CN1865457A - Heat treatment method for iron base MgB2 superconductor wire and belt - Google Patents
Heat treatment method for iron base MgB2 superconductor wire and belt Download PDFInfo
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- CN1865457A CN1865457A CNA2006100122150A CN200610012215A CN1865457A CN 1865457 A CN1865457 A CN 1865457A CN A2006100122150 A CNA2006100122150 A CN A2006100122150A CN 200610012215 A CN200610012215 A CN 200610012215A CN 1865457 A CN1865457 A CN 1865457A
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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
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- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
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Abstract
The invention discloses a heat disposal method of iron-base magnesium diboride superconductive wire, which is characterized by the following: disposing the core superconductive material through joule heat of current flow; blending magnesite powder and boron powder evenly according to chemical gauge rate; filling the mixture in the iron pipe after grinding; producing iron-base leptctene and fasciola material with magnesite powder and boron powder in the middle through rotating, drawing and rolling; connecting two ends of leptctene or fasciola with blaster fuse in the Ar quartz tube; controlling the heating speed at 45-900 deg.c per min and heat disposal temperature at 600-900 deg.c; keeping temperature for 10-60 min; cooling at 30-300 deg.c per min to approach indoor temperature. The invention can improve the heating and cooling speed in the heat disposal course, which increases the marginal current density value of magnesium diboride superconductive wire.
Description
Technical field
The invention belongs to preparation method, particularly a kind of heat treating method of MgB 2 superconductor wire and belt to superconducting material.
Background technology
On January 10 calendar year 2001, the Japanese green hill professor Qiu Guangchun people such as (J.Akimitsu) of institute announces to find magnesium diboride (MgB
2) when 39K, have superconductivity.It is a compound superconductive between the highest binary metal of the critical temperature found so far, and the highest binary compound of Tc that the past is found is niobium three germanium (Nb
3Ge), its transition temperature is 23.2K, improves nearly 16K.And magnesium diboride material is a kind of A15 structure binary compound, has characteristics such as weak connection of simple, with low cost, the no crystal boundary of synthesis technique and room temperature resistance rate are low.In addition, MgB
2The magnet of superconducting line coiled also can be worked under the temperature of 20K well, and available power gas driving refrigerator substitutes expensive liquid helium and implements cooling.Thereby MgB
2Being found to be of supraconductivity developed cheaply superconducting material and opened up new way, is expected to become cheapness, practical new superconduction material.At present the preparation process of MgB 2 superconductor wire and belt comprises: in the metal jacket filler, be cold worked into the tape material and the final thermal treatment that contain superconducting core.Yet, Nb than widespread use is a low temperature superconducting material at present, the critical current of magnesium diboride super conductive material is also very low, and this practicalization that just influences magnesium diboride super conductive material greatly (sees C.Buzea et al for details, Review of superconductingproperties of MgB
2, cond-mat/0108265,2001).
As everyone knows, boron powder and magnesium powder are in different adding under the gentle cooling rate, the inner defect Mechanism that produces is different, because the pinning effect of defective, the magnesium diboride super conductive material critical current of preparing is also made a world of difference and (is seen S.K.Chen for details, etal., Applied Physics Letters 87,182504,2005).Generally speaking, fast heat-up rate and cooling rate form small grains in superconductor, can improve the critical current density of MgB 2 superconductor wire and belt material.And at present the resistance furnace mode is adopted in magnesium diboride super conductive material thermal treatment.Though at present the resistance furnace heat treatment mode is improved to some extent, as: adopt resistance furnace heat treatment mode under the high-intensity magnetic field, also obtain good effect, as the method for CN1683281A proposition.But because resistance furnace device structure restriction, lifting temperature speed generally is no more than 90 ℃/min, is unfavorable for increasing the defect concentration of material behind the magnesium diboride material sintering.And defect concentration is low, and effectively pinning center's density must reduce the corresponding reduction of superconducting critical current density value.
Summary of the invention
The objective of the invention is to propose a kind of heat treating method of new MgB 2 superconductor wire and belt material, to improve the critical current density of mgb 2 superconductor.
