CN100376010C - Preparation method of high density MgB2 superconduction wire material - Google Patents
Preparation method of high density MgB2 superconduction wire material Download PDFInfo
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- CN100376010C CN100376010C CNB200510111917XA CN200510111917A CN100376010C CN 100376010 C CN100376010 C CN 100376010C CN B200510111917X A CNB200510111917X A CN B200510111917XA CN 200510111917 A CN200510111917 A CN 200510111917A CN 100376010 C CN100376010 C CN 100376010C
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- mgb
- mgb2
- heating tube
- superconducting wire
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
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Abstract
The present invention relates to a high density MgB2 superconducting wire and a preparation method thereof, which comprises the steps that after Mg powder and B powder are ground, the Mg powder and the B powder are sealed into Ta foil, the Ta foil is placed in a heating tube, the temperature is raised to 650 to 950 DEG C in an inert atmosphere to carry out heat preservation for 0.5 to ten hours, and first sintering work is carried out to manufacture MgB2 superconducting materials; the MgB2 superconducting materials are ground into MgB2 powder, the granularity of which is from two mu m to three mu m, the MgB2 powder, the Mg powder and the B powder are mixed to carry out second sintering work, and the high density MgB2 superconducting wire is obtained. The MgB2 superconducting wire manufactured by the method of the present invention has the advantages of fine crystal particle, larger crystal boundary area, ideal crystal boundary connection, no microcrack, no doping of other compounds and high purity.
Description
Technical field
The present invention relates to a kind of MgB
2The preparation method of superconductor, particularly a kind of high density MgB
2The preparation method of superconducting wire.
Background technology
Calendar year 2001, find intermetallic compound Mg B
2Result with superconductivity has caused the very big sensation of Condensed Matter Physics educational circles, material educational circles.Because its many special performances are not familiar with fully and are understood by people as yet, have caused common attention at a plurality of ambits such as material, physics, chemistry.MgB
2The critical inversion temperature of superconduction be 39K, its superconducting temperature is only second to oxide superconductor, doping C
60The solid material superconductor is high, simple, the most stable intermetallic compound superconductor of finding up to now of superconducting temperature.MgB
2Structure be class graphite sandwich, its chemical composition and crystal structure are all very simple, and high-critical temperature (T is arranged
c), high current density (J
c), high coherence length, and have characteristics such as easily synthetic, easily processing, lighter weight, easily make film or wire rod, be expected to become the superconductor of fairly large application.
Yet, at MgB
2Especially in the preparation process of bulk, wire rod and band, because Mg and B are the less raw materials of density, the density of Mg is 1.74g/cm to superconductor
3, the density of B is 2.34g/cm
3Even, reach 100% packing through compacting, in the sintering process its volume can narrow down to original 76%, the MgB that obtains
2Sample in have a large amount of shrinkage cavities, density is well below its theoretical value 2.62g/cm
3Moreover compacting can not reach 100%, so generally have to 1.1～1.5g/cm behind the sintering
3Open structure, be to limit the main cause that this material critical current density improves, simultaneously to MgB
2Carrying out basic research, performance test and production and processing etc. all has a significant impact.
Record can prepare highdensity MgB with the method for high temperature insostatic pressing (HIP) in the document
2Bulk (Nesterenko V F, Gu Y.Elastic properties of hot-isostatically-pressed magnesium diboride.Appllied physics letters.2003,82 (23): 4104-4106), but its apparatus and process complexity, and can only be used for the bulk preparation, can not be used for the preparation of wire rod and band.Also put down in writing in the document and can directly use MgB
2The highdensity MgB of powder pressing forming
2Material (Frederick N A, Li S, Maple M B, et al.Improvedsuperconducting properties of MgB
2.Physica C, 2001,363:1-5.), but because made MgB
2There is a large amount of micro-cracks in the material the inside, and the superconduction current capacity also is restricted.
Summary of the invention
The object of the present invention is to provide a kind of high density MgB
2The preparation method of superconducting wire.
