CN114164490A - Method for preparing high-temperature superconducting oxide ceramic epitaxial film by heating through induction method - Google Patents
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Abstract
The invention discloses a method for realizing rapid epitaxial growth of a high-temperature superconducting oxide ceramic epitaxial film by heating with an induction method, which is used for the high-temperature crystallization step in the process of preparing a second-generation high-temperature superconducting tape superconducting layer by a metallorganic deposition method and comprises rapid heating and rapid epitaxial growth. The method prepares a precursor film of Yttrium Barium Copper Oxide (YBCO) on a metal substrate with a buffer layer by a fluorine-free metal organic deposition (FF-MOD) method, then the precursor film is placed in the center of a quartz tube, the film layer is rapidly heated by an induction heating coil outside the quartz tube, rapid epitaxial growth is realized, rapid heating and rapid epitaxial growth of an oxide film layer are realized by induction heating, impurities and formation of secondary phases are inhibited, and compared with the conventional method, the method reduces the reaction temperature and improves the growth rate of the material.
Description
Technical Field
The invention relates to the technical field of high-temperature superconducting materials, in particular to a method for realizing rapid epitaxial growth of a high-temperature superconducting oxide film in an induction heating mode.
Background
Yttrium barium copper oxide of the formula YBa2Cu3O7-δHereinafter abbreviated as YBCO. The high-temp. superconductive oxide film of yttrium barium copper oxide has high irreversible field and strong current-carrying capacityThe method has potential in the fields of medical treatment, electric power, traffic and the like. The Metal Organic Deposition (MOD) method in the chemical solution deposition method utilizes physical and chemical changes such as synthetic decomposition of organic matters to prepare the YBCO superconducting film, can accurately control raw material components, does not need high vacuum conditions, and belongs to a low-cost route. In the traditional fluorine-free metal organic deposition (FF-MOD) method, a YBCO high-temperature superconducting oxide film is generally subjected to high-temperature treatment within the range of 10-25 ℃/min, mainly the reaction between solid phases, the growth time of the film is more than 30min, generally 30-120 min, and BaCO which is one of the products of a precursor film3And the phase forming temperature of YBCO is stable, and the phase forming process is still remained on a crystal boundary after the phase forming process is finished, so that the transmission of current is influenced, and the performance is reduced.
Research shows that in the constant-pressure heating, the YBCO high-temperature superconducting oxide film is prepared by means of the rapid heating rate of 1 ℃/s-100 ℃/s, the time of the preparation process is shortened to 1/50 times of that of the traditional preparation process, and BaCO in the fluorine-free precursor film3React with CuO to generate BaCuO2During rapid heating, the formation of a transient liquid phase, Y, is promoted2O3The dissolution and diffusion are accelerated in the transient liquid phase, which is beneficial to widening the processing condition window of YBCO epitaxial growth, and the adjustment of process parameters can control BaCO3Eliminating reaction rate to avoid carbon retention in epitaxial film and solve BaCO in traditional FF-MOD method3The impact of the process. Thereby accelerating the epitaxial growth of the YBCO superconducting oxide film, but has the disadvantages of higher difficulty in rapid temperature rise, higher energy consumption, poor environmental protection property and the like.
Disclosure of Invention
The invention aims to provide a method for preparing a high-temperature superconducting oxide ceramic epitaxial film by heating through an induction method, which realizes the rapid heating and the rapid epitaxial growth of an oxide film layer through induction heating. Aiming at the characteristic of high-temperature crystallization of a fluorine-free precursor film, the method for realizing rapid epitaxial growth of the YBCO superconducting film is characterized in that an induction heating coil is utilized to generate eddy current heating for a metal layer below the YBCO precursor film prepared by an FF-MOD method, and the internal environment of a quartz tube is N2/O2The temperature rise rate of 1-200 ℃/s is realized under the atmosphere of the mixed gas, so that the precursor film is formedAnd the temperature is rapidly raised to the crystallization temperature, so that the rapid epitaxial growth of the YBCO high-temperature superconducting oxide film is realized.
