CN115745595A - High-temperature electronic superconductor - Google Patents
High-temperature electronic superconductor Download PDFInfo
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- CN115745595A CN115745595A CN202211364886.9A CN202211364886A CN115745595A CN 115745595 A CN115745595 A CN 115745595A CN 202211364886 A CN202211364886 A CN 202211364886A CN 115745595 A CN115745595 A CN 115745595A
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- 239000002887 superconductor Substances 0.000 title claims abstract description 44
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 90
- 239000000843 powder Substances 0.000 claims abstract description 48
- 239000011787 zinc oxide Substances 0.000 claims abstract description 45
- 239000000463 material Substances 0.000 claims abstract description 40
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000004246 zinc acetate Substances 0.000 claims abstract description 23
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 19
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000002994 raw material Substances 0.000 claims abstract description 16
- 238000001354 calcination Methods 0.000 claims abstract description 15
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 14
- PQVSTLUFSYVLTO-UHFFFAOYSA-N ethyl n-ethoxycarbonylcarbamate Chemical compound CCOC(=O)NC(=O)OCC PQVSTLUFSYVLTO-UHFFFAOYSA-N 0.000 claims abstract description 12
- GLXDVVHUTZTUQK-UHFFFAOYSA-M lithium hydroxide monohydrate Substances [Li+].O.[OH-] GLXDVVHUTZTUQK-UHFFFAOYSA-M 0.000 claims abstract description 12
- 229940040692 lithium hydroxide monohydrate Drugs 0.000 claims abstract description 12
- 239000000443 aerosol Substances 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 10
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000005751 Copper oxide Substances 0.000 claims abstract description 9
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 9
- 229910000416 bismuth oxide Inorganic materials 0.000 claims abstract description 7
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 7
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- BDAGIHXWWSANSR-NJFSPNSNSA-N hydroxyformaldehyde Chemical compound O[14CH]=O BDAGIHXWWSANSR-NJFSPNSNSA-N 0.000 claims abstract description 7
- 229910000464 lead oxide Inorganic materials 0.000 claims abstract description 7
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000010791 quenching Methods 0.000 claims abstract description 7
- 229910000018 strontium carbonate Inorganic materials 0.000 claims abstract description 7
- 238000007599 discharging Methods 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 230000008020 evaporation Effects 0.000 claims abstract description 6
- 238000011049 filling Methods 0.000 claims abstract description 6
- 230000000171 quenching effect Effects 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 45
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 40
- 238000005245 sintering Methods 0.000 claims description 32
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 30
- 238000010438 heat treatment Methods 0.000 claims description 29
- 238000001816 cooling Methods 0.000 claims description 27
- 238000000889 atomisation Methods 0.000 claims description 21
- HZAXFHJVJLSVMW-UHFFFAOYSA-N 2-Aminoethan-1-ol Chemical compound NCCO HZAXFHJVJLSVMW-UHFFFAOYSA-N 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 229910052573 porcelain Inorganic materials 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 8
- 229910002804 graphite Inorganic materials 0.000 claims description 8
- 239000010439 graphite Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- 229910052786 argon Inorganic materials 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 4
- 230000032683 aging Effects 0.000 claims description 4
- 239000012159 carrier gas Substances 0.000 claims description 4
- 238000000605 extraction Methods 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 238000002791 soaking Methods 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 10
- 239000000919 ceramic Substances 0.000 abstract description 4
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 abstract description 4
- 238000000498 ball milling Methods 0.000 abstract description 2
- 230000003301 hydrolyzing effect Effects 0.000 abstract description 2
- 239000002585 base Substances 0.000 description 21
- 230000000052 comparative effect Effects 0.000 description 11
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical group [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 4
- 230000035882 stress Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 239000004964 aerogel Substances 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011859 microparticle Substances 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 230000004913 activation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 239000012300 argon atmosphere Substances 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 229920006351 engineering plastic Polymers 0.000 description 1
- 239000010419 fine particle Substances 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910000734 martensite Inorganic materials 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
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- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/453—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on zinc, tin, or bismuth oxides or solid solutions thereof with other oxides, e.g. zincates, stannates or bismuthates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- 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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- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
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- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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Abstract
The invention discloses a high-temperature electronic superconductor and a preparation method thereof. Firstly, ball milling bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide to prepare raw materials, pre-burning the raw materials in a tetragonal zirconia ceramic boat at high temperature by discharging plasma, and grinding the raw materials to obtain pre-burned powder; hydrolyzing zinc acetate, atomizing into aerosol micro-droplets, reacting with lithium hydroxide monohydrate to obtain a material, drying the material, pyrolyzing to obtain a zinc oxide precursor, preparing the zinc oxide precursor into zinc oxide gel by using a gel sol method, filling pre-sintered powder into the zinc oxide gel to obtain pre-modified zinc oxide gel, performing high-temperature evaporation treatment on the pre-modified zinc oxide gel to obtain a superconducting base material, calcining the superconducting base material at a high temperature, and quenching to obtain the high-temperature electronic superconductor. The high-temperature electronic superconductor prepared by the invention is applied to a servo motor in a lifting elevator, and can prevent the servo motor from being failed due to overhigh temperature while realizing superconductivity and wear resistance.
