CN102082009A - Process for preparing bronze Nb3Sn superconducting wire material - Google Patents
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- CN102082009A CN102082009A CN2010106090319A CN201010609031A CN102082009A CN 102082009 A CN102082009 A CN 102082009A CN 2010106090319 A CN2010106090319 A CN 2010106090319A CN 201010609031 A CN201010609031 A CN 201010609031A CN 102082009 A CN102082009 A CN 102082009A
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Abstract
The invention discloses a process for preparing a bronze Nb3Sn superconducting wire material. The process comprises the following steps of: drilling a hole on a high tin bronze ingot, assembling the drilled ingot with a niobium alloy rod, soldering and sealing under vacuum, and performing hot extrusion to obtain a rod blank a which serves as a tensile blank; filling the tensile blank in an annealing furnace to perform first annealing; charging a furnace chamber of the annealing furnace with high-purity argon or nitrogen; heating the furnace chamber to the temperature of between 420 and 480 DEG C at the rate of 4 to 8 DEG C/minute; preserving the heat for 30 to 90 minutes; performing forced cooling by circulating the argon or the nitrogen; discharging when the material is cooled to the temperature of between 50 and 100 DEG C; repeatedly processing the material; performing a subcomponent molding process to obtain a hexagonal subcomponent; assembling, soldering and sealing under vacuum and performing the hot extrusion to obtain a rod blank b; and performing second annealing, twisting, performing final stretching and electroplating to obtain the Nb3Sn superconducting wire material. By the process for preparing the bronze Nb3Sn superconducting wire material, the surface of an Nb alloy is improved, and the performance of a strand wire is improved.
Description
Technical field
The invention belongs to the superconductor processing technique field, relate to a kind of bronze method Nb
3The preparation technology of Sn superconducting wire.
Background technology
Bronze method Nb
3The Sn low-temperature superconducting wire is an a kind of practical wire rod of making the above cryogenic magnet of 10T, and it is by bronze, oxygen-free copper, and Nb alloy and barrier material Compound Machining form.In order to produce the bronze method Nb of high critical current
3Sn superconduction strand needs to adopt high-tin bronze that sufficient tin is provided, and is beneficial to follow-up Nb
3The generation of Sn.But high-tin bronze can produce the work hardening that is exceedingly fast in the cold working process, follow-up processing can't be carried out at all, therefore needs a kind of effective intermediate annealing process to improve the following process plasticity of high-tin bronze.
Existing bronze method Nb
3The intermediate annealing of Sn typically refers to the annealing of carrying out in bronze monophase field, and its technology essence is the heterogeneousization full annealing of bronze, and promptly high-tin bronze has in the time of 520 ℃
Phase composition change, be heated to phase point temperature and obtain single-phase αGu Rongti for 520 ℃, form duplex structure with the stove cooling, such tissue has taken place softening.But such temperature has caused its long heat treatment cycle, about 15 hours of every stove, so repeatedly Tui Huo total time very long, can not satisfy suitability for industrialized production, and the most serious be that too high temperature and long intensification and temperature fall time cause the surperficial too early generation Nb at the Nb alloy
3The Sn layer makes wire rod intensity reduction in the cold working process, influences wire rod plastic forming and the moulding of final core silk, and the moulding situation of core silk directly influences the ability of product line current-carrying, present 520 ℃ of Technologies for Heating Processing that adopt, critical current I
cFor 100A lower.
Summary of the invention
The purpose of this invention is to provide a kind of bronze method Nb
3The preparation technology of Sn superconducting wire, its heat treatment temperature is low, the cycle short, anneals at bronze low temperature two-phase section, obtains the wire rod of good plasticity.
