AU2021102202A4 - Multilayer structure for high-temperature superconductor-coated conductors and method for preparing thick films - Google Patents
Multilayer structure for high-temperature superconductor-coated conductors and method for preparing thick films Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 26
- 239000004020 conductor Substances 0.000 title abstract description 3
- 239000002887 superconductor Substances 0.000 title abstract description 3
- 229910021521 yttrium barium copper oxide Inorganic materials 0.000 claims abstract description 75
- 229920002873 Polyethylenimine Polymers 0.000 claims abstract description 56
- 238000002360 preparation method Methods 0.000 claims abstract description 26
- 229910000856 hastalloy Inorganic materials 0.000 claims abstract description 22
- 239000002243 precursor Substances 0.000 claims abstract description 21
- 238000000197 pyrolysis Methods 0.000 claims abstract description 21
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 239000000395 magnesium oxide Substances 0.000 claims abstract description 16
- 229910052761 rare earth metal Inorganic materials 0.000 claims abstract description 15
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000005751 Copper oxide Substances 0.000 claims abstract description 14
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910000431 copper oxide Inorganic materials 0.000 claims abstract description 14
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 14
- 239000011572 manganese Substances 0.000 claims abstract description 14
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims abstract description 14
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003618 dip coating Methods 0.000 claims abstract description 12
- 238000005245 sintering Methods 0.000 claims abstract description 11
- 239000000872 buffer Substances 0.000 claims abstract description 8
- 239000000126 substance Substances 0.000 claims abstract description 5
- 229910052692 Dysprosium Inorganic materials 0.000 claims abstract description 4
- 229910052688 Gadolinium Inorganic materials 0.000 claims abstract 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 54
- 239000000243 solution Substances 0.000 claims description 41
- 239000000654 additive Substances 0.000 claims description 38
- 230000000996 additive effect Effects 0.000 claims description 37
- 239000000084 colloidal system Substances 0.000 claims description 27
- 239000008139 complexing agent Substances 0.000 claims description 25
- 239000002131 composite material Substances 0.000 claims description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 18
- 238000004090 dissolution Methods 0.000 claims description 18
- 229910052760 oxygen Inorganic materials 0.000 claims description 18
- 239000001301 oxygen Substances 0.000 claims description 18
- 239000010949 copper Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 7
- 229910052751 metal Inorganic materials 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 7
- 238000002390 rotary evaporation Methods 0.000 claims description 7
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 6
- 150000001768 cations Chemical class 0.000 claims description 6
- 238000002425 crystallisation Methods 0.000 claims description 6
- 230000008025 crystallization Effects 0.000 claims description 6
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 6
- 235000019260 propionic acid Nutrition 0.000 claims description 6
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- YTAHJIFKAKIKAV-XNMGPUDCSA-N [(1R)-3-morpholin-4-yl-1-phenylpropyl] N-[(3S)-2-oxo-5-phenyl-1,3-dihydro-1,4-benzodiazepin-3-yl]carbamate Chemical compound O=C1[C@H](N=C(C2=C(N1)C=CC=C2)C1=CC=CC=C1)NC(O[C@H](CCN1CCOCC1)C1=CC=CC=C1)=O YTAHJIFKAKIKAV-XNMGPUDCSA-N 0.000 claims description 5
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- GNFTZDOKVXKIBK-UHFFFAOYSA-N 3-(2-methoxyethoxy)benzohydrazide Chemical compound COCCOC1=CC=CC(C(=O)NN)=C1 GNFTZDOKVXKIBK-UHFFFAOYSA-N 0.000 claims description 3
- FGUUSXIOTUKUDN-IBGZPJMESA-N C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 Chemical compound C1(=CC=CC=C1)N1C2=C(NC([C@H](C1)NC=1OC(=NN=1)C1=CC=CC=C1)=O)C=CC=C2 FGUUSXIOTUKUDN-IBGZPJMESA-N 0.000 claims description 3
- 239000012298 atmosphere Substances 0.000 claims description 3
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 claims description 3
- 230000008595 infiltration Effects 0.000 claims description 3
- 238000001764 infiltration Methods 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 150000004696 coordination complex Chemical class 0.000 claims description 2
- 150000002910 rare earth metals Chemical class 0.000 claims 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims 2
- 229910052693 Europium Inorganic materials 0.000 claims 2
- 229910052772 Samarium Inorganic materials 0.000 claims 2
- 238000010438 heat treatment Methods 0.000 claims 1
- 238000000576 coating method Methods 0.000 abstract description 10
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000005204 segregation Methods 0.000 abstract description 5
- BYFGZMCJNACEKR-UHFFFAOYSA-N aluminium(i) oxide Chemical compound [Al]O[Al] BYFGZMCJNACEKR-UHFFFAOYSA-N 0.000 abstract description 4
- 239000000758 substrate Substances 0.000 abstract description 4
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract 2
- 230000004907 flux Effects 0.000 abstract 1
- 229910052757 nitrogen Inorganic materials 0.000 abstract 1
- 239000010410 layer Substances 0.000 description 72
- 229910045601 alloy Inorganic materials 0.000 description 10
- 239000000956 alloy Substances 0.000 description 10
- 238000010586 diagram Methods 0.000 description 5
- 239000012535 impurity Substances 0.000 description 3
- 239000002356 single layer Substances 0.000 description 3
