CN105513712A - Preparation method of high-critical-current-density Nb3Sn superconductive wire rod - Google Patents
Preparation method of high-critical-current-density Nb3Sn superconductive wire rod Download PDFInfo
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- CN105513712A CN105513712A CN201510833485.7A CN201510833485A CN105513712A CN 105513712 A CN105513712 A CN 105513712A CN 201510833485 A CN201510833485 A CN 201510833485A CN 105513712 A CN105513712 A CN 105513712A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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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
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- 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
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- 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
Abstract
The invention discloses a preparation method of a high-critical-current-density Nb3Sn superconductive wire rod. The preparation method comprises: an oxygen-free copper ingot unit is drilled along the length direction to form a plurality of through holes, thereby obtaining a porous copper ingot unit; Nb rods are inserted into the trough holes and copper covers cover the two ends and sealing and welding are carried out, thereby obtaining a CuNb multi-core cladding sheath; extruding is carried out after heating, and the obtained rod material is stretched and then is cut off with a fixed dimension to obtain a CuNb composite rod; deep hole drilling is carried out on the composite rod to obtain a CuNb composite tube, insertion of an SnTi alloy rod is carried out, and stretching moulding is carried out to obtain a sub component; the SnTi or SnCu alloy rod is arranged in the oxygen-free copper tube and stretching is carried out to obtain a Sn/Cu insertion rod; and the sub component, the Sn/Cu insertion rod, and a blocked layer bundle are arranged in the oxygen-free copper tube to obtain an Nb3Sn final blank, and then stretching is carried out by multiple times to obtain a finished Nb3Sn superconductive wire rod. According to the invention, because the a Sn/Cu insertion rod is arranged during the final blank assembling processing, the generated Nb3Sn content during the thermal processing process is improved, so that the critical current density Jc is obviously improved under the circumstance that the low hysteresis loss level of the piled yarn is kept.
Description
Technical field
The invention belongs to superconductor processing technique field, relate to a kind of high critical current densities Nb
3the preparation method of Sn superconducting wire.
Background technology
International Thermal-Nuclear Experimental Reactor (InternationalThermonuclearExperimentalReactor); i.e. ITER; be nuclear fusion device maximum in the world, be intended to obtain new energy source to solve increasingly serious energy crisis by controllable thermonuclear fusion reaction.China becomes a full member of ITER plan negotiation in February, 2003, becomes a full member of ITER plan in November, 2006.One of Chinese member state as ITER project will provide about 30 tons of Nb with physical form
3sn superconducting wire is used for the manufacture of toroidal field (TF) coil.
ITER Nb
3sn superconducting wire requires moderate critical current density (J
c) and low magnetic hysteresis loss.Nei Xifa produces Nb at present
3the prefered method of Sn superconducting wire, its process-cycle is short, and cost is lower, and wire rod combination property is better.Need the content increasing copper in strand to reduce the coupling of core silk or bridging to reduce magnetic hysteresis loss, thus reduce effective core filament diameter, but Nb while the increase of copper content
3the content of Sn superconducting phase reduces relatively, can cause J
cthere is decline to a certain degree, cannot meet the demands.In existing ITER wire rod, because heat treatment process ectomesoderm core flight lead Sn source is comparatively far away, after heat treatment, core silk does not fully react, and have impact on the current capacity of wire rod.
Summary of the invention
The object of this invention is to provide a kind of high critical current densities Nb
3the preparation method of Sn superconducting wire, solves existing Nb
3what Sn superconducting wire preparation method existed does not fully react because of core silk behind heat treatment process ectomesoderm core flight lead Sn the source comparatively process of long-range guided missile pyrogenicity, thus affects the problem of the current capacity of wire rod.
