CN113488285B - Preparation method of Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction - Google Patents
Preparation method of Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction Download PDFInfo
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Abstract
The invention discloses a preparation method of a Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction, which comprises the following steps: filling Bi-2223 precursor powder into an AgAu alloy tube to obtain a first tube-loading composite body; secondly, assembling the single-core wire bundle into an AgAu alloy tube after drawing to obtain a second tube-loading composite body; thirdly, drawing and processing after hole-pattern rolling, and then rolling by adopting a flat roller to prepare a multi-core Bi-2223/AgAu strip; fourthly, obtaining the Bi-2223/AgAu superconducting strip through heat treatment. The invention adopts AgAu alloy tubes with low thermal conductivity as the inner sheath and the outer sheath, and adopts multi-roll pass rolling to ensure the cooperative deformation between the metal sheath and the ceramic core wire, and the prepared multi-core Bi-2223/AgAu strip has lower thermal conductivity, higher core wire density and critical current density, and is beneficial to the application on high-temperature superconducting current leads.
Description
Technical Field
The invention belongs to the technical field of superconducting material preparation, and particularly relates to a preparation method of a Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction.
Background
Bi-2223/AgAu strips produced by powder thimble method (PIT) with high critical current density (J)c) And lower thermal conductivity, are considered to be one of the best materials for manufacturing high temperature superconducting current leads. The critical current density of the Bi-2223/AgAu strip is one of the most important parameters of the application of the Bi-2223/AgAu superconductive strip, and the current-carrying performance of the current lead can be rapidly improved and the heat leakage quantity is gradually reduced by improving the critical current density of the Bi-2223/AgAu superconductive strip and optimizing the structure of the current lead. Therefore, the high-temperature superconducting current lead prepared from the Bi-2223/AgAu strip is developed and applied in more and more large-scale projects in the world. Switzerland plasma physical research Center (CRPP), Karlsruhe technical institute of Germany (KIT), Japan atomic force institute (JAERI) and Chinese academy of sciencesThe institute of physical and physical (ASIPP) undertakes the preparation work of high-temperature superconducting current leads of Large scientific engineering including International Thermal Experimental Reader (ITER), Wendelstein 7-X, Large logical device (LHD), JT-60SA, Large Hardon Cooler (LHC), EAST and the like.
Compared with the conventional Bi-2223/Ag strip, the Bi-2223/AgAu strip has lower current-carrying performance, which seriously limits the development of the domestic high-temperature superconducting current lead research. At present, the Bi-2223/AgAu strip preparation process mainly has the problem that the strength of the Ag-Au alloy is lower than that of the Ag-Mg alloy after annealing and is basically the same as that of pure Ag. Therefore, the influence of the AgAu/AgAu sheath with lower strength on the density and the silver/super interface of the core wire during mechanical deformation is different from that of the traditional Ag/AgMg sheath, and the final problems of lower density of the core wire of the strip material, uneven silver/super interface and the like can be caused. Therefore, the current carrying performance of the Bi-2223/AgAu prepared by different processes at present is generally reduced by 20-30% compared with that of the conventional Bi-2223/Ag strip.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a preparation method of a Bi-2223/AgAu superconducting tape with high current carrying and low heat conductivity aiming at the defects of the prior art. According to the method, the AgAu alloy pipe with low thermal conductivity is used as the inner and outer sleeves of the strip, and continuous rolling is performed by adopting a multi-roll pass rolling process, so that the cooperative deformation between the metal sleeve and the ceramic core wire is ensured, the core breaking is avoided, and the density of the core wire is increased, so that the prepared multi-core Bi-2223/AgAu strip has low thermal conductivity, high core wire density and critical current density, and is favorable for application to a high-temperature superconducting current lead.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows: a preparation method of a Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction is characterized by comprising the following steps:
under the protection of low-oxygen partial pressure atmosphere, vibrating a tube in a glove box by using a vibrating table, filling Bi-2223 precursor powder into an AgAu alloy tube with one closed end, and then sealing the other end of the AgAu alloy tube to obtain a first tube-filling composite body; the Bi-2223 precursor powder comprises Bi-2212 and CaCuO2And Bi-2212 and CaCuO2In a molar ratio of 1: 1;
step two, drawing the first tubulation complex obtained in the step one to obtain single-core wires, and then assembling a plurality of single-core wires into an AgAu alloy tube according to a set core wire structure in a bundling manner to obtain a second tubulation complex;
step three, performing hole-pattern rolling on the second tubulation composite body obtained in the step two, then performing drawing processing to obtain a multi-core Bi-2223/AgAu wire rod, and then rolling the multi-core wire rod into a multi-core Bi-2223/AgAu strip by adopting flat roll rolling;
step four, carrying out heat treatment on the multi-core Bi-2223/AgAu strip obtained in the step three under a low-oxygen atmosphere to obtain a Bi-2223/AgAu superconducting strip; the critical current density of the Bi-2223/AgAu superconducting strip is 1.53 multiplied by 10 under the self-field condition of 77K4A/cm2～1.9×104A/cm2。
The invention adopts AgAu5 wt% alloy with low thermal conductivity as the inner and outer jackets of the strip, the thermal conductivity of pure silver reaches 4000W/(m.K) when 20K, the thermal conductivity of silver-magnesium alloy is 80W/(m.K) when 20K, and the thermal conductivity of silver-gold alloy is only about 20W/(m.K), which is two orders of magnitude lower than that of pure silver and is only 1/4 of silver-magnesium alloy. The thermal conductivity of the 37-core Bi-2223/AgAu strip prepared by the invention is only 6.64W/(m.K) at 4.2K, and the application on a high-temperature superconducting current lead is facilitated.
