CN100354986C - High critical current density MgB2-base super conductor and producing method thereof - Google Patents
High critical current density MgB2-base super conductor and producing method thereof Download PDFInfo
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- CN100354986C CN100354986C CNB2005101327261A CN200510132726A CN100354986C CN 100354986 C CN100354986 C CN 100354986C CN B2005101327261 A CNB2005101327261 A CN B2005101327261A CN 200510132726 A CN200510132726 A CN 200510132726A CN 100354986 C CN100354986 C CN 100354986C
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- mgb
- critical current
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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
- 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
Abstract
The present invention relates to a high critical current density MgB2 base superconductor and a preparation method thereof. The present invention is characterized in that carbon, zirconium and compounds thereof are dispersed in the MgB2 base superconductor. The preparation process comprises that firstly, dried magnesium powder, boron powder, zirconium powder and carbon powder are proportionally and fully mixed for one to two hours, the mixed powder is formed, then the formed mixed powder is placed in a vacuum annealing furnace, and is kept at the temperature of 740 DEG C to 760 DEG C for one to ten hours under the protection of pure argon or mixed gas of argon and hydrogen, finally, the formed mixed powder is cooled to room temperature, and thus, the high critical current density MgB2 base superconductor is manufactured. The carbon and the metal zirconium are used as auxiliary burning agents, and the carbon, the zirconium and the compounds thereof are dispersed in the MgB2 base superconductor which is finally obtained, thereby refining MgB2 crystal particles which are finally formed and effectively strengthening the connection of the MgB2 crystal particles. The method of the present invention has the advantage of low preparation cost, second phase particles are simultaneously introduced, and the flux pinning effect of the MgB2 base superconductor is effectively improved.
Description
Technical field
The present invention relates to a kind of high critical current densities MgB
2Base super conductor and preparation method thereof.
Background technology
Critical temperature is the magnesium diboride (MgB of 39K at the beginning of calendar year 2001
2) discovery of new superconductors caused the common concern of international academic community, because it has created the new record of intermetallic compound superconductor transition temperature, theoretical research and application study all had crucial learning value.Though MgB
2The critical temperature of superconductor only is 39K, but different with oxide high temperature superconductor, MgB
2Have foolproof chemical composition and crystal structure, the cost of material is very low, the electric current that the crystal boundary energy carrying is very high, and its intrinsic critical current density (Jc) is very high (to surpass 10
7A/cm
2).While MgB
2The coherence length and the oxide coherence length of perovskite structure want big, this just means MgB
2In be easier to introduce useful flux pinning center, improve superconductivity.MgB
2Can just realize using at liquid hydrogen warm area (20K-30K), and cryogenic superconductor can't be worked at this warm area, the liquid hydrogen warm area just can obtain need not complicated and expensive liquid helium easily by refrigeration machine.Comprehensive refrigeration cost and material cost, MgB
2Superconductor is at 20-30K, and low field condition is used the price advantage that has clearly down, especially in MRI magnet (work magnetic field 1-2T) manufacturing field.
But MgB
2The practical application of superconductor must solve a key issue, promptly improves MgB
2The flux pinning of superconductor.Pure MgB
2Irreversible the value of superconductor under 20K only is 4-5T, and main cause is MgB
2Lack effective pinning center in the superconductor, flux pinning a little less than, this just causes the MgB under High-Field
2(Jc) is lower for the critical current density of superconductor, has influenced MgB
2Superconductor is in high temperature (＞20K) under the High-Field (＞4T) practical application.Therefore improve MgB
2Superconductor magnetic flux pinning characteristic will promote MgB greatly
2The practicability of superconductor.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of preparation process simple and be suitable for having in large-scale production and the background magnetic field more than 3 teslas the MgB of high critical current densities
2Base super conductor and manufacture method thereof.
The objective of the invention is to be achieved through the following technical solutions.
A kind of high critical current densities MgB
2Base super conductor is characterized in that this superconductor is at MgB
2Distributing carbon, zirconium and compound thereof of disperse in the base super conductor, this superconductor atomic ratio consists of Mg: Zr: B: C=(1-x): x: (2-x): x, wherein 0.05≤x≤0.20.
A kind of high critical current densities MgB of the present invention
2Base super conductor is characterized in that this MgB
2Base super conductor is sheet or bulk.