The technical solution adopted in the present invention is: a kind of high critical current densities Nb
3the preparation method of Sn superconducting wire, specifically comprises the following steps:
Step 1: choose anaerobic copper ingot as billet, adopts the method for depth drill to bore the equally distributed some through holes of multilayer along billet length direction, obtains porous copper ingot;
Step 2: the porous copper ingot that step 1 obtains is cleaned, then the Nb rod after cleaning is inserted in the porous copper ingot through hole after cleaning, two ends add copper lid and use electron beam soldering and sealing, obtain CuNb multicore jacket;
Step 3: CuNb multicore jacket step 2 obtained is heated to 550 ~ 650 DEG C, is incubated after 1 ~ 4 hour and extrudes, and after the bar drawing obtain extruding, fixed ruler cutting obtains CuNb compound bar;
Step 4: CuNb compound bar step 3 obtained is carried out depth drill and obtained CuNb multiple tube, inserted in CuNb multiple tube by the SnTi alloy bar after clean and obtain subgroup unit blank, drawing and forming obtains subgroup unit;
Step 5: SnTi, SnCu alloy bar after clean or pure Sn rod are loaded in the oxygen-free copper pipe after cleaning, stretches and obtain Sn/Cu plunger;
Step 6: obtain Nb in the oxygen-free copper pipe after the Sn/Cu plunger that subgroup unit step 4 obtained, step 5 obtain and barrier layer clean rear boundling loading cleaning
3the final blank of Sn, then carries out multi-drawing, obtained finished product Nb
3sn superconducting wire.
Feature of the present invention is also,
In step 1, anaerobic copper ingot diameter is 200 ~ 300mm, length is 500 ~ 800mm.
In step 1, through hole is 4 ~ 5 layers, and each through-hole diameter is 9 ~ 15mm, totally 100 ~ 250 through holes.
In step 2, the cleaning agent of cleaning porous copper ingot to be volumetric concentration be 25% ~ 40% salpeter solution; The cleaning agent of cleaning Nb rod is nitric acid, and the mixed solution of hydrofluoric acid and water composition, in mixed solution, the volumetric concentration of each component is: nitric acid 25% ~ 35%, hydrofluoric acid 15% ~ 25%, and surplus is water.
In step 2, the electric current of electron beam soldering and sealing is 50 ~ 150mA, and vacuum degree is not more than 10
-2pa.
In step 3, extruding the multicore composite rod diameter obtained is 50 ~ 100mm, and it is 40 ~ 60mm that sizing cuts off the CuNb compound bar diameter obtained, and length is 1000 ~ 2000mm.
In step 4, CuNb multiple tube center bore is that Φ 15 ~ 25mm, SnTi alloy bar adopts acetone to clean, and the cut lengths of subgroup unit is 1500 ~ 3000mm.
In step 5, adopt SnTi or SnCu alloy bar or pure Sn rod, diameter is that 10 ~ 20mm, anaerobic Cu bore is Φ 10 ~ 20mm, wall thickness is 3 ~ 10mm, and the Sn/Cu plunger diameter obtained that stretches is 2 ~ 4mm, and fixed ruler cutting length is 1500 ~ 3000mm.
In step 6, subgroup unit and oxygen-free copper pipe adopt nitric acid clean, the volumetric concentration of nitric acid is 25% ~ 40%, barrier material is Ta, employing cleaning agent is nitric acid, the mixed solution of hydrofluoric acid and water composition, and in mixed solution, the volumetric concentration of each component is: nitric acid 25% ~ 35%, hydrofluoric acid 15% ~ 25%, surplus is water.
In step 6, rate of extension is 5 ~ 60m/min, and pass reduction is 10% ~ 20%.
The invention has the beneficial effects as follows, a kind of high critical current densities Nb
3the preparation method of Sn superconducting wire, by adding Sn/Cu plunger when final blank is assembled, improve the content of Sn in strand, make in heat treatment process, have more Sn to participate in reaction, the Sn increased diffuses in contiguous semicircle and fan-shaped subgroup unit core silk, to improve in core silk the Nb generated in particularly outermost layer core silk
3sn phase content, makes strand when keeping lower magnetic hysteresis loss level, critical current density J
cimprove more than 10%.
