CN101279741A - Method for preparing magnesium diboride superconductive material - Google Patents
Method for preparing magnesium diboride superconductive material Download PDFInfo
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- CN101279741A CN101279741A CNA2008100444670A CN200810044467A CN101279741A CN 101279741 A CN101279741 A CN 101279741A CN A2008100444670 A CNA2008100444670 A CN A2008100444670A CN 200810044467 A CN200810044467 A CN 200810044467A CN 101279741 A CN101279741 A CN 101279741A
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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 invention relates to a method for preparing magnesium boride superconducting material. The method for preparing the magnesium boride superconducting material is that magnesium powder and boron powder are respectively weighted according to 1:0.7-2.5 of molar ratio; adulterant which is one of citric acid and citrate is weighted according to 1:0.01-1 of mass ratio between the total mass of the magnesium powder and the boron powder and the mass of the adulterant is weighted; the magnesium powder, the boron powder and the adulterant are evenly mixed into mixing powder, then sintered under the protection of argon atmosphere at the temperature of 600-1200 DEG C and the product is obtained after the heat is preserved for 0.5-12 hours. The method has short preparation time, low reaction temperature, high efficiency and low cost and is especially suitable for industrial production; the critical current density of the magnesium boride superconducting material prepared by the method is increased remarkably and is especially very high in highfield, thereby being good for the application in highfield and having strong practicability.
Description
Technical field
The present invention relates to a kind of method for preparing magnesium diboride super conductive material, relate in particular to a kind of preparation method of adulterated magnesium diboride super conductive material.
Background technology
The calendar year 2001 discovery of magnesium diboride supraconductivity has caused the very big interest of Condensed Matter Physics circle and superconduction industry member, and the scientists and engineers of various countries has carried out big quantity research to magnesium diboride super conductive material.Magnesium diboride is the twice of compound superconductive between known binary metal (Nb3Sn and Nb-Ti) near the transition temperature of 40K.The lower superconducting transition temperature of tradition superconductor makes its practical application can only be confined to the liquid helium warm area, thereby operation and maintenance cost is very expensive.Compare with traditional superconductor, the superconducting transition temperature of magnesium diboride 40K can easily use mini refrigerating machine to obtain, and does not need with complicated and expensive liquid helium refrigeration system, thereby makes the industrial application of magnesium diboride super conductive material become possibility.And compare with the high-temperature superconductor (HTSC) of perovskite structure, the advantage of magnesium diboride is: anisotropy is very little, and coherence length is longer, and it is good that crystal boundary connects, and do not have the weak problem that connects of crystal boundary, simple in structure, prepares easy.In a word, still be that high-temperature superconductor is compared with traditional superconductor, magnesium diboride all has himself special advantages, has very big potentiality to be exploited in the Application Areas of electromagnetic application fields such as levitated superconducting magnet train and microelectronics superconductive device.But because the critical current density of pure magnesium diboride super conductive material is very fast with the foreign field decay, limited the application of magnesium diboride super conductive material in the contour magnetic field environment of levitated superconducting magnet train, had a strong impact on its practical performance.Therefore, how to improve the emphasis that the critical current density of magnesium diboride super conductive material under the upfield becomes research.Many researchs all find can effectively improve by the nano-sized carbon doping upper critical field of mgb 2 superconductor; thereby improve its current-carrying performance under the upfield; the carbon doping particle of nanometer scale can also improve the performance of mgb 2 superconductor as effective pinning center on the other hand.But existing solid phase reaction method is with behind magnesium powder, boron powder and the nano-sized carbon powder mixed grinding, carries out sintering under the high temperature more than 900 ℃.Because the existence of effects such as the reunion of adulterated nano-scale carbon powder can't disperse adulterated nano-sized carbon powder equably, thereby cause the doping component of mgb 2 superconductor of preparation inhomogeneous, influence the overall performance of superconduction piece.In addition, the nanometer powder of reunion can cause the local excessive of hotchpotch, and unreacted hotchpotch is deposited in the intergranule of sample, becomes the obstruction barrier of supercurrent, further influences superconductivity.The carbon material price of nano particle is higher on the other hand, the preparation difficulty, and the doping of solid-state carbon enters MgB
2Lattice is difficulty relatively, needs higher temperature of reaction and long reaction times, and these have all limited the preparation of adulterated magnesium diboride super conductive material.