A kind of high critical current densities MgB of the present invention
2Base super conductor is characterized in that this MgB
2Base super conductor is that cross sectional shape is round wire rod.
A kind of high critical current densities MgB
2The preparation method of base super conductor, it is characterized in that preparation process be at first with magnesium, boron, zirconium and the carbon dust of drying according to atomic ratio Mg: Zr: B: C=(1-x): the ratio of x: (2-x): x was fully mixed 1-2 hour, wherein 0.05≤x≤0.20; Mixed powder is exerted pressure to 20-80MPa suppresses in flakes or piece, place vacuum annealing furnace then, under room temperature, vacuumize, treat that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, sheet or bulk heating will make then greater than 60 ℃/minute heating rate, insulation is 1-10 hour under 740 ℃-760 ℃ temperature, at last be cooled to room temperature, make the MgB of high critical current densities with cooldown rate greater than 25 ℃/minute
2Substrate or bulk superconductor.
A kind of high critical current densities MgB of the present invention
2The preparation method of base super conductor is characterized in that preparation process is at first with magnesium, boron, zirconium and the carbon dust of drying, and according to atomic ratio Mg: Zr: B: C=(1-x): the ratio of x: (2-x): x was fully mixed 1-3 hour, wherein 0.05≤x≤0.20; With mixed powder pack into seamless low carbon steel pipe or niobium pipe, again this complex is packed into and be assembled into complex in the oxygen-free copper pipe, again complex is carried out room temperature cold working process, through swaging, the comprehensive use of groove rolling and three kinds of processing technologys of drawing is processed into wire rod, the final cross sectional shape of wire rod is round; The wire rod that is worked into final size and shape is placed vacuum annealing furnace, under room temperature, vacuumize, treat that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, with the heating rate that is not less than 60 ℃/minute wire rod is heated then, insulation is 1-10 hour under 740 ℃-760 ℃ temperature, at last with the cooldown rate that is not less than 25 ℃/minute wire rod is cooled to room temperature, making cross sectional shape is round MgB
2The base superconducting wire.
At the research of method of the present invention, the mixed-powder of finding to adopt magnesium and boron can't obtain to have the MgB of high critical current densities as sintered powder under High-Field in the conventional method that equals to prepare under the atmospheric pressure
2Superconductor.And if in the mixed-powder of magnesium and boron, add an amount of carbon and metal zirconium simultaneously as sintering agent, at the MgB that equals to prepare under the atmospheric pressure
2Distributing carbon, zirconium and compound thereof of disperse in the base super conductor, MgB
2Base super conductor shows the feature of high critical current densities.
Method of the present invention adopts carbon and metallic Z r as sintering agent, and after sintering process was finished, carbon, zirconium and compound disperse thereof were distributed in the MgB of final acquisition
2In the base super conductor, the MgB that is obtained
2Has high critical current density in the background magnetic field of base super conductor more than 3 teslas.Carbon, zirconium and compound disperse thereof are distributed in the MgB of final acquisition
2In the base super conductor, make the MgB of final formation
2Grain refinement, efficient hardening MgB
2Crystal grain connects.The present invention can realize MgB
2The second phase particle has been introduced in the low cost preparation of base superconductor simultaneously, has effectively improved MgB
2The flux pinning of base super conductor.
Specific embodiments
A kind of high critical current densities MgB
2Base super conductor is characterized in that this superconductor is at MgB
2Distributing carbon, zirconium and compound thereof of disperse in the base super conductor, this MgB
2The base atomic ratio consists of Mg: Zr: B: C=(1-x): x: (2-x): x, wherein 0.05≤x≤0.20.
