CN115083689B - Preparation method of reinforced Cu-Nb composite wire - Google Patents
Preparation method of reinforced Cu-Nb composite wire Download PDFInfo
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Abstract
The invention discloses a preparation method of a reinforced Cu-Nb composite wire, which comprises the following steps: 1. vacuum annealing treatment is carried out on the Cu-Nb composite wire rod prepared by adopting a winding method and a multi-core cluster drawing method; 2. soaking in a foam box body filled with liquid nitrogen, fully cooling, and performing primary drawing; 3. and (3) continuously soaking the reinforced Cu-Nb composite wire into a foam box body filled with liquid nitrogen, fully cooling, continuously carrying out primary drawing, repeatedly cooling for multiple times, and carrying out primary drawing to obtain the reinforced Cu-Nb composite wire. According to the invention, liquid nitrogen cooling is adopted for the Cu-Nb composite wire before and during drawing, the occurrence of dynamic recovery recrystallization and dislocation slip in the drawing process are restrained by utilizing cooling, the generation of deformed twin crystals is promoted, grains are further refined, and the strength, the shaping and the conductivity of the reinforced Cu-Nb composite wire are improved.
Description
Technical Field
The invention belongs to the technical field of high-performance copper-based composite materials, and particularly relates to a preparation method of a reinforced Cu-Nb composite wire.
Background
The pulse strong magnetic field is a main carrier for realizing the high-strength magnetic field of more than 80 tesla, and the research of the international large magnet research centers for decades shows that the Cu-Nb and Cu-Ag composite material with high strength and high conductivity is the first choice of conductor materials. Because the preparation process of the Cu-Ag composite material is complex and the manufacturing cost is high, mass production of a production line is difficult to form, and the Cu-Nb composite material has remarkably improved material strength because of sufficient nanocrystallization and interface strengthening of Nb core wires, and has been successfully applied to several pulse magnet facilities internationally.
In 2012, the national pulse high-intensity magnetic field laboratory adopted a Cu-Nb composite material to generate a world record of a 100.7T high-intensity magnetic field, and the pulse high-intensity magnetic field record in China is 90.6T of the national pulse magnetic field center. Through calculation, the tensile strength of the wire rod is at least 1.1GPa, and the conductivity is required to reach 70% IACS in order to realize a pulse magnetic field of 100T and above. The Cu-Nb composite material prepared by normal temperature cluster drawing is close to the theoretical processing limit, and the tensile strength and the electrical conductivity are difficult to be matched with each other by more than 1GPa and 65% IACS, which brings a plurality of difficulties to the preparation of the material. Therefore, how to effectively reduce the work hardening of the materials and realize ideal matching of high strength and high conductivity is the key of the technical innovation of the materials.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of the reinforced Cu-Nb composite wire rod aiming at the defects of the prior art. The method carries out repeated liquid nitrogen cooling and one-pass drawing processing after vacuum annealing on the Cu-Nb composite wire prepared by combining the winding method with the multi-core cluster drawing method, inhibits the occurrence of dynamic recovery recrystallization and dislocation slip in the drawing process by using liquid nitrogen cooling, promotes the generation of deformed twin crystals and further refines grains, and simultaneously improves the strength, the shaping and the conductivity of the reinforced Cu-Nb composite wire.
In order to solve the technical problems, the invention adopts the following technical scheme: the preparation method of the reinforced Cu-Nb composite wire is characterized by comprising the following steps of:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire prepared by combining a winding method with a multi-core cluster drawing method;
soaking the Cu-Nb composite wire subjected to vacuum annealing treatment in the step one in a foam box body filled with liquid nitrogen for full cooling until no bubbles are generated on the surface, and then carrying out primary drawing;
and thirdly, continuously soaking the Cu-Nb composite wire subjected to primary drawing in the second step in a foam box body filled with liquid nitrogen for full cooling until no bubble is generated on the surface, continuously carrying out primary drawing, and repeatedly carrying out the full cooling process and the primary drawing process in the third step for multiple times to obtain the reinforced Cu-Nb composite wire.