Summary of the invention
Purpose of the present invention just provides a kind of method for preparing magnesium diboride super conductive material, and this method preparation time is short, and temperature of reaction is low, the efficient height, and cost is low, is particularly suitable for suitability for industrialized production; Utilize the magnesium diboride super conductive material of this method preparation, the critical current density height, especially close very high at upfield lower critical electric current, help its application under the upfield, practical.
The present invention realizes that the technical scheme that its goal of the invention adopts is: a kind of method for preparing magnesium diboride super conductive material, and its practice is:
In molar ratio 1: 0.7-2.5 is weighing magnesium powder and boron powder respectively; Press the total mass of magnesium powder and boron powder and the mass ratio 1 of hotchpotch again: 0.01-1 weighing hotchpotch, hotchpotch are a kind of in citric acid or the Citrate trianion; The powder of magnesium powder, boron powder and hotchpotch is uniformly mixed into mixed powder, carries out sintering then under argon gas atmosphere protection, the agglomerating temperature is 600 ℃-1200 ℃, soaking time 0.5-12 hour, promptly.
Compared with prior art, the invention has the beneficial effects as follows:
One, with citric acid or Citrate trianion as hotchpotch and magnesium powder and boron powder uniform mixing, behind the certain temperature sintering, citric acid and Citrate trianion are decomposed into hotchpotchs such as carbon, hydrogen, oxygen and compound thereof, are dispersed in the magnesium diboride super conductive material.Because citric acid or the Citrate trianion lesser temps (150-200 ℃) when heating up issues estranged separating, again under 600 ℃-1200 ℃ around knot, form adulterated magnesium diboride super conductive material.Compare with existing solid state reaction, make temperature of reaction can be lower, the time is shorter, the efficient height.
Two, because the carbon source in the citric acid is to decompose to generate carbon source in the agglomerating temperature-rise period, with directly do as the doping carbon source with carbon dust, have stronger chemically reactive, can directly be incorporated in the magnesium diboride lattice, thereby make carbon atom can be doped to MgB more equably
2Lattice in, form MgB
2Lattice distortion, strengthen MgB
2The impurity scattering of energy interband improves MgB
2Upper critical field, thereby obviously improve MgB
2Critical current density under the upfield.It is compared with the carbon nano tube-doped magnesium diboride super conductive material of existing solid reaction process preparation, and critical current density can improve 2 times.
Three, the used hotchpotch of the present invention is citric acid or Citrate trianion, is industrial chemicals commonly used and food interpolation product, and it is cheap, nontoxic and easy to prepare.And the carbon material of existing hotchpotch nano particle such as Nano diamond, nano-sized carbon etc. are the price costliness all, complicated process of preparation and be unsuitable for industrial production in enormous quantities.
Experiment showed, the magnesium diboride super conductive material after the citric acid that utilizes the inventive method preparation or Citrate trianion mix, in the 20K temperature, when adding the upfield of 4T, critical current density can improve more than 400% than plain magnesium diboride super conductive material.
The concrete practice that the above-mentioned powder with magnesium powder, boron powder and hotchpotch is uniformly mixed into mixed powder is: hotchpotch is dissolved in forms hotchpotch solution in the solvent earlier, solvent is a kind of in alcohol, acetone, benzene, toluene or the water; Thorough mixing in the boron powder adding hotchpotch solution is become suspension liquid, will add the magnesium powder after the suspension liquid vacuum-drying again,
Utilize chemical dissolution method that citric acid and Citrate trianion are dissolved in the middle of alcohol, acetone, benzene, this class organic solvent of toluene or the water, vacuum-drying makes after the chemical solvents evaporation, citric acid of separating out or Citrate trianion be parcel boron powder evenly, thereby hotchpotch can be distributed in the boron powder starting material equably, hotchpotch can not produce the phenomenon of reunion, local excessive phenomenon, has further improved the critical supercurrent that makes thing.
