CN102690114B - Method for preparing YBCO superconducting composite film - Google Patents
Method for preparing YBCO superconducting composite film Download PDFInfo
- Publication number
- CN102690114B CN102690114B CN2012101148030A CN201210114803A CN102690114B CN 102690114 B CN102690114 B CN 102690114B CN 2012101148030 A CN2012101148030 A CN 2012101148030A CN 201210114803 A CN201210114803 A CN 201210114803A CN 102690114 B CN102690114 B CN 102690114B
- Authority
- CN
- China
- Prior art keywords
- ybco
- film
- heat treatment
- gel
- precursor liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E40/00—Technologies for an efficient electrical power generation, transmission or distribution
- Y02E40/60—Superconducting electric elements or equipment; Power systems integrating superconducting elements or equipment
Landscapes
- Superconductor Devices And Manufacturing Methods Thereof (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Superconductors And Manufacturing Methods Therefor (AREA)
Abstract
Disclosed is a method for preparing a YBa2Cu3O7-x (YBCO) superconducting composite film, comprising mixing and dissolving ytterbium acetate <Y(CH3COO)3>, barium acetate <Ba(CH3COO)2>, and cupric acetate <Cu(CH3COO)2> into a water solution of trifluoroacetic acid according to a molar ratio of Y:Ba:Cu of 1.5:2:3; uniformly stirring, and evaporating the above solvent to dryness in vacuum to acquire a gel; adding methanol, uniformly stirring, and evaporating the resulting solvent to dryness to acquire a gel; adding methanol to prepare a precursor liquid in which the total concentration of the three types of metal ions of Y, Ba, and Cu is 1.5-3.0mol/L; coating the precursor liquid on a substrate; allowing the coated film to undergo a process of low-temperature heat treatment to decompose trifluoroacetate; allowing the coated film to undergo a process of high-temperature heat treatment to acquire a YBCO film having a tetragonal phase; coating a precursor liquid of cerium acetylacetonate on the YBCO film and carrying out a high-temperature heat treatment at a temperature ranged from 1000 DEG C to 1100 DEG C; and coating the precursor of Y, Ba, and Cu and the precursor of cerium acetylacetonate in turn repeatedly and carrying out corresponding heat treatment to acquire the YBCO superconducting film having a five-layer structure of YBCO/CeO2/YBCO/CeO2/YBCO with a thickness of 1.5 microns.
Description
Technical field
The present invention relates to a kind of preparation method of conductor of high-temperature superconductor coat, particularly a kind of preparation method of YBCO superconduction composite membrane.
Background technology
With YBa
2Cu
3O
7-x(YBCO) superconducting coating be conductor second generation belt material of high temperature superconduct due to its excellent intrinsic performance (irreversiblely under 77K reach 7T, critical current density reaches 10
6A/cm
2), attracting people constantly to explore and studying its practicality technology of becoming a useful person.Second generation belt material of high temperature superconduct is the important development direction of present superconductor, has broad application prospects and huge market potential, can be widely used in the aspects such as the energy, war industry, medical treatment, traffic and scientific research.Therefore, high temperature superconducting materia and technology of preparing are listed in the cutting edge technology of National Program for Medium-to Long-term Scientific and Technological Development (2006-2020).
