CN106242553A - A kind of preparation method of high-temperature superconductor REBCO thin film - Google Patents

A kind of preparation method of high-temperature superconductor REBCO thin film Download PDF

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CN106242553A
CN106242553A CN201610623602.1A CN201610623602A CN106242553A CN 106242553 A CN106242553 A CN 106242553A CN 201610623602 A CN201610623602 A CN 201610623602A CN 106242553 A CN106242553 A CN 106242553A
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floride
free
fluorine
thin film
preparation
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CN106242553B (en
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金利华
冯建情
李成山
王耀
张平祥
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Northwest Institute for Non Ferrous Metal Research
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    • 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
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Abstract

The invention provides the preparation method of a kind of high-temperature superconductor REBCO thin film, the method comprises the following steps: one, prepare floride-free precursor liquid according to the atomic ratio of RE: Ba: Cu=1: 1.75: 3；Two, by RE: Ba: Cu=1: (1.5～2): the atomic ratio of 3 prepares fluorine-containing precursor liquid；Three, use spin-coating method that described floride-free precursor liquid is coated uniformly on LaAlO3On substrate, after heat treatment obtain floride-free monolayer precursor film；Four, use spin-coating method to be coated uniformly on by fluorine-containing precursor liquid on floride-free monolayer precursor film, after heat treatment obtain free-floride/fluorine-containing double-deck precursor film；Five, described free-floride/fluorine-containing double-deck precursor film after heat treatment obtains REBCO superconducting thin film.Preparation method of the present invention is simple, and the high-temperature superconductor REBCO thin film of preparation has sharp keen cube orientation and excellent superconductivity, and improves high-temperature superconductor REBCO thin film current-carrying performance under 77K.

Description

A kind of preparation method of high-temperature superconductor REBCO thin film
Technical field
The invention belongs to high temperature superconducting materia technical field, be specifically related to the preparation side of a kind of high-temperature superconductor REBCO thin film Method.
Background technology
The multilayer materials that coating conductor is made up of metal base band/cushion/superconducting layer/protective layer.Due to its Current capacity excellent under High-Field, will be that high temperature superconducting materia really realizes the unique hope in the application of liquid nitrogen temperature forceful electric power, closely The core superconductor of always developed country's development over Nian.Low cost chemical solution deposition technique is used to prepare at present REBa2Cu3Oy(REBCO) superconducting layer becomes one of study hotspot.
Chemical solution deposition prepare high-temperature superconductor REBCO thin film generally comprise precursor liquid prepare, apply, be pyrolyzed, crystallization With ooze the steps such as oxygen.Become mechanism classification mutually according to superconducting layer, substantially comprise two classes.The first uses floride-free presoma to obtain free-floride Precursor liquid, becoming phase process is that presoma is decomposed to form BaCO3、CuO、RE2O3, the reaction of these three compound generates REBCO superconduction Phase.The second uses fluorine-containing presoma preparation tradition perfluor precursor liquid, becomes camera to be made as " BaF2Mechanism ".The most fluorine-containing presoma divides Solution becomes BaF2、CuO、RE2O3, BaF2It is converted into BaO, further with CuO, RE by reacting with water2O3Reaction, ultimately forms REBCO superconducting phase.Both approaches has certain defect, wherein first method in preparation process containing being difficult to decompose Brium carbonate, it is generally required to relatively high crystallization temperature just can completely remove, residual carbon hydrochlorate can cause the performance of REBCO superconducting thin film to drop Low.Second method Oil repellent can cause into phase process liquid phase and be formed too much, non-oriented forming core, poor growth occurs, also can lead Cause performance reduces.
Summary of the invention
The technical problem to be solved is for above-mentioned the deficiencies in the prior art, it is provided that a kind of high-temperature superconductor The preparation method of REBCO thin film.The method is prepared for floride-free/fluorine-containing double-deck precursor film of REBCO, by the fluorine-containing precursor film in upper strata Being diffused in lower floor's free-floride precursor film of fluorine, it is suppressed that the carbon content in lower floor's free-floride precursor film, biaxial orientation can be promoted Forming core, it is to avoid residual brium carbonate reduces the performance of superconducting thin film.Meanwhile, along with in the fluorine-containing precursor film in upper strata fluorine progressively to lower floor Floride-free precursor film diffusion, the Oil repellent in the fluorine-containing precursor film in upper strata reduces, advantageously reduces the fluorine-containing precursor film in upper strata and become phase process Liquid phase, reduce any bodily form core, form extension fast-growth.
