CN100354985C - Preparation method of MgB2 superconductor - Google Patents
Preparation method of MgB2 superconductor Download PDFInfo
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- CN100354985C CN100354985C CNB2005101327219A CN200510132721A CN100354985C CN 100354985 C CN100354985 C CN 100354985C CN B2005101327219 A CNB2005101327219 A CN B2005101327219A CN 200510132721 A CN200510132721 A CN 200510132721A CN 100354985 C CN100354985 C CN 100354985C
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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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Abstract
The present invention provides a method for preparing MgB2 superconductors, which relates to a method for preparing MgB2 superconductors in fractional reactions. The present invention is characterized in that firstly, magnesium and boron mixing powder with the atomic ratio (the magnesium to the boron) of 1 to 4 is sintered, and then a right amount of metallic magnesium powder is added to sintered products and sintered for the second time to obtain MgB2 superconductors. The MgB2 superconductors which are prepared by the method have the characteristic of high density and high critical temperature.
Description
Technical field
A kind of MgB
2The preparation method of superconductor relates to a kind of stepwise reaction and prepares MgB
2The method of superconductor.
Background technology
Superconducting transition temperature is the novel type MgB of 39K
2Discovery, in worldwide, started research boom, compare MgB with oxide superconductor
2Middle Superconducting Current Density is higher, and crystal boundary is " transparent " to supercurrent, and promptly supercurrent is not subjected to the restriction of crystal boundary connectedness, simultaneously MgB
2It is simpler than the oxide high temperature superconductor of perovskite structure that superconductor also has a crystal structure, and preparation is than being easier to MgB
2The wire strip price low than HTS (high-temperature superconductor) and LTS (cryogenic superconductor), so MgB
2Wide application prospect is arranged.MgB
2Be compound superconductive between the simple binary metal of a kind of crystal structure, belong to hexagonal crystal system.MgB
2Crystal alternately pile up by Mg layer and B layer and form, have six side's symmetry, lattice parameter a=0.3086nm, c=0.3524nm, the volume of unit cell equals
Its molal volume V=17.62cm
3/ mol, MgB
2The density of crystal is 2.065g/cm
3
Prepare MgB at present
2What superconductor adopted mainly is normal pressure-sintered technology, and its general technical process is: after Mg powder, B powder and dopant mixing, grinding, compression molding, pressed compact with Ta paper tinsel parcel, is carried out sintering reaction then and obtains MgB in high-purity Ar
2The polycrystalline superconductor.Also have pressed compact is enclosed in and carry out sintering in the metal tubes such as Ta pipe.Normal pressure-sintered technology is fairly simple, grind evenly according to 1: 2 ratio Mg powder, B powder after, sintering promptly obtains MgB under the uniform temperature
2Bulk.But the MgB for preparing
2Bulk usually is a porous, and density is lower, causes its critical current density also very low.In order to improve MgB
2The density of bulk, many research groups have adopted high-pressure sinter technology again.This technology is after earlier grinding evenly according to 1: 2 ratio Mg powder, B powder, under condition of high voltage (＞1GPa), (＞900 ℃) sintering certain hour under the high temperature, after the release cooling, promptly obtain fine and close MgB
2Bulk.But the method for high pressure exist the cost height, can't be at MgB
2Shortcoming such as use in the superconducting wire preparation process.
Summary of the invention
The objective of the invention is to overcome existing MgB
2The deficiency of superconductor technology of preparing provides a kind of preparation method simple and be suitable for the MgB of large-scale production
2The preparation method of superconductor.
The objective of the invention is to be achieved through the following technical solutions.