Have at least in the world at present five units to prepare length and surpass the YBCO superconducting tape of 250A over 500m, critical current (Ic).Also obtained breakthrough domestic recent years, reported at the beginning of Shanghai Communications University 2011 that succeeding in developing current capacity reaches 194 amperes, the second generation belt material of high temperature superconduct of hundred meter levels.Yet the cost for preparing at present the YBCO band is high.The price of being made the YBCO superconducting tape of businessman U.S. SuperPower company preparation by the world two best generations is 400 dollars/kilo-ampere rice, more than 50 times of copper cash, the application that wants it has competitiveness more, must further improve its performance and then improve cost performance and could satisfy demand widely.YBCO as coating conductor can use in the forceful electric power field be mainly due to it has can load current and the characteristic of not loss.Concerning superconducting tape, remaining unchanged in critical current density (Jc) increases its thickness and has also just improved its current capacity.Therefore, how to prepare the thick film with high critical current densities and just become the key issue that needs to be resolved hurrily in current YBCO high-temperature superconducting coating application process.USAF laboratory T.Haugan research group has reported pulsed laser deposition (PLD) method on Nature, the method adopts two different target alternating deposit ybco films and non-superconducting Y mutually
2BaCuO
5(211)." 211 " nanoparticle size of deposition is 0.5～1.5nm, and density is 5～6 * 10
11/ cm
2These highdensity point defects have played the effect of flux pinning, make critical current density by the 2-3MA/cm of pure ybco film
2Bring up to 4MA/cm
2Above.They have finally prepared high performance YBCO coating by the mode with the multilayer film stack, have improved its current capacity.Although the USAF laboratory adopts the PLD method to prepare the YBCO thick film by the mode of multiple-layer stacked, the pulsed laser deposition that this method adopts needs expensive vacuum system, and deposition rate is lower, and technique more complicated, cost are very high.The domestic preparation of only having Chinese patent CN 101719399A to mention thick film at present.This patent adopts chemical solution method to replace trifluoroacetic acid copper with acrylic acid copper, and adding ethylene glycol amine in precursor liquid, to have prepared thickness be the YBCO thick film of 1 micron.Although this patent system is for the YBCO thick film, thickness is only 1 micron, and is limited to the current capacity that improves the YBCO coating.The more important thing is for two most important index critical currents estimating superconductor and critical current density all not relate in this patent, can't estimate its superconductivity.
Summary of the invention
The objective of the invention is to overcome the weak shortcoming of YBCO superconducting thin film current capacity of prior art preparation, a kind of preparation method with multilayer YBCO film of high current carrying capacity is provided.
The present invention adopts full chemical solution method alternately to deposit YBCO film and CeO on matrix
2Film namely prepares the YBCO/CeO that structure is multilayer
2Film, thickness reach the YBCO superconducting film of 1.5 microns.The multilayer film that the present invention is prepared, particularly YBCO/CeO
2/ YBCO/CeO
2/ YBCO five tunics, its structure is: what at first deposit on matrix is the YBCO film, and namely the first tunic is the YBCO film, the CeO that deposits on ground floor YBCO film
2Film is the second tunic, the like, at second layer CeO
2The 3rd layer that deposits on film is the YBCO film, and the 4th layer is CeO
2Film, layer 5 are the YBCO film.
Concrete steps order of the present invention is as follows:
(1) according to Y: Ba: Cu=1.5: the mol ratio of 2: 3 is Y (CH
3COO)
3, Ba (CH
3COO)
2And Cu (CH
3COO)
2Three kinds of powder mix, are dissolved under room temperature in the deionized water of the trifluoroacetic acid that contains 10-30mol%, and wiring solution-forming, in described solution, the mol ratio of solute and solvent is 1: 100;
(2) with the described solution of step (1) preparation through magnetic stirrer 1-3h, then adopt Rotary Evaporators to steam to desolventize to obtain gel;
(3) gel that described step (2) is made adds in methyl alcohol, and the mol ratio of the gel described in this step and methyl alcohol is 1: 50.After magnetic stirrer 0.5-1.5h, then adopt the Rotary Evaporators steaming to desolventize, with impurity such as further removal moisture, obtain pure gel;
(4) gel that described step (3) is made joins in methyl alcohol, the precursor liquid that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5-3.0mol/L;
(5) precursor liquid of described step (4) being made adopts spin coating or method of pulling up to be coated on substrate;
(6) substrate after step (5) applies is placed in the quartzy stove of high-temperature tubular, carries out the Low Temperature Heat Treatment of 10h at 300 ℃ of-500 ℃ of temperature, decompose trifluoroacetate; The heating rate of this step is 40 ℃/h;
(7) will be placed in through the substrate that step (6) is processed heat treatment 2-4h under the high temperature of 750 ℃-850 ℃, generate Tetragonal YBCO film; The programming rate of this step is 400 ℃/h;
(8) the acetylacetone,2,4-pentanedione cerium is dissolved in methyl alcohol under room temperature, preparation obtains the precursor liquid that the metallic cerium ion concentration is 0.1～0.5mol/L; This precursor liquid is spin-coated on ybco film through step (7) sintering;
(9) will be placed in through the sample that step (8) is processed heat treatment 1-2h under the high temperature of 1000 ℃-1100 ℃, generate CeO
2Film; The programming rate of this step is 400 ℃/h;
(10) on the sample of processing through step (9) successively according to step (5)-(7) and step (8)-(9) alternating deposit YBCO film and CeO
2Film is heat-treated in the oxygen atmosphere at last, and preparing structure is YBCO/CeO
2/ YBCO/CeO
2Five layers of/YBCO, thickness are the YBCO superconducting thick-film of 1.5 microns.