Above-mentioned becomes the concrete practice of suspension liquid to be thorough mixing in the boron powder adding hotchpotch solution: adopt ultrasonic blended method.Like this, can make hotchpotch more even with mixing of boron powder.
To carry out sintering again behind the above-mentioned mixed powder tablet forming.But sintering goes out superconductive block like this, can be used as superconductive block and directly uses.
The present invention is further detailed explanation below in conjunction with accompanying drawing and concrete embodiment.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the magnesium diboride superconductive block of the embodiment of the invention one preparation.
Fig. 2 is the critical current density curve of the magnesium diboride superconductive block of the magnesium diboride superconductive block of the embodiment of the invention one preparation and last doping.
Fig. 3 be the magnesium diboride superconductive block of the embodiment of the invention two preparation and last doping the magnesium diboride superconductive block the critical current density curve.
Fig. 4 be the magnesium diboride superconductive block of the embodiment of the invention three preparation and last doping the magnesium diboride superconductive block the critical current density curve.
Fig. 5 be the magnesium diboride superconductive block of the embodiment of the invention four preparation and last doping the magnesium diboride superconductive block the critical current density curve.
Wherein, the curve that " " constitutes among Fig. 2-5 is the critical current density curve of the magnesium diboride superconductive block of last doping.The curve that " △ " constitutes among " zero ", Fig. 5 among " ▲ ", Fig. 4 among " zero ", Fig. 3 among Fig. 2 is respectively the critical current density curve of the magnesium diboride superconductive block of embodiment 1-4 preparation.And be labeled as the curve of 10K and 20k among Fig. 2-5, its probe temperature is respectively 10K and 20k.
Embodiment
Embodiment one
A kind of embodiment of the present invention is, a kind of preparation method of magnesium diboride super conductive material, and its concrete practice is:
1: 2 in molar ratio weighing magnesium powder and boron powder; Press the total mass of magnesium powder and boron powder and 1: 0.05 weighing hotchpotch of mass ratio of hotchpotch again, hotchpotch is a citric acid; Directly the powder uniform mixing with magnesium powder and boron powder and hotchpotch becomes mixed powder; Behind the mixed powder tablet forming, under the argon gas atmosphere protection, carry out sintering then, 800 ℃ of sintering temperatures are incubated 1 hour, promptly get the magnesium diboride superconductive block.
Fig. 2 illustrates, the magnesium diboride superconductive block that this example makes, and at 10K, its critical current density can reach 15000A/cm under the 4T condition
2, to compare with plain magnesium diboride superconductive block, critical current density has improved 70%.Temperature 20K, when foreign field was 4T, after the doping, the critical current density of magnesium diboride superconductive block reached 430A/cm
2, improved 480% than plain magnesium diboride superconductive block.Fig. 1 is the X ray diffracting spectrum of the magnesium diboride superconductive block of this example preparation.As seen from the figure, the magnesium boride doped superconductive block of this example preparation has good crystal phase structure.
Embodiment two
1: 2.1 in molar ratio, weighing Mg powder and B powder.Be 1: 0.1 weighing hotchpotch citric acid powder by the total mass of Mg powder and B powder and the mass ratio of hotchpotch again.Citric acid powder is dissolved in forms solution in the acetone, then with this solution with obtain even suspension liquid after the B powder ultra-sonic dispersion of weighing mixes, vacuum-drying obtains mixed powder, the Mg powder with itself and weighing is mixed into mixed powder then, and with the mixed powder tablet forming.In argon gas atmosphere compressing tablet is carried out sintering, i.e. 1000 ℃ of insulations were cooled fast to room temperature, the adulterated magnesium diboride superconductive block that promptly gets after 0.5 hour.Fig. 3 is the critical current density curve of the magnesium diboride superconductive block of this example preparation, and as seen from the figure, at 10K, its critical current density can reach 18200A/cm under the 4T condition
2Compare with plain magnesium diboride superconductive block, its critical current density has improved 96.8%.Temperature 20K, when foreign field was 4T, after the doping, the critical current density of magnesium diboride superconductive block reached 381A/cm
2, improved 415% than plain magnesium diboride superconductive block.
