CN104022454B - Preparation method of Nb3Al superconducting wire rod - Google Patents
Preparation method of Nb3Al superconducting wire rod Download PDFInfo
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- CN104022454B CN104022454B CN201410288807.XA CN201410288807A CN104022454B CN 104022454 B CN104022454 B CN 104022454B CN 201410288807 A CN201410288807 A CN 201410288807A CN 104022454 B CN104022454 B CN 104022454B
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Abstract
The invention discloses a preparation method of an Nb3Al superconducting wire rod. The preparation method comprises the steps of firstly producing a plurality of Cu/Nb-Al single-core bars at room temperature by virtue of hydrostatic extrusion, then mounting the Cu/Nb-Al single-core bars into a Cu tube, machining to obtain a Cu/Nb-Al composite wire rod, and finally carrying out heat treatment so as to obtain the Nb3Al superconducting wire rod. The preparation method has the beneficial effects that the composite wire rod formed by winding an Nb foil and an Al foil is subjected to extrusion processing at the room temperature by virtue of a hydrostatic extrusion technique, so that the combination between the Nb foil and the Al foil is improved due to high-deformation plastic deformation, and the problem that the critical current density of the finished Nb3Al superconducting wire rod is influenced due to the uneven deformation of the Nb foil and the Al foil in a preparation process of an Nb3Al precursor wire rod by virtue of a winding method is solved; the method is simple, is suitable for the preparation of superconducting long wires, is beneficial to the large-scale popularization and application and has a huge commercial value.
Description
Technical field
The invention belongs to low temperature superconducting material preparation method technical field, be specifically related to a kind of Nb3The preparation method of Al superconducting wire.
Background technology
Nb3Al is current superconducting transition temperature (Tc), critical current density (Jc) and upper critical field (Hc2) etc. the best low temperature superconducting material of comprehensive practical performance.It and Nb3Sn compares, TcReach 19.3K, fall within A15 structural intermetallic compounds and Grain boundary pinning superconductor；And there is higher Hc2With more preferable High-Field JcCharacteristic；It is of particular importance that it compares Nb3Sn has more excellent stress-strain and allows characteristic.Therefore, Nb3Al superconducting wire is considered there are huge potentiality in the superconducting magnet application such as pyromagnetic constraint fusion reactor (ITER) of future generation, high-energy particle accelerator (LHC) and nuclear magnetic resonance spectrometer (NMR).According to the difference of heat treatment mode, Nb3Al superconducting wire can be divided into two kinds, and one is Nb based on " low temperature diffusion heat treatment "3Al superconducting wire, another kind is the Nb based on " high temperature rapid heating and cooling (RHQ) with become phase heat treatment "3Al superconducting wire.For guarantee presoma wire rod in low temperature diffusion heat treatment process, Nb and Al reacts generation Nb completely3Al superconductor, the diffusion spacing of Nb and Al should be less than 200nm, and i.e. in presoma wire rod, Al core diameter or Al paper tinsel thickness need to be less than 200nm.The former preparation technology is simple, with low cost, but performance is relatively low, main magnetic field intensity less than 100, the Nb of 000 Gauss3Al superconducting magnet；The latter's performance is more excellent, complex manufacturing technology, is mainly used in the magnetic field intensity Nb higher than 150,000 Gauss3Al superconducting magnet.
Nb3The preparation process of Al superconducting wire is divided into " prepared by presoma wire rod " and " heat treatment " two parts, and wherein the preparation of presoma wire rod currently mainly has winding method and tiretube process two kinds.In general, the long Nb of km3The plastic working of Al presoma wire rod, Nb and Al need to be carried out stress relief annealing, but owing to Nb-Al initial reaction temperature is about 650 DEG C, and the stress relief annealing temperature of Nb is at about 700 DEG C, Nb is carried out the interface diffusion and reaction that stress relief annealing can cause Nb-Al, affecting the plastic working that presoma wire rod is follow-up, therefore this presoma wire rod cannot carry out stress relief annealing to Nb in whole plastic processing.Owing in winding method, the thickness of Al paper tinsel is more much smaller than the diameter of Al rod in tiretube process, therefore, compared to tiretube process, the plastic working amount of winding method presoma wire rod is less, it is easier to processing.
