CN110835699A - High-strength high-conductivity copper-chromium-zirconium alloy material and preparation method thereof - Google Patents
High-strength high-conductivity copper-chromium-zirconium alloy material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a high-strength high-conductivity copper chromium zirconium series alloy material and a preparation method thereof. The material comprises the following components in percentage by weight: 0.5-1.5% of Cr0.05-0.3% of Zr0.05-0.3%, 0.02-0.1% of Mg0.005-0.01% of Si, 0.002-0.005% of Fe0.002% of Cu, and the balance of Cu, and in addition, the alloy also comprises two of Ti, La, B and Ca, the content of each element is 0.001-0.005%, and the total content of alloy elements is 0.005-0.01%. The material is prepared by smelting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling and aging treatment. The high-strength high-conductivity copper-chromium-zirconium alloy material has the tensile strength of 500-800 MPa, the yield strength of 350-700 MPa, the elongation of 3-10%, the conductivity of 75-90% IACS, the softening temperature of 500-600 ℃, the stress relaxation rate of 1000h at 150 ℃ of less than 10%, and no cracks at 90-degree and 180-degree bending when the R/t of the transverse and longitudinal sections is less than or equal to 1.5. Completely meets the use requirement of the high-end electronic component precision plug-in terminal on the copper alloy material.
Description
Technical Field
The invention relates to a high-strength high-conductivity copper chromium zirconium series alloy material and a preparation method thereof, belonging to the field of nonferrous metal processing.
Background
The high-performance copper alloy is an important industrial base material, is widely applied to core devices of industrial equipment such as integrated circuits, traffic equipment, aerospace, new energy, electric power, electronic communication, intelligent household appliances and the like, and is mainly applied to lead frames of ultra-large scale integrated circuits in the electronic information industry, USB Type-c interfaces, electric connectors of new energy automobiles, high-current connectors for electronic equipment, overhead wires for high-speed rail transit, conductors for electronic countermeasure radars and high-pulse magnetic fields, rotor wires of large-sized high-speed turbine generators, resistance welding electrodes for the industry of new energy automobiles, electro-vacuum devices, switch contact bridges for electrical engineering and other functional conductor devices. With the continuous development of high and new technologies, miniaturization, high load, high reliability, long service life and environmental protection have become the main development directions of conductor functional devices, which makes the service conditions of copper alloy materials more rigorous, and not only requires higher strength and conductivity, but also requires excellent softening resistance and bending resistance.
Compared with the copper alloy brass, tin-phosphor bronze and C70250 alloy for the current electric connector, the copper-chromium-zirconium alloy has higher conductivity and excellent high-temperature and stress relaxation resistance, and is an ideal material for high-performance copper alloy materials in the fields of high-speed transmission standardized ports of new-generation intelligent terminals, high-voltage and large-current connectors of new energy automobiles, 5G base stations and the like. However, Cr and Zr are easy to oxidize in a non-vacuum environment, and the use of alloy materials is influenced because the components of cast ingots are easy to be uneven in the industrial production process of large-tonnage non-vacuum environments, so that the demand of high-end copper chromium zirconium products in China at present mainly depends on developed countries such as imported Japan, Germany and the like.
The patent mainly provides a high-strength high-conductivity copper-chromium-zirconium alloy material and a heat treatment technology for solving the problems of smelting and casting of the alloy in a non-vacuum environment and subsequent processing of the alloy, and obtains the high-performance copper alloy material and a preparation method thereof.
Disclosure of Invention
The invention mainly aims to make up the performance deficiency of the existing copper alloy and develop a high-strength high-conductivity copper chromium zirconium alloy material and a preparation method thereof.