- WQXKGOOORHDGFP-UHFFFAOYSA-N 1,2,4,5-tetrafluoro-3,6-dimethoxybenzene Chemical compound COC1=C(F)C(F)=C(OC)C(F)=C1F WQXKGOOORHDGFP-UHFFFAOYSA-N 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- KBQHZAAAGSGFKK-UHFFFAOYSA-N dysprosium atom Chemical compound [Dy] KBQHZAAAGSGFKK-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002427 irreversible effect Effects 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
- C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
- C23C28/042—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material including a refractory ceramic layer, e.g. refractory metal oxides, ZrO2, rare earth oxides
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- C—CHEMISTRY; METALLURGY
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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
- C04B35/45—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 copper oxide or solid solutions thereof with other oxides
- C04B35/4504—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 copper oxide or solid solutions thereof with other oxides containing rare earth oxides
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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
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/32—Filling or coating with impervious material
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N—ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
- H10N60/00—Superconducting devices
- H10N60/01—Manufacture or treatment
- H10N60/0268—Manufacture or treatment of devices comprising copper oxide
- H10N60/0296—Processes for depositing or forming copper oxide superconductor layers
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- H—ELECTRICITY
- H10—SEMICONDUCTOR DEVICES; ELECTRIC SOLID-STATE DEVICES NOT OTHERWISE PROVIDED FOR
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- H10N60/00—Superconducting devices
- H10N60/20—Permanent superconducting devices
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- 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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- C04B2235/30—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
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- 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
- C04B2235/3224—Rare earth oxide or oxide forming salts thereof, e.g. scandium oxide
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- 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
- C04B2235/3281—Copper oxides, cuprates or oxide-forming salts thereof, e.g. CuO or Cu2O
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- C23C18/00—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating
- C23C18/02—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition
- C23C18/12—Chemical coating by decomposition of either liquid compounds or solutions of the coating forming compounds, without leaving reaction products of surface material in the coating; Contact plating by thermal decomposition characterised by the deposition of inorganic material other than metallic material
- C23C18/1225—Deposition of multilayers of inorganic material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
OF THE DISCLOSURE
The present disclosure discloses a multilayer structure for high-temperature
superconductor-coated conductors and a method for preparing superconducting thick films by
a chemical solution method. The structure is: YBCO/Y(RE)BCO/manganese copper
oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy tape. This method adjusts
the stoichiometric ratio and directional growth conditions by adding RE (rare earth elements
such as Dy, Gd and the like) to the first chemically prepared superconducting layer, and
provides more possibilities for the magnetic flux pinning of superconducting layers.
In the chemical preparation of the second layer, polyethyleneimine (PEI) is added to the
precursor, wherein Cu2+ and PEI undergo a complex reaction, which on one hand, reduces
the volatilization of Cu2+ in the low-temperature pyrolysis stage, and on the other hand,
effectively inhibits the segregation of Cu2+, and meanwhile, improves the phenomenon that
the surface of the thick film is easy to crack. Multiple coatings are carried out by dip coating,
and low-temperature treatment and medium-temperature treatment are performed. By
carrying out low-temperature pyrolysis in steps and high-temperature sintering in one step, a
multilayer ReBCO thick film without cracks on the surface and with a biaxial texture and
excellent grain orientation can be prepared. Its critical current density can still reach 1.4
MA/cm2 (77K, OT), and the superconducting current-carrying capacity Ic in the liquid
nitrogen temperature zone reaches 140 A/cm.
(Figure 1)
- Page 1/4
2 nd HTS Layer: PEI-assisted YBaCuO
14 HTS Layer: Y(RE)BaCuO
Oxide buffers: LaMnO/MgO/Y2O,/Al2O
Substrate: Hastelloy Tape
FIG.1
Description
- Page 1/4
2 nd HTS Layer: PEI-assisted YBaCuO
14 HTS Layer: Y(RE)BaCuO
Oxide buffers: LaMnO/MgO/Y2O,/Al2O
Substrate: Hastelloy Tape
FIG.1
[01] The present disclosure relates to a high-temperature superconducting material and a preparation method thereof, in particular to a high-temperature superconducting film and a preparation method thereof, and it is applied to the technical field of high-temperature superconducting material manufacture.
[02] High-temperature superconducting materials are a new kind of materials. Second generation high-temperature superconducting tapes are metal oxides based on REBCO, RE=Y or other rare earth elements, B=Ba, C=Cu, which an irreversible field and a higher current-carrying capacity than first generation high-temperature superconducting tapes. In a strong magnetic field, certain high critical magnetic field superconductor materials can still carry very high superconducting currents, and plus their zero-resistance characteristics, they have a huge application potential in superconducting transmission cables, strong magnets, generators, transformers, overcurrent limiters, and the military.