For solving above-mentioned technical problem, the technical solution used in the present invention is: the preparation of a kind of high-temperature superconductor REBCO thin film Method, it is characterised in that the method comprises the following steps:
Step one, the floride-free precursor liquid of preparation: by the propionate of RE, barium propionate, propanoic acid copper according to RE: Ba: Cu=1: 1.75: The atomic ratio of 3 is dissolved in the mixed solvent of propanoic acid and ethanol, stirs to being completely dissolved under conditions of 40 DEG C～100 DEG C, To the floride-free precursor liquid that total cation molar concentration is 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: (1～10)；The propionate of described RE is propanoic acid yttrium or propanoic acid gadolinium；
Step 2, prepare fluorine-containing precursor liquid: by the propionate of RE, the organic salt of barium, propanoic acid copper by RE: Ba: Cu=1: (1.5～2): the atomic ratio of 3 is dissolved in the mixed solvent of propanoic acid and ethanol, under conditions of 40 DEG C～100 DEG C, stirring is to complete CL, obtains the fluorine-containing precursor liquid that total cation molar concentration is 1.5mol/L～2mol/L；Propanoic acid in described mixed solvent It is 1 with the volume ratio of ethanol: (1～10)；The propionate of described RE is propanoic acid yttrium or propanoic acid gadolinium；The organic salt of described barium is trifluoro The mixture of Barium acetate or trifluoroacetic acid barium and barium propionate；
The propionate of RE described in step 2 is identical with the propionate of RE described in step one；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, being subsequently placed in temperature is 120 DEG C～the quartz tube furnace of 200 DEG C, and logical in described quartz tube furnace Enter the oxygen atmosphere of humidity, with the ramp of 5 DEG C/min to 400 DEG C～500 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain To floride-free monolayer precursor film；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 Being coated in described in step 3 on floride-free monolayer precursor film, being subsequently placed in temperature is 120 DEG C～the quartz tube furnace of 200 DEG C, and The oxygen atmosphere of humidity it is passed through in described quartz tube furnace, with the ramp of 5 DEG C/min to 400 DEG C～500 DEG C, constant temperature 10min, cools to room temperature with the furnace and obtains free-floride/fluorine-containing double-deck precursor film；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through, the most again with the ramp of 10 DEG C/min～100 DEG C/min the most extremely to described quartz tube furnace 770 DEG C～810 DEG C, it is incubated 1h～2h, when furnace temperature is down to 450 DEG C, is incubated 1h carries out oozing oxygen process, cool to room temperature with the furnace, To critical temperature high-temperature superconductor REBCO thin film more than liquid nitrogen temperature (77K).
The preparation method of above-mentioned high-temperature superconductor REBCO thin film, it is characterised in that stir described in step one and step 2 Time be 1h～3h.
The preparation method of above-mentioned high-temperature superconductor REBCO thin film, it is characterised in that in the organic salt of barium described in step 2 The mole percent of trifluoroacetic acid barium is not less than 15%.
The preparation method of above-mentioned high-temperature superconductor REBCO thin film, it is characterised in that spin coating described in step 3 and step 4 Rotating speed be 500r/min～4500r/min, the time of described spin coating is 30s～180s.
The preparation method of above-mentioned high-temperature superconductor REBCO thin film, it is characterised in that humidity described in step 3 and step 4 In oxygen atmosphere, the volumn concentration of oxygen is 97%～98%, and surplus is steam.
The preparation method of above-mentioned high-temperature superconductor REBCO thin film, it is characterised in that argon oxygen mixing moist described in step 5 In gas, the volumn concentration of argon is 95.73%～98.78%, and the volumn concentration of oxygen is 0.02%～0.07%, Surplus is steam.
The present invention compared with prior art has the advantage that
1, the present invention is prepared for the free-floride/fluorine-containing double-deck precursor film of REBCO thin film, and the lower floor of this precursor film is floride-free forerunner Film, upper strata is fluorine-containing precursor film, is diffused in lower floor's free-floride precursor film by the fluorine in the fluorine-containing precursor film in upper strata, it is suppressed that lower floor Carbon content in floride-free precursor film, can promote biaxial orientation forming core in lower floor's free-floride precursor film, it is to avoid residual brium carbonate reduces super Lead the superconductivity of thin film, simultaneously along with in the fluorine-containing precursor film in upper strata fluorine progressively to lower floor's free-floride precursor film diffusion, upper strata forerunner Oil repellent in film reduces, this liquid phase being beneficial to reduce into phase process, reduces any bodily form core, forms extension fast-growth, this The high-temperature superconductor REBCO thin film that invention prepares solves the floride-free presoma of tradition or perfluor presoma prepares REBCO thin film superconduction The problem that performance is the best.
