CN108823464B - Copper alloy material and preparation method thereof - Google Patents
Copper alloy material and preparation method thereof Download PDFInfo
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- CN108823464B CN108823464B CN201810707575.5A CN201810707575A CN108823464B CN 108823464 B CN108823464 B CN 108823464B CN 201810707575 A CN201810707575 A CN 201810707575A CN 108823464 B CN108823464 B CN 108823464B
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- C22C9/00—Alloys based on copper
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- 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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- 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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Abstract
A process for preparing Cu-Ag alloy includes such steps as 1) alloying Cu with Ag under vacuum degree not higher than 9.0 × 10‑3Heating under the condition of Pa, stopping vacuumizing until the heating temperature is 800-900 ℃, heating under the protection of inert gas until copper is completely melted, adding silver, mixing to form a melt, and casting to form an ingot; 2) alloy solution treatment: carrying out solution treatment on the cast ingot; 3) cold deformation processing; 4) and (4) aging heat treatment. The copper alloy prepared by the method has less silver content, and the preparation process can greatly reduce the burning loss of noble metal silver and reduce the production cost; the copper alloy material obtained by matching with proper heat treatment and cold processing technology has the characteristics of high strength and high conductivity, uniform components and stable performance, is convenient to process into various copper materials, and provides guarantee for wide application of the copper alloy material.
Description
Technical Field
The invention relates to the field of copper alloy smelting and processing, in particular to a copper alloy material and a preparation method thereof.
Background
For conventional conductive materials of copper, aluminum and their alloys, there is a trade-off between strength and conductivity, and it is generally difficult to have both high conductivity and high strength. Because the metal copper and the metal silver have excellent conductivity and are not solid-dissolved with each other at normal temperature, the metal copper and the metal silver are ideal candidate materials for realizing high strength and high conductivity and are widely applied to the fields of electric locomotive transmission lines, transportation leads, lead frames, high magnetic field pulse magnets and the like. The conventional method for realizing the high-strength and high-conductivity copper-silver alloy material is to realize copper-silver alloying, and the strength of the material is improved by adjusting the content of silver in the alloy.
For example, CN 103572184a discloses a preparation method of a high-strength copper-silver alloy material, which comprises the following steps: 1) copper and silver are used as raw materials, and the raw materials are proportioned according to the mass fraction of 15-20% of silver and the balance of copper; 2) preparing a copper-silver alloy bar by adopting a vacuum melting technology; 3) refining the copper-silver alloy bar by adopting a vacuum consumable arc melting technology; 4) hot extrusion: extruding at 800-900 ℃, keeping the temperature for 2-4 h, and extruding into a bar material, wherein the extrusion ratio is 8-10; 5) and (3) heat treatment: annealing at 200-250 ℃ for 1-2 h, and cooling along with the furnace; 6) and (4) drawing to obtain the product.
CN 101643866A discloses a high-strength high-conductivity Cu-Ag alloy material and a preparation method thereof, and specifically discloses a preparation method of the alloy material, wherein the alloy material comprises Ag5 wt-10 wt%, and the balance of copper, and the preparation method comprises the following steps: 1) designing chemical components; 2) vacuumizing the smelting chamber and the directional solidification chamber; 3) preheating a graphite crucible; 4) alloy smelting; 5) pulling down the graphite crucible; 6) taking out the alloy ingot; 7) hot extrusion; 8) heat treatment; 9) and (4) drawing.
However, the methods in the prior art are all modes for realizing copper-silver alloying, and the strength of the material is improved by adding a large amount of noble metal silver to sacrifice the conductivity of the conductor, so that the optimal performance of the copper-silver alloy material cannot be realized.
Disclosure of Invention
In view of the above-mentioned drawbacks of the prior art, an object of the present invention is to provide a copper alloy and a method for preparing the same, which solve the problems of the prior art.
To achieve the above objects and other related objects, the present invention is achieved by the following technical solutions.