Accompanying drawing explanation
Fig. 1 is a kind of high critical current densities Nb of the present invention
3final blank structure schematic diagram in the preparation method of Sn superconducting wire.
In figure, 1. oxygen-free copper pipe, 2. subgroup unit, 3.Sn/Cu plunger, 4. barrier layer.
Embodiment
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
A kind of high critical current densities Nb of the present invention
3the preparation method of Sn superconducting wire, specifically comprises the following steps:
Step 1: choose diameter is 200 ~ 300mm, length is 500 ~ 800mm anaerobic copper ingot as billet, adopting the method for depth drill to bore 4 ~ 5 layers of equally distributed 100 ~ 250 diameter altogether along billet length direction is the through hole of 9 ~ 15mm, obtains porous copper ingot;
Step 2: first adopt metal detergent to remove surface and oil contaminant to the porous copper ingot that step 1 obtains, then endoporus and surface is cleaned with the salpeter solution that volumetric concentration is 25% ~ 40%, Nb rod after cleaning is inserted in the porous copper ingot through hole after cleaning, add copper lid at porous copper ingot two ends and use electron beam soldering and sealing, soldering and sealing electric current is 50 ~ 150mA, and vacuum degree is not more than 10
-2pa, obtains CuNb multicore jacket;
Step 3: CuNb multicore jacket step 2 obtained is heated to 500 DEG C ~ 650 DEG C, be incubated and extrude after 1 ~ 4 hour, obtain the multicore CuNb compound bar that diameter is 50 ~ 100mm, after multicore composite rod being stretched to Φ 40 ~ 60mm, fixed ruler cutting is the CuNb compound bar of 1000 ~ 2000mm;
Step 4: CuNb compound bar step 3 obtained is carried out depth drill and obtained CuNb multiple tube, center bore is Φ 15 ~ 25mm, SnTi alloy bar after cleaning with acetone is inserted in CuNb multiple tube and obtain subgroup unit 2 blanks, through multi-pass stretch and shaping, fixed ruler cutting obtains six sides and special-shaped subgroup unit 2, and cut lengths is 1500 ~ 3000mm;
Step 5: be that SnTi, SnCu alloy bar of 10 ~ 20mm or pure Sn rod acetone clean that rear loading internal diameter is Φ 10 ~ 20mm, wall thickness is in the oxygen-free copper pipe 1 of 3 ~ 10mm by diameter, Φ 2 ~ 4mm is stretched to through multi-pass, fixed ruler cutting obtains Sn/Cu plunger 3, and cut lengths is 1500 ~ 3000mm;
Step 6: the Sn/Cu plunger 3 that the subgroup unit 2 obtained with the salpeter solution cleaning 4 that volumetric concentration is 25% ~ 40%, step 5 obtain and oxygen-free copper pipe 1, with 25 ~ 35% nitric acid, 15 ~ 25% hydrofluoric acid and surplus are the solvent clean Ta barrier layer 4 of water, as shown in Figure 1,19 subgroup units, 2,12 the Sn/Cu plungers 3 after clean and Ta barrier layer 4 boundling are loaded clean after oxygen-free copper pipe 1 in obtain Nb
3the final blank of Sn, then carries out multi-pass stretching, and draw speed selects 5 ~ 30m/min, and working modulus selects 10 ~ 20%, can obtain finished product Nb
3sn superconducting wire.
