CN112111671A - Environment-friendly conductive elastic copper alloy, preparation method thereof and application thereof in connector - Google Patents
Environment-friendly conductive elastic copper alloy, preparation method thereof and application thereof in connector Download PDFInfo
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- CN112111671A CN112111671A CN202010979294.2A CN202010979294A CN112111671A CN 112111671 A CN112111671 A CN 112111671A CN 202010979294 A CN202010979294 A CN 202010979294A CN 112111671 A CN112111671 A CN 112111671A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
- C22C9/06—Alloys based on copper with nickel or cobalt as the next major constituent
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/02—Making non-ferrous alloys by melting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/02—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working in inert or controlled atmosphere or vacuum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22F—CHANGING THE PHYSICAL STRUCTURE OF NON-FERROUS METALS AND NON-FERROUS ALLOYS
- C22F1/00—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working
- C22F1/08—Changing the physical structure of non-ferrous metals or alloys by heat treatment or by hot or cold working of copper or alloys based thereon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/026—Alloys based on copper
Abstract
The invention belongs to the technical field of nonferrous metal processing, and provides an environment-friendly conductive elastic copper alloy and a preparation method and application thereof. The copper alloy provided by the invention comprises the following chemical components in percentage by weight: 2.0-4.3% of Ni, 0.5-0.85% of Si, 0.05-0.4% of Mn, 0.01-0.2% of Mg0.01-1.0% of rare earth elements and the balance of Cu. The copper alloy provided by the invention has ultrahigh strength, can keep high conductivity, has the characteristics of high temperature resistance, stress relaxation resistance, complex environment corrosion resistance and high elasticity, has excellent forming performance and high reliability, can meet the use requirements of connectors in different application scenes, and is a new generation of alloy material for connectors. The copper alloy is prepared by smelting, casting, hot rolling, blooming, intermediate annealing, intermediate rolling, rapid solid solution treatment, finish rolling and aging treatment, the microstructure of the copper alloy can be effectively controlled, and various performances of the copper alloy are ensured.
Description
Technical Field
The invention relates to the technical field of nonferrous metal processing, in particular to an environment-friendly conductive elastic copper alloy, a preparation method thereof and application thereof in a connector.
Background
The connector is used as a key element for current or signal connection, is an important component of an industrial system, is widely applied to the fields of military industry, communication, automobiles, electronics and the like, and the high-performance copper alloy material is a key raw material for realizing the functions of the connector. With the rapid development of important fields such as 5G communication, mobile terminals, artificial intelligence, aerospace and the like, the connector technology mainly develops towards microminiaturization, integration, intellectualization, high performance and humanization in use, which requires that the size of the connector not only be more miniaturized, but also the performance develop towards high frequency, high power and large current, low impedance and low temperature rise, extreme environment resistance, use reliability and environmental protection. The copper alloy material has more rigorous requirements on the performance, and not only has high yield strength (more than 900 MPa), high elastic performance (more than 125 GPa), excellent conductive performance (more than 30% IACS), long-time high-temperature resistance and stress relaxation resistance (stress relaxation rate of less than 20% when the temperature is kept at 150 ℃ for 1000 hours), but also has excellent bending forming performance (no defect occurs when the copper alloy material is bent at 90 degrees when the transverse direction and the longitudinal direction are R/T = 3).
At present, the ultrahigh-strength elastic copper alloy materials for the conventional connector mainly comprise beryllium bronze and tin-phosphor bronze. The beryllium bronze is a main copper alloy elastic material used for high-reliability connectors at home and abroad at present, but because the beryllium bronze alloy contains highly toxic substance beryllium and the stress relaxation rate is sharply increased in the environment of more than 150 ℃, the contact pressure of an elastic component in a working state is easily changed, so that the connector works inefficiently. In addition, because the tin-phosphor bronze alloy belongs to a work hardening alloy, the alloy is poor in bending forming, high-temperature stress relaxation resistance and conductivity, and the use requirement of the high-end connector cannot be met.