A high-strength high-conductivity copper chromium zirconium series alloy material comprises the following components in percentage by weight: 0.5-1.5% of Cr0.05-0.3% of Zr0.05-0.3%, 0.02-0.1% of Mg, 0.005-0.01% of Si, 0.002-0.005% of Fe0.002% of Cu, and the balance of Cu, wherein the alloy also comprises two of Ti, La, B and Ca, the content of each element is 0.001-0.005%, and the total content of alloy elements is 0.005-0.01%. The average grain size of the copper alloy material is 5-10 mu m, the standard deviation of the grain size satisfies the condition that the sigma is less than 1.0 mu m, and the number density of large-grain-size Cr phases with the grain size of 2-10 mu m can be observed on the transverse and longitudinal sections of the copper alloy material and is 1 multiplied by 1012～5×1015m-3It was observed that the number density of Cr precipitate phases having a particle diameter of 2 to 10nm was 1X 1023～5×1024m-3Alloy S {123}<634>Texture accounts for 15-25%, and Brass {011}<211>Texture accounts for 5-15%, and Cu {112}<111>Textured panel15-30% and Cube {001}<100>30-50% of texture, 500-800 MPa of tensile strength, 350-700 MPa of yield strength, 3-10% of elongation and 75-90% of electrical conductivity IACS of the alloy, 500-600 ℃ of softening temperature, less than 10% of stress relaxation rate for 1000h at 150 ℃, and no crack appears when R/t of the transverse and longitudinal sections is less than or equal to 1.5 at 90-degree and 180-degree bending.
The function of the added alloy elements is as follows:
chromium: the chromium element is mainly separated out as simple substance chromium in the aging process, and the strength and the conductivity of the alloy are improved. Because the maximum solubility of chromium element in copper is 0.75%, redundant Cr can be enriched in grain boundary, the occurrence of recrystallization process is effectively inhibited, and the crystal grain of the alloy can be obviously refined.
Zirconium: according to a copper-zirconium binary phase diagram, a zirconium element can be combined with copper in an aging process to form a copper-zirconium precipitated phase, so that the strength and the conductivity of the alloy are improved, the zirconium content is usually 0.05-0.3%, and the method mainly has the effects of promoting the precipitation of a simple substance chromium phase, inhibiting the growth of the simple substance chromium phase and improving the high-temperature stability of the alloy.
Magnesium, iron and silicon: the addition of the three elements mainly generates a synergistic effect with the chromium-rich phase, so that the comprehensive performance of the alloy is improved. The three alloy elements are added into the pure copper alloy to play a solid solution role, but the addition of the three alloy elements into the Cu-Cr-Zr alloy can inhibit the growth of a chromium-rich phase and obviously improve the softening resistance and the stress relaxation resistance of the alloy.
Titanium, lanthanum, boron, calcium: the addition of the four elements mainly has a synergistic effect with the Zr-rich phase, can promote the precipitation of the Zr-rich phase and inhibit the growth of the Zr-rich phase, obviously improves the influence degree of the Zr-rich phase on the alloy structure performance, and improves the bending forming performance of the alloy.
The invention also aims to provide a preparation and processing method of the high-strength high-conductivity copper chromium zirconium series alloy material.
A preparation method of a high-strength high-conductivity copper chromium zirconium series alloy material comprises the following steps: a. the method comprises the following steps of proportioning, feeding, smelting and casting according to mass percent, b, hot rolling, c, milling surface, d, rough rolling, e, intermediate annealing treatment, f, intermediate rolling, g, high-temperature rapid solid solution treatment, h, finish rolling and i, aging treatment.
In the step a, a non-vacuum intermediate frequency induction furnace is adopted for casting, the smelting temperature is 1300-1350 ℃, and the casting temperature is controlled to be 1225-1275 ℃.
Adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, continuously adding two of copper-chromium intermediate alloy, copper-magnesium intermediate alloy and copper-boron intermediate alloy, copper-lanthanum intermediate alloy, sponge titanium and copper-calcium intermediate alloy after the materials are melted, raising the temperature to 1300-1350 ℃, pouring the melt into a heat preservation furnace after the melt is completely melted, uniformly stirring, adding copper-zirconium intermediate alloy with the content consistent with the designed content, subsequently supplementing the melt into the heat preservation furnace with 0.02-0.1kg of copper-zirconium intermediate alloy per minute, controlling the casting temperature at 1225-1275 ℃, preserving the heat for 10min, and then casting.
And b, heating the alloy ingot in a stepping box type furnace at 850-920 ℃ for 2-6 h, then carrying out hot rolling, controlling the final rolling temperature at 750-800 ℃, and then carrying out water cooling.
And d, performing rough rolling on the alloy plate after surface milling, wherein the cold rolling processing rate is 85-95%.
And step e, placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 500-600 ℃, the heat preservation time is 6-10 h, and the cooling mode is a mixed gas of hydrogen and nitrogen.
