CN114649115A - double-Sn source type Nb3Preparation method of Sn superconducting wire - Google Patents

double-Sn source type Nb3Preparation method of Sn superconducting wire Download PDF

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CN114649115A
CN114649115A CN202210561604.8A CN202210561604A CN114649115A CN 114649115 A CN114649115 A CN 114649115A CN 202210561604 A CN202210561604 A CN 202210561604A CN 114649115 A CN114649115 A CN 114649115A
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superconducting wire
bronze
phi
wire
niobium composite
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CN114649115B (en
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郭强
陈建亚
武博
于宣
李建峰
刘向宏
冯勇
张平祥
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Western Superconducting Technologies Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
    • H01B12/02—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
    • H01B12/10—Multi-filaments embedded in normal conductors
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
    • H01B12/02—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by their form
    • H01B12/08—Stranded or braided wires
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
    • H01B12/16—Superconductive or hyperconductive conductors, cables, or transmission lines characterised by cooling
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
    • Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment

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Abstract

The invention relates to a double Sn source type Nb3The preparation method of the Sn superconducting wire rod comprises the following steps: s1, inserting a plurality of Nb rods into the casting cylinder, injecting Sn-containing bronze liquid, adding bronze covers at two ends of the casting cylinder, and sealing and welding by electron beams to obtain a bronze-niobium composite sheath; s2, heating and preserving heat of the bronze-niobium composite sheath obtained in the step S1 to obtain a bronze-niobium composite rod; s3, drilling the center position of the bronze-niobium composite rod obtained in the step S2, and inserting the Sn-Ta-Hf alloy rod into the bronze-niobium composite rod after drilling to obtain the Nb3A Sn superconducting wire subcomponent; s4, and a plurality of Nb obtained in the step S33The Sn superconducting wire sub-component is put into a Nb pipe and then put into an oxygen-free copper pipe to obtain a final blank, and finally, Nb is obtained3And a Sn superconducting wire. The method is used for preparingThe time consumption of the heat treatment of the process is shortened, and the critical current of the wire is obviously improved.

Description

double-Sn source type Nb3Preparation method of Sn superconducting wire
Technical Field
The invention belongs to the technical field of preparation of superconducting wires, and relates to a double-Sn-source Nb-type Nb3A method for preparing Sn superconducting wire.
Background
Nb3Sn superconducting wire is an important material for manufacturing large-scale particle accelerators, and the bronze Nb method is internationally delivered in batches in various scientific projects at present3Sn and ITER type Nb3The Jc of the Sn superconducting wire can reach 1100-1300A/mm under the conditions of 12T and 4.2K2. Obtaining stable and novel Nb with higher critical current density3The long-line preparation technology and the mass production capacity of the Sn wire rod are important basic material problems to be solved by guiding a large-scale particle accelerator.
Influence of Nb3The main factor of the critical current density of the Sn superconducting wire is Nb3Sn phase content and Nb3Sn grain boundary density for increasing Nb3The critical current-carrying capacity of the Sn superconducting wire needs to fully ensure that the Nb element in the wire is fully reacted to form Nb3A Sn phase. Bronze Nb method3The Sn wire is affected by a low Sn content in its bronze matrix, in which Nb element is not sufficiently reacted, and thus the critical current density of the wire is low. Further bronze method Nb3Sn is easy to crack due to work hardening because of high Sn content of bronze matrix, so the bronze Nb method3The Sn wire needs to be annealed for multiple times in the processing process, so that the processing period is extremely long. ITER type Nb3The Sn superconducting wire adopts an internal tin process route, so that the aperture of a drilled hole is required to be as large as possible in the CuNb composite rod drilling process for ensuring the Sn content in the wire, and the Sn is easy to penetrate through an interlayer Cu between an Nb core wire and an Sn source to break the wire in the wire stretching process. Furthermore ITER type Nb3Sn in the heat treatment processThe medium-temperature, medium-temperature and high-temperature treatment stages are required, the total heat treatment time is as long as 20 days, and the Nb can be treated by the long-time heat treatment3Sn crystal grains grow up, so that the critical current density of the wire rod is reduced.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a double-Sn-source Nb3The preparation method of the Sn superconducting wire has the advantages that the heat treatment time in the preparation process is shortened, and the critical current of the wire is obviously improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