Flow through joule heating that MgB 2 superconductor wire band sheath material electric current produces of utilization of the present invention heats superconduction powder in the jacket.Its method and processing step are as follows successively:
(1) with purity 99.5%, granularity is that 100～200 purpose magnesium powder and purity are 92%～99.99%, and granularity is 100 purpose boron powder, mixes by magnesium diboride theoretical chemistry metered proportions, and ball milling is 1 hour then;
(2) magnesium powder behind the ball milling and boron powder are inserted iron pipe, compress, tamp the blended powder after, sealing iron pipe two ends port;
(3) iron pipe is adopted 20～40 passages are swaged, the cold mechanical workout mode of drawing, control every time deflection in 1%～50% scope, the center of must arrive is filled with the iron-based fine rule of magnesium powder and boron powder, and fine rule is through acquisition faciola material behind the flat rolling; To can obtain split conductor, carrying material more than the stranded back cold working of two iron-based fine rule;
(4) line sample or carry sample two ends are connected lead-in wire and place silica tube, quartzy cap on the two end cap is taken out silica tube to vacuum tightness＜1Pa with vacuum pump, feeds high-purity Ar subsequently and (also can be other rare gas element such as N
2, H
2, CH
4Or vacuum state) under protection of inert gas, begins heated sample;
(5) with power supply on two terminations, regulate supply current value size, (30～100A), the test sample temperature is behind 45 ℃/min of control sample heat-up rate～900 ℃/min to 600～900 ℃ through the current value size of sample for controlling flow, insulation 10min～60min, control power supply output then, be chilled to room temperature, close Ar gas with 30 ℃/min～300 ℃/min speed cooling, take out sample, get iron base MgB 2 superconductor wire and belt.
When big electric current flows through the outer sheath material of iron-based, can produce certain electromagnetic field in core body, while thermal treatment product magnesium diboride has conductive capability, also has electric current and flows through, and magnetic field will produce Lorentz force: F=J * B to inner transverse current component.In the high-temperature fusion process, this internal forces makes the material production stirring effect, get rid of inner entrap bubble cavity, help the crystal refinement, material component is more even, make the densification of magnesium diboride core material, improve the crystalline connectivity, finally improve the critical current density of MgB 2 superconductor wire and belt material.The present invention has actual application value in serialization scale production process.
The preparation method of MgB 2 superconductor wire and belt of the present invention, the atmosphere when it is characterized in that thermal treatment be vacuum condition or oxygen-free inert atmosphere conditions, and rare gas element is as Ar, N
2, H
2Or CH
4Deng.
Embodiment
Further specify the present invention below in conjunction with embodiment.
Embodiment 1
By 1: 2 molar ratio with purity 99.5%, granularity 100 purpose magnesium powder and purity are 92%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 14mm internal diameter 10mm iron pipe, after compressing, tamping, the sealing iron pipe two ends.Then iron pipe is swaged through 40 passages, the cold working of drawing series, control every time deflection in 1%～5% scope, the center of must arriving is filled with the iron-based Φ 1.75mm fine rule of magnesium powder and boron powder, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 70A, controlling flow is through the current value size of sample, after making 100 ℃ of sample heat-up rates/min to 750 ℃, insulation 45min, control current then, be chilled to room temperature with the cooling of 30 ℃/min speed, close Ar gas, take out sample, get the iron base MgB 2 superconductor wire material.
Embodiment 2
Pressing 1: 2 molar ratio with purity 99.5%, granularity 200 purpose magnesium powder and purity are 99.99%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 14mm internal diameter 10mm iron pipe, after compressing, tamping, shut the iron pipe two ends, then with iron pipe through the swaging of 36 passages, drawing, control every time deflection in 3%～16% scope, obtain fine rule, must arrive iron-based 4 * 0.5mm that the center is filled with magnesium powder and boron powder through rolling again
2Faciola.Two ends connect lead-in wire and place silica tube, and quartzy cap on two end caps is taken out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 100A, controlling flow is through the current value size of sample, make 900 ℃ of sample heat-up rates/min to 700 ℃ after, insulation 60min, control current is chilled to room temperature with the cooling of 300 ℃/min speed then, closes Ar gas, take out sample, get iron-based magnesium diboride superconducting tape.
Embodiment 3
Pressing 1: 2 molar ratio with purity 99.5%, granularity 150 purpose magnesium powder and purity are 96%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 14mm internal diameter 10mm iron pipe, after compressing, tamping, shut the iron pipe two ends, with iron pipe through the swaging of 20 passages, drawing, control every time deflection in 2%～30% scope, obtain fine rule, must arrive iron-based 4 * 0.5mm that the center is filled with magnesium powder and boron powder through rolling again
2Faciola, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 30-50A, controlling flow is through the current value size of sample, after making 45 ℃ of sample heat-up rates/min to 900 ℃, insulation 10min, control current then, be chilled to room temperature with the cooling of 30 ℃/min speed, close Ar gas, take out sample, get iron-based magnesium diboride superconducting tape.
