CN100345224C - Method for preparing original autogeny MgB2 superconductive material under pulsed magnetic field action - Google Patents

Method for preparing original autogeny MgB2 superconductive material under pulsed magnetic field action Download PDF

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CN100345224C
CN100345224C CNB2005100282386A CN200510028238A CN100345224C CN 100345224 C CN100345224 C CN 100345224C CN B2005100282386 A CNB2005100282386 A CN B2005100282386A CN 200510028238 A CN200510028238 A CN 200510028238A CN 100345224 C CN100345224 C CN 100345224C
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powder
magnetic field
mgb
superconductor
present
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CN1731537A (en
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李瑛�
朱明原
李文献
金红明
任钟鸣
李喜
窦士学
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University of Shanghai for Science and Technology
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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 method for preparing in-situ synthesized MgB2 superconducting materials under the action of pulse magnetic fields, which belongs to the technical field of preparing technology for low temperature superconducting materials. In the method of the present invention, high purity Mg powder and B powder are used as raw materials, the Mg powder and the B powder are mixed according to a stated stoichiometric ratio (Mg: B=0.7: 2.0 to 1.3: 2.0), the pulse magnetic fields whose operating frequency is from 0.03 to 0.1 Hertz and intensity is from 1 to 100 T (Tesla) are used on the basis of a sleeve method, and the in-situ synthesized reaction temperature of the Mg powder and B powder is in the range of 600 to 1000 DEG C. The method of the present invention can prepare the low temperature superconducting materials which have the advantages of small crystal particle, consistent crystal direction arrangement, large crystal boundary area, few impurities among crystal boundaries, compact structure and high superconductivity critical current density.

Description

In-situ authigenic MgB under the pulsed magnetic field action 2The preparation method of superconductor
Technical field
The present invention relates to a kind of under pulsed magnetic field action in-situ authigenic MgB 2The preparation method of superconductor belongs to low temperature superconducting material fabricating technology field.
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.
Find by literature search, Chinese patent application number is 88106462.9, patent name is a report in " method and the device therefor of making superconductivity ceramics in magnetic field ", when heating prepares superconducting thin film, the C axis of perovskite sample crystalline texture adds a direct current magnetic field on film after the improvement of this film, crystalline texture is arranged in a straight line in one direction, can makes superconducting thin film with respect to the critical current density of the electric current that flows through the C plane and increase to 1 * 10 4Peace/square centimeter.If when adding magnetic field crystalline texture is heated to 300～1000 ℃, then critical current density can also further increase.
Summary of the invention
The purpose of this invention is to provide a kind of in-situ authigenic MgB that under pulsed magnetic field action, prepares 2The process of superconductor.Another object of the present invention provides superconductor a kind of grain refinement, that orientation is consistent.
The present invention relates to a kind of MgB 2The preparation method of superconductor is characterized in that having following technical process and step:
A, high-purity Mg powder and high-purity B powder are placed respectively in the vacuum drying chamber 120 ℃ of following freeze-day with constant temperature 24 hours, take by weighing Mg and B powder subsequently respectively, mol ratio is in accordance with regulations prepared burden, and both mol ratios are: Mg: B=0.7: 2.0～1.3: 2.0; After batch evenly ground, it is enclosed in the low carbon steel pipe of end sealing, and under certain pressure, after the compacting other end is sealed;
B, the low carbon steel pipe of 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;
C, above-mentioned heating tube is placed heating in the tube furnace, starting impulse magnetic field simultaneously, its pulse frequency is 0.03～0.1 hertz, magnetic field intensity is 1～100T (tesla); Programming rate is 3～30 ℃/minute; Be warming up to after 600～1000 ℃ of the reaction temperatures insulation 30 minutes; Then sample is cooled off with stove, take out sample MgB 2, be a kind of MgB of in-situ authigenic 2Superconductor.
The present invention adopts the conventional pulsed magnetic generator that uses, and can obtain under pulsed magnetic field action was spontaneous MgB originally 2The MgB that superconductor, the inventive method make 2Have the crystal grain of refinement, bigger grain boundary area, its grain orientation unanimity and be not mingled with other compound, its purity is very high.
In addition, compare, because MgB with other process 2Grain refinement produced more crystal boundary, strengthened the pinning effect of crystal boundary, finally make total flux pinning force be improved, thereby improved critical current density.
Concrete execution mode:
Now embodiments of the invention are summarized as follows:
Embodiment 1
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 diameter is in 10 millimeters the low carbon steel pipe of end sealing, and after compacting under the 10MPa pressure other end is sealed;
(2), the low carbon steel pipe 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, start the conventional pulsed magnetic generator that uses simultaneously, produce pulsed magnetic field, its pulse frequency is 0.03 hertz, and magnetic field intensity is 5T (tesla); Programming rate is 3 ℃/minute; Be warming up to after 800 ℃ of the reaction temperatures insulation 30 minutes; Then sample is cooled off with stove, take out sample MgB 2, be a kind of MgB of in-situ authigenic 2Superconductor
Embodiment 2
Preparation process in the present embodiment and the foregoing description 1 are identical.1., adopt the stoichiometric proportion of Mg and B to be different is:: Mg: B=0.7: 2; 2., the magnetic field intensity that adopts is 1T (tesla), its pulse frequency is 0.04 hertz; 3., being warming up to reaction temperature is 650 ℃.Finally make MgB 2Superconductor.
Embodiment 3
Preparation process in the present embodiment and the foregoing description 1 are identical.1., adopt the stoichiometric proportion of Mg and B to be different is:: Mg: B=0.85: 2; 2., the magnetic field intensity that adopts is 3T (tesla), its pulse frequency is 0.07 hertz; 3., being warming up to reaction temperature is 700 ℃.Finally make MgB 2Superconductor.
Embodiment 4
Preparation process in the present embodiment and the foregoing description 1 are identical.1., adopt the stoichiometric proportion of Mg and B to be different is:: Mg: B=1.15: 2; 2., the magnetic field intensity that adopts is 10T (tesla), its pulse frequency is 0.05 hertz; 3., being warming up to reaction temperature is 900 ℃.Finally make MgB 2Superconductor.
Embodiment 5
Preparation process in the present embodiment and the foregoing description 1 are identical.1., adopt the stoichiometric proportion of Mg and B to be different is:: Mg: B=1.2: 2; 2., the magnetic field intensity that adopts is 20T (tesla), its pulse frequency is 0.06 hertz; 3., being warming up to reaction temperature is 700 ℃.Finally make MgB 2Superconductor.
Embodiment 6
Preparation process in the present embodiment and the foregoing description 1 are identical.1., adopt the stoichiometric proportion of Mg and B to be different is:: Mg: B=1.3: 2; 2., the magnetic field intensity that adopts is 50T (tesla), its pulse frequency is 0.07 hertz; 3., being warming up to reaction temperature is 800 ℃.Finally make MgB 2Superconductor.
Embodiment 7
Preparation process in the present embodiment and the foregoing description 1 are identical.1., adopt the stoichiometric proportion of Mg and B to be different is:: Mg: B=1: 2.2; 2., the magnetic field intensity that adopts is 80T (tesla), its pulse frequency is 0.08 hertz; 3., being warming up to reaction temperature is 900 ℃.Finally make MgB 2Superconductor.
Embodiment 8
Preparation process in the present embodiment and the foregoing description 1 are identical.1., adopt the stoichiometric proportion of Mg and B to be different is:: Mg: B=1: 2.4; 2., the magnetic field intensity that adopts is 100T (tesla), its pulse frequency is 0.1 hertz; 3., being warming up to reaction temperature is 900 ℃.Finally make MgB 2Superconductor.