[03] Preparation of ReBCO high-temperature superconducting tapes by metal organic deposition (MOD) is characterized with lower costs, higher utilization of raw material and higher production rate compared with physical methods (PLD). In order to obtain a larger transmission current, it is necessary to prepare a ReBCO coating that is as thick as possible and has a certain critical current density. Chinese Patent No. CN101746807A discloses that Lu Xudong, et al. obtained a YBCO film with a thickness of 1.5 pm without cracking on the surface by 5 times of coatings. However, it was achieved by the perfluorination process, which is not environmentally friendly, and the time of preparing a single layer was up to 10 to 20 hours. It is generally believed that the addition of additives helps improve properties and control viscosity of ReBCO films. Chinese Patent No. CN103436865A discloses that Chen Yuanqing, et al. obtained a film with a thickness of 600 nm by adding polyvinylpyrrolidone (PVP) and polyethylene glycol (PEG). It does not relate to preparation of thick films, and also does not describe the properties. In addition, Chinese Patent No. CN103102162A discloses that properties of films were improved solely by doping elements, which belongs to preparation of films. Thick films in the prior art are easy to crack, and lattice distortion leads to degradation in performance, copper segregation, and other problems. Existing methods are mostly suitable for the preparation of single-layer films, rather than the preparation of thick films, and a structure that improves the performance by modifying different layers of precursor solutions has not yet appeared in the preparation of thick films by multiple coatings.
[04] In order to solve the existing problems, it is an object of the present disclosure to provide a multilayer high-temperature superconducting thick film and a preparation method thereof to overcome the shortcomings of the prior art. By adding Dy to the first superconducting layer, the pinning force is enhanced, which provides a good foundation for the development of subsequent superconducting layers. Starting from the second superconducting layer, polyethyleneimine (PEI) is added to initiate a complex reaction of Cu2+ and PEI, which on one hand, reduces the volatilization of Cu2+ in the low-temperature pyrolysis stage, and on the other hand, effectively inhibits the segregation of Cu2+, and meanwhile, improves the phenomenon that the surface of the thick film is easy to crack. The present disclosure carries out multiple coatings by dip coating, low-temperature treatment at 400°C for 20 to 30 minutes, and medium-temperature treatment at 550°C for 30 to 60 minutes. By carrying out low-temperature pyrolysis in steps and high-temperature sintering in one step, the present disclosure successfully prepares a multilayer ReBCO thick film without cracks on the surface and with a biaxial texture and excellent grain orientation. After thickness conversion, its critical current density can still reach 1.4 MA/cm2 (77K, OT) on the Hastelloy buffer layer, and Ic can reach 140A/cm.
[05] In order to achieve the above object of the present disclosure, the present disclosure uses the following technical solutions:
[06] A high-temperature superconducting thick film with a multilayer structure, wherein the high-temperature superconducting thick film has a total thickness of no less than 1 m, and comprises two superconducting layers, wherein the first superconducting layer is incorporated with a rare earth element, dysprosium, and the second superconducting layer is incorporated with an additive; the additive is a complexing agent, and reacts with at least one metal element in the second superconducting layer to form a metal complex; the layered composite structure is: composite layer of YBCO and additive/Y(Dy)BCO layer/manganese copper oxide layer/magnesium oxide layer/yttrium oxide layer/aluminum oxide layer/Hastelloy tape, wherein the material in the Y(Dy)BCO layer is prepared in a molar ratio of Y : Dy : Ba : Cu of 1 : (0.1-0.5) : 2 : (3-3.6), and the composite material in the composite layer of YBCO and additive is prepared in a molar ratio of additive : Y: Ba : Cu of (0.0036-0.0390) : 1 : 2 : ( 3-3.6).
[07] The additive used for the preparation of the above composite layer of YBCO and additive is preferably an additive such as polyethyleneimine, polyvinylpyrrolidone or polyethylene glycol.
[08] When polyethyleneimine is used as the additive, the composite layer of YBCO and additive is prepared by using polyethyleneimine preferably in a molar amount of 0.21% (mol/mol) of the total molar amount of the composite material in the composite layer of YBCO and additive.
[09] The total thickness of the above high-temperature superconducting thick film is preferably not less than 1.0 [m.
