CN115581114A - Preparation method of YBCO multilayer thick film - Google Patents
Preparation method of YBCO multilayer thick film Download PDFInfo
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- CN115581114A CN115581114A CN202210108443.7A CN202210108443A CN115581114A CN 115581114 A CN115581114 A CN 115581114A CN 202210108443 A CN202210108443 A CN 202210108443A CN 115581114 A CN115581114 A CN 115581114A
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Abstract
The invention relates to C084B, in particular to a preparation method of a YBCO multilayer thick film. The method comprises the following steps of preparing a semi-grown film: coating the YBCO colloid on a texture substrate to obtain a colloid film, and sequentially carrying out low-temperature treatment and high-temperature pretreatment to obtain a semi-grown film. The method provided by the invention overcomes the thick film effect, can be used for continuous and large-scale production of YBCO high-performance thick films, promotes the YBCO superconducting films with multilayer structures to form more compact structures, the thickness of the thick films can reach more than 3 mu m, the thickness of the thick films is obviously higher than that of the YBCO superconducting films obtained by the existing similar methods, the Ic with the width of 12mm can also reach more than 1000A, and the critical current density can reach 2.8MA/cm 2 As described above.
Description
Technical Field
The invention relates to C084B, in particular to a preparation method of a YBCO multilayer thick film.
Background
Yttrium barium copper oxide (YBa) 2 Cu 3 O 7 Delta, YBCO for short) high-temperature superconducting films as superconducting materials have good application prospects in many fields, such as transmission cables, generators, transformers and the like. With the improvement of the requirements of the fields on critical current (Ic), the current carrying capacity of the YBCO high-temperature superconducting thin film is higher, the current carrying capacity depends on the control of the critical current density (Jc) to be basically unchanged, and the thickness is increased, but the thickness effect exists along with the increase of the thickness of the existing superconducting material, namely, the thickness is simply increased, the Jc is rapidly reduced, even the Ic is reduced, and the preparation process of the YBCO thin film is challenged.
At present, a common preparation process is a metal organic solution chemical method (TFA-MOD), the YBCO precursor liquid colloid is coated, low-temperature pyrolysis is carried out to convert an organic phase into an inorganic phase, and finally high-temperature phase sintering is carried out to obtain a crystallized structure, and then steps of oxygen absorption, silver plating of a protective layer, packaging and the like are carried out to obtain a YBCO high-temperature superconducting strip which is finally used commercially, wherein in the low-temperature pyrolysis process, the contraction of the thickness of 90 percent can be generated; after high temperature crystallization sintering, the film shrinks by 50% again, so in order to obtain a thick film structure, the steps of colloid coating and low temperature pyrolysis are carried out for many times, and then high temperature sintering is carried out, but the obtained thick film structure has poor uniformity, various segregation problems exist, and the Jc stability and the Ic improvement under the height are difficult to maintain.
The U.S. air force laboratory t.haugan research group reports a Pulsed Laser Deposition (PLD) method in Nature, and a high-performance YBCO coating is prepared by using a multilayer film superposition mode, so that the current carrying capacity of the coating is improved, but the pulsed laser deposition adopted by the method needs an expensive vacuum system, the deposition rate is low, the process is complex, and the cost is high. CN102560378B reports that a problem that cubic texture of a YBCO layer is deteriorated along with increase of thickness is solved by layering deposition and properly increasing temperature among layers, but the requirement on the process is high, CN102142300B improves Jc by adding 0.1-5% of second-phase nano particles into a thin film, but a thick film is difficult to prepare, and CN102690114B provides a YBa2Cu3O7-x (YBCO) superconducting composite film, so that a YBCO/CeO2/YBCO/CeO 2/superconductive film with the five-layer thickness of 1.5 microns can be obtained, but the requirement on the YBCO film thickness is still difficult to meet. How to overcome the thickness effect, the preparation of thick films with high critical current (Ic) is a key problem in the preparation of current YBCO high-temperature films.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of a YBCO superconducting thick film with a multilayer structure, the thickness can reach more than 3 microns, the thickness effect is overcome to a certain extent, the current carrying capacity of a high-temperature superconducting tape is greatly improved, and meanwhile, a method for continuously producing the YBCO superconducting thick film tape is provided.