2, in the free-floride of REBCO thin film of the present invention/fluorine-containing double-deck precursor film, fluorine diffusion can be formed in double-deck precursor film Fluorine gradient, weakens the impact at superconducting layer interface, it is to avoid the interface enrichment of copper fluorine-containing precursor film on upper strata, beneficially epitaxial growth Cross over interface, make superconducting thin film become an entirety.By reducing the cavity blemish in superconducting thin film, improve high-temperature superconductor thin The uniformity of film, is integrally improved the superconductivity of high-temperature superconducting thin film.
3, preparation method of the present invention is simple, and the high-temperature superconductor REBCO thin film of preparation has sharp keen cube orientation, has good Good superconductivity, and improve high-temperature superconductor REBCO thin film current-carrying under 77K by the structure improving superconducting thin film Energy.
Below by drawings and Examples, technical scheme is described in further detail.
Accompanying drawing explanation
Fig. 1 is the X diffracting spectrum of the HTS YBCO thin film of the embodiment of the present invention 1 preparation.
Fig. 2 is the scanning electron microscope collection of illustrative plates of the HTS YBCO thin film of the embodiment of the present invention 1 preparation.
Fig. 3 is the X diffracting spectrum of the high-temperature superconductor GdBCO thin film of the embodiment of the present invention 2 preparation.
Fig. 4 is the scanning electron microscope collection of illustrative plates of the high-temperature superconductor GdBCO thin film of the embodiment of the present invention 2 preparation.
Detailed description of the invention
Embodiment 1
The present embodiment is prepared the method for HTS YBCO thin film and is comprised the following steps:
Step one, the floride-free precursor liquid of preparation: by propanoic acid yttrium, barium propionate, propanoic acid copper according to Y: Ba: Cu=1: 1.75: 3 former Son is than in the mixed solvent being dissolved in propanoic acid and ethanol, and under conditions of 70 DEG C, stirring 2h is to being completely dissolved, and obtains total cation Molar concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 5.5；
Step 2, prepare fluorine-containing precursor liquid: by propanoic acid yttrium, the organic salt of barium, propanoic acid copper by Y: Ba: Cu=1: 1.75: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs 2h to being completely dissolved under conditions of 70 DEG C, obtain total sun from Sub-molar concentration is the fluorine-containing precursor liquid of 1.8mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 5.5；Described The organic salt of barium is the mixture of trifluoroacetic acid barium and barium propionate, the mole percent of trifluoroacetic acid barium in the organic salt of described barium It is 60%；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, it is subsequently placed in the quartz tube furnace that temperature is 160 DEG C, and in described quartz tube furnace, is passed through humidity Oxygen atmosphere, with the ramp of 5 DEG C/min to 450 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain floride-free monolayer forerunner Film；The rotating speed of described spin coating is 2500rpm, and the time of described spin coating is 105s；The body of oxygen in the oxygen atmosphere of described humidity Long-pending percentage composition is 97.5%, and surplus is steam；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 It is coated in free-floride monolayer precursor film described in step 3, is subsequently placed in the quartz tube furnace that temperature is 160 DEG C, and to described stone The oxygen atmosphere of humidity it is passed through in English tube furnace, with the ramp of 5 DEG C/min to 450 DEG C, constant temperature 10min, cool to the furnace Room temperature obtains free-floride/fluorine-containing double-deck precursor film；The rotating speed of described spin coating is 2500rpm, and the time of described spin coating is 105s；Described In moist oxygen atmosphere, the volumn concentration of oxygen is 97.5%, and surplus is steam；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through to described quartz tube furnace, the most again with the ramp of 55 DEG C/min to 790 DEG C, insulation 1.5h, is incubated 1h when furnace temperature is down to 450 DEG C and carries out oozing oxygen process, cool to room temperature with the furnace, obtain critical temperature in liquid nitrogen temperature HTS YBCO thin film more than degree (77K)；In the argon oxygen gas mixture of described humidity, the volumn concentration of argon is 97.23%, the volumn concentration of oxygen is 0.04%, and surplus is steam.
Fig. 1 is the X diffracting spectrum of the HTS YBCO thin film of the embodiment of the present invention 1 preparation, as can be seen from Figure 1 makes Standby ybco film has (00l) peak, and does not substantially have other dephasign peaks, and display has good c-axis orientation, and this explanation free-floride/ Fluorine-containing double-deck precursor film promotes c-axis oriented nucleation and the growth of ybco film.Fig. 2 is the high temperature of the embodiment of the present invention 1 preparation The scanning electron microscope collection of illustrative plates of superconduction ybco film, from figure 2 it can be seen that ybco film surface is without a axialite, shows high-temperature superconductor Ybco film has good biaxial orientation, and in the most traditional method preparing ybco film, high fluoro-gas volatilization can cause thin film The a lot of hole of upper appearance, in comparison, the YBCO surface that the present embodiment prepares has minimal amount of hole, shows free-floride/contain Fluorine bilayer precursor film really affects and reduces the Oil repellent of this HTS YBCO thin film, it is suppressed that due to foreign gas volatilization shape The hole become.