Embodiment 4
Pressing 1: 2 molar ratio with purity 99.5%, granularity 100 purpose magnesium powder and purity are 94%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 14mm internal diameter 10mm iron pipe, after compressing, tamping, shut the iron pipe two ends, with iron pipe through the swaging of 25 passages, drawing, control every time deflection in 2%～40% scope, obtain fine rule, must arrive iron-based 4 * 0.5mm that the center is filled with magnesium powder and boron powder through rolling again
2Faciola, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 80A, controlling flow is through the current value size of sample, after making 300 ℃ of sample heat-up rates/min to 800 ℃, insulation 30min, control current then, be chilled to room temperature with the cooling of 100 ℃/min speed, close Ar gas, take out sample, get iron-based magnesium diboride superconducting tape.
Embodiment 5
Pressing 1: 2 molar ratio with purity 99.5%, granularity 200 purpose magnesium powder and purity are 92%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 14mm internal diameter 10mm iron pipe, after compressing, tamping, shut the iron pipe two ends, iron pipe is through the swaging of 30 passages, drawing, control every time deflection in 3%～30% scope, obtain fine rule, must arrive iron-based 4 * 0.5mm that the center is filled with magnesium powder and boron powder through rolling again
2Faciola, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, regulate electric power outputting current 75A, controlling flow is through the current value size of sample, make 200 ℃ of sample heat-up rates/min to 750 ℃ after, insulation 45min, control current is chilled to room temperature with the cooling of 90 ℃/min speed then, removes vacuum state, take out sample, get iron-based magnesium diboride superconducting tape.
Embodiment 6
Pressing 1: 2 molar ratio with purity 99.5%, granularity 100 purpose magnesium powder and purity are 99.99%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 16mm internal diameter 11mm iron pipe, after compressing, tamping, shut the iron pipe two ends, iron pipe is through the swaging of 27 passages, drawing, control every time deflection in 2%～40% scope, obtain fine rule, process to such an extent that be filled with the iron-based 4 * 0.5mm of magnesium powder and boron powder to the center through rolling again
2Faciola, two ends connect lead-in wire and place silica tube, and quartzy cap on two end caps is taken out silica tube to vacuum tightness＜1Pa with vacuum pump, feeds N then
2Gas is regulated electric power outputting current 70A, and controlling flow is through the current value size of sample, make 150 ℃ of sample heat-up rates/min to 850 ℃ after, insulation 30min, control current is chilled to room temperature with the cooling of 100 ℃/min speed then, closes N
2Gas takes out sample, gets iron-based magnesium diboride superconducting tape.
Embodiment 7
Pressing 1: 2 molar ratio with purity 99.5%, granularity 100 purpose magnesium powder and purity are 97%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 16mm internal diameter 10mm iron pipe, after compressing, tamping, shut the iron pipe two ends, iron pipe is through the swaging of 20 passages, drawing, control every time deflection in 5%～50% scope, obtain fine rule, must arrive iron-based 4 * 0.5mm that the center is filled with magnesium powder and boron powder through rolling again
2Faciola, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 60A, controlling flow is through the current value size of sample, after making 100 ℃ of sample heat-up rates/min to 900 ℃, insulation 10min, control current then, be chilled to room temperature with the cooling of 50 ℃/min speed, close Ar gas, take out sample, get iron-based magnesium diboride superconducting tape.
Embodiment 8
Pressing 1: 2 molar ratio with purity 99.5%, granularity 100 purpose magnesium powder and purity are 99.99%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 14mm internal diameter 10mm iron pipe, after compressing, tamping, shut the iron pipe two ends, iron pipe through 35 passages swage, drawing, control every time deflection in 1%～16% scope, obtain fine rule, must arrive iron-based 4 * 0.5mm that the center is filled with magnesium powder and boron powder through rolling again
2Faciola, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 90A, controlling flow is through the current value size of sample, after making 500 ℃ of sample heat-up rates/min to 600 ℃, insulation 10min, control current then, be chilled to room temperature with the cooling of 200 ℃/min speed, close Ar gas, take out sample, get iron-based magnesium diboride superconducting tape.