As shown in fig. 1, the present invention provides a method for preparing a YBCO multilayer thick film, comprising:
coating and low-temperature treatment: coating a YBCO colloid on a texture substrate to obtain a colloid film, performing low-temperature treatment to obtain a low-temperature pyrolysis film, and repeating coating and low-temperature treatment to obtain M layers of low-temperature pyrolysis films, wherein M is more than or equal to 1; by the method provided by the invention, high-temperature pretreatment can be carried out on 1 layer of low-temperature pyrolysis film, and high-temperature pretreatment can also be carried out after multiple layers of low-temperature pyrolysis films are obtained by repeating the low-temperature pyrolysis process for multiple times, without specific limitation, preferably, M is 1-3.
High-temperature pretreatment: performing high-temperature pretreatment on the M low-temperature pyrolysis film to obtain a semi-grown film, wherein a YBCO layer is arranged on one side of the semi-grown film close to the texture substrate, and a non-epitaxial growth layer is arranged on one side of the semi-grown film far away from the texture substrate;
preparing a multilayer film: and coating the YBCO colloid on the non-epitaxial growth layer, and repeating the preparation of the semi-growth film to obtain a multilayer film. In the preparation process, the conventional repeated steps of coating and low-temperature pyrolysis are replaced by the processes of coating, low-temperature treatment and high-temperature pretreatment, so that a semi-grown film can be obtained, the structural uniformity after subsequent coating is promoted, and the problems of segregation and the like are reduced. The coating method of the present invention is spin coating, pulling, casting, etc., and is not particularly limited.
As a preferred technical solution of the present invention, the concentration of cations of the YBCO colloid is 1.5 to 2.5mol/L, and the cations include cations having a molar ratio of 1 to 1.5: 1.5-2: 3-3.6 of yttrium ions, barium ions and copper ions. The yttrium ions, the barium ions and the copper ions can be prepared according to the stoichiometric proportion of the YBCO film of 1:2:3, or non-stoichiometric amounts such as 1 to 1.5: 1.5-2: 3-3.6, etc., to promote the increase of the magnetic field performance by certain impurity defects, and is not particularly limited. The yttrium ions, barium ions and copper ions can be from yttrium salts, barium salts and copper salts, such as acetate and propionate of yttrium, barium and copper, and are not particularly limited.
The preparation method of the colloid is not specifically limited, and the preparation method comprises the following steps: respectively dissolving yttrium salt, barium salt and copper salt in an organic acid-water solution, adding alkyl alcohol, distilling, mixing and fixing the volume to obtain the YBCO colloid. The organic acid-water solution of yttrium salt, barium salt and copper salt can be selected according to the dissolving types of different metal salts, for example, yttrium salt and barium salt are trifluoroacetic acid water solution, copper salt is propionic acid water solution, wherein the organic acid can be respectively stoichiometric with yttrium salt, barium salt and copper salt, or the organic acid can be weighed in excess stoichiometric amount, that is, the molar ratio of the organic acid to yttrium salt, barium salt and copper salt is more than 1, the method is not particularly limited, if the types of the used organic acid are the same, yttrium salt, barium salt, copper salt and the like can also be added into the organic acid-water solution to be mixed together, after dissolving, the water is removed and mixed in the distillation process by adding alkyl alcohol, and the alkyl alcohol is subjected to constant volume to reach a proper cation concentration. The alkyl alcohol of the present invention is well known in the art, such as methanol, ethanol, etc., and is not particularly limited.
As a preferred embodiment of the present invention, the low-temperature treatment includes: and heating the colloid film to 350-450 ℃ in the mixed atmosphere of oxygen and water vapor, and cooling to obtain the low-temperature pyrolysis film. The temperature reduction of the invention is generally carried out along with furnace cooling, and is not particularly limited.
In a preferred embodiment of the present invention, the low-temperature treatment is performed for 30 to 60min. The heating rate in the low-temperature treatment is not specifically required, wherein the heating rate is generally 5-20 ℃/min, and the specific requirement is not required, and only the colloidal organic substance is converted into a crystalline or amorphous inorganic substance.
As a preferable technical scheme of the invention, the flow of the oxygen in the low-temperature treatment is 1-2L/min.
As a preferred technical solution of the present invention, the high-temperature pretreatment comprises: and heating the low-temperature pyrolysis film to 750-800 ℃ in the mixed atmosphere of oxygen, water vapor and nitrogen, and preserving the temperature to obtain the semi-grown film.
