CN100375794C - Bismuth high-temperature superconducting tape and its manufacturing method - Google Patents
Bismuth high-temperature superconducting tape and its manufacturing method Download PDFInfo
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- CN100375794C CN100375794C CNB2005101327242A CN200510132724A CN100375794C CN 100375794 C CN100375794 C CN 100375794C CN B2005101327242 A CNB2005101327242 A CN B2005101327242A CN 200510132724 A CN200510132724 A CN 200510132724A CN 100375794 C CN100375794 C CN 100375794C
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Abstract
The present invention relates to a preparation method of a bismuth series Bi-2223 high-temperature superconductive belt material, which is characterized in that bismuth series superconductive powder is pressed into bar material by an isostatic pressing method and is immediately loaded into a sealed and welded silver tube after arranged in a furnace to be heated to 300 to 600 DEG for 20 hours of thermal insulation, a pumping end is pressed and sealed after the vacuum of the silver tube which is loaded with the bar material is pumped to 10<-3> by a vacuum device, and the silver tube is processed in a drawing way. The gas adsorbed in the powder and the gas in gaps between the inner wall of the silver tube and the bar material can be effectively removed by the present invention, and the surface of the bismuth series belt material can be prevented from bubbling because of residual gas expansion in the process of high temperature heat treatment. The method has the advantages of simplicity, convenience, good technology repeatability and high productive efficiency; furthermore, the present invention is favorable to enhance the homogeneity and the current carrying performance of the belt material.
Description
Technical field
A kind of bismuth is the preparation method of Bi-2223 belt material of high temperature superconduct, relates to rational tubulature of a kind of employing and degasification system and avoids band bubbling and improve the inhomogeneity method of band electrical property in heat treatment process.
Background technology
Since high temperature superconducting materia in 1986 was found, the Bi-based high-temperature superconductive body was considered to one of high temperature superconducting materia of tool large-scale application prospect owing to its good processing properties is easy to process growth line (band) material.Through the development in surplus ten years, Bi-based high-temperature superconductive strip all had breakthrough on current-carrying performance and band single line length, and its critical current density (Jc) reaches as high as 74000A/cm
2(77K, self-fields), single line length surpasses 1500m, satisfies the requirement that engineering is used substantially.But adopt the bi tape of ordinary powder tubulature method (PIT) preparation, silver-colored pipe process is carried out in atmosphere because powder is packed into, can in silver-colored pipe, introduce gas inevitably, when band thermal treatment, can expand and cause strip surface the bubbling phenomenon to occur thereby remain in gas in the silver pipe.The bubbling of band in heat treatment process not only can destroy the orientations of the inner superconduction crystal grain of bubbling place band, make the current-carrying degradation of band, and can cause the current-carrying performance of band to present significant ununiformity along the band length direction, be that bubbling place band critical current density is low, still place band critical current density height.Bismuth is the performance ununiformity that this because bubbling of superconducting tape causes, and becomes a big obstacle of its large-scale engineering applications.From the essence of bubbling, caused by entrap bubble in the powder of the silver-colored pipe of packing into.Residual gas produces very big pressure owing to expanding when band thermal treatment, and the very low parchment covering of intensity is heaved.For preventing that the bubbling phenomenon from appearring in strip surface, adopt two kinds of means usually: 1) external pressurized method: at high temperature (840 ℃) are pressurized to 〉=0.5Mp, make the band air pressure that external pressure produces owing to gas expansion greater than inside when thermal treatment; 2) avoid the adsorbed gas method: pack into the silver-colored pipe stage at powder, powder, silver-colored pipe are placed assembling under the vacuum state.Above-mentioned two kinds of methods all need to purchase special equipment, invest very greatly, are unfavorable for the promotion and application of technology.
Summary of the invention
The deficiency that the purpose of invention exists at above-mentioned prior art, providing a kind of can effectively remove powder pack into when pipe silver and enter the gas of silver-colored pipe with powder, avoid bi tape the bubbling phenomenon when thermal treatment, to occur, improve the critical current density of the long band of bismuth system and the homogeneity of electrical property, the preparation method of simple Bi-based high-temperature superconductive strip.
The objective of the invention is to be achieved through the following technical solutions.
