging on the copper-chromium alloy bar with the total strain of 3 +/-0.2, then performing rolling with the processing deformation rate of 70 +/-2%, and finally performing final aging treatment to obtain the high-strength and high-conductivity copper-chromium intermediate alloy. Under the organic combination of rotary swaging and rolling processes, the prepared copper-chromium intermediate alloy has the advantages of high strength, good conductivity, uniform structure, low cost and the like, and has high yield, and can be used in subsequent processing and the like.
Description
Technical Field
The invention belongs to the field of copper-chromium alloy, and particularly relates to a high-strength high-conductivity CuCr copper intermediate alloy and a preparation method thereof.
Background
The copper-based deformation in-situ fiber reinforced composite material is a high-strength and high-conductivity material with excellent comprehensive performance, and has better application prospect in the fields of high-speed electrified locomotive contact wires, super-large-scale lead frames, vacuum contacts in high-power vacuum circuit breakers and the like. As a conductor material with high cost performance, fiber reinforced Cu-Fe, cu-Nb, cu-Ag alloy and the like have been developed so as to meet the industrial requirements in various aspects. Unfortunately, the problem of low electrical conductivity has not been solved despite the relatively high strength of Cu-Fe and Cu-Nb alloys. Although the Cu-Ag alloy has good high strength and low conductivity, its cost is too high to be applied to industry in a large scale.
Compared with Cu-Ag alloy, cu-Cr deformation copper-based in-situ fiber reinforced composite material (Cu-Cr alloy for short) has higher cost performance and is concerned. Researches show that the comprehensive performance of the Cu-Cr (the mass fraction of Cr is generally 8-20%) alloy can be improved by adding a third component. At present, reported ternary alloying elements applied to Cu-Cr series alloy comprise Ti, ag, co, mo, zr and the like, but the addition of a third component can further break the continuity of a copper matrix, so that the conductivity of the alloy is reduced. Therefore, the mechanical property of the material is improved by adding a large amount of chromium into copper, the material is subjected to multi-dimensional high-speed strain processing by rotary swaging and rolling, and excessive chromium in a copper matrix is distributed more uniformly, has more orientation and forms a fine long fibrous shape by using a proper heat treatment mode, so that electrons can move in the matrix more conveniently. The material has improved mechanical performance and conductivity.
High strength and high conductivity have been a pair of conflicting parameters in the development and preparation of copper-based alloys, and this problem has plagued most of those engaged in related research.
Disclosure of Invention
The invention aims to provide a low-cost high-strength high-conductivity copper-chromium alloy and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows: a preparation method of a high-strength high-conductivity CuCr copper intermediate alloy comprises the following steps:
step (1): selecting cathode electrolytic pure copper and chromium as raw materials, wherein the mass percent of the chromium is 15wt% +/-1%;
step (2): smelting by adopting a vacuum intermediate frequency induction furnace, and preparing as-cast copper-chromium alloy in a vacuum environment;
and (3): carrying out solid solution treatment and turning on the as-cast copper-chromium alloy to prepare a copper-chromium alloy bar;
and (4): and (3) carrying out rotary forging and intermediate aging on the copper-chromium alloy bar with the total strain of 3 +/-0.2, then carrying out rolling with the processing deformation rate of 70 +/-2%, and finally carrying out final aging treatment to obtain the high-strength and high-conductivity copper-chromium intermediate alloy.
Further, in the step (1), the purity of cathode electrolysis pure copper is more than 99.99%, and the purity of chromium is more than 99.5%.
Further, the step (2) is specifically as follows: and (3) heating the solution to 1250-1300 ℃ in the smelting process of the vacuum intermediate frequency induction furnace, preserving heat, smelting for 1-2H, injecting the solution into a graphite cylindrical cast iron ingot mold, and slowly cooling to room temperature to obtain the cast-state rod-shaped copper-chromium intermediate alloy.
Further, the step (3) is specifically as follows: in the method, rod-shaped copper-chromium intermediate alloy is subjected to solution treatment by preserving heat for 2H in a muffle furnace at 1000 +/-20 ℃, and then is subjected to turning processing at room temperature to obtain the rod-shaped copper-chromium alloy.