The technical solution adopted in the present invention is bronze method Nb
3The preparation technology of Sn superconducting wire, specifically carry out according to following steps:
EB electron beam vacuum seal is adopted in high-tin bronze ingot boring back and the assembling of niobium alloy rod afterwards, obtains blank to be extruded, obtain excellent base a through hot extrusion again, excellent base a as the stretching blank annealing furnace of packing into, is carried out the annealing first time, and annealing process specifically carries out according to following steps for the first time:
Step 1
Use mechanical pump to be extracted into low vacuum and use diffusion pump to be extracted into high vacuum then, vacuum degree≤1.0 * 10
-2Pa; Fill high-purity argon gas or nitrogen in the furnace chamber of annealing furnace, vacuum degree is 5.3 * 10
3Pa-1.01 * 10
5Pa with furnace chamber heating, is heated to 420 ℃-480 ℃ with raise 4 ℃-8 ℃ speed of per minute, adopts thermocouple monitoring material temperature, is incubated 30-90 minute then; Adopt argon gas or nitrogen circulation cold by force at last, come out of the stove when the material temperature is cooled to 50 ℃-100 ℃;
Step 2
According to the technical process of step 1 and adopt 10%～30% working modulus processing materials repeatedly, annealing process is finished for the first time;
And then process subgroup unit moulding process obtains six side's subgroup units, the six side's subgroups unit and barrier layer, the copper-clad cover that obtain are assembled, adopt vacuum seal to obtain billet to be extruded, obtain excellent base b through hot extrusion, should rod base b as the stretching blank annealing furnace of packing into, carry out second time annealing process and obtain twisting line base, for the second time annealing process with the first time annealing process step and annealing conditions identical, then the line base is passed through twisting again, finally stretches and electroplates, obtain bronze method Nb
3The Sn superconducting wire.
Adopt bronze method Nb of the present invention
3The preparation technology of Sn superconducting wire, control material temperature obtains the bronze two-phase annealed structure of certain mechanical property at 420 ℃-480 ℃, satisfies follow-up cold worked requirement.Protective gas when adopting argon gas or nitrogen as insulation, bonding when under vacuum, anneal to reduce material, the temperature homogeneity when improving the surface quality of material and insulation adopts Fast Heating, argon gas or nitrogen circulation cold by force, the shortening heat treatment cycle.The heat treatment cycle that solution present stage annealing process causes is long, the problem that current capacity is low.By adjusting heat treatment temperature and intensification rate of temperature fall technology is optimized, obtained the line base of well processed plasticity, improved the Nb alloy surface simultaneously, reduce influence, suppressed Nb final strand current capacity
3The too early generation of Sn has improved the strand performance, and critical current has reached more than the 160A.
Description of drawings
Fig. 1 is the core silk exterior view that adopts existing bronze heterogeneousization full annealing prepared under the scanning electron microscopy.
Fig. 2 is the core silk exterior view that adopts prepared of the present invention under the scanning electron microscopy.
Fig. 3 is bronze method Nb
3Sn superconducting wire preparation technology flow chart.
Embodiment
The present invention is described in detail below in conjunction with Figure of description and embodiment.
The present invention's bronze method Nb
3Sn superconducting wire prepared flow process as shown in Figure 3, bronze method Nb
3Sn superconducting wire technology is more complicated specifically, be to adopt high-tin bronze ingot boring back and niobium alloy rod once to assemble in brief, adopt EB electron beam vacuum seal afterwards, obtain blank to be extruded, obtain six side's subgroup units through hot extrusion, stretching annealing for the first time again, subgroup unit finally assembles soldering and sealing again with barrier layer that rolls and copper-clad cover and obtains billet to be extruded, again through hot extrusion, stretch for the second time annealing, twisting, finally stretch and electroplate the wire rod that obtains required specification.Preparation Nb
3Other step of Sn superconducting wire can be with reference to the open text of patent application, denomination of invention is " a kind of method for preparing bronze method Nb3Sn superconducting wire " (application number: 200910254552.4, the applying date: 2009.12.28, publication No.: CN101719400A), bronze method Nb of the present invention
3The preparation technology of Sn superconducting wire mainly is at existing preparation Nb
3The improvement that annealing process step in the Sn superconducting wire technology is carried out.The annealing process that adopts among the preparation technology of the present invention is twice stretching annealing process part in the middle of the flow chart.The step and the annealing conditions of twice stretching annealing process are identical.