A kind of MgB
2The preparation method of superconductor is characterized in that preparation process is:
(1) with the magnesium of drying, boron powder according to atomic ratio Mg: B=1: 4 ratio was fully mixed 1-2 hour, and mixed powder compaction is in flakes or piece;
(2) sheet that will suppress or piece place vacuum annealing furnace, under room temperature, vacuumize, charge into the gaseous mixture of pure argon or argon gas and hydrogen then, then to be not less than 60 ℃/minute heating rate heating, insulation is 1-10 hour under 650 ℃-1000 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates it is cooled to room temperature at last;
(3) sheet that sintering is obtained or piece carry out fragmentation, are 1: 2 to wherein adding the atom proportioning of metal magnesium powder to magnesium and boron then, more mixed powder are used the in blocks or piece of compacting;
(4) sheet that will suppress or piece place vacuum annealing furnace, under room temperature, vacuumize, charge into the gaseous mixture of pure argon or argon gas and hydrogen then, then to be not less than 60 ℃/minute heating rate heating, be not higher than under 1000 ℃ the temperature insulation 1-10 hour, to be not less than 25 ℃ of/minute cooldown rates it is cooled to room temperature at last, makes MgB
2Superconductor.
At the research that invention is carried out, find that the Mg-B system phase diagram shows that there are two stable phase: MgB in the boride of magnesium
4And MgB
2, MgB
4And reactive magnesium (650-1000 ℃) can generate MgB
2Therefore can adopt following method to obtain MgB
2Superconductor: the atom proportioning that at first adopts magnesium and boron is that 1: 4 mixed-powder is as sintered powder, equaling sintering under the atmospheric pressure, in the sintered body that obtains, add metal magnesium powder then, the atom proportioning that obtains magnesium and boron is 1: 2 a mixed-powder, equaling under the atmospheric pressure, under the uniform temperature this mixed-powder being carried out sintering, finally obtain MgB
2Superconductor.The MgB of preparation
2Superconductor shows the characteristics of high-compactness, still keeps the high-critical temperature feature simultaneously.
Method of the present invention adopts the stepwise reaction legal system to be equipped with the MgB of high-compactness
2Superconductor, effectively refinement MgB
2Crystal grain is strengthened MgB
2Crystal grain connects.Overcome simultaneously because the magnesium of capacity reacts in the generative process with boron,, effectively improved MgB owing to the cavity that the gasification of magnesium generates
2The density of superconductor.The present invention can realize MgB
2Low cost, the mass preparation of base superconductor.
Specific embodiments
A kind of MgB
2The preparation method of superconductor, preparation process for (1) with the magnesium of drying, boron powder according to atomic ratio Mg: B=1: 4 ratio was fully mixed 1-2 hour, and mixed powder compaction is in flakes or piece; (2) sheet that will suppress or piece place vacuum annealing furnace, under room temperature, vacuumize, charge into the gaseous mixture of pure argon or argon gas and hydrogen then, then to be not less than 60 ℃/minute heating rate heating, insulation is 1-10 hour under 650 ℃-1000 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates it is cooled to room temperature at last; (3) sheet that sintering is obtained or piece carry out fragmentation, are 1: 2 to wherein adding the atom proportioning of metal magnesium powder to magnesium and boron then, more mixed powder are used the in blocks or piece of compacting; (4) sheet that will suppress or piece place vacuum annealing furnace, under room temperature, vacuumize, charge into the gaseous mixture of pure argon or argon gas and hydrogen then, then to be not less than 60 ℃/minute heating rate heating, insulation is 1-10 hour under 650 ℃-1000 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates it is cooled to room temperature at last, makes MgB
2Superconductor.
Specify technical examples according to the invention below.
Example 1
With the magnesium (99%) of drying, boron (99%) powder according to atomic ratio Mg: B=1: 4 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 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, then with 60 ℃/minute heating rate with sheet or piece heating, insulation is 2 hours under 650 ℃ temperature, with 25 ℃ of/minute cooldown rates sheet or piece is cooled to room temperature at last.Then sheet or piece are broken into the powder that granularity is the 10-15 micron, to wherein adding metal magnesium powder, the atom proportioning that obtains magnesium and boron is 1: 2 a mixed-powder.The mixed powder art is pressed into the sheet 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 pure argon behind the Pa, with 60 ℃/minute heating rate sheet is heated then, insulation is 10 hours under 650 ℃ temperature, with 25 ℃ of/minute cooldown rates sheet or bulk is cooled to room temperature at last, just making superconducting transition temperature is 38.4K, and apparent density is 1.923g/cm
3MgB
2Superconductor.
