CN102992771A - Method for producing magnesium diboride-based superconducting block - Google Patents
Method for producing magnesium diboride-based superconducting block Download PDFInfo
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- CN102992771A CN102992771A CN2012104725701A CN201210472570A CN102992771A CN 102992771 A CN102992771 A CN 102992771A CN 2012104725701 A CN2012104725701 A CN 2012104725701A CN 201210472570 A CN201210472570 A CN 201210472570A CN 102992771 A CN102992771 A CN 102992771A
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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 invention discloses a method for producing magnesium diboride-based superconducting block. The method comprises the steps that (1) dried magnesium, boron, hafnium and silicon powders are fully mixed for 1-2 hours according to the atomic ratio of Mg, Hf, B and Si is (1-x):x:(2-x):x, wherein x is in the range from more than or equal to 0.05 to smaller than or equal to 0.20; (2) the mixed powders are pressed into blocks by applying 20-80 Mpa pressure; (3) the pressed blocks are put in a vacuum annealing furnace, are vacuumized under the room temperature, and are inflated with pure argon gas or the mixed gas of argon gas and hydrogen gas when the vacuum degree reaches 10<-3> Pa, then the produced superconducting blocks are heated with the temperature rise speed of more than 60 DEG C/minute and insulated for 1-10 hours under the temperature of 740-760 DEG C; and (4) finally the magnesium diboride-based superconducting block is produced by cooling the superconducting blocks to the room temperature with the cooling speed of more than 25 DEG C/minute. Based on the method, the MgB2-based superconducting material which is simple in preparation process, suitable for large-scale production and has high critical current density in a background magnetic field of more than 3 Tesla and the production method thereof are provided.
Description
Technical field
The present invention relates to a kind of preparation method of superconducting material.
Background technology
Magnesium diboride (MgB
2) be the highest intermetallic compound superconducting material of present critical transition temperature, its critical transition temperature (39-40K) is higher than the Nb that has carried out practical application at present
3The superconducting material such as Sn and NbTi.Higher transition temperature, larger coherence length, higher upper critical field, crystal boundary do not exist weak connection, the advantage such as simple in structure, with low cost to make MgB
2Become the strongest rival of material who is applied in the 20K-30K temperature range.
Particularly in a low field, as at magnet for magnetic resonant imaging application facet, MgB
2Show great advantage, had data to show, MgB
2Practically will bring billions of economic benefits, and owing to can under the refrigeration mechanism cool condition, work MgB
2Application will greatly promote the popularization of magnetic resonance imager, be of great significance for the raising tool of the vast rural people's medical level of China.
Yet, the MgB for preparing at present
2It is also lower that the critical current density of material and low temperature superconducting material are compared with the A15 superconducting material, and can rapid the reducing along with the increase of magneticstrength.Improve MgB
2Critical current density be a difficult problem because will produce the electronics vortex during by superconducting material when electric current, the motion consumed energy of electronics vortex, and then destroy the superconduction ability of material.If vortex can be pinned on impurity or the defective and not affect flowing of without hindrance electric current, can greatly improve critical current density.
Therefore, in order to improve MgB
2Critical current density under certain magnetic field can adopt the methods such as neutron (proton) bombardment, chemical corrosion, mechanical workout, doping, and since mix have easier fast, can carry out the characteristics such as even modification, become present raising MgB
2The main method of flux pinning ability.The Zr that has tested, Mo, Nb, W, Ti, Al, Fe, WSi
2, ZrSi
2All can only improve by a small margin MgB Deng doping
2Performance.
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 scale operation and the background magnetic field more than 3 teslas the MgB of high critical current densities
2Base superconducting material and manufacture method thereof.
The manufacture method of magnesium diboride base superconductive block of the present invention comprises the steps:
(1) magnesium, boron, hafnium and the Si powder of drying were fully mixed 1-2 hour according to the ratio of atomic ratio Mg: Hf: B: Si=1-x: x: 2-x: x, wherein 0.05≤x≤0.20;
(2) mixed powder is exerted pressure be the 20-80MPa briquetting;
(3) piece that will suppress places vacuum annealing furnace, vacuumizes under room temperature, treats that vacuum tightness reaches 10
-3Be filled with the gas mixture of pure argon or argon gas and hydrogen behind the Pa, then with the temperature rise rate greater than 60 ℃/minute the superconducting block that makes heated, insulation is 1-10 hour under 740 ℃-760 ℃ temperature;
(4) be cooled to room temperature with the rate of cooling greater than 25 ℃/minute at last, make magnesium diboride base superconductive block.