A kind of bismuth is the preparation method of Bi-2223 belt material of high temperature superconduct, is characterised in that its preparation process is followed successively by:
A. be bismuth that the Bi-2223 superconductive powder is made bar with the method compacting that waits static pressure;
B. bar is heated to 300-600 ℃, insulation 20h;
C. will install to one from the bar that process furnace takes out immediately by the silver-colored pipe of soldering and sealing, be evacuated down to 10 with will pack into the silver-colored pipe of bar of vacuum unit
-3Handkerchief keeps after one hour the press seal end of bleeding, the silver that obtains sealing-superconduction rod complex body;
Filament is processed in the drawing of the silver that d. will seal-superconduction rod complex body, arranges by six sides after being cut into 37 sections and is assembled into the AgMn compo pipe, obtains the multiple-unit tube of 37 cores, carries out drawing again and is processed into filament, and filament is rolled into the centre strip on accurate flat roll mill;
E. be to heat-treat 40 hours under 840 ℃ of temperature with the intermediate thin band of making, carry out intermediate rolling subsequently, be rolled into the final size band, carry out the thermal treatment second time again, thermal treatment temp is 825 ℃, and soaking time 70 hours obtains the finished product band.
Method of the present invention is characterized in that heat treated atmosphere is the argon oxygen gas mixture.
Method of the present invention, when the preparation bismuth was the Bi-2223 belt material of high temperature superconduct, used powder was removed residual gas when tubulature, and method is simple, efficient is high, is applicable to the degasification of bismuth series superconducting material in the tubulature process of adopting the powder-in-tube technique preparation.Can effectively remove the gas that adsorbs in the powder and the gas in the gap between silver-colored inside pipe wall and the powder bar, the bismuth that guarantees hundred meters magnitude length is superconducting tape zero bubbling when thermal treatment, prevent the reaction of gas and powder, improve the homogeneity of band critical current density and current-carrying performance.The bubbling number is zero after the bi tape thermal treatment of hundred meters magnitude length, has improved the homogeneity of band performance.Compare with common band without the tubulature degasification, the bubbling number of strip surface is by the individual zero that is reduced to of original hundreds of after the thermal treatment for the first time, band electrical property homogeneity (n value) is brought up to 18-25 by original 7-9, critical current (Ic) is brought up to 80-90A by 60-70A, and the band over-all properties significantly improves.Present method does not need expensive complicated Special Equipment, less investment, and simple to operate, good reproducibility just can be realized at general production unit, is suitable for large-scale application.
Specific embodiments
A kind of bismuth is the preparation method of Bi-2223 belt material of high temperature superconduct, it is equipped with process and is followed successively by: a. is bismuth the method that superconductive powder usefulness waits static pressure, under 100Mpa pressure, being pressed into the uniform diameter of size is the bar of 8-20mm, can discharge gas in the powder gap by this process.B. the powder bar is placed process furnace to be heated to 300-600 ℃, insulation 20h makes the gaseous diffusion of bar internal physical absorption also overflow to the bar surface.C. will install to one from the bar that process furnace takes out immediately by the silver-colored pipe of soldering and sealing, be evacuated down to 10 with will pack into the silver-colored pipe of bar of vacuum unit
-3Handkerchief keeps after one hour with the clamp press seal end of bleeding, the silver that obtains sealing-superconduction rod complex body.Can discharge gas in the gap between silver-colored inside pipe wall and the bar by this process.The silver that d. will seal-superconduction rod complex body drawing processing, obtain the filament of φ 2.55mm, be assembled into the AgMn compo pipe by six sides arrangement after being cut into 37 sections, obtain the multiple-unit tube of 37 cores, carry out drawing processing again, obtain the filament of φ 1.70mm, filament is rolled into thickness on accurate flat roll mill be that 0.33mm, width are the strip of 3.7mm.E. the thermal treatment first time of band is carried out in air, select 840 ℃ of thermal treatments 40 hours for use, carry out intermediate rolling subsequently, being rolled into thickness is that 0.26mm, width are the final size band of 4.1mm, carry out the thermal treatment second time again, thermal treatment temp is 825 ℃, soaking time 70 hours, and heat-treating atmosphere is the argon oxygen gas mixture.After finishing, band thermal treatment for the second time obtains the finished product band, the no bubble in surface.Strip surface does not all have bubble and occurs after thermal treatment for the first time and the thermal treatment for the second time, and the band critical current (Ic) that finally obtains be 80-90A, and the inhomogeneity n value of sign band electrical property is 18-25, increases significantly than the band of usual way tubulature.
Specify example according to the invention below.