Description
Technical Field
The invention relates to the technical field of new materials, in particular to a high-temperature electronic superconductor.
Background
The superconducting material has zero resistance characteristic and Meissner effect at low temperature, is not greatly different from the conventional material at normal temperature, and shows zero resistance characteristic at low temperature. The high-temperature electronic superconductor prepared by the invention is applied to a servo motor in a lifting elevator, and when the high-temperature electronic superconductor operates, electrons in the high-temperature electronic superconductor can quickly transfer current to an engine with low loss, so that electric energy is converted into kinetic energy to push the elevator to operate; when the servo motor rotates, the pre-sintering powder is high in strength after being sintered twice, the strength of the agglomerated micro particles is overlapped, the wear resistance of the high-temperature electronic superconductor is improved due to the excessively high hardness, the abrasion of the motor to the high-temperature electronic superconductor is reduced, and heat generated by friction of the servo motor can be rapidly led out due to the ultra-high heat conductivity, so that the servo motor is prevented from being broken down due to the excessively high temperature.
Disclosure of Invention
The invention aims to provide a high-temperature electronic superconductor and a preparation method thereof, which are used for solving the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme: the preparation method of the high-temperature electronic superconductor is characterized in that the process flow for preparing the high-temperature electronic superconductor is as follows:
raw material preparation, pre-sintering powder preparation, zinc acetate preparation, material preparation, zinc oxide precursor preparation, zinc oxide gel preparation, modified zinc oxide gel preparation, superconducting base material preparation and finished product preparation.
Further, the preparation method of the high-temperature electronic superconductor mainly comprises the following specific steps:
(1) Uniformly mixing bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide according to a mass ratio of 4.7;
(2) Placing the raw material on a zirconia porcelain boat, placing the porcelain boat in a graphite mold, after placing the porcelain boat, still forming a gap between the periphery of the porcelain boat and the graphite mold, sintering by using SPS equipment under the mechanical pressure of 25 to 30MPa and the air pressure of 5 to 6Pa, wherein the sintering condition is 820 ℃, the heating rate from room temperature to 700 ℃ is 100 ℃/min, the heating rate from 700 to 820 ℃ is 20 ℃/min, the sintering time is 10 to 15min, and the heat preservation time is 10 to 15min; after sintering, releasing pressure, cooling along with the furnace, and grinding after cooling to obtain pre-sintered powder;
(3) Dissolving zinc acetate in absolute ethyl alcohol, heating to 50-60 ℃, and stirring at the speed of 200r/min until the zinc acetate is completely dissolved to obtain a zinc acetate solution; adding the zinc acetate solution into an atomization tank for atomization, raising the temperature to 350-370 ℃, raising the temperature for 30min, adjusting the flow rate of carrier gas to 4-5L/min, adopting a working frequency of 1.5-1.7 MHz for an atomization sheet, controlling the atomization working voltage to 20V and the atomization power to 30W, and discharging in an air extraction mode to obtain aerosol micro-droplets; dissolving lithium hydroxide monohydrate in absolute ethyl alcohol to obtain a lithium hydroxide solution; transferring the prepared aerosol micro-droplets into a reactor, dripping a lithium hydroxide solution into the reactor by using a constant-pressure feeding funnel, wherein the volume ratio of the lithium hydroxide solution to a zinc acetate solution is 1;