[10] A method for preparing a high-temperature superconducting thick film with a multilayer structure of the present disclosure, comprising the following steps:
[11] a. Barium acetate is dissolved in methanol and 1- to 2-fold excess of trifluoroacetic acid is add to enable sufficient dissolution; after sufficient dissolution, the solvent is removed by a rotary evaporator to obtain a colorless transparent colloidal liquid A;
[12] b. Yttrium acetate, dysprosium acetate and copper acetate are dissolved in methanol in a molar ratio of 1 : (0.1-0.5) : (3-3.6) and 3- to 5-fold excess of propionic acid is added to enable sufficient dissolution; after sufficient dissolution, a green transparent colloid B is obtained;
[13] c. Apart of the colorless transparent colloidal liquid A prepared instep a and the green transparent colloid B prepared in step b are mixed in a molar ratio of Y: Dy : Ba: Cu of 1 : (0.1-0.5) : 2 : (3-3.6), and subjected to repeated rotary evaporation at 85°C to obtain a pure blue-green transparent colloid; then a constant volume is set by using methanol to obtain a Y(Dy)BCO precursor solution C with a cation concentration of 1.5 to 2.5 mol/L;
[14] d. Yttrium acetate and copper acetate are dissolved in methanol in a molar ratio of 1 (3-3.6), and 3- to 5-fold excess of propionic acid is added to enable sufficient dissolution; after sufficient dissolution, a green transparent colloid D is obtained;
[15] e. The other part of the colorless transparent colloidal liquid A prepared in step a and the green transparent colloid D prepared in step d are mixed in a molar ratio of Y : Ba : Cu of 1 : 2 : (3-3.6) to obtain a green transparent colloid E;
[16] f. A certain mass of polyethyleneimine is dissolved in methanol and stirred evenly to obtain a colorless transparent solution F with a polyethyleneimine concentration of 7.7x10 to 1.6x10-2 mol/L;
[17] g. The green transparent colloid E prepared in step e is mixed with the colorless transparent solution F prepared in step f and sufficiently stirred; the resulting mixed solution is subjected to repeated rotary evaporation at 85°C to obtain a dark blue transparent colloid; then a constant volume of the dark blue transparent colloid is set by using methanol as solvent to finally obtain a YBCO precursor solution G with a total metal cation concentration of 1.5 to 2.5 mol/L;
[18] h. The Y(Dy)BCO precursor solution C obtained in step c is applied on a Hastelloy buffer layer by dip coating to form a liquid film of Y(Dy)BCO precursor solution C; parameters of the dip coating process are controlled to be: a falling speed of 80 to 100 [m/s, and a withdrawal speed of 200 to 1000 [m/s; the coated film is treated by sintering, that is, first subjected to a low-temperature pyrolysis at 150°C to 400°C at a pyrolysis rate of 2 to 10°C/min with an introduction of wet oxygen at 150 to 200°C and a partial pressure of water vapor of 2 to 3%, then kept warm at 550 to 580°C for 20 to 30 minutes, and cooled to room temperature to obtain Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy, and complete the preparation of the first superconducting layer of Y(Dy)BCO;
[19] i. The YBCO precursor solution G obtained in step g is applied on the first superconducting layer of Y(Dy)BCO on the Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy prepared in step h by dip coating to form a liquid film of YBCO precursor solution G; parameters of the dip coating process are controlled to be: a falling speed of 80 to 100 m/s, and a withdrawal speed of 200 to 1000 [m/s; the coated film is treated by sintering, that is, first subjected to a low-temperature pyrolysis at 150°C to 400°C for 30 to 50 minutes at a pyrolysis rate of 2 to 10°C/min; subsequently, wet oxygen is introduced at 150 to 365°C at a partial pressure of water vapor of 2 to 3%; then it is subjected to a low-temperature treatment at a temperature maintained at 365 to 400°C for 20 to 30 minutes; a mixture of wet N2/02 is introduced at 550°C at a partial pressure of water vapor of 3 to 5%; thereafter, the partial pressure of oxygen is controlled to be 100 to 200 PPm at 550 to 580°C; it is subjected to a medium-temperature treatment at a maintained temperature for 30 to 60 minutes and cooled to room temperature to prepare a second superconducting layer, i.e., a YBCO layer with the addition of a polyethyleneimine complexing agent; a medium-temperature treated film of
YBCO (additive)/Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy is obtained, i.e., a first YBCO layer with the addition of a polyethyleneimine complexing agent is prepared;
[20] j. At least one subsequent YBCO layer with the addition of a polyethyleneimine complexing agent is then prepared for the YBCO composite layer according to the process as described in step i to form at least one superconducting layer, i.e., YBCO layer with the addition of a polyethyleneimine complexing agent, with an increased thickness; a multilayer medium-temperature pyrolysis film composed of a plurality of YBCO layers with the addition of a polyethyleneimine complexing agent is obtained, and it has a multilayer structure system of YBCO (additive)/YBCO (additive)/Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy; then the film with such a multilayer structure is subjected to a high-temperature crystallization treatment to prepare a final high-temperature superconducting thick film with a total thickness of no less than 1 m.
[21] As a preferred technical solution of the present disclosure, in the step j, after the preparation of the second superconducting layer, i.e., the YBCO layer with the addition of a polyethyleneimine complexing agent; at least two subsequent YBCO composite layers, i.e., YBCO layers with the addition of a polyethyleneimine complexing agent, are continually prepared to form at least two layers of superconducting layers, i.e., YBCO layers with the addition of a polyethyleneimine complexing agent, with increased thickness; each of the subsequent YBCO layers with the addition of a polyethyleneimine complexing agent is prepared according to a process as described in step i.