Bronze method Nb of the present invention
3The preparation technology of Sn superconducting wire, specifically carry out according to following steps:
High-tin bronze ingot boring back and the assembling of niobium alloy rod, the welding cap seal is covered with copper in two ends, and welding current is 35-50mA, welding vacuum degree＜10
-3Pa; The blank to be extruded that will obtain then carries out hot extrusion behind the insulation 60-120min down at 520-650 ℃, extrusion ratio is 7-15, obtains excellent base a, with excellent base a as the stretching blank annealing furnace of packing into, carry out the annealing first time, annealing process specifically carries out according to following steps for the first time:
Step 1
Use mechanical pump to be extracted into low vacuum and use diffusion pump to be extracted into high vacuum then, vacuum degree≤1.0 * 10
-2Pa; Fill high-purity argon gas or nitrogen in the furnace chamber of annealing furnace, vacuum degree is 5.3 * 10
3Pa-1.01 * 10
5Pa with furnace chamber heating, is heated to 420 ℃-480 ℃ with raise 4 ℃-8 ℃ speed of per minute, adopts thermocouple monitoring material temperature, is incubated 30-90 minute then; Adopt argon gas or nitrogen circulation cold by force at last, come out of the stove when the material temperature is cooled to 50 ℃-100 ℃;
Step 2
Material is stretched repeatedly: adopt 10%～30% working modulus according to the technical process of step 1 processing materials repeatedly, make the stretching blank be stretched to Φ 4mm-Φ 8mm from Φ 30mm-Φ 60mm;
After annealing process is finished for the first time, obtain six side's subgroup units through subgroup unit moulding process again, the six side's subgroups unit and barrier layer, the copper-clad cover that obtain are assembled, and adopt vacuum seal to obtain billet to be extruded, and welding current is 70-90mA, welding vacuum degree＜10
-3Pa; Carry out hot extrusion behind the insulation 60-120min down at 520-650 ℃, extrusion ratio is 7-15, obtain excellent base b through hot extrusion, should rod base b as the stretching blank annealing furnace of packing into, carry out the annealing process second time, obtain twisting line base, the technology of annealing is with annealing process step and annealing conditions are identical for the first time for the second time, the line base is passed through twisting again, finally stretches and electroplates, obtain TF (toroidal field coil) and use Φ 0.82mmNb
3The Sn superconducting wire.
Embodiment 1
High-tin bronze ingot boring back and the assembling of niobium alloy rod, adopt EB electron beam vacuum seal afterwards, obtain the blank to be extruded of diameter of phi 200mm, obtain diameter of phi 60mm rod base a through hot extrusion again, with excellent base a as the stretching blank annealing furnace of packing into, carry out the annealing first time, be evacuated down to less than 1.0 * 10 behind the annealing furnace of packing into
-2Pa fills high-purity argon gas in the furnace chamber, vacuum degree is 8.5 * 10
3Pa adopts the programming rate of 4 ℃/min to be heated to 420 ℃; Adopt thermocouple to monitor the material temperature, the material temperature is incubated 30 minutes after 420 ℃; Insulation finishes the back and adopts the pure argon circulation cold by force, the material temperature is come out of the stove for 50 ℃, according to 10% working modulus material is stretched repeatedly, obtain six side's subgroup units through subgroup unit moulding process again, the six side's subgroups unit and barrier layer, the copper-clad cover that obtain are finally assembled, and adopt vacuum seal to obtain billet to be extruded, obtain excellent base b through hot extrusion, should rod base b as the stretching blank annealing furnace of packing into, carry out the annealing process second time, be evacuated down to less than 1.0 * 10 behind the annealing furnace of packing into
-2Pa fills high-purity argon gas in the furnace chamber, vacuum degree is 8.5 * 10
3Pa adopts the programming rate of 4 ℃/min to be heated to 420 ℃; Adopt thermocouple to monitor the material temperature, the material temperature is incubated 30 minutes after 420 ℃; Insulation finishes the back and adopts the pure argon circulation cold by force, and the material temperature is come out of the stove for 50 ℃, according to 10% working modulus material is stretched repeatedly, obtains twisting line base, with the line base again through twisting, finally stretch and electroplate, obtain the Nb that toroidal field coil is used Φ 0.82mm
3The Sn superconducting wire.
Finally record wire rod performance I
cBe 160A.