The copper-titanium and copper-nickel-tin alloys have the performances of high strength, elasticity and the like which are comparable to those of beryllium bronze, and more excellent processing forming performance, corrosion resistance and high-temperature stress relaxation resistance, the two alloys are researched, developed and industrialized by the countries such as the United states, Japan and the like, the typical brands are C19900, NKT322, C72700, C72900 and the like respectively, the former has more excellent bending forming performance and meets the use requirement of a more miniaturized structural connector, the latter has more excellent corrosion resistance and meets the use requirement of a corrosion-resistant environmental connector, the two alloys are respectively applied to important fields such as aerospace, communication, mobile terminals and the like, but cannot meet the use requirement of a functional terminal connector material due to insufficient conductivity, and the new generation high-strength conductive material is Cu-Ni-Co-Si series alloy, the yield strength of the industrial production is 800-850 MPa, the strength is still to be improved, and the bending performance of the Cu-Ni-Co-Si alloy is poor.
Therefore, a new generation of environment-friendly conductive elastic copper alloy with ultrahigh strength, stress relaxation resistance, excellent forming performance and high reliability is developed, the use requirements of the connector under different application scenes are met, and the conductive elastic copper alloy is an important measure for solving the key industry and major engineering requirements in China.
Disclosure of Invention
In view of the above, the present invention provides an environment-friendly conductive elastic copper alloy, a method for preparing the same, and an application of the same in a connector. The environment-friendly conductive elastic copper alloy provided by the invention has the characteristics of ultrahigh strength, stress relaxation resistance, good elasticity and high conductivity, is excellent in forming performance, high in reliability, free of toxic elements and good in environment friendliness, can meet the use requirements of connectors in different application scenes, and is a copper alloy material for a new generation of connectors.
In order to achieve the above object, the present invention provides the following technical solutions:
an environment-friendly conductive elastic copper alloy comprises the following chemical components in percentage by mass: ni: 2.0-4.3%, Si: 0.5 to 0.85%, Mn: 0.05-0.4%, Mg: 0.01-0.2%, 0.01-1.0% of rare earth elements and the balance of Cu; the mass ratio of nickel element to silicon element in the copper alloy is (4.8-5.5): 1.
Preferably, the copper alloy has Ni in the form of a rod and/or a disk in longitudinal and transverse cross sections2Si phase, said rod-like and/or disk-like Ni2The average particle diameter of the Si phase is independently 6 to 20 nm.
Preferably, the copper alloy comprises 7-25% of S {123} <634> texture, 14-40% of Brass {011} <211> texture, 10-28% of Cu {112} <111> texture and 20-35% of Cube {001} <100> texture.
Preferably, the copper alloy further comprises an auxiliary element; the auxiliary element is one or more of Co, Fe, Cr, Sn, Ti, Ag, Zr and Zn; the mass percentage of the auxiliary elements is 0.01-1.0% independently.
The invention also provides a preparation method of the environment-friendly conductive elastic copper alloy, which comprises the following steps:
(1) smelting and casting a copper alloy raw material to obtain an ingot;
(2) and sequentially carrying out hot rolling, initial rolling, intermediate annealing treatment, intermediate rolling, rapid solid solution treatment, finish rolling and aging treatment on the cast ingot to obtain the environment-friendly conductive elastic copper alloy.
Preferably, the smelting is carried out in a non-vacuum induction furnace, and the smelting temperature is 1230-1270 ℃; the casting temperature is 1120-1180 ℃.
Preferably, the initial rolling temperature of the hot rolling is 920-960 ℃, and the final rolling temperature is 760-820 ℃;
the initial rolling is cold rolling, and the processing rate is 60-80%;
the annealing temperature of the intermediate annealing treatment is 500-600 ℃, the heat preservation time is 5-8 hours, the cooling mode is gas cooling, and the gas used for the gas cooling is mixed gas of hydrogen and nitrogen;
the intermediate rolling is cold rolling, and the processing rate is 50-80%;
the temperature of the rapid solution treatment is 920-1020 ℃, the annealing speed is 10-20 m/min, the cooling speed is 60-80 ℃/s, the cooling mode is gas cooling, and the gas used for the gas cooling is a mixed gas of hydrogen and nitrogen;
the finish rolling is cold rolling, and the machining rate is 30-60%;
the aging temperature of the aging treatment is 450-600 ℃, the heat preservation time is 1-6 h, the cooling mode is gas cooling, and the gas used for the gas cooling is mixed gas of hydrogen and nitrogen.
Preferably, the hot rolling further comprises milling the alloy blank after the hot rolling.