double-Sn source type Nb3The preparation method of the Sn superconducting wire is characterized by comprising the following steps of:
s1, inserting a plurality of Nb rods into the casting cylinder, injecting bronze liquid containing Sn to form a bronze ingot, adding bronze covers at two ends of the casting cylinder, and sealing and welding by electron beams to obtain a bronze-niobium composite sheath;
s2, heating and preserving heat of the bronze-niobium composite sheath obtained in the step S1, and extruding the bronze-niobium composite sheath by adopting a reverse extrusion method to obtain a bronze-niobium composite rod;
s3, drilling the center position of the bronze-niobium composite rod obtained in the step S2, and inserting the Sn-Ta-Hf alloy rod into the bronze-niobium composite rod after drilling to obtain the Nb3Subcomponent of Sn superconducting wire, to obtain Nb3Drawing the Sn superconducting wire material sub-component, and drawing the drawn Nb3Straightening and cutting the Sn superconducting wire sub-components into a plurality of wires which are uniformly distributed;
s4, and a plurality of Nb obtained in the step S33Placing the Sn superconducting wire sub-component into a Nb tube, then placing the Nb tube and the oxygen-free copper tube to obtain a final blank, and drawing and twisting the obtained final blank to finally obtain Nb3An Sn superconducting wire.
Further, the content of Sn in the bronze liquid of step S1 is 5wt% to 10 wt%.
Further, the content of the boron element in the bronze liquid of the step S1 is 0.3wt% to 1wt%, and the content of the rhenium element is 0.5wt% to 2 wt%.
Further, the number of the Nb rods in the step S1 is 120-240, the specification of the Nb rods is phi 9 mm-phi 12mm, and the bronze ingot machine is added to the specification of phi 280 mm-phi 320 mm.
Further, in the step S2, the extrusion temperature is 500-650 ℃, and the heat preservation time is 30-60 min.
Further, the outer diameter of the bronze-niobium composite rod obtained in the step S2 is phi 45 mm-phi 75mm, the hole diameter of the drill hole in the step S3 is phi 18 mm-phi 23mm, and the hole diameter of the drill hole is 1.2-1.8mm larger than that of the Sn-Ta-Hf alloy rod.
Further, Nb is processed in step S33The drawing mode of the Sn superconducting wire sub-component comprises roller die drawing and conventional drawing when Nb is used3Stretching the Sn superconducting wire by adopting a rolling die drawing mode when the opposite side size of the Sn superconducting wire subcomponent is not less than 20mm, and when Nb is larger than3Stretching the Sn superconducting wire material by a conventional drawing mode after the opposite side size of the Sn superconducting wire material sub-component is less than 20mm, and obtaining the Nb after drawing3The size of the opposite side of the Sn superconducting wire subcomponent is 5 mm-15 mm.
Further, the inner wall of the Nb tube is electroplated with Ta with a thickness of 500 to 1000 μm in step S4. The outer diameter of the oxygen-free copper pipe is phi 60 mm-phi 75mm, the inner diameter of the oxygen-free copper pipe is phi 45 mm-phi 60mm, and the size of the Nb pipe is phi 44 mm-phi 59 mm.
Further, the drawing of the final billet in the step S4 includes roller die drawing and conventional drawing, the final billet is drawn by roller die drawing when the diameter of the final billet is greater than or equal to 20mm, the final billet is drawn by conventional drawing when the diameter of the final billet is less than 20mm, and then Nb is obtained by twisting and final drawing3The Sn superconducting wire has a twisting pitch of 15mm to 40 mm.
Further, the double Sn derived Nb3The method for producing the Sn superconducting wire further includes: nb obtained from step S43Sampling the Sn superconducting wire, carrying out heat treatment, and testing the critical current value after discharging; the heat treatment of the wire sample is carried out at 650 ℃, the heat preservation time is 250h, and the total time of the heat treatment of the sample is 12.5 days, wherein the time of the temperature rise is 1 day, and the time of the temperature reduction is 1 day.