Embodiment 2
High-tin bronze ingot boring back and the assembling of niobium alloy rod, adopt EB electron beam vacuum seal afterwards, obtain the blank to be extruded of diameter of phi 100mm, obtain diameter of phi 30mm rod base a through hot extrusion again, with excellent base a as the stretching blank annealing furnace of packing into, carry out the annealing first time, be evacuated down to 8.5 * 10 behind the annealing furnace of packing into
-3Pa fills high pure nitrogen in the furnace chamber, vacuum degree is 5.3 * 10
3Pa adopts the speed of 5 ℃/min to be heated to 480 ℃; Adopt thermocouple to monitor the material temperature, the material temperature is incubated 60 minutes after 480 ℃; Insulation finishes the back and adopts the pure nitrogen gas circulation cold by force, and the material temperature is come out of the stove for 100 ℃; According to 20% working modulus material is stretched repeatedly, obtain six side's subgroup units through subgroup unit moulding process again, the six side's subgroups unit and barrier layer, the copper-clad cover that obtain are finally assembled, adopt vacuum seal to obtain billet to be extruded, obtain excellent base b through hot extrusion, should rod base b as the stretching blank annealing furnace of packing into, carry out the annealing process second time, be evacuated down to 8.5 * 10 behind the annealing furnace of packing into
-3Pa fills high pure nitrogen in the furnace chamber, vacuum degree is 5.3 * 10
3Pa adopts the speed of 5 ℃/min to be heated to 480 ℃; Adopt thermocouple to monitor the material temperature, the material temperature is incubated 60 minutes after 480 ℃; Insulation finishes the back and adopts the pure nitrogen gas circulation cold by force, and the material temperature is come out of the stove for 100 ℃; According to 20% working modulus material is stretched repeatedly, obtain twisting line base, the line base is passed through twisting again, finally stretches and electroplates, obtain the Nb of toroidal field coil with Φ 0.82mm
3The Sn superconducting wire.
Final test wire rod performance I
cBe 180A.
Embodiment 3
High-tin bronze ingot boring back and the assembling of niobium alloy rod, adopt EB electron beam vacuum seal afterwards, obtain the blank to be extruded of diameter of phi 170mm, obtain diameter of phi 55mm rod base a through hot extrusion again, with excellent base a as the stretching blank annealing furnace of packing into, carry out the annealing first time, be evacuated down to 6.5 * 10 behind the annealing furnace of packing into
-3Pa fills high-purity argon gas in the furnace chamber, vacuum degree is 1.01 * 10
5Pa adopts the speed of 8 ℃/min to be heated to 430 ℃; Adopt thermocouple to monitor the material temperature, the material temperature is incubated 90 minutes after 430 ℃; Insulation finishes the back and adopts the pure argon circulation cold by force, and the material temperature is come out of the stove for 60 ℃; According to 30% working modulus material is stretched repeatedly; Obtain six side's subgroup units through subgroup unit moulding process again, the six side's subgroups unit and barrier layer, the copper-clad cover that obtain are finally assembled, adopt vacuum seal to obtain billet to be extruded, obtain excellent base b through hot extrusion, should rod base b as the stretching blank annealing furnace of packing into, carry out the annealing process second time, be evacuated down to 6.5 * 10 behind the annealing furnace of packing into
-3Pa fills high-purity argon gas in the furnace chamber, vacuum degree is 1.01 * 10
5Pa adopts the speed of 8 ℃/min to be heated to 430 ℃; Adopt thermocouple to monitor the material temperature, the material temperature is incubated 90 minutes after 430 ℃; Insulation finishes the back and adopts the pure argon circulation cold by force, and the material temperature is come out of the stove for 60 ℃; According to 30% working modulus material is stretched repeatedly; Obtain twisting line base, the line base is passed through twisting again, finally stretches and electroplates, obtain the Nb of toroidal field coil with Φ 0.82mm
3The Sn superconducting wire.
Final test wire rod performance I
cBe 170A.
By embodiment 1 to embodiment 3 as can be seen the product line performance be improved I
cReached more than the 160A, be far longer than existing 520 ℃ of product line current-carrying I that Technology for Heating Processing makes
c100A.
Fig. 1 is the core silk exterior view that adopts existing bronze heterogeneousization full annealing technology under the scanning electron microscopy, and Fig. 2 is the step that adopts embodiment 2, core silk exterior view under the scanning electron microscopy.Existing as can be seen annealing process and the improved annealing process of this patent are to the influence of core silk surface appearance, and the core silk of Fig. 1 is rough, have graininess to rise and fall, and this is owing to generate Nb too early in annealing process
3The cause of Sn like this can be to Nb
3The mechanical property of Sn superconducting wire and current-carrying performance are influential, and Fig. 2 core silk surface is smooth than Fig. 1 as can be seen, the improved annealing process of the present invention has effectively improved core silk surface, has reduced too early generation Nb
3The situation of Sn, the current-carrying performance also is improved, and is brought up to more than the 160A by 100A.