As a preferable technical scheme of the invention, in the high-temperature pretreatment, the heating rate is 20-100 ℃/min, preferably 60-80 ℃/min, and the heat preservation time is 5-30 min.
In a preferred embodiment of the present invention, the oxygen content of the mixed atmosphere of the high temperature pretreatment is 100 to 200ppm, the gas pressure is 20 to 1000Pa, and the oxygen content is selected according to the performance of different furnaces, which is not particularly limited. The oxygen content of the invention is the volume ratio of oxygen to mixed atmosphere.
As a preferred technical scheme of the invention, after the multilayer film is prepared, the multilayer film is subjected to high-temperature treatment to obtain the YBCO film crystallized at high temperature. The film after the last coating and low-temperature treatment can be directly subjected to high-temperature treatment without high-temperature pretreatment.
As a preferred technical solution of the present invention, the high temperature treatment includes: and heating the multilayer film to 750-800 ℃ in the mixed atmosphere of oxygen, water vapor and nitrogen, and preserving the heat to obtain the YBCO film crystallized at high temperature.
In a preferred embodiment of the present invention, the oxygen content of the mixed atmosphere for the high-temperature treatment is 100 to 200ppm, and the atmospheric pressure is 20 to 1000Pa.
As a preferable technical scheme of the invention, the heating rate of the high-temperature treatment is 20-100 ℃/min, preferably 60-80 ℃/min, and the heat preservation time is 60-150 min.
The post-treatment of the present invention is well known in the art and is not particularly limited. As a preferred technical scheme of the invention, the YBCO film crystallized at high temperature is subjected to post-treatment.
As a preferable technical solution of the present invention, the post-processing includes: cooling the YBCO superconducting film to 400-500 ℃, and cooling after heat preservation in an oxygen atmosphere.
As a preferable technical scheme of the invention, the heat preservation time of the post-treatment is 40-90 min, the pressure of the oxygen atmosphere is 0.8-1.5 atm, and the pressure is generally 1 standard atmosphere. And silver plating protective layers, packaging and the like can be further carried out after the post-treatment.
In a preferred embodiment of the present invention, the thickness of the film after the high temperature treatment is 4 μm or less, and the film is prepared from N-layer half-grown films, the thickness of each half-grown film after the final shrinkage by the high temperature treatment can be about 0.6 to 1 μm, preferably about 0.6 to 0.9 μm, and N can be adjusted about 1 to 6 by the method provided by the present invention.
In a preferred embodiment of the present invention, the critical current (Ic) of the post-treated thin film is 1000A or more when the width of the post-treated thin film is 12 mm. As a preferable technical scheme of the invention, the length of the film after post-treatment reaches more than 300 meters.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention provides a method, which comprises the steps of controlling a colloid film to be subjected to low-temperature treatment firstly, changing organic matters into inorganic amorphous and nanocrystalline films, then carrying out high-temperature pretreatment, and controlling treatment time to control crystallization degree, so as to obtain a YBCO layer structure with complete crystallization epitaxy on one side and a structure with incomplete epitaxy on the other side, which is still similar to the film subjected to low-temperature treatment, so that when colloid is further coated, the pyrolytic forming of the inorganic amorphous and nanocrystalline films of a second layer of colloid film is continuously promoted, and when the high-temperature pretreatment is carried out, the epitaxial growth is continuously carried out along with the non-epitaxial growth layer of a first layer of semi-grown film, so as to continuously obtain 2 layers of semi-grown films, so that the process is repeated, the thickening is realized, the sintering uniformity after the subsequent high-temperature treatment is promoted, and the problems of segregation and the like are reduced.
(2) The semi-grown film can promote the gas to enter and flow in the processes of low-temperature treatment and high-temperature pretreatment, and can promote the consistent growth direction of crystal grains, obtain a more compact structure, promote the high thickness of the YBCO superconducting film with a multi-layer structure, and improve the Ic and the like.
(3) In addition, the prior film with good epitaxy processed at high temperature is easy to be corroded by acid and also causes difficulty to the preparation of a multilayer film, and in the process of coating the film colloid, the contact surface is the non-epitaxy growth surface which has good corrosion resistance and protection effects, so that the structural stability of the thick film is further promoted, and the complete thick film is formed.