Nb is prepared in the most common winding method3During Al presoma wire rod, it is common that Nb paper tinsel and Al paper tinsel are wound in Nb or Cu metal bar, then by drawing or milling method, it is processed into Nb-Al single rod, then carries out multicore assembling, and process growth line.The method there is the problem that owing in winding process, the combination of Nb paper tinsel and Al paper tinsel is not the compactest, causes wire rod in follow-up drawing or the rolling course of processing, and the deformation of Nb paper tinsel and Al paper tinsel is uneven, thus affects the long Nb of km3The plastic working uniformity of Al presoma wire rod, and final finished Nb3The critical current density performance of Al superconducting wire.
Summary of the invention
It is an object of the invention to provide a kind of Nb3The preparation method of Al superconducting wire, solves winding method and prepares Nb3During Al presoma wire rod, Nb paper tinsel and the deformation of Al paper tinsel are uneven thus affect finished product Nb3The problem of the critical current density of Al wire rod.
The technical solution adopted in the present invention is: a kind of Nb3Many Cu/Nb-Al single rods, first with hydrostatic extrusion fabrication techniques Cu/Nb-Al single rod, are then encased in Cu pipe, are processed into Cu/Nb-Al composite wire, finally by being thermally treated resulting in Nb by the preparation method of Al superconducting wire3Al superconducting wire.
The feature of the present invention also resides in,
Specifically include following steps:
Step 1: make Cu/Nb-Al single rod
To be wound on Cu rod after Nb paper tinsel and Al paper tinsel superposition and load in Cu canning tube, it is thus achieved that Cu/Nb-Al complex；At room temperature utilize hydrostatic extrusion method, with the speed of 1～5m/min, Cu/Nb-Al complex is extruded into bar, it is thus achieved that Cu/Nb-Al single rod；
Step 2: tubulature drawing
The Cu/Nb-Al single rod many steps 1 obtained is encased in Cu pipe, and with 10～the pass deformation rate of 20%, by cold drawing or cold rolling process, is processed into multicore Cu/Nb-Al composite wire；
Step 3: heat treatment
Multicore Cu/Nb-Al composite wire step 2 obtained is put into and is carried out heat treatment in Ar atmosphere or vacuum heat treatment furnace and get final product.
In step 1, Nb paper tinsel and Al paper tinsel width are 100～300mm, and Nb paper tinsel thickness is 0.03～0.3mm, and Al paper tinsel thickness is the 1/3 of Nb paper tinsel.
The thickness that in step 1, Nb-Al is wound on Cu rod is 1～2 with the ratio of Cu rod diameter.
Step 1 obtains Cu/Nb-Al single rod a diameter of 1.0～10.0mm.
In step 2, Cu/Nb-Al single rod is 19.
The multicore Cu/Nb-Al composite wire a diameter of 0.1～1.5mm obtained in step 2.
In step 3, the temperature of heat treatment is 750 DEG C～950 DEG C, and temperature retention time is 10～100h.
The invention has the beneficial effects as follows: one Nb of the present invention3The preparation method of Al superconducting wire, uses hydrostatic extrusion technology, and the single bar after winding Nb paper tinsel and Al paper tinsel carries out room temperature extruding so that the combination between Nb paper tinsel and Al paper tinsel is improved by the extruding of aximal deformation value, solves winding method and prepares Nb3During Al presoma wire rod, Nb paper tinsel and the deformation of Al paper tinsel are uneven thus affect finished product Nb3The problem of the critical current density of Al wire rod, method is simple, is suitable for the preparation of the long line of superconduction, the most large-scale popularization and application, has huge commercial value.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is described in detail.