Example 1
With bismuth is that superconductive powder is packed in the rubber sleeve, two ends shutoff jam-pack, and the overcoat protection metal pipe, pressure 100MPa, pressurize 1 minute, isostatic pressing, the rod that obtains is of a size of φ 19 * 420mm.Smooth being placed on of excellent surfacing is heated to 600 ℃ and be incubated 20h in the tubular oven, installs to immediately in φ 21 * 1.8mm silver pipe after process furnace takes out bar, silver-colored Guan Yiduan is with copper plug welded seal, and the other end is with having the plug welding that copper pipe is bled and chewed.The silver-colored pipe coupling of bar will pack into to the vacuum unit, use diffusion pump again with mechanical pump earlier, and make the system vacuum degree reach 1.0 * 10
-3Pa keeps after 1 hour the copper extraction pipe being heated to 600 ℃, uses clamp extraction pipe soldering and sealing again, the silver that obtains sealing-superconduction rod complex body.Silver-superconduction rod complex body the drawing of sealing is worked into the filament that is of a size of φ 2.55mm, is cut into after 37 sections and arranges the AgMn compo pipe that is assembled into φ 21 * 1.5mm, obtain the multiple-unit tube of 37 cores, carry out drawing processing again, obtain the filament of φ 1.70mm by six sides.Filament is rolled into thickness on accurate flat roll mill be that 0.33mm, width are the strip of 3.7mm.The band heat treatment process parameter is as follows: thermal treatment (HT1) for the first time, and thermal treatment temp is 840 ℃, and soaking time is 40h, and heat-treating atmosphere is an air; Carry out intermediate rolling subsequently, being rolled into thickness is that 0.26mm, width are the final size band of 4.1mm, carries out the thermal treatment second time (HT2) again, and thermal treatment temp is 825 ℃, soaking time 70 hours, and heat-treating atmosphere is the argon oxygen gas mixture.After finishing, band thermal treatment for the second time obtains the finished product band.Strip surface does not all have bubble and occurs after thermal treatment for the first time and the thermal treatment for the second time, and the band length that finally obtains is 350 meters, and critical current (Ic) be 82A, and the inhomogeneity n value of sign band electrical property is 18, increases significantly than the band of usual way tubulature.
Example 2
With bismuth is that superconductive powder is packed in the rubber sleeve, two ends shutoff jam-pack, and the overcoat protection metal pipe, pressure 100Mpa, pressurize 1 minute, isostatic pressing, the rod that obtains is of a size of φ 16 * 550mm.Smooth being placed on of excellent surfacing is heated to 450 ℃ and be incubated 20h in the tubular oven, installs to immediately in φ 18 * 1.5mm silver pipe after process furnace takes out bar, silver-colored Guan Yiduan is with copper plug welded seal, and the other end is with having the plug welding that copper pipe is bled and chewed.The silver-colored pipe coupling of bar will pack into to the vacuum unit, use diffusion pump again with mechanical pump earlier, and make the system vacuum degree reach 1.0 * 10
-3Pa keeps after 1 hour the copper extraction pipe being heated to 700 ℃, uses clamp extraction pipe soldering and sealing again, the silver that obtains sealing-superconduction rod complex body.Silver-superconduction rod complex body the drawing of sealing is worked into the filament that is of a size of φ 2.55mm, is cut into after 37 sections and arranges the AgMn compo pipe that is assembled into φ 21 * 1.5mm, obtain the multiple-unit tube of 37 cores, carry out drawing processing again, obtain the filament of φ 1.70mm by six sides.Filament is rolled into thickness on accurate flat roll mill be that 0.33mm, width are the strip of 3.7mm.The band heat treatment process parameter is as follows: thermal treatment (HT1) for the first time, and thermal treatment temp is 840 ℃, and soaking time is 40h, and heat-treating atmosphere is an air; Carry out intermediate rolling subsequently, being rolled into thickness is that 0.26mm, width are the final size band of 4.1mm, carries out the thermal treatment second time (HT2) again, and thermal treatment temp is 825 ℃, soaking time 70 hours, and heat-treating atmosphere is the argon oxygen gas mixture.After finishing, band thermal treatment for the second time obtains the finished product band.Strip surface does not all have bubble and occurs after thermal treatment for the first time and the thermal treatment for the second time, and the band length that finally obtains is 288 meters, and critical current (Ic) be 85A, and the inhomogeneity n value of sign band electrical property is 21, increases significantly than the band of usual way tubulature.