Preparation process for (1) with magnesium, boron, zirconium and the carbon dust of drying according to atomic ratio Mg: Zr: B: C=(1-x): the ratio of x: (2-x): x was fully mixed 1-2 hour, wherein 0.05≤x≤0.20; (2) mixed powder is exerted pressure into 20-80MPa suppresses in flakes or piece, place vacuum annealing furnace then, under room temperature, vacuumize, treat that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, sheet or bulk heating will make then greater than 60 ℃/minute heating rate, insulation is 1-10 hour under 740 ℃-760 ℃ temperature, at last be cooled to room temperature, make the MgB of high critical current densities with cooldown rate greater than 25 ℃/minute
2Substrate or bulk superconductor.(4) or with mixed powder pack into seamless low carbon steel pipe or niobium pipe, again this complex is packed into and be assembled into complex in the oxygen-free copper pipe, again complex is carried out room temperature cold working process, through swaging, the comprehensive use of groove rolling and three kinds of processing technologys of drawing is processed into wire rod, the final cross sectional shape of wire rod is round; The wire rod that is worked into final size and shape is placed vacuum annealing furnace, under room temperature, vacuumize, treat that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, with the heating rate that is not less than 60 ℃/minute wire rod is heated then, insulation is 1-10 hour under 740 ℃-760 ℃ temperature, at last with the cooldown rate that is not less than 25 ℃/minute wire rod is cooled to room temperature, making cross sectional shape is round MgB
2The base superconducting wire.
Specify technical examples according to the invention below.
Example 1
With magnesium (99%), boron (99%), zirconium (99%) and carbon (99%) powder of drying according to atomic ratio Mg: Zr: B: C=0.95: 0.05: 1.95: 0.05 ratio was fully mixed 2 hours.Mixed powder is pressed into the piece of diameter 20mm with hydraulic press, and exerting pressure is to place vacuum annealing furnace then by 20MPa, vacuumizes under room temperature, treats that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, with the heating rate that is not less than 60 ℃/minute wire rod is heated then, insulation is 10 hours under 740 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates sheet or bulk are cooled to room temperature at last, just making superconducting transition temperature is 38.6K, and critical current density is 4.1 * 10
4A/cm
2(20K, MgB 4T)
2Base super conductor.
Example 2
With magnesium (99%), boron (99%), zirconium (99%) and carbon (99%) powder of drying according to atomic ratio Mg: Zr: B: C=0.9: 0.1: 1.9: 0.1 ratio was fully mixed 1 hour.Mixed powder is pressed into the sheet of diameter 20mm with hydraulic press, and exerting pressure is to place vacuum annealing furnace then by 80MPa, vacuumizes under room temperature, treats that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, then to be not less than 60 ℃/minute heating rate with the heating of sheet or bulk, insulation is 1 hour under 760 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates wire rod is cooled to room temperature at last, just making superconducting transition temperature is 37.2K, and critical current density is 5.2 * 10
4A/cm
2(20K, MgB 4T)
2Base super conductor.
Example 3
With magnesium (99%), boron (99%), zirconium (99%) and carbon (99%) powder of drying according to atomic ratio Mg: Zr: B: C=0.8: 0.2: 1.8: 0.2 ratio was fully mixed 1.5 hours.Mixed powder is pressed into the sheet of diameter 20mm with hydraulic press, and exerting pressure is to place vacuum annealing furnace then by 60MPa, vacuumizes under room temperature, treats that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, with the heating rate that is not less than 60 ℃/minute wire rod is heated then, insulation is 6 hours under 750 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates sheet or bulk are cooled to room temperature at last, just making superconducting transition temperature is 35.3K, and critical current density is 2.0 * 10
4A/cm
2(20K, MgB 4T)
2Base super conductor.
Example 4
With magnesium (99%), boron (99%), zirconium (99%) and carbon (99%) powder of drying according to atomic ratio Mg: Zr: B: C=0.95: 0.05: 1.95: 0.05 ratio was fully mixed 1 hour.Powder after grinding is packed in 0.9 meter long low carbon steel pipe (internal diameter 10mm, wall thickness 1.5mm), make powder in pipe, reach substantial, tight, seal the steel pipe two ends then, in the 1 meter long oxygen-free copper pipe of again steel pipe being packed into (internal diameter 13.5mm, wall thickness 2mm).Then, the complex of this assembling is swaged, being machined to diameter according to the pass reduction of each 0.5mm is 7mm.Carry out groove rolling then, be processed into the square line that the length of side is 3mm according to the pass reduction of each 1.0mm.It is 1.2mm that square line is processed into diameter according to the pass reduction of each 0.2mm, and length is 50 meters wire rod.To process the back wire rod and place vacuum annealing furnace, under room temperature, vacuumize, wait to reach 10
-3Charge into pure argon (＞99%) after the vacuum degree of Pa, begin then wire rod to be heated with the heating rate that is not less than 60 ℃/minute, insulation is 3 hours under 750 ℃ temperature, to be not less than 20 ℃ of/minute cooldown rates wire rod is cooled to room temperature at last, just making superconducting transition temperature is 35.2K, and critical current density reaches 7.0 * 10
4A/cm
2(25K, MgB 1T)
2Practical super-conduct composite line material.