And f, carrying out medium rolling on the alloy plate subjected to annealing treatment, wherein the cold rolling processing rate is 60-80%.
And step g, carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 920-1020 ℃, the annealing speed is 10-20 m/min, the cooling speed is 60-80 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
And h, performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling processing rate is 20-60%.
And in the step i, placing the cold-rolled sheet in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 400-600 ℃, the heat preservation time is 1-6 h, and the cooling mode is mixed gas of hydrogen and nitrogen.
The invention has the advantages that: the invention designs and optimizes the components of the copper alloy and regulates and controls the microstructure through thermodynamic software, high-temperature rapid solid solution treatment and corresponding aging matching treatment technology, so as to obtain the high-strength high-conductivity copper chromium zirconium series alloy material with fine and uniform structure and dispersed distribution of precipitated phases, wherein the material comprises the following components in percentage by weight: 0.5-1.5% of Cr, 0.05-0.3% of ZrC, 0.02-0.1% of Mg, 0.005-0.01% of Si, 0.002-0.005% of Fe0.002, and the balance of Cu, and in addition, the alloy also comprises two of Ti, La, B and Ca, the content of each element is 0.001-0.005%, and the total content of alloy elements is 0.005-0.01%. The average grain size of the copper alloy material is 5-10 mu m, the standard deviation of the grain size satisfies the condition that the sigma is less than 1.0 mu m, and the number density of large-grain-size Cr phases with the grain size of 2-10 mu m can be observed on the transverse and longitudinal sections of the copper alloy material and is 1 multiplied by 1012～5×1015m-3It was observed that the number density of Cr precipitate phases having a particle diameter of 2 to 10nm was 1X 1023～5×1024m-3Alloy S {123}<634>Texture accounts for 15-25%, and Brass {011}<211>Texture accounts for 5-15%, and Cu {112}<111>Texture accounts for 15-30% and Cube {001}<100>And 30-50% of texture. The material is prepared by smelting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling and aging treatment. The high-strength high-conductivity copper-chromium-zirconium alloy material has the tensile strength of 500-800 MPa, the yield strength of 350-700 MPa, the elongation of 3-10%, the conductivity of 75-90% IACS, the softening temperature of 500-600 ℃, the stress relaxation rate of 1000h at 150 ℃ of less than 10%, and no cracks at 90-degree and 180-degree bending when the R/t of the transverse and longitudinal sections is less than or equal to 1.5. Completely meets the use requirement of the high-end electronic component precision plug-in terminal on the copper alloy material.
The present invention is further illustrated by the following specific embodiments, which are not meant to limit the scope of the invention.
Detailed Description
The high-strength high-conductivity copper-chromium-zirconium alloy material containsThe material comprises the following chemical components in percentage by weight: 0.5-1.5% of Cr, 0.05-0.3% of Zr, 0.02-0.1% of Mg, 0.005-0.01% of Si, 0.002-0.005% of Fe, and the balance of Cu, and in addition, the alloy also at least comprises two of Ti, La, B and Ca, the content of each element is 0.001-0.005%, and the total content of alloy elements is 0.005-0.01%. The average grain size of the copper alloy material is 5-10 mu m, the standard deviation of the grain size satisfies the condition that the sigma is less than 1.0 mu m, and the number density of large-grain-size Cr phases with the grain size of 2-10 mu m can be observed on the transverse and longitudinal sections of the copper alloy material and is 1 multiplied by 1012～5×1015m-3It was observed that the number density of Cr precipitate phases having a particle diameter of 2 to 10nm was 1X 1023～5×1024m-3Alloy S {123}<634>Texture accounts for 15-25%, and Brass {011}<211>Texture accounts for 5-15%, and Cu {112}<111>Texture accounts for 15-30% and Cube {001}<100>And 30-50% of texture.