One Nb of the present invention3The preparation method of Al superconducting wire, specifically includes following steps:
Step 1: make Cu/Nb-Al single rod
By width be 100～300mm, thickness be 0.03～0.3mm Nb paper tinsel and width be 100～300mm, thickness be 0.01～0.1mm Al paper tinsel superposition after be wound on Cu rod and load in Cu canning tube, the thickness that Nb-Al is wound on Cu rod is 1～2 with the ratio of Cu rod diameter, obtain Cu/Nb-Al complex, at room temperature utilize hydrostatic extrusion method, with the speed of 1～5m/min, Cu/Nb-Al complex is extruded into bar, it is thus achieved that the Cu/Nb-Al single rod of a diameter of 1.0～10.0mm；
Step 2: tubulature drawing
The Cu/Nb-Al single rod 19 described steps 1 obtained is encased in Cu pipe, and with 10～the pass deformation rate of 20%, by cold drawing or cold rolling process, is processed into the multicore Cu/Nb-Al composite wire of a diameter of 0.1～1.5mm；
Step 3: heat treatment
The multicore Cu/Nb-Al composite wire described step 2 obtained puts into Ar atmosphere or vacuum heat treatment furnace, and (vacuum is not less than 10-2Pa) carrying out heat treatment in, the temperature of heat treatment is 750 DEG C～950 DEG C, and temperature retention time is 10～100h, to obtain final product.
Using hydrostatic extrusion technology, the single bar after winding Nb paper tinsel and Al paper tinsel carries out room temperature extruding so that the combination between Nb paper tinsel and Al paper tinsel is improved by the extruding of aximal deformation value；Thus strengthen the long Nb of km3The uniformity of Al presoma wire rod and finished product Nb3Al superconducting wire superconductivity.The method is simple, is suitable for the preparation of the long line of superconduction, the most large-scale popularization and application, has huge commercial value.
One Nb of the present invention3The preparation method of Al superconducting wire, solves winding method and prepares Nb3During Al presoma wire rod, Nb paper tinsel and Al paper tinsel deform uneven problem, and are added, by what this problem caused, series of problems such as easily breaking man-hour, wire rod critical current properties is relatively low, and preparation method is simple, has huge commercial value.
Embodiment 1
Step 1: make Cu/Nb-Al single rod
By width be 100mm, thickness be the Nb paper tinsel of 0.03mm and width 100mm, thickness 0.01mm Al paper tinsel superposition after outside the Cu rod of diameter 5.0mm, be wound to a diameter of 25mm, and load in the Cu canning tube of internal diameter 26mm, wall thickness 3.0mm, obtain Cu/Nb-Al complex, at room temperature utilize hydrostatic extrusion method, with the speed of 1m/min, Cu/Nb-Al complex extrusion is obtained diameter 5.0mm Cu/Nb-Al single rod；
Step 2: tubulature drawing
The Cu/Nb-Al single rod 19 steps 1 obtained is encased in Cu pipe, and with the pass deformation rate drawing of 10%, is processed into the 19 core Cu/Nb-Al composite wires of diameter 1.2mm；
Step 3: heat treatment
19 core Cu/Nb-Al composite wires step 2 obtained are put in Ar atmosphere, carry out heat treatment, and the temperature of heat treatment is 750 DEG C, and temperature retention time is 100h, to obtain final product.
