CN102122549B - Application of glucose in preparation of magnesium diboride-doped superconducting material - Google Patents
Application of glucose in preparation of magnesium diboride-doped superconducting material Download PDFInfo
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Abstract
The invention provides application of glucose to preparation of a magnesium diboride-doped superconducting material, and relates to the technical field of preparation of high-temperature superconducting materials. The preparation method comprises the following steps of: weighing magnesium powder and boron powder in a molar ratio of 1:(2-2.1) respectively; weighing glucose based on the ratio of the total mass of the magnesium powder and the boron powder to mass of the glucose of 1:(0.03-0.1); uniformly mixing the magnesium powder, the boron powder and the glucose powder to form mixed powder; sintering the mixed powder under the protection of argon atmosphere at the temperature of between 800 and 900 DEG C; and preserving heat for 0.5 to 2 hours to obtain the magnesium diboride-doped superconducting material in which the glucose is used as a carbon source. In the magnesium diboride superconducting material prepared by the method, critical current density is obviously improved, and particularly, the critical current density in a high magnetic field is extremely high; and the application of the material in the high magnetic field is facilitated, and the material has high practicability.
Description
Technical field
The present invention relates to the high temperature superconducting materia preparing technical field.
Background technology
The calendar year 2001 discovery of magnesium diboride superconductivity has caused the very big interest of Condensed Matter Physics circle and superconduction industrial quarters, and the scientists and engineers of various countries carried out big quantity research to magnesium diboride super conductive material.Magnesium diboride is the twice of compound superconductive (Nb3Sn and Nb-Ti) between known binary metal 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 need not use complicated with expensive liquid helium refrigerating system, thereby make the commercial 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 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 external magnetic field decay, limited magnesium diboride super conductive material, had a strong impact on and used performance in fact in highfield environmental applications such as levitated superconducting magnet trains.Therefore, how to improve the emphasis that the critical current density of magnesium diboride super conductive material under the highfield becomes research.Many researchs all find can effectively improve through the nano-sized carbon doping upper critical field of mgb 2 superconductor; Thereby improve its current-carrying performance under the highfield; The carbon doping particle of nanometer scale can also improve the performance of mgb 2 superconductor as effective pinning center on the other hand.The existing method for preparing the nano-sized carbon magnesium boride doped superconduction material adopts solid reaction process, and it is with behind magnesium powder, boron powder and the nano-sized carbon powder mixed grinding, under the high temperature more than 900 ℃, carries out sintering.Because the existence of effects such as the reunion of the nano-scale carbon powder that mixes can't disperse the nano-sized carbon powder of doping 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 alloy, and unreacted alloy is deposited in the intergranule of sample, becomes the obstruction barrier of supercurrent, further influences superconductivity.The material with carbon element price of nano particle is higher on the other hand, the preparation difficulty, and the doping of solid-state carbon gets into MgB
2Lattice is difficulty relatively, needs higher reaction temperature and long reaction time, and these have all limited the preparation of the magnesium diboride super conductive material that mixes.
Summary of the invention
The object of the present invention is to provide the purposes of a kind of glucose in the preparation magnesium boride doped superconduction material; Utilize the magnesium boride doped superconduction material of glucose for the carbon source preparation; Critical current density is high; Especially the lower critical electric current is close very high in the highfield, helps its application under the highfield, and is practical.
The present invention realizes that the technical scheme that its goal of the invention adopts is: the purposes of a kind of glucose in the preparation magnesium boride doped superconduction material is that glucose is mixed as the superconductor of carbon source to magnesium diboride, and its concrete practice is:
In molar ratio 1: 2-2.1 is weighing magnesium powder, boron powder respectively, is 1 by the gross mass of magnesium powder, boron powder and the mass ratio of glucose again: 0.03-0.1 weighing glucose, and magnesium powder, boron powder and glucose evenly is mixed into mixed-powder;
With the mixed-powder tablet forming, under the argon gas atmosphere protection, carry out sintering again, 800 ℃-900 ℃ of sintering temperatures, temperature retention time 0.5-2 hour, promptly getting a kind of was the magnesium boride doped superconductor of carbon source with glucose.
Compared with prior art, the invention has the beneficial effects as follows:
One, glucose is evenly mixed with magnesium powder and boron powder as alloy, behind the uniform temperature sintering, breakdown of glucose is alloys such as carbon, hydrogen, oxygen and compound thereof, is dispersed in the magnesium diboride super conductive material.Because the lower temperature (150-200 ℃) of glucose when heating up issues estranged separating, again under 800 ℃-900 ℃ around knot, form the magnesium diboride super conductive material that mixes.Compare with existing solid phase reaction, make reaction temperature can be lower, the time is shorter, efficient is high.