The preparation and processing method of the high-strength high-conductivity copper-chromium-zirconium alloy material comprises the following process flows of: a. the method comprises the following steps of proportioning, feeding, smelting and casting according to mass percent, b, hot rolling, c, milling surface, d, rough rolling, e, intermediate annealing treatment, f, intermediate rolling, g, high-temperature rapid solid solution treatment, h, finish rolling and i, aging treatment. Wherein, the specific feeding sequence is as follows: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding one or two of copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-boron intermediate alloy, copper-lanthanum intermediate alloy, sponge titanium and copper-calcium intermediate alloy, raising the temperature to 1300-1350 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniformly stirring, then adding copper-zirconium intermediate alloy with the content consistent with the designed content, subsequently feeding 0.02-0.1kg of copper-zirconium intermediate alloy into the heat preservation furnace per minute, controlling the casting temperature to 1225-1275 ℃, preserving heat for 10min, and then casting; the hot rolling temperature is 850-920 ℃, the heat preservation time is 2-6 h, and the final rolling temperature is controlled at 750-800 ℃; the machining rate of rough rolling is 85-95%; the annealing temperature is 500-600 ℃, the heat preservation time is 6-10 h, and the cooling mode is a mixed gas of hydrogen and nitrogen. The processing rate of the medium rolling is 60-80%; performing high-temperature rapid solution treatment, wherein the solution treatment temperature is 920-1020 ℃, the annealing speed is 10-20 m/min, the cooling speed is 60-80 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen; the finish rolling processing rate is 20-60%; the aging temperature is 400-600 ℃, the heat preservation time is 1-6 h, and the cooling mode is a mixed gas of hydrogen and nitrogen.
Example 1
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, copper-chromium intermediate alloy, copper-zirconium intermediate alloy, copper-magnesium intermediate alloy, copper-iron intermediate alloy, copper-silicon intermediate alloy, titanium sponge and copper-boron intermediate alloy. The composition of the alloy is shown in table 1, example 1.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-boron intermediate alloy and titanium sponge, raising the temperature to 1300 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently feeding 0.02kg of copper-zirconium intermediate alloy into the heat preservation furnace per minute, controlling the casting temperature at 1225 ℃, preserving the temperature for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 920 ℃ for 2h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 85%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 500 ℃, the heat preservation time is 6 hours, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 60%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 920 ℃, the annealing speed is 20m/min, the cooling speed is 60 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 20%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 400 ℃, the heat preservation time is 6h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties are shown in table 2 and table 3 of example 1.
Example 2
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, copper-chromium intermediate alloy, copper-zirconium intermediate alloy, copper-magnesium intermediate alloy, copper-iron intermediate alloy, copper-silicon intermediate alloy, titanium sponge and copper-boron intermediate alloy. The composition of the alloy is shown in table 1, example 2.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-boron intermediate alloy and sponge titanium, raising the temperature to 1350 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently adding 0.1kg of copper-zirconium intermediate alloy material into the heat preservation furnace per minute, controlling the casting temperature to 1275 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 850 ℃ for 6h, then carrying out hot rolling, controlling the final rolling temperature at 750 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 95%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 600 ℃, the heat preservation time is 10 hours, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 80%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 1020 ℃, the annealing speed is 10m/min, the cooling speed is 80 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 60%.
8. Aging treatment: and placing the cold-rolled sheet in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 600 ℃, the heat preservation time is 1h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties are shown in table 2 and table 3 of example 2.
Example 3
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, a copper-chromium intermediate alloy, a copper-zirconium intermediate alloy, a copper-magnesium intermediate alloy, a copper-iron intermediate alloy, a copper-silicon intermediate alloy, a copper-lanthanum intermediate alloy and a copper-boron intermediate alloy. The composition of the alloy is shown in table 1, example 3.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-boron intermediate alloy and copper-lanthanum intermediate alloy, raising the temperature to 1320 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently feeding the copper-zirconium intermediate alloy into the heat preservation furnace by 0.08kg per minute, controlling the casting temperature at 1250 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 880 ℃ for 4h, then carrying out hot rolling, controlling the final rolling temperature at 775 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 90%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 550 ℃, the heat preservation time is 8h, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 70%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 950 ℃, the annealing speed is 15m/min, the cooling speed is 70 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 40%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 500 ℃, the heat preservation time is 4h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and example 3 in table 3.
