CN112063941A - Preparation method of reinforced Cu-Cr-Zr alloy - Google Patents
Preparation method of reinforced Cu-Cr-Zr alloy Download PDFInfo
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- CN112063941A CN112063941A CN202010882045.1A CN202010882045A CN112063941A CN 112063941 A CN112063941 A CN 112063941A CN 202010882045 A CN202010882045 A CN 202010882045A CN 112063941 A CN112063941 A CN 112063941A
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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
Abstract
The invention discloses a preparation method of a reinforced Cu-Cr-Zr alloy, which comprises the following steps: carrying out solution treatment on a Cu-Cr-Zr cast rod prepared in advance, wherein the solution treatment temperature is 920-960 ℃, and the time is 0.5-2; carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to the solution treatment for multiple times; carrying out aging treatment on the Cu-Cr-Zr alloy, wherein the aging treatment temperature is 430-460 ℃, and the heat preservation time is 2-6 tools; carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to aging treatment for multiple times; and carrying out subzero treatment on the Cu-Cr-Zr alloy at the temperature of-170 to-190 ℃ for 1 to 3. The preparation method of the reinforced Cu-Cr-Zr alloy can prepare the Cu-Cr-Zr alloy with greatly improved strength and greatly improved conductivity.
Description
Technical Field
The invention relates to the technical field of copper alloy material processing, in particular to a preparation method of a reinforced Cu-Cr-Zr alloy.
Background
The Cu-Cr-Zr alloy has the characteristics of high strength, high electrical conductivity, good thermal conductivity, good oxidation resistance and the like, is considered to be the alloy with the most application prospect in high-strength and high-conductivity copper alloys, belongs to one of precipitation strengthening alloys, has excellent electric and thermal conductivity and tensile strength, and is mainly applied to manufacturing motors of automatic welding machines, electronic industry frame materials, electric railway locomotive sliding lines, large cast steel crystallizer materials and the like.
At present, the traditional preparation method of the Cu-Cr-Zr alloy material comprises the following steps: smelting → casting → post-treatment, and the research on the high-strength and high-conductivity Cu-Cr-Zr alloy is mainly focused on the research on the post-treatment (processes such as solution aging strengthening). At present, the strengthening technology adopted at home and abroad is solution quenching, cold deformation and aging, wherein the solution quenching forms supersaturated solid solution, the cold deformation can cause defects such as dislocation, vacancy and the like, so as to increase the nucleation rate during aging and form highly dispersed Cr particles and Cu during aging3The Zr particles strengthen the alloy.
How to improve the above process method to further process the Cu-Cr-Zr alloy to prepare the Cu-Cr-Zr alloy with high strength and high conductivity is the subject of intensive research by the present inventors.
Disclosure of Invention
The invention aims to provide a preparation method of a reinforced Cu-Cr-Zr alloy, which can prepare the Cu-Cr-Zr alloy with greatly improved strength and greatly improved conductivity.
In order to achieve the above object, the present invention provides a method for preparing a strengthened Cu-Cr-Zr alloy, comprising the steps of:
(1) carrying out solid solution treatment on a Cu-Cr-Zr cast rod prepared in advance;
(2) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to the solution treatment for multiple times;
(3) carrying out aging treatment on the Cu-Cr-Zr alloy;
(4) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to aging treatment for multiple times;
(5) and carrying out cryogenic treatment on the Cu-Cr-Zr alloy.
The preparation method of the reinforced Cu-Cr-Zr alloy comprises the step (1) of carrying out solid solution treatment at 920-960 ℃ for 0.5-2 h.
The preparation method of the reinforced Cu-Cr-Zr alloy comprises the step (2) and the step (4) of carrying out 2-4 times of ECAP extrusion cold deformation.
The invention relates to a preparation method of a reinforced Cu-Cr-Zr alloy, wherein the ECAP extrusion deformation process is carried out at room temperature.
The preparation method of the reinforced Cu-Cr-Zr alloy comprises the step (3) of ageing treatment at the temperature of 430-460 ℃ for 2-6 hours.
The preparation method of the reinforced Cu-Cr-Zr alloy comprises the step (5) of carrying out cryogenic treatment at-170 ℃ to-190 ℃ for 1-3 hours.
A reinforced Cu-Cr-Zr alloy prepared according to said method of preparation.
