CN111825444B - Method for introducing columnar defects into ex-situ high-temperature superconducting thin film - Google Patents
Method for introducing columnar defects into ex-situ high-temperature superconducting thin film Download PDFInfo
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- CN111825444B CN111825444B CN202010770668.XA CN202010770668A CN111825444B CN 111825444 B CN111825444 B CN 111825444B CN 202010770668 A CN202010770668 A CN 202010770668A CN 111825444 B CN111825444 B CN 111825444B
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Abstract
The invention relates to a method for introducing columnar defects into an ex-situ high-temperature superconducting film, which mainly solves the technical problem that the energy level required for manufacturing the columnar defects by laser irradiation is very high. The invention creatively provides a method for introducing columnar defects through femtosecond laser irradiation in the phase forming intermediate process of a YBCO superconducting film strip. Namely, various types of irradiation in the vertical direction on the surface of an intermediate product are carried out in the preparation process, so that the defect of preferred orientation is generated, and further, the columnar defect is introduced into a final product. The practical application of the YBCO superconducting tape is improved.
Description
Technical Field
The invention relates to a method for introducing columnar defects into an ex-situ high-temperature superconducting film, which is characterized in that femtosecond laser irradiation in the vertical direction of the surface of an intermediate product is carried out in the preparation process to generate preferentially oriented defects, and then the columnar defects are introduced into a final product, and belongs to the field of material design and processing.
Background
Yttrium barium copper oxide (YBa) 2 Cu 3 O 7-δ YBCO) high-temperature superconducting films have been the focus of research in the field of practical superconductivity due to their excellent performance and potential price advantage. However, the practical application of the current YBCO superconducting thin film still faces two problems: firstly, a Josephson type weak connection phenomenon exists between crystal boundaries of a YBCO superconducting film, so that the inside of a superconductor crystal grain and the crystal boundaries have different current carrying capacities, and the improvement of critical current density is limited; secondly, the application of the YBCO superconducting film in many fields is limited by the lower critical current density under an external magnetic field, so that the improvement of the field performance is necessary.
As a second type of superconductor, YBCO is exposed to an external magnetic fieldH Above the lower critical field, a mixed state with magnetic flux eddy lines is present, the movement of the eddy lines under the Lorentz force causing a superconductor critical current density ( Jc) A sharp drop in. For an undoped YBCO superconductor:ab the presence of intrinsic pinning centers in the plane,J(θ) Will be atH‖abA strong peak value exists when the surface is flat; for thec The axis, due to the lack of corresponding intrinsic pinning centers,H‖cin the axial directionJcIt is much smaller; so in the undoped YBCO thin filmThe critical current density exhibits a large anisotropy.
In order to improve the electric transport performance of the YBCO superconducting film in an external magnetic field, researchers introduce a magnetic flux pinning center into the YBCO superconducting film by manual means for pinning the movement of a magnetic flux vortex line. The Artificial Pinning Centers (APCs) are classified into: (1) zero-dimensional APCs, oxygen vacancies, element substitution and other point defects existing in a superconductor; (2) the one-dimensional APCs comprise linear dislocation or artificially formed nano-columns which appear in the superconductor, (3) the two-dimensional APCs have defects that stacking faults, nano-sheets, twin crystal boundaries and the like which exist in the superconductor can become pinning centers, and (4) the three-dimensional APCs take nano-scale heterogeneous particles which are dispersedly distributed in the superconductor as the main pinning centers.
The method for introducing the artificial pinning center comprises the following steps: (1) high-energy heavy particle beam irradiates high-temperature YBCO superconductor to generatecLine defects of axial alignment; (2) adding second phase nanoparticles including BaMO 3 (M = Zr, Hf, Sm, etc.) perovskite structure compounds; (3) depositing a layer of nano particles on a metal substrate and then epitaxially growing YBCO. Currently, the addition of second phase nanoparticles is an effective means. However, whether the in-situ method or the ex-situ method is adopted to add the second phase nano particles, firstly, the preparation and growth of the YBCO film can be directly influenced, the technological parameters need to be adjusted in time, and secondly, the size and the distribution of the nano particles have great influence on the performance of the YBCO superconducting film and are sensitive to the preparation process. High-energy heavy particle beam radiation is used as a pure and additive-free means, and is to directly carry out heavy particle bombardment on a well-grown YBCO superconducting film to manufacture a film parallel to the surface of the filmcSmall size in the axial direction and uniform distribution of columnar physical defects. Research shows that the defects formed by irradiation can be effectively improvedH‖cIn the axial directionJcAnd the practical application potential value of the YBCO coating conductor is improved.