(4) Heating the material to 250 ℃, wherein the heating rate from room temperature to 200 ℃ is 50 ℃/min, the heating speed from 200 to 250 ℃ is 10 ℃/min, keeping the temperature for 30 to 60min, then cooling, wherein the cooling rate from 250 to 100 ℃ is 10 ℃/min, and then cooling to room temperature along with the furnace to obtain a zinc oxide precursor;
(5) Putting a zinc oxide precursor into a flask, adding ethylene glycol monomethyl ether to obtain a mixed solution, stirring for 30-40min at 60-70 ℃ by using a constant-temperature stirrer, then adding ethanolamine, continuously stirring for 1-2h to obtain a clear solution, and aging the clear solution at room temperature for 20-24h to obtain zinc oxide gel;
(6) Dispersing the pre-sintering powder in an ethanol solution to obtain a pre-sintering powder solution, adding vinyl triamine, uniformly mixing to obtain a curing liquid, pouring the curing liquid into a mold, soaking zinc oxide gel into the curing liquid, closing the mold, pressurizing the interior of the mold, filling the curing liquid under the action of pressure until the zinc oxide gel is saturated, and curing by hot air at 50 ℃ to obtain modified zinc oxide gel; wherein the mass ratio of the pre-sintered powder to the ethanol solution to the vinyl triamine is 1; the pressure is 2MPa;
(7) Putting the modified zinc oxide gel into a high-temperature forced air dryer to evaporate the modified zinc oxide gel at high temperature, raising the temperature to 130-150 ℃, drying for 1-2h, and naturally cooling to obtain a superconducting base material;
(8) Preheating a calcining furnace, simultaneously introducing argon to replace air in the calcining furnace, placing the superconducting base material in the calcining furnace for high-temperature calcination, and cooling along with the furnace to obtain a sintered base material; and (3) quenching the sintered base material by using alkali liquor, and naturally drying to obtain the high-temperature electronic superconductor.
Further, in the step (2), the particle size of the calcined powder after grinding is 500 to 800nm.
Further, in the step (3), the mass ratio of zinc acetate to absolute ethyl alcohol in the zinc acetate solution is 1; in the lithium hydroxide solution, the mass ratio of the lithium hydroxide monohydrate to the absolute ethyl alcohol is 1.
Further, in the step (5), the mass ratio of the zinc oxide precursor to ethylene glycol monomethyl ether to ethanolamine is 0.7.
Further, in the step (8), the preheating temperature is 600 ℃, and the heating rate is 50 ℃/min.
Further, in the step (8), the calcination temperature is 800 ℃, the heating rate is 50 ℃/min, and the sintering time is 1 to 2h.
Further, in the step (8), the alkali liquor is a sodium hydroxide solution with a mass fraction of 30%.
Further, the high-temperature electronic superconductor prepared by the preparation method of the high-temperature electronic superconductor comprises the following raw materials in parts by weight: 100 to 150 parts of pre-sintered powder, 70 to 80 parts of zinc oxide gel and 40 to 50 parts of superconducting base material; the pre-sintering powder is obtained by processing bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide; the zinc oxide gel is obtained by processing zinc acetate and lithium hydroxide monohydrate; the superconductor base material is obtained by processing zinc oxide gel.
