CN102255041B - Preparation method of YBCO (Yttrium Barium Copper Oxide) superconducting thin film - Google Patents
Preparation method of YBCO (Yttrium Barium Copper Oxide) superconducting thin film Download PDFInfo
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- CN102255041B CN102255041B CN 201110195847 CN201110195847A CN102255041B CN 102255041 B CN102255041 B CN 102255041B CN 201110195847 CN201110195847 CN 201110195847 CN 201110195847 A CN201110195847 A CN 201110195847A CN 102255041 B CN102255041 B CN 102255041B
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Abstract
The invention discloses a preparation method of a YBCO (Yttrium Barium Copper Oxide) superconducting thin film. The method comprises the following steps of: preparing a precursor solution, mixing yttrium acetate Y(CH3COO)3, barium acetate Ba(CH3COO)2 and copper acetate Cu(CH3COO)2 in the molar ratio (1.2-1.5):2:3 and dissolving the mixture into 10-30 mole percent aqueous solution of trifluoroacetic acid; uniformly stirring and evaporating a solvent in vacuum to obtain gel; adding methanol, uniformly stirring and evaporating a solvent to obtain gel; adding an appropriate amount of methanol and terpineol to obtain a solution in which the total concentration of metal ions such as Y, Ba and Cu is 1.5-3.0 mol/L, uniformly stirring and adding zirconium acetylacetonate in which the total ion molar concentration of three metals is 5-10 percent to obtain a precursor solution; coating the precursor solution on a substrate; thermally treating a coated thin film at the low temperature 300-500 DEG C and decomposing trifluoroacetates; and thermally treating at high temperature 750-850 DEG C and annealing at the temperature 450-550 DEG C to form the YBCO superconducting thin film containing nanometer yttrium oxide and nanometer barium zirconate. The critical current density of the YBCO thin film is 6 MA/cm<2> (77K, 0T).
Description
Technical field
The present invention relates to a kind of preparation method of second generation belt material of high temperature superconduct, particularly a kind of preparation method of YBCO superconducting thin film.
Background technology
Second generation belt material of high temperature superconduct refers to the terres rares barium-copper oxide superconducting coating conductor based on the YBCO-123 series superconducting material.It is made of metal alloy base band, Seed Layer, barrier layer, cap layer, rare earth barium copper oxide superconducting layer, protective layer and stabilized zone etc., is a kind of sandwich construction.Compare with first generation Bi based high-temperature superconductive strip, second generation belt material of high temperature superconduct has the ability of the high electric current of load under the highfield, can under higher temperature and magnetic field, use, and be the focus that various countries competitively research and develop in the high-temperature superconductor field.
At present, have at least 7 tame units all to prepare length in the world and surpass 100m, Ic surpasses the band of 150A.Especially the Superpower company of the U.S., it has been prepared and has reached 1311m, and Ic reaches the long band of km level of 153A, has stepped major step to batch process.But the cost for preparing the YBCO band now remains 50 times of copper cash, and the performance that must further improve the YBCO coating conductor could satisfy requirement widely.
YBCO can use in the forceful electric power field as coating conductor, mainly be since it have can load current and the characteristic of not loss.Concerning same band, the critical current density (Jc) that increases it has also just improved its current capacity.Therefore the critical current density that improves the YBCO superconducting film is research focus in recent years.
The people such as J.L.MacManus-Driscoll of U.S. Los Alamos National Laboratories and Cambridge University then directly mix zirconia and excessive barium dust in the YBCO ceramic target, adopt the PLD method to obtain containing the BaZrO that is of a size of 10nm according to the process conditions of preparation ybco film
3(BZO) laminated film of particle.Its critical current density all is higher than the critical current density of pure ybco film at whole externally-applied magnetic field, and especially when externally-applied magnetic field was 7T, its critical current density was five times of pure ybco film.Barcelona, ESP university 2007 has reported at Nature materials that employing trifluoroacetate-metal organic deposit method (TFA-MOD method) has prepared contains nanometer BaZrO
3Ybco film.Its critical current density has not only had large increase than the pure ybco film of TFA-MOD method preparation, and its pining force to be issued to maximum in the condition of 77K, externally-applied magnetic field 2T be 21GN m-3, BZO/YBCO nano compound film than the preparation of PLD method has improved 175%, has improved 60% than the performance at the NiTb of 4.2K alloy.The preparation method that the present domestic patent overwhelming majority about the YBCO superconducting film is ybco film has only Chinese patent CN 101320604A (Granted publication 101320604B) to mention in the YBCO superconducting film and adds SrZrO
3Improve the effect of its critical current density.But the doping SrZrO for preparing in this patent
3Just just increase in High-Field lower critical current density.