[22] As a further preferred technical solution of the present disclosure, in the step j, when the film with a multilayer structure is subjected to the high-temperature crystallization treatment, the coated composite layer flm is treated by sintering: first, it is heated from a temperature below 550°C to 780 to 800°C at a rate of 5 to 20°C/min, and the temperature is maintained for 2 to 3 hours; the partial pressure of water vapor is controlled to be 3 to 5%, and the partial pressure of oxygen is controlled to be 100 to 200 PPm; subsequently, it is subjected to an oxygen infiltration treatment at 450 to 525°C in a dry oxygen atmosphere for 60 to 180 minutes, and finally cooled to room temperature to obtain a YBCO thick film.
[23] As a preferred technical solution of the present disclosure, a water-free preparation process is used all through the preparation of the a to g intermediate substances.
[24] Compared with the prior art, the present disclosure has the following obvious prominent substantive features and significant advantages:
[25] 1. Compared with existing techniques, the main advantage of the present disclosure is that the first layer of the superconducting layers is incorporated with a Dy rare earth element, which enhances the pinning force compared with pure YBCO and provides good growth environment for subsequent superconducting coatings. Starting from the second layer, polyethyleneimine is added as additive; during repeated rotary evaporation, polyethyleneimine is complexed with Cu2+, which increases the viscosity and stability of the solution, effectively improves the surface structure of the film, and increase the thickness of the single layer, reduces the volatilization of Cu2+, and efficiently inhibits the segregation of Cu2+ to enhance the properties of the film;
[26] 2. The present disclosure can prepare thick films of 1 m or more by multiple coatings. The thick films prepared by this method have good texture orientation, dense surface and low roughness; the critical current density on a metal substrate can reach 1-3 MA/cm 2 ; the increase in thickness enables Ic to reach 140 A/cm or more.
[27] FIG. 1 is a diagram showing the structure of a multilayer high-temperature superconducting film doped with Dy and coated with a YBCO solution of polyethyleneimine in the example of the present disclosure.
[28] FIG. 2 is an X-ray diffraction pattern of a multilayer high-temperature superconducting film doped with Dy and coated with a YBCO solution of polyethyleneimine in the example of the present disclosure.
[29] FIG. 3 is a Jc data diagram of a multilayer high-temperature superconducting film doped with Dy and coated with a YBCO solution of polyethyleneimine in the example of the present disclosure.
[30] FIG. 4 is a diagram showing the performance relationship of samples coated with varying numbers of layers of a multilayer high-temperature superconducting film doped with Dy and coated with a YBCO solution of polyethyleneimine in the example of the present disclosure.
[31] A preferred example of the present disclosure is described hereinbelow with details:
[32] In this example, by referring to FIGs. 1 to 4, a method for preparing a high-temperature superconducting thick flm with a multilayer structure comprises the following steps:
[33] a. Barium acetate is dissolved in methanol and trifluoroacetic acid in excess of 200% is add to enable sufficient dissolution; after sufficient dissolution, the solvent is removed by a rotary evaporator to obtain a colorless transparent colloidal liquid A;
[34] b. Yttrium acetate, dysprosium acetate and copper acetate are dissolved in methanol in a molar ratio of 1 : 0.5 : 3.15, and 3-fold excess of propionic acid is added to enable sufficient dissolution; after sufficient dissolution, a green transparent colloid B is obtained;
[35] c. Apart of the colorless transparent colloidal liquid A prepared instep a and the green transparent colloid B prepared in step b are mixed in a molar ratio of Y : Dy : Ba: Cu of 1 : 0.5 : 2 : 3.15, and subjected to rotary evaporation at 85°C three times to obtain a pure blue-green transparent colloid; then a constant volume is set by using methanol to obtain Y(Dy)BCO precursor solution C with a cation concentration of 1.9 mol/L;
[36] d. Yttrium acetate and copper acetate are dissolved in methanol in a molar ratio of 1 3.15, and 3-fold excess of propionic acid is added to enable sufficient dissolution; after sufficient dissolution, a green transparent colloid D is obtained;
[37] e. The other part of the colorless transparent colloidal liquid A prepared in step a and the green transparent colloid D prepared in step d are mixed in a molar ratio of Y : Ba : Cu of 1 : 2 : 3.15 to obtain a green transparent colloid E;
[38] f. A certain mass of polyethyleneimine is dissolved in methanol and stirred evenly to obtain a colorless transparent solution F with a polyethyleneimine concentration of 3.9x10 -3 mol/L;
[39] g. The green transparent colloid E prepared in step e is mixed with the colorless transparent solution F prepared in step f and sufficiently stirred; the resulting mixed solution is subjected to rotary evaporation at 85°C three times to obtain a dark blue transparent colloid; then a constant volume of the dark blue transparent colloid is set by using methanol as solvent to finally obtain a YBCO precursor solution G with a total metal cation concentration of 1.9 mol/L;
