CN111943681B - Method for preparing novel superconducting material - Google Patents
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- CN111943681B CN111943681B CN202010651633.4A CN202010651633A CN111943681B CN 111943681 B CN111943681 B CN 111943681B CN 202010651633 A CN202010651633 A CN 202010651633A CN 111943681 B CN111943681 B CN 111943681B
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Abstract
The invention discloses a method for preparing a novel superconducting material, which is prepared from boron powder, magnesium powder and an organic dopant, wherein the organic dopant is uniformly mixed with the magnesium powder and the boron powder, the organic dopant is decomposed into dopants such as carbon, hydrogen, oxygen, metal ions and compounds thereof after being sintered at a certain temperature and is uniformly dispersed in the magnesium diboride superconducting material, and the organic dopant is decomposed to generate a carbon source in the temperature rise process of sintering, can be directly doped into magnesium diboride crystal lattices and is more uniformly doped into MgB2Thereby significantly increasing MgB2Critical current density at high magnetic field while MgB2Metal boride is dispersed in the base superconductor to change MgB2The crystal structure of the superconductor is simultaneously introduced with second phase particles as effective pinning centers, so that the obtained MgB2The base superconductor has a high critical current density; the preparation method is simple, is convenient for large-scale production, and has wide application prospect.
Description
Technical Field
The invention relates to the technical field of superconducting materials, in particular to a preparation method of a novel superconducting material.
Background
Superconduction is one of the wonderful phenomena in the physical world, the resistance of a general superconducting alloy is reduced to zero when the temperature is close to absolute zero, and the resistance of the high-temperature superconducting alloy is suddenly reduced to zero at a certain relatively high critical temperature, so that the superconducting alloy has completely different physical mechanisms and wider application prospects. In 1986, physicists discovered copper oxide high temperature superconductors, and this work gained the Nobel prize in the next year. Since then, scientists have never stopped exploring new high temperature superconducting materials, and while continuing to pursue higher critical temperatures, physicists have been trying to reveal the mechanisms therein. Currently, research institutions are engaged in high temperature superconduction in almost all developed countries of the world. On the one hand, the exploration of the high-temperature superconducting mechanism attracts the attention of numerous physicists; on the other hand, due to energy and other special requirements, the industry holds great promise for superconducting technology, but the critical temperature of general superconducting alloy is close to absolute zero, so that the application is seriously hindered due to refrigeration, and high-temperature superconducting is one of the expected future exits.
MgB2Is the metal with the highest critical transition temperature at presentThe critical transition temperature (39-40K) of the meta-compound superconducting material is higher than that of Nb which is practically used at present3And superconductive materials such as Sn and NbTi. Higher transition temperature, larger coherence length, higher upper critical field, no weak connection of grain boundary, simple structure, low cost and the like2Becomes the most powerful competitor for materials used in the temperature range of 20-30K. MgB, particularly in low field applications, such as in MRI magnet applications2The method has great advantages, and data show that MgB2The practicability of the MgB can bring billions of economic benefits, and the MgB can work under the refrigeration condition of a refrigerator2The application of the magnetic resonance imaging device can greatly promote the popularization of the magnetic resonance imaging device, and has very important significance for improving the medical level of people in vast villages in China. However pure MgB2The critical current density (Jc) of the superconducting material is rapidly reduced along with the increase of an external magnetic field, and the problem greatly hinders MgB2The use of superconductors in practice. The research shows that the MgB is treated2Doping modification is carried out, defects are artificially introduced into the superconductor and pinning centers are formed, the movement of magnetic flux lines is prevented, and MgB can be effectively improved2The high field performance of the superconductor improves the critical current density under the high field.
At present, the substances used for doping are mainly: nanoscale metal simple substance particles such as Ti, Zr, Zn, Cu and the like; nanoscale intermetallic compounds, e.g. Ho2O3、ZrSi、ZrB2And Si3N4Etc.; nano-sized elemental carbon and carbide particles, e.g. diamond particles, SiC, B4C, TiC and the like. Researches show that the MgB can be better improved by nano-scale particles than by micro-scale particles2The critical current density of superconductors is therefore widely used in the laboratory development phase. However, the nano-scale particles are expensive, greatly increase the manufacturing cost in the large-scale production of factories, and cannot meet the requirement of industrial production.