The invention also provides application of the environment-friendly conductive elastic copper alloy or the environment-friendly conductive elastic copper alloy prepared by the preparation method in the scheme in a connector.
The invention provides an environment-friendly conductive elastic copper alloy which comprises the following chemical components in percentage by mass: ni: 2.0-4.3%, Si: 0.5 to 0.85%, Mn: 0.05-0.4%, Mg: 0.01-0.2%, 0.01-1.0% of rare earth elements and the balance of Cu. According to the invention, through the design and optimization of copper alloy components and the regulation and control of microstructure, the high-strength copper-nickel-silicon-manganese-magnesium alloy material with fine and uniform structure and dispersed precipitated phase is obtained, and the alloy material has ultrahigh strength, can keep higher conductivity, has the characteristics of good stress relaxation resistance and good elasticity, and is excellent in forming performance and high in reliability; in addition, the environment-friendly conductive elastic copper alloy provided by the invention also has excellent high temperature resistance and complex environment corrosion resistance. The yield strength of the environment-friendly conductive elastic copper alloy is 800-1050 MPa, the electric conductivity is 30-45% IACS, the hardness is 220-375 HV, the stress relaxation rate of 150 ℃ multiplied by 1000h is 12-18%, when the stress relaxation rate is R/T =3 in the transverse direction and the longitudinal direction, no defect occurs when the copper alloy is bent for 90 degrees, the comprehensive performance is good, and the use requirements of connectors under different application scenes can be met.
The invention also provides a preparation method of the environment-friendly conductive elastic copper alloy, and the copper alloy is prepared by smelting, casting, hot rolling, initial rolling, intermediate annealing, intermediate rolling, rapid solid solution treatment, finish rolling and aging treatment. The preparation method provided by the invention can effectively control the microstructure of the copper alloy, ensure various properties of the copper alloy and obtain the copper alloy material with excellent comprehensive properties.
Drawings
FIG. 1 is a schematic diagram of a gold phase of a longitudinal cross section of an environmentally friendly conductive elastic copper alloy obtained in example 6 of the present invention.
Detailed Description
The invention provides an environment-friendly conductive elastic copper alloy which comprises the following chemical components in percentage by mass: ni: 2.0-4.3%, Si: 0.5 to 0.85%, Mn: 0.05-0.4%, Mg: 0.01-0.2%, 0.01-1.0%, and the balance of Cu.
In the environment-friendly conductive elastic copper alloy, the content of Ni is 2.0-4.3% by mass, preferably 2.5-4.0% by mass, and the content of Si is 0.5-0.85% by mass, preferably 0.6-0.75% by mass. In the present invention, the mass ratio of the nickel element to the silicon element is (4.8 to 5.5):1, and more preferably (5.0 to 5.3): 1. In the present invention, the copper alloy has Ni in the form of a rod and/or a disk in longitudinal and transverse cross sections2Si phase, said rod-like and/or disk-like Ni2The average particle size of the Si phase is preferably 6 to 20nm independently; in the invention, Ni2The average grain diameter of the Si phase is controlled within the range, so that precipitated phases are dispersed in a matrix structure to form uniform dispersion structure strengthening, the stress relaxation resistance of the copper alloy is improved, and meanwhile, Ni2The Si phase is uniformly dispersed and distributed, so that the anisotropy of the material is improved, and the bending and bending performance of the material is obviously improved; especially, in the bending property, if there is uneven distribution of large and small precipitated phases, the precipitation of large particles during the bending forming process of the material will cause the bending formabilityThe energy is obviously reduced, which is also the reason that the size of the precipitated phase needs to be controlled in a certain range, and meanwhile, the structure of the precipitated phase is similar to a circle and forms a coherent interface with the matrix structure, which is also beneficial to improving the bending performance of the material.
In the present invention, Ni element mainly forms Ni with Si element during aging2Si precipitate phase, Ni with increasing Ni content2The larger the amount of precipitated Si phase, the more the Ni content becomes, the more Ni becomes2The Si phase is agglomerated and loses the function of the strengthening phase, so the proportion of the nickel element and the silicon element in the alloy needs to be reasonably controlled, and the content and the proportion of the Ni element and the Si element are controlled within the range, so that the elements can be fully precipitated and form a fine and dispersed strengthening phase.