Further, the specific process of the step (4) is as follows:
step (41): continuously rotary forging the copper-chromium alloy bar until the strain is 2 +/-0.2, then placing the bar in a muffle furnace, heating to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, then preserving heat for 1H, and then cooling to room temperature in the air;
step (42): continuously carrying out rotary swaging on the copper-chromium alloy bar until the strain capacity is 3 +/-0.2;
step (43): rolling a copper-chromium alloy bar with the strain capacity of 3 +/-0.2, wherein the rolling processing deformation rate is 70 +/-2%;
step (44): and (3) placing the rolled copper-chromium alloy in a muffle furnace, heating to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, preserving the heat for 0.5H, and then placing in the air to cool to room temperature.
Further, the swaging of step (42) is specifically:
when the strain is less than 2, the pressing amount of each pass is 0.6-0.8 mm;
when the strain is more than 2 and less than 3, the pressing amount of each pass is 0.6-0.8 mm;
when the strain is 3 +/-0.2, rolling the copper-chromium alloy, and pressing down by 1mm in each pass by 15-20% of pass deformation.
A high-strength high-conductivity CuCr copper intermediate alloy is prepared by the method.
Compared with the prior art, the invention has the remarkable advantages that:
(1) According to the invention, through technical optimization, the rotary forging and rolling processes are organically combined, the uniformity of an alloy grain structure is ensured to the maximum extent, the mechanical property of the material is improved by adding a large amount of chromium into copper, the rotary forging and rolling enable the material to be subjected to multi-dimensional high-speed strain processing, and the original granular chromium in a copper matrix is pulled into a fibrous shape along the same direction by using a proper heat treatment mode, so that the negative influence caused by cutting the copper matrix by excessive chromium in the copper matrix is reduced, the chromium is distributed more uniformly and has more orientation, fine long-strip fibrous shapes are formed, and electrons are more convenient to move in the matrix. The conductivity of the material is improved while the mechanical property is improved; the method can be stably put into industrial production, has high efficiency and yield, and has relatively low cost.
(2) The copper-chromium alloy has high strength and good conductivity, reasonably exerts the strengthening effect of the copper-chromium alloy, keeps the overall conductivity of the material, and can well meet the performance requirements of various industrial environments on the copper-chromium alloy.
(3) The method provided by the invention has the advantages of simple production steps, easiness in operation, suitability for large-scale industrial production, uniform tissue, difficulty in fracture, high cost rate and low cost; therefore, the preparation method of the high-strength high-conductivity copper-chromium alloy has excellent industrial application value and market potential.
Drawings
FIG. 1 is a tensile curve of Cu15Cr prepared in example 1 of the present invention.
FIG. 2 is a TEM image of Cu15Cr final aging prepared in example 1 of the present invention.
FIG. 3 is a final aging SEM image of Cu15Cr prepared in example 1 of the present invention.
FIG. 4 is a Cu15Cr final aging Cu energy spectrum of Cu prepared in example 1 of the present invention.
FIG. 5 is a diagram of the final aging Cr energy spectrum of Cu15Cr prepared in example 1 of the present invention.
Detailed Description
The present invention is described in further detail below with reference to the attached drawing figures.
The invention discloses a high-strength high-conductivity copper-chromium alloy and a preparation method thereof, wherein the high-strength high-conductivity copper-chromium alloy takes electrolytic pure copper and industrial pure with the mass fraction of more than 99.5 percent as raw materials, the common content of copper and chromium is 99.995wt percent, and the weight ratio of Cr:15wt% + -1% and the sum of the contents of oxygen, sulphur and unavoidable impurities does not exceed 10ppm. Smelting by adopting a vacuum intermediate frequency induction furnace, and preparing as-cast copper-chromium alloy in a vacuum environment; and carrying out solution treatment on the as-cast copper-chromium alloy at the temperature of 1000 +/-20 ℃ for 2H. Then turning to obtain a copper-chromium alloy bar; the accumulated strain of the copper-chromium alloy bar is swaged for a plurality of times to reach 2 +/-0.2, the pressing amount is 0.6-0.8 mm each time, and then the intermediate aging is carried out on the bar, and the temperature is kept at 450 +/-20 ℃ for 1H. Continuously carrying out rotary swaging on the copper-chromium alloy bar until the strain capacity is 3 +/-0.2, and the pressing amount is 0.6-0.8 mm each time. And then rolling the alloy for 1mm each time, wherein the deformation of each pass is 15-20%, and the accumulated final deformation is 70% +/-2%, and finally performing final time effect treatment at the temperature of 450 +/-20 ℃ for 30min to obtain the high-strength and high-conductivity copper-chromium intermediate alloy. The copper-chromium intermediate alloy prepared by the method has the advantages of high strength, good conductivity, uniform structure, low cost and the like, has high yield, and can be used in subsequent processing; can meet the requirements of the fields such as high-speed rail wires and the like on high-strength high-conductivity materials.