One section that takes wire rod in the present embodiment carries out superconductivity test, and its superconducting transition temperature reaches 15.6K, critical current density JcUnder 4.2K, 12T, reach 400A/mm2。
Embodiment 2
Step 1: make Cu/Nb-Al single rod
By width be 200mm, thickness be the Nb paper tinsel of 0.12mm and width 200mm, thickness 0.04mm Al paper tinsel superposition after outside the Cu rod of diameter 5.0mm, be wound to a diameter of 15mm, and load in the Cu canning tube of internal diameter 16mm, wall thickness 3.0mm, obtain Cu/Nb-Al complex, at room temperature utilize hydrostatic extrusion method, with the speed of 4m/min, Cu/Nb-Al complex extrusion is obtained diameter 8.0mm Cu/Nb-Al single rod；
Step 2: tubulature drawing
The Cu/Nb-Al single rod 19 steps 1 obtained is encased in Cu pipe, and with the pass deformation rate drawing of 14%, is processed into the 19 core Cu/Nb-Al composite wires of diameter 0.6mm；
Step 3: heat treatment
19 core Cu/Nb-Al composite wires step 2 obtained put in vacuum heat treatment furnace that (vacuum is not less than 10-2Pa), carrying out heat treatment, the temperature of heat treatment is 850 DEG C, and temperature retention time is 40h, to obtain final product.
One section that takes wire rod in the present embodiment carries out superconductivity test, and its superconducting transition temperature reaches 15.8K, critical current density JcUnder 4.2K, 12T, reach 380A/mm2。
Embodiment 3
Step 1: make Cu/Nb-Al single rod
By width be 300mm, thickness be the Nb paper tinsel of 0.24mm and width 300mm, thickness 0.08mm Al paper tinsel superposition after outside the Cu rod of diameter 5.0mm, be wound to a diameter of 20mm, and load in the Cu canning tube of internal diameter 21mm, wall thickness 3.0mm, obtain Cu/Nb-Al complex, at room temperature utilize hydrostatic extrusion method, with the speed of 5m/min, Cu/Nb-Al complex extrusion is obtained diameter 10mmCu/Nb-Al single rod；
Step 2: tubulature drawing
The Cu/Nb-Al single rod 19 steps 1 obtained is encased in Cu pipe, and with the pass deformation rate of 18%, the cold rolling 19 core Cu/Nb-Al composite wires being processed into diameter 0.1mm；
Step 3: heat treatment
19 core Cu/Nb-Al composite wires step 2 obtained are put in Ar atmosphere, carry out heat treatment, and the temperature of heat treatment is 950 DEG C, and temperature retention time is 10h, to obtain final product.
One section that takes wire rod in the present embodiment carries out superconductivity test, and its superconducting transition temperature reaches 15.0 K, critical current density JcUnder 4.2K, 12T, reach 280A/mm2。
Embodiment 4
Step 1: make Cu/Nb-Al single rod
By width be 200mm, thickness be the Nb paper tinsel of 0.3mm and width 200mm, thickness 0.1mm Al paper tinsel superposition after outside the Cu rod of diameter 5.0mm, be wound to a diameter of 20mm, and load in the Cu canning tube of internal diameter 21mm, wall thickness 3.0mm, obtain Cu/Nb-Al complex, at room temperature utilize hydrostatic extrusion method, with the speed of 2m/min, Cu/Nb-Al complex extrusion is obtained diameter 1.0mm Cu/Nb-Al single rod；
Step 2: tubulature drawing
The Cu/Nb-Al single rod 19 steps 1 obtained is encased in Cu pipe, and with the pass deformation rate of 20%, the 19 core Cu/Nb-Al composite wires of diameter 1.5mm are processed in drawing；
Step 3: heat treatment
19 core Cu/Nb-Al composite wires step 2 obtained put in vacuum heat treatment furnace that (vacuum is not less than 10-2Pa), carrying out heat treatment, the temperature of heat treatment is 900 DEG C, and temperature retention time is 30h, to obtain final product.