The invention adopts the multi-roll pass rolling process to carry out continuous rolling, on one hand, the problems of irregular shape of the core wire and core breakage of the multi-core wire material caused by the fact that the metal sheath and the ceramic core wire cannot be deformed cooperatively can be avoided, and on the other hand, the density of the core wire can be increased more effectively, so that the strip material prepared by the method has lower heat conductivity, higher density of the core wire and critical current density, and is beneficial to the application on high-temperature superconducting current leads.
The preparation method of the Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction is characterized in that in the step one, the volume percentage of oxygen in the low-oxygen partial pressure atmosphere is 7.5%, the balance gas is argon, and the mass purity of the argon is 99.995%. The Bi-2223 phase forming process belongs to oxygen release, and in the initial stage of Bi-2223 phase formation, the low oxygen partial pressure and the balance gas are preferably selected to contribute to the generation of the Bi-2223 phase, so that the multi-core Bi-2223/AgAu superconducting tape can obtain more Bi-2223 phase content under the same heat treatment condition, the critical current density of the multi-core Bi-2223/AgAu superconducting tape is further improved, the powder is prevented from adsorbing other gases such as water and carbon dioxide, the bubbling phenomenon is prevented as much as possible, and the quality of the multi-core Bi-2223/AgAu superconducting tape is improved.
The preparation method of the high-current-carrying low-heat-conductivity Bi-2223/AgAu superconducting strip is characterized in that in the step one, the mass content of the Au element in the AgAu alloy tube is 5%, the outer diameter of the AgAu alloy tube is 12mm, and the wall thickness is 1 mm-1.5 mm. By adopting the AgAu alloy tube with the gold content, the thermal conductivity of the sheath material is greatly reduced, and further the conduction heat leakage of the Bi-2223/AgAu superconducting strip is reduced.
The preparation method of the Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction is characterized in that the opposite edge distance of the cross section of the single-core wire in the step two is 1.36-2.05 mm; the number of the single-core wires is 37, 55 or 85, and the mass content of the Au element in the AgAu alloy tube is 5%. The number of the preferable multiple single-core wires effectively increases the area of a high-current-carrying area, namely a silver/super interface, and further improves the critical current density of the Bi-2223/AgAu superconducting tape.
The preparation method of the Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction is characterized in that the pass processing rate of the pass rolling in the step three is 10%, and the pass processing rate of the drawing processing is 10% -20%. The optimal pass processing rate of pass rolling and drawing effectively promotes the uniform deformation of the second tubulation complex, improves the core wire density in the multi-core Bi-2223/AgAu strip, and is beneficial to preparing the multi-core Bi-2223/AgAu strip with high current-carrying performance.
The preparation method of the Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction is characterized in that in the fourth step, the volume content of oxygen in the low-oxygen atmosphere is 7.5%, the equilibrium gas is argon, the mass purity of the argon is 99.995%, and the temperature of the heat treatment is 822-828 ℃. The optimized heat treatment process parameters furthest ensure the generation of Bi-2223 phases and the improvement of intercrystalline connectivity, and further improve the high current-carrying performance of the multi-core Bi-2223/AgAu strip.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts the multi-roll pass rolling process to carry out continuous rolling, ensures the cooperative deformation between the metal sheath and the ceramic core wire, avoids core breaking, and increases the density of the core wire, so that the prepared multi-core Bi-2223/AgAu strip has lower heat conductivity, higher density of the core wire and critical current density, and is beneficial to the application on high-temperature superconducting current leads.