Example 2
With the magnesium (99%) of drying, boron (99%) powder according to atomic ratio Mg: B=1: 4 ratio was fully mixed 2 hours.Mixed powder is pressed into sheet or the piece 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 argon gas and hydrogen behind the Pa, then with 60 ℃/minute heating rate with sheet or piece heating, insulation is 5 hours under 700 ℃ temperature, with 25 ℃ of/minute cooldown rates sheet or piece is cooled to room temperature at last.Then sheet or piece are broken into the powder that granularity is the 10-15 micron, to wherein adding metal magnesium powder, the atom proportioning that obtains magnesium and boron is 1: 2 a mixed-powder.Mixed-powder is pressed into sheet or the piece of diameter 20mm with hydraulic press, and exerting pressure is to place vacuum annealing furnace then by 20-80MPa, 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 with 65 ℃/minute heating rate with sheet or bulk heating, insulation is 5 hours under 700 ℃ temperature, with 30 ℃ of/minute cooldown rates sheet or bulk are cooled to room temperature at last, just making superconducting transition temperature is 38.6K, and apparent density is 1.935g/cm
3MgB
2Superconductor.
Example 3
With the magnesium (99%) of drying, boron (99%) powder according to atomic ratio Mg: B=1: 4 ratio was fully mixed 1-2 hour.Mixed powder is pressed into sheet or the piece 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 argon gas behind the Pa, with 60 ℃/minute heating rate piece is heated then, insulation is 7 hours under 750 ℃ temperature, with 25 ℃ of/minute cooldown rates piece is cooled to room temperature at last.Then sheet or piece are broken into the powder that granularity is the 10-15 micron, to wherein adding metal magnesium powder, the atom proportioning that obtains magnesium and boron is 1: 2 a mixed-powder.Mixed-powder is pressed into sheet or the piece 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 with 65 ℃/minute heating rate with sheet or bulk heating, insulation is 7 hours under 750 ℃ temperature, with 30 ℃ of/minute cooldown rates bulk is cooled to room temperature at last, just making superconducting transition temperature is 38.8K, and apparent density is 1.947g/cm
3MgB
2Superconductor.
Example 4
With the magnesium (99%) of drying, boron (99%) powder according to atomic ratio Mg: B=1: 4 ratio was fully mixed 1-2 hour.Mixed powder is pressed into sheet or the piece 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, then with 60 ℃/minute heating rate with sheet or piece heating, insulation is 2 hours under 800 ℃ temperature, with 25 ℃ of/minute cooldown rates sheet or piece is cooled to room temperature at last.Then sheet or piece are broken into the powder that granularity is the 10-15 micron, to wherein adding metal magnesium powder, the atom proportioning that obtains magnesium and boron is 1: 2 a mixed-powder.Mixed-powder is pressed into sheet or the piece 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, then with 65 ℃/minute heating rate with sheet or bulk heating, insulation is 2 hours under 800 ℃ temperature, with 30 ℃ of/minute cooldown rates sheet or bulk are cooled to room temperature at last, just making superconducting transition temperature is 38.3K, and apparent density is 1.912g/cm
3MgB
2Superconductor.