HTS YBCO thin film prepared by this example has sharp keen c-axis orientation, and surface hole defect is less, smooth, superconducting layer 77K reaches 3MA/cm from critical current density after the match2。
Embodiment 2
The present embodiment is prepared the method for high-temperature superconductor GdBCO thin film and is comprised the following steps:
Step one, the floride-free precursor liquid of preparation: by propanoic acid gadolinium, barium propionate, propanoic acid copper according to Gd: Ba: Cu=1: 1.75: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs 3h to being completely dissolved under conditions of 80 DEG C, obtain total sun from Sub-molar concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 5；
Step 2, prepare fluorine-containing precursor liquid: by propanoic acid gadolinium, the organic salt of barium, propanoic acid copper by Gd: Ba: Cu=1: 1.8: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs 3h to being completely dissolved under conditions of 80 DEG C, obtain total sun from Sub-molar concentration is the fluorine-containing precursor liquid of 1.8mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 5；Described barium The mixture that organic salt is trifluoroacetic acid barium and barium propionate；In the organic salt of described barium, the mole percent of trifluoroacetic acid barium is 50%；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, it is subsequently placed in the quartz tube furnace that temperature is 160 DEG C, and in described quartz tube furnace, is passed through humidity Oxygen atmosphere, with the ramp of 5 DEG C/min to 400 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain floride-free monolayer forerunner Film；The rotating speed of described spin coating is 3000rpm, and the time of described spin coating is 105s；The body of oxygen in the oxygen atmosphere of described humidity Long-pending percentage composition is 98%, and surplus is steam；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 It is coated in free-floride monolayer precursor film described in step 3, is subsequently placed in the quartz tube furnace that temperature is 160 DEG C, and to described stone The oxygen atmosphere of humidity it is passed through in English tube furnace, with the ramp of 5 DEG C/min to 400 DEG C, constant temperature 10min, cool to the furnace Room temperature obtains free-floride/fluorine-containing double-deck precursor film；The rotating speed of described spin coating is 3000rpm, and the time of described spin coating is 105s；Described In moist oxygen atmosphere, the volumn concentration of oxygen is 98%, and surplus is steam；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through to described quartz tube furnace, the most again with the ramp of 60 DEG C/min to 810 DEG C, insulation 2h, is incubated 1h when furnace temperature is down to 450 DEG C and carries out oozing oxygen process, cool to room temperature with the furnace, obtain critical temperature in liquid nitrogen temperature (77K) the high-temperature superconductor GdBCO thin film more than；In the argon oxygen gas mixture of described humidity, the volumn concentration of argon is 97%, The volumn concentration of oxygen is 0.05%, and surplus is steam.
Fig. 3 is the X diffracting spectrum of the high-temperature superconductor GdBCO thin film of the embodiment of the present invention 2 preparation, from figure 3, it can be seen that The GdBCO thin film prepared has (00l) peak, and does not substantially have other dephasign peaks, and display has good c-axis orientation, and this illustrates nothing Fluorine/fluorine-containing double-deck precursor film promotes c-axis oriented nucleation and the growth of GdBCO thin film.Fig. 4 is the embodiment of the present invention 2 preparation The scanning electron microscope collection of illustrative plates of high-temperature superconductor GdBCO thin film, figure 4, it is seen that GdBCO film surface is without a axialite, and substantially without Hole, shows that thin film has good biaxial orientation and good microstructure.