Compared with the prior art, the invention has the following beneficial effects:
the method comprises the steps of ball-milling bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide to prepare raw materials, pre-burning the raw materials in a tetragonal zirconia ceramic boat at high temperature by discharging plasma, and grinding the raw materials to obtain pre-burnt powder; hydrolyzing zinc acetate, atomizing into aerosol micro-droplets through fog, reacting with lithium hydroxide monohydrate in a reactor, drying to obtain a material, pyrolyzing the material to obtain a zinc oxide precursor, preparing the zinc oxide precursor into zinc oxide gel by using a gel sol method, filling pre-sintering powder into the zinc oxide gel to obtain pre-modified zinc oxide gel, directly performing high-temperature evaporation treatment on the pre-modified zinc oxide gel to obtain a superconducting base material, calcining the superconducting base material at high temperature in an argon atmosphere, and quenching to obtain a high-temperature electronic superconductor; when the raw material is presintered in the zirconia ceramic boat at high temperature, current is introduced into the gap of the raw material powder and energy of high-temperature plasma is generated, at the moment, a tetragonal phase region in the tetragonal phase zirconia ceramic boat can form huge tensile stress with concentrated stress, and stress transfer is generated under high temperature and high pressure, so that the internal stress of the raw material powder is increased, the activation is carried out, and the molecular activity of the raw material powder is increased; the aerogel micro-droplets prepared by mist atomization are finer, and the prepared zinc oxide has higher crystal strength, so that the high-temperature electronic superconductor can resist high temperature when in service; the aerogel micro-droplets react with lithium hydroxide monohydrate, so that the generated product is filled in the aerosol; during pyrolysis, the gaseous product is evaporated, and the solid substance is generated and deposited at the bottom of the kettle; the pre-sintering powder is filled in the modified zinc oxide gel, is more fully doped with a zinc oxide precursor, and is self-agglomerated into tiny particles in the gel, so that the agglomeration phenomenon generated after zinc oxide is directly added into the pre-sintering powder is prevented, the gel is quickly shrunk and dehydrated through high-temperature evaporation, the pre-sintering powder is wrapped in the modified zinc oxide gel, and when the pre-sintering powder is limited, lead atoms replace part of zinc atoms in a superconducting base material, so that free zinc atoms are embedded into gaps of copper oxide lattices, the side faces assist the phase formation of a superconducting phase, and the superconducting performance of the superconductor is improved; on one hand, the argon environment protects the pre-sintered powder from reacting with the atmosphere during sintering, on the other hand, the argon can reduce the reactivity of the pre-sintered powder during sintering, prevent the generation of reaction impurities of the pre-sintered powder at high temperature, and quench to enable partial crystals in the pre-sintered powder to generate phase change, obtain a harder martensite structure, increase the hardness of the high-temperature electronic superconductor and simultaneously increase the wear resistance of the superconductor.
The prepared high-temperature electronic superconductor is applied to a servo motor in a lifting elevator, and when the high-temperature electronic superconductor operates, electrons in the high-temperature electronic superconductor can quickly transfer current to an engine with low loss, so that electric energy is converted into kinetic energy to push the elevator to operate; when the servo motor rotates, the pre-sintering powder is high in strength after being sintered twice, the strength of the agglomerated micro particles is overlapped, the wear resistance of the high-temperature electronic superconductor is improved due to the excessively high hardness, the abrasion of the motor to the high-temperature electronic superconductor is reduced, and heat generated by friction of the servo motor can be rapidly led out due to the ultra-high heat conductivity, so that the servo motor is prevented from being broken down due to the excessively high temperature.
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.
In order to more clearly illustrate the method provided by the present invention, the following examples are used to illustrate the method for testing each index of the high-temperature electronic superconductor manufactured in the following examples:
thermal conductivity: the thermal conductivity engineering plastics obtained in the examples 1 and 2 and the comparative examples 1 and 2 are subjected to a thermal conductivity test by using a transient plane heat source method ISO22007-2, wherein the higher the thermal conductivity coefficient is, the higher the thermal conductivity of the substance is.
Example 1
A high-temperature electronic superconductor mainly comprises the following components in parts by weight: 150 parts of pre-sintered powder, 80 parts of zinc oxide gel and 50 parts of superconducting base material.