The specific process of preparing the Cu-Nb composite wire by adopting a winding method and a multi-core bundling drawing method in the invention is disclosed in patent application No. 201610369202.2, namely a preparation method of a high-strength high-conductivity copper-niobium multi-core composite wire.
The invention firstly adopts the winding method to combine the Cu-Nb composite wires prepared by the multi-core bundling drawing method, namely, the Cu foil and the Nb foil are generally used as starting materials, the characteristics of large contact area and small starting size of the winding method are fully exerted, the advantages of fully thinning the core wire and forming the large-size section material by combining the multi-core bundling are combined, the problem of fully nanocrystallization of the core wire caused by large plastic deformation and work hardening is overcome, the potential of the strength of the material is fully developed, and the high-strength characteristic of the Cu-Nb composite wires is ensured on the basis; the processing stress of the Cu-Nb composite wire is eliminated through vacuum annealing treatment, the Cu-Nb composite wire is soaked in a foam box body containing liquid nitrogen for full cooling and then subjected to primary drawing, and the full cooling and primary drawing processes are continuously repeated, so that dynamic reversion and recrystallization in the drawing process and dislocation slip are effectively inhibited by utilizing cooling, the accumulated efficiency of dislocations is improved, the strength of the reinforced Cu-Nb composite wire is improved, the Cu-Nb composite wire is deformed in a lower temperature state after being fully cooled, the generation of deformed twin crystals is promoted, grains are further refined, the shaping of the reinforced Cu-Nb composite wire is effectively improved, part of large-angle grain boundaries are replaced by Luan Jing, the influence of the grain boundaries on the conductivity is reduced, the strength and the conductivity of the reinforced Cu-Nb composite wire are improved, and the reinforced Cu-Nb composite wire with high strength, high conductivity and high shaping is obtained.
The preparation method of the reinforced Cu-Nb composite wire is characterized in that the diameter of the Cu-Nb composite wire prepared by combining a winding method with a multi-core cluster drawing method in the first step is 11.0-13.1 mm. The Cu-Nb rod blank prepared by multi-core bundling is subjected to multi-pass drawing processing and then is subjected to work hardening, and the subsequent process can be performed by carrying out recrystallization annealing treatment in the diameter.
The preparation method of the reinforced Cu-Nb composite wire is characterized in that the temperature of the vacuum annealing treatment in the first step is 630-700 ℃ and the time is 3h. The technical parameters of the vacuum annealing treatment ensure that the Nb core wires in the Cu-Nb composite wires obtained by cluster drawing are recrystallized, and the Nb core wires are effectively prevented from being broken in the subsequent processing process.
Preparation of the reinforced Cu-Nb composite wireThe method is characterized in that the time for full cooling in the second step is 15min, the pass processing rate of the first drawing process is 19-20.5%, and the adopted lubricant is MoS 2 And (3) powder. The time of the full cooling enables the Cu-Nb composite wires after the vacuum annealing treatment to be fully cooled and approach the temperature of liquid nitrogen.
The preparation method of the reinforced Cu-Nb composite wire is characterized in that the full cooling time in the third step is 5-10 min, and the pass processing rate of the primary drawing process is 8-19%. The time of full cooling enables the Cu-Nb composite wire subjected to primary drawing to be fully cooled and to be close to the temperature of liquid nitrogen, and meanwhile, the preferred primary drawing pass working rate can enable the Cu-Nb composite wire to be more uniformly deformed, the Cu-Nb composite wire is prevented from breaking in the drawing process, and smooth molding of the reinforced Cu-Nb composite wire is ensured.
Compared with the prior art, the invention has the following advantages:
1. the invention carries out repeated liquid nitrogen cooling and one-pass drawing processing after vacuum annealing on the Cu-Nb composite wire prepared by combining the winding method with the multi-core cluster drawing method, and utilizes the cooling to inhibit the occurrence of dynamic recovery recrystallization and dislocation slip in the drawing process, promote the generation of deformed twin crystals and further refine grains, and simultaneously improve the strength, the shaping and the conductivity of the reinforced Cu-Nb composite wire.
2. Compared with normal temperature drawing, the invention has better effect of drawing refined grains after cooling by liquid nitrogen, and finer grain size after refining, and simultaneously improves the strength and the shaping of the reinforced Cu-Nb composite wire, and realizes good matching of tensile strength and plasticity.