Example 5
With magnesium (99%), boron (99%), zirconium (99%) and carbon (99%) powder of drying according to atomic ratio Mg: Zr: B: C=0.9: 0.1: 1.9: 0.1 ratio was fully mixed 1 hour.Powder after grinding is packed in 0.9 meter long low carbon steel pipe (internal diameter 10mm, wall thickness 1.5mm), make powder in pipe, reach substantial, tight, seal the steel pipe two ends then, in the 1 meter long oxygen-free copper pipe of again steel pipe being packed into (internal diameter 13.5mm, wall thickness 2mm).Then, the complex of this assembling is swaged, being machined to diameter according to the pass reduction of each 0.5mm is 7mm.Carry out groove rolling then, be processed into the square line that the length of side is 3mm according to the pass reduction of each 1.0mm.It is 1.2mm that square line is processed into diameter according to the pass reduction of each 0.2mm, and length is 50 meters wire rod.Wire rod after the processing is placed vacuum annealing furnace, under room temperature, vacuumize, wait to reach 10
-3Charge into pure argon (＞99%) after the vacuum degree of Pa, begin then wire rod to be heated with the heating rate that is not less than 60 ℃/minute, insulation is 1 hour under 760 ℃ temperature, to be not less than 20 ℃ of/minute cooldown rates wire rod is cooled to room temperature at last, just making superconducting transition temperature is 35.1K, and critical current density reaches 7.7 * 10
4A/cm
2(25K, MgB 1T)
2Practical super-conduct composite line material.
Example 6
At first with magnesium (99%), boron (99%), zirconium (99%) and carbon (99%) powder of drying according to atomic ratio Mg: Zr: B: C=0.8: 0.2: 1.8: 0.2 ratio was fully mixed 2 hours.Powder after grinding is packed in 0.9 meter long low carbon steel pipe (internal diameter 10mm, wall thickness 1.5mm), make powder in pipe, reach substantial, tight, seal the steel pipe two ends then, in the 1 meter long oxygen-free copper pipe of again steel pipe being packed into (internal diameter 13.5mm, wall thickness 2mm).Then, the complex of this assembling is swaged, being machined to diameter according to the pass reduction of each 0.5mm is 7mm.Carry out groove rolling then, be processed into the square line that the length of side is 3mm according to the pass reduction of each 1.0mm.It is 1.2mm that square line is processed into diameter according to the pass reduction of each 0.2mm, and length is 50 meters wire rod.To process the back wire rod and place vacuum annealing furnace, under room temperature, vacuumize, wait to reach 10
-3Charge into pure argon (＞99%) after the vacuum degree of Pa, begin then wire rod to be heated with the heating rate that is not less than 60 ℃/minute, insulation is 10 hours under 740 ℃ temperature, to be not less than 20 ℃ of/minute cooldown rates wire rod is cooled to room temperature at last, just making superconducting transition temperature is 35.2K, and critical current density reaches 5.9 * 10
4A/cm
2(25K, MgB 1T)
2Practical super-conduct composite line material.
Claims (5)
1. high critical current densities MgB
2Base super conductor is characterized in that this superconductor is at MgB
2Distributing carbon, zirconium and compound thereof of disperse in the base super conductor, the atomic ratio of this superconductor consists of Mg: Zr: B: C=(1-x): x: (2-x): x, wherein 0.05≤x≤0.20.
2. a kind of high critical current densities MgB according to claim 1
2Base super conductor is characterized in that this MgB
2Base super conductor is sheet or bulk.
3. a kind of high critical current densities MgB according to claim 1
2Base super conductor is characterized in that this MgB
2Base super conductor is that cross sectional shape is round wire rod.