Substrate described in step (5) is lanthanum aluminate, strontium titanates or magnesium oxide single-crystal substrate.
Compared with prior art, the present invention has following beneficial effect:
The present invention adopts chemical solution method to prepare the ultra-thin CeO with epitaxial structure on the basis of trifluoroacetate-metal organic deposit YBCO film
2Film.This layer CeO
2Film can not only play the effect of transmitting biaxial texture, can also be as YBCO film effectively pin center, and the stress in the YBCO thick film that can also relax, avoid cracking.Adopt the not decay rapidly of YBCO thick film critical current density of the method preparation, reach 3.8MA/cm in null field lower critical current density
2, greatly improved the current capacity of YBCO thick film, reduced the production cost of coating conductor, widened the range of application of YBCO coating conductor.
Description of drawings
Fig. 1 is the field emission scanning electron microscope picture of the YBCO thick film of embodiment 1 preparation;
Fig. 2 is the X-ray diffraction halfwidth collection of illustrative plates of YBCO thick film (005) face of embodiment 2 preparations;
Fig. 3 is the X-ray diffraction halfwidth collection of illustrative plates of YBCO thick film (005) face of embodiment 3 preparations;
Fig. 4 is the field emission scanning electron microscope picture of the YBCO thick film of embodiment 4 preparations;
Fig. 5 is the X-ray diffraction halfwidth collection of illustrative plates of YBCO thick film (005) face of embodiment 4 preparations;
Fig. 6 is the critical current density (77K, 0T) of the YBCO thick film of embodiment 4 preparations.
The specific embodiment mode
(1) take yttrium acetate, barium acetate and copper acetate and be respectively 0.005mol, 0.01mol and 0.015mol, be dissolved in wiring solution-forming in the 100ml deionized water of the trifluoroacetic acid that contains 10mol% after yttrium acetate, barium acetate and copper acetate are mixed;
(2) solution that step (1) is made then adopts Rotary Evaporators to steam to desolventize and obtains gel after magnetic stirrer 1h;
(3) methyl alcohol of 30mL is added in the gel that described step (2) makes, then adopt again Rotary Evaporators to steam after magnetic stirrer 0.5h to desolventize with the impurity such as further removal moisture and obtain very pure gel;
(4) gel that step (3) is made joins in 20ml methyl alcohol, the precursor liquid that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5mol/L;
(5) precursor liquid that step (4) is made is spin-coated on strontium titanate monocrystal chip with the speed of 1500 rev/mins, and the spin coating time is 90s;
(6) the coated substrate of step (5) that coating is good is placed on to send in quartz boat in the quartzy stove of high-temperature tubular and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains at last the YBCO film of Tetragonal;
Described Low Temperature Heat Treatment is to carry out under moistening Oxygen Condition, through the vial that distilled water is housed, steam to be brought the oxygen of 500sccm into reative cell, make that in reative cell, water vapour pressure is 100hPa, on average be warming up to 300 ℃ with the heating rate of 40 ℃/h from room temperature, and then stove is cooled to room temperature.The purpose of Low Temperature Heat Treatment is to decompose trifluoroacetate, forms unformed precursor film and discharges harmful residual substance.The whole resolving time is about 10h.
Described high-temperature heat treatment is to carry out under moistening oxygen and argon gas mixed atmosphere, the argon gas mist that 500sccm is contained 500ppm oxygen is brought steam into reative cell through the vial that distilled water is housed, make that in reative cell, water vapour pressure is 160hPa, heating rate with 400 ℃/h rose to 750 ℃ of the highest temperatures before this, directly pass into the argon gas mist that contains 500ppm oxygen after 750 ℃ of insulation 2h, then be cooled to room temperature with 100 ℃/h, obtain the YBCO film of Tetragonal;
(7) the acetylacetone,2,4-pentanedione cerium with 0.0001mol is dissolved in the methyl alcohol of 10mL in room temperature, and preparation obtains the precursor liquid that the metallic cerium ion concentration is 0.1mol/L; This precursor liquid is spin-coated on ybco film through step (6) sintering with the speed of 1500 rev/mins;
(8) will be placed in through the sample that step (7) is processed heat treatment 1h under the high temperature of 1000 ℃, generate CeO
2Film; The programming rate of this step is 400 ℃/h;
(9) on the sample of processing through step (8) successively according to step (5)-(6) and step (7)-(8) alternating deposit YBCO film and CeO
2Film carries out 500 ℃ of heat treatment 1h at last in 500sccm oxygen atmosphere, prepare YBCO/CeO
2/ YBCO/CeO
2/ YBCO five layer thicknesses are the YBCO superconducting thick-film of 1.5 microns.With field emission scanning electron microscope, this sample has been carried out the surface topography observation, the YBCO thick film surface is smooth, fine and close, there is no crackle, as Fig. 1 not.