Example 3
With bismuth is that superconductive powder is packed in the rubber sleeve, two ends shutoff jam-pack, and the overcoat protection metal pipe, pressure 100Mpa, pressurize 1 minute, isostatic pressing, the rod that obtains is of a size of φ 9 * 700mm.Smooth being placed on of excellent surfacing is heated to 300 ℃ and be incubated 20h in the tubular oven, installs to immediately in φ 11 * 1.2mm silver pipe after process furnace takes out bar, silver-colored Guan Yiduan is with copper plug welded seal, and the other end is with having the plug welding that copper pipe is bled and chewed.The silver-colored pipe coupling of bar will pack into to the vacuum unit, use diffusion pump again with mechanical pump earlier, and make the system vacuum degree reach 1.0 * 10
-3Pa keeps after 1 hour the copper extraction pipe being heated to 650 ℃, uses clamp extraction pipe soldering and sealing again, the silver that obtains sealing-superconduction rod complex body.Silver-superconduction rod complex body the drawing of sealing is worked into the filament that is of a size of φ 2.55mm, is cut into after 37 sections and arranges the AgMn compo pipe that is assembled into φ 21 * 1.5mm, obtain the multiple-unit tube of 37 cores, carry out drawing processing again, obtain the filament of φ 1.70mm by six sides.Filament is rolled into thickness on accurate flat roll mill be that 0.33mm, width are the strip of 3.7mm.The band heat treatment process parameter is as follows: thermal treatment (HT1) for the first time, and thermal treatment temp is 840 ℃, and soaking time is 40h, and heat-treating atmosphere is an air; Carry out intermediate rolling subsequently, being rolled into thickness is that 0.26mm, width are the final size band of 4.1mm, carries out the thermal treatment second time (HT2) again, and thermal treatment temp is 825 ℃, soaking time 70 hours, and heat-treating atmosphere is the argon oxygen gas mixture.After finishing, band thermal treatment for the second time obtains the finished product band.Strip surface does not all have bubble and occurs after thermal treatment for the first time and the thermal treatment for the second time, and the band length that finally obtains is 235 meters, and critical current (Ic) be 90A, and the inhomogeneity n value of sign band electrical property is 25, increases significantly than the band of usual way tubulature.
Claims (2)
1. preparation method that bismuth is the Bi-2223 belt material of high temperature superconduct is characterised in that its preparation process is followed successively by:
A. be bismuth that the Bi-2223 superconductive powder is made bar with the method compacting that waits static pressure;
B. bar is heated to 300-600 ℃, insulation 20h;
C. will install to one from the bar that process furnace takes out immediately by the silver-colored pipe of soldering and sealing, be evacuated down to 10 with will pack into the silver-colored pipe of bar of vacuum unit
-3Pa keeps after one hour the press seal end of bleeding, the silver that obtains sealing-superconduction rod complex body;
Filament is processed in the drawing of the silver that d. will seal-superconduction rod complex body, arranges by six sides after being cut into 37 sections and is assembled into the AgMn compo pipe, obtains the multiple-unit tube of 37 cores, carries out drawing again and is processed into filament, and filament is rolled into the centre strip on accurate flat roll mill;
E. be to heat-treat 40 hours under 840 ℃ of temperature with the intermediate thin band of making, carry out intermediate rolling subsequently, be rolled into the final size band, carry out the thermal treatment second time again, thermal treatment temp is 825 ℃, and soaking time 70 hours obtains the finished product band.
2. method according to claim 1 is characterized in that heat treated atmosphere is the argon oxygen gas mixture.
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| CN100375794C true CN100375794C (en) | 2008-03-19 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101361144B (en) * | 2007-01-11 | 2012-04-04 | 住友电气工业株式会社 | Oxide superconducting wire rod, superconducting structure, method for manufacturing oxide superconducting wire rod, superconducting cable, superconducting magnet, and product comprising superconductin |
| CN101714429B (en) * | 2009-12-18 | 2011-06-08 | 西北有色金属研究院 | Preparation method for Bi-2212 high-temperature superconducting wires |
| CN101872659B (en) * | 2010-05-21 | 2012-04-18 | 西北有色金属研究院 | Preparation method of Bi-2212 high-temperature superconductivity wire |
| CN103839630B (en) * | 2014-03-25 | 2015-12-30 | 西北有色金属研究院 | A kind of preparation method of Bi-2212 hts tape/band |
| CN106057353B (en) * | 2016-05-18 | 2017-05-31 | 西北有色金属研究院 | A kind of preparation method of the multi-core superconducting bands of Bi 2223 |
| CN105869777B (en) * | 2016-05-20 | 2017-12-26 | 西北有色金属研究院 | A kind of preparation method of the superconducting tapes of Bi 2223 |
| CN108538499B (en) * | 2018-04-10 | 2019-12-10 | 西部超导材料科技股份有限公司 | Bi-2223 superconducting strip preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039922A (en) * | 1988-07-25 | 1990-02-21 | 富士通株式会社 | Be used to prepare the technology of superconductor |
| CN1041058A (en) * | 1988-09-03 | 1990-04-04 | 赫彻斯特股份公司克纳普萨克工厂 | The production method of high-temperature superconductor and by its formed body of forming |
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- 2005-12-28 CN CNB2005101327242A patent/CN100375794C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1039922A (en) * | 1988-07-25 | 1990-02-21 | 富士通株式会社 | Be used to prepare the technology of superconductor |
| CN1041058A (en) * | 1988-09-03 | 1990-04-04 | 赫彻斯特股份公司克纳普萨克工厂 | The production method of high-temperature superconductor and by its formed body of forming |
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