High-temperature superconductor GdBCO thin film prepared by this example has a sharp keen c-axis orientation, and surfacing, microscopic appearance are good, 77K reaches 2MA/cm from critical current density after the match2。
Embodiment 3
The present embodiment is prepared the method for HTS YBCO thin film and is comprised the following steps:
Step one, the floride-free precursor liquid of preparation: by propanoic acid yttrium, barium propionate, propanoic acid copper according to Y: Ba: Cu=1: 1.75: 3 former Son, than being dissolved in the mixed solvent of propanoic acid and ethanol, stirs 1.5h to being completely dissolved under conditions of 80 DEG C, obtain total sun from Sub-molar concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 8；
Step 2, prepare fluorine-containing precursor liquid: by propanoic acid yttrium, the organic salt of barium, propanoic acid copper by Y: Ba: Cu=1: 1.75: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs 2h to being completely dissolved under conditions of 80 DEG C, obtain total sun from Sub-molar concentration is the fluorine-containing precursor liquid of 1.8mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 8；Described barium The mixture that organic salt is trifluoroacetic acid barium and barium propionate, in the organic salt of described barium, the mole percent of trifluoroacetic acid barium is 75%；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, it is subsequently placed in the quartz tube furnace that temperature is 180 DEG C, and in described quartz tube furnace, is passed through humidity Oxygen atmosphere, with the ramp of 5 DEG C/min to 420 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain floride-free monolayer forerunner Film；The rotating speed of described spin coating is 3000rpm, and the time of described spin coating is 120s；The body of oxygen in the oxygen atmosphere of described humidity Long-pending percentage composition is 97%, and surplus is steam；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 It is coated in free-floride monolayer precursor film described in step 3, is subsequently placed in the quartz tube furnace that temperature is 140 DEG C, and to described stone The oxygen atmosphere of humidity it is passed through in English tube furnace, with the ramp of 5 DEG C/min to 480 DEG C, constant temperature 10min, cool to the furnace Room temperature obtains free-floride/fluorine-containing double-deck precursor film；The rotating speed of described spin coating is 2500rpm, and the time of described spin coating is 150s；Described In moist oxygen atmosphere, the volumn concentration of oxygen is 97%, and surplus is steam；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through to described quartz tube furnace, the most again with the ramp of 80 DEG C/min to 800 DEG C, insulation 1.5h, is incubated 1h when furnace temperature is down to 450 DEG C and carries out oozing oxygen process, cool to room temperature with the furnace, and critical temperature is in liquid nitrogen temperature (77K) HTS YBCO thin film is obtained more than；In the argon oxygen gas mixture of described humidity, the volumn concentration of argon is 97%, the volumn concentration of oxygen is 0.05%, and surplus is steam.
HTS YBCO thin film prepared by this example has a sharp keen c-axis orientation, and surfacing, microscopic appearance are good, 77K reaches 2.6MA/cm from critical current density after the match2。
Embodiment 4
The present embodiment is prepared the method for high-temperature superconductor GdBCO thin film and is comprised the following steps:
Step one, the floride-free precursor liquid of preparation: by propanoic acid gadolinium, barium propionate, propanoic acid copper according to Gd: Ba: Cu=1: 1.75: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs 3h to being completely dissolved under conditions of 50 DEG C, obtain total sun from Sub-molar concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 7；
Step 2, prepare fluorine-containing precursor liquid: by propanoic acid gadolinium, trifluoroacetic acid barium, propanoic acid copper by Gd: Ba: Cu=1: 2: 3 former Son is than in the mixed solvent being dissolved in propanoic acid and ethanol, and under conditions of 50 DEG C, stirring 3h is to being completely dissolved, and obtains total cation Molar concentration is the fluorine-containing precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 7；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, it is subsequently placed in the quartz tube furnace that temperature is 200 DEG C, and in described quartz tube furnace, is passed through humidity Oxygen atmosphere, with the ramp of 5 DEG C/min to 400 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain floride-free monolayer forerunner Film；The rotating speed of described spin coating is 2500rpm, and the time of described spin coating is 180s；The body of oxygen in the oxygen atmosphere of described humidity Long-pending percentage composition is 97%, and surplus is steam；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 It is coated in free-floride monolayer precursor film described in step 3, is subsequently placed in the quartz tube furnace that temperature is 200 DEG C, and to described stone The oxygen atmosphere of humidity it is passed through in English tube furnace, with the ramp of 5 DEG C/min to 400 DEG C, constant temperature 10min, cool to the furnace Room temperature obtains free-floride/fluorine-containing double-deck precursor film；The rotating speed of described spin coating is 2500rpm, and the time of described spin coating is 180s；Described In moist oxygen atmosphere, the volumn concentration of oxygen is 97%, and surplus is steam；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through to described quartz tube furnace, the most again with the ramp of 10 DEG C/min to 810 DEG C, insulation 1h, is incubated 1h when furnace temperature is down to 450 DEG C and carries out oozing oxygen process, cool to room temperature with the furnace, obtain critical temperature in liquid nitrogen temperature (77K) the high-temperature superconductor GdBCO thin film more than；In the argon oxygen gas mixture of described humidity, the volumn concentration of argon is 98.78%, the volumn concentration of oxygen is 0.05%, and surplus is steam.