The content of Mn in the environment-friendly conductive elastic copper alloy is 0.05-0.4% by mass, and preferably 0.1-0.3%. In the present invention, Mn element can form a small amount of Mn2The Si phase increases the yield strength and the hardness of the alloy, simultaneously refines crystal grains, and realizes good matching of the strength and the electric conductivity by adjusting the content of Mn; meanwhile, the Mn element can obviously improve the distribution of precipitated phase particles, thereby changing the anisotropic state and greatly improving the bending property of the material.
The content of Mg in the environment-friendly conductive elastic copper alloy is 0.01-0.2% by mass percentage, and the preferable content is 0.05-0.15%. In the invention, the Mg element can prevent the growth of a precipitated phase in the aging process, and can improve the fatigue resistance and reliability of the alloy.
The content of the rare earth element in the environment-friendly conductive elastic copper alloy is preferably 0.01-1.0% by mass, and more preferably 0.03-0.6% by mass. The invention has no special requirement on the kind of the rare earth element, in the specific embodiment of the invention, the rare earth element can be lanthanum (La), cerium (Ce), praseodymium (Pr), neodymium (Nd), yttrium (Y), scandium (Sc) and the like, the rare earth element can be single rare earth or mixed rare earth, and when the rare earth element is mixed rare earth, the invention has no special requirement on the kind and proportion of the rare earth element in the mixed rare earthAny kind and ratio can be obtained. In the invention, the rare earth element can purify the melt, improve the flow property of the melt, facilitate the casting and subsequent processing of the material, refine crystal grains, improve the mechanical property of the material and accelerate the second phase particle Ni2And Si phase particles are separated out, and the separated phase structure is improved to be distributed in a shape similar to a circle, so that the mechanical property of the material is improved, and the bending property is improved.
The environment-friendly conductive elastic copper alloy provided by the invention comprises the balance of Cu.
In the present invention, the environmentally friendly conductive elastic copper alloy preferably further comprises an auxiliary element; the auxiliary element is preferably one or more of Co, Fe, Cr, Sn, Ti, Ag and Zr; the mass percentage of the auxiliary elements is preferably 0.01-1.0%, and more preferably 0.05-0.6%. In the present invention, Co, Fe, Cr, Ti, Ag, Zr and Zn promote Ni2Si phase is separated out or forms a simple substance phase to block the movement of particles, so that the conductivity, the stress relaxation resistance and the high temperature softening resistance of the alloy can be improved, but the quantity of nickel-silicon precipitation phases can be reduced due to the excessively high addition of the elements, so that the mechanical property of the alloy is reduced. Zn and Sn can be dissolved in copper in a solid mode, and the mechanical property of the alloy is improved.
In the present invention, the content of the S {123} <634> texture in the copper alloy is preferably 7 to 25%, more preferably 8 to 22%, the content of the Brass {011} <211> texture is preferably 14 to 40%, more preferably 20 to 35%, the content of the Cu {112} <111> texture is preferably 10 to 28%, more preferably 15 to 25%, and the content of the Cube {001} <100> texture is preferably 20 to 35%, more preferably 25 to 30%.
The invention also provides a preparation method of the environment-friendly conductive elastic copper alloy, which comprises the following steps:
(1) smelting and casting a copper alloy raw material to obtain an ingot;
(2) and sequentially carrying out hot rolling, initial rolling, intermediate annealing treatment, intermediate rolling, rapid solid solution treatment, finish rolling and aging treatment on the cast ingot to obtain the environment-friendly conductive elastic copper alloy.
The method comprises the steps of smelting and casting a copper alloy raw material to obtain an ingot. The copper alloy is prepared according to the mass percent of elements in the copper alloy, and then the copper alloy raw material is sequentially smelted and cast. In the present invention, the copper alloy raw material is preferably electrolytic copper, electrolytic nickel, a nickel-silicon alloy, a copper-manganese alloy, and a copper-magnesium alloy.
In the invention, the smelting is preferably carried out in a non-vacuum induction furnace, the smelting temperature is preferably 1230-1270 ℃, more preferably 1235-1260 ℃, and the casting temperature is preferably 1120-1180 ℃, more preferably 1130-1160 ℃. According to the invention, electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy are preferably added into a non-vacuum induction furnace, after the materials are melted, the copper-magnesium alloy is continuously added, after the raw materials are completely melted, the melt is poured into a heat preservation furnace to be uniformly stirred, and casting is carried out after heat preservation is carried out for 20 min.