Summary of the invention
The objective of the invention is to overcome the more weak shortcoming of YBCO superconducting thin film current capacity of prior art for preparing, a kind of preparation method of ybco film of critical current density of effective raising ybco film is provided.
The present invention contains the ybco film of nano yttrium oxide and nanometer barium zirconate by adopting trifluoroacetate-metal organic deposit (TFA-MOD) method preparation, the present invention adds terpinol and acetylacetone,2,4-pentanedione zirconium in the precursor liquid that contains trifluoroacetic acid yttrium, trifluoroacetic acid barium and trifluoroacetic acid copper, and makes the proportioning of trifluoroacetic acid yttrium excessive.Concentration by the control metal ion, after through low temperature thermal decomposition and high temperature sintering, prepare the YBCO superconducting thin film that contains nano yttrium oxide and nanometer barium zirconate, utilized two kinds of nano particle synergies of nano yttrium oxide and nanometer barium zirconate, the flux pinning effect that improves ybco film.
Concrete steps order of the present invention is as follows:
(1) according to Y: Ba: Cu=1.2-1.5: 2: 3 mol ratio is Y (CH
3COO)
3, Ba (CH
3COO)
2And Cu (CH
3COO)
2Three kinds of powder are dissolved under room temperature in the deionized water of the trifluoroacetic acid that contains 10-30mol%, wiring solution-forming, and the mol ratio of solute and solvent is 1: 100 in the described solution;
(2) the described solution that step (1) is prepared adopts Rotary Evaporators to steam to desolventize again and obtains gel through magnetic stirrer 1-3h;
(3) gel that described step (2) is made adds in the methyl alcohol, gel in this step and the mol ratio of methyl alcohol are 1: 50, behind magnetic stirrer 0.5-1.5h, adopt Rotary Evaporators to steam again and desolventize, with impurity such as further removal moisture, obtain pure gel;
(4) gel that described step (3) is made joins in methyl alcohol and the terpinol, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5-3.0mol/L, the volume ratio of described methyl alcohol and terpinol is 1: 1, the solution that will contain described Y, Ba and Cu stirs, add the acetylacetone,2,4-pentanedione zirconium again, the acetylacetone,2,4-pentanedione zirconium that adds is Y, Ba in the described Y of containing, Ba and the Cu solution and the 5%-10% of three kinds of total ion molar concentrations of metal of Cu, is prepared into precursor liquid;
(5) precursor liquid of described step (4) being made adopts spin coating or method of pulling up to be coated on the substrate;
(6) substrate after step (5) applies is placed the quartzy stove of high-temperature tubular, under 300 ℃ of-500 ℃ of temperature, carry out the Low Temperature Heat Treatment of 10h, decompose trifluoroacetate; The heating rate of this step is 40 ℃/h;
(7) will place heat treatment 2-4h under 750 ℃～-850 ℃ the high temperature through the substrate that described step (6) is handled, generate the cubic phase YBCO film that contains nano yttrium oxide, nanometer barium zirconate; The programming rate of this step is 400 ℃/h;
(8) will place through the substrate that step (7) is handled under 450 ℃-550 ℃ and the pure oxygen condition the film heat treatment 0.5-1.5h that anneals, be prepared into the YBCO superconducting thin film that contains nano yttrium oxide and nanometer barium zirconate.