Disclosure of Invention
The invention aims to provide a novel superconducting material and a preparation method thereof, which are used for solving the problems in the prior art.
In order to achieve the purpose, the invention provides the following technical scheme:
the novel superconducting material is prepared from boron powder, magnesium powder and an organic dopant, wherein the mass ratio of the boron powder to the magnesium powder to the organic dopant is 2:1: 0.01-0.1.
Preferably, the organic dopant is any one of titanium acrylate, zirconium acrylate, tungsten acrylate, holmium acrylate or molybdenum acrylate; the organic dopant used in the invention is a common chemical raw material, has low price, no toxicity, no harm and convenient preparation, and the carbon materials of the existing dopant nanoparticles, such as nano diamond, nano carbon and the like, have expensive price, complex preparation process and are not suitable for large-scale industrial production.
A preparation method of a novel superconducting material comprises the following steps:
(1) preparing pretreated magnesium powder;
(2) preparing primary mixed powder;
(3) preparing a block sheet blank;
(4) and (4) sintering the block-sheet blank prepared in the step (3) to obtain the novel superconducting material.
As optimization, the preparation method of the novel superconducting material is characterized by comprising the following steps of:
(1) spreading magnesium powder in a quartz boat, putting the quartz boat in a tubular furnace, introducing a mixed gas of hydrogen and argon, heating, preserving heat and cooling to obtain pretreated magnesium powder;
(2) dissolving an organic dopant in an organic solvent to form an organic dopant solution, adding boron powder into the organic dopant solution, mixing to form a suspension, and drying the suspension to obtain primary mixed powder;
(3) placing the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box, sealing the vacuum ball milling tank, taking out the sealed vacuum ball milling tank, placing the sealed vacuum ball milling tank into a high-energy ball mill for high-energy ball milling treatment, and performing compression molding to obtain a block-sheet blank;
(4) and (4) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tube furnace, introducing a mixed gas of hydrogen and argon, carrying out a sintering reaction, and cooling to obtain a novel superconducting material.
As optimization, the preparation method of the novel superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a mixed boat which is formed by introducing hydrogen and argon into a quartz tube furnace, putting the quartz boat into the tube furnace, mixing gas, preserving the temperature for 3-5h at the temperature of 200-250 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder; the invention generates magnesium powder containing hydrogen and trace magnesium hydride through the physical and chemical action of hydrogen and magnesium powder, achieves the aim of refining magnesium powder, greatly reduces the activation energy in the reaction and reduces the synthesis difficulty;
(2) dissolving an organic dopant in an organic solvent with the weight 5-10 times that of the organic dopant to form an organic dopant solution, adding boron powder into the organic dopant solution, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 60-80 ℃ for 3-5 hours to obtain primary mixed powder; dissolving an organic dopant in an organic solvent, adopting an ultrasonic mixing method to enable the organic dopant and boron powder to be mixed more uniformly, carrying out vacuum drying to enable a chemical solvent to be evaporated, enabling the precipitated organic dopant to uniformly wrap the boron powder, enabling the organic dopant to be uniformly dispersed in the boron powder raw material, avoiding the phenomena of agglomeration and local excess of the organic dopant, and further improving the critical superconducting current of a novel superconducting material;
(3) placing the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box filled with inert gas, sealing the vacuum ball milling tank, taking out the sealed vacuum ball milling tank, placing the sealed vacuum ball milling tank into a high-energy ball mill, carrying out high-energy ball milling treatment for 5-10h at the rotation speed of 2000-3000r/min, and then carrying out compression molding by using a mold at the compression pressure of 8-10MPa to obtain a block-sheet blank; according to the invention, the boron powder, the organic dopant and the magnesium powder are subjected to high-energy ball milling treatment in a short time by using the high-energy ball mill, so that the solid solution of the organic dopant, Mg and B is obtained while the original particle sizes of the organic dopant, the boron powder and the magnesium powder are reduced, and the organic dopant, the boron powder and the magnesium powder are mixed at an atomic level, so that the method has the advantages of low energy consumption, short process flow, strong repeatability and the like; compared with the traditional method for preparing the superconducting material by planetary ball milling auxiliary sintering, the process for carrying out high-energy ball milling treatment by adopting the high-energy ball mill greatly shortens the time required by ball milling (the planetary ball milling needs more than 20 hours), avoids the defect that boron powder and magnesium powder are oxidized possibly due to long-time ball milling, reduces the energy consumption, and is more uniform in distribution of organic dopants, the boron powder and the magnesium powder after the high-energy ball milling treatment, thereby being suitable for industrial large-scale production;
(4) and (4) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, preserving the heat for 10-15h at 1400-1600 ℃ for sintering reaction, and naturally cooling to room temperature to obtain the novel superconducting material.