After the scheme is adopted, the preparation method of the reinforced Cu-Cr-Zr alloy carries out ECAP extrusion deformation on the Cu-Cr-Zr alloy after solution treatment, single slip or multiple slip occurs on coarse crystal grains in the crystal at the beginning of the extrusion deformation, and the coarse crystal grains are changed into a strip structure parallel to the shear strain direction from the original equiaxial crystal along with the continuous slip. Meanwhile, a large amount of dislocations are generated inside the large grains, and the dislocations are also evolved into small-angle subgrain boundaries in the process of further deformation, so that relatively coarse grains in the grains are developed into fine subgrain grains. As the amount of deformation increases, more dislocations appear in the structure, which are concentrated between the subgrains while forming equiaxed lines outside the subgrains. Finally, as the number of extrusion passes is increased, the position orientation among equiaxial crystals becomes very random, and the original large grains are finally refined into submicron or dozens of nanometers of superfine nano-crystals; the Cu-Cr-Zr alloy is subjected to cold deformation before aging, so that a large number of defects such as vacancies, dislocations and the like can be generated, the nucleation core of the second phase becomes more, the precipitation speed is accelerated, the second phase can be effectively promoted to be fully precipitated, the conductivity is correspondingly improved, and the mechanical and electrical properties of the material can be improved through the cold deformation before aging; the electric conductivity and tensile strength of the Cu-Cr-Zr alloy can be improved simultaneously by adopting cryogenic treatment on the Cu-Cr-Zr alloy, and the main reason for improving the electric conductivity of the alloy after cryogenic treatment is because the precipitation of second phase particles and the reduction of microscopic defects; it is known from the analysis by SEM and EDS that the main reason for strengthening after the cryogenic treatment is due to the diffusion precipitation of the second phase particles. The invention effectively combines the ECAP extrusion technology, the heat treatment technology and the cryogenic treatment technology to obviously improve the mechanical property and the electrical conductivity of the Cu-Cr-Zr. On one hand, ECAP and other channel extrusion can refine the crystal grains of the alloy, and simultaneously can generate the effect of work hardening, improve the tissue distribution and finally improve the strength of the material; on the other hand, after the alloy is extruded by the ECAP and other channels, a large number of dislocation and other microscopic defects are generated inside the alloy, the diffusion channels of Cr and Zr are increased, the nucleation positions of the Cr and Zr are obviously increased, a second phase can be fully precipitated in the subsequent heat treatment or deep cooling process, and various macroscopic properties of the Cu-Cr-Zr alloy are obviously improved due to the microscopic change of the alloy structure.
Drawings
FIG. 1 is a schematic view of an ECAP extrusion channel die used in an embodiment of the method for preparing the reinforced Cu-Cr-Zr alloy of the present invention;
FIG. 2 is a Cu-Cr-Zr metallographic structure diagram of a Cu-Cr-Zr alloy prepared by a first embodiment of the method for preparing a strengthened Cu-Cr-Zr alloy according to the invention;
FIG. 3 is a Cu-Cr-Zr metallographic structure diagram of a Cu-Cr-Zr alloy prepared by a second method for preparing a strengthened Cu-Cr-Zr alloy according to the present invention;
FIG. 4 is a metallographic structure diagram of Cu-Cr-Zr prepared by a third method for preparing a strengthened Cu-Cr-Zr alloy according to the present invention.
Detailed Description
The first embodiment is as follows:
the preparation method of the reinforced Cu-Cr-Zr alloy comprises the following steps:
(1) carrying out solution treatment on a Cu-Cr-Zr cast rod prepared in advance, wherein the diameter of the cast rod is 20mm, the solution treatment temperature is 960 ℃, and the time is 1 h;
(2) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to the solution treatment for 3 times, wherein each extrusion process is carried out at room temperature;
(3) carrying out aging treatment on the Cu-Cr-Zr alloy, wherein the aging treatment temperature is 450 ℃, and the heat preservation time is 4 h;
(4) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to aging treatment for 3 times, wherein each extrusion process is carried out at room temperature;
(5) and (3) carrying out subzero treatment on the Cu-Cr-Zr alloy at the subzero treatment temperature of-170 ℃ for 2 hours.
Referring to fig. 1, ECAP extrusion in the above steps (2) and (4) is also called equal channel angular extrusion, which is performed on a square extrusion die 1, the extrusion die 1 has an L-shaped channel 2, the cross-sectional diameter of the channel 2 in this embodiment is 20mm, one end of the channel 2 is opened on the upper surface, the other end is opened on the side surface, the cast rod 3 enters from the upper end of the channel 2 of the extrusion die 1 under the action of the extrusion force, the sample undergoes a large deformation of almost pure shear at the intersection of the channel 2, and then a strong plastic deformation is generated inside the sample, and uniform submicron crystals or nano-nodules can be generated after repeated extrusion: the ECAP extrusion is performed in one pass by introducing the casting bar 3 into the channel 2 at one end and withdrawing the bar from the channel 2 at the other end. In this example, a round bar having a diameter of 20mm and a length of 100mm was processed and subjected to ECAP extrusion. The whole extrusion process is carried out at room temperature. Referring to FIG. 2, a metallographic structure diagram of the prepared strengthened Cu-Cr-Zr alloy is shown.