Compared with the prior art, the invention has the following beneficial effects:
1. double Sn derived Nb3The low-temperature heat preservation process is not needed in the heat treatment process of the Sn superconducting wire, the medium-temperature and high-temperature heat preservation heat treatment can be directly carried out, and the critical current-carrying capacity of the finished heat treatment is higher than that of the bronze Nb method3Sn wire rod and ITER type Nb3Sn wire rod and Nb prepared by adopting method3Compared with ITER type Nb in the heat treatment process of the Sn superconducting wire3The heat treatment time of the Sn wire can be shortened by 7 days, the grain size is reduced, and the critical current of the wire is obviously improved.
2. Nb method with existing bronze3Sn superconducting wire preparation technology and ITER type Nb3Compared with the Sn superconducting wire preparation technology, the invention can effectively improve the processing hardening of bronze by adopting the mode of preparing the porous bronze ingot from the bronze ingot with low Sn content, so that the wire processing process does not need an annealing procedure. Because the bronze already contains a certain amount of Sn element, the hole diameter of the drilled hole can be properly reduced when the bronze-niobium composite rod is drilled, the ductility of the bronze can be effectively improved by combining the doping of the element in the bronze, the wire breakage risk in the wire processing process is greatly reduced, and the Nb in the wire heat treatment process can be inhibited3Sn phase is rapidly nucleated, and Nb is realized3Sn crystal grains are refined, so that the critical current of the wire is improved; due to the rhenium element doped in bronze, the double Sn source is Nb3Rhenium element effectively inhibits Nb in heat treatment process of Sn superconducting wire3Sn rapidly nucleates to realize Nb3Sn crystal grains are refined, and the critical current density of the wire rod is obviously improved.
3. The invention relates to a double-Sn source type Nb3The preparation method of the Sn superconducting wire rod realizes the double-Sn source type Nb by using low-Sn-content bronze to replace oxygen-free copper and combining an internal tin method3The preparation of Sn superconducting wire and the solution of Nb in bronze method3Insufficient Sn content in Sn superconducting wire, bronze work hardening breakage, ITER type Nb3The problem of increased wire breakage risk due to oversize drilling of Sn CuNb composite rod and long-time heat treatment of Nb3The growth of Sn crystal grains causes the problem of the reduction of the critical current density of the wire rod, and the Nb is greatly promoted3A process for preparing Sn superconducting wires in batches.
Other features of the present invention and advantages thereof will become apparent from the following detailed description of exemplary embodiments thereof, which proceeds with reference to the accompanying drawings.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description, serve to explain the principles of the invention.
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a schematic cross-sectional view of a bronze-niobium composite sheath according to the present invention;
FIG. 2 shows a Nb of the present invention3A schematic cross-sectional view of a Sn superconducting wire;
wherein: 1. an Nb rod; 2, bronze ingots; 3. an oxygen-free copper pipe; 4. a Nb tube; 5. nb3And a Sn superconducting wire subcomponent.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus consistent with certain aspects of the invention, as detailed in the appended claims.
In order to make those skilled in the art better understand the technical solution of the present invention, the following detailed description of the present invention is provided with reference to the accompanying drawings and examples.
double-Sn source type Nb3The preparation method of the Sn superconducting wire comprises the following steps:
s1, inserting a plurality of Nb rods 1 into the casting cylinder, injecting bronze liquid containing Sn to form a bronze ingot 2, machining, adding bronze covers at two ends of the casting cylinder, and sealing and welding through electron beams to obtain a bronze-niobium composite sheath;
s2, heating and preserving heat of the bronze-niobium composite sheath obtained in the step S1 through a high-current superconducting induction heating system, and extruding the bronze-niobium composite sheath by adopting a backward extrusion method to obtain a bronze-niobium composite rod;
s3, drilling the center position of the bronze-niobium composite rod obtained in the step S2, and inserting the Sn-Ta-Hf alloy rod into the bronze-niobium composite rod after drilling and cleaning are completed to obtain the Nb3Subcomponent 5 of Sn superconducting wire, pair of Nb3Drawing the Sn superconducting wire sub-component 5, and drawing the Nb3The Sn superconducting wire sub-components 5 are corrected and cut into a plurality of pieces and are uniformly distributed;
s4, and a plurality of Nb obtained in the step S33Placing the Sn superconducting wire sub-component 5 into an Nb tube 4, then placing the Nb tube 4 into an oxygen-free copper tube 3 to obtain a final blank, and drawing and twisting the obtained final blank to finally obtain Nb3An Sn superconducting wire.