As optimization, the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon in the step (1) and the step (4) are respectively 5-99% and 1-95%.
Preferably, the organic solvent in step (2) is any one of methanol, acetone, dichloromethane, cyclohexane or ethyl acetate.
As optimization, the density of the ball milling tank in the step (3) is 8-15g/cm3(ii) a The invention utilizes the high-density ball milling tank to increase the instantaneous impact force of ball milling, can effectively refine organic dopants, boron powder and magnesium powder, provides activation energy for reaction and leads MgB to be2The synthesis is easier and the crystal grains are fine; simultaneously violent collision can peel off and refine B on the surfaces of the boron powder and the magnesium powder2O3MgO, etc., in which the refined second phase is dispersed throughout the MgB2Can be well used as a pinning center in a superconductor to improve the MgB content of the superconductor2Critical current density of (1).
Compared with the prior art, the invention has the beneficial effects that:
the invention relates to a novel superconducting material and a preparation method thereofUniformly mixing an organic dopant with magnesium powder and boron powder, and after sintering at a certain temperature, decomposing the organic dopant into dopants such as carbon, hydrogen, oxygen, metal ions and compounds thereof, and uniformly dispersing the dopants in the magnesium diboride superconducting material; the carbon source in the organic dopant is decomposed to generate the carbon source in the temperature rise process of sintering, and the carbon source has stronger chemical activity with the carbon powder directly used as the doping carbon source, and can be directly doped into the magnesium diboride crystal lattice, so that carbon atoms can be more uniformly doped into MgB2In the crystal lattice of (2), MgB is formed2Twisting of the crystal lattice of (1), reinforcing MgB2Impurity scattering between energy bands and increasing MgB2Thereby obviously improving MgB2Critical current density at high magnetic field while MgB2Metal boride is dispersed in the superconductor to change MgB2The crystal structure of the superconductor is based, and second phase particles are introduced to be used as effective pinning centers, so that the obtained MgB2The base superconductor has a high critical current density in a background magnetic field of 3 Tesla or more;
the invention produces magnesium powder containing hydrogen and trace magnesium hydride compound through the physical and chemical action of hydrogen and magnesium powder, thus achieving the purpose of thinning the magnesium powder, greatly reducing the activation energy in the reaction and reducing the synthesis difficulty;
dissolving an organic dopant in an organic solvent, adopting an ultrasonic mixing method to uniformly mix the organic dopant and boron powder, evaporating a chemical solvent by vacuum drying, and uniformly wrapping the boron powder with the separated organic dopant, so that the organic dopant can be uniformly dispersed in the boron powder raw material, the organic dopant cannot generate the phenomena of agglomeration and local excess, and the critical superconducting current of the novel superconducting material is further improved;
the invention relates to a novel superconducting material and a preparation method thereof, and the novel superconducting material is characterized in that a high-energy ball mill is used for carrying out high-energy ball milling treatment on boron powder, organic dopant and magnesium powder in a short time, so that solid solution of the organic dopant, Mg and B is obtained while the original particle sizes of the organic dopant, the boron powder and the magnesium powder are reduced, the organic dopant, the boron powder and the magnesium powder are mixed at an atomic level, and the novel superconducting material has the advantages of low energy consumption, short process flow, strong repeatability and the like; compared with the traditional method for preparing the superconducting material by planetary ball milling auxiliary sintering, the process for carrying out high-energy ball milling treatment by adopting the high-energy ball mill greatly shortens the time required by ball milling (the planetary ball milling needs more than 20 hours), avoids the defect that boron powder and magnesium powder are oxidized possibly due to long-time ball milling, reduces the energy consumption, and is more uniform in distribution of organic dopants, the boron powder and the magnesium powder after the high-energy ball milling treatment, thereby being suitable for industrial large-scale production;
the invention uses a general tube furnace to effectively reduce the cost, simplify the preparation process, avoid introducing other impurities, have small influence on the performance of the prepared material due to the change of different preparation process parameters, meet the requirements of industrial production, facilitate large-scale production and have wide application prospect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the novel superconducting material is prepared from boron powder, magnesium powder and titanium acrylate, wherein the mass ratio of the boron powder to the magnesium powder to the titanium acrylate is 2:1: 0.01.