Embodiment three
1: 2 in molar ratio, weighing Mg powder and B powder.Be 1: 0.05 weighing hotchpotch citric acid calcium powder by the total mass of Mg powder and B opaque amount and the mass ratio of hotchpotch again.Three kinds of powder mixes are even, and, compressing tablet is carried out sintering in argon gas atmosphere with the mixed powder tablet forming, 700 ℃ of insulations cooled to room temperature with the furnace after 5 hours, made magnesium boride doped superconductive block.Fig. 4 is the critical current density curve of the magnesium diboride superconductive block of this example preparation.As seen from the figure, temperature 20K, when foreign field was 4T, the critical current density of magnesium diboride superconductive block reached 613A/cm
2, improved 939% than plain magnesium diboride superconductive block.
Embodiment four
1: 2 in molar ratio weighing Mg powder and B powder.Mass ratio by Mg powder and B opaque amount sum and hotchpotch is 1: 0.3 weighing hotchpotch trisodium citrate powder again, and three kinds of powder mixes are obtained mixed powder.And with the mixed powder tablet forming, compressing tablet carried out 1 hour sintering of 900 ℃ of insulations in argon gas atmosphere after, cool to room temperature with the furnace.Fig. 5 is the critical current density curve of the magnesium diboride superconductive block of this example preparation.As seen from the figure, temperature 20K, when foreign field was 4T, after the doping, the critical current density of magnesium diboride superconductive block reached 769A/cm
2, improved 728% than plain magnesium diboride superconductive block.
Embodiment five
1: 2.5 in molar ratio, weighing Mg powder and B powder.Mass ratio by Mg powder and B opaque amount sum and hotchpotch is 1: 0.7 weighing hotchpotch citric acid iron powder again.The ironic citrate powder dissolution in water, is obtained suspension liquid behind the B powder uniform mixing with this solution and weighing then, and vacuum-drying, the Mg powder uniform mixing with weighing obtains mixed powder again.With the mixed powder tablet forming, in argon gas atmosphere, carry out sintering, 600 ℃ are incubated 8 hours, cool to room temperature, promptly.
Embodiment six
1: 1.9 in molar ratio, weighing Mg powder and B powder.Mass ratio by Mg powder and B opaque amount sum and hotchpotch is 1: 0.5 weighing hotchpotch citric acid iron powder again.Three kinds of powder uniform mixing are obtained mixed powder, carry out sintering in argon gas atmosphere, 600 ℃ of insulations are after 10 hours, and furnace cooling promptly gets magnesium diboride superconduction powder to room temperature.
Embodiment seven
1: 0.7 in molar ratio, weighing Mg powder and B powder.Mass ratio by Mg powder and B opaque amount sum and hotchpotch is 1: 0.01 weighing hotchpotch citric acid calcium powder again.The citrate of lime powder dissolution in toluene, is obtained suspension liquid with the B powder of weighing after ultrasonic the mixing with this solution then, and vacuum-drying, the Mg powder uniform mixing with weighing obtains mixed powder again.Mixed powder is carried out sintering in argon gas atmosphere, 1200 ℃ of insulations are after 12 hours, and furnace cooling promptly gets magnesium diboride superconduction powder to room temperature.
Embodiment eight
1: 2.5 in molar ratio, weighing Mg powder and B powder.Mass ratio by Mg powder and B opaque amount sum and hotchpotch is 1: 1 weighing hotchpotch magnesium citrate powder again.The magnesium citrate powder dissolution in benzene, is obtained suspension liquid with the B powder of weighing after ultrasonic the mixing with this solution then, and vacuum-drying, the Mg powder uniform mixing with weighing obtains mixed powder again.To mixed powder, in argon gas atmosphere, carry out sintering, 900 ℃ of insulations are after 1 hour, and furnace cooling promptly gets magnesium diboride superconduction powder to room temperature.
