CN112927858B - New energy high-temperature superconducting material and preparation method thereof - Google Patents
New energy high-temperature superconducting material and preparation method thereof Download PDFInfo
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- CN112927858B CN112927858B CN202110101594.5A CN202110101594A CN112927858B CN 112927858 B CN112927858 B CN 112927858B CN 202110101594 A CN202110101594 A CN 202110101594A CN 112927858 B CN112927858 B CN 112927858B
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- H—ELECTRICITY
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- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B12/00—Superconductive or hyperconductive conductors, cables, or transmission lines
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Abstract
The invention discloses a new energy high-temperature superconducting material and a preparation method thereofThe method comprises Y 2 O 3 Powder, baCO 3 Powder, cuO powder, and surfactant. According to the preparation method of the new energy high-temperature superconducting material, the raw material powder is subjected to ball milling one by one and then mixed and ground, so that the particle size of the raw material powder is ensured to be uniform, in addition, after the raw material powder is mixed, a surfactant is added into the mixed raw material, the surface energy of the raw material powder particles is reduced, the problem that the raw material powder is easy to agglomerate after mixing is solved, the performance of a finished product of the superconducting material is further improved, the strip is annealed to ensure precipitation of a lead-rich phase, so that the strip obtains good inter-crystal connectivity, the current carrying performance of the strip is improved, the performance of the finished product of the superconducting material is further improved, and in addition, the adopted surfactant can enable the surface tension of the raw material powder to be lower, and the critical concentration to be smaller, so that the problem that the raw material powder is agglomerated after mixing can be well avoided.
Description
Technical Field
The invention relates to the technical field of superconducting materials, in particular to a new energy high-temperature superconducting material and a preparation method thereof.
Background
The high-temperature superconducting material is a superconducting material with high critical transition temperature (Tc) capable of working under the condition of liquid nitrogen temperature, and the superconducting technology is a technology with great development potential and great strategic significance in the 21 st century, has high current carrying capacity and low energy consumption, and can be widely applied to the fields of energy sources, national defense, traffic, medical treatment and the like. Because of the higher critical temperature of the high-temperature superconductor, and the low price of the liquid ammonia used for cooling the high-temperature superconductor, the high-temperature superconductor is convenient to operate, and is a new energy material with practical significance.
Reference to chinese patent publication No. CN105390209a proposes a high temperature superconducting material, the preparation method of which includes the following steps: (100) refining and reacting: boron powder and magnesium powder are mixed according to the mole ratio of 1: 1-1.2, putting the mixture into a wear-resistant ball milling tank, putting the ball milling tank into a high-temperature energy ball mill, and performing ball milling for 2-3 hours at the temperature of 150-500 ℃ under the protection of argon protective atmosphere; (200) second grinding: adding a small amount of boron oxide powder and metallic silver powder into the mixed powder, mixing and regrinding; (300) briquetting: then pouring the mixed powder after the second grinding into a mould under the atmosphere of argon gas to press into a block; (400) sintering: finally, the block is packaged in a quartz tube, vacuumized, sintered in the protection atmosphere of argon, the pressure range is 0.01-0.02 MPa, and sintered for 5-8 hours after the temperature is raised to 600-750 ℃ at the heating rate of 10 ℃/min;
according to the scheme, boron powder and magnesium powder are mixed and then put into a wear-resistant ball milling tank for ball milling treatment, so that after the treatment, the mixing uniformity of raw materials boron powder and magnesium powder is general, the particle sizes of the boron powder and magnesium powder are also uneven, the boron powder and magnesium powder after ball milling treatment are easy to agglomerate, the performance of a finished superconducting material is influenced, in addition, the final sintering process in the scheme is only one sintering treatment, so that the sintered material does not have superconducting performance, and in order to solve the problems, a new energy high-temperature superconducting material and a preparation method thereof are provided by a person skilled in the art.
Disclosure of Invention
(one) solving the technical problems
Aiming at the defects of the prior art, the invention provides a new energy high-temperature superconducting material and a preparation method thereof, which solve the problems that after the boron powder and the magnesium powder are mixed in a comparative scheme CN105390209A and then put into a wear-resistant ball milling tank together for ball milling treatment, the mixing uniformity of raw materials boron powder and magnesium powder is general, the particle sizes of the boron powder and the magnesium powder are also uneven, the boron powder and the magnesium powder after ball milling treatment are easy to agglomerate and influence the performance of a finished superconducting material, and in addition, the final sintering process in the scheme only has one sintering treatment, so that the sintered material does not have superconducting performance.