For 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 ordinary method that equals to prepare under the atmospheric pressure
2Superconducting material.And if in the mixed powder of magnesium and boron, add simultaneously an amount of silicon and metal hafnium as sintering agent, at the MgB that equals to prepare under the atmospheric pressure
2Disperse distributing silicon, hafnium and compound thereof in the base superconducting material, MgB
2The base superconducting material shows the feature of high critical current densities.
Method of the present invention adopts silicon and metal Hf as sintering agent, and after sintering process was finished, silicon, hafnium and compound disperse thereof were distributed in the MgB of final acquisition
2In the base superconducting material, the MgB that obtains
2Has high critical current density in the background magnetic field of base superconducting material more than 3 teslas.Silicon, hafnium and compound disperse thereof are distributed in the MgB of final acquisition
2In the base superconducting material, make the MgB of final formation
2Grain refining, efficient hardening MgB
2Crystal grain connects.The present invention can realize MgB
2Second phase particles has been introduced in the low cost preparation of base superconducting material simultaneously, has effectively improved MgB
2The flux pinning of base superconducting material.
Embodiment
In order to make those skilled in the art more clearly understand the present invention, describe its technical scheme in detail below by embodiment.
The manufacture method of magnesium diboride base superconductive block disclosed by the invention comprises the steps:
(1) magnesium, boron, hafnium and the Si powder of drying were fully mixed 1-2 hour according to the ratio of atomic ratio Mg: Hf: B: Si=1-x: x: 2-x: x, wherein 0.05≤x≤0.20;
(2) mixed powder is exerted pressure be the 20-80MPa briquetting;
(3) this piece is placed vacuum annealing furnace, under room temperature, vacuumize, treat that vacuum tightness reaches 10
-3Be filled with the gas mixture of pure argon or argon gas and hydrogen behind the Pa, then with the temperature rise rate greater than 60 ℃/minute the bulk that makes heated, insulation is 1-10 hour under 740 ℃-760 ℃ temperature;
(4) be cooled to room temperature with the rate of cooling greater than 25 ℃/minute at last, make the MgB of high critical current densities
2Matrix or bulk superconducting material.
The magnesium diboride superconductive block that adopts method of the present invention to make, wherein this superconducting material is at MgB
2Disperse distributing silicon, hafnium and compound thereof in the base superconducting material, this MgB
2The base atomic ratio consists of Mg: Hf: B: Si=1-x: x: 2-x: x, wherein 0.05≤x≤0.20.
The below specifies specific embodiment according to the invention.
Example 1
With magnesium (99%), boron (99%), hafnium (99%) and silicon (99%) powder of drying according to atomic ratio Mg: Hf: B: Si=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 oil press, exert pressure and be 20MPa, then place vacuum annealing furnace, under room temperature, vacuumize, after reaching 10-3 Pa, vacuum tightness is filled with the gas mixture of pure argon or argon gas and hydrogen, then with the temperature rise rate that is not less than 60 ℃/minute wire rod is heated, insulation is 10 hours under 740 ℃ temperature, to be not less than 25 ℃ of/minute rate of cooling piece 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
2The MgB of (20K, 4T)
2The base superconductive block.
Example 2
With magnesium (99%), boron (99%), hafnium (99%) and silicon (99%) powder of drying according to atomic ratio Mg: Hf: B: Si=0.9: 0.1: 1.9: 0.1 ratio was fully mixed 1 hour.Mixed powder is pressed into the piece of diameter 20mm with oil press, and exerting pressure is then to place vacuum annealing furnace by 80MPa, vacuumizes under room temperature, treats that vacuum tightness reaches 10
-3Be filled with the gas mixture of pure argon or argon gas and hydrogen behind the Pa, then to be not less than 60 ℃/minute temperature rise rate with the heating of piece or bulk, insulation is 1 hour under 760 ℃ temperature, to be not less than 25 ℃ of/minute rate of cooling 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
2The MgB of (20K, 4T)
2The base superconductive block.