Substrate described in the 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 adds terpinol and acetylacetone,2,4-pentanedione zirconium in traditional precursor liquid that contains trifluoroacetic acid yttrium, trifluoroacetic acid barium and trifluoroacetic acid copper.And make the proportioning of trifluoroacetic acid yttrium excessive.By the concentration of control metal ion, after through low temperature thermal decomposition and high temperature sintering, prepared the YBCO superconducting thin film that contains nano yttrium oxide and nanometer barium zirconate.These have the yittrium oxide of nano-scale and the effect that barium zirconate has well played flux pinning, and compare with single nano particle, and the nano-substance of two kinds of different structures can be worked in coordination with the critical current density that improves the YBCO film.Adopting the ybco film critical current density of this method preparation is at null field or at High-Field raising to be arranged all, reaches 6MA/cm in null field lower critical current density
2, improved the current capacity of YBCO thick film greatly, 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 film of embodiment 1 preparation;
Fig. 2 is the X ray diffracting spectrum of the YBCO film of embodiment 2 preparations;
Fig. 3 is the critical current density curve of the YBCO film of embodiment 2 preparations;
Fig. 4 is the X ray diffracting spectrum of the YBCO film of embodiment 3 preparations;
Fig. 5 is the critical transition temperature curve of the YBCO film of embodiment 4 preparations.
Embodiment
Embodiment 1
(1) takes by weighing yttrium acetate, barium acetate and copper acetate and be respectively 0.006mol, 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 adopts Rotary Evaporators to steam to desolventize again and obtains gel behind magnetic stirrer 1h;
(3) methyl alcohol of 1.55mol is added in the gel that described step (2) makes, behind magnetic stirrer 0.5h, adopt Rotary Evaporators to steam again again to desolventize with impurity such as further removal moisture to obtain very pure gel;
(4) gel that step (4) is made joins in the mixed liquor of 10.3ml methyl alcohol and 10.3ml terpinol, and the volume ratio of described methyl alcohol and terpinol is 1: 1, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5mol/L.The methyl alcohol that contains Y, Ba and Cu and the terpineol solution of gained are stirred, add the acetylacetone,2,4-pentanedione zirconium again, the acetylacetone,2,4-pentanedione zirconium that adds be in the described Y of containing, Ba and three kinds of metallic solutions of Cu Y, Ba and three kinds of total ion molar concentrations of metal of Cu 5%, be prepared into precursor liquid;
(5) precursor liquid that step (4) is made is spin-coated on the strontium titanate monocrystal chip with 1500 rev/mins speed, and the spin coating time is 90s;
(6) the coated substrate of step (5) that coating is good is placed on to send in the quartz boat in the quartzy stove of high-temperature tubular and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains containing the YBCO high temperature superconducting film of nano yttrium oxide and nanometer barium zirconate at last.
Low Temperature Heat Treatment is to carry out under the moistening oxygen condition, be through the vial that distilled water is housed steam to be brought the oxygen of 500sccm into reative cell, make that water vapour pressure is 100hPa in the reative cell, 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.
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 water vapour pressure is 160hPa in the reative cell, heating rate with 400 ℃/h rose to 750 ℃ of the highest temperatures before this, behind 750 ℃ of insulation 2h, directly feed the argon gas mist that contains 500ppm oxygen, be cooled to 450 ℃ with 100 ℃/h then, insulation 0.5h makes the YBCO oxygen uptake of cubic phase change the YBCO with superconductivity of quadrature phase in 450 ℃ purity oxygen atmosphere, and sample stove under the oxygen atmosphere is chilled to room temperature subsequently.With field emission scanning electron microscope sample has been carried out the surface topography observation, the YBCO thick film surface is smooth, fine and close; And film surface is obviously found out nano particle, as shown in Figure 1.
Embodiment 2
(1) takes by weighing yttrium acetate, barium acetate and copper acetate and be respectively 0.0135mol, 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) the described solution that step (1) is made adopts Rotary Evaporators to steam to desolventize again and obtains gel behind magnetic stirrer 2h;
(3) 3.175mol methyl alcohol is joined in the gel that step (2) makes, behind magnetic stirrer 1h, adopt Rotary Evaporators to steam again again to desolventize with impurity such as further removal moisture to obtain very pure gel;
(4) gel that step (3) is made joins in the mixed liquor of 15.8ml methyl alcohol and 15.8ml terpinol, and the volume ratio of described methyl alcohol and terpinol is 1: 1, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 2.0mol/L.The methyl alcohol that contains Y, Ba and Cu and the terpineol solution of gained are stirred, add the acetylacetone,2,4-pentanedione zirconium again, the titanium acetylacetone that adds be in the methyl alcohol of the described Y of containing, Ba and Cu and the terpineol solution Y, Ba and three kinds of total ion molar concentrations of metal of Cu 7.5%, be prepared into precursor liquid;
(5) precursor liquid that step (4) is made is spin-coated on the lanthanuma luminate single crystal substrate with 1500 rev/mins speed, and the spin coating time is 90s;
(6) substrate that coating is good is placed on to send in the quartz boat in the quartzy stove of tubular type and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains containing the YBCO high temperature superconducting film of nano yttrium oxide and nanometer barium zirconate at last.