3. Compared with normal temperature drawing, the invention promotes the generation of uniform and fine nanometer twin crystals in the Cu-Nb composite wire by adopting liquid nitrogen cooling and drawing, obviously enhances the plastic deformation capacity of the Cu-Nb composite wire, improves the elongation of the reinforced Cu-Nb composite wire by more than 20 percent and improves the tensile strength by about 5 percent.
The technical scheme of the invention is further described in detail through the drawings and the embodiments.
Drawings
Fig. 1 is a stress-strain graph of the reinforced Cu-Nb composite wire rod prepared in example 1 of the present invention and the conventional Cu-Nb composite wire rod prepared in comparative example 1.
Fig. 2 is a longitudinal section scanning electron microscope image of the reinforced Cu-Nb composite wire rod prepared in example 1 of the present invention.
Detailed Description
Example 1
The embodiment comprises the following steps:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire rod with the diameter of 13.1mm prepared by combining a winding method with a multi-core cluster drawing method; the temperature of the vacuum annealing treatment is 630 ℃ and the time is 3 hours;
soaking the Cu-Nb composite wires subjected to the vacuum annealing treatment in the step one in a foam box filled with liquid nitrogen for full cooling for 15min, and then adopting MoS 2 Powder lubrication, carrying out primary drawing processing to a diameter of 11.8mm;
step three, continuously soaking the Cu-Nb composite wire subjected to primary drawing in the step two in a foam box body filled with liquid nitrogen for full cooling, continuously carrying out primary drawing, and repeatedly carrying out the full cooling process and the primary drawing process in the step three for multiple times to obtain the reinforced Cu-Nb composite wire with the diameter of 6.7mm; the diameters of the corresponding wires after the primary drawing and repeated primary drawing process are as follows: 10.7mm, 9.82mm, 8.5mm, 7.94mm, 7.33mm, 6.7mm; the time for full cooling is 5 min-10 min.
Comparative example 1
The comparative example comprises the following steps:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire rod with the diameter of 13.1mm by adopting a winding method and a multi-core cluster drawing method; the temperature of the vacuum annealing treatment is 630 ℃ and the time is 3 hours;
step two, carrying out multi-pass drawing on the Cu-Nb composite wire subjected to the vacuum annealing treatment in the step one, and adopting MoS 2 Powder lubrication to obtainTo a conventional Cu-Nb composite wire with a diameter of 6.7mm; the diameters of the corresponding wires after the multi-pass drawing are as follows: 11.8mm, 10.7mm, 9.82mm, 8.5mm, 7.94mm, 7.33mm, 6.7mm.
According to detection, the specified plastic elongation strength (Rp 0.2) of the reinforced Cu-Nb composite wire prepared in the embodiment 1 of the invention is 827MPa, which is improved by 4.9% compared with 788MPa of the specified plastic elongation strength of the conventional Cu-Nb composite wire with the same size prepared in the comparative example 1 by room temperature drawing, the plastic elongation is improved by 14.1%, and the good matching of the tensile strength and the plasticity is realized.
Fig. 1 is a stress-strain graph of the reinforced Cu-Nb composite wire rod prepared in example 1 of the present invention and the conventional Cu-Nb composite wire rod prepared in comparative example 1, and it is understood from fig. 1 that the predetermined plastic elongation strength (rp 0.2) of the reinforced Cu-Nb composite wire rod prepared in example 1 of the present invention is 827MPa and the predetermined plastic elongation strength (rp 0.2) of the conventional Cu-Nb composite wire rod of the same size prepared by room temperature drawing in comparative example 1 is 788MPa.
Fig. 2 is a scanning electron microscope image of a longitudinal section of the reinforced Cu-Nb composite wire rod prepared in example 1 of the present invention, and it is understood from fig. 2 that the longitudinal section of the reinforced Cu-Nb composite wire rod prepared in example 1 of the present invention shows no deformed twin compared with the conventional Cu-Nb composite wire rod prepared by normal temperature drawing in comparative example 1.