(II) technical scheme
In order to achieve the above purpose, the invention is realized by the following technical scheme: a new energy high-temperature superconducting material comprises Y 2 O 3 Powder, baCO 3 Powder, cuO powder, and surfactant;
the new energy high-temperature superconducting material is prepared by the following method:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, the temperature in the drying oven is set to be 200-260 ℃, and the temperature of Y is set to be equal to that of the powder 2 O 3 Powder, baCO 3 Drying powder and CuO powder for 30-45min, and weighing Y separately by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 260-480 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 45-60min, and ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1-2h to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 30-40 short wires with equal length and filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 810-835 ℃, preserving heat for 15-20h, cooling the annealing furnace to 775-790 ℃ and preserving heat for 20h, and finally cooling the strip to room temperature along with the annealing furnace;
and fifthly, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material.
Preferably, in step one, Y 2 O 3 Powder, baCO 3 Powder and CuO powderProportioning according to the molar ratio of Y to Ba to Cu=1:2:3, and calculating Y required for preparing the high-temperature superconducting material 2 O 3 Powder, baCO 3 The mass of the powder and the mass of the CuO powder are weighed by an electronic balance.
Preferably, in the second step, the surfactant is used in an amount of Y 2 O 3 Powder, baCO 3 15% of the total mass of powder and CuO powder.
Preferably, in step three, the mill rolls the multicore wire into a strip with a thickness of 0.3mm by 5 pass rolling.
Preferably, the surfactant is prepared by the following method:
selecting raw materials including fatty alcohol, maleic anhydride, concentrated sulfuric acid and toluene, placing a magnetite in a three-neck round bottom flask, fixing the three-neck flask in a magnetic stirring oil bath pot, connecting a condensing pipe and a liquid separating pipe on the flask, connecting the condensing pipe with a tap water faucet, connecting a U-shaped drying pipe on the condensing pipe, introducing the fatty alcohol, the maleic anhydride and the toluene into the three-neck flask together, turning on a stirring device, adding the concentrated sulfuric acid, turning on a tap water faucet, turning on a heating switch of the oil bath pot, setting the temperature to be 150 ℃, carrying out constant-temperature reaction for 5 hours, dropwise adding saturated sodium bicarbonate aqueous solution and excessive concentrated sulfuric acid into the three-neck flask after the reaction is finished, adjusting the pH value to be 7, using saturated sodium chloride solution to wash and extract the solution in the three-neck flask, taking supernatant, drying the supernatant with anhydrous sodium sulfate solid, filtering, and evaporating the solvent in the filtrate to obtain a basic body;
adding a basic body into a three-neck round bottom flask provided with a constant pressure dropping funnel, simultaneously adding hydrogen peroxide and toluene into the three-neck flask, plugging a plug of the three-neck flask, dropwise adding a saturated sodium hydroxide aqueous solution into the three-neck flask through the constant pressure dropping funnel, opening a magnetic stirring oil bath pot and a tap, setting the reaction temperature to be 70 ℃, stirring and reacting for 8 hours, filtering a reaction product, extracting with dichloromethane, taking a lower layer solution, adding anhydrous sodium sulfate solid, and drying to obtain an intermediate;
adding the intermediate into a three-neck round-bottom flask, adding a sodium bisulphite saturated aqueous solution, tetrabutylammonium bromide and methylene dichloride into the three-neck round-bottom flask, opening a magnetic stirring oil bath pot and a tap on a plug of the three-neck flask, setting the reaction temperature to 70 ℃, stirring and reacting for 5 hours, cleaning a reaction product by using saturated saline water, extracting by using methylene dichloride, taking a lower solution, adding anhydrous sodium sulfate for drying, and spin-drying filtrate after filtering to obtain a white waxy solid, namely the surfactant.
The preparation method of the new energy high-temperature superconducting material specifically comprises the following steps:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, the temperature in the drying oven is set to be 200-260 ℃, and the temperature of Y is set to be equal to that of the powder 2 O 3 Powder, baCO 3 Drying powder and CuO powder for 30-45min, and weighing Y separately by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 260-480 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 45-60min, and ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1-2h to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 30-40 short wires with equal length and filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 810-835 ℃, preserving heat for 15-20h, cooling the annealing furnace to 775-790 ℃ and preserving heat for 20h, and finally cooling the strip to room temperature along with the annealing furnace;
and fifthly, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material.