Embodiment 1
Step 1: choose diameter is 200mm, length is 600mm anaerobic copper ingot as billet, adopting the method for depth drill to bore 4 layers along billet length direction, equally distributed to amount to 100 diameters be the through hole of 9mm, obtains porous copper ingot;
Step 2: first adopt metal detergent to remove surface and oil contaminant to the porous copper ingot that step 1 obtains, then endoporus and surface is cleaned with the salpeter solution that volumetric concentration is 30%, Nb rod after cleaning is inserted in the porous copper ingot through hole after cleaning, add copper lid at porous copper ingot two ends and use electron beam soldering and sealing, soldering and sealing electric current is 90mA, and vacuum degree is not more than 10
-2pa, obtains CuNb multicore jacket;
Step 3: CuNb multicore jacket step 2 obtained is heated to 500 DEG C, is incubated and extrudes after 2 hours, and obtain the multicore CuNb compound bar that diameter is 50mm, after multicore composite rod being stretched to Φ 40mm, fixed ruler cutting is the CuNb compound bar of 1400mm;
Step 4: CuNb compound bar step 3 obtained is carried out depth drill and obtained CuNb multiple tube, center bore is Φ 15mm, SnTi alloy bar after cleaning with acetone is inserted in CuNb multiple tube and obtain subgroup unit 2 blanks, through multi-pass stretch and shaping, fixed ruler cutting obtains six sides and special-shaped subgroup unit 2, and cut lengths is 2000mm;
Step 5: be that the SnTi alloy bar acetone of 20mm cleans in the oxygen-free copper pipe 1 that rear loading internal diameter is Φ 20mm, wall thickness is 10mm by diameter, be stretched to Φ 3mm through multi-pass, fixed ruler cutting obtains Sn/Cu plunger 3, and cut lengths is 2000mm;
Step 6: the Sn/Cu plunger 3 that the subgroup unit 2 obtained with the salpeter solution cleaning 4 that volumetric concentration is 30%, step 5 obtain and oxygen-free copper pipe 1, use 30% nitric acid, 20% hydrofluoric acid and surplus are the solvent clean Ta barrier layer 4 of water, 19 subgroup units, 2,12 the Sn/Cu plungers 3 after clean and Ta barrier layer 4 boundling are loaded clean after oxygen-free copper pipe 1 in obtain Nb
3the final blank of Sn, then carries out multi-pass stretching, and rate of extension is 5m/min, and pass reduction is 10%, obtained finished product Nb
3sn superconducting wire.
Embodiment 2
Step 1: choose diameter is 260mm, length is 720mm anaerobic copper ingot as billet, adopting the method for depth drill to bore 4 layers along billet length direction, equally distributed to amount to 150 diameters be the through hole of 11mm, obtains porous copper ingot;
Step 2: first adopt metal detergent to remove surface and oil contaminant to the porous copper ingot that step 1 obtains, then endoporus and surface is cleaned with the salpeter solution that volumetric concentration is 25%, Nb rod after cleaning is inserted in the porous copper ingot through hole after cleaning, add copper lid at porous copper ingot two ends and use electron beam soldering and sealing, soldering and sealing electric current is 50mA, and vacuum degree is not more than 10
-2pa, obtains CuNb multicore jacket;
Step 3: CuNb multicore jacket step 2 obtained is heated to 600 DEG C, is incubated and extrudes after 1 hour, and obtain the multicore CuNb compound bar that diameter is 70mm, after multicore composite rod being stretched to Φ 50mm, fixed ruler cutting is the CuNb compound bar of 1000mm;
Step 4: CuNb compound bar step 3 obtained is carried out depth drill and obtained CuNb multiple tube, center bore is Φ 20mm, SnTi alloy bar after cleaning with acetone is inserted in CuNb multiple tube and obtain subgroup unit 2 blanks, through multi-pass stretch and shaping, fixed ruler cutting obtains six sides and special-shaped subgroup unit 2, and cut lengths is 1500mm;
Step 5: be that the SnCu alloy bar acetone of 25mm cleans in the oxygen-free copper pipe 1 that rear loading internal diameter is Φ 25mm, wall thickness is 5mm by diameter, be stretched to Φ 2mm through multi-pass, fixed ruler cutting obtains Sn/Cu plunger 3, and cut lengths is 1500mm;
Step 6: the Sn/Cu plunger 3 that the subgroup unit 2 obtained with the salpeter solution cleaning 4 that volumetric concentration is 25%, step 5 obtain and oxygen-free copper pipe 1, use 25% nitric acid, 15% hydrofluoric acid and surplus are the solvent clean Ta barrier layer 4 of water, 19 subgroup units, 2,12 the Sn/Cu plungers 3 after clean and Ta barrier layer 4 boundling are loaded clean after oxygen-free copper pipe 1 in obtain Nb
3the final blank of Sn, then carries out multi-pass stretching, and rate of extension is 30m/min, and pass reduction is 15%, obtained finished product Nb
3sn superconducting wire.