Embodiment 2
(1) take yttrium acetate, barium acetate and copper acetate and be respectively 0.01mol, 0.02mol and 0.03mol, be dissolved in wiring solution-forming in the 200ml deionized water of the trifluoroacetic acid that contains 20mol% after yttrium acetate, barium acetate and copper acetate are mixed;
(2) solution that step (1) is made then adopts Rotary Evaporators to steam to desolventize and obtains gel after magnetic stirrer 2h;
(3) methyl alcohol of 60mL is added in the gel that described step (2) makes, then adopt again Rotary Evaporators to steam after magnetic stirrer 1h to desolventize with the impurity such as further removal moisture and obtain very pure gel;
(4) gel that step (3) is made joins in 30ml methyl alcohol, the precursor liquid that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 2mol/L;
(5) precursor liquid that step (4) is made is spin-coated on the lanthanuma luminate single crystal substrate with the speed of 3000 rev/mins, and the spin coating time is 90s.
(6) the coated substrate of step (5) that coating is good is placed on to send in quartz boat in the quartzy stove of high-temperature tubular and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains at last the YBCO film of Tetragonal;
Low Temperature Heat Treatment is to carry out under moistening Oxygen Condition, through the vial that distilled water is housed, steam to be brought the oxygen of 500sccm into reative cell, make that in reative cell, water vapour pressure is 130hPa, on average be warming up to 400 ℃ with the heating rate of 40 ℃/h from room temperature, and then stove is cooled to room temperature.The purpose of Low Temperature Heat Treatment is to decompose trifluoroacetate, forms unformed precursor film and discharges harmful residual substance.The whole resolving time is about 10h;
High-temperature heat treatment is to carry out under moistening oxygen and argon gas mixed atmosphere, the argon gas mist that 500sccm is contained 500ppm oxygen is brought steam into reative cell through the vial that distilled water is housed, make that in reative cell, water vapour pressure is 200hPa, heating rate with 400 ℃/h rose to 800 ℃ of the highest temperatures before this, directly pass into the argon gas mist that contains 500ppm oxygen after 800 ℃ of insulation 3h, then be cooled to room temperature with 100 ℃/h, obtain the YBCO film of Tetragonal;
(7) the acetylacetone,2,4-pentanedione cerium with 0.00025mol is dissolved in the methyl alcohol of 10mL in room temperature, and preparation obtains the precursor liquid that the metallic cerium ion concentration is 0.25mol/L; This precursor liquid is spin-coated on ybco film through step (6) sintering with the speed of 3000 rev/mins;
(8) will be placed in through the sample that step (7) is processed heat treatment 1.5h under the high temperature of 1050 ℃, generate CeO
2Film; The programming rate of this step is 400 ℃/h;
(9) on the sample of processing through step (8) successively according to step (5)-(6) and step (7)-(8) alternating deposit YBCO film and CeO
2Film carries out 500 ℃ of heat treatment 1h at last in 500sccm oxygen atmosphere, prepare YBCO/CeO
2/ YBCO/CeO
2/ YBCO five layer thicknesses are the YBCO superconducting thick-film of 1.5 microns.Be used in PhilipsX ' Pert type X-ray diffractometer and sample done the ω scanning of (005) face, as shown in Figure 2.The halfwidth at YBCO (005) peak is only 0.83 °, illustrates that ybco film has orientation in good face, does not exist high-angle boundary.