(III) beneficial effects
The invention provides a new energy high-temperature superconducting material and a preparation method thereof. Compared with the prior art, the method has the following beneficial effects:
(1) The preparation method of the new energy high-temperature superconducting material comprises the following steps of weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 260-480 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 45-60min, and ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1-2h to obtain precursor powder, and carrying out one-by-one treatment on the raw material powderThe ball milling treatment is carried out again, so that the particle size of the raw material powder is ensured to be uniform, in addition, after the raw material powder is mixed, the surfactant is added into the mixed raw material, and the surface energy of the raw material powder particles is reduced, thereby solving the problem that the raw material powder is easy to agglomerate after being mixed, and further improving the performance of the finished superconducting material.
(2) According to the new energy high-temperature superconducting material and the preparation method thereof, the strip is cut into a 10cm sample and is placed into an annealing furnace, meanwhile, mixed gas of argon and oxygen is introduced into the annealing furnace, the temperature in the annealing furnace is raised to 810-835 ℃, the temperature is kept for 15-20h, then the annealing furnace is cooled down to 775-790 ℃, the temperature is kept for 20h, finally the strip is cooled to room temperature along with the annealing furnace, precipitation of a lead-rich phase can be ensured by annealing the strip, so that good inter-crystal connectivity of the strip can be obtained, the current carrying performance of the strip is improved, and further, the performance of a finished product of the superconducting material is improved.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A new energy high-temperature superconducting material comprises Y 2 O 3 Powder, baCO 3 Powder, cuO powder, and surfactant;
the new energy high-temperature superconducting material is prepared by the following method:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, and the temperature inside the drying oven is setThe temperature is 200 ℃ and the temperature is equal to Y 2 O 3 Powder, baCO 3 Drying the powder and CuO powder for 30min, and weighing Y by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 260 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 45min, and then ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1h to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 30 short wires with equal length and filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and then rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 810 ℃, preserving heat for 15 hours, cooling the annealing furnace to 775 ℃, preserving heat for 20 hours, and finally cooling the strip to room temperature along with the annealing furnace;
and fifthly, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material.
Example 2
A new energy high-temperature superconducting material comprises Y 2 O 3 Powder, baCO 3 Powder, cuO powder, and surfactant;
the new energy high-temperature superconducting material is prepared by the following method:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, the temperature in the drying oven is set to 260 ℃, and the temperature of Y is set 2 O 3 Powder, baCO 3 Drying the powder and CuO powder for 45min, and weighing Y by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 480 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 60min, and then ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 2 hours to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 40 short wires with equal length and filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and then rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 835 ℃, preserving heat for 20 hours, cooling the annealing furnace to 790 ℃, preserving heat for 20 hours, and finally cooling the strip to room temperature along with the annealing furnace;
and fifthly, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material.
Example 3
A new energy high-temperature superconducting material comprises Y 2 O 3 Powder, baCO 3 Powder, cuO powder, and surfactant;
the new energy high-temperature superconducting material is prepared by the following method:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, the temperature in the drying oven is set to be 230 ℃, and the temperature of Y is set to be equal to 2 O 3 Powder, baCO 3 Drying the powder and CuO powder for 38min, and weighing Y by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 370 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 52min, and then ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1.5h to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 35 short wires with equal length, filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and then rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 825 ℃, preserving heat for 18h, cooling the annealing furnace to 880 ℃, preserving heat for 20h, and finally cooling the strip to room temperature along with the annealing furnace;
and fifthly, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material.
In step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are proportioned according to the molar ratio of Y to Ba to Cu=1 to 2 to 3, and Y is needed for preparing the high-temperature superconducting material by calculation 2 O 3 Powder, baCO 3 The mass of the powder and the mass of the CuO powder are weighed by an electronic balance.
In the second step, the usage amount of the surfactant is Y 2 O 3 Powder, baCO 3 15% of the total mass of powder and CuO powder.
In the third step, the rolling mill rolls the multi-core wire rod into a strip with the thickness of 0.3mm through 5-pass rolling.