2. The invention adopts the process of combining multi-roll pass rolling with rotary swaging and drawing, not only increases the deformation uniformity of the core wire, but also can improve the density of the multi-core wire rod and the connectivity among crystal grains, and is more beneficial to preparing the multi-core Bi-2223/AgAu superconducting wire rod with high current-carrying performance.
3. Compared with the conventional plastic drawing processing, the invention adopts the multi-roll pass rolling process to carry out continuous rolling, maintains higher silver-to-super ratio to a greater extent and is beneficial to the processing of the multi-core Bi-2223/AgAu superconducting strip.
4. The invention adopts AgAu5 wt% alloy with low thermal conductivity as the inner and outer jackets of the strip, reduces the thermal conductivity of the Bi-2223/AgAu superconducting strip while ensuring high current carrying, and is beneficial to the application on high-temperature superconducting current leads.
5. The preparation method has the advantages of simple preparation process, reasonable design, low manufacturing cost and large popularization range, and can be used for industrial production of the multi-core Bi-2223/AgAu superconducting tape.
Drawings
FIG. 1 is a cross-sectional view of the structure of a second tubulation complex obtained in example 2 of the present invention.
FIG. 2 is a cross-sectional view of a second tubulation complex obtained in example 3 of the present invention.
Detailed Description
Example 1E of the inventionBi-2212 and CaCuO contained in the Bi-2223 precursor powder of example 32All are prepared by coprecipitation, and the specific procedures are described in Methods of introducing introduced lead into biological-2223 and the effects on phase reduction and superconduction properties of Dorris S E et al (Physica C, 1994,223(1-2), 163).
Example 1
The embodiment comprises the following steps:
step one, in a glove box with oxygen volume content of 7.5% and balance gas of argon gas with mass purity of 99.995%, vibrating and tubing by using a vibrating table under the condition that the vibration frequency is 40Hz, filling Bi-2223 precursor powder into an AgAu alloy tube with one closed end through a metal funnel, starting the vibrating table to vibrate the AgAu alloy tube at the same time, filling the Bi-2223 precursor powder into the AgAu alloy tube, and then sealing the other end of the AgAu alloy tube to obtain a first tubing composite; the Bi-2223 precursor powder comprises Bi-2212 and CaCuO2And Bi-2212 and CaCuO2The molar ratio of the AgAu alloy tube to the metal tube is 1:1, the outer diameter of the AgAu alloy tube is 12mm, the wall thickness of the AgAu alloy tube is 1mm, and the mass content of an Au element in the AgAu alloy tube is 5%;
step two, drawing the first tubulation complex obtained in the step one by adopting a pass machining rate of 15% to obtain a single-core wire with the diameter of 1.57mm, then processing the single-core wire into a hexagonal single-core wire with the edge distance of 1.36mm, sequentially sizing, cutting, straightening and heating to degas the hexagonal single-core wire according to 30cm, and assembling 37 hexagonal single-core wires subjected to heating and degassing into an AgAu alloy tube in a bundling manner to obtain a second tubulation complex; the outer diameter of the AgAu alloy tube is 12mm, the wall thickness is 1mm, and the mass content of Au in the AgAu alloy tube is 5%;
step three, performing pass rolling and drawing processing on the second tubulation complex obtained in the step two by adopting a pass processing rate of 10% to obtain a 37-core Bi-2223/AgAu wire rod with the diameter of 1.51mm, and then performing 2-pass back-and-forth rolling on the 37-core Bi-2223/AgAu wire rod by adopting flat roll rolling to obtain a 37-core Bi-2223/AgAu strip with the thickness of 0.3 mm; the reduction of each pass of the flat roll rolling is 0.6 mm;
step four, heating the 37-core Bi-2223/AgAu strip obtained in the step three to 826 ℃ at a heating rate of 100 ℃/h in an argon-oxygen mixed atmosphere with an oxygen partial pressure of 7.5%, carrying out heat preservation and heat treatment for 95h, and cooling to 25 ℃ along with a furnace to obtain a 37-core Bi-2223/AgAu superconducting strip; the mass purity of argon in the argon-oxygen mixed atmosphere is 99.995%.