The invention provides a preparation method of a copper alloy material, which comprises the following steps:
1) alloying copper and silver, namely, alloying copper in vacuum degree of more than 9.0 × 10-3Heating under the condition of Pa, stopping vacuumizing when the heating temperature is 800-900 ℃, heating under the protection of inert gas until copper is completely melted, adding silver, mixing to form a solution, and casting to form an ingot;
2) alloy solution treatment: carrying out solution treatment on the cast ingot;
3) cold deformation processing;
4) and (4) aging heat treatment.
Preferably, in step 1), the amount of silver is 0.1 wt% to 1.0 wt% based on the total mass of silver and copper.
Preferably, in the step 1), the heating temperature is 1150-1200 ℃.
Preferably, in the step 1), silver particles are adopted as the silver, and the diameter of the silver particles is 0.01 cm-0.5 cm. The silver particles are added into the completely molten copper melt, so that the silver particles are quickly dissolved and fully and uniformly mixed with the copper melt.
Preferably, in step 1), oxygen-free copper is used as the copper.
Preferably, in step 1), the purity of the silver particles is 99.9%.
Preferably, in the step 2), the ingot solution treatment means that the ingot is heated to a high-temperature single-phase region and kept at a constant temperature, so that the silver phase is fully dissolved in the copper melt and then rapidly cooled to obtain a supersaturated solid solution.
Preferably, the temperature of the high-temperature single-phase zone is 700-850 ℃. Keeping the constant temperature for 4-12 h.
Preferably, the mixture is quickly put into water for cooling after the constant-temperature heating is finished. More preferably, the time interval from the end of the constant-temperature heating to the time of putting into water is not more than 5 s.
Preferably, in step 3), the cold deformation means cold working the solution-treated ingot at a temperature not higher than the recrystallization temperature, and more preferably, the deformation ratio η in the cold deformation step is 1 to 4, wherein η ═ ln (S) (where S is equal to or greater than the value of ln)0/S)，S0And S are the cross-sectional areas of the sample before and after cold deformation processing. More preferably, cold deformation processing in the present application refers to cold rolling and cold drawing.
Preferably, the cold-deformation process may be one or more times. More preferably, the deformation amount Q per cold deformation process is not more than 15%, and the deformation amount Q is (S)0-S)/S0Wherein S is0And S are the cross-sectional areas of the sample before and after cold deformation.
Preferably, in step 4), the aging heat treatment is a treatment placed in a certain temperature zone for achieving a large precipitation of silver in a supersaturated state. The temperature of the aging heat treatment is 350-500 ℃. The heat preservation time during aging heat treatment is 4-8 h.
The invention also discloses a copper alloy material, which is prepared by any one of the methods.
The copper alloy and the preparation method thereof disclosed by the invention have the following beneficial effects: according to the invention, the copper-silver alloy is smelted by separating copper and silver, so that the burning loss of silver is reduced, the crystal structure is improved by solution treatment, the supersaturated state of silver in copper is realized, the activation energy of silver is increased by cold deformation, a large amount of silver is uniformly precipitated by aging treatment, the structure is adjusted, the structure defect is eliminated, and the high-strength and high-conductivity copper alloy is finally obtained. The copper alloy prepared by the method has less silver content, and the preparation process can greatly reduce the burning loss of noble metal silver and reduce the production cost; meanwhile, the obtained copper alloy material obtained by matching with proper heat treatment and cold processing technology has the characteristics of high strength and high conductivity, has stable performance, is convenient to process into various copper materials, and provides guarantee for the wide application of the copper alloy material.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Before the present embodiments are further described, it is to be understood that the scope of the invention is not limited to the particular embodiments described below; it is also to be understood that the terminology used in the examples is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the present invention. Test methods in which specific conditions are not specified in the following examples are generally carried out under conventional conditions or under conditions recommended by the respective manufacturers.