The surfactant is prepared by the following method:
selecting raw materials including fatty alcohol, maleic anhydride, concentrated sulfuric acid and toluene, placing a magnetite in a three-neck round bottom flask, fixing the three-neck flask in a magnetic stirring oil bath pot, connecting a condensing pipe and a liquid separating pipe on the flask, connecting the condensing pipe with a tap water faucet, connecting a U-shaped drying pipe on the condensing pipe, introducing the fatty alcohol, the maleic anhydride and the toluene into the three-neck flask together, turning on a stirring device, adding the concentrated sulfuric acid, turning on a tap water faucet, turning on a heating switch of the oil bath pot, setting the temperature to be 150 ℃, carrying out constant-temperature reaction for 5 hours, dropwise adding saturated sodium bicarbonate aqueous solution and excessive concentrated sulfuric acid into the three-neck flask after the reaction is finished, adjusting the pH value to be 7, using saturated sodium chloride solution to wash and extract the solution in the three-neck flask, taking supernatant, drying the supernatant with anhydrous sodium sulfate solid, filtering, and evaporating the solvent in the filtrate to obtain a basic body;
adding a basic body into a three-neck round bottom flask provided with a constant pressure dropping funnel, simultaneously adding hydrogen peroxide and toluene into the three-neck flask, plugging a plug of the three-neck flask, dropwise adding a saturated sodium hydroxide aqueous solution into the three-neck flask through the constant pressure dropping funnel, opening a magnetic stirring oil bath pot and a tap, setting the reaction temperature to be 70 ℃, stirring and reacting for 8 hours, filtering a reaction product, extracting with dichloromethane, taking a lower layer solution, adding anhydrous sodium sulfate solid, and drying to obtain an intermediate;
adding the intermediate into a three-neck round-bottom flask, adding a sodium bisulphite saturated aqueous solution, tetrabutylammonium bromide and methylene dichloride into the three-neck round-bottom flask, opening a magnetic stirring oil bath pot and a tap on a plug of the three-neck flask, setting the reaction temperature to 70 ℃, stirring and reacting for 5 hours, cleaning a reaction product by using saturated saline water, extracting by using methylene dichloride, taking a lower solution, adding anhydrous sodium sulfate for drying, and spin-drying filtrate after filtering to obtain a white waxy solid, namely the surfactant.
The preparation method of the new energy high-temperature superconducting material specifically comprises the following steps:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, the temperature in the drying oven is set to be 200-260 ℃, and the temperature of Y is set to be equal to that of the powder 2 O 3 Powder, baCO 3 Drying powder and CuO powder for 30-45min, and weighing Y separately by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 260-480 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 45-60min, and ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1-2h to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 30-40 short wires with equal length and filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 810-835 ℃, preserving heat for 15-20h, cooling the annealing furnace to 775-790 ℃ and preserving heat for 20h, and finally cooling the strip to room temperature along with the annealing furnace;
and fifthly, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material.
And all that is not described in detail in this specification is well known to those skilled in the art.
Comparative example
The comparative example adopts a new energy high-temperature superconducting material in the market;
the new energy high temperature superconducting materials of examples 1 to 3 and comparative example were selected for critical temperature and critical current detection as shown in table 1:
TABLE 1
| Critical temperature/K | Critical current/kA | |
| Example 1 | 100 | 6.0 |
| Example 2 | 110 | 5.0 |
| Example 3 | 108 | 5.5 |
| Comparative example | 90 | 2.5 |
From the above results, the new energy high temperature superconducting material prepared by the invention has higher critical temperature and critical current, which are superior to the new energy high temperature superconducting material prepared by the comparative example.
It is noted that relational terms such as first and second, and the like are used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made therein without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A new energy high temperature superconducting material is characterized in that: comprising Y 2 O 3 Powder, baCO 3 Powder, cuO powder, and surfactant;
the new energy high-temperature superconducting material is prepared by the following method:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, and the drying oven is setThe internal temperature is 200-260 ℃, for Y 2 O 3 Powder, baCO 3 Drying powder and CuO powder for 30-45min, and weighing Y separately by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 260-480 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 45-60min, and ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1-2h to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 30-40 short wires with equal length and filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 810-835 ℃, preserving heat for 15-20h, cooling the annealing furnace to 775-790 ℃ and preserving heat for 20h, and finally cooling the strip to room temperature along with the annealing furnace;
step five, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material;
step three, rolling the multi-core wire rod into a strip with the thickness of 0.3mm by a rolling mill through 5-pass rolling;
the surfactant is prepared by the following method:
selecting raw materials including fatty alcohol, maleic anhydride, concentrated sulfuric acid and toluene, placing a magnetite in a three-neck round bottom flask, fixing the three-neck flask in a magnetic stirring oil bath pot, connecting a condensing pipe and a liquid separating pipe on the flask, connecting the condensing pipe with a tap water faucet, connecting a U-shaped drying pipe on the condensing pipe, introducing the fatty alcohol, the maleic anhydride and the toluene into the three-neck flask together, turning on a stirring device, adding the concentrated sulfuric acid, turning on a tap water faucet, turning on a heating switch of the oil bath pot, setting the temperature to be 150 ℃, carrying out constant-temperature reaction for 5 hours, dropwise adding saturated sodium bicarbonate aqueous solution and excessive concentrated sulfuric acid into the three-neck flask after the reaction is finished, adjusting the pH value to be 7, using saturated sodium chloride solution to wash and extract the solution in the three-neck flask, taking supernatant, drying the supernatant with anhydrous sodium sulfate solid, filtering, and evaporating the solvent in the filtrate to obtain a basic body;
adding a basic body into a three-neck round bottom flask provided with a constant pressure dropping funnel, simultaneously adding hydrogen peroxide and toluene into the three-neck flask, plugging a plug of the three-neck flask, dropwise adding a saturated sodium hydroxide aqueous solution into the three-neck flask through the constant pressure dropping funnel, opening a magnetic stirring oil bath pot and a tap, setting the reaction temperature to be 70 ℃, stirring and reacting for 8 hours, filtering a reaction product, extracting with dichloromethane, taking a lower layer solution, adding anhydrous sodium sulfate solid, and drying to obtain an intermediate;
adding the intermediate into a three-neck round-bottom flask, adding a sodium bisulphite saturated aqueous solution, tetrabutylammonium bromide and methylene dichloride into the three-neck round-bottom flask, opening a magnetic stirring oil bath pot and a tap on a plug of the three-neck flask, setting the reaction temperature to 70 ℃, stirring and reacting for 5 hours, cleaning a reaction product by using saturated saline water, extracting by using methylene dichloride, taking a lower solution, adding anhydrous sodium sulfate for drying, and spin-drying filtrate after filtering to obtain a white waxy solid, namely the surfactant.