The invention relates to a preparation method of a high-strength high-conductivity copper-chromium alloy, which comprises the following steps:
step 1: cathode electrolysis pure copper with the purity of more than 99.99 percent is selected and used as a raw material;
in the specific implementation, the raw materials are high-purity cathode electrolytic pure copper and industrial pure chromium with the mass fraction of more than 99.5 percent, and the raw materials are calculated by weight percent: the combined copper and chromium content is 99.995%, the chromium content is 15% + -1%, the oxygen content is less than 5ppm, and no more than 10ppm follows the sulfur, phosphorus and other unavoidable impurities content.
Step 2: smelting by adopting a vacuum intermediate frequency induction furnace, and preparing as-cast copper-chromium alloy in a vacuum environment;
in the specific implementation, the solution is heated to 1250-1300 ℃ in the melting process of the vacuum medium-frequency induction furnace, is subjected to heat preservation melting for 1-2H, and then is injected into a graphite cylindrical cast iron ingot mold and is slowly cooled to room temperature, so that the cast rod-shaped copper-chromium intermediate alloy with the diameter of 40mm +/-0.2 multiplied by 100mm is obtained.
And step 3: carrying out solid solution treatment and turning processing on the as-cast copper-chromium alloy to prepare;
in the specific implementation, the rodlike copper-chromium-copper-chromium intermediate alloy is subjected to solution treatment by maintaining 2H in a muffle furnace at 1000 +/-20 ℃, and then is subjected to turning processing at room temperature to obtain the rodlike copper-chromium alloy with phi of 35mm +/-0.2 multiplied by 100 mm.
And 4, step 4: and (3) performing multiple rotary swaging and intermediate aging on the copper-chromium alloy bar, then rolling the bar, and finally performing final aging treatment to obtain the high-strength and high-conductivity copper-chromium intermediate alloy.
In specific implementation, the continuous multiple rotary swaging, rolling and aging processes are as follows:
step 4.1: continuously rotary forging the copper-chromium alloy bar until the strain is 2 +/-0.2, then placing the bar in a muffle furnace, heating to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, then preserving heat for 1H, and then cooling to room temperature in the air;
step 4.2: and continuously carrying out rotary swaging on the copper-chromium alloy bar until the strain capacity is 3 +/-0.2.
Step 4.3: and (3) rolling the copper-chromium alloy bar with the strain capacity of 3 +/-0.2, wherein the processing deformation rate of rolling is 70 +/-2%.
Step 4.4: and (3) putting the rolled copper-chromium alloy into a muffle furnace, heating to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, preserving heat for 0.5H, and then cooling to room temperature in the air.
The technical solution of the present invention will be described in detail with reference to the following examples, which are provided for illustrative purposes only and do not limit the scope of the present invention. The purity of the metal copper adopted in the embodiment of the invention is 99.99%, and the purity of the chromium is 99.5%. The diameter of the cast ingot is 40mm +/-0.2 cylinder.
Example 1
(1) The copper-chromium alloy comprises the following raw material components in percentage by mass: cu + Cr:99.995%, cr:15% +/-1% and the balance of inevitable impurities, heating to 1300 +/-20 ℃ by using a vacuum intermediate frequency induction furnace, preserving heat, smelting for 1H, pouring into a graphite cylindrical cast iron ingot mold, and cooling and forming to obtain a copper-chromium intermediate alloy cast ingot;
(2) Heating to 1000 +/-20 ℃ by using a muffle furnace, preserving heat for 2H, taking out, immediately putting into water, cooling, carrying out solid solution treatment, turning the material, and turning off defects such as an oxide layer and shrinkage porosity on the surface to obtain a phi 35mm +/-0.2 copper-chromium metal round bar;
(3) Continuously rotary forging the copper-chromium alloy bar until the strain capacity is 2 +/-0.2, and the processing yield is 0.6-0.8 mm to obtain the copper-chromium metal round bar with phi of 12.7 +/-0.2. Then carrying out intermediate aging treatment, placing the mixture into a muffle furnace, keeping the temperature for 1H after the temperature is increased to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, and then cooling the mixture to room temperature in the air;
(4) Continuing to carry out rotary swaging on the aged rod-shaped copper-chromium alloy in the step (3), continuing to carry out continuous rotary swaging on a copper-chromium alloy bar until the strain capacity is 3 +/-0.2 and the processing reduction is 0.6 mm-0.8 mm, and obtaining a copper-chromium metal round bar with phi of 7.5mm +/-0.2
(5) And (3) continuously rolling the rod-shaped copper-chromium alloy with the strain of 3 +/-0.2 in the step (4) in multiple passes, wherein the processing deformation rate of rolling is 70 +/-2%, the deformation of each pass is 15-20%, and the pressing amount of each pass is 1mm, so that the sheet copper-chromium metal with the thickness of 1.5mm is obtained. Finally, the mixture is placed in a muffle furnace for final aging treatment, the temperature is raised to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, the temperature is kept for 0.5H, and then the mixture is placed in the air and cooled to the room temperature.