In order to achieve the purpose, the invention adopts the following inventive concept:
the invention realizes the rapid temperature rise and the rapid epitaxial growth of the high-temperature superconducting oxide ceramic epitaxial film by using an induction heating mode. The induction heating method is a heating means which utilizes an electromagnetic induction method to generate current inside a heated material and achieves the heating purpose by depending on the energy of eddy current, and has wide and higher high-temperature areas in various industrial productions. The high efficiency of eddy heating is combined with the preparation of high-temperature superconducting materials, and the preparation of the high-temperature superconducting oxide ceramic epitaxial film is realized by a heating mode mainly using electric energy. Therefore, an induction heating rapid heating device which is efficient, energy-saving, low in consumption, environment-friendly, convenient and high in yield is developed, and the preparation of the high-temperature superconducting oxide ceramic epitaxial film can be realized in an induction heating mode.
When epitaxial crystallization is carried out, the growth of an intermediate phase can be inhibited through rapid temperature rise, so that a liquid phase appears at a lower temperature, the atomic diffusion process is accelerated, and the rapid epitaxial growth of a high-temperature superconducting oxide film layer is realized.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for preparing high-temperature superconducting oxide ceramic epitaxial film by induction heating comprises selecting a substrate, preparing a YBCO precursor film on a buffer layer, and placing the YBCO precursor film in the center of a quartz tube for rapid heating; introducing N into the quartz tube2/O2And (2) arranging an induction heating coil outside the quartz tube, carrying out induction heating through the induction heating coil, rapidly heating the YBCO precursor film at the heating rate of 1-200 ℃/s, carrying out high-temperature heat treatment, rapidly carrying out epitaxial growth on the YBCO precursor film, forming an epitaxial crystal film through rapid crystallization, and carrying out oxygen absorption treatment on the superconducting oxide film subjected to the high-temperature heat treatment to obtain the YBCO high-temperature superconducting oxide ceramic epitaxial film.
Preferably, the heating mode is induction heating, the heat source is mainly a metal substrate layer with a buffer layer, and the metal gasket is used for adjusting the heating rate, so that the rapid heating of the high-temperature superconducting oxide film is realized.
Preferably, the heating rate is 1-200 ℃/s; the crystallization time of the rapid crystallization, namely the epitaxial growth time is less than or equal to 5 min. Further preferably, the epitaxial growth time is less than or equal to 1 min.
Preferably, N with oxygen content of 100-10000 ppm is introduced into the quartz tube2/O2Mixing gas; preferably, the high-temperature heat treatment is carried out at the temperature of 740-840 ℃.
Preferably, the metal substrate having the buffer layer is LaMnO3/MgO/Al2O3/Y2O3/Hastelloy。
Preferably, the method for preparing the high-temperature superconducting oxide ceramic epitaxial film by heating by the induction method comprises the following steps:
(1) according to a stoichiometric ratio of Y, Ba to Cu of 1: 2: 3, dissolving yttrium acetate, barium acetate and copper acetate powder serving as raw materials in a propionic acid solvent, stirring, adding methanol, continuously stirring for dissolving, and finally fixing the volume to obtain YBCO colloid with the required ion concentration;
(2) coating a YBCO colloid on a metal substrate with a buffer layer to form a YBCO colloid film;
(3) placing the metal substrate coated with the YBCO colloid film and provided with the buffer layer in a tube furnace, drying, slowly heating to 400-500 ℃ at a heating rate of not higher than 5 ℃/min, and carrying out a low-temperature pyrolysis process to obtain a YBCO precursor film;
(4) placing the metal substrate with the buffer layer combined with the YBCO precursor film in the center of a quartz tube of an induction heating system for rapid heating, and carrying out high-temperature heat treatment on the YBCO precursor film;
(5) and carrying out oxygen absorption treatment on the superconducting oxide film subjected to high-temperature heat treatment, thereby preparing the high-temperature superconducting oxide ceramic epitaxial film.