Claims (1)
1. the preparation technology of a bronze method Nb3Sn superconducting wire, it is characterized in that, high-tin bronze ingot boring back and the assembling of niobium alloy rod, adopt EB electron beam vacuum seal afterwards, obtain blank to be extruded, obtain excellent base a through hot extrusion again, with excellent base a as the stretching blank annealing furnace of packing into, carry out the annealing first time, annealing process specifically carries out according to following steps for the first time:
Step 1
Use mechanical pump to be extracted into low vacuum and use diffusion pump to be extracted into high vacuum then, vacuum degree≤1.0 * 10
-2Pa; Fill high-purity argon gas or nitrogen in the furnace chamber of annealing furnace, vacuum degree is 5.3 * 10
3Pa-1.01 * 10
5Pa with furnace chamber heating, is heated to 420 ℃-480 ℃ with raise 4 ℃-8 ℃ speed of per minute, adopts thermocouple monitoring material temperature, is incubated 30-90 minute then; Adopt argon gas or nitrogen circulation cold by force at last, come out of the stove when the material temperature is cooled to 50 ℃-100 ℃;
Step 2
According to the technical process of step 1 and adopt 10%～30% working modulus processing materials repeatedly, annealing process is finished for the first time;
And then process subgroup unit moulding process obtains six side's subgroup units, the six side's subgroups unit and barrier layer, the copper-clad cover that obtain are assembled, adopt vacuum seal to obtain billet to be extruded, obtain excellent base b through hot extrusion, should rod base b as the stretching blank annealing furnace of packing into, carry out second time annealing process and obtain twisting line base, for the second time annealing process with described first time annealing process step and annealing conditions identical, then the line base is passed through twisting again, finally stretches and electroplates, obtain bronze method Nb
3The Sn superconducting wire.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106057356A (en) * | 2016-06-14 | 2016-10-26 | 西部超导材料科技股份有限公司 | Preparation method of CuNb reinforced Nb3Sn low-temperature superconducting wire fabricated by bronze process |
| CN110580984A (en) * | 2018-06-11 | 2019-12-17 | 西部超导材料科技股份有限公司 | Preparation method of copper-clad bronze/Nb composite rod |
| CN113373404A (en) * | 2021-06-10 | 2021-09-10 | 中国科学院近代物理研究所 | Copper-based thick-wall Nb3Sn film superconducting cavity and preparation method thereof |
| CN115295242A (en) * | 2022-09-30 | 2022-11-04 | 西部超导材料科技股份有限公司 | Preparation method of niobium-tin superconducting strand with high critical current density |
| CN117292887A (en) * | 2023-11-27 | 2023-12-26 | 西安聚能超导线材科技有限公司 | Preparation method of bronze niobium three-tin superconducting wire and superconducting wire |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106057356A (en) * | 2016-06-14 | 2016-10-26 | 西部超导材料科技股份有限公司 | Preparation method of CuNb reinforced Nb3Sn low-temperature superconducting wire fabricated by bronze process |
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| CN110580984B (en) * | 2018-06-11 | 2021-08-03 | 西部超导材料科技股份有限公司 | Preparation method of copper-clad bronze/Nb composite rod |
| CN113373404A (en) * | 2021-06-10 | 2021-09-10 | 中国科学院近代物理研究所 | Copper-based thick-wall Nb3Sn film superconducting cavity and preparation method thereof |
| CN113373404B (en) * | 2021-06-10 | 2022-09-27 | 中国科学院近代物理研究所 | Copper-based thick-wall Nb 3 Sn film superconducting cavity and preparation method thereof |
| CN115295242A (en) * | 2022-09-30 | 2022-11-04 | 西部超导材料科技股份有限公司 | Preparation method of niobium-tin superconducting strand with high critical current density |
| CN115295242B (en) * | 2022-09-30 | 2023-01-24 | 西部超导材料科技股份有限公司 | Preparation method of niobium tri-tin superconducting stranded wire with high critical current density |
| CN117292887A (en) * | 2023-11-27 | 2023-12-26 | 西安聚能超导线材科技有限公司 | Preparation method of bronze niobium three-tin superconducting wire and superconducting wire |
| CN117292887B (en) * | 2023-11-27 | 2024-02-20 | 西安聚能超导线材科技有限公司 | Preparation method of bronze niobium three-tin superconducting wire and superconducting wire |
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Address after: 710018 Shaanxi Province Economic and Technological Development Zone Xi'an Mingguang Road No. 12 Patentee after: Western Superconducting Technologies Co., Ltd. Address before: 710018, Mingguang Road, Xi'an, Shaanxi, 12 Patentee before: Western Superconducting Technologies Co., Ltd. |