After obtaining the ingot, the ingot is hot rolled. In the invention, the initial rolling temperature of the hot rolling is preferably 920-960 ℃, more preferably 930-950 ℃, and the final rolling temperature is preferably 760-820 ℃, more preferably 780-800 ℃. The cast ingot is preferably heated in a stepping box type furnace to 920-960 ℃, then heat preservation is carried out for 2-6 h, then hot rolling is carried out, and water cooling is carried out after the hot rolling is finished.
After the hot rolling is finished, the obtained hot rolled blank is preferably subjected to surface milling in the invention. The method for operating the milling surface is not particularly limited, and a method known to those skilled in the art may be used.
After the surface is milled, the hot rolled blank after the surface milling is subjected to initial rolling. In the invention, the initial rolling is preferably cold rolling, and the working ratio is preferably 60-80%, more preferably 65-75%.
After the blooming is finished, the intermediate annealing treatment is carried out on the obtained blooming blank. In the invention, the annealing temperature of the intermediate annealing treatment is preferably 500-600 ℃, more preferably 530-560 ℃, the heat preservation time is preferably 5-8 h, more preferably 6-7 h, the cooling mode is preferably gas cooling, and the gas used for the gas cooling is preferably the mixture of hydrogen and nitrogenGas; the volume ratio of hydrogen to nitrogen in the mixed gas is preferably (2-3) to 1; the invention carries out cooling in a gas cooling mode, and can realize bright protection while carrying away heat; the intermediate annealing treatment is preferably performed in a bell jar annealing furnace; the temperature of the intermediate annealing treatment is controlled to be 500-600 ℃, and Ni can be kept2Si is relatively well and completely precipitated, the size of a precipitated phase is not increased, and the uniform precipitation of the precipitated phase is favorable for improving the conductivity performance of the strip; if the intermediate annealing treatment temperature is higher than 600 ℃, the grain size of the precipitated phase grows, and the precipitated phase presents the condition of different sizes, although the material can keep certain mechanical strength and better conductivity, the bending performance of the material is obviously reduced, which is also an important consideration that the annealing temperature is strictly controlled in the aspect of comprehensive performance matching.
After the intermediate annealing treatment is finished, the intermediate blank obtained by the invention is subjected to intermediate rolling. In the invention, the intermediate rolling is preferably cold rolling, and the reduction ratio is preferably 50-80%, and more preferably 60-70%.
After the medium rolling is finished, the invention carries out rapid solid solution treatment on the obtained medium rolled blank. In the invention, the temperature of the rapid solution treatment is preferably 920-1020 ℃, more preferably 950-1000 ℃, the annealing speed is preferably 10-20 m/min, more preferably 13-15 m/min, the cooling speed is preferably 60-80 ℃/s, more preferably 65-75 ℃/s, the cooling mode is preferably gas cooling, the gas used for gas cooling is preferably a mixed gas of hydrogen and nitrogen, the volume ratio of the hydrogen and the nitrogen in the mixed gas is consistent with the scheme, and the description is omitted.
After the rapid solution treatment is finished, the alloy solid solution is subjected to finish rolling. In the present invention, the finish rolling is preferably cold rolling, and the reduction ratio is preferably 30 to 60%, and more preferably 40 to 50%.
After finishing the finish rolling, the invention carries out aging treatment on the obtained finish rolled blank to obtain the environment-friendly conductive elastic copper alloy. In the invention, the aging temperature of the aging treatment is preferably 450-600 ℃, more preferably 500-550 ℃, the heat preservation time is preferably 1-6 h, more preferably 2-5 h, the cooling mode is preferably gas cooling, the gas used for the gas cooling is preferably a mixed gas of hydrogen and nitrogen, the volume ratio of the hydrogen and the nitrogen in the mixed gas is consistent with the scheme, and the details are not repeated; the aging treatment is preferably carried out in a bell jar annealing furnace.
The invention regulates and controls the microstructure of the copper alloy through rapid solid solution treatment and a matched aging treatment technology, and obtains the copper-nickel-silicon-manganese-magnesium alloy material which has fine and uniform structure, high strength with dispersed precipitated phases and higher conductivity.