Preferably, in the step (1), YBCO colloid having a total ion concentration of not less than 1.5mol/L is prepared.
Preferably, in the step (3), the metal with the buffer layer combined with the YBCO colloid filmThe substrate is placed in a tube furnace at O2Performing low-temperature pyrolysis at 400-500 ℃ in the atmosphere, then adding deionized water, and performing organic matter decomposition by using moist oxygen to finally obtain BaCO3、Y2O3And CuO.
Preferably, in the step (4), the YBCO precursor film is subjected to high-temperature heat treatment to obtain a high-temperature superconducting oxide ceramic epitaxial film.
Preferably, in the step (5), the temperature is maintained at 450 ℃ for at least 30min during the oxygen absorption treatment.
Preferably, the precursor film is placed in the center of a quartz tube in an induction heating system, an induction coil is arranged outside the quartz tube, and the atmosphere in the quartz tube is N2/O2And (4) mixing the gases. The principle is that by utilizing the principle of electromagnetic induction heating, when an induction heating power supply is electrified and alternating current is provided for a coil, the coil generates an alternating magnetic field, so that a metal basal layer below a buffer layer generates eddy current to heat, and the high-temperature phase forming temperature is reached at the heating rate of 1-100 ℃/s. The method is characterized in that the fluorine-free YBCO high-temperature superconducting oxide precursor film is heated by the induction coil, the heating rate is rapidly increased, and the complete growth of the epitaxial film can be realized within 5 minutes. The rapid temperature rise can inhibit the coarsening of a precursor phase, and the appearance of a transient liquid phase is accelerated in the crystallization process, so that the Y atom diffusion is accelerated, and the rapid growth of the YBCO epitaxial film is realized after the rapid nucleation growth of an interface.
The invention discloses a method for preparing a high-temperature superconducting oxide ceramic epitaxial film by an induction heating method. The temperature controller is connected with the induction heating power supply and controls the power supply to heat according to the set temperature curve. The infrared temperature measurement detects the temperature change in real time and feeds the temperature change back to the temperature controller so as to control the power supply to work. The oxide precursor film on the metal substrate with the buffer layer is arranged inside, the heat source is mainly the metal substrate layer, and a metal gasket can be used for further adjusting the heating rate.
The invention utilizes the principle of electromagnetic induction, an induction coil outside a quartz tube generates alternating magnetic flux inside the coil through alternating current given by a power supply, so that a metal substrate generates induced electromotive force to heat an oxide precursor film, and the rapid epitaxial growth of the YBCO superconducting film is realized.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the YBCO high-temperature superconducting oxide ceramic epitaxial film prepared by the method and the heating device of the invention has the following practical effects: with the increase of the temperature rise rate, the high-temperature pyrolysis phase forming time is shortened, the phase forming window is enlarged, and the preparation efficiency is improved; simultaneously reduces the coarsening problem of the precursor phase generated by the traditional slow temperature rise and the BaCO3The residue of the YBCO superconductive film is improved, so that the superconductive performance is improved;
2. the invention realizes the rapid heating and the rapid epitaxial growth of the oxide film layer by induction heating, inhibits the formation of impurities and secondary phases, reduces the reaction temperature and improves the growth rate of the material compared with the conventional method;
3. the induction heating rapid heating device has the advantages of high efficiency, energy conservation, low consumption, environmental protection, low cost, convenience and high yield, and can realize the high-quality preparation of the high-temperature superconducting oxide ceramic epitaxial film in an induction heating mode.
Drawings
Fig. 1 is a schematic view of an induction heating apparatus according to a preferred embodiment of the present invention.
1-a temperature controller; 2-an infrared thermometer; 3-a flange; 4-induction heating coil; 5-induction heating power supply; 6-quartz tube; 7-metal substrate with buffer layer and quartz plate.