A preparation method of a high-temperature electronic superconductor mainly comprises the following preparation steps:
(1) Uniformly mixing bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide according to a mass ratio of 4;
(2) Placing the raw material on a zirconia porcelain boat, placing the porcelain boat in a graphite mold, wherein gaps still exist between the periphery of the porcelain boat and the graphite mold after the porcelain boat is placed, sintering by adopting SPS equipment under the mechanical pressure of 30MPa and the air pressure of 6Pa, wherein the sintering condition is 820 ℃, the heating rate from room temperature to 700 ℃ is 100 ℃/min, the heating rate from 700 ℃ to 820 ℃ is 20 ℃/min, the sintering time is 15min, and the heat preservation time is 15min; after sintering, pressure is relieved and the sintered powder is cooled along with the furnace, grinding is carried out after cooling, and the particle size of the ground pre-sintered powder is 800nm, so that pre-sintered powder is obtained;
(3) Dissolving zinc acetate in absolute ethyl alcohol, wherein the mass ratio of the zinc acetate to the absolute ethyl alcohol is 1; adding the zinc acetate solution into an atomization tank for atomization, raising the temperature to 370 ℃, raising the temperature for 30min, adjusting the flow rate of carrier gas to 5L/min, adopting the working frequency of 1.7MHz for an atomization sheet, controlling the atomization working voltage to 20V and the atomization power to 30W, and discharging in an air extraction mode to obtain aerosol micro-droplets; dissolving lithium hydroxide monohydrate in absolute ethyl alcohol, wherein the mass ratio of the lithium hydroxide monohydrate to the absolute ethyl alcohol is 1; transferring the prepared aerosol micro-droplets into a reactor, dropwise adding a lithium hydroxide solution into the reactor by using a constant-pressure feeding funnel, wherein the volume ratio of the lithium hydroxide solution to a zinc acetate solution is 1;
(4) Heating the material to 250 ℃, wherein the heating rate from room temperature to 200 ℃ is 50 ℃/min, the heating rate from 200 to 250 ℃ is 10 ℃/min, keeping the temperature for 60min, then cooling, wherein the cooling rate from 250 to 100 ℃ is 10 ℃/min, and then cooling to room temperature along with the furnace to obtain a zinc oxide precursor;
(5) Putting a zinc oxide precursor into a flask, adding ethylene glycol monomethyl ether to obtain a mixed solution, stirring for 40min at 70 ℃ by using a constant-temperature stirrer, then adding ethanolamine, continuously stirring for 2h to obtain a clear solution, and aging the clear solution at room temperature for 24h to obtain zinc oxide gel, wherein the mass ratio of the zinc oxide precursor to the ethylene glycol monomethyl ether to the ethanolamine is 0.7;
(6) Dispersing presintering powder in an ethanol solution to obtain a presintering powder solution, adding vinyl triamine, uniformly mixing to obtain a curing liquid, pouring the curing liquid into a mold, soaking zinc oxide gel into the curing liquid, sealing the mold, pressurizing the interior of the mold, filling the curing liquid under the action of pressure until the zinc oxide gel is saturated, and curing with hot air at 50 ℃ to obtain modified zinc oxide gel; wherein the mass ratio of the pre-sintered powder to the ethanol solution to the vinyl triamine is 1; the pressure is 2MPa;
(7) Putting the modified zinc oxide gel into a high-temperature forced air dryer to evaporate the modified zinc oxide gel at high temperature, raising the temperature to 130-150 ℃, drying for 1-2h, and naturally cooling to obtain a superconducting base material;
(8) Preheating a calcining furnace, simultaneously introducing argon to replace air in the calcining furnace, wherein the preheating temperature is 600 ℃, the heating rate is 50 ℃/min, placing the superconducting base material in the calcining furnace for high-temperature calcination, the preheating temperature is 600 ℃, the heating rate is 50 ℃/min, and cooling along with the furnace to obtain a sintered base material; and (3) quenching the sintered base material by using a sodium hydroxide solution with the mass fraction of 30%, and naturally drying to obtain the high-temperature electronic superconductor.
Example 2
A high-temperature electronic superconductor mainly comprises the following components in parts by weight: 100 parts of pre-sintered powder, 70 parts of zinc oxide gel and 40 parts of superconducting base material.
A preparation method of a high-temperature electronic superconductor mainly comprises the following preparation steps:
(1) Uniformly mixing bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide according to a mass ratio of 4.7;
(2) Placing the raw material on a zirconia porcelain boat, placing the porcelain boat in a graphite mold, wherein gaps still exist between the periphery of the porcelain boat and the graphite mold after the porcelain boat is placed, sintering by adopting SPS equipment under the mechanical pressure of 25MPa and the air pressure of 5Pa, wherein the sintering condition is 820 ℃, the heating rate from room temperature to 700 ℃ is 100 ℃/min, the heating rate from 700 ℃ to 820 ℃ is 20 ℃/min, the sintering time is 10min, and the heat preservation time is 10min; after sintering, relieving pressure, cooling along with the furnace, grinding after cooling, wherein the particle size of the ground pre-sintered powder is 500nm to obtain pre-sintered powder;