Embodiment 3
Step 1: choose diameter is 300mm, length is 800mm anaerobic copper ingot as billet, adopting the method for depth drill to bore 5 layers along billet length direction, equally distributed to amount to 250 diameters be the through hole of 15mm, obtains porous copper ingot;
Step 2: first adopt metal detergent to remove surface and oil contaminant to the porous copper ingot that step 1 obtains, then endoporus and surface is cleaned with the salpeter solution that volumetric concentration is 40%, Nb rod after cleaning is inserted in the porous copper ingot through hole after cleaning, add copper lid at porous copper ingot two ends and use electron beam soldering and sealing, soldering and sealing electric current is 150mA, and vacuum degree is not more than 10
-2pa, obtains CuNb multicore jacket;
Step 3: CuNb multicore jacket step 2 obtained is heated to 650 DEG C, is incubated and extrudes after 4 hours, and obtain the multicore CuNb compound bar that diameter is 100mm, after multicore composite rod being stretched to Φ 60mm, fixed ruler cutting is the CuNb compound bar of 2000mm;
Step 4: CuNb compound bar step 3 obtained is carried out depth drill and obtained CuNb multiple tube, center bore is Φ 25mm, SnTi alloy bar after cleaning with acetone is inserted in CuNb multiple tube and obtain subgroup unit 2 blanks, through multi-pass stretch and shaping, fixed ruler cutting obtains six sides and special-shaped subgroup unit 2, and cut lengths is 3000mm;
Step 5: be that the pure Sn rod acetone of 10mm cleans in the oxygen-free copper pipe 1 that rear loading internal diameter is Φ 10mm, wall thickness is 3mm by diameter, be stretched to Φ 4mm through multi-pass, fixed ruler cutting obtains Sn/Cu plunger 3, and cut lengths is 3000mm;
Step 6: the Sn/Cu plunger 3 that the subgroup unit 2 obtained with the salpeter solution cleaning 4 that volumetric concentration is 40%, step 5 obtain and oxygen-free copper pipe 1, use 35% nitric acid, 15% hydrofluoric acid and surplus are the solvent clean Ta barrier layer 4 of water, 19 subgroup units, 2,12 the Sn/Cu plungers 3 after clean and Ta barrier layer 4 boundling are loaded clean after oxygen-free copper pipe 1 in obtain Nb
3the final blank of Sn, then carries out multi-pass stretching, and rate of extension is 60m/min, and pass reduction is 20%, obtained finished product Nb
3sn superconducting wire.
Claims (10)
1. a high critical current densities Nb
3the preparation method of Sn superconducting wire, is characterized in that, specifically comprises the following steps:
Step 1: choose anaerobic copper ingot as billet, adopts the method for depth drill to bore some through holes along billet length direction, obtains porous copper ingot;
Step 2: the porous copper ingot obtained to described step 1 cleans, then the Nb rod after cleaning is inserted in the porous copper ingot through hole after cleaning, two ends add the soldering and sealing of copper lid electron beam, obtain CuNb multicore jacket;
Step 3: the CuNb multicore jacket described step 2 obtained is heated to 550 ~ 650 DEG C, is incubated after 1 ~ 4 hour and extrudes, and after the bar drawing obtain extruding, fixed ruler cutting obtains CuNb compound bar;
Step 4: the CuNb compound bar described step 3 obtained is carried out depth drill and obtained CuNb multiple tube, inserted in CuNb multiple tube by the SnTi alloy bar after clean and obtain subgroup unit (2) blank, drawing and forming obtains subgroup unit;
Step 5: SnTi, SnCu alloy bar after clean or pure Sn rod are loaded in the oxygen-free copper pipe (1) after cleaning, stretches and obtain Sn/Cu plunger (3);
Step 6: obtain Nb in the oxygen-free copper pipe (1) after the Sn/Cu plunger (3) that the subgroup unit (2) step 4 obtained, step 5 obtain and the clean rear boundling of barrier layer (4) load cleaning
3the final blank of Sn, then carries out multi-drawing, can obtain finished product Nb
3sn superconducting wire.