The invention also provides application of the environment-friendly conductive elastic copper alloy or the environment-friendly conductive elastic copper alloy prepared by the preparation method in the scheme in a connector. The environment-friendly conductive elastic copper alloy provided by the invention has the characteristics of ultrahigh strength, high temperature resistance, stress relaxation resistance, complex environment corrosion resistance, good conductivity and elasticity, is excellent in forming performance, high in reliability, free of toxic elements and good in environmental friendliness, can meet the use requirements of connectors in different application scenes, and is a copper alloy material for a new generation of connectors.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention.
Example 1
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1260 ℃, continuing to add copper-magnesium alloy after the materials are all molten, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely molten, preserving the heat for 20min, and casting at 1160 ℃ to obtain the cast ingot.
2. Hot rolling: heating the cast ingot in a stepping box type furnace at 950 ℃ for 3h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 65%.
4. Intermediate annealing treatment: and (3) placing the primary rolling blank in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 550 ℃, the heat preservation time is 7 hours, and the cooling mode is gas cooling, and the used gas is a mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to the intermediate annealing treatment, wherein the cold rolling processing rate is 70%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 980 ℃, the annealing speed is 12m/min, the cooling speed is 65 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 45%.
8. Aging treatment: and placing the finish rolled blank in a bell jar type annealing furnace for aging treatment, wherein the aging temperature is 520 ℃, the heat preservation time is 4 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Example 2
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1250 ℃, continuing to add the copper-magnesium alloy after the materials are all melted, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely melted, preserving the heat for 20min, and then casting at 1150 ℃.
2. Hot rolling: and heating the obtained cast ingot in a stepping box type furnace at 930 ℃ for 5h, then carrying out hot rolling, controlling the final rolling temperature to 780 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 70%.
4. Intermediate annealing treatment: and (3) placing the primary rolling blank in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 570 ℃, the heat preservation time is 5 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling processing rate is 55%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 960 ℃, the annealing speed is 18m/min, the cooling speed is 75 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 55%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 570 ℃, the heat preservation time is 3 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Example 3
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1240 ℃, continuing to add the copper-magnesium alloy after the materials are all melted, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely melted, preserving the heat for 20min, and then casting at 1140 ℃.
2. Hot rolling: heating the obtained cast ingot in a stepping box furnace at the temperature of 960 ℃ for 5h, then carrying out hot rolling, controlling the final rolling temperature at 770 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 70%.
4. Intermediate annealing treatment: and (3) placing the bloom in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 570 ℃, the heat preservation time is 5 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling reduction rate is 55%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 980 ℃, the annealing speed is 15m/min, the cooling speed is 75 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 50%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 550 ℃, the heat preservation time is 3 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Example 4
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1270 ℃, continuing to add copper-magnesium alloy after the materials are all molten, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely molten, preserving the heat for 20min, and then casting at 1170 ℃.
2. Hot rolling: and heating the obtained cast ingot in a stepping box type furnace at 930 ℃ for 5h, then carrying out hot rolling, controlling the final rolling temperature to 780 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 70%.
4. Intermediate annealing treatment: and (3) placing the bloom in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 570 ℃, the heat preservation time is 5 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling processing rate is 55%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 960 ℃, the annealing speed is 18m/min, the cooling speed is 75 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 55%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 520 ℃, the heat preservation time is 5 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Example 5
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1270 ℃, continuing to add copper-magnesium alloy after the materials are all melted, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely melted, preserving the heat for 20min, and then casting at 1180 ℃.
2. Hot rolling: and heating the obtained cast ingot in a stepping box type furnace at 930 ℃ for 5h, then carrying out hot rolling, controlling the final rolling temperature to 780 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 70%.
4. Intermediate annealing treatment: and (3) placing the bloom in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 570 ℃, the heat preservation time is 5 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling processing rate is 55%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 1000 ℃, the annealing speed is 18m/min, the cooling speed is 75 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 60%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 530 ℃, the heat preservation time is 4 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Example 6
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1250 ℃, continuing to add copper-magnesium alloy after the materials are all melted, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely melted, preserving the heat for 20min, and then casting at 1140 ℃.
2. Hot rolling: and heating the obtained cast ingot in a stepping box type furnace at 930 ℃ for 5h, then carrying out hot rolling, controlling the final rolling temperature to 780 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 70%.