(3) Dissolving zinc acetate in absolute ethyl alcohol, wherein the mass ratio of the zinc acetate to the absolute ethyl alcohol is 1; adding the zinc acetate solution into an atomization tank for atomization, raising the temperature to 350 ℃, raising the temperature for 30min, adjusting the flow rate of carrier gas to be 4L/min, adopting a working frequency of 1.5MHz for an atomization sheet, controlling the atomization working voltage to be 20V and the atomization power to be 30W, and discharging in an air extraction mode to obtain aerosol micro-droplets; dissolving lithium hydroxide monohydrate in absolute ethyl alcohol, wherein the mass ratio of the lithium hydroxide monohydrate to the absolute ethyl alcohol is 1; transferring the prepared aerosol micro-droplets into a reactor, dripping a lithium hydroxide solution into the reactor by using a constant-pressure feeding funnel, wherein the volume ratio of the lithium hydroxide solution to a zinc acetate solution is 1;
(4) Heating the material to 250 ℃, wherein the heating rate from room temperature to 200 ℃ is 50 ℃/min, the heating rate from 200 to 250 ℃ is 10 ℃/min, preserving heat for 30min, then cooling, wherein the cooling rate from 250 to 100 ℃ is 10 ℃/min, and then cooling to room temperature along with the furnace to obtain a zinc oxide precursor;
(5) Putting a zinc oxide precursor into a flask, adding ethylene glycol monomethyl ether to obtain a mixed solution, stirring for 30min at 60 ℃ by using a constant-temperature stirrer, then adding ethanolamine, continuously stirring for 1h to obtain a clear solution, and aging the clear solution at room temperature for 20h to obtain zinc oxide gel, wherein the mass ratio of the zinc oxide precursor to the ethylene glycol monomethyl ether to the ethanolamine is 0.7;
(6) Dispersing presintering powder in an ethanol solution to obtain a presintering powder solution, adding vinyl triamine, uniformly mixing to obtain a curing liquid, pouring the curing liquid into a mold, soaking zinc oxide gel into the curing liquid, sealing the mold, pressurizing the interior of the mold, filling the curing liquid under the action of pressure until the zinc oxide gel is saturated, and curing with hot air at 50 ℃ to obtain modified zinc oxide gel; wherein the mass ratio of the pre-sintered powder to the ethanol solution to the vinyl triamine is 1; the pressure is 2MPa;
(7) Putting the modified zinc oxide gel into a high-temperature forced air dryer to carry out high-temperature evaporation on the modified zinc oxide gel, raising the temperature to 130 ℃, drying for 1h, and naturally cooling to obtain a superconducting base material;
(8) Preheating a calcining furnace, simultaneously introducing argon to replace air in the calcining furnace, wherein the preheating temperature is 600 ℃, the heating rate is 50 ℃/min, placing the superconducting base material in the calcining furnace for high-temperature calcination, the preheating temperature is 600 ℃, the heating rate is 50 ℃/min, and cooling along with the furnace to obtain a sintered base material; and (3) quenching the sintered base material by using a sodium hydroxide solution with the mass fraction of 30%, and naturally drying to obtain the high-temperature electronic superconductor.
Comparative example 1
The formulation of comparative example 1 was the same as example 1. The method for producing the high-temperature electronic superconductor is different from example 1 only in that the processes from step (1) to step (2) are not performed, and the remaining production steps are the same as example 1.
Comparative example 2
Comparative example 2 was formulated as in example 1. The method for preparing the high-temperature electronic superconductor is different from that of example 1 only in that the processes from step (4) to step (6) are not performed, and the remaining preparation steps are the same as those of example 1.
Effects of the invention
The following table 1 shows the results of thermal conductivity analysis of the high-temperature electronic superconductors prepared using the components of example 1, example 2, comparative example 1 and comparative example 2 according to the present invention.
TABLE 1
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | |
| Thermal conductivity W/(m.K) | 851 | 871 | 593 | 621 |
As can be seen from the above table, the high-temperature electronic superconductor obtained by the component in example 2 has better heat conductivity than the components in example 1, comparative example 1 and comparative example 2, which indicates that the pre-sintered powder is filled in the modified zinc oxide gel, is more fully doped with the zinc oxide precursor, and self-aggregates in the gel to form fine particles, thereby preventing the aggregation phenomenon after the zinc oxide is directly added into the pre-sintered powder, the gel is rapidly shrunk and dehydrated by high-temperature evaporation, the pre-sintered powder is wrapped in the modified zinc oxide gel, the pre-sintered powder is limited, and lead atoms replace part of zinc atoms in the superconducting base material, so that free zinc atoms are embedded in the gaps of the copper oxide lattice, and the side surface assists in the phase formation of the superconducting phase, thereby increasing the superconducting performance of the superconductor.