High-temperature superconductor GdBCO thin film prepared by this example has a sharp keen c-axis orientation, and surfacing, microscopic appearance are good, 77K reaches 2.1MA/cm from critical current density after the match2。
Embodiment 5
The present embodiment is prepared the method for HTS YBCO thin film and is comprised the following steps:
Step one, the floride-free precursor liquid of preparation: by propanoic acid yttrium, barium propionate, propanoic acid copper according to Y: Ba: Cu=1: 1.75: 3 former Son is than in the mixed solvent being dissolved in propanoic acid and ethanol, and under conditions of 40 DEG C, stirring 3h is to being completely dissolved, and obtains total cation Molar concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 10；
Step 2, prepare fluorine-containing precursor liquid: by propanoic acid yttrium, trifluoroacetic acid barium, propanoic acid copper by Y: Ba: Cu=1: 2: 3 former Son is than in the mixed solvent being dissolved in propanoic acid and ethanol, and under conditions of 40 DEG C, stirring 3h is to being completely dissolved, and obtains total cation Molar concentration is the fluorine-containing precursor liquid of 2mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 10；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, it is subsequently placed in the quartz tube furnace that temperature is 200 DEG C, and in described quartz tube furnace, is passed through humidity Oxygen atmosphere, with the ramp of 5 DEG C/min to 500 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain floride-free monolayer forerunner Film；The rotating speed of described spin coating is 4500rpm, and the time of described spin coating is 30s；The volume of oxygen in the oxygen atmosphere of described humidity Percentage composition is 98%, and surplus is steam；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 It is coated in free-floride monolayer precursor film described in step 3, is subsequently placed in the quartz tube furnace that temperature is 200 DEG C, and to described stone The oxygen atmosphere of humidity it is passed through in English tube furnace, with the ramp of 5 DEG C/min to 500 DEG C, constant temperature 10min, cool to the furnace Room temperature obtains free-floride/fluorine-containing double-deck precursor film；The rotating speed of described spin coating is 4500rpm, and the time of described spin coating is 30s；Described In moist oxygen atmosphere, the volumn concentration of oxygen is 98%, and surplus is steam；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through to described quartz tube furnace, the most again with the ramp of 100 DEG C/min to 810 DEG C, insulation 1h, is incubated 1h when furnace temperature is down to 450 DEG C and carries out oozing oxygen process, cool to room temperature with the furnace, obtain critical temperature in liquid nitrogen temperature (77K) the HTS YBCO thin film more than；In the argon oxygen gas mixture of described humidity, the volumn concentration of argon is 98.78%, the volumn concentration of oxygen is 0.07%, and surplus is steam.
HTS YBCO thin film prepared by the present embodiment has good c-axis orientation and biaxial texture, surfacing, surpasses Lead thin film 77K and reach 2.7MA/cm from critical current density after the match2。
Embodiment 6
The present embodiment is prepared the method for HTS YBCO thin film and is comprised the following steps:
Step one, the floride-free precursor liquid of preparation: by propanoic acid yttrium, barium propionate, propanoic acid copper according to Y: Ba: Cu=1: 1.75: 3 former Son is than in the mixed solvent being dissolved in propanoic acid and ethanol, and under conditions of 100 DEG C, stirring 1h is to being completely dissolved, and obtains total cation Molar concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 1；
Step 2, prepare fluorine-containing precursor liquid: by propanoic acid yttrium, the organic salt of barium, propanoic acid copper by Y: Ba: Cu=1: 1.5: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs 1h to being completely dissolved under conditions of 100 DEG C, obtain total sun from Sub-molar concentration is the fluorine-containing precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 10；Described The organic salt of barium is the mixture of trifluoroacetic acid barium and barium propionate, the mole percent of trifluoroacetic acid barium in the organic salt of described barium It is 15%；；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, it is subsequently placed in the quartz tube furnace that temperature is 120 DEG C, and in described quartz tube furnace, is passed through humidity Oxygen atmosphere, with the ramp of 5 DEG C/min to 400 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain floride-free monolayer forerunner Film；The rotating speed of described spin coating is 500rpm, and the time of described spin coating is 180s；The volume of oxygen in the oxygen atmosphere of described humidity Percentage composition is 97%, and surplus is steam；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 It is coated in free-floride monolayer precursor film described in step 3, is subsequently placed in the quartz tube furnace that temperature is 120 DEG C, and to described stone The oxygen atmosphere of humidity it is passed through in English tube furnace, with the ramp of 5 DEG C/min to 400 DEG C, constant temperature 10min, cool to the furnace Room temperature obtains free-floride/fluorine-containing double-deck precursor film；The rotating speed of described spin coating is 500rpm, and the time of described spin coating is 180s；Described In moist oxygen atmosphere, the volumn concentration of oxygen is 97%, and surplus is steam；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through to described quartz tube furnace, the most again with the ramp of 10 DEG C/min to 770 DEG C, insulation 2h, is incubated 1h when furnace temperature is down to 450 DEG C and carries out oozing oxygen process, cool to room temperature with the furnace, obtain critical temperature in liquid nitrogen temperature (77K) the HTS YBCO thin film more than；In the argon oxygen gas mixture of described humidity, the volumn concentration of argon is 95.73%, the volumn concentration of oxygen is 0.02%, and surplus is steam.