Claims (4)
1, a kind of method for preparing magnesium diboride super conductive material, its practice is:
In molar ratio 1: 0.7-2.5 is weighing magnesium powder and boron powder respectively; Press the total mass of magnesium powder and boron powder and the mass ratio 1 of hotchpotch again: 0.01-1 weighing hotchpotch, hotchpotch are a kind of in citric acid or the Citrate trianion; The powder of magnesium powder, boron powder and hotchpotch is uniformly mixed into mixed powder, carries out sintering then under argon gas atmosphere protection, the agglomerating temperature is 600 ℃-1200 ℃, soaking time 0.5-12 hour, promptly.
2, a kind of method for preparing magnesium diboride super conductive material as claimed in claim 1, it is characterized in that: the concrete practice that described powder with magnesium powder, boron powder and hotchpotch is uniformly mixed into mixed powder is: hotchpotch is dissolved in forms hotchpotch solution in the solvent earlier, solvent is a kind of in alcohol, acetone, benzene, toluene or the water; Thorough mixing in the boron powder adding hotchpotch solution is become suspension liquid, will add the magnesium powder after the suspension liquid vacuum-drying again, and uniform mixing is a mixed powder.
3, the preparation method of a kind of magnesium diboride super conductive material as claimed in claim 2 is characterized in that: describedly the boron powder is added thorough mixing becomes the concrete practice of suspension liquid to be in the hotchpotch solution: adopt ultrasonic blended method.
4, the preparation method of a kind of magnesium diboride super conductive material as claimed in claim 1 or 2 is characterized in that: will carry out sintering behind the described mixed powder tablet forming again.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101814344A (en) * | 2010-03-10 | 2010-08-25 | 中国科学院电工研究所 | Method for preparing iron-based superconductor |
| CN101462881B (en) | 2009-01-05 | 2011-12-21 | 西南交通大学 | Preparation of magnesium boride doped superconduction material |
| CN106205861A (en) * | 2016-06-29 | 2016-12-07 | 西北有色金属研究院 | A kind of preparation method of graphene-supported multi-element doping magnesium diboride superconductive bulk |
| CN107244921A (en) * | 2017-05-16 | 2017-10-13 | 天津大学 | The method of the first position sintering of copper addition activation magnesium diboride superconductive block |
| CN110229005A (en) * | 2019-07-16 | 2019-09-13 | 史玉成 | A kind of superconduction new material and preparation method thereof |
| CN112408988A (en) * | 2020-11-25 | 2021-02-26 | 郑州华晶实业有限公司 | High-temperature high-pressure preparation method of superconducting material magnesium diboride |
-
2008
- 2008-05-28 CN CNA2008100444670A patent/CN101279741A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101462881B (en) | 2009-01-05 | 2011-12-21 | 西南交通大学 | Preparation of magnesium boride doped superconduction material |
| CN101814344A (en) * | 2010-03-10 | 2010-08-25 | 中国科学院电工研究所 | Method for preparing iron-based superconductor |
| CN106205861A (en) * | 2016-06-29 | 2016-12-07 | 西北有色金属研究院 | A kind of preparation method of graphene-supported multi-element doping magnesium diboride superconductive bulk |
| CN106205861B (en) * | 2016-06-29 | 2017-05-10 | 西北有色金属研究院 | Preparation method for graphene-loaded multielement-doped magnesium diboride superconducting bulk material |
| CN107244921A (en) * | 2017-05-16 | 2017-10-13 | 天津大学 | The method of the first position sintering of copper addition activation magnesium diboride superconductive block |
| CN110229005A (en) * | 2019-07-16 | 2019-09-13 | 史玉成 | A kind of superconduction new material and preparation method thereof |
| CN111943681A (en) * | 2019-07-16 | 2020-11-17 | 史玉成 | Method for preparing novel superconducting material |
| CN111978086A (en) * | 2019-07-16 | 2020-11-24 | 史玉成 | Preparation method of novel superconducting material |
| CN111943681B (en) * | 2019-07-16 | 2022-07-22 | 苏州鱼得水电气科技有限公司 | Method for preparing novel superconducting material |
| CN112408988A (en) * | 2020-11-25 | 2021-02-26 | 郑州华晶实业有限公司 | High-temperature high-pressure preparation method of superconducting material magnesium diboride |
| 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 |
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Open date: 20081008 |