Two, because the carbon source in the glucose is in the temperature-rise period of sintering, to decompose to generate carbon source; With directly do as the doping carbon source with carbon dust; Have stronger chemism, 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 ability interband improves MgB
2Upper critical field, thereby obviously improve MgB
2Critical current density under the highfield.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 alloy of the present invention is a glucose, is industrial chemicals commonly used and food interpolation product, and it is cheap, nontoxic and preparation is convenient.And the material with carbon element of existing alloy nano particle such as Nano diamond, nano-sized carbon etc. all price are expensive, complicated process of preparation and be inappropriate for commercial production in enormous quantities.
Four, with carrying out sintering behind the mixed-powder tablet forming again, but sintering goes out superconduction block material, directly is applied.
Experiment showed, the magnesium diboride super conductive material that utilizes after glucose mixes, in the 20K temperature, when adding the highfield of 3.5T, its critical current density can improve more than 390% than plain magnesium diboride super conductive material.
Above-mentioned is glucose to be dissolved in to form alloy solution in the acetone earlier with the mixed uniformly concrete practice of magnesium powder, boron powder and glucose; Again the boron powder is added in the alloy solution and fully be mixed into suspension-turbid liquid; With adding magnesium powder after the suspension-turbid liquid vacuumize, and evenly be mixed into mixed-powder.
Utilize chemical dissolution method that glucose is dissolved in this organic solvent of acetone; Vacuumize makes after the chemical solvent evaporation; The glucose of separating out is parcel boron powder evenly; Thereby alloy can be distributed in the boron powder raw material equably, and alloy can not produce the phenomenon of reunion, local excessive phenomenon, has further improved the critical supercurrent that makes thing.
The above-mentioned concrete practice with fully being mixed into suspension-turbid liquid in the boron powder adding alloy solution is: adopt ultrasonic method of mixing.Like this, can make alloy more even with mixing of boron powder.
Description of drawings
Fig. 1 is the X ray diffracting spectrum of the magnesium diboride superconduction block material of the embodiment of the invention one preparation.
Fig. 2 is the magnesium diboride superconduction block material of the embodiment of the invention one preparation and the critical current density curve of the magnesium diboride superconduction block material of the last doping of preparation under the same conditions.
Fig. 3 is the magnesium diboride superconduction block material of the embodiment of the invention two preparation and the critical current density curve of the magnesium diboride superconduction block material of the last doping of preparation under the same conditions.
Fig. 4 is the magnesium diboride superconduction block material of the embodiment of the invention three preparation and the critical current density curve of the magnesium diboride superconduction block material of the last doping of preparation under the same conditions.
The curve that " △ " constitutes among Fig. 2-4 is respectively the critical current density curve of the magnesium diboride superconduction block material of embodiment one, two, three preparations.The curve that " ■ " constitutes be last doping, other condition respectively with the critical current density curve of embodiment one, two, the three identical magnesium diboride superconduction block materials that prepare.Be labeled as the curve of 10K and 20k, its probe temperature is respectively 10K and 20k.
Below in conjunction with accompanying drawing and concrete execution mode the present invention is done further detailed explanation.
Embodiment
Embodiment one
A kind of embodiment of the present invention does, the purposes of a kind of glucose in the preparation magnesium boride doped superconduction material is that glucose is mixed as the superconductor of carbon source to magnesium diboride, and its concrete practice is:
Distinguished weighing magnesium powder, boron powder in 1: 2 in molar ratio, be 1: 0.03 weighing glucose by the gross mass of magnesium powder, boron powder and the mass ratio of glucose again, and magnesium powder, boron powder and glucose evenly are mixed into mixed-powder.
This example with the concrete practice that magnesium powder, boron powder and glucose evenly are mixed into mixed-powder is: glucose is dissolved in forms alloy solution in the acetone earlier; Again the boron powder is added in the alloy solution; Adopt ultrasonic method of mixing fully to be mixed into suspension-turbid liquid; With adding magnesium powder after the suspension-turbid liquid vacuumize, and evenly be mixed into mixed-powder.
With the mixed-powder tablet forming, under the argon gas atmosphere protection, carry out sintering again, 800 ℃ of sintering temperatures, temperature retention time 2 hours, promptly getting a kind of is the magnesium boride doped superconductor of carbon source with glucose.
Fig. 1 is the X ray diffracting spectrum of the magnesium diboride superconduction block material of this example preparation.Visible by Fig. 1, this routine prepared product is really for being the magnesium diboride super conductive material that is doped with carbon.
Fig. 2 be the magnesium diboride superconduction block material of this example preparation and under the same conditions the last doping of preparation the magnesium diboride superconduction block material the critical current density curve.The curve that " ■ " constitutes among Fig. 2 is the critical current density curve of the magnesium diboride superconduction block material of last doping.The curve that " △ " constitutes, the critical current density curve of the magnesium diboride superconduction block material for preparing for mixing with glucose.Be labeled as the curve of 10K and 20k, its probe temperature is respectively 10K and 20k.