Example 4
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, a copper-chromium intermediate alloy, a copper-zirconium intermediate alloy, a copper-magnesium intermediate alloy, a copper-iron intermediate alloy, a copper-silicon intermediate alloy, a copper-lanthanum intermediate alloy and a copper-boron intermediate alloy. The composition of the alloy is shown in table 1, example 4.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-boron intermediate alloy and copper-lanthanum intermediate alloy, raising the temperature to 1330 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently feeding 0.06kg of copper-zirconium intermediate alloy into the heat preservation furnace per minute, controlling the casting temperature at 1235 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 870 ℃ for 3h, then carrying out hot rolling, controlling the final rolling temperature at 780 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 90%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 575 ℃, the heat preservation time is 7h, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate subjected to annealing treatment, wherein the cold rolling processing rate is 75%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 975 ℃, the annealing speed is 15m/min, the cooling speed is 65 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 30%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 550 ℃, the heat preservation time is 3h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and example 4 in table 3.
Example 5
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, copper-chromium intermediate alloy, copper-zirconium intermediate alloy, copper-magnesium intermediate alloy, copper-iron intermediate alloy, copper-silicon intermediate alloy, sponge titanium and copper-calcium intermediate alloy. The composition of the alloy is shown in table 1, example 5.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, sponge titanium and copper-calcium intermediate alloy, raising the temperature to 1320 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently feeding 0.04kg of copper-zirconium intermediate alloy into the heat preservation furnace per minute, controlling the casting temperature at 1235 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 870 ℃ for 4h, then carrying out hot rolling, controlling the final rolling temperature at 780 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 90%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 575 ℃, the heat preservation time is 8h, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 70%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 975 ℃, the annealing speed is 10m/min, the cooling speed is 70 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 50%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 500 ℃, the heat preservation time is 4h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and table 3 of example 5.
Example 6
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, copper-chromium intermediate alloy, copper-zirconium intermediate alloy, copper-magnesium intermediate alloy, copper-iron intermediate alloy, copper-silicon intermediate alloy, sponge titanium and copper-calcium intermediate alloy. The composition of the alloy is shown in table 1, example 6.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, sponge titanium and copper-calcium intermediate alloy, raising the temperature to 1320 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently feeding 0.06kg of copper-zirconium intermediate alloy into the heat preservation furnace per minute, controlling the casting temperature to 1275 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 850 ℃ for 4h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 90%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 500 ℃, the heat preservation time is 10 hours, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 60%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 975 ℃, the annealing speed is 15m/min, the cooling speed is 80 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 40%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 400 ℃, the heat preservation time is 6h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and table 3 of example 6.
Example 7
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, a copper-chromium intermediate alloy, a copper-zirconium intermediate alloy, a copper-magnesium intermediate alloy, a copper-iron intermediate alloy, a copper-silicon intermediate alloy, a copper-lanthanum intermediate alloy and a copper-calcium intermediate alloy. The composition of the alloy is shown in table 1, example 7.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-lanthanum intermediate alloy and copper-calcium intermediate alloy, raising the temperature to 1300 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently supplementing the copper-zirconium intermediate alloy into the heat preservation furnace by 0.06kg of copper-zirconium intermediate alloy per minute, controlling the casting temperature to 1275 ℃, preserving the temperature for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 875 ℃ for 6h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 85%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 500 ℃, the heat preservation time is 8 hours, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 70%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 950 ℃, the annealing speed is 15m/min, the cooling speed is 60 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 50%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 500 ℃, the heat preservation time is 6h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and table 3 of example 7.
Example 8
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, a copper-chromium intermediate alloy, a copper-zirconium intermediate alloy, a copper-magnesium intermediate alloy, a copper-iron intermediate alloy, a copper-silicon intermediate alloy, a copper-lanthanum intermediate alloy and a copper-calcium intermediate alloy. The composition of the alloy is shown in table 1, example 8.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-lanthanum intermediate alloy and copper-calcium intermediate alloy, raising the temperature to 1350 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently supplementing the copper-zirconium intermediate alloy into the heat preservation furnace by 0.05kg per minute, controlling the casting temperature to 1275 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 850 ℃ for 6h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 95%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 550 ℃, the heat preservation time is 8h, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 70%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 950 ℃, the annealing speed is 20m/min, the cooling speed is 60 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 40%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 500 ℃, the heat preservation time is 4h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and table 3 of example 8.