Embodiment 9
By 1: 2 molar ratio with purity 99.5%, granularity 120 purpose magnesium powder and purity are 95%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 16mm internal diameter 11mm iron pipe, after compressing, tamping, shut the iron pipe two ends.Iron pipe is swaged through 22 passages, drawing, control every time deflection in 4%～30% scope, process to such an extent that be filled with the iron-based Φ 2.05mm fine rule of magnesium powder and boron powder to the center, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 100A, controlling flow is through the current value size of sample, after making 100 ℃ of sample heat-up rates/min to 750 ℃, insulation 45min, control current then, be chilled to room temperature with the cooling of 30 ℃/min speed, close Ar gas, take out sample, get the iron base MgB 2 superconductor wire material.
Embodiment 10
Pressing 1: 2 molar ratio with purity 99.5%, granularity 200 purpose magnesium powder and purity are 99.0%, granularity 100 purpose boron powder mix, behind the ball milling, insert in the external diameter 12mm internal diameter 9mm iron pipe, after compressing, tamping, shut the iron pipe two ends, iron pipe is through the swaging of 32 passages, drawing, control every time deflection in 1%～16% scope, obtain fine rule, process to such an extent that be filled with the iron-based 3.1 * 0.4mm of magnesium powder and boron powder to the center through rolling again
2Faciola, two ends connect lead-in wire and place silica tube, quartzy cap on two end caps, take out silica tube to vacuum tightness＜1Pa with vacuum pump, feed Ar gas then, regulate electric power outputting current 45A, controlling flow is through the current value size of sample, after making 80 ℃ of sample heat-up rates/min to 800 ℃, insulation 30min, control current then, be chilled to room temperature with the cooling of 45 ℃/min speed, close Ar gas, take out sample, get the iron base MgB 2 superconductor wire material.
Claims (2)
1, a kind of heat treating method of iron base MgB 2 superconductor wire and belt is characterized in that its processing step is as follows successively:
(1) with purity 99.5%, granularity is that 100～200 purpose magnesium powder and purity are 92%～99.99%, and granularity is 100 purpose boron powder, mixes by magnesium diboride theoretical chemistry metered proportions, and ball milling is 1 hour then;
(2) magnesium powder behind the ball milling and boron powder are inserted in the iron pipe, compress tamp the blended powder after, sealing iron pipe two ends;
(3) iron pipe is carried out 20～40 passages are swaged, the cold mechanical workout of drawing, control every time deflection in 1%～50% scope, the iron-based fine rule that the center of must arriving is filled with magnesium powder and boron powder passes through the flat rolling operation then, obtains iron-based faciola material; More than the stranded back cold working of two iron-based fine rule, can obtain the multicore material;
(4) line sample or carry sample two ends are connected lead-in wire and place silica tube, take out quartzy intraductal pressure＜1Pa, feed Ar gas then;
(5) regulate output power of power supply, controlling flow is through the current value size of sample, the test sample temperature, behind control sample heat-up rate 45 ℃/min～900 ℃/min to 600～900 ℃, insulation 10min～60min controls power supply output then, be chilled to room temperature with 30 ℃/min～300 ℃/min speed cooling, close Ar gas, take out sample, get iron base MgB 2 superconductor wire and belt.