Through detection, the 37-core Bi-2223/AgAu superconducting tape prepared in the embodiment has the critical current density at 77K and under the self-field of 1.3 multiplied by 10 from the conventional 37-core Bi-2223/AgAu tape4A/cm2Increased to 1.52 × 104A/cm2。
Example 2
The embodiment comprises the following steps:
step one, in a glove box with oxygen volume content of 7.5% and balance gas of argon gas with mass purity of 99.995%, vibrating and tubing by using a vibrating table under the condition that the vibration frequency is 40Hz, filling Bi-2223 precursor powder into an AgAu alloy tube with one closed end through a metal funnel, starting the vibrating table to vibrate the AgAu alloy tube at the same time, filling the Bi-2223 precursor powder into the AgAu alloy tube, and then sealing the other end of the AgAu alloy tube to obtain a first tubing composite; the Bi-2223 precursor powder comprises Bi-2212 and CaCuO2And Bi-2212 and CaCuO2The molar ratio of (1: 1), the outer diameter of the AgAu alloy tube is 12mm, the wall thickness is 1.1mm, and the mass content of an Au element in the AgAu alloy tube is 5%;
step two, drawing the first tubulation complex obtained in the step one by adopting a pass machining rate of 15% to obtain single-core wires with the diameter of 2.29mm, then processing the single-core wires into hexagonal wires with the edge distance of 2.05mm, sequentially sizing, cutting, straightening and heating the hexagonal wires according to 30cm, degassing, bundling and assembling 55 hexagonal single-core wires subjected to heating and degassing into an AgAu alloy tube, and filling a silver rod with the diameter of 1.57mm between the bundled and assembled single-core wires and the inner wall gap of the AgAu alloy tube to ensure that the single-core wires close to the edge of the inner wall are fully deformed in subsequent processing to obtain a second tubulation complex; the outer diameter of the AgAu alloy tube is 21mm, the wall thickness is 1.5mm, and the mass content of Au in the AgAu alloy tube is 5%;
step three, performing hole-pattern rolling and drawing processing on the second tubulation complex obtained in the step two by respectively adopting pass processing rates of 10% and 20% to obtain 55-core Bi-2223/AgAu wire rods with the diameter of 1.51mm, and then performing 2-pass back-and-forth rolling on the 55-core Bi-2223/AgAu wire rods by adopting flat roll rolling to obtain 37-core Bi-2223/AgAu strip with the thickness of 0.3 mm; the reduction of each pass of the flat roll rolling is 0.6 mm;
step four, heating the 55-core Bi-2223/AgAu strip obtained in the step three to 828 ℃ at a heating rate of 100 ℃/h in an argon-oxygen mixed atmosphere with an oxygen partial pressure of 7.5%, carrying out heat preservation and heat treatment for 95h, and cooling to 25 ℃ along with a furnace to obtain a 55-core Bi-2223/AgAu superconducting strip; the mass purity of argon in the argon-oxygen mixed atmosphere is 99.995%.
As a result of examination, the 55-core Bi-2223/AgAu superconducting tape prepared in this example had a critical current density at 77K under a self-field of 1.3X 10 from that of a conventional 37-core Bi-2223/AgAu tape4A/cm2Increased to 1.66X 104A/cm2。
Example 3
The embodiment comprises the following steps:
step one, in a glove box with oxygen volume content of 7.5% and balance gas of argon gas with mass purity of 99.995%, vibrating and tubing by using a vibrating table under the condition that the vibration frequency is 40Hz, filling Bi-2223 precursor powder into an AgAu alloy tube with one closed end through a metal funnel, starting the vibrating table to vibrate the AgAu alloy tube at the same time, filling the Bi-2223 precursor powder into the AgAu alloy tube, and then sealing the other end of the AgAu alloy tube to obtain a first tubing composite; the Bi-2223 precursor powder comprises Bi-2212 and CaCuO2And Bi-2212 and CaCuO2The molar ratio of the AgAu alloy tube to the metal tube is 1:1, the outer diameter of the AgAu alloy tube is 12mm, the wall thickness of the AgAu alloy tube is 1.5mm, and the mass content of an Au element in the AgAu alloy tube is 5%;