Low Temperature Heat Treatment is to carry out under the moistening oxygen condition, be through the vial that distilled water is housed steam to be brought the oxygen of 500sccm into reative cell, make that water vapour pressure is 130hPa in the reative cell, 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 water vapour pressure is 200hPa in the reative cell, heating rate with 400 ℃/h rose to 800 ℃ of the highest temperatures before this, behind 800 ℃ of insulation 3h, directly feed the argon gas mist that contains 500ppm oxygen, be cooled to 500 ℃ with 100 ℃/h then, insulation 1h makes the YBCO oxygen uptake of cubic phase change the YBCO with superconductivity of quadrature phase in 500 ℃ purity oxygen atmosphere, and sample stove under the oxygen atmosphere is chilled to room temperature subsequently.
With X-ray diffractometer sample has been carried out analysis of components.Compare with the XRD of the pure ybco film shown in Fig. 2 a, except YBCO (001) diffraction maximum is arranged, also have some more weak diffraction maximums in addition in the sample.Through the retrieval of JCPDS card, (622) and (200) diffraction maximum of barium zirconate of the corresponding yittrium oxide of diffraction maximum difference that these intensity are more weak illustrate and contain yittrium oxide and barium zirconate in the prepared ybco film, as shown in Figure 2.Adopt comprehensive rerum natura to measure (PPMS) sample has been carried out the M-H test, by the Bean model sample critical current density is calculated, as shown in Figure 3.No matter be that the critical current density that contains the ybco film of yittrium oxide and barium zirconate under the null field or under the High-Field all is higher than pure ybco film.
Embodiment 3
(1) takes by weighing yttrium acetate, barium acetate and copper acetate and be respectively 0.0225mol, 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 adopts Rotary Evaporators to steam to desolventize again and obtains gel behind magnetic stirrer 3h;
(3) methyl alcohol of 4.875mol is joined in the gel that step (2) makes, behind magnetic stirrer 1.5h, adopt Rotary Evaporators to steam again again to desolventize with impurity such as further removal moisture to obtain very pure gel;
(4) gel that step (3) is made joins in the mixed liquor of 16.25ml methyl alcohol and 16.25ml terpinol, and the volume ratio of described methyl alcohol and terpinol is 1: 1, makes Y, Ba and Cu three metal ion species concentration are the solution of 3.0mol/L.The methyl alcohol that contains Y, Ba and Cu and the terpineol solution of gained are stirred, add the acetylacetone,2,4-pentanedione zirconium again, the acetylacetone,2,4-pentanedione zirconium that adds be in the methyl alcohol of the described Y of containing, Ba and Cu and the terpineol solution Y, Ba and three kinds of total ion molar concentrations of metal of Cu 10%, be prepared into precursor liquid;
(5) speed of above-mentioned precursor liquid with 1500 rev/mins is spin-coated on the lanthanuma luminate single crystal matrix, the spin coating time is 90s;
(6) sample that coating is good is placed on to send in the quartz boat in the quartzy stove of tubular type and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains containing the YBCO high temperature superconducting film of yittrium oxide and nanometer barium zirconate at last.Low Temperature Heat Treatment is to carry out under the moistening oxygen condition, be through the vial that distilled water is housed steam to be brought the oxygen of 500sccm into reative cell, make that water vapour pressure is 160hPa in the reative cell, on average be warming up to 500 ℃ with the heating rate of 40 ℃/h from room temperature, and then stove is chilled 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 water vapour pressure is 240hPa in the reative cell, heating rate with 400 ℃/h rose to 850 ℃ of the highest temperatures before this, behind 850 ℃ of insulation 4h, directly feed the argon gas mist that contains 500ppm oxygen, be cooled to 550 ℃ with 100 ℃/h then, insulation 1.5h makes the YBCO oxygen uptake of cubic phase change the YBCO with superconductivity of quadrature phase in 550 ℃ purity oxygen atmosphere, and sample stove under the oxygen atmosphere is cooled to room temperature subsequently.With X-ray diffractometer sample has been carried out analysis of components.Except YBCO (001) diffraction maximum, also have some more weak diffraction maximums in addition in the sample.Through the retrieval of JCPDS card, (622) and (200) diffraction maximum of barium zirconate of the corresponding yittrium oxide of diffraction maximum difference that these intensity are more weak illustrate and contain yittrium oxide and barium zirconate in the prepared ybco film, as shown in Figure 4.