Example 2
The embodiment comprises the following steps:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire rod with the diameter of 11.0mm prepared by combining a winding method with a multi-core cluster drawing method; the temperature of the vacuum annealing treatment is 700 ℃ and the time is 3 hours;
soaking the Cu-Nb composite wire subjected to vacuum annealing treatment in the first step in a foam box body filled with liquid nitrogen, fully cooling for 15min, and then carrying out primary drawing processing until the diameter is 9.82mm;
step three, continuously soaking the Cu-Nb composite wire subjected to primary drawing in the step two in a foam box body containing liquid nitrogen for full cooling, continuously carrying out primary drawing, and repeatedly carrying out the full cooling process and the primary drawing process in the step three for multiple times to obtain the reinforced Cu-Nb composite wire with the diameter of 2.71mm; the diameters of the corresponding wires after the primary drawing and repeated primary drawing process are as follows: 8.5mm, 7.94mm, 7.33mm, 6.7mm, 6.21mm, 5.71mm, 5.32mm, 5.08mm, 4.87mm, 4.67mm, 4.48mm, 4.3mm, 4.2mm, 3.95mm, 3.83mm, 3.64mm, 3.35mm, 3.21mm, 3.12mm, 3.08mm, 2.95mm, 2.83mm, 2.71mm; the time for full cooling is 5 min-10 min.
Comparative example 2
The comparative example comprises the following steps:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire rod with the diameter of 11.0mm prepared by combining a winding method with a multi-core cluster drawing method; the temperature of the vacuum annealing treatment is 700 ℃ and the time is 3 hours;
carrying out multi-pass drawing on the Cu-Nb composite wire subjected to the vacuum annealing treatment in the step one to obtain a conventional Cu-Nb composite wire with the diameter of 2.71mm; the diameters of the corresponding wires after the multi-pass drawing are as follows: 9.82mm, 8.5mm, 7.94mm, 7.33mm, 6.7mm, 6.21mm, 5.71mm, 5.32mm, 5.08mm, 4.87mm, 4.67mm, 4.48mm, 4.3mm, 4.2mm, 3.95mm, 3.83mm, 3.64mm, 3.35mm, 3.21mm, 3.12mm, 3.08mm, 2.95mm, 2.83mm, 2.71mm.
According to detection, the temperature tensile strength (Rm) of the reinforced Cu-Nb composite wire prepared in the embodiment 2 of the invention is 1219MPa, the specified plastic elongation strength (Rp 0.2) is 760MPa, and compared with the specified plastic elongation strength of the conventional Cu-Nb composite wire with the same size prepared in the comparative example 2 by room temperature drawing, the specified plastic elongation strength is improved by 6.3%, the plastic elongation percentage is improved by 15.1%, and the good matching of the tensile strength and the plasticity is realized.
Example 3
The embodiment comprises the following steps:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire rod with the diameter of 12.0mm prepared by combining a winding method with a multi-core cluster drawing method; the temperature of the vacuum annealing treatment is 660 ℃, and the time is 3 hours;
soaking the Cu-Nb composite wire subjected to vacuum annealing treatment in the first step in a foam box body filled with liquid nitrogen, fully cooling for 15min, and then carrying out primary drawing processing until the diameter is 10.7mm;
step three, continuously soaking the Cu-Nb composite wire subjected to primary drawing in the step two in a foam box body containing liquid nitrogen for full cooling, continuously carrying out primary drawing, and repeatedly carrying out the full cooling process and the primary drawing process in the step three for multiple times to obtain the reinforced Cu-Nb composite wire with the diameter of 3.08mm; the diameters of the corresponding wires after the primary drawing and repeated primary drawing process are as follows: 9.82mm, 8.5mm, 7.94mm, 7.33mm, 6.7mm, 6.21mm, 5.71mm, 5.32mm, 5.08mm, 4.87mm, 4.67mm, 4.48mm, 4.3mm, 4.2mm, 3.95mm, 3.83mm, 3.64mm, 3.35mm, 3.21mm, 3.12mm, 3.08mm; the time for full cooling is 5 min-10 min.