The mechanical properties and electrical conductivity of the copper-chromium alloy prepared in this example were measured to determine 855MPa for tensile strength and 82.5% IACS for electrical conductivity. Therefore, the present embodiment combines the rotary swaging process and the rolling process, and optimizes the heat treatment mode and the heat treatment parameter process, so that the high-strength and high-conductivity copper-chromium alloy can be prepared.
FIG. 1 is a tensile curve of the copper-chromium alloy of example 1 of the present invention, and it can be seen from FIG. 1 that the yield strength reaches 810MPa, the tensile strength is 855MPa, and the uniform elongation is 7%; FIG. 2 is a TEM photograph of the final aging of the Cu-Cr alloy of example 1, wherein it can be seen from the second photograph that a large amount of Cr is precipitated on the surface of the Cu matrix and a large amount of Cr is precipitated at the grain boundary of the Cu crystal, so as to effectively prevent the sliding of the Cu grain boundary and effectively improve the strength of the material; FIG. 3 is a SEM-EDS photograph showing the final aging of the copper-chromium alloy of example 1 of the present invention, and from FIG. 3, it can be seen that Cr is drawn into a fibrous form and the degree of cleavage of the copper matrix is smaller than that in the case of the granular form. After rotary swaging and rolling, cr has the original disordered orientation and is changed into the same orientation, and the conductivity of the alloy is improved due to the movement of electrons and the alternating uniform distribution and distribution of Cu and Cr.
Example 2
(1) The copper-chromium alloy comprises the following raw material components in percentage by mass: cu + Cr:99.995%, cr:15% +/-1% and the balance of inevitable impurities, heating to 1300 +/-20 ℃ by using a vacuum intermediate frequency induction furnace, preserving heat, smelting for 1H, pouring into a graphite cylindrical cast iron ingot mold, and cooling and forming to obtain a copper-chromium intermediate alloy cast ingot;
(2) Heating to 1000 +/-20 ℃ by using a muffle furnace, preserving heat for 2H, taking out, immediately putting into water, cooling, performing solid solution treatment, turning the material, and removing defects such as an oxide layer, shrinkage porosity and the like on the surface to obtain a phi 35mm +/-0.2 copper-chromium metal round bar;
(3) Continuously rotary forging the copper-chromium alloy bar until the strain capacity is 2 +/-0.2, and obtaining the copper-chromium metal round bar with phi of 12.7 +/-0.2, wherein the processing yield is 0.6-0.8 mm. Then carrying out intermediate aging treatment, placing the mixture into a muffle furnace, keeping the temperature for 1H after the temperature is increased to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, and then cooling the mixture to room temperature in the air;
(4) Continuing to carry out rotary swaging on the aged rod-shaped copper-chromium alloy in the step (3), continuing to carry out continuous rotary swaging on a copper-chromium alloy bar until the strain capacity is 3 +/-0.2 and the processing reduction is 0.6-0.8 mm, and obtaining a copper-chromium metal round bar with phi of 7.5 +/-0.2
(5) And (3) continuously rolling the rod-shaped copper-chromium alloy with the strain of 3 +/-0.2 in the step (4) in multiple passes, wherein the processing deformation rate of the rolling is 70 +/-2%, the deformation of each pass is 15-20%, and the pressing amount of each pass is 1mm, so that the sheet-shaped copper-chromium metal with the thickness of 1.5mm +/-0.2 is obtained. Finally, the mixture is put into a muffle furnace for final aging treatment, heated to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, kept for 0.5H, and then placed in the air for cooling to room temperature.