In the process of preparing the YBCO superconducting tape by a metal organic solution chemical method (TFA-MOD), the raw materials are subjected to the steps of precursor liquid preparation, low-temperature coating and pyrolysis, medium-temperature presintering, high-temperature phase-forming sintering, oxygen absorption, silver-plated protective layer, packaging and the like respectively, and finally the YBCO high-temperature superconducting tape which can be used commercially is formed. In the whole process, the low-temperature coating film shrinks by 100% from colloid to the pyrolytic film; after the intermediate-temperature pre-sintering, the film shrinks by 10 percent again; and finally, sintering at high temperature, and enabling the film to shrink by 50% of the thickness again. In the means of introducing artificial pinning centers, the surface modification of the substrate occurs before the coating step of YBCO raw materials, the addition of second-phase nano particles occurs in the preparation process of YBCO precursor liquid, and the radiation of high-energy particles at present directly acts on a high-temperature crystallized film. Generally, high-energy heavy particles are irradiated on a YBCO dense ceramic film sintered into a phase at high temperature to effectively bombard columnar defects, but the required energy level is very high, and the energy level is generally higher than GeV. By adjusting the energy level of the particle beam radiated by the high-energy particles, the defect size and density distribution in the film can be directly and effectively controlled. This is currently difficult to achieve by other means. However, high energy particle irradiation also has its limitation that the energy level for making columnar defects is high. If the particle irradiation method is applied to the large-scale industrial manufacture of YBCO superconducting tapes, the equipment and energy cost is too large.
Disclosure of Invention
The invention aims to provide a method for introducing columnar defects into an ex-situ high-temperature superconducting film, which mainly solves the technical problem that the energy level required for manufacturing the columnar defects by laser irradiation is very high. The idea of the invention is as follows: the method for introducing the columnar defects through femtosecond laser irradiation in the intermediate phase process of the YBCO superconducting thin film strip is provided creatively. The method is characterized in that various types of irradiation in the vertical direction of the surface of an intermediate product are carried out in the preparation process, so that the defect of preferred orientation is generated, and then the columnar defect is introduced into a final product, and the method belongs to the field of material design and processing.
The technical scheme of the invention is as follows: the method for introducing columnar defects into the ex-situ high-temperature superconducting thin film comprises the following steps of:
(1) preparing a YBCO precursor solution: weighing raw materials of yttrium acetate, barium acetate and copper acetate, dissolving the yttrium acetate and the barium acetate in deionized water and trifluoroacetic acid, stirring, dissolving the copper acetate in the deionized water and propionic acid, and stirring; adding methanol into the two solutions, carrying out reduced pressure distillation for three times, mixing, adding methanol to a constant volume, and preparing a YBCO precursor solution;
(2) spin coating: spin-coating TFA-YBCO precursor liquid on a Hastelloy substrate on a spin-coating machine to obtain a precursor film;
(3) low-temperature treatment: placing the film obtained by spin coating in a muffle furnace for low-temperature pyrolysis, introducing oxygen into room-temperature deionized water, and then introducing the oxygen into a hearth, wherein the film is subjected to low-temperature treatment in the hearth;
(4) intermediate temperature treatment: performing medium temperature treatment on the low-temperature treated pyrolytic film in the atmosphere of oxygen and water vapor to obtain a medium-temperature treated film;
(5) and (3) femtosecond laser irradiation punching: horizontally placing the low-temperature pyrolysis film or the medium-temperature treatment film, placing the surface coated with the raw material upwards, and irradiating and punching by femtosecond laser vertical to the plane of the film;
(6) high-temperature treatment: the irradiated film is subjected to high-temperature heat treatment in a high-temperature hearth, wherein the atmosphere is nitrogen, oxygen and water vapor; then cooling in the nitrogen and oxygen atmosphere to obtain a high-temperature crystallized YBCO film with irradiation columnar physical defects;
(7) and (3) post-treatment: and then carrying out oxygen absorption treatment on the high-temperature crystallization film, and keeping the temperature in pure oxygen for a period of time to obtain the yttrium barium copper oxide superconducting film strip.
In the step (1), yttrium acetate, barium acetate and copper acetate are weighed according to the stoichiometric ratio of 1:2: 3; the stirring time is 1-2 h, and the total cation concentration of the prepared YBCO precursor solution is 2.5 mol/L.
In the step (2), the spin coater adopts the rotating speed of 3000-.
In the step (3), the low-temperature treatment is carried out in such a way that the temperature of a hearth is reduced from 350 ℃ to 150 ℃ within 40 min.
In the step (4), the medium-temperature treatment is heat treatment at 600 ℃ for 10 min, the total pressure of water vapor and oxygen atmosphere is about 20-23 Pa, preferably the oxygen pressure is 13 Pa, and the water vapor pressure is 10 Pa.