The new superconducting material is prepared from the raw materials, and the preparation method of the new superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat in a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 5 percent and 95 percent respectively, preserving heat for 3-5 hours at 200 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) dissolving titanium acrylate in methanol with the weight 5 times that of the titanium acrylate to form a methanol solution of the titanium acrylate, adding boron powder into the methanol solution of the titanium acrylate, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 60 ℃ for 3-5 hours to obtain primary mixed powder;
(3) putting the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 8g/cm3Sealing the vacuum ball milling tank, taking out the vacuum ball milling tank, placing the vacuum ball milling tank in a high-energy ball mill, carrying out high-energy ball milling treatment for 5 hours at the rotating speed of 2000r/min, and then carrying out compression molding by using a mold, wherein the compression pressure is 8MPa, so as to obtain a block-sheet blank;
(4) and (4) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 5% and 95%, preserving the temperature for 10 hours at 1400 ℃ for sintering reaction, and naturally cooling to room temperature to obtain the novel superconducting material.
Example 2:
the novel superconducting material is prepared from boron powder, magnesium powder and zirconium acrylate, wherein the mass ratio of the boron powder to the magnesium powder to the zirconium acrylate is 2:1: 0.02.
The novel superconducting material is prepared by adopting the raw materials, and the preparation method of the novel superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat into a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 20 percent and 80 percent respectively, preserving heat for 3.5 hours at 210 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) dissolving zirconium acrylate in acetone with the weight 6 times that of the zirconium acrylate to form an acetone solution of the zirconium acrylate, adding boron powder into the acetone solution of the zirconium acrylate, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 65 ℃ for 3.5 hours to obtain primary mixed powder;
(3) putting the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 9g/cm3Sealing the vacuum ball milling tank, taking out the vacuum ball milling tank, placing the vacuum ball milling tank in a high-energy ball mill, carrying out high-energy ball milling treatment for 6 hours at the rotating speed of 2200r/min, and then carrying out compression molding by using a mold, wherein the compression pressure is 8.5MPa, so as to obtain a block-sheet blank;
(4) and (4) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 20 percent and 80 percent respectively, preserving heat at 1450 ℃ for 11 hours to carry out a sintering reaction, and naturally cooling to room temperature to obtain the novel superconducting material.
Example 3:
the novel superconducting material is prepared from boron powder, magnesium powder and tungsten acrylate, wherein the mass ratio of the boron powder to the magnesium powder to the tungsten acrylate is 2:1: 0.05.