When numerical ranges are given in the examples, it is understood that both endpoints of each of the numerical ranges and any value therebetween can be selected unless the invention otherwise indicated. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In addition to the specific methods, devices, and materials used in the examples, any methods, devices, and materials similar or equivalent to those described in the examples may be used in the practice of the invention in addition to the specific methods, devices, and materials used in the examples, in keeping with the knowledge of one skilled in the art and with the description of the invention.
Example 1
The preparation method of the copper-silver alloy material of the embodiment comprises the following steps:
1) taking oxygen-free copper and silver particles with the purity of 99.9 percent and the diameter of 0.5cm as raw materials, and batching according to the proportion that the silver accounts for 0.5 weight percent and the balance is copper;
2) preparing ingot by vacuum melting technique, charging proportioned copper and silver into vacuum melting furnace at one time without mixing, charging silver particles into storage chamber, vacuumizing until the vacuum degree reaches 9.0 × 10-3Heating at Pa, increasing power, stopping vacuum when temperature reaches 900 deg.C, and introducing argon gas to vacuum degree of 1.0 × 102Pa, adding silver when the temperature reaches 1150 ℃, stirring, casting after stirring for 2-3min, and naturally cooling to obtain the ingot.
3) The temperature of the solution treatment of the cast ingot is 700 ℃, the heat preservation time is 4h, the time interval between the discharging and the water entering is less than 5s, and the cast ingot is placed in water for water cooling.
4) The ingot after solid solution treatment was subjected to cold deformation processing as needed, and the deformation rate η was 2, and the deformation Q per time was 10%.
5) The temperature of the aging heat treatment of the alloy after cold deformation processing is 350 ℃, the heat preservation time is 4 hours, and the alloy is cooled along with the furnace.
Example 2
The preparation method of the high-strength copper-silver alloy material comprises the following steps:
1) taking oxygen-free copper and silver particles with the purity of 99.9 percent and the diameter of 0.01cm as raw materials, and batching according to the proportion that the silver accounts for 1.0 weight percent and the balance is copper;
2) preparing a copper-silver alloy bar by adopting a vacuum melting technology, filling proportioned copper and silver into a vacuum melting furnace at one time without mixing, filling silver particles into a storage chamber, vacuumizing until the vacuum degree reaches 9.0 × 10-3Heating at Pa, increasing power, closing vacuum when temperature reaches 800 deg.C, and introducing argon gas to vacuum degree of 1.0 × 102Pa, adding silver when the temperature reaches 1200 ℃,stirring, casting after stirring for 2-3min, and cooling to obtain the cast ingot.
3) The temperature of the solution treatment of the cast ingot is 850 ℃, the heat preservation time is 12h, the time interval between the discharging and the water entering is less than 5s, and the cast ingot is placed in water for water cooling.
4) The ingot after solid solution was subjected to cold deformation processing as needed, and the deformation rate η was 4, and the deformation Q per pass was 13%.
5) The temperature of aging treatment of the alloy after cold deformation processing is 500 ℃, the heat preservation time is 8h, and the alloy is cooled along with the furnace.
Example 3
The preparation method of the high-strength copper-silver alloy material comprises the following steps:
1) taking oxygen-free copper and silver particles with the purity of 99.9 percent and the diameter of 0.05cm as raw materials, and batching according to the proportion that the silver accounts for 0.1 weight percent and the balance is copper;
2) preparing a copper-silver alloy bar by adopting a vacuum melting technology, filling proportioned copper and silver into a vacuum melting furnace at one time without mixing, filling silver particles into a storage chamber, vacuumizing until the vacuum degree reaches 9.0 × 10-3Heating at Pa, increasing power, stopping vacuum when temperature reaches 850 deg.C, and introducing argon gas to vacuum degree of 1.0 × 102And Pa, adding silver when the temperature reaches 1180 ℃, stirring, casting after stirring for 2-3min, and cooling to obtain an ingot.
3) The temperature of the solution treatment of the cast ingot is 800 ℃, the heat preservation time is 10h, the time interval between the discharging and the water entering is less than 5s, and the cast ingot is placed in water for water cooling.