One section that takes wire rod in the present embodiment carries out superconductivity test, and its superconducting transition temperature reaches 15.7K, critical current density JcUnder 4.2K, 12T, reach 420A/mm2。
Claims (5)
1. a Nb3The preparation method of Al superconducting wire, it is characterised in that specifically include following steps:
Step 1: make Cu/Nb-Al single rod
To be wound on Cu rod after Nb paper tinsel and Al paper tinsel superposition and load in Cu canning tube, it is thus achieved that
Cu/Nb-Al complex；Hydrostatic extrusion method is at room temperature utilized to incite somebody to action with the speed of 1～5m/min
Cu/Nb-Al complex is extruded into bar, it is thus achieved that Cu/Nb-Al single rod；
Wherein Nb paper tinsel and Al paper tinsel width are 100～300mm, and Nb paper tinsel thickness is 0.03～0.3mm, Al
Paper tinsel thickness is the 1/3 of Nb paper tinsel；The thickness that Nb-Al is wound on Cu rod with the ratio of Cu rod diameter is
1～2；
Step 2: tubulature drawing
The Cu/Nb-Al single rod many described steps 1 obtained is encased in Cu pipe, and with 10～20%
Pass deformation rate, by cold drawing or cold rolling process, be processed into multicore Cu/Nb-Al composite wire；
Step 3: heat treatment
The multicore Cu/Nb-Al composite wire described step 2 obtained puts into Ar atmosphere or vacuum heat
Stove carries out heat treatment and get final product.
2. a kind of Nb as claimed in claim 13The preparation method of Al superconducting wire, it is characterised in that
Described step 1 obtains Cu/Nb-Al single rod a diameter of 1.0～10.0mm.
3. a kind of Nb as claimed in claim 13The preparation method of Al superconducting wire, it is characterised in that
In described step 2, Cu/Nb-Al single rod is 19.
4. a kind of Nb as claimed in claim 13The preparation method of Al superconducting wire, it is characterised in that
The multicore Cu/Nb-Al composite wire a diameter of 0.1～1.5mm obtained in described step 2.
5. a kind of Nb as claimed in claim 13The preparation method of Al superconducting wire, it is characterised in that
In described step 3, the temperature of heat treatment is 750 DEG C～950 DEG C, and temperature retention time is 10～100h.
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| 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 |
| CN114822981B (en) * | 2022-06-20 | 2022-09-20 | 西部超导材料科技股份有限公司 | Method for preparing niobium three-aluminum superconducting wire by hot extrusion method |
| CN116200690B (en) * | 2023-01-29 | 2024-07-30 | 西南交通大学 | Preparation of high-current-carrying Nb by multiple instantaneous high-temperature heat treatments3Method of Al superconducting wire |
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| EP1058321A2 (en) * | 1999-06-04 | 2000-12-06 | JAPAN as represented by NATIONAL RESEARCH INSITUTE FOR METALS | Process for producing ultrafine multifilamentary Nb3(Al, Ge) or Nb3(Al, Si) superconducting wire |
| CN102751049A (en) * | 2012-07-24 | 2012-10-24 | 西部超导材料科技股份有限公司 | Manufacturing method of Nb3Al superconducting wire precursor material |
| CN103871683A (en) * | 2012-12-18 | 2014-06-18 | 张亮 | Preparation method of superconducting wires |
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Patent Citations (3)
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|---|---|---|---|---|
| EP1058321A2 (en) * | 1999-06-04 | 2000-12-06 | JAPAN as represented by NATIONAL RESEARCH INSITUTE FOR METALS | Process for producing ultrafine multifilamentary Nb3(Al, Ge) or Nb3(Al, Si) superconducting wire |
| CN102751049A (en) * | 2012-07-24 | 2012-10-24 | 西部超导材料科技股份有限公司 | Manufacturing method of Nb3Al superconducting wire precursor material |
| CN103871683A (en) * | 2012-12-18 | 2014-06-18 | 张亮 | Preparation method of superconducting wires |
Non-Patent Citations (2)
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| New Nb3AL multifilamentary conductor and its application to high field superconducting magnet;K Inoue，Y Iijima，T Takeuchi等;《Physica B：Condensed Matter》;19981231;第365页左栏第2节第1段 * |
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