The new superconducting material is prepared from the raw materials, and the preparation method of the new superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat into a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 50 percent and 50 percent respectively, preserving heat for 4 hours at 225 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) dissolving tungsten acrylate in dichloromethane 7.5 times of the weight of the tungsten acrylate to form a dichloromethane solution of the tungsten acrylate, adding boron powder into the dichloromethane solution of the tungsten acrylate, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 70 ℃ for 4 hours to obtain primary mixed powder;
(3) putting the pretreated magnesium powder prepared in the step (1) and the pretreated magnesium powder prepared in the step (2) into a glove box filled with inert gasThe prepared primary mixed powder is placed in a vacuum ball milling tank, and the density of the ball milling tank is 11.5g/cm3Sealing the vacuum ball milling tank, taking out the vacuum ball milling tank, placing the vacuum ball milling tank in a high-energy ball mill, carrying out high-energy ball milling treatment for 7.5 hours at the rotating speed of 2500r/min, and then carrying out compression molding by using a mold, wherein the compression pressure is 9MPa, so as to obtain a block-sheet blank;
(4) and (4) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 50% and 50%, preserving the temperature at 1500 ℃ for 12.5h for sintering reaction, and naturally cooling to room temperature to obtain the novel superconducting material.
Example 4:
the novel superconducting material is prepared from boron powder, magnesium powder and holmium acrylate, wherein the mass ratio of the boron powder to the magnesium powder to the holmium acrylate is 2:1: 0.09.
The novel superconducting material is prepared by adopting the raw materials, and the preparation method of the novel superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat in a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 80% and 20%, preserving heat for 4.5h at 240 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) dissolving holmium acrylate in cyclohexane with the weight 9 times that of holmium acrylate to form a cyclohexane solution of holmium acrylate, adding boron powder into the cyclohexane solution of holmium acrylate, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 75 ℃ for 4.5 hours to obtain primary mixed powder;
(3) putting the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 14g/cm3Sealing the vacuum ball milling tank, taking out, placing in a high-energy ball mill, performing high-energy ball milling treatment at 2800r/min for 9h, and usingPressing and molding by using a mold, wherein the pressing pressure is 9.5MPa, and obtaining a block-sheet blank;
(4) and (4) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 80 percent and 20 percent respectively, preserving heat at 1550 ℃ for 14 hours to carry out sintering reaction, and naturally cooling to room temperature to obtain the novel superconducting material.
Example 5:
the novel superconducting material is prepared from boron powder, magnesium powder and molybdenum acrylate, wherein the mass ratio of the boron powder to the magnesium powder to the molybdenum acrylate is 2:1: 0.1.
The novel superconducting material is prepared by adopting the raw materials, and the preparation method of the novel superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat in a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 99 percent and 1 percent, preserving heat for 3-5 hours at 250 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) dissolving molybdenum acrylate in ethyl acetate which is 10 times of the weight of the molybdenum acrylate to form an ethyl acetate solution of the molybdenum acrylate, adding boron powder into an organic dopant solution, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 80 ℃ for 5 hours to obtain primary mixed powder;
(3) putting the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 15g/cm3Sealing the vacuum ball milling tank, taking out the vacuum ball milling tank, placing the vacuum ball milling tank in a high-energy ball mill, performing high-energy ball milling treatment for 10 hours at the rotating speed of 3000r/min, and then performing compression molding by using a mold at the compression pressure of 10MPa to obtain a block-sheet blank;
(4) and (3) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 99 percent and 1 percent respectively, preserving the heat at 1600 ℃ for 15 hours for sintering reaction, and naturally cooling to room temperature to obtain the novel superconducting material.
Comparative example 1:
the novel superconducting material is prepared from boron powder, magnesium powder and titanium acrylate, wherein the mass ratio of the boron powder to the magnesium powder to the titanium acrylate is 2:1: 0.01.
The novel superconducting material is prepared by adopting the raw materials, and the preparation method of the novel superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat in a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 5 percent and 95 percent respectively, preserving heat for 3-5 hours at 200 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) putting the pretreated magnesium powder, boron powder and titanium acrylate prepared in the step (1) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 8g/cm3Sealing the vacuum ball milling tank, taking out the vacuum ball milling tank, placing the vacuum ball milling tank in a high-energy ball mill, carrying out high-energy ball milling treatment for 5 hours at the rotating speed of 2000r/min, and then carrying out compression molding by using a mold, wherein the compression pressure is 8MPa, so as to obtain a block-sheet blank;
(3) and (3) putting the block-sheet blank prepared in the step (2) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 5% and 95%, preserving the temperature for 10 hours at 1400 ℃ for sintering reaction, and naturally cooling to room temperature to obtain the superconducting material.