Embodiment 3
(1) take yttrium acetate, barium acetate and copper acetate and be respectively 0.015mol, 0.03mol and 0.045mol, be dissolved in wiring solution-forming in the 300ml deionized water of the trifluoroacetic acid that contains 30mol% after yttrium acetate, barium acetate and copper acetate are mixed;
(2) solution that step (1) is made then adopts Rotary Evaporators to steam to desolventize and obtains gel after magnetic stirrer 3h;
(3) methyl alcohol of 90mL is added in the gel that described step (2) makes, then adopt again Rotary Evaporators to steam after magnetic stirrer 1.5h to desolventize with the impurity such as further removal moisture and obtain very pure gel;
(4) gel that step (3) is made joins in 30ml methyl alcohol, the precursor liquid that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 3.0mol/L;
(5) precursor liquid that step (4) is made is spin-coated on the magnesium oxide single-crystal substrate with the speed of 4500 rev/mins, and the spin coating time is 90s;
(6) the coated substrate of step (5) that coating is good is placed on to send in quartz boat in the quartzy stove of high-temperature tubular and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains at last the YBCO film of Tetragonal;
Low Temperature Heat Treatment is to carry out under moistening Oxygen Condition, through the vial that distilled water is housed, steam to be brought the oxygen of 500sccm into reative cell, make that in reative cell, water vapour pressure is 160hPa, on average be warming up to 500 ℃ with the heating rate of 40 ℃/h from room temperature, and then stove is cooled to room temperature.The purpose of Low Temperature Heat Treatment is to decompose trifluoroacetate, forms unformed precursor film and discharges harmful residual substance.The whole resolving time is about 10h;
High-temperature heat treatment is to carry out under moistening oxygen and argon gas mixed atmosphere, the argon gas mist that 500sccm is contained 500ppm oxygen is brought steam into reative cell through the vial that distilled water is housed, make that in reative cell, water vapour pressure is 240hPa, heating rate with 400 ℃/h rose to 850 ℃ of the highest temperatures before this, directly pass into the argon gas mist that contains 500ppm oxygen after 850 ℃ of insulation 4h, then be cooled to room temperature with 100 ℃/h, obtain the YBCO film of Tetragonal;
(7) the acetylacetone,2,4-pentanedione cerium with 0.0005mol is dissolved in the methyl alcohol of 10mL in room temperature, and preparation obtains the precursor liquid that the metallic cerium ion concentration is 0.5mol/L; This precursor liquid is spin-coated on ybco film through step (6) sintering with the speed of 4500 rev/mins;
(8) will be placed in through the sample that step (7) is processed heat treatment 2h under the high temperature of 1100 ℃, generate CeO
2Film; The programming rate of this step is 400 ℃/h;
(9) on the sample of processing through step (8) successively according to step (5)-(6) and step (7)-(8) alternating deposit YBCO film and CeO
2Film carries out 500 ℃ of heat treatment 1h at last in 500sccm oxygen atmosphere, prepare YBCO/CeO
2/ YBCO/CeO
2/ YBCO five layer thicknesses are the YBCO superconducting thick-film of 1.5 microns.Be used in PhilipsX ' Pert type X-ray diffractometer and sample done the ω scanning of (005) face, as shown in Figure 3.The halfwidth at YBCO (005) peak is only 0.85 °, illustrates that ybco film has orientation in good face, does not exist high-angle boundary.
Embodiment 4
(1) take yttrium acetate, barium acetate and copper acetate and be respectively 0.01mol, 0.02mol and 0.03mol, be dissolved in wiring solution-forming in the 200ml deionized water of the trifluoroacetic acid that contains 20mol% after yttrium acetate, barium acetate and copper acetate are mixed;
(2) solution that step (1) is made then adopts Rotary Evaporators to steam to desolventize and obtains gel after magnetic stirrer 2h;
(3) methyl alcohol of 60mL is added in the gel that described step (2) makes, then adopt again Rotary Evaporators to steam after magnetic stirrer 1h to desolventize with the impurity such as further removal moisture and obtain very pure gel;
(4) gel that step (3) is made joins in 30ml methyl alcohol, the precursor liquid that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 2mol/L;
(5) precursor liquid that step (4) is made is coated on the lanthanuma luminate single crystal substrate with the pull rate of 10cm/min;
(6) the coated substrate of step (5) that coating is good is placed on to send in quartz boat in the quartzy stove of high-temperature tubular and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains at last the YBCO film of Tetragonal;