For achieving the above object, the present invention adopts following technical scheme:
A kind of high density MgB
2The preparation method of superconducting wire is characterized in that this method may further comprise the steps:
A) Mg powder and the B powder that will cross through vacuum drying treatment in the amount of substance ratio is: the ratio of Mg: B=0.7～1.3: 2 is prepared burden, and after batching is evenly ground, encloses the tantalum paper tinsel;
B) above-mentioned tantalum paper tinsel is positioned in the heating tube, and under inert atmosphere, heating tube is heated, be warming up to 650～950 ℃, be incubated 0.5～10 hour; Then sample is cooled off with stove, promptly make MgB
2Superconductor;
C) with above-mentioned MgB
2Superconductor grinds to form the MgB that granularity is 2～3 μ m after taking out from the tantalum paper tinsel
2Powder; Then at MgB
2The mixture that adds Mg powder and B powder in the powder, the mixture and the MgB of Mg powder and B powder
2The mass ratio of powder is 0.01～0.2: 1, and the amount of substance ratio of Mg powder and B powder is 0.7～1.3: 2 in the mixture of described Mg powder and B powder;
A) after the compound that step c is obtained evenly grinds, make prefabricated component; Then above-mentioned prefabricated component is positioned in the heating tube, and under inert atmosphere, heating tube is heated, be incubated 0.5～10 hour after being warming up to 650～950 ℃; With the stove cooling, promptly obtain highdensity MgB then
2Superconducting wire.
Compared with prior art, the inventive method has following outstanding substantive distinguishing features and remarkable advantage: because the inventive method has adopted mixed sintering technology, be that a kind of simple preparation does not have gross imperfection, high density MgB 1.
2Superconducting wire technology; 2. because MgB
2The raising of density, carrier concentration is improved, thereby has improved critical current density.3. because MgB
2The raising of density has produced more crystal boundary, and crystal boundary connects closely, has strengthened the pinning effect of crystal boundary, finally makes total flux pinning force be improved, thereby has improved critical current density.Thus, the MgB that makes of the inventive method
2Superconducting wire has the crystal grain of refinement, bigger grain boundary area, desirable crystal boundary connection, does not have micro-crack, and is not mingled with other compound, and purity is very high.
Concrete execution mode:
Embodiment one:
The MgB of present embodiment
2The preparation process of superconductor is as follows:
(1) be that Mg powder 99%, that cross 325 mesh sieves and purity are that 99% B powder places respectively in the vacuum drying chamber in 120 ℃ of following freeze-day with constant temperature 24 hours with purity, take by weighing Mg and B powder subsequently respectively, by stoichiometric proportion Mg: B=1: 2 prepare burden, after batch evenly ground, it is enclosed the tantalum paper tinsel;
(2) the tantalum paper tinsel with the above-mentioned Mg of being contained with, B compound is positioned in the heating tube, with diffusion vacuum pump the air in the heating tube is taken out and to be made into vacuum, charge into high-purity argon gas subsequently and carry out gas washing, vacuumize again, so repeatedly after three times, continue slowly to charge into high-purity argon gas and guarantee inert atmosphere in the pipe;
(3) above-mentioned heating tube is placed heating in the tube furnace, programming rate is 100 ℃/h; Be warming up to after 650 ℃ of the reaction temperatures insulation 1 hour; Then sample is cooled off with stove, take out sample, being a kind of was spontaneous MgB originally
2Superconductor;
(4) with the MgB of above-mentioned in-situ authigenic
2Superconduction block material grinds with ball mill after taking out from the tantalum paper tinsel, obtains the MgB that granularity is 2～3 μ m
2Powder;
(5) above-mentioned powder being carried out accurate weighing, obtain one group of powder, will be Mg: B=1 in stoichiometric proportion then: the ratio of 2 Mg powder and the addition of B powder and once sintered sample powder is that 0.01: 1 weight ratio adds wherein.
(6) above-mentioned compound is evenly ground respectively after, the low carbon steel pipe pipe of packing into, again through swaging, wire drawing, moulding, make the wire rod prefabricated component.