4. Intermediate annealing treatment: and (3) placing the primary rolling blank in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 570 ℃, the heat preservation time is 5 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling processing rate is 55%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 960 ℃, the annealing speed is 18m/min, the cooling speed is 75 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 55%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 570 ℃, the heat preservation time is 3 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Example 7
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1260 ℃, continuing to add copper-magnesium alloy after the materials are all molten, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely molten, preserving the heat for 20min, and casting at 1160 ℃.
2. Hot rolling: heating the obtained cast ingot in a stepping box type furnace at 950 ℃ for 4h, then carrying out hot rolling, controlling the final rolling temperature at 810 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 70%.
4. Intermediate annealing treatment: and (3) placing the bloom in a bell-type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 560 ℃, the heat preservation time is 6 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling processing rate is 75%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 930 ℃, the annealing speed is 18m/min, the cooling speed is 65 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 30-60%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 55 ℃, the heat preservation time is 2 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Example 8
The composition of the alloy is shown in table 1.
1. Smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1260 ℃, continuing to add copper-magnesium alloy after the materials are all molten, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely molten, preserving the heat for 20min, and then casting at 1150 ℃.
2. Hot rolling: and heating the obtained cast ingot in a stepping box type furnace at 930 ℃ for 3h, then carrying out hot rolling, controlling the final rolling temperature at 800 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 65%.
4. Intermediate annealing treatment: and (3) placing the primary rolling blank in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 500 ℃, the heat preservation time is 6 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling processing rate is 55%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 960 ℃, the annealing speed is 14m/min, the cooling speed is 70 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 40%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 500 ℃, the heat preservation time is 4 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the obtained environmentally friendly conductive elastic copper alloy are shown in Table 2.
Comparative examples 1 to 4
The composition of the alloy is shown in table 1. The preparation methods of comparative examples 1 to 4 are the same, and the preparation steps are as follows:
1. smelting: adding electrolytic copper, electrolytic nickel, nickel-silicon alloy and copper-manganese alloy into a non-vacuum induction furnace, controlling the smelting temperature to 1250 ℃, continuing to add the copper-magnesium alloy after the materials are all melted, pouring the melt into a heat preservation furnace for uniform stirring after the melt is completely melted, preserving the heat for 20min, and then casting at 1150 ℃.
2. Hot rolling: and heating the obtained cast ingot in a stepping box type furnace at 930 ℃ for 5h, then carrying out hot rolling, controlling the final rolling temperature to 780 ℃, and then carrying out water cooling.
3. Initial rolling: and milling the surface of the alloy blank subjected to water cooling, and then carrying out primary rolling, wherein the cold rolling processing rate is 70%.
4. Intermediate annealing treatment: and (3) placing the bloom in a bell jar type annealing furnace for intermediate annealing treatment, wherein the annealing temperature is 570 ℃, the heat preservation time is 5 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
5. Intermediate rolling: and (4) carrying out medium rolling on the alloy blank subjected to annealing treatment, wherein the cold rolling processing rate is 70%.
6. On-line high-temperature rapid solution treatment: and (3) carrying out on-line high-temperature rapid solution treatment on the medium-rolled blank, wherein the solution treatment temperature is 960 ℃, the annealing speed is 18m/min, the cooling speed is 75 ℃/s, the cooling mode is gas cooling, and the used gas is a mixed gas of nitrogen and hydrogen.
7. Finish rolling: and (3) performing finish rolling on the alloy solid solution after the solution treatment, wherein the cold rolling reduction rate is 70%.
8. Aging treatment: and placing the finish rolled blank in a bell-type annealing furnace for aging treatment, wherein the aging temperature is 570 ℃, the heat preservation time is 3 hours, the cooling mode is gas cooling, and the used gas is mixed gas of hydrogen and nitrogen.
The properties of the resulting copper alloy are shown in Table 2.
TABLE 1 alloy composition formulas (wt.%) of examples 1-8 and comparative examples 1-4
TABLE 2 tables of alloy Properties and texture structures of examples 1 to 8 and comparative examples 1 to 4
According to the results in the table 2, the copper alloy prepared by the invention has high yield strength and hardness, higher conductivity and good bending resistance, and can be bent by 90 degrees without any defect when the copper alloy is transversely and longitudinally R/T =3, so that the use requirements of the connector under different application scenes can be met; the comparative example 1 does not contain rare earth elements, and Ni/Si is higher than the range of the invention, so that the hardness of the alloy is reduced, and the comparative example 2, Ni/Si is lower than the range of the invention, so that the hardness and the bending resistance of the alloy are reduced; in comparative examples 3-4, the content of the Mn element is higher than the range of the invention, and at the moment, the yield strength and the hardness of the obtained copper alloy are higher, but the conductivity is obviously reduced, so that the requirements of the connector cannot be met.