Low Temperature Heat Treatment is to carry out under moistening Oxygen Condition, through the vial that distilled water is housed, steam to be brought the oxygen of 500sccm into reative cell, make that in reative cell, water vapour pressure is 130hPa, on average be warming up to 400 ℃ with the heating rate of 40 ℃/h from room temperature, and then stove is cooled to room temperature.The purpose of Low Temperature Heat Treatment is to decompose trifluoroacetate, forms unformed precursor film and discharges harmful residual substance.The whole resolving time is about 10h;
High-temperature heat treatment is to carry out under moistening oxygen and argon gas mixed atmosphere, the argon gas mist that 500sccm is contained 500ppm oxygen is brought steam into reative cell through the vial that distilled water is housed, make that in reative cell, water vapour pressure is 200hPa, heating rate with 400 ℃/h rose to 800 ℃ of the highest temperatures before this, directly pass into the argon gas mist that contains 500ppm oxygen after 800 ℃ of insulation 3h, then be cooled to room temperature with 100 ℃/h, obtain the YBCO film of Tetragonal;
(7) the acetylacetone,2,4-pentanedione cerium with 0.00025mol is dissolved in the methyl alcohol of 10mL in room temperature, and preparation obtains the precursor liquid that the metallic cerium ion concentration is 0.25mol/L; This precursor liquid is spin-coated on ybco film through step (6) sintering with the speed of 3000 rev/mins;
(8) will be placed in through the sample that step (7) is processed heat treatment 1.5h under the high temperature of 1050 ℃, generate CeO
2Film; The programming rate of this step is 400 ℃/h;
(9) on the sample of processing through step (8) successively according to step (5)-(6) and step (7)-(8) alternating deposit YBCO film and CeO
2Film carries out 500 ℃ of heat treatment 1h at last in 500sccm oxygen atmosphere, prepare YBCO/CeO
2/ YBCO/CeO
2/ YBCO five layer thicknesses are the YBCO superconducting thick-film of 1.5 microns.With field emission scanning electron microscope, this sample has been carried out the surface topography observation, the YBCO thick film surface is smooth, fine and close, there is no crackle, as shown in Figure 4.Adopt Philips X ' Pert type X-ray diffractometer sample to be done the ω scanning of (005) face, as shown in Figure 5.The halfwidth at YBCO (005) peak is only 0.72 °, illustrates that ybco film has orientation in good face, does not exist high-angle boundary.With Lepi-system, the YBCO thick film that prepared one-tenth contains nano-titanium oxide has been carried out the test of critical current density, critical current Ic/cm maximum reaches 570A/cm, as shown in Figure 6.
Claims (2)
1. the preparation method of a YBCO superconduction composite membrane, is characterized in that, described preparation YBCO superconducting thick-film method comprises the steps:
(1) according to Y: Ba: Cu=1.5: the mol ratio of 2: 3 is with Y (CH
3COO)
3, Ba (CH
3COO)
2And Cu (CH
3COO)
2Mix, be dissolved under room temperature in the deionized water of the trifluoroacetic acid that contains 10-30mol%, be made into the solution of trifluoroacetate, in described trifluoroacetic acid salting liquid, the mol ratio of solute and solvent is 1: 100;
(2) with the trifluoroacetic acid salting liquid of step (1) preparation through magnetic stirrer 1-3h, then adopt Rotary Evaporators to steam to desolventize to obtain gel;
(3) gel that described step (2) is made adds in methyl alcohol, gel in this step and the mol ratio of methyl alcohol are 1: 50, after magnetic stirrer 0.5-1.5h, then adopt the Rotary Evaporators steaming to desolventize, with impurity such as further removal moisture, obtain pure gel;
(4) gel that described step (3) is made joins in methyl alcohol, the precursor liquid that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5-3.0mol/L;
(5) the described precursor liquid of above-mentioned steps (4) being made adopts spin coating or method of pulling up to be coated on substrate;
(6) substrate after step (5) applies is placed in the quartzy stove of high-temperature tubular, carries out the Low Temperature Heat Treatment of 10h at 300 ℃ of-500 ℃ of temperature, decompose trifluoroacetate; The heating rate of this step is 40 ℃/h;
(7) will be placed in through the substrate that step (6) is processed heat treatment 2-4h under the high temperature of 750 ℃-850 ℃, generate Tetragonal YBCO film; The programming rate of this step is 400 ℃/h;
(8) the acetylacetone,2,4-pentanedione cerium is dissolved in methyl alcohol in room temperature, preparation obtains the precursor liquid that the metallic cerium ion concentration is 0.1～0.5mol/L; This precursor liquid is spin-coated on ybco film through step (7) sintering;
(9) will be placed in through the sample that step (8) is processed heat treatment 1-2h under the high temperature of 1000 ℃-1100 ℃, generate CeO
2Film; The programming rate of this step is 400 ℃/h;
(10) on the sample of processing through step (9) successively according to step (5)-(7) and step (8)-(9) alternating deposit YBCO film and CeO
2Film is heat-treated in the oxygen atmosphere at last and is prepared YBCO/CeO
2/ YBCO/CeO
2/ YBCO five layer thicknesses are the YBCO superconducting thick-film of 1.5 microns.