HTS YBCO thin film prepared by the present embodiment has good c-axis orientation and biaxial texture, surfacing, surpasses Lead thin film 77K and reach 2.5MA/cm from critical current density after the match2。
Embodiment 7
The present embodiment is prepared the method for high-temperature superconductor GdBCO thin film and is comprised the following steps:
Step one, the floride-free precursor liquid of preparation: by propanoic acid gadolinium, barium propionate, propanoic acid copper according to Gd: Ba: Cu=1: 1.75: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs 2h to being completely dissolved under conditions of 60 DEG C, obtain total sun from Sub-molar concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 3；
Step 2, prepare fluorine-containing precursor liquid: by propanoic acid gadolinium, the organic salt of barium, propanoic acid copper by Gd: Ba: Cu=1: 2: 3 former Son is than in the mixed solvent being dissolved in propanoic acid and ethanol, and under conditions of 60 DEG C, stirring 2h is to being completely dissolved, and obtains total cation Molar concentration is the fluorine-containing precursor liquid of 2mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: 3；Having of described barium Machine salt is the mixture of trifluoroacetic acid barium and barium propionate；In the organic salt of described barium, the mole percent of trifluoroacetic acid barium is 35%；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method uniformly to coat precursor liquid floride-free described in step one At LaAlO3On substrate, it is subsequently placed in the quartz tube furnace that temperature is 140 DEG C, and in described quartz tube furnace, is passed through humidity Oxygen atmosphere, with the ramp of 5 DEG C/min to 480 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain floride-free monolayer forerunner Film；The rotating speed of described spin coating is 4500rpm, and the time of described spin coating is 120s；The body of oxygen in the oxygen atmosphere of described humidity Long-pending percentage composition is 98%, and surplus is steam；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: use spin-coating method uniform fluorine-containing precursor liquid described in step 2 It is coated in free-floride monolayer precursor film described in step 3, is subsequently placed in the quartz tube furnace that temperature is 180 DEG C, and to described stone The oxygen atmosphere of humidity it is passed through in English tube furnace, with the ramp of 5 DEG C/min to 420 DEG C, constant temperature 10min, cool to the furnace Room temperature obtains free-floride/fluorine-containing double-deck precursor film；The rotating speed of described spin coating is 4500rpm, and the time of described spin coating is 120s；Described In moist oxygen atmosphere, the volumn concentration of oxygen is 98%, and surplus is steam；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, The argon oxygen gas mixture of humidity it is passed through to described quartz tube furnace, the most again with the ramp of 30 DEG C/min to 810 DEG C, insulation 1h, is incubated 1h when furnace temperature is down to 450 DEG C and carries out oozing oxygen process, cool to room temperature with the furnace, obtain critical temperature in liquid nitrogen temperature (77K) the high-temperature superconductor GdBCO thin film more than；In the argon oxygen gas mixture of described humidity, the volumn concentration of argon is 96%, The volumn concentration of oxygen is 0.05%, and surplus is steam.
High-temperature superconductor GdBCO thin film prepared by the present embodiment has good c-axis and is orientated and biaxial texture, surfacing, Superconducting thin film 77K reaches 1.9MA/cm from critical current density after the match2。
The above, be only presently preferred embodiments of the present invention, and the present invention not does any restriction, every according to invention skill Any simple modification, change and the equivalent structure change that above example is made by art essence, all still falls within the technology of the present invention In the protection domain of scheme.