Example two:
the embodiment adopts the prior art to prepare the reinforced Cu-Cr-Zr alloy, and comprises the following steps:
(1) carrying out solution treatment on a Cu-Cr-Zr cast rod prepared in advance, wherein the diameter of the cast rod is 20mm, the solution treatment temperature is 960 ℃, and the time is 1 h;
(2) and (3) carrying out aging treatment on the Cu-Cr-Zr alloy, wherein the aging treatment temperature is 450 ℃, and the heat preservation time is 4 h.
Example three:
the embodiment adopts the following steps to prepare the reinforced Cu-Cr-Zr alloy, and specifically comprises the following steps:
(1) carrying out solution treatment on a Cu-Cr-Zr cast rod prepared in advance, wherein the diameter of the cast rod is 20mm, the solution treatment temperature is 960 ℃, and the time is 1 h;
(2) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to the solution treatment for 3 times, wherein each extrusion process is carried out at room temperature. Referring to FIG. 3, a metallographic structure diagram of the prepared strengthened Cu-Cr-Zr alloy is shown.
Example four:
the embodiment adopts the following steps to prepare the reinforced Cu-Cr-Zr alloy, and specifically comprises the following steps:
(1) carrying out solution treatment on a Cu-Cr-Zr cast rod prepared in advance, wherein the diameter of the cast rod is 20mm, the solution treatment temperature is 960 ℃, and the time is 1 h;
(2) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to the solution treatment for 3 times, wherein each extrusion process is carried out at room temperature;
(3) the Cu-Cr-Zr alloy is subjected to aging treatment, the aging treatment temperature is 450 ℃, the heat preservation time is 4h, and referring to a metallographic structure diagram of the prepared strengthened Cu-Cr-Zr alloy shown in figure 4, the metallographic structure diagram is obtained.
Example five:
the embodiment adopts the following steps to prepare the reinforced Cu-Cr-Zr alloy, and specifically comprises the following steps:
(1) carrying out solution treatment on a Cu-Cr-Zr cast rod prepared in advance, wherein the diameter of the cast rod is 20mm, the treatment temperature is 960 ℃, and the time is 1 h;
(2) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to the solution treatment for 3 times, wherein each extrusion process is carried out at room temperature;
(3) and (3) carrying out subzero treatment on the Cu-Cr-Zr alloy at the subzero treatment temperature of-170 ℃ for 2 hours.
The following table shows the results of the test performance tests performed on the Cu-Cr-Zr alloys prepared in the above five examples:
by comparing the five examples, the reinforced Cu-Cr-Zr alloy prepared by the first example of the invention is a typical aging reinforced high-strength high-conductivity copper alloy, and is superior to the Cu-Cr-Zr alloy prepared by other examples in terms of tensile strength, HB and electric conductivity. The cold deformation before aging can effectively promote the sufficient precipitation of the second phase, because the cold deformation before aging can generate a large amount of defects such as vacancies, dislocations and the like, so that the nucleation core of the second phase becomes more, the precipitation speed is accelerated, the conductivity is correspondingly higher, and the mechanical and electrical properties of the material can be improved through the cold deformation before aging. The process of grain refinement during ECAP deformation is as follows: first, relatively coarse crystal grains in the crystal grains undergo single slip or multiple slip at the beginning of the extrusion deformation, and the coarse crystal grains develop into a long structure parallel to the shear strain direction from the original equiaxial crystal as the slip progresses. Meanwhile, a large amount of dislocations are generated inside the large grains, and the dislocations are also evolved into small-angle subgrain boundaries in the process of further deformation, so that relatively coarse grains in the grains are developed into fine subgrain grains. As the amount of deformation increases, more dislocations will appear in the structure, which subsequently collect between the subgrains while forming equiaxed grains outside the subgrains. Finally, with the increase of extrusion passes, the position orientation among equiaxed crystals becomes very random, and the original large grains are finally refined into submicron or dozens of nanometers of ultrafine nano-crystals.