Further, the content of Sn in the bronze liquid of step S1 is 5wt% to 10 wt%.
Specifically, the initial bronze hardness gradually increased with an increase in Sn content therein, and when the Sn content was 5wt.%, 6wt.%, 7wt.%, 8wt.%, 9wt.%, 10wt.%, 15wt.%, the bronze initial vickers hardness was 90, 92, 95, 97, 100, 100, 130, Nb, respectively3The hardness of the Sn superconducting wire sub-component is 125, 130, 140, 148, 155, 160 and 200 after three times of stretching (the pass processing rate is 17%), when the Sn content is 15wt.%, the hardness reaches 200, and only annealing but not drawing can be carried out at the moment, and Nb method is adopted for the bronze process3And after the Sn wire is subjected to heat treatment, the Sn content in the copper matrix is about 5wt.%, so that bronze with the Sn content of 5wt.% to 10wt.% is finally selected.
Furthermore, the content of boron element in the bronze liquid of the step S1 is 0.3wt% -1 wt%, the content of rhenium element is 0.5wt% -2 wt%, and the rhenium element is doped in the bronze, so that the novel double-Sn source type Nb is formed3Rhenium element effectively inhibits Nb in heat treatment process of Sn superconducting wire3Sn rapidly nucleates to realize Nb3Sn crystal grains are refined, and the critical current density of the wire rod is obviously improved.
Further, the number of the Nb rods 1 in the step S1 is 120-240, the specification of the Nb rods 1 is phi 9 mm-phi 12mm, and the bronze ingot 2 is machined to be phi 280 mm-phi 320 mm.
Further, the method for heating the bronze-niobium composite sheath in the step S2 is an induction heating method, so as to achieve that the inner and outer portions of the sheath quickly reach the extrusion temperature, effectively reduce the reaction of the Sn element and the Nb element in bronze caused by the excessively long heat preservation time, the extrusion temperature is 500-650 ℃, the heat preservation time is 30-60 min, and the bronze-niobium composite rod is extruded by a back extrusion method after the heat preservation is finished, so as to reduce the friction force in the extrusion process to the maximum extent, and finally obtain the bronze-niobium composite rod.
Further, the outer diameter of the bronze-niobium composite rod obtained in the step S2 is phi 45 mm-phi 75mm, the hole diameter of the drilled hole in the step S3 is phi 18 mm-phi 23mm, the hole diameter of the drilled hole is 1.2-1.8mm larger than that of the Sn-Ta-Hf alloy rod, the Sn-Ta-Hf alloy rod is inserted into the bronze-niobium composite rod after the drilled hole is formed, and the double-Sn source type Nb is obtained3Sn is respectively from a bronze liquid containing Sn and an Sn-Ta-Hf alloy rod.
Further, Nb is processed in step S33The drawing modes of the Sn superconducting wire subcomponent 5 comprise roller die drawing and conventional drawing when Nb is used3When the opposite side size of the Sn superconducting wire subcomponent 5 is more than or equal to 20mm, the Sn superconducting wire subcomponent is stretched in a rolling die drawing mode to reduce the wire breakage risk and the processing difficulty, and when Nb is adopted3Stretching the Sn superconducting wire material by a conventional drawing mode after the opposite side size of the Sn superconducting wire material subcomponent is less than 20mm, and obtaining Nb after drawing3And the size of the opposite side of the Sn superconducting wire sub-component is 5 mm-15 mm, and the Sn superconducting wire is cut to length after being formed.
Furthermore, in the step S4, Ta with a thickness of 500 μm to 1000 μm is electroplated on the inner wall of the Nb tube (to prevent Sn from penetrating the Nb tube to cause pollution to the copper matrix). The outer diameter of the oxygen-free copper pipe is phi 60 mm-phi 75mm, the inner diameter of the oxygen-free copper pipe is phi 45 mm-phi 60mm, and the size of the Nb pipe is phi 44 mm-phi 59 mm.
Further, the drawing manner of the final blank in the step S4 includes roller die drawing and conventional drawing, when the diameter of the final blank is more than or equal to 20mmThe billet is drawn by a rolling die drawing mode when the diameter of the final billet is less than 20mm, and is drawn by a conventional drawing mode, and then Nb is obtained by twisting and final drawing3The Sn superconducting wire has a twisting pitch of 15mm to 40 mm.