Comparative example 1 compares with example 1 except that magnesium powder, boron powder and titanium acrylate are directly mixed to be subjected to high energy ball milling treatment.
Comparative example 2:
the novel superconducting material is prepared from boron powder, magnesium powder and tungsten acrylate, wherein the mass ratio of the boron powder to the magnesium powder to the tungsten acrylate is 2:1: 0.05.
The novel superconducting material is prepared by adopting the raw materials, and the preparation method of the novel superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat in a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 50% and 50%, preserving heat for 4 hours at 225 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) dissolving tungsten acrylate in dichloromethane 7.5 times of the weight of the tungsten acrylate to form a dichloromethane solution of the tungsten acrylate, adding boron powder into the dichloromethane solution of the tungsten acrylate, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 70 ℃ for 4 hours to obtain primary mixed powder;
(3) putting the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 3g/cm3Sealing the vacuum ball milling tank, taking out the vacuum ball milling tank, placing the vacuum ball milling tank in a high-energy ball mill, performing high-energy ball milling treatment for 7.5 hours at the rotating speed of 2500r/min, and then performing compression molding by using a mold at the compression pressure of 9MPa to obtain a block-sheet blank;
(4) and (3) putting the block and sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 50% and 50%, preserving the temperature at 1500 ℃ for 12.5h for sintering reaction, and naturally cooling to room temperature to obtain the superconducting material.
Comparative example 2 compared with example 3, except that the ball-milling jar in step (3) had a density of 3g/cm3。
Comparative example 3:
the novel superconducting material is prepared from boron powder and magnesium powder, wherein the mass ratio of the boron powder to the magnesium powder is 2: 1.
The novel superconducting material is prepared by adopting the raw materials, and the preparation method of the novel superconducting material comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat into a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 80% and 20%, preserving heat for 4.5h at 240 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) putting the pretreated magnesium powder and boron powder prepared in the step (1) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 14g/cm3Sealing the vacuum ball milling tank, taking out the vacuum ball milling tank, placing the vacuum ball milling tank in a high-energy ball mill, performing high-energy ball milling treatment for 9 hours at the rotation speed of 2800r/min, and then performing compression molding by using a mold, wherein the compression pressure is 9.5MPa, so as to obtain a block-sheet blank;
(3) and (3) putting the block and sheet blank prepared in the step (2) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 80% and 20%, preserving the heat at 1550 ℃ for 14h for a sintering reaction, and naturally cooling to room temperature to obtain the superconducting material.
Comparative example 3 compares to example 4 except that no holmium acrylate organic dopant was used in the feed.
The effect example:
experimental sample: novel superconducting materials obtained in examples 1 to 5 of the present invention and superconducting materials obtained in comparative examples 1 to 3.
The experimental method comprises the following steps: the critical current Ic of the experimental sample is measured by a standard four-lead method under 4.2K along with the change of the magnetic field, the criterion of quench is 1 mu V/cm, and the critical current density of the experimental sample is calculated according to the critical current Ic and the cross-sectional area of the MgB2 superconducting core, and the result is shown in Table 1.
TABLE 1
The experimental results are as follows: as can be seen from table 1, it is,the critical current density of the new superconducting material prepared in example 1 was 3079A/cm2Comparative example 1 the critical current density of the superconducting material was 171.4A/cm2The critical current density of the new superconducting material prepared in example 1 was 17.9 times that of the superconducting material prepared in comparative example 1; the critical current density of the new superconducting material prepared in example 3 was 3127A/cm2Comparative example 2 the superconducting material had a critical current density of 187.3A/cm2The critical current density of the new superconducting material prepared in example 3 was 16.6 times that of the superconducting material prepared in comparative example 2; the critical current density of the new superconducting material prepared in example 4 was 2974A/cm2Comparative example 3 the critical current density of the superconducting material was 82.6A/cm2The critical current density of the new superconducting material obtained in example 4 was 36.0 times that of the superconducting material obtained in comparative example 3, and the critical current density of the new superconducting material obtained in example 2 was 2998A/cm2The critical current density of the new superconducting material prepared in example 5 was 3087A/cm2。
Compared with the comparative example 1, in the embodiment 1, the organic dopant is dissolved in the organic solvent, the organic dopant and the boron powder are mixed more uniformly by adopting an ultrasonic mixing method, the chemical solvent is evaporated by vacuum drying, the precipitated organic dopant can uniformly wrap the boron powder, so that the organic dopant can be uniformly dispersed in the boron powder raw material, and the phenomenon of agglomeration and local excess of the organic dopant cannot be generated, so that the novel superconducting material prepared in the embodiment 1 has higher critical superconducting current.