The step (5), the femtosecond laser energy is 4-10μJ, preferably 5μJ, spot diameter about 2μm。
In the step (6), the high-temperature treatment is to heat the room temperature to 780 ℃ at a heating rate of 25 ℃, the temperature is kept for 120 min, wherein the atmosphere in the first 60 min of heat preservation time is nitrogen-oxygen mixed gas (the air pressure is 1 atm) with the oxygen content of 150 ppm, and the mixed gas is firstly introduced into a water bath at the temperature of 35 ℃ and then enters a hearth of a muffle furnace; the atmosphere of the later 60 min heat preservation time is dry nitrogen-oxygen mixed gas.
In the step (7), in the post-treatment, after the heat preservation in the step (6) is finished, the temperature is reduced to 450 ℃ along with the furnace, the heat preservation is carried out for 60 min, and the reaction atmosphere in the process is changed from the nitrogen-oxygen mixed gas to pure oxygen atmosphere; and cooling to room temperature along with the furnace after the heat preservation is finished.
And then sintering the pyrolytic film with the columnar defects at high temperature to obtain the high-temperature crystallized YBCO superconducting film with the columnar defects. The femtosecond laser is radiated perpendicular to the surface of the sample, and the columnar defect formed on the YBCO low-temperature pyrolysis film can also break down the film to form a channel of columnar defect perpendicular to the surface of the film.
The thickness range of the YBCO low-temperature pyrolysis film for manufacturing the columnar defects is 100-3000 nm.
The columnar defects can directly and effectively control the size and density distribution of the columnar defects by adjusting the energy and the intensity of the femtosecond laser.
The invention has the beneficial effects that: defects are introduced in the intermediate link of preparation of the YBCO superconducting film and the coating conductor thereof, and researches show that the low-temperature pyrolysis film and the medium-temperature pre-sintering film before the high-temperature crystallization step are loose in structure, so that columnar defects can be bombarded and manufactured on the film by adopting femtosecond laser irradiation with lower energy level, and effective artificial pinning centers are finally formed.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a surface topography (SEM) of the low-temperature pyrolysis film obtained in example 1 of the present invention after femtosecond laser drilling.
FIG. 3 is a surface topography (SEM) of the mesophilic treated film obtained in example 1 of the present invention after femtosecond laser drilling.
FIG. 4 is a surface topography (SEM) of the perforated low-temperature pyrolytic film obtained in example 1 of the invention after high-temperature crystallization.
FIG. 5 is a surface topography (SEM) of the punched middle-temperature processed film obtained in example 1 of the present invention after high-temperature crystallization.
Detailed Description
The present invention is further illustrated by the following examples, which are to be construed as merely illustrative, and not a limitation of the present invention. With reference to figure 1 of the drawings,
the process for preparing the YBCO superconducting thin film by the TFA-MOD method comprises the following steps:
1. raw materials of yttrium acetate, barium acetate and copper acetate are weighed according to the stoichiometric ratio (1: 2: 3.3), yttrium acetate and barium acetate are dissolved in a proper amount of deionized water and excessive trifluoroacetic acid and stirred for 1-2 hours, and copper acetate is dissolved in a proper amount of deionized water and excessive propionic acid and stirred for 1-2 hours. Methanol is added into the two solutions to carry out reduced pressure distillation for three times, then the two solutions are mixed, and methanol is added to a constant volume to prepare YBCO precursor solution with the total cation concentration of 2.5 mol/L.
2. And spin-coating the YBCO precursor liquid with the total cation concentration of 2.5 mol/L on the surface of the Hastelloy alloy substrate by adopting the rotating speed of 3000-6000 rpm on a spin-coating machine for 1 min.
3. And (3) 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, carrying out low-temperature treatment on the film in the hearth for 40min, and reducing the temperature from 350 ℃ to 150 ℃ within the time.
4. And (3) carrying out heat treatment on the low-temperature treated pyrolytic film at 600 ℃ for 10 min under the atmosphere of 13 Pa oxygen and 10 Pa water vapor to obtain a medium-temperature treated film.
5. Horizontally placing the low-temperature pyrolysis film or the medium-temperature treatment film, placing the surface coated with the raw material upwards, and placing the film under femtosecond laser for vertical irradiation punching; the femtosecond laser energy is 5μJ, spot diameter 2μAnd m is selected. The surface appearance of the low-temperature pyrolysis film after femtosecond laser drilling is shown in figure 2, and the surface appearance of the medium-temperature treatment film after femtosecond laser drillingSee fig. 3 for an external view.