Further, the double Sn derived Nb3The method for producing the Sn superconducting wire further includes: nb obtained from step S43Sampling the Sn superconducting wire, carrying out heat treatment, and testing the critical current value after discharging; the heat treatment of the wire sample is carried out at 650 ℃, the heat preservation time is 250h, and the total time of the heat treatment of the sample is 12.5 days, wherein the time of the temperature rise is 1 day, and the time of the temperature reduction is 1 day.
Double Sn derived Nb3The low-temperature heat preservation process is not needed in the heat treatment process of the Sn superconducting wire, the medium-temperature and high-temperature heat preservation heat treatment can be directly carried out, and the critical current-carrying capacity of the finished heat treatment is higher than that of the bronze Nb method3Sn wire rod and ITER type Nb3Sn wire rod and Nb prepared by adopting method3Compared with ITER type Nb in the heat treatment process of the Sn superconducting wire3The heat treatment time of the Sn wire can be shortened by 7 days, and the critical current of the wire is obviously improved.
Nb method with existing bronze3Sn superconducting wire preparation technology and ITER type Nb3Compared with the Sn superconducting wire preparation technology, the invention can effectively improve the processing hardening of bronze by adopting the mode of preparing the porous bronze ingot from the bronze ingot with low Sn content, so that the wire processing process does not need an annealing procedure. Because the bronze already contains a certain amount of Sn element, the hole diameter of the drilled hole can be properly reduced when the bronze-niobium composite rod is drilled, the ductility of the bronze can be effectively improved by combining the doping of the element in the bronze, the wire breakage risk in the wire processing process is greatly reduced, and the Nb in the wire heat treatment process can be inhibited3Sn phase is rapidly nucleated, and Nb is realized3Sn crystal grains are refined, so that the critical current of the wire is improved; due to the rhenium element doped in bronze, the double Sn source is Nb3Rhenium element effectively inhibits Nb in heat treatment process of Sn superconducting wire3Sn rapidly nucleates to realize Nb3Sn crystal grains are refined, and the critical current density of the wire rod is obviously improved.
The invention relates to a pairSn source type Nb3The preparation method of the Sn superconducting wire rod realizes the double-Sn source type Nb by using low-Sn-content bronze to replace oxygen-free copper and combining an internal tin method3The preparation of Sn superconducting wire and the solution of Nb by bronze method3Insufficient Sn content in Sn superconducting wire, bronze work hardening breakage, ITER type Nb3The problem of increased wire breakage risk due to oversize drilling of Sn CuNb composite rod and long-time heat treatment of Nb3The growth of Sn crystal grains causes the problem of the reduction of the critical current density of the wire rod, and the Nb is greatly promoted3A process for preparing Sn superconducting wires in batches.
The following is described with reference to specific process procedures:
example 1
Step 1, inserting 120 Nb rods with the diameter of 9.0mm into a casting cylinder, injecting bronze liquid with the Sn content of 5wt.%, wherein the boron element content in the bronze liquid is 0.3wt.%, and the rhenium element content is 2.0wt.%, forming a bronze ingot 2, machining to the diameter of 280mm, adding bronze covers at two ends of the casting cylinder, and sealing and welding by electron beams to obtain a bronze-niobium composite sheath;
step 2, heating the bronze-niobium composite sheath obtained in the step 1 to 500 ℃ by adopting an induction heating method, preserving heat for 30min, and extruding the bronze-niobium composite sheath to phi 45mm by adopting a backward extrusion method to obtain a bronze-niobium composite rod;
step 3, drilling a hole phi of 18mm in the center of the bronze-niobium composite rod obtained in the step 2, inserting the Sn-Ta-Hf alloy rod into the bronze-niobium composite tube after drilling and cleaning to obtain Nb3Subcomponent 5 of Sn superconducting wire, pair of Nb3Rolling and drawing the Sn superconducting wire sub-component 5, conventionally drawing, forming, and then carrying out Nb3The Sn superconducting wire sub-component 5 is corrected and cut into a plurality of pieces which are uniformly distributed;
step 4, Nb obtained in step 33Placing the Sn superconducting wire sub-component into a Nb tube 4 with 500 mu mTa electroplated on the inner wall, and placing Nb3The Nb tube of the Sn superconducting wire sub-component is filled into an oxygen-free copper tube 3 to obtain a final blank, and the final blank is subjected to rolling die drawing, conventional drawing and twisting to obtain the double Sn source type Nb with the length of 11000m after final drawing3Sn superconducting wire rod, the specification of which is phi 1.0 mm.