Example 9
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, a copper-chromium intermediate alloy, a copper-zirconium intermediate alloy, a copper-magnesium intermediate alloy, a copper-iron intermediate alloy, a copper-silicon intermediate alloy, a copper-lanthanum intermediate alloy and a copper-boron intermediate alloy. The composition of the alloy is shown in table 1, example 9.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, copper-lanthanum intermediate alloy and copper-boron intermediate alloy, raising the temperature to 1300 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently feeding the copper-zirconium intermediate alloy into the heat preservation furnace by 0.04kg per minute, controlling the casting temperature at 1250 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 900 ℃ for 5h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 95%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 550 ℃, the heat preservation time is 6 hours, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 60%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 950 ℃, the annealing speed is 20m/min, the cooling speed is 70 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 50%.
8. Aging treatment: and placing the cold-rolled plate in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 550 ℃, the heat preservation time is 5 hours, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and table 3 of example 9.
Example 10
The alloy of the invention is smelted by adopting the following raw materials: electrolytic copper, copper-chromium intermediate alloy, copper-zirconium intermediate alloy, copper-magnesium intermediate alloy, copper-iron intermediate alloy, copper-silicon intermediate alloy, sponge titanium and copper-calcium intermediate alloy. The composition of the alloy is shown in Table 1, example 10.
1. Smelting: before smelting, adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, after the materials are molten, continuously adding copper-chromium intermediate alloy, copper-magnesium intermediate alloy, sponge titanium and copper-calcium intermediate alloy, raising the temperature to 1320 ℃, after the melt is completely molten, pouring the melt into a heat preservation furnace for uniform stirring, then adding copper-zirconium intermediate alloy, wherein the content of the copper-zirconium intermediate alloy is consistent with the designed content, subsequently adding 0.05kg of copper-zirconium intermediate alloy material into the heat preservation furnace per minute, controlling the casting temperature at 1250 ℃, preserving the heat for 10min, and then casting.
2. Hot rolling: heating the alloy cast ingot in a stepping box type furnace at 920 ℃ for 4h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Rough rolling: and (4) roughly rolling the alloy plate after surface milling, wherein the cold rolling processing rate is 85%.
4. Intermediate annealing treatment: and (3) placing the cold-rolled sheet in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 550 ℃, the heat preservation time is 8h, and the cooling mode is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy plate after annealing treatment, wherein the cold rolling processing rate is 70%.
6. High-temperature rapid solution treatment: and (3) carrying out high-temperature rapid solution treatment on the cold-rolled alloy plate, wherein the solution treatment temperature is 970 ℃, the annealing speed is 10m/min, the cooling speed is 70 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy strip subjected to the solution treatment, wherein the cold rolling reduction rate is 50%.
8. Aging treatment: and placing the cold-rolled sheet in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 450 ℃, the heat preservation time is 5h, and the cooling mode is mixed gas of hydrogen and nitrogen.
After the above-described processing treatments of melting and casting, hot rolling, surface milling, rough rolling, intermediate annealing, intermediate rolling, high-temperature rapid solution treatment, finish rolling, aging treatment, etc., the structure and properties thereof are shown in table 2 and table 3 of example 10.
TABLE 1 alloy composition recipes (wt%) for examples 1-10
TABLE 2 microstructure morphology of alloys of examples 1-10
Remarking: (1) n is a radical of(2μm～10μm): the number density of Cr phases with the grain diameter of 2-10 mu m;
(2)N(2nm～10nm): the number density of Cr phases with the grain diameter of 2 nm-10 nm;
TABLE 3 alloy Properties of examples 1-10
Claims (12)
1. A high-strength high-conductivity copper chromium zirconium series alloy material is characterized in that: the material comprises the following components in percentage by weight: 0.5-1.5% of Cr, 0.05-0.3% of ZrC, 0.02-0.1% of Mg, 0.005-0.01% of Si, 0.002-0.005% of Fe0.002, and the balance of Cu, and in addition, the alloy also comprises two of Ti, La, B and Ca, the content of each element is 0.001-0.005%, and the total content of alloy elements is 0.005-0.01%.