2. The new energy high temperature superconducting material according to claim 1, wherein: in step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are proportioned according to the molar ratio of Y to Ba to Cu=1 to 2 to 3, and Y is needed for preparing the high-temperature superconducting material by calculation 2 O 3 Powder, baCO 3 The mass of the powder and the mass of the CuO powder are weighed by an electronic balance.
3. The new energy high temperature superconducting material according to claim 1, wherein: in the second step, the usage amount of the surfactant is Y 2 O 3 Powder, baCO 3 15% of the total mass of powder and CuO powder.
4. A preparation method of a new energy high-temperature superconducting material is characterized by comprising the following steps: the method specifically comprises the following steps:
step one, Y 2 O 3 Powder, baCO 3 The powder and CuO powder are put into three containers, then the containers are put into an electrothermal constant temperature drying oven, the temperature in the drying oven is set to be 200-260 ℃, and the temperature of Y is set to be equal to that of the powder 2 O 3 Powder, baCO 3 Drying powder and CuO powder for 30-45min, and weighing Y separately by electronic day 2 O 3 Powder, baCO 3 Powder, cuO powder for standby;
step two, weighing Y 2 O 3 Powder, baCO 3 Respectively placing powder and CuO powder into three wear-resistant ball milling tanks, sequentially placing the three ball milling tanks into a high-temperature ball mill, introducing argon into the high-temperature ball mill, simultaneously raising the temperature of the ball mill to 260-480 ℃, setting the grinding fineness of the ball mill to 300 meshes, and respectively carrying out grinding on Y 2 O 3 Powder, baCO 3 Ball milling the powder and CuO powder for 45-60min, and ball milling the ball milled Y 2 O 3 Powder, baCO 3 Adding the powder and CuO powder into an agate mortar, adding a surfactant into the agate mortar, and utilizing the agate mortar to make the Y 2 O 3 Powder, baCO 3 Uniformly mixing the powder and CuO powder, and for Y 2 O 3 Powder, baCO 3 Grinding the powder and CuO powder for 1-2h to obtain precursor powder;
step three, filling the obtained precursor powder into a silver tube with the diameter of 12mm, vacuum sealing the two ends of the silver tube, then processing the silver tube into a single-core wire with the diameter of 1.3mm through a drawing process, cutting the single-core wire into 30-40 short wires with equal length and filling the short wires into a silver alloy tube, vacuum sealing the two ends of the silver alloy tube, processing the silver alloy tube into a multi-core wire with the diameter of 1.5mm through the drawing process, and rolling the multi-core wire into a strip with the thickness of 0.3mm through a rolling mill;
cutting the strip into a 10cm sample, putting the 10cm sample into an annealing furnace, simultaneously introducing mixed gas of argon and oxygen into the annealing furnace, raising the temperature inside the annealing furnace to 810-835 ℃, preserving heat for 15-20h, cooling the annealing furnace to 775-790 ℃ and preserving heat for 20h, and finally cooling the strip to room temperature along with the annealing furnace;
and fifthly, placing the annealed strip in a crucible, then placing the crucible in a sintering furnace, setting a temperature controller to raise the temperature inside the sintering furnace to 935 ℃, keeping for 3 hours, cooling the sintering furnace to 500 ℃, keeping for 2 hours, finally cooling the crucible to room temperature along with the sintering furnace, and taking out the crucible to obtain the new energy high-temperature superconducting material.
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