Step 5, Nb obtained from step 43Sampling the Sn superconducting wire, carrying out heat treatment on the Sn superconducting wire according to a 665 ℃/250h schedule, and testing the critical current value of the Sn superconducting wire after the sample is taken out of the furnace.
The low-temperature performance test results of the samples are as follows:
Figure DEST_PATH_IMAGE002
example 1 the use of Nb with double Sn sources3The preparation method of the Sn superconducting wire successfully prepares a wire with the length of 11000m, and the critical current Ic of the wire is obviously higher than that of the wire prepared by the Nb method3Sn superconducting wire and ITER type Nb3The appearance characterization result of the Sn superconducting wire shows that the double Sn source type Nb is3Sn wire with grain size of 110 nm-120 nm and bronze Nb3Sn wire and ITER type Nb3The size of crystal grains in the Sn wire is 120 nm-150 nm. At the same time, the heat treatment of the wire sample is time consuming compared with bronze Nb3Sn wire and ITER type Nb3The Sn wire rod is shortened by 7 days.
Example 2
Step 1, inserting 180 Nb rods with the diameter of 9.0mm into a casting cylinder, injecting bronze liquid with the Sn content of 7wt.%, wherein the boron element content in the bronze liquid is 0.5wt.%, and the rhenium element content is 1.0wt.%, forming a bronze ingot 2, machining to the diameter of 300mm, adding bronze covers at two ends of the casting cylinder, and sealing and welding by electron beams to obtain a bronze-niobium composite sheath;
step 2, heating the bronze-niobium composite sheath obtained in the step 1 to 600 ℃ by adopting an induction heating method, preserving the temperature for 45min, and extruding the bronze-niobium composite sheath to phi 65mm by adopting a backward extrusion method to obtain a bronze-niobium composite rod;
step 3, drilling a hole with the diameter of 20mm at the center of the bronze-niobium composite rod obtained in the step 2, inserting the Sn-Ta-Hf alloy rod into the bronze-niobium composite tube after drilling and cleaning to obtain the Nb3Subcomponent 5 of Sn superconducting wire, pair of Nb3Rolling and drawing the Sn superconducting wire sub-component 5, conventionally drawing, forming, and then carrying out Nb3The Sn superconducting wire sub-component 5 is corrected and cut into a plurality of pieces which are uniformly distributed;
step 4, Nb obtained in step 33Placing the Sn superconducting wire sub-component into an Nb tube with 800 mu mTa electroplated inner wall, and placingWith Nb3The Nb tube of the Sn superconducting wire sub-component is filled into an oxygen-free copper tube 3 to obtain a final blank, and the final blank is subjected to rolling die drawing, conventional drawing and twisting to obtain a novel double-Sn-source Nb tube with the length of 10000m after final drawing3Sn superconducting wire rod, the specification of which is phi 1.0 mm.
Step 5, Nb obtained from step 43And (3) sampling the Sn superconducting wire, carrying out heat treatment on the Sn superconducting wire according to a 665 ℃/250h system, and testing the critical current value of the sample after the sample is taken out of the furnace.
The low-temperature performance test results of the samples are as follows:
Figure DEST_PATH_IMAGE004
this example uses a dual Sn source Nb3The preparation method of the Sn superconducting wire successfully prepares a wire with the length of 10000m, and the critical current of the wire is higher than that of the Nb wire prepared by a bronze method3Sn superconducting wire and ITER type Nb3Sn superconducting wire, novel dual Sn source type Nb3Sn wire with grain size of 110nm to 125nm and bronze Nb3Sn wire and ITER type Nb3The size of crystal grains in the Sn wire is 120 nm-150 nm. The time of the heat treatment process is shortened by 7 days.