Embodiment 4
(1) takes by weighing yttrium acetate, barium acetate and copper acetate and be respectively 0.0135mol, 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) the described solution that step (1) is made adopts Rotary Evaporators to steam to desolventize again and obtains gel behind magnetic stirrer 2h;
(3) 3.175mol methyl alcohol is joined in the gel that step (2) makes, behind magnetic stirrer 1h, adopt Rotary Evaporators to steam again again to desolventize with impurity such as further removal moisture to obtain very pure gel;
(4) gel that step (3) is made joins in the mixed liquor of 15.8ml methyl alcohol and 15.8ml terpinol, and the volume ratio of described methyl alcohol and terpinol is 1: 1, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 2.0mol/L.The methyl alcohol that contains Y, Ba and Cu and the terpineol solution of gained are stirred, add the acetylacetone,2,4-pentanedione zirconium again, the titanium acetylacetone that adds be in the methyl alcohol of the described Y of containing, Ba and Cu and the terpineol solution Y, Ba and three kinds of total ion molar concentrations of metal of Cu 7.5%, be prepared into precursor liquid;
(5) precursor liquid that step (4) is made is coated on the magnesium oxide single-crystal substrate with 5 millimeters/minute pull rate;
(6) substrate that coating is good is placed on to send in the quartz boat in the quartzy stove of tubular type and carries out Low Temperature Heat Treatment and high-temperature heat treatment, obtains containing the YBCO high temperature superconducting film of nano yttrium oxide and nanometer barium zirconate at last.
Low Temperature Heat Treatment is to carry out under the moistening oxygen condition, be through the vial that distilled water is housed steam to be brought the oxygen of 500sccm into reative cell, make that water vapour pressure is 130hPa in the reative cell, 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 water vapour pressure is 200hPa in the reative cell, heating rate with 400 ℃/h rose to 800 ℃ of the highest temperatures before this, behind 800 ℃ of insulation 3h, directly feed the argon gas mist that contains 500ppm oxygen, be cooled to 500 ℃ with 100 ℃/h then, insulation 1h makes the YBCO oxygen uptake of cubic phase change the YBCO with superconductivity of quadrature phase in 500 ℃ purity oxygen atmosphere, and sample stove under the oxygen atmosphere is chilled to room temperature subsequently.
Fig. 5 is sample critical transition temperature curve.The sample critical transition temperature is about 91K as can be seen from Figure 5, and is suitable with pure YBCO.
Claims (2)
1. the preparation method of a YBCO superconducting thin film, described preparation method adds terpinol and acetylacetone,2,4-pentanedione zirconium in the precursor liquid that contains trifluoroacetic acid yttrium, trifluoroacetic acid barium and trifluoroacetic acid copper, and makes the proportioning of trifluoroacetic acid yttrium excessive; Concentration by the control metal ion, through low temperature thermal decomposition and high temperature sintering, preparation contains the YBCO superconducting thin film of nano yttrium oxide and nanometer barium zirconate, utilize two kinds of nano particle synergies of nano yttrium oxide and nanometer barium zirconate, improve the flux pinning effect of ybco film, it is characterized in that described preparation method comprises the steps:
(1) according to the mol ratio of Y:Ba:Cu=1.2-1.5:2:3 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, the mol ratio of solute and solvent is 1:100 in the described trifluoroacetic acid salting liquid;
(2) the trifluoroacetic acid salting liquid that step (1) is prepared adopts Rotary Evaporators to steam to desolventize again and obtains gel through magnetic stirrer 1-3h;
(3) gel that described step (2) is made adds in the methyl alcohol, gel in this step and the mol ratio of methyl alcohol are 1:50, behind magnetic stirrer 0.5-1.5h, adopt Rotary Evaporators to steam again and desolventize, with impurity such as further removal moisture, obtain pure gel;