2. the preparation method of YBCO superconduction composite membrane as claimed in claim 1, is characterized in that, substrate described in described step (5) is lanthanum aluminate, strontium titanates or magnesium oxide single-crystal substrate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101148030A CN102690114B (en) | 2012-04-18 | 2012-04-18 | Method for preparing YBCO superconducting composite film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101148030A CN102690114B (en) | 2012-04-18 | 2012-04-18 | Method for preparing YBCO superconducting composite film |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102690114A CN102690114A (en) | 2012-09-26 |
| CN102690114B true CN102690114B (en) | 2013-11-06 |
Family
ID=46855872
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012101148030A Expired - Fee Related CN102690114B (en) | 2012-04-18 | 2012-04-18 | Method for preparing YBCO superconducting composite film |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102690114B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086722B (en) * | 2013-01-31 | 2015-04-15 | 清华大学 | Preparation method of high temperature superconducting film |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6383989B2 (en) * | 2000-06-21 | 2002-05-07 | The Regents Of The University Of California | Architecture for high critical current superconducting tapes |
| CN102255041B (en) * | 2011-07-13 | 2013-07-03 | 中国科学院电工研究所 | Preparation method of YBCO (Yttrium Barium Copper Oxide) superconducting thin film |
-
2012
- 2012-04-18 CN CN2012101148030A patent/CN102690114B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN102690114A (en) | 2012-09-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| RU2662040C1 (en) | Oxide superconductor and method of its manufacture | |
| EP1805817A2 (en) | Thick superconductor films with improved performance | |
| WO2008100281A2 (en) | High temperature superconductors having planar magnetic flux pinning centers and methods for making the same | |
| CN102931338B (en) | A kind of YBCO superconducting film with multi-layer compound structure and preparation method thereof | |
| CN102531567A (en) | Preparation method of high temperature superconductive film adopting modified low fluoride solution method | |
| CN102731083B (en) | Method for preparing yttrium-barium-copper-oxygen high-temperature superconducting film | |
| CN102173820B (en) | Preparation method of YBa2Cu3O7-x(YBCO) high-temperature superconductive thick film | |
| CN102255041B (en) | Preparation method of YBCO (Yttrium Barium Copper Oxide) superconducting thin film | |
| CN101320604B (en) | SrZrO3 doped YBCO thin film and preparation method thereof | |
| CN101747031B (en) | High-temperature superconducting nanometer composite film and method for preparing same | |
| CN102584204A (en) | Method for preparing yttrium barium copper oxide (YBCO) superconductive composite film | |
| WO2011017454A1 (en) | Critical current density enhancement via incorporation of nanoscale ba2(y,re) tao6 in rebco films | |
| CN105541317B (en) | A kind of preparation method of yttrium barium copper oxide superconducting thick-film | |
| CN101471161B (en) | Method for producing high-temperature superconducting thin film by tri-fluorate | |
| CN104446435B (en) | The preparation method of Ag doping terres rares barium copper oxygen conductor of high-temperature superconductor coat material | |
| CN202871869U (en) | YBCO superconducting film having multilayered composite structure | |
| CN102690114B (en) | Method for preparing YBCO superconducting composite film | |
| CN105198401A (en) | Method for preparing double mismatch multi-element doped composite YBCO thin film | |
| Feng et al. | Property improvement of 600-nm-thick YBCO superconducting films fabricated using a Pb-modified MOD method | |
| CN101746807A (en) | Method for increasing thickness of YBCO film prepared through TFA-MOD method | |
| CN103274682B (en) | Preparation method of high-temperature superconductive film | |
| AU2021102202A4 (en) | Multilayer structure for high-temperature superconductor-coated conductors and method for preparing thick films | |
| JP6212241B2 (en) | Superconductor and manufacturing method thereof | |
| JP6602427B2 (en) | Oxide superconductor | |
| CN102751044A (en) | Preparation method of yttrium barium copper oxide (YBCO) coating conductor |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131106 Termination date: 20140418 |