4) The ingot after solid solution was subjected to cold deformation processing as needed, and the deformation rate η was 1, and the deformation Q per pass was 14%.
5) The temperature of aging treatment of the alloy after cold deformation processing is 400 ℃, the heat preservation time is 5 hours, and the alloy is cooled along with the furnace.
Example 4
The preparation method of the high-strength copper-silver alloy material comprises the following steps:
1) taking oxygen-free copper and silver particles with the purity of 99.9 percent and the diameter of 0.2cm as raw materials, and batching according to the proportion that the silver accounts for 0.3 weight percent and the balance is copper;
2) preparing a copper-silver alloy bar by adopting a vacuum melting technology, filling proportioned copper and silver into a vacuum melting furnace at one time without mixing, filling silver particles into a storage chamber, vacuumizing until the vacuum degree reaches 9.0 × 10-3Heating at Pa, increasing power, stopping vacuum when temperature reaches 830 deg.C, and introducing argon gas to vacuum degree of 1.0 × 102Pa, when the temperature reaches 1160 ℃, adding silver, stirring, casting after 2-3min of stirring, and cooling to obtain a cast ingot.
3) The temperature of the solution treatment of the cast ingot is 750 ℃, the heat preservation time is 8h, the time interval between the discharging and the water entering is less than 5s, and the cast ingot is placed in water for water cooling.
4) The ingot after solid solution was subjected to cold deformation processing as needed, and the deformation rate η was 3, and the deformation Q per pass was 11%.
5) The temperature for aging treatment of the alloy after cold deformation processing is 450 ℃, the heat preservation time is 7 hours, and the alloy is cooled along with the furnace.
Comparative example 1
1) Taking oxygen-free copper and silver particles with the purity of 99.9 percent and the diameter of 0.2cm as raw materials, and batching according to the proportion that the silver accounts for 0.3 weight percent and the balance is copper;
2) preparing a copper-silver alloy bar by adopting a vacuum melting technology, filling the proportioned copper and silver into a vacuum melting furnace for one time to mix, then vacuumizing until the vacuum degree reaches 9.0 × 10-3Heating at Pa, increasing power, stopping vacuum when temperature reaches 830 deg.C, and introducing argon gas to vacuum degree of 1.0 × 102Pa, when the total melting temperature of the metal reaches 1160 ℃, stirring, casting after 2-3min of stirring, and cooling to obtain the cast ingot.
3) The temperature of the solution treatment of the cast ingot is 750 ℃, the heat preservation time is 8h, the time interval between the discharging and the water entering is less than 5s, and the cast ingot is placed in water for water cooling.
4) The ingot after solid solution was subjected to cold deformation processing as needed, and the deformation rate η was 3, and the deformation Q per pass was 11%.
5) The temperature for aging treatment of the alloy after cold deformation processing is 450 ℃, the heat preservation time is 7 hours, and the alloy is cooled along with the furnace.
Comparative example 2
1) Taking oxygen-free copper and silver particles with the purity of 99.9 percent and the diameter of 0.2cm as raw materials, and batching according to the proportion that the silver accounts for 0.3 weight percent and the balance is copper;
2) preparing a copper-silver alloy bar by adopting a vacuum melting technology, filling proportioned copper and silver into a vacuum melting furnace at one time without mixing, wherein Ag is filled into a material storage chamber, then vacuumizing, and when the vacuum degree reaches 9.0 × 10-3Heating at Pa, increasing power, stopping vacuum when temperature reaches 830 deg.C, and introducing argon gas to vacuum degree of 1.0 × 102Pa, when the temperature reaches 1160 ℃, adding silver, stirring, casting after 2-3min of stirring, and cooling to obtain a cast ingot.
3) And (3) carrying out cold deformation processing on the cast ingot, wherein the deformation rate eta value is 3, and the deformation quantity Q of each time is 11%.