(4) The method provided by the invention overcomes the thick film effect, can be used for continuous and large-scale production of YBCO thick films, obtains a more compact structure, increases the thickness of a YBCO superconducting film with a multi-layer structure, and can reach the thickness of 3 mu m or moreWhile the thickness is obviously higher than that of the YBCO superconducting film obtained by the prior similar method, the Ic of 12mm width can reach more than 1000A, and the critical current density can reach 2.8MA/cm 2 As described above.
Drawings
FIG. 1 is a schematic diagram of preparation of a YBCO multilayer thick film.
FIG. 2 is a graph comparing the Ic and Jc changes of a simple thick film with a half-grown thick film.
Fig. 3 is an XRD pattern of YBCO multilayer thick film obtained in example 1 of the present invention.
FIG. 4 is a cross-sectional metallographic image and a Raman spectrum of a YBCO multilayer thick film obtained in example 1 of the present invention.
Fig. 5 is a step tester test chart of the YBCO multilayer thick film obtained in example 1 of the present invention.
Fig. 6 is a topographical view (TEM) of a cross-section of a YBCO multilayer thick film obtained in example 1 of the present invention.
FIG. 7 is a performance test chart of a long tape Ic of more than 300m of the YBCO multilayer thick film obtained in the embodiment 1 of the invention.
Detailed Description
Examples
Example 1
The YBCO multilayer thick film is produced by the method provided by the invention, wherein the YBCO colloid used is obtained by market or self-made, such as yttrium acetate, barium acetate and copper acetate are weighed according to the stoichiometric ratio (1.
The method provided by the embodiment comprises the following steps:
1) Coating: spin-coating YBCO colloid with the total cation concentration of 2.5mol/L on the surface of the Hastelloy alloy substrate plated with the buffer layer on a spin-coating machine by adopting the rotating speed of 3000-6000 rpm;
2) Low-temperature treatment: putting the spin-coated film into a muffle furnace for low-temperature pyrolysis, introducing oxygen with the flow rate of 1.5L/min into room-temperature deionized water, introducing into a hearth, raising the temperature from room temperature to 400 ℃, then reducing the temperature to 150 ℃, and allowing the film to pass through the hearth for 40min;
3) High-temperature pretreatment: repeating the steps 1) and 2) to obtain 2 layers of pyrolysis films after low-temperature treatment, raising the temperature from room temperature to 785 ℃ at a heating rate of 80 ℃/min, and preserving the temperature for 10min, wherein the atmosphere in the heat preservation time is nitrogen, oxygen and water vapor mixed gas with the oxygen content of 150ppm (the air pressure is 160-200 Pa);
4) Coating and low-temperature treatment: spin-coating a YBCO precursor liquid with the total cation concentration of 2.5mol/L on the surface of the high-temperature pretreatment film by a spin coater at the rotating speed of 3000-6000rpm, putting the spin-coated film into a muffle furnace for low-temperature pyrolysis, introducing oxygen with the flow of 1.5L/min into room-temperature deionized water, introducing the oxygen into a hearth, heating the temperature from room temperature to 400 ℃, then cooling the temperature to 150 ℃, subjecting the film to 40min in the hearth to obtain 3 layers of thick films, and then coating and low-temperature treating according to the step 4) to obtain 4 layers of thick films;
5) High-temperature crystallization: the 4-layer thick film after low-temperature treatment is then heated to 785 ℃ from room temperature at the heating rate of 80 ℃/min in a high-temperature furnace chamber, and is kept for 120min, wherein the atmosphere is a nitrogen, oxygen and water vapor mixed gas (the air pressure is 80 Pa) with the oxygen content of 150 ppm.
6) And (3) post-treatment: after the heat preservation is finished, carrying out oxygen absorption treatment, namely, cooling to 450 ℃ along with the furnace, and preserving the heat for 60min, wherein the reaction atmosphere begins to be nitrogen-oxygen mixed gas after the temperature is reduced in the process, and the heat is preserved and is changed into pure oxygen atmosphere (the air pressure is 1 atm); and after the heat preservation is finished, cooling the film to room temperature along with the furnace to obtain the oxygen-absorbed yttrium barium copper oxide superconducting film strip.
Comparative example 1
This example provides a method of making a simple thick film, as shown in example 1, except that no high temperature pretreatment is included.
Evaluation of Performance
1. Ic-Jc Change: the thick films provided by the embodiment 1 and the comparative embodiment 1 are respectively tested according to the change of Ic-Jc with thickness, as shown in fig. 2, wherein the open circular broken line and the solid circular broken line are respectively the change of Ic with thickness of the comparative embodiment 1 and the embodiment 1, and the open star broken line and the solid star broken line are respectively the change of Jc with thickness of the comparative embodiment 1 and the embodiment 1.