Example 3
Step 1, inserting 240 Nb rods with the diameter of 12.0mm into a casting cylinder, injecting bronze liquid with the Sn content of 10wt.%, wherein the boron element content in the bronze liquid is 1.0wt.%, and the rhenium element content is 0.5wt.%, forming a bronze ingot 2, machining to the diameter of 320mm, adding bronze covers at two ends of the casting cylinder, and sealing and welding by electron beams to obtain a bronze-niobium composite sheath;
step 2, heating the bronze-niobium composite sheath obtained in the step 1 to 650 ℃ by adopting an induction heating method, preserving heat for 60min, and extruding the bronze-niobium composite sheath to phi 75mm by adopting a backward extrusion method to obtain a bronze-niobium composite rod;
step 3, drilling a hole phi 23mm in the center of the bronze-niobium composite rod obtained in the step 2, inserting the Sn-Ta-Hf alloy rod into the bronze-niobium composite tube after drilling and cleaning to obtain Nb3Subcomponent 5 of Sn superconducting wire, pair of obtained Nb3Rolling and drawing the Sn superconducting wire sub-component 5, conventionally drawing, forming, and carrying out Nb3Sn superconductivityThe wire sub-components 5 are straightened and cut into a plurality of wires which are uniformly distributed;
step 4, Nb obtained in step 33Placing the Sn superconducting wire sub-component into a Nb tube with the inner wall electroplated with 1000 mu mTa, and placing Nb3Putting the Nb pipe of the Sn superconducting wire sub-component into an oxygen-free copper pipe to obtain a final blank, and obtaining the double-Sn-source Nb with the length of 13000m after rolling die drawing, conventional drawing, twisting and final drawing3Sn superconducting wire rod, the specification of which is phi 1.0 mm.
Step 5, Nb obtained from step 43Sampling the Sn superconducting wire, carrying out heat treatment on the Sn superconducting wire according to a 665 ℃/250h schedule, and testing the critical current value of the Sn superconducting wire after the sample is taken out of the furnace.
The low-temperature performance test results of the samples are as follows:
Figure DEST_PATH_IMAGE006
this example uses a dual Sn source Nb3The preparation method of the Sn superconducting wire successfully prepares a wire with the length of 13000m, and the critical current of the wire is obviously higher than that of the Nb wire prepared by a bronze method3Sn superconducting wire and ITER type Nb3Sn superconducting wire, novel dual Sn source type Nb3Sn wire with grain size of 100nm to 120nm and bronze Nb3Sn wire and ITER type Nb3The size of crystal grains in the Sn wire is 120 nm-150 nm. The time of the heat treatment process is shortened by 7 days.
The invention relates to a double-Sn source type Nb3The preparation method of the Sn superconducting wire rod realizes the double-Sn source type Nb by using low-Sn-content bronze to replace oxygen-free copper and combining an internal tin method3The preparation of Sn superconducting wire and the solution of Nb in bronze method3Insufficient Sn content in Sn superconducting wire, bronze work hardening breakage, ITER type Nb3The problem of increasing the wire breakage risk due to overlarge drilling size of the Sn CuNb composite rod is solved, and Nb is thermally treated for a long time3The growth of Sn crystal grains causes the problem of the reduction of the critical current density of the wire rod, and the Nb is greatly promoted3A process for preparing Sn superconducting wires in batches.
The foregoing are merely exemplary embodiments of the present invention, which enable those skilled in the art to understand or practice the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention.
It is to be understood that the present invention is not limited to what has been described above, and that various modifications and changes may be made without departing from the scope thereof. The scope of the invention is limited only by the appended claims.

Claims (10)

1. double-Sn source type Nb3The preparation method of the Sn superconducting wire is characterized by comprising the following steps of:
s1, inserting a plurality of Nb rods (1) into the casting cylinder, injecting bronze liquid containing Sn to form a bronze ingot (2), adding bronze covers at two ends of the casting cylinder, and sealing and welding through electron beams to obtain a bronze-niobium composite sheath;
s2, heating and preserving heat of the bronze-niobium composite sheath obtained in the step S1, and extruding the bronze-niobium composite sheath by adopting a reverse extrusion method to obtain a bronze-niobium composite rod;
s3, drilling the center position of the bronze-niobium composite rod obtained in the step S2, and inserting the Sn-Ta-Hf alloy rod into the bronze-niobium composite rod after drilling to obtain the Nb3Sn superconducting wire subcomponent (5) to obtain Nb3Drawing the Sn superconducting wire subcomponent (5), and drawing the drawn Nb3The Sn superconducting wire sub-components (5) are corrected and cut into a plurality of equal-length components which are uniformly distributed;
s4, and a plurality of Nb obtained in the step S33The Sn superconducting wire sub-component (5) is arranged in an Nb tube (4) and then is arranged in an oxygen-free copper tube (3) to obtain a final blank, and the obtained final blank is drawn and twisted to finally obtain Nb3An Sn superconducting wire.