[40] h. The Y(Dy)BCO precursor solution C obtained in step c is applied on a Hastelloy buffer layer by dip coating to form a liquid film of Y(Dy)BCO precursor solution C; parameters of the dip coating process are controlled to be: a falling speed of 83 m/s, and a withdrawal speed of 1000 [m/s; the coated film is treated by sintering, that is, first subjected to a low-temperature pyrolysis at 400°C for 30 minutes with an introduction of wet oxygen at 200°C and a partial pressure of water vapor of 2%, then kept warm at 550°C for 30 minutes, and cooled to room temperature to obtain Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy, and complete the preparation of the first superconducting layer of Y(Dy)BCO;
[41] i. The YBCO precursor solution G obtained in step g is applied on the first superconducting layer of Y(Dy)BCO on the Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy prepared in step h by dip coating to form a liquid film of YBCO precursor solution G; parameters of the dip coating process are controlled to be: a falling speed of 83 m/s, and a withdrawal speed of 1000 Im/s; the coated film is treated by sintering, that is, first subjected to a low-temperature pyrolysis at 150°C to 400°C at a pyrolysis rate of 5°C/min; wet oxygen is introduced at 200°C at a partial pressure of water vapor of 2%; then it is subjected to a low-temperature treatment at a temperature maintained at 400°C for 20 minutes; a mixture of wet N2/02 is introduced at 550°C at a partial pressure of water vapor of 5%; thereafter, the partial pressure of oxygen is controlled to be 150 PPm at 550°C; it is subjected to a medium-temperature treatment at a maintained temperature for 30 minutes and cooled to room temperature to prepare a second superconducting layer, i.e., a YBCO layer with the addition of a polyethyleneimine complexing agent; a medium-temperature treated film of YBCO (additive)/Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy is obtained, i.e., a first YBCO layer with the addition of a polyethyleneimine complexing agent is prepared;
[42] j. Subsequent YBCO layers with the addition of a polyethyleneimine complexing agent are then prepared for the YBCO composite layer according to the process as described in step i to form subsequent superconducting layers, i.e., YBCO layers with the addition of a polyethyleneimine complexing agent, with an increased thickness; a multilayer medium-temperature pyrolysis film composed of a plurality of YBCO layers with the addition of a polyethyleneimine complexing agent is obtained, and it has a multilayer structure system of YBCO (additive)/YBCO (additive)/Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy; then the film with such a multilayer structure is subjected to a high-temperature crystallization treatment to prepare a final high-temperature superconducting thick film.
[43] In this example, in the step j, the medium-temperature pyrolysis film with the structure of YBCO (additive)/YBCO (additive)/Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy is subjected to a high-temperature crystallization treatment; parameters of the process are controlled: it is first heated from 550°C to 780°C at a rate of 20°C/min, and the temperature is maintained for 2.5 hours; the partial pressure of water vapor is 5%, and the partial pressure of oxygen is 150 PPm; subsequently, it is subjected to an oxygen infiltration treatment at 450°C in a dry oxygen atmosphere for 60 minutes, and finally cooled to room temperature. A subsequent YBCO composite layer is then continually prepared on the second superconducting layer, i.e., the YBCO layer with the addition of a polyethyleneimine complexing agent; a YBCO layer with a total thickness of1 m is prepared to complete the preparation of the second superconducting layer, i.e., the YBCO layer with the addition of a polyethyleneimine complexing agent; finally, YBCO (additive)/Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy alloy is obtained; after thickness conversion, the critical current density of the YBCO thick flm is up to 1.4 MA/cm2 (77K, OT).
[44] In this example, a water-free preparation process is used all through the preparation of the A to G intermediate substances, which avoids the addition of water impurity, simplifies the process of impurity removal, and significantly shortens the time of formulating the solution.
[45] The high-temperature superconducting ReBCO thick film prepared in this example has a multilayer structure, which is: YBCO (additive)/YBCO (additive)/Y(Dy)BCO/manganese copper oxide/magnesium oxide/yttrium oxide/aluminum oxide/Hastelloy tape, wherein the first superconducting layer is incorporated with a rare earth element, dysprosium, and starting from the second superconducting layer an additive is added. FIG. 2 is an X-ray diffraction pattern of a multilayer high-temperature superconducting film doped with Dy and coated with a Y(Dy)BCO solution of polyethyleneimine in Example 1. It can be seen from FIG. 2 that the XRD (006) peak value of the high-temperature superconducting thick film coated with the Y(Dy)BCO precursor solution prepared by adding Dy and polyethyleneimine can reach more than 10,000, and there are almost no impurity peaks. The sample prepared in this example with such a thickness has good texture, and there is no a-axis-oriented (200) peak that affects performance.
[46] FIG. 3 is a Jc data diagram of a multilayer high-temperature superconducting film doped with Dy and coated with a YBCO solution of polyethyleneimine in in Example 1. It can be seen from FIG. 3 that the high-temperature superconducting thick film obtained by coating the Hastelloy buffer layer as the substrate three times has a thickness of 1 m, and the obtained Jc data is 7.1 MA/cm2 under the test conditions of 200 nm thickness. The Jc obtained by thickness conversion is 1.4 MA/cm2 (77K, OT). For the preparation of high-temperature superconducting tapes based on metal materials, the sample prepared by this method has a higher critical current density.