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. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (1)
1. A high temperature electronic superconductor, comprising: the composite material mainly comprises the following components in parts by weight: 100 parts of pre-sintered powder, 70 parts of zinc oxide gel and 40 parts of superconducting base material;
the preparation method of the high-temperature electronic superconductor comprises the following preparation steps:
(1) Uniformly mixing bismuth oxide, lead oxide, strontium carbonate, calcium carbonate and copper oxide according to a mass ratio of 4.7;
(2) Placing the raw material on a zirconia porcelain boat, placing the porcelain boat in a graphite mold, wherein gaps still exist between the periphery of the porcelain boat and the graphite mold after the porcelain boat is placed, sintering by adopting SPS equipment under the mechanical pressure of 25MPa and the air pressure of 5Pa, wherein the sintering condition is 820 ℃, the heating rate from room temperature to 700 ℃ is 100 ℃/min, the heating rate from 700 ℃ to 820 ℃ is 20 ℃/min, the sintering time is 10min, and the heat preservation time is 10min; after sintering, relieving pressure, cooling along with the furnace, grinding after cooling, wherein the particle size of the ground pre-sintered powder is 500nm to obtain pre-sintered powder;
(3) Dissolving zinc acetate in absolute ethyl alcohol, wherein the mass ratio of the zinc acetate to the absolute ethyl alcohol is 1; adding the zinc acetate solution into an atomization tank for atomization, raising the temperature to 350 ℃, raising the temperature for 30min, adjusting the flow rate of carrier gas to be 4L/min, adopting the working frequency of 1.5MHz for an atomization sheet, controlling the atomization working voltage to be 20V and the atomization power to be 30W, and discharging in an air extraction mode to obtain aerosol micro-droplets; dissolving lithium hydroxide monohydrate in absolute ethyl alcohol, wherein the mass ratio of the lithium hydroxide monohydrate to the absolute ethyl alcohol is 1; transferring the prepared aerosol micro-droplets into a reactor, dripping a lithium hydroxide solution into the reactor by using a constant-pressure feeding funnel, wherein the volume ratio of the lithium hydroxide solution to a zinc acetate solution is 1;
(4) Heating the material to 250 ℃, wherein the heating rate from room temperature to 200 ℃ is 50 ℃/min, the heating rate from 200 to 250 ℃ is 10 ℃/min, preserving heat for 30min, then cooling, wherein the cooling rate from 250 to 100 ℃ is 10 ℃/min, and then cooling to room temperature along with the furnace to obtain a zinc oxide precursor;
(5) Putting a zinc oxide precursor into a flask, adding ethylene glycol monomethyl ether to obtain a mixed solution, stirring for 30min at 60 ℃ by using a constant-temperature stirrer, then adding ethanolamine, continuously stirring for 1h to obtain a clear solution, and aging the clear solution at room temperature for 20h to obtain zinc oxide gel, wherein the mass ratio of the zinc oxide precursor to the ethylene glycol monomethyl ether to the ethanolamine is 0.7;
(6) Dispersing the pre-sintering powder in an ethanol solution to obtain a pre-sintering powder solution, adding vinyl triamine, uniformly mixing to obtain a curing liquid, pouring the curing liquid into a mold, soaking zinc oxide gel into the curing liquid, closing the mold, pressurizing the interior of the mold, filling the curing liquid under the action of pressure until the zinc oxide gel is saturated, and curing by hot air at 50 ℃ to obtain modified zinc oxide gel; wherein the mass ratio of the pre-sintered powder to the ethanol solution to the vinyl triamine is 1; the pressure is 2MPa;
(7) Putting the modified zinc oxide gel into a high-temperature forced air dryer to carry out high-temperature evaporation on the modified zinc oxide gel, raising the temperature to 130 ℃, drying for 1h, and naturally cooling to obtain a superconducting base material;
(8) Preheating a calcining furnace, simultaneously introducing argon to replace air in the calcining furnace, wherein the preheating temperature is 600 ℃, the heating rate is 50 ℃/min, placing the superconducting base material in the calcining furnace for high-temperature calcination, the preheating temperature is 600 ℃, the heating rate is 50 ℃/min, and cooling along with the furnace to obtain a sintered base material; and (3) quenching the sintered base material by using a sodium hydroxide solution with the mass fraction of 30%, and naturally drying to obtain the high-temperature electronic superconductor.
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