Can find out by Fig. 2, the magnesium diboride superconduction block material that this example makes, at 10K, its critical current density can reach 17000A/cm under the 4T condition
2, compare with plain magnesium diboride superconduction block material and to have improved 140%, at 20K, under the 3.5T condition, the critical current density of the magnesium diboride superconduction block material that this example makes is 1400A/cm
2, compare with plain magnesium diboride superconduction block material and to have improved 170%.
Embodiment two
The purposes of a kind of glucose in the preparation magnesium boride doped superconduction material is that glucose is mixed as the superconductor of carbon source to magnesium diboride, and its concrete practice is:
1: 2.1 in molar ratio weighing magnesium powder and boron powder.Be 1: 0.05 weighing powdered glucose by the gross mass of magnesium powder and boron powder and the mass ratio of alloy again.And magnesium powder, boron powder and glucose evenly is mixed into mixed-powder.
This example with the concrete practice that magnesium powder, boron powder and glucose evenly are mixed into mixed-powder is: glucose is dissolved in forms alloy solution in the acetone earlier; Again the boron powder is added in the alloy solution; Adopt ultrasonic method of mixing fully to be mixed into suspension-turbid liquid; With adding magnesium powder after the suspension-turbid liquid vacuumize, and evenly be mixed into mixed-powder.
With the mixed-powder tablet forming, under the argon gas atmosphere protection, carry out sintering again, 900 ℃ of sintering temperatures, temperature retention time 0.5 hour, promptly getting a kind of is the magnesium boride doped superconductor of carbon source with glucose.
Fig. 3 be the magnesium diboride superconduction block material of this example preparation and under the same conditions the last doping of preparation the magnesium diboride superconduction block material the critical current density curve.The curve that " ■ " constitutes among Fig. 3 is the critical current density curve of the magnesium diboride superconduction block material of last doping.The curve that " △ " constitutes, the critical current density curve of the magnesium diboride superconduction block material for preparing for mixing with glucose; Be labeled as the curve of 10K and 20k, its probe temperature is respectively 10K and 20k.
Visible from Fig. 3, at 10K, its critical current density can reach 25000A/cm under the 4T condition
2Compare with plain magnesium diboride superconduction block material, its critical current density has improved 230%.At 20K, under the 3.5T condition, the critical current density of magnesium boride doped superconduction block material is 2300A/cm
2, improved 390% than plain magnesium diboride superconduction block material.
Embodiment three
The purposes of a kind of glucose in the preparation magnesium boride doped superconduction material is that glucose is mixed as the superconductor of carbon source to magnesium diboride, and its concrete practice is:
Distinguished weighing magnesium powder, boron powder in 1: 2.05 in molar ratio, be 1: 0.1 weighing glucose by the gross mass of magnesium powder, boron powder and the mass ratio of glucose again, and magnesium powder, boron powder and glucose directly are mixed into mixed-powder.
With the mixed-powder tablet forming, under the argon gas atmosphere protection, carry out sintering again, 870 ℃ of sintering temperatures, temperature retention time 1.7 hours, promptly getting a kind of is the magnesium boride doped superconductor of carbon source with glucose.
Fig. 4 be the magnesium diboride superconduction block material of this example preparation and under the same conditions the last doping of preparation the magnesium diboride superconduction block material the critical current density curve.The curve that " ■ " constitutes among Fig. 4 is the critical current density curve of the magnesium diboride superconduction block material of last doping.The curve that " △ " constitutes, the critical current density curve of the magnesium diboride superconduction block material for preparing for mixing with glucose.Be labeled as the curve of 10K and 20k, its probe temperature is respectively 10K and 20k.
Visible from Fig. 4, at 10K, its critical current density can reach 19940A/cm under the 4T condition
2Compare with plain magnesium diboride superconduction block material, its critical current density has improved 142%.At 20K, under the 3.5T condition, the critical current density of magnesium boride doped superconduction block material is 1390A/cm
2, improved 200% than plain magnesium diboride superconduction block material.
Claims (1)
1. the purposes of a glucose in the preparation magnesium boride doped superconduction material is that glucose is mixed as the superconductor of carbon source to magnesium diboride, and its concrete practice is:
In molar ratio 1: 2-2.1 is weighing magnesium powder, boron powder respectively; Be 1 by the gross mass of magnesium powder, boron powder and the mass ratio of glucose again: 0.03-0.1 weighing glucose after the weighing, is dissolved in formation alloy solution in the acetone with glucose; Again the boron powder is added in the alloy solution; Adopt ultrasonic method of mixing fully to be mixed into suspension-turbid liquid,, and evenly be mixed into mixed-powder adding magnesium powder after the suspension-turbid liquid vacuumize;
With the mixed-powder tablet forming, under the argon gas atmosphere protection, carry out sintering again, 800 ℃-900 ℃ of sintering temperatures, temperature retention time 0.5-2 hour, promptly getting a kind of was the magnesium boride doped superconductor of carbon source with glucose.
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