FIG. 2 is a diagram showing a structure of a high-temperature superconducting oxide material according to a preferred embodiment of the present invention.
From bottom to top are respectively a metal layer, a buffer layer and a high-temperature superconducting oxide ceramic epitaxial film
FIG. 3 is an XRD pattern of a high-temperature superconducting epitaxial film of YBCO with rapid temperature rise and phase formation obtained in accordance with an embodiment of the present invention.
FIG. 4 is an XRD pattern of a high-temperature superconducting epitaxial film of YBCO with rapid temperature rise and phase formation obtained in example two of the present invention.
Fig. 5 is an SEM image of a high-temperature superconducting epitaxial film of YBCO that is obtained by the first and second embodiments of the present invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in this embodiment, a method for preparing a high temperature superconducting oxide ceramic epitaxial film by induction heating comprises the following steps:
(1) according to the metal organic salt raw materials of yttrium acetate, barium acetate and copper acetate, according to the ratio of Y: ba: cu atomic ratio of 1: 2: dissolving yttrium acetate, barium acetate and copper acetate powder serving as raw materials in a propionic acid solvent, stirring, adding methanol, continuously stirring for dissolving, and finally fixing the volume to obtain a YBCO colloid with the total cation concentration of 1.5 mol/L;
(2) adopts the metal substrate material with the buffer layer as LaMnO3/MgO/Al2O3/Y2O3Coating 1.5mol/L YBCO colloid on a metal substrate with a buffer layer by using a drawing machine to form a YBCO colloid film;
(3) placing the metal substrate coated with the YBCO colloid film and provided with the buffer layer in a tubular furnace, drying, slowly heating to 500 ℃ at the heating rate of 3 ℃/min, carrying out low-temperature pyrolysis in the wet oxygen atmosphere containing room-temperature deionized water, then cooling to 300 ℃, and changing the atmosphere into dry oxygen to obtain a YBCO superconducting oxide precursor film;
(4) placing a metal substrate with a buffer layer and combined with a YBCO precursor film in the center of a quartz tube, and introducing N with oxygen content of 5000ppm2/O2Heating the mixed gas at a heating rate of 20 ℃/s, respectively carrying out high-temperature heat treatment at 780 ℃ and 820 ℃ for 1 minute, rapidly heating, and carrying out high-temperature heat treatment on the YBCO precursor film;
(5) and carrying out oxygen absorption treatment on the superconducting oxide film subjected to high-temperature heat treatment, and keeping the temperature at 450 ℃ for 60min in a dry pure oxygen atmosphere to obtain the high-temperature superconducting oxide ceramic epitaxial film. See fig. 2.
Experimental test analysis:
in this embodiment, a high temperature superconducting oxide ceramic epitaxial film with texture is prepared by using a 5000ppm oxygen pressure, a temperature rise rate of 20 ℃/s, and a sintering temperature of 780 ℃ and 820 ℃ and having XRD as shown in fig. 3 and a surface morphology SEM as shown in fig. 5. The YBCO high-temperature superconducting film prepared by the method and the equipment of the invention forms a ceramic epitaxial film with good phase formation and better c-axis epitaxial texture within 1 minute, and does not have BaCO3The residue of (1). The induction heating equipment can realize the liquid phase auxiliary growth of the epitaxial film by utilizing the rapid temperature rise, and the YBCO high-temperature superconducting oxide film can be obtained in a short time, and the growth time is improved by at least 30 times compared with the traditional slow temperature rise growth time.