Claims (6)

1. the preparation method of a high-temperature superconductor REBCO thin film, it is characterised in that the method comprises the following steps:
Step one, the floride-free precursor liquid of preparation: by the propionate of RE, barium propionate, propanoic acid copper according to RE: Ba: Cu=1: 1.75: 3 Atomic ratio is dissolved in the mixed solvent of propanoic acid and ethanol, stirs to being completely dissolved under conditions of 40 DEG C～100 DEG C, obtains total Cation mole concentration is the floride-free precursor liquid of 1.5mol/L；In described mixed solvent, the volume ratio of propanoic acid and ethanol is 1: (1～ 10)；The propionate of described RE is propanoic acid yttrium or propanoic acid gadolinium；
Step 2, prepare fluorine-containing precursor liquid: by the propionate of RE, the organic salt of barium, propanoic acid copper by RE: Ba: Cu=1: (1.5～ 2): the atomic ratio of 3 is dissolved in the mixed solvent of propanoic acid and ethanol, stir to being completely dissolved under conditions of 40 DEG C～100 DEG C, Obtain the fluorine-containing precursor liquid that total cation molar concentration is 1.5mol/L～2mol/L；Propanoic acid and ethanol in described mixed solvent Volume ratio is 1: (1～10)；The propionate of described RE is propanoic acid yttrium or propanoic acid gadolinium；The organic salt of described barium be trifluoroacetic acid barium or Person's trifluoroacetic acid barium and the mixture of barium propionate；
The propionate of RE described in step 2 is identical with the propionate of RE described in step one；
Step 3, the floride-free monolayer precursor film of preparation: use spin-coating method to be coated uniformly on precursor liquid floride-free described in step one LaAlO3On substrate, being subsequently placed in temperature is 120 DEG C～the quartz tube furnace of 200 DEG C, and is passed through in described quartz tube furnace Moist oxygen atmosphere, with the ramp of 5 DEG C/min to 400 DEG C～500 DEG C, constant temperature 10min, cool to room temperature with the furnace and obtain Floride-free monolayer precursor film；
Step 4, floride-free/fluorine-containing double-deck precursor film of preparation: the employing spin-coating method of fluorine-containing precursor liquid described in step 2 is uniformly coated Described in step 3 on floride-free monolayer precursor film, being subsequently placed in temperature is 120 DEG C～the quartz tube furnace of 200 DEG C, and to institute The oxygen atmosphere of humidity it is passed through in stating quartz tube furnace, with the ramp of 5 DEG C/min to 400 DEG C～500 DEG C, constant temperature 10min, Cool to room temperature with the furnace and obtain free-floride/floride-free/fluorine-containing double-deck precursor film of fluorine-containing double-deck precursor film；
Step 5, crystallization and thermal treatment: double-deck precursor film floride-free/fluorine-containing described in step 4 is placed in quartz tube furnace, to institute State quartz tube furnace and be passed through the argon oxygen gas mixture of humidity, the most again with the ramp of 10 DEG C/min～100 DEG C/min to 770 DEG C ～810 DEG C, it is incubated 1h～2h, when furnace temperature is down to 450 DEG C, is incubated 1h carries out oozing oxygen process, cool to room temperature with the furnace, faced Boundary's temperature high-temperature superconductor REBCO thin film more than liquid nitrogen temperature 77K.
The preparation method of a kind of high-temperature superconductor REBCO thin film the most according to claim 1, it is characterised in that step one and The time of stirring described in step 2 is 1h～3h.
The preparation method of a kind of high-temperature superconductor REBCO thin film the most according to claim 1, it is characterised in that in step 2 In the organic salt of described barium, the mole percent of trifluoroacetic acid barium is not less than 15%.
The preparation method of a kind of high-temperature superconductor REBCO thin film the most according to claim 1, it is characterised in that step 3 and The rotating speed of spin coating described in step 4 is 500r/min～4500r/min, and the time of described spin coating is 30s～180s.
The preparation method of a kind of high-temperature superconductor REBCO thin film, it is characterised in that step 3 and step In oxygen atmosphere moist described in rapid four, the volumn concentration of oxygen is 97%～98%, and surplus is steam.
The preparation method of a kind of high-temperature superconductor REBCO thin film, it is characterised in that institute in step 5 Stating the volumn concentration of argon in the argon oxygen gas mixture of humidity is 95.73%～98.78%, and the volumn concentration of oxygen is 0.02%～0.07%, surplus is steam.
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CN108752048A (en) * 2018-06-29 2018-11-06 西北有色金属研究院 A kind of preparation method of YBCO composite graphites ene coatings
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
WO2024023294A1 (en) 2022-07-29 2024-02-01 Consejo Superior De Investigaciones Científicas (Csic) PRECURSOR SOLUTION SUITABLE FOR THE PREPARATION OF HIGH PERFORMANCE EPITAXIAL REBa2Cu3O7-x SUPERCONDUCTORS

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CN103864461A (en) * 2014-03-13 2014-06-18 西北有色金属研究院 Method for preparing REBCO superconducting thin film

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CN102807372A (en) * 2012-08-28 2012-12-05 西北有色金属研究院 Preparation method of gadolinium-barium-copper-oxygen compact film
CN103864461A (en) * 2014-03-13 2014-06-18 西北有色金属研究院 Method for preparing REBCO superconducting thin film

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CN107459055A (en) * 2017-09-11 2017-12-12 西北有色金属研究院 A kind of method that nano-particle induction epitaxial growth prepares ybco film
CN107459055B (en) * 2017-09-11 2019-03-05 西北有色金属研究院 A kind of method that nanoparticle induction epitaxial growth prepares ybco film
CN108752048A (en) * 2018-06-29 2018-11-06 西北有色金属研究院 A kind of preparation method of YBCO composite graphites ene coatings
WO2024023294A1 (en) 2022-07-29 2024-02-01 Consejo Superior De Investigaciones Científicas (Csic) PRECURSOR SOLUTION SUITABLE FOR THE PREPARATION OF HIGH PERFORMANCE EPITAXIAL REBa2Cu3O7-x SUPERCONDUCTORS
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