And (3) metallographic testing:
the metallographic view of the longitudinal section of the eco-friendly conductive elastic copper alloy obtained in example 6 is shown in FIG. 1, and rod-like Ni can be observed from FIG. 12A Si phase;
metallographic test of the cross and longitudinal sections of the environmentally friendly conductive elastic copper alloys obtained in examples 1 to 5 and 7 to 8 revealed that uniformly distributed rod-like or disk-like Ni was observed in both the cross and longitudinal sections of the alloys2A Si phase.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (9)
1. An environment-friendly conductive elastic copper alloy comprises the following chemical components in percentage by mass: ni: 2.0-4.3%, Si: 0.5 to 0.85%, Mn: 0.05-0.4%, Mg: 0.01-0.2%, rare earth elements: 0.01-1.0% and the balance of Cu; the mass ratio of nickel element to silicon element in the copper alloy is (4.8-5.5): 1.
2. The environmentally friendly electrically conductive elastic copper alloy according to claim 1, wherein the copper alloy has Ni in the form of a rod and/or a disk in longitudinal and transverse cross-sections2Si phase, said rod-like and/or disk-like Ni2The average particle diameter of the Si phase is independently 6 to 20 nm.
3. The environmentally friendly conductive elastic copper alloy according to claim 1, wherein the copper alloy comprises 7-25% of S {123} <634> texture, 14-40% of Brass {011} <211> texture, 10-28% of Cu {112} <111> texture, and 20-35% of Cube {001} <100> texture.
4. The environmentally friendly electrically conductive resilient copper alloy according to claim 1, further comprising an auxiliary element; the auxiliary element is one or more of Co, Fe, Cr, Sn, Ti, Ag, Zr and Zn; the mass percentage of the auxiliary elements is 0.01-1.0% independently.
5. The method for preparing the environment-friendly conductive elastic copper alloy according to any one of claims 1 to 4, characterized by comprising the following steps:
(1) smelting and casting a copper alloy raw material to obtain an ingot;
(2) and sequentially carrying out hot rolling, initial rolling, intermediate annealing treatment, intermediate rolling, rapid solid solution treatment, finish rolling and aging treatment on the cast ingot to obtain the environment-friendly conductive elastic copper alloy.
6. The preparation method of claim 5, wherein the smelting is carried out in a non-vacuum induction furnace, and the smelting temperature is 1230-1270 ℃; the casting temperature is 1120-1180 ℃.
7. The production method according to claim 5, wherein the hot rolling is performed at a start rolling temperature of 920 to 960 ℃ and a finish rolling temperature of 760 to 820 ℃;
the initial rolling is cold rolling, and the processing rate is 60-80%;
the annealing temperature of the intermediate annealing treatment is 500-600 ℃, the heat preservation time is 5-8 hours, the cooling mode is gas cooling, and the gas used for the gas cooling is mixed gas of hydrogen and nitrogen;
the intermediate rolling is cold rolling, and the processing rate is 50-80%;
the temperature of the rapid solution treatment is 920-1020 ℃, the annealing speed is 10-20 m/min, the cooling speed is 60-80 ℃/s, the cooling mode is gas cooling, and the gas used for the gas cooling is a mixed gas of hydrogen and nitrogen;
the finish rolling is cold rolling, and the machining rate is 30-60%;
the aging temperature of the aging treatment is 450-600 ℃, the heat preservation time is 1-6 h, the cooling mode is gas cooling, and the gas used for the gas cooling is mixed gas of hydrogen and nitrogen.
8. The method of claim 5, 6 or 7, wherein the hot rolling further comprises milling the alloy billet after the hot rolling.
9. Use of the environmentally friendly conductive elastic copper alloy according to any one of claims 1 to 4 or the environmentally friendly conductive elastic copper alloy prepared by the preparation method according to any one of claims 5 to 8 in a connector.
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