(7) with above-mentioned Mg powder, B powder and the MgB of being contained with
2The prefabricated component of powder compound is positioned in the heating tube, with diffusion vacuum pump the air in the heating tube is taken out and to be made into vacuum, charge into high-purity argon gas subsequently and carry out gas washing, vacuumize again, so repeatedly after three times, continue slowly to charge into high-purity argon gas and guarantee inert atmosphere in the pipe;
(8) above-mentioned heating tube is placed heating in the tube furnace, programming rate is 100 ℃/h; Be warming up to after 650 ℃ of the reaction temperatures insulation 1 hour; Then sample is cooled off with stove, take out sample MgB
2, be a kind of highdensity MgB
2Superconducting wire.
Embodiment two: the preparation process in the present embodiment and the foregoing description one are identical.Different is: 1. Mg powder and B powder are by Mg: B=0.7: 2 take by weighing batching; 2. the MgB that ball milling is obtained
2Be Mg: B=0.7 by stoichiometric proportion: when 2 Mg powder and B powder mixed, the addition of Mg powder and B powder and the ratio of once sintered sample powder were 0.02: 1; 3. the reaction temperature of material all is controlled at 750 ℃, and temperature retention time all is 0.5 hour.
Embodiment three: the preparation process in the present embodiment and the foregoing description one are identical.Different is: 1. Mg powder and B powder are by Mg: B=0.8: 2 take by weighing batching; 2. the MgB that ball milling is obtained
2Be Mg: B=0.8 by stoichiometric proportion: when 2 Mg powder and B powder mixed, the addition of Mg powder and B powder and the ratio of once sintered sample powder were 0.05: 1; 3. the reaction temperature of material all is controlled at 800 ℃, and temperature retention time all is 2 hours.
Embodiment four: the preparation process in the present embodiment and the foregoing description one are identical.Different is: 1. Mg powder and B powder are by Mg: B=1.1: 2 take by weighing batching; 2. the MgB that ball milling is obtained
2Be Mg: B=1.1 by stoichiometric proportion: when 2 Mg powder and B powder mixed, the addition of Mg powder and B powder and the ratio of once sintered sample powder were 0.1: 1; 3. the reaction temperature of material all is controlled at 850 ℃, and temperature retention time all is 5 hours.
Embodiment five: the preparation process in the present embodiment and the foregoing description one are identical.Different is: 1. Mg powder and B powder are by Mg: B=1.2: 2 take by weighing batching; 2. the MgB that ball milling is obtained
2Be Mg: B=1.2 by stoichiometric proportion: when 2 Mg powder and B powder mixed, the total weight of Mg powder and B powder was 15%; 3. the reaction temperature of material all is controlled at 900 ℃, and temperature retention time all is 8 hours.
Embodiment six: the preparation process in the present embodiment and the foregoing description one are identical.Different is: 1. Mg powder and B powder are by Mg: B=1.3: 2 take by weighing batching; 2. the MgB that ball milling is obtained
2Be Mg: B=1.3 by stoichiometric proportion: when 2 Mg powder and B powder mixed, the addition of Mg powder and B powder and the ratio of once sintered sample powder were 0.2: 1; 3. the reaction temperature of material all is controlled at 950 ℃, and temperature retention time all is 10 hours.
Embodiment seven: the preparation process in the present embodiment and the foregoing description one are identical.Different is: 1. Mg powder and B powder are by Mg: B=1.3: 2 take by weighing batching; 2. with the MgB once sintered, that ball milling obtains
2Powder carries out according to step 6; 3. once sintered reaction temperature is 800 ℃, and temperature retention time is 2 hours, and the temperature of double sintering is 900 ℃, and temperature retention time is 1 hour.