[47] By adding Dy to thefirst superconducting layer, the pinning force is enhanced, which provides a good foundation for the development of subsequent superconducting layers. Starting from the second superconducting layer, polyethyleneimine (PEI) is added to initiate a complex reaction of Cu2+ and PEI, which on one hand, reduces the volatilization of Cu2+ in the low-temperature pyrolysis stage, and on the other hand, effectively inhibits the segregation of Cu2+, and meanwhile, improves the phenomenon that the surface of the thick film is easy to crack. Multiple coatings are carried out by dip coating, and low-temperature treatment at 400°C for 20 to 30 minutes, and medium-temperature treatment at 550°C for 30 to 60 minutes are performed. By carrying out low-temperature pyrolysis in steps and high-temperature sintering in one step, a multilayer ReBCO thick film without cracks on the surface and with a biaxial texture and excellent grain orientation is successfully prepared. After thickness conversion, its critical current density can still reach 1.4 MA/cm2 (77K, OT) on the Hastelloy buffer layer, and Ic can reach 140A/cm.
[48] FIG. 4 is a diagram showing the performance relationship of samples coated with varying numbers of layers of a multilayer high-temperature superconducting film doped with Dy and coated with a YBCO solution of polyethyleneimine in the above example. It can be seen that the first layers are all Y(Dy)BCO superconducting layer, and the subsequent coatings are all YBCO (additive) high-temperature superconducting layers. With the increase of the number of coating layers, the thickness effect is obvious, and the critical current density Jc has a downward trend. However, in another aspect, calculation according to Ic=Jcxh shows that the increase in thickness increases the critical current value. According to FIG. 4, the sample Ic obtained by the solution of Example 1 reaches 140 A/cm.
[49] The example of the present disclosure is described with reference to accompanying drawings, but the present disclosure is not limited to the above example, and various changes can be made according to the purpose of the present disclosure. Any changes, modifications, substitutions, combinations or simplifications made in accordance with the spirit and principle of the technical solution of the present disclosure should be equivalent replacements, and all belong to the protection scope of the present disclosure as long as they comply with the purpose of the present disclosure, and do not deviate from the technical principle and inventive concept of the multilayer high-temperature superconducting thick film and its preparation method in the present disclosure.
Claims (5)
1. A high-temperature superconducting thick film with a multilayer structure, wherein the
high-temperature superconducting thick film has a total thickness of no less than 1 m, and
comprises two superconducting layers, wherein the first superconducting layer is incorporated
with a rare earth (RE) element, Dy, Sm, Eu or Gd, and the second superconducting layer is
incorporated with an additive; the additive is a complexing agent, and reacts with at least one
metal element in the second superconducting layer to form a metal complex; the layered
composite structure is: composite layer of YBCO and additive/Y(RE)BCO layer/manganese
copper oxide layer/magnesium oxide layer/yttrium oxide layer/aluminum oxide
layer/Hastelloy tape, wherein the material in the Y(RE)BCO layer is prepared in a molar ratio
of Y : RE : Ba : Cu of1 : (0.1-0.5) : 2 : (3-3.6), and the composite material in the composite
layer of YBCO and additive is prepared in a molar ratio of additive : Y : Ba : Cu of
(0.0036-0.0390) : 1 : 2 : ( 3-3.6).
2. The high-temperature superconducting thick film with a multilayer structure according
to claim 1, wherein the additive used for the preparation of the above composite layer of
YBCO and additive is polyethyleneimine, polyvinylpyrrolidone or polyethylene glycol;
wherein when polyethyleneimine is used as the additive, the composite layer of YBCO
and additive is prepared by using polyethyleneimine preferably in a molar amount of 0.21%
(mol/mol) of the total molar amount of the composite material in the composite layer of YBCO
and additive.
3. The high-temperature superconducting thick film with a multilayer structure according
to any one of claims 1-2, wherein the total thickness of the high-temperature superconducting
thick film is not less than 1.0 [m.