2. The dual Sn sourced Nb of claim 13The preparation method of the Sn superconducting wire is characterized in that the content of Sn in the bronze liquid in the step S1 is 5-10 wt%.
3. The dual Sn sourced Nb of claim 13The preparation method of the Sn superconducting wire is characterized in that the content of the boron element in the bronze liquid in the step S1 is 0.3-1 wt%, and the content of the rhenium element is 0.5-2 wt%.
4. The dual Sn sourced Nb of claim 13The preparation method of the Sn superconducting wire is characterized in that the number of the Nb rods (1) in the step S1 is 120-240, the specification of the Nb rods (1) is phi 9 mm-phi 12mm, and the bronze ingot (2) is machined to be phi 280 mm-phi 320 mm.
5. A dual Sn-sourced Nb as in claim 13The preparation method of the Sn superconducting wire is characterized in that the extrusion temperature in the step S2 is 500-650 ℃, and the heat preservation time is 30-60 min.
6. The dual Sn sourced Nb of claim 13The preparation method of the Sn superconducting wire is characterized in that the outer diameter of the bronze-niobium composite rod obtained in the step S2 is phi 45 mm-phi 75mm, the hole diameter of the drilled hole in the step S3 is phi 18 mm-phi 23mm, and the hole diameter of the drilled hole is 1.2-1.8mm larger than that of the Sn-Ta-Hf alloy rod.
7. The dual Sn sourced Nb of claim 13The method for producing a Sn superconducting wire rod is characterized in that Nb is treated in step S33The drawing mode of the Sn superconducting wire subcomponent (5) comprises roller die drawing and conventional drawing when Nb is used3When the opposite side size of the Sn superconducting wire subcomponent (5) is more than or equal to 20mm, the Sn superconducting wire subcomponent is stretched in a rolling die drawing mode, and when Nb is larger than or equal to 20mm3Stretching the Sn superconducting wire material by a conventional drawing mode after the opposite side size of the Sn superconducting wire material subcomponent is less than 20mm, and obtaining Nb after drawing3The size of the opposite side of the Sn superconducting wire subcomponent is 5 mm-15 mm.
8. The dual Sn sourced Nb of claim 13Sn superconducting wireThe preparation method of the material is characterized in that Ta with the thickness of 500-1000 μm is electroplated on the inner wall of the Nb pipe in the step S4, the outer diameter of the oxygen-free copper pipe is phi 60-phi 75mm, the inner diameter of the oxygen-free copper pipe is phi 45-phi 60mm, and the size of the Nb pipe is phi 44-phi 59 mm.
9. The dual Sn sourced Nb of claim 13The preparation method of the Sn superconducting wire is characterized in that the drawing modes of the final blank in the step S4 comprise roll die drawing and conventional drawing, when the diameter of the final blank is more than or equal to 20mm, the rolling die drawing is adopted to draw the final blank, when the diameter of the final blank is less than 20mm, the conventional drawing is adopted to draw the final blank, and then the Nb is obtained through twisting and final drawing3And a Sn superconducting wire, wherein the twisting pitch is 15mm to 40 mm.
10. The dual Sn sourced Nb of claim 13The method for preparing the Sn superconducting wire rod is characterized in that the double Sn source type Nb3The method for producing a Sn superconducting wire further includes: nb obtained from step S43Sampling the Sn superconducting wire, carrying out heat treatment, and testing the critical current value after discharging; the heat treatment of the wire sample is carried out at 650 ℃, the heat preservation time is 250h, and the total time of the heat treatment of the sample is 12.5 days, wherein the time of the temperature rise is 1 day, and the time of the temperature reduction is 1 day.
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