Example 3
With magnesium (99%), boron (99%), hafnium (99%) and silicon (99%) powder of drying according to atomic ratio Mg: Hf: B: Si=0.8: 0.2: 1.8: 0.2 ratio was fully mixed 1.5 hours.Mixed powder is pressed into the piece of diameter 20mm with oil press, and exerting pressure is then to place vacuum annealing furnace by 60MPa, vacuumizes under room temperature, treats that vacuum tightness reaches 10
-3Be filled with the gas mixture of pure argon or argon gas and hydrogen behind the Pa, then with the temperature rise rate that is not less than 60 ℃/minute wire rod is heated, insulation is 6 hours under 750 ℃ temperature, to be not less than 25 ℃ of/minute rate of cooling piece 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
2The MgB of (20K, 4T)
2The base superconductive block.
Certainly; the present invention also can have other various embodiments; in the situation that does not deviate from spirit of the present invention and essence thereof; those of ordinary skill in the art work as can make according to the present invention various corresponding changes and distortion, but these corresponding changes and distortion all should belong to the protection domain of the appended claim of the present invention.
Claims (4)
1. the manufacture method of a magnesium diboride base superconductive block is characterized in that, comprises the steps:
(1) magnesium, boron, hafnium and the Si powder of drying were fully mixed 1-2 hour according to the ratio of atomic ratio Mg: Hf: B: Si=1-x: x: 2-x: x, wherein 0.05≤x≤0.20;
(2) mixed powder is exerted pressure be the 20-80MPa briquetting;
(3) piece that will suppress places vacuum annealing furnace, vacuumizes under room temperature, treats that vacuum tightness reaches 10
-3Be filled with the gas mixture of pure argon or argon gas and hydrogen behind the Pa, then with the temperature rise rate greater than 60 ℃/minute the superconducting block that makes heated, insulation is 1-10 hour under 740 ℃-760 ℃ temperature;
(4) be cooled to room temperature with the rate of cooling greater than 25 ℃/minute at last, make magnesium diboride base superconductive block.
2. manufacture method as claimed in claim 1 is characterized in that, Mg: Hf: B: Si=0.95: 0.05: 1.95: 0.05.
3. manufacture method as claimed in claim 1 is characterized in that, Mg: Hf: B: Si=0.9: 0.1: 1.9: 0.1.
4. manufacture method as claimed in claim 1 is characterized in that, Mg: Hf: B: Si=0.8: 0.2: 1.8: 0.2.
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| CN2012104725701A CN102992771A (en) | 2012-11-20 | 2012-11-20 | Method for producing magnesium diboride-based superconducting block |
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| CN2012104725701A CN102992771A (en) | 2012-11-20 | 2012-11-20 | Method for producing magnesium diboride-based superconducting block |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541338A (en) * | 2016-01-13 | 2016-05-04 | 天津大学 | Method for increasing superconducting critical current density of ex-situ magnesium diboride block through self reaction |
| CN106521291A (en) * | 2016-11-04 | 2017-03-22 | 金福兴 | Composite superconductive nanometer block material and preparation method thereof |
Citations (2)
| 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 |
| CN101343184A (en) * | 2008-09-10 | 2009-01-14 | 西北有色金属研究院 | Preparation method for MgB2 based composite element doped cryogenic conductor |
-
2012
- 2012-11-20 CN CN2012104725701A patent/CN102992771A/en active Pending
Patent Citations (2)
| 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 |
| CN101343184A (en) * | 2008-09-10 | 2009-01-14 | 西北有色金属研究院 | Preparation method for MgB2 based composite element doped cryogenic conductor |
Non-Patent Citations (1)
| Title |
|---|
| X.L.WANG ET AL.: "Significant enhancement of critical current density and flux pinning in MgB2 with nano-SiC，Si，and C doping", 《PHYSICA C》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105541338A (en) * | 2016-01-13 | 2016-05-04 | 天津大学 | Method for increasing superconducting critical current density of ex-situ magnesium diboride block through self reaction |
| CN106521291A (en) * | 2016-11-04 | 2017-03-22 | 金福兴 | Composite superconductive nanometer block material and preparation method thereof |
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Application publication date: 20130327 |