The tensile strength and the electrical conductivity of the copper alloy materials prepared in examples 1, 2, 3 and 4 and comparative examples 1 and 2 were measured, and the results are shown in table 1.
The tensile strength is specified in GB/T228.1.
The conductivity was carried out as specified in GB/T32791.
Table 1 test items for tensile strength and conductivity test results of copper alloy materials of examples 1, 2, 3, 4 and comparative examples 1, 2
As can be seen from table 1 above: the test method provided by the invention can effectively reduce the burning loss of the noble metal silver, and the heat treatment and cold working process provided by the invention can simultaneously improve the conductivity and tensile strength of the alloy.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (3)
1. A preparation method of a copper alloy material comprises the following steps:
1) alloying copper and silver, namely, alloying copper in vacuum degree of not more than 9.0 × 10-3Heating under the condition of Pa, stopping vacuumizing until the heating temperature is 800-900 ℃, heating under the protection of inert gas until copper is completely melted, adding silver, mixing to form a melt, heating to 1150-1200 ℃, and casting into an ingot; the dosage of the silver is 0.1 wt% -1.0 wt% based on the total mass of the silver and the copper;
2) alloy solution treatment: carrying out solid solution treatment on the cast ingot, wherein the solid solution treatment of the cast ingot refers to heating the cast ingot to a high-temperature single-phase region and keeping the temperature constant, so that the silver phase is fully dissolved in the copper melt and then is rapidly cooled to obtain a supersaturated solid solution; the temperature of the high-temperature single-phase area is 700-850 ℃; keeping the constant temperature for 4-12 h; after the constant-temperature heating is finished, quickly putting the mixture into water for cooling;
3) cold deformation, wherein the ingot after solution treatment is subjected to cold working at a temperature below recrystallization temperature, and the deformation η value in the cold working procedure is 1-4, wherein η ═ ln (S)0/S)，S0S is the cross sectional area of the sample before and after cold deformation processing;
4) performing aging heat treatment, wherein the aging heat treatment is to place the silver in a certain specific temperature area for realizing the massive precipitation of the silver in a supersaturated state, and the temperature of the aging heat treatment is 350-500 ℃; the heat preservation time during aging heat treatment is 4-8 h.
2. The method according to claim 1, wherein the silver particles used in step 1) have a diameter of 0.01cm to 0.5 cm.
3. A copper alloy material prepared by the preparation method according to any one of claims 1 to 2.
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| CN110468297A (en) * | 2019-09-09 | 2019-11-19 | 上海电缆研究所有限公司 | A kind of high performance audio transmission alloy wire and preparation method thereof |
| CN111101008B (en) * | 2019-12-26 | 2021-08-17 | 浙江杭机新型合金材料有限公司 | High-strength high-conductivity copper-silver alloy material and preparation method thereof |
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| CN101054654A (en) * | 2006-04-11 | 2007-10-17 | 中国科学院金属研究所 | High-strength high-conductivity oxidation-resisting low-silver copper-base alloy and preparation thereof |
| CN101215681A (en) * | 2008-01-09 | 2008-07-09 | 浙江大学 | Solid solution aging technique for modifying Cu-Ag alloy rigidity and electric conductivity |
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| CN101054654A (en) * | 2006-04-11 | 2007-10-17 | 中国科学院金属研究所 | High-strength high-conductivity oxidation-resisting low-silver copper-base alloy and preparation thereof |
| CN101215681A (en) * | 2008-01-09 | 2008-07-09 | 浙江大学 | Solid solution aging technique for modifying Cu-Ag alloy rigidity and electric conductivity |
| CN101265558A (en) * | 2008-04-18 | 2008-09-17 | 浙江大学 | Solid solution and aging treatment method for cooperating Cu-Ag alloy cold drawing processing |
| CN102031467A (en) * | 2010-11-29 | 2011-04-27 | 东北大学 | Method for preparing in-situ deformation Cu-Ag composite material by using magnetic field |
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