Claims (1)

1. in-situ authigenic MgB 2The preparation method of superconductor is characterized in that having following technical process and step:
A, highly purified Mg powder and highly purified B powder are placed respectively in the vacuum drying chamber 120 ℃ of following freeze-day with constant temperature 24 hours, take by weighing Mg and B powder subsequently respectively, stoichiometric proportion is in accordance with regulations prepared burden, both mol ratios are: Mg: B=0.7: 2.0～1.3: 2.0, after batch evenly ground, enclose in the low carbon steel pipe of end sealing, and under certain pressure, after the compacting other end is sealed;
B, the low carbon steel pipe of the above-mentioned Mg of being contained with powder, B 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;
C, above-mentioned heating tube is placed heating in the tube furnace, starting impulse magnetic field simultaneously, its pulse frequency is 0.03～0.10 hertz, magnetic field intensity is 1～100T; Programming rate is 3～30 ℃/minute; Be warming up to after 600～1000 ℃ of the reaction temperatures insulation 30 minutes; Then sample is cooled off with stove, take out sample MgB 2, be a kind of MgB of in-situ authigenic 2Superconductor.
CNB2005100282386A 2005-07-28 2005-07-28 Method for preparing original autogeny MgB2 superconductive material under pulsed magnetic field action Expired - Fee Related CN100345224C (en)

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Publication number Priority date Publication date Assignee Title
CN1915626B (en) * 2006-09-01 2010-11-10 浙江大学 Method for preparing gradient material of strong magnetism and weak magnetism through flow casting molding in pulse magnetism
CN1911619B (en) * 2006-09-01 2010-07-28 浙江大学 Preparation method of strong magnetic-weak magnetic gradient material gel injection mould in pulse magnetic field
CN1915625B (en) * 2006-09-01 2010-12-08 浙江大学 Method for preparing gradient material of strong magnetism and weak magnetism through pressure filtration molding in pulse magnetism
CN102303353B (en) * 2011-06-29 2014-01-29 浙江大学 Gel-casting preparation method for gradient material in moving magnetic field

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1329370A (en) * 2001-07-16 2002-01-02 西北有色金属研究院 MgB2 superconducting material and its preparation method
JP2003089516A (en) * 2001-09-14 2003-03-28 Internatl Superconductivity Technology Center MgB2 SUPERCONDUCTOR AND METHOD FOR PRODUCING THE SAME
CN1439601A (en) * 2002-12-09 2003-09-03 甘肃工业大学 Manufacture of MgB2 superconductive blanks
JP2003331670A (en) * 2002-05-16 2003-11-21 National Institute For Materials Science CREATING METHOD FOR MgB2 SUPERCONDUCTING WIRE
CN1560314A (en) * 2004-03-10 2005-01-05 上海大学 Technology method for fining aluminium crystal particle of use in industry
CN1569633A (en) * 2004-04-27 2005-01-26 上海大学 Method for preparing MgB2 superconductive material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1329370A (en) * 2001-07-16 2002-01-02 西北有色金属研究院 MgB2 superconducting material and its preparation method
JP2003089516A (en) * 2001-09-14 2003-03-28 Internatl Superconductivity Technology Center MgB2 SUPERCONDUCTOR AND METHOD FOR PRODUCING THE SAME
JP2003331670A (en) * 2002-05-16 2003-11-21 National Institute For Materials Science CREATING METHOD FOR MgB2 SUPERCONDUCTING WIRE
CN1439601A (en) * 2002-12-09 2003-09-03 甘肃工业大学 Manufacture of MgB2 superconductive blanks
CN1560314A (en) * 2004-03-10 2005-01-05 上海大学 Technology method for fining aluminium crystal particle of use in industry
CN1569633A (en) * 2004-04-27 2005-01-26 上海大学 Method for preparing MgB2 superconductive material

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