4. a kind of high critical current densities MgB according to claim 2
2The preparation method of base super conductor, it is characterized in that preparation process be at first with magnesium, boron, zirconium and the carbon dust of drying according to atomic ratio Mg: Zr: B: C=(1-x): the ratio of x: (2-x): x was fully mixed 1-2 hour, wherein 0.05≤x≤0.20; Mixed powder is exerted pressure to 20-80MPa suppresses in flakes or piece, place vacuum annealing furnace then, under room temperature, vacuumize, treat that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, sheet or bulk heating will make then greater than 60 ℃/minute heating rate, insulation is 1-10 hour under 740 ℃-760 ℃ temperature, at last be cooled to room temperature, make the MgB of high critical current densities with cooldown rate greater than 25 ℃/minute
2Substrate or bulk superconductor.
5. a kind of high critical current densities MgB according to claim 3
2The preparation method of base super conductor is characterized in that preparation process is at first with magnesium, boron, zirconium and the carbon dust of drying, and according to atomic ratio Mg: Zr: B: C=(1-x): the ratio of x: (2-x): x was fully mixed 1-3 hour, wherein 0.05≤x≤0.20; With mixed powder pack into seamless low carbon steel pipe or niobium pipe, again this complex is packed into and be assembled into complex in the oxygen-free copper pipe, again complex is carried out room temperature cold working process, through swaging, the comprehensive use of groove rolling and three kinds of processing technologys of drawing is processed into wire rod, the final cross sectional shape of wire rod is round; The wire rod that is worked into final size and shape is placed vacuum annealing furnace, under room temperature, vacuumize, treat that vacuum degree reaches 10
-3Charge into the gaseous mixture of pure argon or argon gas and hydrogen behind the Pa, with the heating rate that is not less than 60 ℃/minute wire rod is heated then, insulation is 1-10 hour under 740 ℃-760 ℃ temperature, at last with the cooldown rate that is not less than 25 ℃/minute wire rod is cooled to room temperature, making cross sectional shape is round MgB
2The base superconducting wire.
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| CN100354986C true CN100354986C (en) | 2007-12-12 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101508571B (en) * | 2009-04-03 | 2011-06-29 | 西北有色金属研究院 | Method for producing carbon doped MgB2 cryogenic conductor by step-by-step sintering reaction |
| CN102122549B (en) * | 2011-01-18 | 2012-11-07 | 西南交通大学 | Application of glucose in preparation of magnesium diboride-doped superconducting material |
| CN102982889B (en) * | 2012-11-20 | 2015-12-09 | 溧阳市生产力促进中心 | MgB 2superconducting line and manufacture method thereof |
| CN104607643A (en) * | 2014-12-25 | 2015-05-13 | 东南大学 | Method for preparing single-core MgB2 superconducting wire through center magnesium diffusion method |
| CN110229005B (en) * | 2019-07-16 | 2020-08-28 | 乐清市川嘉电气科技有限公司 | Novel superconducting material and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035324A (en) * | 1988-02-21 | 1989-09-06 | 中国科学院物理研究所 | No rare earth high-temperature superconductor Alloy And Preparation Method |
| JP2004296156A (en) * | 2003-03-26 | 2004-10-21 | National Institute For Materials Science | MANUFACTURING METHOD OF MgB2 SUPERCONDUCTING WIRE |
| JP2004307256A (en) * | 2003-04-07 | 2004-11-04 | Internatl Superconductivity Technology Center | MgB2-BASED SUPERCONDUCTOR WITH HIGH CRITICAL CURRENT DENSITY AND HIGH IRREVERSIBLE MAGNETIC FIELD |
-
2005
- 2005-12-28 CN CNB2005101327261A patent/CN100354986C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1035324A (en) * | 1988-02-21 | 1989-09-06 | 中国科学院物理研究所 | No rare earth high-temperature superconductor Alloy And Preparation Method |
| JP2004296156A (en) * | 2003-03-26 | 2004-10-21 | National Institute For Materials Science | MANUFACTURING METHOD OF MgB2 SUPERCONDUCTING WIRE |
| JP2004307256A (en) * | 2003-04-07 | 2004-11-04 | Internatl Superconductivity Technology Center | MgB2-BASED SUPERCONDUCTOR WITH HIGH CRITICAL CURRENT DENSITY AND HIGH IRREVERSIBLE MAGNETIC FIELD |
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