Claims (1)
1. high density MgB
2The preparation method of superconducting wire is characterized in that this method may further comprise the steps:
A, Mg powder and the B powder that will cross through vacuum drying treatment in the amount of substance ratio are: the ratio of Mg: B=0.7～1.3: 2 is prepared burden, and after batching is evenly ground, encloses the tantalum paper tinsel;
B, above-mentioned tantalum paper tinsel is positioned in the heating tube, and under inert atmosphere, heating tube is heated, be warming up to 650～950 ℃, be incubated 0.5～10 hour; Then sample is cooled off with stove, promptly make MgB
2Superconductor;
C, with above-mentioned MgB
2Superconductor grinds to form the MgB that granularity is 2～3 μ m after taking out from the tantalum paper tinsel
2Powder; Then at MgB
2The mixture that adds Mg powder and B powder in the powder, the mixture and the MgB of Mg powder and B powder
2The mass ratio of powder is 0.01～0.2: 1, and the amount of substance ratio of Mg powder and B powder is 0.7～1.3: 2 in the mixture of described Mg powder and B powder;
After d, the compound that step c is obtained evenly grind, make prefabricated component; Then above-mentioned prefabricated component is positioned in the heating tube, and under inert atmosphere, heating tube is heated, be incubated 0.5～10 hour after being warming up to 650～950 ℃; With the stove cooling, promptly obtain highdensity MgB then
2Superconducting wire.
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|---|---|---|---|
| CNB200510111917XA CN100376010C (en) | 2005-12-23 | 2005-12-23 | Preparation method of high density MgB2 superconduction wire material |
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| CNB200510111917XA CN100376010C (en) | 2005-12-23 | 2005-12-23 | Preparation method of high density MgB2 superconduction wire material |
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| CN100376010C true CN100376010C (en) | 2008-03-19 |
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| CN100442398C (en) * | 2006-08-15 | 2008-12-10 | 北京工业大学 | Method for preparing MgB2 single core supper conducting wire material using continuous pipeline forming and filling technique |
Citations (6)
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|---|---|---|---|---|
| JP2003095650A (en) * | 2001-06-01 | 2003-04-03 | Internatl Superconductivity Technology Center | MgB2-BASED SUPERCONDUCTOR HAVING HIGH CRITICAL CURRENT DENSITY AND METHOD FOR MANUFACTURING THE SAME |
| CN1439601A (en) * | 2002-12-09 | 2003-09-03 | 甘肃工业大学 | Manufacture of MgB2 superconductive blanks |
| US20030207767A1 (en) * | 2001-06-01 | 2003-11-06 | Electronics And Telecommunications Research Institute. | Superconductor incorporating therein superconductivity epitaxial thin film and manufacturing method thereof |
| US20050159318A1 (en) * | 2002-05-10 | 2005-07-21 | Giovanni Giunchi | Method for the production of superconductive wires based on hollow filaments made of MgB2 |
| CN1683281A (en) * | 2004-04-14 | 2005-10-19 | 中国科学院电工研究所 | Process for preparing magnesium diboride superconductor |
| CN1794364A (en) * | 2005-12-23 | 2006-06-28 | 上海大学 | Preparation method of high density MgB2 superconduction band |
-
2005
- 2005-12-23 CN CNB200510111917XA patent/CN100376010C/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2003095650A (en) * | 2001-06-01 | 2003-04-03 | Internatl Superconductivity Technology Center | MgB2-BASED SUPERCONDUCTOR HAVING HIGH CRITICAL CURRENT DENSITY AND METHOD FOR MANUFACTURING THE SAME |
| US20030207767A1 (en) * | 2001-06-01 | 2003-11-06 | Electronics And Telecommunications Research Institute. | Superconductor incorporating therein superconductivity epitaxial thin film and manufacturing method thereof |
| US20050159318A1 (en) * | 2002-05-10 | 2005-07-21 | Giovanni Giunchi | Method for the production of superconductive wires based on hollow filaments made of MgB2 |
| CN1439601A (en) * | 2002-12-09 | 2003-09-03 | 甘肃工业大学 | Manufacture of MgB2 superconductive blanks |
| CN1683281A (en) * | 2004-04-14 | 2005-10-19 | 中国科学院电工研究所 | Process for preparing magnesium diboride superconductor |
| CN1794364A (en) * | 2005-12-23 | 2006-06-28 | 上海大学 | Preparation method of high density MgB2 superconduction band |
Non-Patent Citations (1)
| Title |
|---|
| 纳米镁粉对制备MgB_2超导样品的作用. 冯庆荣，陈晋平，徐军，王宇昊，陈鑫.低温物理学报，第26卷第1期. 2004 * |
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