Example 5
With the magnesium (99%) of drying, boron (99%) powder according to atomic ratio Mg: B=1: 4 ratio was fully mixed 1-2 hour.Mixed powder is pressed into sheet or the piece of diameter 20mm with hydraulic press, and exerting pressure is to place vacuum annealing furnace then by 40MPa, vacuumizes under room temperature, treats that vacuum degree reaches 10
-3Charge into the gaseous mixture of hydrogen behind the Pa, then with 60 ℃/minute heating rate with sheet or piece heating, insulation is 1.5 hours under 900 ℃ temperature, with 25 ℃ of/minute cooldown rates sheet is cooled to room temperature at last.Then sheet or piece are broken into the powder that granularity is the 10-15 micron, to wherein adding metal magnesium powder, the atom proportioning that obtains magnesium and boron is 1: 2 a mixed-powder.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 argon gas and hydrogen behind the Pa, then with 65 ℃/minute heating rate with sheet or bulk heating, insulation is 1.5 hours under 900 ℃ temperature, with 35 ℃ of/minute cooldown rates sheet or bulk are cooled to room temperature at last, just making superconducting transition temperature is 38.1K, and apparent density is 1.878g/cm
3MgB
2Superconductor.
Example 6
With the magnesium (99%) of drying, boron (99%) powder according to atomic ratio Mg: B=1: 4 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 40MPa, vacuumizes under room temperature, treats that vacuum degree reaches 10
-3Charge into the gaseous mixture of hydrogen behind the Pa, then with 60 ℃/minute heating rate with sheet or piece heating, insulation is 1 hour under 1000 ℃ temperature, with 25 ℃ of/minute cooldown rates sheet is cooled to room temperature at last.Then sheet or piece are broken into the powder that granularity is the 10-15 micron, to wherein adding metal magnesium powder, the atom proportioning that obtains magnesium and boron is 1: 2 a mixed-powder.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 argon gas and hydrogen behind the Pa, with 65 ℃/minute heating rate sheet material is heated then, insulation is 1 hour under 1000 ℃ temperature, with 35 ℃ of/minute cooldown rates sheet or bulk is cooled to room temperature at last, just making superconducting transition temperature is 38.0K, and apparent density is 1.877g/cm
3MgB
2Superconductor.
Claims (1)
1. MgB
2The preparation method of superconductor is characterized in that preparation process is:
(1) with the magnesium of drying, boron powder according to atomic ratio Mg: B=1: 4 ratio was fully mixed 1-2 hour, and mixed powder compaction is in flakes or piece;
(2) sheet that will suppress or piece place vacuum annealing furnace, under room temperature, vacuumize, charge into the gaseous mixture of pure argon or argon gas and hydrogen then, then to be not less than 60 ℃/minute heating rate heating, insulation is 1-10 hour under 650 ℃-1000 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates it is cooled to room temperature at last;
(3) sheet that sintering is obtained or piece carry out fragmentation, are 1: 2 to wherein adding the atom proportioning of metal magnesium powder to magnesium and boron then, more mixed powder are used the in blocks or piece of compacting;
(4) sheet that will suppress or piece place vacuum annealing furnace, under room temperature, vacuumize, charge into the gaseous mixture of pure argon or argon gas and hydrogen then, then to be not less than 60 ℃/minute heating rate heating, insulation is 1-10 hour under 650 ℃-1000 ℃ temperature, to be not less than 25 ℃ of/minute cooldown rates it is cooled to room temperature at last, makes MgB
2Superconductor.
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| CN101515493B (en) * | 2009-04-03 | 2010-12-29 | 西北有色金属研究院 | Method of preparing MgB2/Nb/Cu multi-core composite superconducting wire |
| CN112408988B (en) * | 2020-11-25 | 2022-12-06 | 郑州华晶实业有限公司 | High-temperature high-pressure preparation method of superconducting material magnesium diboride |
| CN114570925B (en) * | 2022-03-03 | 2023-12-08 | 江苏徐工工程机械研究院有限公司 | Ceramic-steel composite and preparation method thereof |
Citations (5)
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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 |
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- 2005-12-28 CN CNB2005101327219A patent/CN100354985C/en active Active
Patent Citations (5)
| 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 |
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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