2, the heat treating method of MgB 2 superconductor wire and belt according to claim 1, the atmosphere when it is characterized in that thermal treatment are vacuum condition or oxygen-free inert atmosphere conditions.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2006100122150A CN1865457A (en) | 2006-06-13 | 2006-06-13 | Heat treatment method for iron base MgB2 superconductor wire and belt |
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| CNA2006100122150A CN1865457A (en) | 2006-06-13 | 2006-06-13 | Heat treatment method for iron base MgB2 superconductor wire and belt |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100587859C (en) * | 2007-08-30 | 2010-02-03 | 中国科学院电工研究所 | Preparation method for Fe/Cu wrapping structure magnesium diboride multiple core superconductive wire |
| CN101888026A (en) * | 2010-06-30 | 2010-11-17 | 中国科学院电工研究所 | Bronze process Nb3Sn superconductor multi-core wire connector and preparation method thereof |
| CN101291021B (en) * | 2007-11-16 | 2011-04-20 | 中国科学院电工研究所 | Connecting method of MgB* superconduction in strip shape |
| CN101707089B (en) * | 2009-12-15 | 2011-08-10 | 中国科学院电工研究所 | Method for improving upper critical field and critical current density of iron-based superconductor |
| CN102280198A (en) * | 2011-08-17 | 2011-12-14 | 西北有色金属研究院 | Preparation method for multi-core MgB2 superconducting wire/band |
| CN102498528A (en) * | 2009-06-05 | 2012-06-13 | 独立行政法人物质·材料研究机构 | Iron-based superconducting wire and manufacturing method therefor |
| CN102593686A (en) * | 2010-06-30 | 2012-07-18 | 中国科学院电工研究所 | Nb3Sn superconductor multi-core cable joint adopting bronze process and preparation method of Nb3Sn superconductor multi-core cable joint |
| CN101271747B (en) * | 2008-05-07 | 2013-05-01 | 中国科学院电工研究所 | Iron based compounds superconducting wire, belt material and method for producing the same |
| CN108565064A (en) * | 2017-12-30 | 2018-09-21 | 西北有色金属研究院 | A kind of MgB2The quick heat treatment method of superconducting wire |
| CN113035443A (en) * | 2021-03-02 | 2021-06-25 | 中国科学院电工研究所 | Preparation method of iron-based superconducting wire |
| CN113484127A (en) * | 2021-06-18 | 2021-10-08 | 合肥原位科技有限公司 | Instantaneous ultra-high temperature vacuum platform device |
-
2006
- 2006-06-13 CN CNA2006100122150A patent/CN1865457A/en active Pending
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100587859C (en) * | 2007-08-30 | 2010-02-03 | 中国科学院电工研究所 | Preparation method for Fe/Cu wrapping structure magnesium diboride multiple core superconductive wire |
| CN101291021B (en) * | 2007-11-16 | 2011-04-20 | 中国科学院电工研究所 | Connecting method of MgB* superconduction in strip shape |
| CN101271747B (en) * | 2008-05-07 | 2013-05-01 | 中国科学院电工研究所 | Iron based compounds superconducting wire, belt material and method for producing the same |
| CN102498528A (en) * | 2009-06-05 | 2012-06-13 | 独立行政法人物质·材料研究机构 | Iron-based superconducting wire and manufacturing method therefor |
| CN102498528B (en) * | 2009-06-05 | 2014-04-16 | 独立行政法人物质·材料研究机构 | Iron-based superconducting wire and manufacturing method therefor |
| CN101707089B (en) * | 2009-12-15 | 2011-08-10 | 中国科学院电工研究所 | Method for improving upper critical field and critical current density of iron-based superconductor |
| CN101888026B (en) * | 2010-06-30 | 2012-07-18 | 中国科学院电工研究所 | Bronze process Nb3Sn superconductor multi-core wire connector |
| CN102593686A (en) * | 2010-06-30 | 2012-07-18 | 中国科学院电工研究所 | Nb3Sn superconductor multi-core cable joint adopting bronze process and preparation method of Nb3Sn superconductor multi-core cable joint |
| CN102593686B (en) * | 2010-06-30 | 2013-09-18 | 中国科学院电工研究所 | Nb3Sn superconductor multi-core cable joint adopting bronze process and preparation method of Nb3Sn superconductor multi-core cable joint |
| CN101888026A (en) * | 2010-06-30 | 2010-11-17 | 中国科学院电工研究所 | Bronze process Nb3Sn superconductor multi-core wire connector and preparation method thereof |
| CN102280198B (en) * | 2011-08-17 | 2012-07-04 | 西北有色金属研究院 | Preparation method for multi-core MgB2 superconducting wire/band |
| CN102280198A (en) * | 2011-08-17 | 2011-12-14 | 西北有色金属研究院 | Preparation method for multi-core MgB2 superconducting wire/band |
| CN108565064A (en) * | 2017-12-30 | 2018-09-21 | 西北有色金属研究院 | A kind of MgB2The quick heat treatment method of superconducting wire |
| CN113035443A (en) * | 2021-03-02 | 2021-06-25 | 中国科学院电工研究所 | Preparation method of iron-based superconducting wire |
| CN113484127A (en) * | 2021-06-18 | 2021-10-08 | 合肥原位科技有限公司 | Instantaneous ultra-high temperature vacuum platform device |
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