2. a kind of high critical current densities Nb according to claim 1
3the preparation method of Sn superconducting wire, is characterized in that, in described step 1, anaerobic copper ingot diameter is 200 ~ 300mm, length is 500 ~ 800mm.
3. a kind of high critical current densities Nb according to claim 1
3the preparation method of Sn superconducting wire, is characterized in that, in described step 1, through hole is 4 ~ 5 layers, and each through-hole diameter is 9 ~ 15mm, totally 100 ~ 250 through holes.
4. a kind of high critical current densities Nb according to claim 1
3the preparation method of Sn superconducting wire, is characterized in that, in described step 2, the cleaning agent of cleaning porous copper ingot to be volumetric concentration be 25% ~ 40% salpeter solution; The cleaning agent of cleaning Nb rod is nitric acid, and the mixed solution of hydrofluoric acid and water composition, in mixed solution, the volumetric concentration of each component is: nitric acid 25% ~ 35%, hydrofluoric acid 15% ~ 25%, and surplus is water.
5. a kind of high critical current densities Nb according to claim 4
3the preparation method of Sn superconducting wire, is characterized in that, in described step 2, the electric current of electron beam soldering and sealing is 50 ~ 150mA, and vacuum degree is not more than 10
-2pa.
6. a kind of high critical current densities Nb according to claim 1
3the preparation method of Sn superconducting wire, is characterized in that, in described step 3, extruding the multicore composite rod diameter obtained is 50 ~ 100mm, and it is 40 ~ 60mm that sizing cuts off the CuNb compound bar diameter obtained, and length is 1000 ~ 2000mm.
7. a kind of high critical current densities Nb according to claim 1
3the preparation method of Sn superconducting wire, is characterized in that, in described step 4, CuNb multiple tube center bore is that Φ 15 ~ 25mm, SnTi alloy bar adopts acetone to clean, and the cut lengths of subgroup unit (2) is 1500 ~ 3000mm.
8. a kind of high critical current densities Nb according to claim 1
3the preparation method of Sn superconducting wire, it is characterized in that, in described step 5, adopt SnTi or SnCu alloy bar or pure Sn rod, diameter is 10 ~ 20mm, anaerobic Cu bore is Φ 10 ~ 20mm, wall thickness is 3 ~ 10mm, and Sn/Cu plunger (3) diameter obtained that stretches is 2 ~ 4mm, and fixed ruler cutting length is 1500 ~ 3000mm.
9. a kind of high critical current densities Nb according to claim 1
3the preparation method of Sn superconducting wire, it is characterized in that, in described step 6, subgroup unit (2) and oxygen-free copper pipe (1) adopt nitric acid clean, and the volumetric concentration of nitric acid is 25% ~ 40%, barrier layer (4) material is Ta, employing cleaning agent is nitric acid, the mixed solution of hydrofluoric acid and water composition, and in mixed solution, the volumetric concentration of each component is: nitric acid 25% ~ 35%, hydrofluoric acid 15% ~ 25%, surplus is water.
10. a kind of high critical current densities Nb according to claim 9
3the preparation method of Sn superconducting wire, is characterized in that, in described step 6, rate of extension is 5 ~ 60m/min, and pass reduction is 10% ~ 20%.
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Cited By (10)
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CN106298059A (en) * | 2016-08-11 | 2017-01-04 | 西部超导材料科技股份有限公司 | Stannum method Nb in a kind of3the assemble method of the final blank of Sn composite superconducting wire |
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