2. Multilayer thick film structure diagram: the thick film provided by the embodiment 1 is respectively subjected to XRD, metallographic phase and Raman spectroscopy, and as shown in figures 3 and 4, the thick film formed by the embodiment has a similar 4-layer film structure, good structural compactness, uniform structure and basically no segregation.
3. Testing the thickness of the thick film: when the thick film provided by the embodiment 1 is subjected to a step meter test, as shown in fig. 5 and 6, the thick film provided by the embodiment 1 can be found to have the thickness of about 3.2 μm, and each layer structure is basically not layered and has uniform thickness.
4. Continuous production performance: when a long strip of 300m or more of the thick film provided in example 1 was subjected to Ic test, as shown in fig. 7, it was found that the Ic of the thick film produced by the method of the present invention was 1000A or more and the Ic data was stable when the thick film was continuously produced for 300m or more.
Claims (10)
1. A preparation method of a YBCO multilayer thick film is characterized by comprising the following steps:
coating and low-temperature treatment: coating a YBCO colloid on a texture substrate to obtain a colloid film, performing low-temperature treatment to obtain a low-temperature pyrolysis film, and repeating coating and low-temperature treatment to obtain M layers of low-temperature pyrolysis films, wherein M is more than or equal to 1;
high-temperature pretreatment: performing high-temperature pretreatment on the M low-temperature pyrolysis film to obtain a semi-grown film, wherein a YBCO layer is arranged on one side of the semi-grown film close to the texture substrate, and a non-epitaxial growth layer is arranged on one side of the semi-grown film far away from the texture substrate;
preparing a multilayer film: and coating the YBCO colloid on the non-epitaxial growth layer, and repeating the preparation of the semi-growth film to obtain a multilayer film.
2. The method of making a YBCO multilayer thick film according to claim 1, wherein said low temperature treatment comprises: heating the colloid membrane to 350-450 ℃ in the mixed atmosphere of oxygen and water vapor, and cooling to obtain a low-temperature pyrolysis membrane;
the high-temperature pretreatment comprises the following steps: and heating the low-temperature pyrolysis film to 750-800 ℃ in the mixed atmosphere of oxygen, water vapor and nitrogen, and preserving the temperature to obtain the semi-grown film.
3. The method for preparing a YBCO multilayer thick film according to claim 2, wherein the time of the low temperature treatment is 30 to 60min;
in the high-temperature pretreatment, the heating rate is 20-100 ℃/min, preferably 60-80 ℃/min, and the heat preservation time is 5-30 min.
4. The method for preparing the YBCO multilayer thick film according to claim 2, characterized in that the flow of the oxygen in the low-temperature treatment is 1-2L/min;
the oxygen content of the mixed atmosphere of the high-temperature pretreatment is 100-200 ppm, and the air pressure is 20-1000 Pa.
5. The method of making a YBCO multilayer thick film according to claim 1, wherein said YBCO colloid has a cation concentration of 1.5 to 2.5mol/L, said cation comprising a molar ratio of 1 to 1.5: 1.5-2: 3-3.6 of yttrium ions, barium ions and copper ions.
6. The method for preparing the YBCO multilayer thick film according to any one of claims 1-5, characterized in that after the preparation of the multilayer thin film, the multilayer thin film is subjected to high temperature treatment to obtain a YBCO thin film crystallized at high temperature.
7. The method of making a YBCO multilayer thick film according to claim 6, wherein said high temperature treatment comprises: and heating the multilayer film to 750-800 ℃ in the mixed atmosphere of oxygen, water vapor and nitrogen, and preserving the heat to obtain the high-temperature crystallized YBCO film.
8. The method for preparing the YBCO multilayer thick film according to claim 7, wherein the oxygen content of the mixed atmosphere of the high temperature treatment is 100-200 ppm, the air pressure is 20-1000 Pa, the temperature rising rate is 20-100 ℃/min, and the heat preservation time is 60-150 min.
9. The method of claim 6, wherein the high temperature crystallized YBCO film is post-processed.
10. The method of making a YBCO multilayer thick film according to claim 9, wherein said post-treatment comprises: cooling the YBCO superconducting film to 400-500 ℃, and cooling after heat preservation in an oxygen atmosphere.
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