(4) gel that described step (3) is made joins in methyl alcohol and the terpinol, the solution that to make three kinds of metal total ion concentrations of Y, Ba and Cu be 1.5-3.0mol/L, and the volume ratio of described methyl alcohol and terpinol is 1:1; The solution that will contain described Y, Ba and Cu stirs, and adds the acetylacetone,2,4-pentanedione zirconium again, and the acetylacetone,2,4-pentanedione zirconium that adds is Y, Ba in the described Y of containing, Ba and the Cu solution and the 5%-10% of three kinds of total ion molar concentrations of metal of Cu, is prepared into precursor liquid;
(5) the described precursor liquid of above-mentioned steps (4) being made adopts spin coating or method of pulling up to be coated on the substrate;
(6) substrate after step (5) applies is placed the quartzy stove of high-temperature tubular, under 300oC-500 ° of C temperature, carry out the Low Temperature Heat Treatment of 10h, decompose trifluoroacetate; The heating rate of this step is 40 ° of C/h;
(7) will place heat treatment 2-4h under the high temperature of 750 ° of C-850 ° of C through the substrate that step (6) is handled, generate the cubic phase YBCO film that contains nano yttrium oxide, nanometer barium zirconate; The programming rate of this step is 400 ° of C/h;
(8) will place through the substrate that step (7) is handled under 450 ° of C-550 ° of C and the pure oxygen condition the film heat treatment 0.5-1.5h that anneals, be prepared into the YBCO superconducting thin film that contains nano yttrium oxide and nanometer barium zirconate.
2. the preparation method of a kind of YBCO superconducting thin film as claimed in claim 1 is characterized in that, substrate described in the described step (5) is lanthanum aluminate, strontium titanates or magnesium oxide single-crystal substrate.
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| CN102584204A (en) * | 2012-02-12 | 2012-07-18 | 中国科学院电工研究所 | Method for preparing yttrium barium copper oxide (YBCO) superconductive composite film |
| CN102690114B (en) * | 2012-04-18 | 2013-11-06 | 中国科学院电工研究所 | Method for preparing YBCO superconducting composite film |
| CN102731083B (en) * | 2012-04-18 | 2014-02-26 | 中国科学院电工研究所 | Method for preparing yttrium-barium-copper-oxygen high-temperature superconducting film |
| CN102751044A (en) * | 2012-07-03 | 2012-10-24 | 中国科学院电工研究所 | Preparation method of yttrium barium copper oxide (YBCO) coating conductor |
| CN106374030A (en) * | 2016-11-10 | 2017-02-01 | 中国科学院电工研究所 | YBCO superconductive composite thin film preparation method |
| CN111533551B (en) * | 2020-05-08 | 2022-07-08 | 中国科学院电工研究所 | YBCO superconducting film and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101238597A (en) * | 2005-07-26 | 2008-08-06 | 洛斯阿拉莫斯国家安全股份有限公司 | Structure for improved high critical current densities in YBCO coatings |
| CN101258618A (en) * | 2004-10-01 | 2008-09-03 | 美国超导公司 | Thick superconductor films with improved performance |
| CN101320604A (en) * | 2008-07-04 | 2008-12-10 | 北京工业大学 | SrZrO3 doped YBCO thin film and preparation method thereof |
| CN101471161A (en) * | 2007-12-28 | 2009-07-01 | 北京有色金属研究总院 | Method for producing high-temperature superconducting thin film by tri-fluorate |
| CN101747031A (en) * | 2008-12-16 | 2010-06-23 | 北京有色金属研究总院 | High-temperature superconducting nanometer composite film and method for preparing same |
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| CN101258618A (en) * | 2004-10-01 | 2008-09-03 | 美国超导公司 | Thick superconductor films with improved performance |
| CN101238597A (en) * | 2005-07-26 | 2008-08-06 | 洛斯阿拉莫斯国家安全股份有限公司 | Structure for improved high critical current densities in YBCO coatings |
| CN101471161A (en) * | 2007-12-28 | 2009-07-01 | 北京有色金属研究总院 | Method for producing high-temperature superconducting thin film by tri-fluorate |
| CN101320604A (en) * | 2008-07-04 | 2008-12-10 | 北京工业大学 | SrZrO3 doped YBCO thin film and preparation method thereof |
| CN101747031A (en) * | 2008-12-16 | 2010-06-23 | 北京有色金属研究总院 | High-temperature superconducting nanometer composite film and method for preparing same |
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