Compared with the comparative example 2, in the embodiment 3, because the instantaneous impact force of ball milling is increased by the high-density ball milling tank, the organic dopant, the boron powder and the magnesium powder can be effectively refined, the activation energy is provided for the reaction, and the MgB is enabled to be2The synthesis is easier and the crystal grains are fine; simultaneously violent collision can peel off and refine B on the surfaces of the boron powder and the magnesium powder2O3MgO, etc., in which the refined second phase is dispersed throughout the MgB2Can be well used as a pinning center in a superconductor to improve the MgB content of the superconductor2The critical current density of (a) is,therefore, the new superconducting material prepared in example 3 has a higher critical current density.
Example 4 compared with comparative example 3, since the carbon source in the organic dopant is decomposed to generate the carbon source in the temperature rise process of sintering, the carbon source has stronger chemical activity and can be directly doped into the magnesium diboride crystal lattice, so that carbon atoms can be more uniformly doped into MgB2In the crystal lattice of (1), MgB is formed2Twisting of the crystal lattice of (1), reinforcing MgB2Impurity scattering between energy bands and increasing MgB2Thereby obviously improving MgB2Critical current density at high magnetic field while MgB2Metal boride is dispersed in the superconductor to change MgB2The second phase particles are introduced as effective pinning centers while the crystal structure of the superconductor is based, so that the new superconducting material prepared in example 4 has high critical current density.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Claims (1)
1. A method for preparing a novel superconducting material is characterized by comprising the following steps: the method comprises the following steps:
(1) uniformly spreading magnesium powder in a quartz boat, putting the quartz boat in a tube furnace, introducing a mixed gas of hydrogen and argon into the tube furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are respectively 99 percent and 1 percent, preserving heat for 3-5 hours at 250 ℃, and naturally cooling to room temperature to obtain pretreated magnesium powder;
(2) dissolving molybdenum acrylate in ethyl acetate which is 10 times of the weight of the molybdenum acrylate to form an ethyl acetate solution of the molybdenum acrylate, adding boron powder into the ethyl acetate solution of the molybdenum acrylate, ultrasonically mixing to form a suspension, and drying the suspension in a vacuum drying oven at 80 ℃ for 5 hours to obtain primary mixed powder;
(3) putting the pretreated magnesium powder prepared in the step (1) and the primary mixed powder prepared in the step (2) into a vacuum ball milling tank in a glove box filled with inert gas, wherein the density of the ball milling tank is 15g/cm3The mass ratio of the boron powder to the magnesium powder to the molybdenum acrylate is 2:1:0.1, the vacuum ball milling tank is sealed and then taken out, the vacuum ball milling tank is placed in a high-energy ball mill, high-energy ball milling treatment is carried out for 10 hours at the rotating speed of 3000r/min, then a mould is used for compression molding, the compression pressure is 10MPa, and a block-sheet blank is obtained;
(4) and (4) putting the block-sheet blank prepared in the step (3) into a quartz boat, putting the quartz boat into a tubular furnace, introducing a mixed gas of hydrogen and argon into the tubular furnace, wherein the volume percentages of the hydrogen and the argon in the mixed gas of the hydrogen and the argon are 99 percent and 1 percent respectively, preserving the temperature for 15 hours at 1600 ℃ for sintering reaction, and naturally cooling to room temperature to obtain the novel superconducting material.
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