6. Heating the irradiated film to 780 ℃ from room temperature at a heating rate of 25 ℃ in a high-temperature hearth, and preserving heat for 120 min, wherein the atmosphere in the first 60 min of heat preservation time is nitrogen-oxygen mixed gas (the air pressure is 1 atm) with the oxygen content of 150 ppm, and the mixed gas is firstly introduced into a water bath at 35 ℃ and then enters a muffle furnace hearth; the atmosphere of the later 60 min heat preservation time is dry nitrogen-oxygen mixed gas. The surface appearance of the perforated low-temperature pyrolysis film after high-temperature crystallization is shown in figure 4, and the surface appearance of the perforated medium-temperature treatment film after high-temperature crystallization is shown in figure 5.
7. After the heat preservation is finished, oxygen absorption treatment is carried out, namely, the temperature is reduced to 450 ℃ along with the furnace, the heat preservation is carried out for 60 min, and the reaction atmosphere is changed from nitrogen-oxygen mixed gas 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 yttrium barium copper oxide superconducting film strip after oxygen absorption.
Claims (7)
1. A method for introducing columnar defects into a high-temperature superconducting thin film by an ex-situ method is characterized by comprising the following steps: the method comprises the following steps:
(1) preparing a YBCO precursor solution: weighing raw materials of yttrium acetate, barium acetate and copper acetate, dissolving the yttrium acetate and the barium acetate in deionized water and trifluoroacetic acid, stirring, dissolving the copper acetate in the deionized water and propionic acid, and stirring; adding methanol into the two solutions, carrying out reduced pressure distillation for three times, mixing, adding methanol to a constant volume, and preparing a YBCO precursor solution;
(2) spin-coating TFA-YBCO precursor liquid on a Hastelloy substrate on a spin-coating machine to obtain a precursor film;
(3) low-temperature treatment: placing the film obtained by spin coating in a muffle furnace for low-temperature pyrolysis, introducing oxygen into room-temperature deionized water, and then introducing oxygen into a hearth, wherein the film is subjected to low-temperature treatment in the hearth; the low-temperature treatment is that the temperature of a hearth is reduced to 150 ℃ within 40 min;
(4) intermediate temperature treatment: performing medium temperature treatment on the low-temperature treated pyrolytic film in the atmosphere of oxygen and water vapor to obtain a medium-temperature treated film; the medium temperature treatment is 600 ℃ heat treatment for 10 min;
(5) and (3) femtosecond laser irradiation punching: horizontally placing the low-temperature pyrolysis film or the medium-temperature treatment film, placing the surface coated with the raw material upwards, and irradiating and punching by femtosecond laser vertical to the plane of the film;
(6) high-temperature treatment: the irradiated film is subjected to high-temperature heat treatment in a high-temperature hearth, wherein the atmosphere is nitrogen, oxygen and water vapor; then cooling in the atmosphere of nitrogen and oxygen to obtain a high-temperature crystallized YBCO film with irradiation columnar physical defects;
(7) and (3) post-treatment: and then carrying out oxygen absorption treatment on the high-temperature crystallization film, and keeping the temperature in pure oxygen for a period of time to obtain the yttrium barium copper oxide superconducting film strip.
2. The method of introducing columnar defects into an ex-situ high temperature superconducting thin film as claimed in claim 1, wherein: in the step (1), yttrium acetate, barium acetate and copper acetate are weighed according to the stoichiometric ratio of 1:2: 3.3; the stirring time is 1-2 h, and the total cation concentration of the prepared YBCO precursor solution is 2.5 mol/L.
3. The method for introducing columnar defects into an ex-situ high temperature superconducting thin film as claimed in claim 1, wherein: and (2) in the step (2), the rotating speed is 3000 and 6000 rpm during spin coating, and the time duration is 1 min.
4. The method of introducing columnar defects into an ex-situ high temperature superconducting thin film as claimed in claim 1, wherein: in the step (5), the femtosecond laser energy is 4-10μJ。
5. The method for introducing columnar defects into an ex-situ high temperature superconducting thin film as claimed in claim 4, wherein: femtosecond laser energy of 5μJ, the diameter of the light spot is 2μm。
6. The method of introducing columnar defects into an ex-situ high temperature superconducting thin film as claimed in claim 1, wherein: in the step (6), the high-temperature treatment is performed at 780 ℃ for 120 minutes, and the heat preservation is performed for 120 minutes, wherein the atmosphere in the first 60 minutes of heat preservation time is wet nitrogen-oxygen mixed gas with the oxygen content of 150 ppm which is firstly introduced into a water bath at 35 ℃; the atmosphere in the later 60 min heat preservation time is dry nitrogen-oxygen mixed gas.
7. The method of introducing columnar defects into an ex-situ high temperature superconducting thin film as claimed in claim 1, wherein: and (7) in the post-treatment, pure oxygen atmosphere is adopted, the air pressure is 1 atm, the oxygen absorption treatment temperature is 450 ℃, the temperature is kept for 60 min, and finally, the temperature is naturally reduced.
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