2. The alloy of claim 1, wherein the average grain size is 5 μm to 10 μm, the standard deviation of the grain sizes is σ of less than 1.0. mu.m, and the number density of Cr phases having a large grain size of 2 μm to 10 μm in a transverse and longitudinal cross section of the copper alloy material is 1X 1012～5×1015m-3It was observed that the number density of Cr precipitate phases having a particle diameter of 2 to 10nm was 1X 1023～5×1024m-3Alloy S {123}<634>Texture accounts for 15-25%, and Brass {011}<211>Texture accounts for 5-15%, and Cu {112}<111>Texture accounts for 15-30% and Cube {001}<100>And 30-50% of texture.
3. The preparation method of the high-strength high-elasticity copper-nickel-silicon alloy material as claimed in claim 1, comprising the following steps: a. the method comprises the following steps of proportioning, feeding, smelting and casting according to mass percent, b, hot rolling, c, milling surface, d, rough rolling, e, intermediate annealing treatment, f, intermediate rolling, g, high-temperature rapid solid solution treatment, h, finish rolling and i, aging treatment.
4. The preparation method of the high-strength high-conductivity copper chromium zirconium series alloy material according to claim 3, characterized in that: and (2) casting by using a non-vacuum intermediate frequency induction furnace, wherein the smelting temperature is 1300-1350 ℃, and the casting temperature is controlled at 1225-1275 ℃.
5. The preparation method of the high-strength high-conductivity copper chromium zirconium series alloy material according to claim 3, characterized in that: adding electrolytic copper, copper-silicon intermediate alloy and copper-iron intermediate alloy into a non-vacuum induction furnace, continuously adding two of copper-chromium intermediate alloy, copper-magnesium intermediate alloy and copper-boron intermediate alloy, copper-lanthanum intermediate alloy, sponge titanium and copper-calcium intermediate alloy after the materials are melted, raising the temperature to 1300-1350 ℃, pouring the melt into a heat preservation furnace after the melt is completely melted, uniformly stirring, adding copper-zirconium intermediate alloy with the content consistent with the designed content, subsequently supplementing the melt into the heat preservation furnace with 0.02-0.1kg of copper-zirconium intermediate alloy per minute, controlling the casting temperature at 1225-1275 ℃, preserving the heat for 10min, and then casting.
6. The preparation method of the high-strength high-conductivity copper chromium zirconium series alloy material according to claim 3, characterized in that: the hot rolling temperature is 850-920 ℃, the heat preservation time is 2-6 h, then the hot rolling is carried out, the final rolling temperature is controlled at 750-800 ℃, and then the water cooling is carried out.
7. The preparation method of the high-strength high-conductivity copper chromium zirconium series alloy material according to claim 3, characterized in that: the primary cold rolling reduction rate is 85-95%.
8. The preparation method of the high-strength high-conductivity copper chromium zirconium series alloy material according to claim 3, characterized in that: the intermediate annealing treatment temperature is 500-600 ℃, the heat preservation time is 6-10 hours, and the cooling mode is a mixed gas of hydrogen and nitrogen.
9. The preparation method of the high-strength high-conductivity copper chromium zirconium series alloy material according to claim 3, characterized in that: the secondary cold rolling reduction rate is 60-80%.
10. The preparation method of the high-strength high-conductivity copper chromium zirconium series alloy material according to claim 3, characterized in that: the high-temperature rapid continuous solution treatment temperature is 920-1020 ℃, the annealing speed is 10-20 m/min, the cooling speed is 60-80 ℃/s, and the cooling mode is a mixed gas of nitrogen and hydrogen.
11. The preparation method of the high-strength high-conductivity copper chromium zirconium alloy material according to claim 3, wherein the alloy strip subjected to the solution treatment is subjected to finish rolling, and the cold rolling reduction rate is 20-60%.
12. The preparation method of the high-strength high-elasticity copper-nickel-silicon alloy material according to claim 3 is characterized in that: the aging treatment temperature is 400-600 ℃, and the heat preservation time is 1-6 h.
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| CN115404327A (en) * | 2022-09-21 | 2022-11-29 | 中色奥博特铜铝业有限公司 | Short-process processing method and application of copper-chromium-zirconium alloy plate strip |
| CN116970839A (en) * | 2023-09-19 | 2023-10-31 | 宁波兴业盛泰集团有限公司 | Copper-chromium alloy material and preparation method thereof |
| CN116970839B (en) * | 2023-09-19 | 2023-12-19 | 宁波兴业盛泰集团有限公司 | Copper-chromium alloy material and preparation method thereof |
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