Comparative example 3
The comparative example comprises the following steps:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire rod with the diameter of 12.0mm by adopting a winding method and a multi-core cluster drawing method; the temperature of the vacuum annealing treatment is 660 ℃, and the time is 3 hours;
carrying out multi-pass drawing on the Cu-Nb composite wire subjected to the vacuum annealing treatment in the step one to obtain a conventional Cu-Nb composite wire with the diameter of 3.08mm; the diameters of the corresponding wires after the multi-pass drawing are as follows: 10.7mm, 9.82mm, 8.5mm, 7.94mm, 7.33mm, 6.7mm, 6.21mm, 5.71mm, 5.32mm, 5.08mm, 4.87mm, 4.67mm, 4.48mm, 4.3mm, 4.2mm, 3.95mm, 3.83mm, 3.64mm, 3.35mm, 3.21mm, 3.12mm, 3.08mm.
According to detection, the room temperature tensile strength (Rm) of the reinforced Cu-Nb composite wire prepared in the embodiment 3 of the invention is 1162MPa, and compared with the room temperature tensile strength of a conventional Cu-Nb composite wire with the same size prepared in the comparative embodiment 3 by room temperature drawing, the room temperature tensile strength is improved by 2.4%, the plastic deformation elongation is improved by 16.2%, and good matching of the tensile strength and the plasticity is realized.
The above description is only of the preferred embodiments of the present invention, and is not intended to limit the present invention. Any simple modification, variation and equivalent variation of the above embodiments according to the technical substance of the invention still fall within the scope of the technical solution of the invention.
Claims (5)
1. The preparation method of the reinforced Cu-Nb composite wire is characterized by comprising the following steps of:
step one, carrying out vacuum annealing treatment on a Cu-Nb composite wire prepared by combining a winding method with a multi-core cluster drawing method;
soaking the Cu-Nb composite wire subjected to vacuum annealing treatment in the step one in a foam box body filled with liquid nitrogen for full cooling until no bubbles are generated on the surface, and then carrying out primary drawing;
and thirdly, continuously soaking the Cu-Nb composite wire subjected to primary drawing in the second step in a foam box body filled with liquid nitrogen for full cooling until no bubble is generated on the surface, continuously carrying out primary drawing, and repeatedly carrying out the full cooling process and the primary drawing process in the third step for multiple times to obtain the reinforced Cu-Nb composite wire.
2. The method for producing a reinforced Cu-Nb composite wire according to claim 1, wherein the diameter of the Cu-Nb composite wire produced by the winding method in combination with the multi-core bundle drawing method in the step one is 11.0mm to 13.1mm.
3. The method for producing a reinforced Cu-Nb composite wire according to claim 1, wherein the vacuum annealing treatment in the step one is performed at a temperature of 630 ℃ to 700 ℃ for 3 hours.
4. The method for producing a reinforced Cu-Nb composite wire according to claim 1, wherein the time for sufficient cooling in the second step is 15 minutes, and the lubricant used for the single drawing pass with the working ratio of 19 to 20.5% is MoS 2 And (3) powder.
5. The method for producing a reinforced Cu-Nb composite wire according to claim 1, wherein the time for sufficient cooling in the third step is 5 to 10 minutes, and the pass processing rates of the one-pass drawing process are all 8 to 19%.
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| JP2865798B2 (en) * | 1990-04-20 | 1999-03-08 | 株式会社フジクラ | Method for producing magnet wire made of Cu-Nb alloy conductor |
| CN101509112A (en) * | 2009-04-03 | 2009-08-19 | 西北有色金属研究院 | Process for producing Cu-Nb composite material |
| CN102168201A (en) * | 2011-03-31 | 2011-08-31 | 西北有色金属研究院 | Short-flow preparation method for Cu-Nb composite material |
| CN105869778B (en) * | 2016-05-30 | 2017-09-19 | 西北有色金属研究院 | A kind of preparation method of high-strength high-conductivity copper niobium Multicore composite material |
| CN112007949B (en) * | 2020-08-27 | 2022-02-08 | 西北有色金属研究院 | Preparation method of reinforced Cu-Nb composite wire |
| CN114643296A (en) * | 2022-03-21 | 2022-06-21 | 西北有色金属研究院 | Preparation method of high-strength and high-toughness Cu-Nb-Cu composite wire |
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