The cryogenic treatment can simultaneously improve the conductivity and tensile strength of the Cu-Cr-Zr alloy, and the main reason for improving the conductivity of the alloy after cryogenic treatment is due to the precipitation of second phase particles and the reduction of microscopic defects; it is known from the analysis by SEM and EDS that the main reason for strengthening after the cryogenic treatment is due to the diffusion precipitation of the second phase particles. The combination of ECAP extrusion, heat treatment technology and cryogenic treatment technology can obviously improve the mechanical property and the electrical conductivity of Cu-Cr-Zr, because: on one hand, ECAP and other channel extrusion can refine the crystal grains of the alloy, and simultaneously can generate the effect of work hardening, improve the tissue distribution and finally improve the strength of the material; on the other hand, after the alloy is extruded by the ECAP and other channels, a large number of dislocation and other microscopic defects are generated inside the alloy, the diffusion channels of Cr and Zr are increased, the nucleation positions of the Cr and Zr are obviously increased, and a second phase can be fully precipitated in the subsequent heat treatment or deep cooling process. The microscopic change of the alloy structure finally obviously improves various macroscopic properties of the Cu-Cr-Zr alloy.
The embodiments of the present invention have been described in detail, but the description is only a preferred example of the present invention, and is not intended to limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the design of the present invention should fall within the protection scope defined by the claims of the present invention.
Claims (7)
1. The preparation method of the reinforced Cu-Cr-Zr alloy is characterized by comprising the following steps:
(1) carrying out solid solution treatment on a Cu-Cr-Zr cast rod prepared in advance;
(2) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to the solution treatment for multiple times;
(3) carrying out aging treatment on the Cu-Cr-Zr alloy;
(4) carrying out ECAP extrusion cold deformation on the Cu-Cr-Zr alloy subjected to aging treatment for multiple times;
(5) and carrying out cryogenic treatment on the Cu-Cr-Zr alloy.
2. The method of claim 1, wherein the solution treatment temperature in step (1) is 920-960 ℃ and the time is 0.5-2 hours.
3. The method for preparing the strengthened Cu-Cr-Zr alloy according to claim 1, wherein ECAP extrusion cold deformation is performed in 2-4 passes in both the step (2) and the step (4).
4. The method of making a strengthened Cu-Cr-Zr alloy according to claim 3, wherein said ECAP extrusion deformation process is performed at room temperature.
5. The method for preparing the strengthened Cu-Cr-Zr alloy according to claim 1, wherein the aging treatment temperature in the step (3) is 430-460 ℃, and the holding time is 2-6 h.
6. The method for preparing the strengthened Cu-Cr-Zr alloy according to claim 1, wherein the cryogenic treatment in the step (5) is carried out at a temperature of-170 ℃ to-190 ℃ for 1 to 3 hours.
7. A strengthened Cu-Cr-Zr alloy prepared according to the method of any one of claims 1 to 6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115305420A (en) * | 2022-09-02 | 2022-11-08 | 南京理工大学 | Method for preparing nano-layer sheet copper-chromium-zirconium alloy through composite plastic deformation |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07166308A (en) * | 1993-12-10 | 1995-06-27 | Mitsubishi Materials Corp | Production of cu-cr-zr copper alloy fine wire |
| WO2016047484A1 (en) * | 2014-09-25 | 2016-03-31 | 三菱マテリアル株式会社 | CASTING MOLD MATERIAL AND Cu-Cr-Zr ALLOY MATERIAL |
| CN105483582A (en) * | 2016-01-27 | 2016-04-13 | 西安交通大学 | Preparation method of high-strength and high-conductivity chromium-zirconium-copper alloy for high-speed railway power grid contact lines |
| CN107502777A (en) * | 2017-09-13 | 2017-12-22 | 临沂市科创材料有限公司 | A kind of method of In-sltu reinforcement Cu-Cr-Zr alloy high-temperature oxidation resistance |
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2020
- 2020-08-28 CN CN202010882045.1A patent/CN112063941A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07166308A (en) * | 1993-12-10 | 1995-06-27 | Mitsubishi Materials Corp | Production of cu-cr-zr copper alloy fine wire |
| WO2016047484A1 (en) * | 2014-09-25 | 2016-03-31 | 三菱マテリアル株式会社 | CASTING MOLD MATERIAL AND Cu-Cr-Zr ALLOY MATERIAL |
| CN105483582A (en) * | 2016-01-27 | 2016-04-13 | 西安交通大学 | Preparation method of high-strength and high-conductivity chromium-zirconium-copper alloy for high-speed railway power grid contact lines |
| CN107502777A (en) * | 2017-09-13 | 2017-12-22 | 临沂市科创材料有限公司 | A kind of method of In-sltu reinforcement Cu-Cr-Zr alloy high-temperature oxidation resistance |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115305420A (en) * | 2022-09-02 | 2022-11-08 | 南京理工大学 | Method for preparing nano-layer sheet copper-chromium-zirconium alloy through composite plastic deformation |
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Application publication date: 20201211 |