4. A method for preparing the high-temperature superconducting thick film with a
multilayer structure according to claim 1, comprising the following steps:
a. Barium acetate is dissolved in methanol and 1- to 2-fold excess of trifluoroacetic acid is
add to enable sufficient dissolution; after sufficient dissolution, the solvent is removed by a
rotary evaporator to obtain a colorless transparent colloidal liquid A; b. Yttrium acetate, Dy (or Gd, Sm, Eu) acetate and Cu acetate are dissolved in methanol in a molar ratio of 1 : (0.1-0.5) : (3-3.6) and 3- to 5-fold excess of propionic acid is added to enable sufficient dissolution; after sufficient dissolution, a green transparent colloid B is obtained; c. A part of the colorless transparent colloidal liquid A prepared in step a and the green transparent colloid B prepared in step b are mixed in a molar ratio of Y : RE : Ba: Cu of 1 :
(0.1-0.5) : 2 : (3-3.6), and subjected to repeated rotary evaporation at 85°C to obtain a pure
blue-green transparent colloid; then a constant volume is set by using methanol to obtain a
Y(Dy)BCO precursor solution C with a cation concentration of 1.5 to 2.5 mol/L;
d. Yttrium acetate and copper acetate are dissolved in methanol in a molar ratio of 1
(3-3.6), and 3- to 5-fold excess of propionic acid is added to enable sufficient dissolution; after
sufficient dissolution, a green transparent colloid D is obtained;
e. The other part of the colorless transparent colloidal liquid A prepared in step a and the
green transparent colloid D prepared in step d are mixed in a molar ratio of Y: Ba: Cu of 1 : 2
(3-3.6) to obtain a green transparent colloid E;
f. A certain mass of polyethyleneimine is dissolved in methanol and stirred evenly to
obtain a colorless transparent solution F with a polyethyleneimine concentration of 7.7x10-4 to
1.6x10-2 mol/L;
g. The green transparent colloid E prepared in step e is mixed with the colorless
transparent solution F prepared in step f and sufficiently stirred; the resulting mixed solution is
subjected to repeated rotary evaporation at 85°C to obtain a dark blue transparent colloid; then
a constant volume of the dark blue transparent colloid is set by using methanol as solvent to
finally obtain a YBCO precursor solution G with a total metal cation concentration of 1.5 to
2.5 mol/L;
h. The Y(RE)BCO precursor solution C obtained in step c is coated on a Hastelloy buffer
layer to form a liquid film of Y(Dy)BCO precursor solution C; the coated film is treated by
sintering, that is, first subjected to a low-temperature pyrolysis at 150°C to 400°C at a
pyrolysis rate of 2 to 10°C/min with an introduction of wet oxygen at 150 to 200°C and a partial pressure of water vapor of 2 to 3%, then kept warm at 550 to 580°C for 20 to 30 minutes, and cooled to room temperature to complete the preparation of the first superconducting layer of Y(RE)BCO; i. The YBCO precursor solution G obtained in step g is coated on the first superconducting layer of Y(RE)BCO prepared in step h to form a liquid film of YBCO precursor solution G; parameters of the dip coating process are controlled to be: a falling speed of 80 to 100 [m/s, and a withdrawal speed of 200 to 1000 [m/s; the coated film is treated by sintering: first subjected to a low-temperature pyrolysis by heating from room temperature to
150°C for 30 to 50 minutes at a pyrolysis rate of 2 to10°C/min; subsequently, wet oxygen is
introduced at 150 to 365°C at a partial pressure of water vapor of 2 to 3%; then it is subjected
to a low-temperature treatment at a temperature maintained at 365 to 400°C for 20 to 30
minutes; then the temperature is increased to 550°C to introduce a mixture of wet N2/02 at a
partial pressure of water vapor of 3 to 5%; thereafter, the partial pressure of oxygen is
controlled to be 100 to 200 PPm at 550 to 580°C; it is subjected to a medium-temperature
treatment at a maintained temperature for 30 to 60 minutes.
j. At least one subsequent YBCO layer with the addition of a polyethyleneimine
complexing agent is then prepared for the YBCO composite layer according to the process as
described in step i to form at least one superconducting layer, i.e., YBCO layer with the
addition of a polyethyleneimine complexing agent, with an increased thickness; a multilayer
medium-temperature pyrolysis film composed of a plurality of YBCO layers with the addition
of a polyethyleneimine complexing agent is obtained, which is a YBCO (additive)/Y(RE)BCO
composite film having at least two layers of YBCO (additive) layers; then the film with such a
multilayer structure is subjected to a high-temperature crystallization treatment to prepare a
final high-temperature superconducting thick film with a total thickness of no less than 1 m.
5. The method for preparing the high-temperature superconducting thick film with a
multilayer structure according to claim 4, wherein in the step j, after the preparation of the
second superconducting layer, i.e., the YBCO layer with the addition of a polyethyleneimine
complexing agent; at least two subsequent YBCO composite layers, i.e., YBCO layers with the
addition of a polyethyleneimine complexing agent, are continually prepared to form at least two layers of superconducting layers, i.e., YBCO layers with the addition of a polyethyleneimine complexing agent, with increased thickness; each of the subsequent YBCO layers with the addition of a polyethyleneimine complexing agent is prepared by the process as described in step i; wherein in the step j, when the film with a multilayer structure is subjected to the high-temperature crystallization treatment, the coated composite layer film is treated by sintering: first, it is heated from a temperature below 550°C to 780 to 800°C at a rate of 5 to °C/min, and the temperature is maintained for 2 to 3 hours; the partial pressure of water vapor is controlled to be 3 to 5%, and the partial pressure of oxygen is controlled to be 100 to 200 PPm; subsequently, it is subjected to an oxygen infiltration treatment at 450 to 525°C in a dry oxygen atmosphere for 60 to 180 minutes, and finally cooled to room temperature to obtain a YBCO thick film; or, wherein a water-free preparation process is used all through the preparation of the a to g intermediate substances.
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