Referring to fig. 1, the induction heating apparatus of the present embodiment includes an induction coil 4, an induction heating power 5, an infrared thermometer 2, a temperature controller 1, a quartz tube 6, and a ventilation system. In the method for preparing the high-temperature superconducting oxide ceramic epitaxial film by heating through the induction method, a metal substrate with a buffer layer is selected as a substrate, a YBCO precursor film is prepared on the buffer layer, and then the substrate is placed in the center of a quartz tube for rapid heating; introducing N with oxygen content of 5000ppm into a quartz tube2/O2And (2) arranging an induction heating coil outside the quartz tube, carrying out induction heating through the induction heating coil, rapidly heating the YBCO precursor film at the heating rate of 20 ℃/s, carrying out high-temperature heat treatment, rapidly carrying out epitaxial growth on the YBCO precursor film, forming an epitaxial crystal film through rapid crystallization, and carrying out oxygen absorption treatment on the superconducting oxide film subjected to high-temperature heat treatment to obtain the YBCO high-temperature superconducting oxide ceramic epitaxial film.
Example two:
this embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, a method for preparing a high temperature superconducting oxide ceramic epitaxial film by induction heating comprises the following steps:
(1) according to the metal organic salt raw materials of yttrium acetate, barium acetate and copper acetate, according to the ratio of Y: ba: cu atomic ratio of 1: 2: dissolving yttrium acetate, barium acetate and copper acetate powder serving as raw materials in a propionic acid solvent, stirring, adding methanol, continuously stirring for dissolving, and finally fixing the volume to obtain a YBCO colloid with the total cation concentration of 1.5 mol/L;
(2) adopts the metal substrate material with the buffer layer as LaMnO3/MgO/Al2O3/Y2O3Coating 1.5mol/L YBCO colloid on a metal substrate with a buffer layer by using a drawing machine to form a YBCO colloid film;
(3) placing the metal substrate coated with the YBCO colloid film and provided with the buffer layer in a tubular furnace, drying, slowly heating to 500 ℃ at the heating rate of 3 ℃/min, carrying out low-temperature pyrolysis in the wet oxygen atmosphere containing room-temperature deionized water, then cooling to 300 ℃, and changing the atmosphere into dry oxygen to obtain a YBCO superconducting oxide precursor film;
(4) placing a metal substrate with a buffer layer and combined with a YBCO precursor film in the center of a quartz tube, and introducing N with the oxygen content of 10000ppm2/O2Heating the mixed gas at a heating rate of 20 ℃/s, respectively carrying out high-temperature heat treatment at 740 ℃, 780 ℃ and 820 ℃ for 1 minute, rapidly heating, and carrying out high-temperature heat treatment on the YBCO precursor film;
(5) and carrying out oxygen absorption treatment on the superconducting oxide film subjected to high-temperature heat treatment, and keeping the temperature at 450 ℃ for 60min in a dry pure oxygen atmosphere to obtain the high-temperature superconducting oxide ceramic epitaxial film.
Experimental test analysis:
in this embodiment, a sintered temperature of 740 ℃ and 820 ℃ is adopted at a rate of 20 ℃/s and an oxygen pressure of 10000ppm, and the prepared YBCO high-temperature superconducting oxide epitaxial film XRD is as shown in fig. 4, and the surface morphology SEM is as shown in fig. 5, and is a textured high-temperature superconducting oxide ceramic epitaxial film. The YBCO high-temperature superconducting thin film prepared by the method and the equipment of the embodiment can form a ceramic epitaxial film with good epitaxial texture within 1 minute, and does not contain BaCO3The residue of (1). The induction heating equipment can realize the liquid phase auxiliary growth of the epitaxial film by utilizing the rapid temperature rise, and the YBCO high-temperature superconducting oxide film can be obtained in a short time. Meanwhile, the epitaxial growth characteristics of the a/b axis obviously change along with the increase of the oxygen pressure and the change of the sintering temperature.
The invention is mainly used for the high-temperature crystallization step in the process of preparing a second-generation high-temperature superconducting tape superconducting layer by a Metal Organic Deposition (MOD) method, and comprises the steps of rapid heating and rapid epitaxial growth. Firstly, preparing a Yttrium Barium Copper Oxide (YBCO) precursor film on a metal substrate with a buffer layer by a fluorine-free metal organic deposition (FF-MOD) method, then placing the precursor film in the center of a quartz tube, rapidly heating the film layer by an induction heating coil outside the quartz tube, realizing rapid epitaxial growth, rapidly heating and rapidly epitaxial growth of an oxide film layer by induction heating, and inhibiting the formation of impurities and secondary phases.