step two, drawing the first tubulation complex obtained in the step one by adopting a pass machining rate of 15% to obtain single-core wires with the diameter of 1.94mm, then processing the single-core wires into hexagonal wires with the side distance of 1.6mm, sequentially sizing, cutting, straightening and heating the hexagonal wires according to 30cm, degassing, bundling and assembling 85 single-core wires subjected to heating and degassing into an AgAu alloy tube, and filling a silver rod with the diameter of 1.11mm between the bundled and assembled single-core wires and the inner wall gap of the AgAu alloy tube to ensure that the single-core wires close to the edge of the inner wall are fully deformed in subsequent processing to obtain a second tubulation complex; the outer diameter of the AgAu alloy tube is 21mm, the wall thickness is 1.5mm, and the mass content of Au in the AgAu alloy tube is 5%;
step three, performing pass rolling and drawing processing on the second tubulation complex obtained in the step two by respectively adopting pass processing rates of 10% and 15% to obtain 85-core Bi-2223/AgAu wires with the diameter of 1.51mm, and then performing 2-pass back-and-forth rolling on the 85-core Bi-2223/AgAu wires by adopting flat roll rolling to obtain 37-core Bi-2223/AgAu strips with the thickness of 0.3 mm; the reduction of each pass of the flat roll rolling is 0.6 mm;
step four, heating the 85-core Bi-2223/AgAu strip obtained in the step three to 822 ℃ at a heating rate of 100 ℃/h in an argon-oxygen mixed atmosphere with an oxygen partial pressure of 7.5%, then carrying out heat preservation and heat treatment for 120h, and cooling to 25 ℃ along with a furnace to obtain an 85-core Bi-2223/AgAu superconducting strip; the mass purity of argon in the argon-oxygen mixed atmosphere is 99.995%.
As a result, the 85-core Bi-2223/AgAu superconducting tape prepared in the present example was examined to have a critical current density at 77K under a self-field of 1.3X 10 from that of a conventional 37-core Bi-2223/AgAu tape4A/cm2Increased to 1.9 × 104A/cm2。
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the present invention in any way. Any simple modification, change and equivalent changes of the above embodiments according to the technical essence of the invention are still within the protection scope of the technical solution of the invention.
Claims (4)
1. A preparation method of a Bi-2223/AgAu superconducting strip with high current carrying and low heat conduction is characterized by comprising the following steps:
step one, protecting the atmosphere with low oxygen partial pressureUnder protection, a vibrating table is adopted in a glove box for vibration tubulation, Bi-2223 precursor powder is filled into an AgAu alloy tube with one closed end, and then the other end of the AgAu alloy tube is sealed to obtain a first tubulation complex; the Bi-2223 precursor powder comprises Bi-2212 and CaCuO2And Bi-2212 and CaCuO2In a molar ratio of 1: 1; the mass content of the Au element in the AgAu alloy tube is 5%, the outer diameter of the AgAu alloy tube is 12mm, and the wall thickness is 1 mm-1.5 mm;
step two, drawing the first tubulation complex obtained in the step one to obtain single-core wires, and then assembling a plurality of single-core wires into an AgAu alloy tube according to a set core wire structure in a bundling manner to obtain a second tubulation complex; the opposite edge distance of the cross section of the single-core wire is 1.36-2.05 mm; the number of the single-core wires is 37, 55 or 85, and the mass content of Au in the AgAu alloy tube is 5%;
step three, performing hole-pattern rolling on the second tubulation composite body obtained in the step two, then performing drawing processing to obtain a multi-core Bi-2223/AgAu wire rod, and then rolling the multi-core wire rod into a multi-core Bi-2223/AgAu strip by adopting flat roll rolling;
step four, carrying out heat treatment on the multi-core Bi-2223/AgAu strip obtained in the step three under a low-oxygen atmosphere to obtain a Bi-2223/AgAu superconducting strip; the critical current density of the Bi-2223/AgAu superconducting strip is 1.53 multiplied by 10 under the self-field condition of 77K4A/cm2～1.9×104A/cm2。
2. The method as claimed in claim 1, wherein the volume percentage of oxygen in the low oxygen partial pressure atmosphere in the step one is 7.5%, the balance gas is argon, and the mass purity of argon is 99.995%.
3. The method for preparing a high current-carrying low thermal conductivity Bi-2223/AgAu superconducting tape as claimed in claim 1, wherein the pass processing rate of the pass rolling in step three is 10%, and the pass processing rate of the drawing processing is 10% -20%.
4. The method as claimed in claim 1, wherein the volume content of oxygen in the low oxygen atmosphere is 7.5%, the balance gas is argon, the mass purity of the argon is 99.995%, and the temperature of the heat treatment is 822-828 ℃.
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