The mechanical properties and electrical conductivity of the Cu-Cr alloy prepared in this example were measured, and the tensile strength of the Cu-Cr alloy prepared in this example was 875MPa, and the electrical conductivity was 76.5% IACS. Therefore, the present embodiment combines the rotary swaging process and the rolling process, and optimizes the heat treatment mode and the heat treatment parameter process, so that the high-strength and high-conductivity copper-chromium alloy can be prepared.
The above description is only a preferred embodiment of the invention, and should not be taken as limiting the scope of the invention, which is defined by the appended claims. Are intended to be encompassed by the present invention.
Claims (7)
1. A preparation method of a high-strength high-conductivity CuCr copper intermediate alloy is characterized by comprising the following steps:
step (1): selecting cathode electrolytic pure copper and chromium as raw materials, wherein the mass percent of the chromium is 15wt% +/-1%;
step (2): smelting by adopting a vacuum intermediate frequency induction furnace, and preparing as-cast copper-chromium alloy in a vacuum environment;
and (3): carrying out solid solution treatment and turning on the as-cast copper-chromium alloy to prepare a copper-chromium alloy bar;
and (4): and (3) carrying out rotary forging and intermediate aging on the copper-chromium alloy bar with the total strain of 3 +/-0.2, then carrying out rolling with the processing deformation rate of 70 +/-2%, and finally carrying out final aging treatment to obtain the high-strength and high-conductivity copper-chromium intermediate alloy.
2. The method of claim 1, wherein the purity of the cathode electrolyzed pure copper in step (1) is greater than 99.99%, and the purity of the chromium is greater than 99.5%.
3. The method according to claim 2, wherein step (2) is specifically: and (3) heating the solution to 1250-1300 ℃ in the smelting process of the vacuum intermediate frequency induction furnace, preserving heat, smelting for 1-2H, injecting the solution into a graphite cylindrical cast iron ingot mold, and slowly cooling to room temperature to obtain the cast-state rod-shaped copper-chromium intermediate alloy.
4. The method according to claim 3, wherein step (3) is specifically: in the method, rod-shaped copper-chromium intermediate alloy is subjected to solution treatment by preserving heat in a muffle furnace at 1000 +/-20 ℃ and then subjected to turning processing at room temperature to obtain the rod-shaped copper-chromium alloy.
5. The method according to claim 4, wherein the step (4) comprises the following specific steps:
step (41): continuously rotary forging the copper-chromium alloy bar until the strain is 2 +/-0.2, then placing the bar in a muffle furnace, heating to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, then preserving heat for 1H, and then cooling to room temperature in the air;
step (42): continuously carrying out rotary swaging on the copper-chromium alloy bar until the strain capacity is 3 +/-0.2;
step (43): rolling a copper-chromium alloy bar with the strain capacity of 3 +/-0.2, wherein the rolling processing deformation rate is 70 +/-2%;
step (44): and (3) placing the rolled copper-chromium alloy in a muffle furnace, heating to 450 +/-20 ℃ at the heating rate of 8-10 ℃/min, preserving the heat for 0.5H, and then placing in the air to cool to room temperature.
6. The method according to claim 5, characterized in that the swaging of step (42) is in particular:
when the strain is less than 2, the pressing amount of each pass is 0.6-0.8 mm;
when the strain is 2< 3, the pressing amount of each pass is 0.6-0.8 mm;
when the strain is 3 +/-0.2, rolling the copper-chromium alloy, and pressing down by 1mm in each pass by 15-20% of pass deformation.
7. A high strength and high conductivity CuCr copper master alloy, characterized in that it is produced by the method according to any one of claims 1 to 6.
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| CN107739878A (en) * | 2017-11-23 | 2018-02-27 | 全南晶环科技有限责任公司 | A kind of anti-softening copper alloy of high-strength highly-conductive and preparation method thereof |
| CN108060323A (en) * | 2017-12-15 | 2018-05-22 | 西北有色金属研究院 | A kind of high-strength highly-conductive CuCrZrMg series copper alloy silk materials and preparation method thereof |
| CN113564408A (en) * | 2021-07-29 | 2021-10-29 | 内蒙古工业大学 | High-strength high-conductivity rare earth copper alloy Cu-Cr-Zr-Y and preparation method thereof |
| CN113699397A (en) * | 2021-08-06 | 2021-11-26 | 中国兵器科学研究院宁波分院 | Preparation process of copper alloy material for short-process lead frame |
| CN114645153A (en) * | 2022-03-17 | 2022-06-21 | 东北大学 | High-strength high-conductivity copper-silver alloy wire and preparation method thereof |
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