The embodiments of the present invention have been described above with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention should be replaced with equivalents as long as the object of the present invention is met, and the technical principle and the inventive concept of the present invention are not departed from the scope of the present invention.
Claims (6)
1. A method for preparing a high-temperature superconducting oxide ceramic epitaxial film by heating by an induction method is characterized by comprising the following steps: selecting a substrate which is a metal base with a buffer layer, preparing a YBCO precursor film on the buffer layer, and then placing the substrate in the center of a quartz tube for rapid heating; introducing N into the quartz tube2/O2Mixing gas, arranging an induction heating coil outside the quartz tube, carrying out induction heating through the induction heating coil to ensure that the YBCO precursor film is rapidly heated up at the heating rate of 1-200 ℃/s, carrying out high-temperature heat treatment to ensure that the YBCO precursor film is rapidly epitaxially grown, and carrying out rapid crystallizationForming an epitaxial crystal film, and then carrying out oxygen absorption treatment on the superconducting oxide film subjected to high-temperature heat treatment to obtain the YBCO high-temperature superconducting oxide ceramic epitaxial film.
2. The method for preparing the epitaxial film of the high-temperature superconducting oxide ceramic by heating according to the induction method of claim 1, wherein: the heating mode is induction heating, the heat source is mainly a metal basal layer with a buffer layer, and the heating rate is adjusted by assisting a metal gasket, so that the rapid heating of the high-temperature superconducting oxide film is realized.
3. The method for preparing the epitaxial film of the high-temperature superconducting oxide ceramic by heating according to the induction method of claim 1, wherein: the heating rate is 1-200 ℃/s; the crystallization time of the rapid crystallization, namely the epitaxial growth time is less than or equal to 5 min.
4. The method for preparing the epitaxial film of the high-temperature superconducting oxide ceramic by heating according to the induction method of claim 1, wherein: introducing N with the oxygen content of 100-10000 ppm into a quartz tube2/O2And (3) carrying out high-temperature heat treatment on the mixed gas at the temperature of 740-840 ℃.
5. The method for preparing the epitaxial film of the high-temperature superconducting oxide ceramic by heating according to the induction method of claim 1, wherein: the metal substrate with the buffer layer is LaMnO3/MgO/Al2O3/Y2O3/Hastelloy。
6. The method for preparing the epitaxial film of the high-temperature superconducting oxide ceramic by heating according to the induction method of claim 1, wherein: the method comprises the following steps:
(1) according to a stoichiometric ratio of Y, Ba to Cu of 1: 2: 3, dissolving yttrium acetate, barium acetate and copper acetate powder serving as raw materials in a propionic acid solvent, stirring, adding methanol, continuously stirring for dissolving, and finally fixing the volume to obtain YBCO colloid with the required ion concentration;
(2) coating a YBCO colloid on a metal substrate with a buffer layer to form a YBCO colloid film;
(3) placing the metal substrate coated with the YBCO colloid film and provided with the buffer layer in a tubular furnace, drying and heating to 400-500 ℃ to obtain a YBCO precursor film serving as a fluorine-free low-temperature pyrolysis film;
(4) placing the metal substrate with the buffer layer combined with the YBCO precursor film in the center of a quartz tube for rapid heating, and carrying out high-temperature heat treatment on the YBCO precursor film;
(5) and carrying out oxygen absorption treatment on the superconducting oxide film subjected to high-temperature heat treatment, thereby preparing the high-temperature superconducting oxide ceramic epitaxial film.
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| CN116477948A (en) * | 2023-03-31 | 2023-07-25 | 上海大学 | Method for preparing superconducting film based on fluorine-free chemical solution oxygen pressure switching method |
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