CN102701729A - Sm1-xCaxBiO3 buffering layer of high-temperature superconductivity coated conductor and preparation method thereof - Google Patents
Sm1-xCaxBiO3 buffering layer of high-temperature superconductivity coated conductor and preparation method thereof Download PDFInfo
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- CN102701729A CN102701729A CN2012101495784A CN201210149578A CN102701729A CN 102701729 A CN102701729 A CN 102701729A CN 2012101495784 A CN2012101495784 A CN 2012101495784A CN 201210149578 A CN201210149578 A CN 201210149578A CN 102701729 A CN102701729 A CN 102701729A
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Abstract
The invention discloses a Sm1-xCaxBiO3 buffering layer of a high-temperature superconductivity coated conductor and a preparation method thereof. After Ca replaces Sm of a SmBiO3 buffering layer of the high-temperature superconductivity coated conductor, the element environment and lattice parameters of the SmBiO3 buffering layer are finely adjusted, accordingly the situation that lattices of the SmBiO3 buffering layer and an REBCO superconductivity layer are mismatched with each other is improved, and a series of novel Sm1-xCaxBiO3 buffering layer of the high-temperature superconductivity coated conductor is obtained, wherein the x is greater than or equal to 0.1 and less than or equal to 0.4. In addition, the buffering layer can extend and grow in the air with the temperature of 800 DEG C and is compact in structure and flat in surface, and the structural stability is kept in the follow-up preparation process of the superconductivity layer of the high-temperature superconductivity coated conductor. The method adopts a chemical solution sedimentation process using nitrate as a predecessor to perform preparation in the air and has the advantages of being low in cost, suitable for large-scale sedimentation and the like.
Description
Technical field
The invention belongs to the high temperature superconducting materia preparing technical field, relate in particular to a kind of conductor of high-temperature superconductor coat Sm
1-xCa
xBiO
3Impact plies and technology of preparing thereof.
Background technology
As s-generation belt material of high temperature superconduct, RE, Ba and Cu oxide (REBCO) coating conductor is because its current capacity good under the upfield, in power system, gathers around to have broad application prospects.Such as a lot of application is arranged in multiple superconducting device; For example cable, X-former, generator and phonomoter. each developed country is from the technical renovation and the long-term interest of national electric power energy; Carry forward vigorously research of s-generation high-temperature superconductor and practicalization, international competition is more and more fierce.
But the dependence to oxygen in the preparation process of REBCO superconducting layer is very serious, and metal base is easy to oxidizedly in the preparation superconducting layer, and simultaneously metals ion also can spread to superconducting layer, and this all will have a strong impact on the superconductivity of REBCO.Therefore; Between metal substrate and REBCO, must increase one deck cushioning layer material; Should serve as metal substrate to the epitaxially grown intermediate die plate of REBCO, stop the phase mutual diffusion of two kinds of materials again, could guarantee to prepare the REBCO conductor of high-temperature superconductor coat of excellent property like this.Therefore, conductor of high-temperature superconductor coat all has substrate, impact plies (one deck at least) and REBCO superconducting coating three-decker.
At present, each developed country drops into huge fund and has developed a series of cushioning layer materials with practicability level through the development of two more than ten years.Such as SrTiO
3, La
2Zr
2O
7, CeO
2, YSZ, RE
2O
3Deng.But these materials mostly fusing point are very high, need about 1000 ℃, just can be epitaxially grown to well behaved impact plies, and need under low oxygen partial pressure, prepare, and the preparation cost of great number has had a strong impact on the practicability progress of high temperature coating conductor.And these cushioning layer materials of what is more important are mostly in Europe, U.S.A, and under the intellectual property protection of states such as day, this will have a strong impact on and restrict China and on s-generation conductor of high-temperature superconductor coat, research and develop and industrialization production.
In addition, the method for preparing s-generation high temperature coating conductor buffer layer mainly comprises physics and chemical process.Wherein physical method comprises pulsed laser deposition (PLD), magnetron sputtering method (MSP), electron-beam evaporation (EBE) etc.Chemical process comprises chemical solution deposition (CSD) and metal organic-matter chemical hydatogenesis (MOCVD) etc.Compare with traditional physical vacuum sedimentation, chemical solution deposition (CSD) has with low cost, simple to operate, unique advantages such as the accurate and suitable big area deposition of Composition Control.Help accelerating s-generation conductor of high-temperature superconductor coat large-scale industrial application process.
Summary of the invention
The object of the present invention is to provide a kind of impact plies (Sm of conductor of high-temperature superconductor coat
1-xCa
xBiO
3).This impact plies can epitaxy in 800 ℃ of left and right sides air, its compact structure and surfacing.And in the preparation process of the superconducting layer of subsequently conductor of high-temperature superconductor coat, keep the stable of structure.
The technical solution adopted for the present invention to solve the technical problems is: a kind of conductor of high-temperature superconductor coat Sm
1-xCa
xBiO
3Impact plies, it is to conductor of high-temperature superconductor coat SmBiO
3Impact plies carries out the substituting and then oxide S m that extension becomes phase thermal treatment to generate of Ca of Sm
1-xCa
xBiO
3Sosoloid.0.1≤x≤0.4 wherein.
REBiO
3The series cushioning layer material is the new buffer layer material of Southwest Jiaotong University's superconduction and the independent research of new forms of energy center; And to they crystalline structure, become phase temperature, electricity, magnetic property and done research in the stability that REBCO prepares in the process; The result shows, REBiO
3The series cushioning layer material is complementary with REBCO on crystalline structure, and lower one-tenth phase temperature becomes the bright spot of this type of material; In addition in the preparation process of REBCO film, REBiO
3Also kept advantages of higher stability.So applied for patent of invention (application number is 200610020920.5), SmBiO in May, 2006
3Be REBiO
3One of series cushioning layer material, the Sm element has the ionic radius approaching with the Ca element in its chemical formula.To SmBiO
3After impact plies carries out the substituting of Ca of Sm, will be to SmBiO
3Impact plies element environment and lattice parameter produce fine setting, thus adjustment SmBiO
3The lattice mismatch situation of impact plies and REBCO superconducting layer.And obtained the impact plies Sm of a series of new conductor of high-temperature superconductor coat
1-xCa
xBiO
3, 0.1≤x≤0.4 wherein.To play important active effect to the patent protection of coating conductor buffer layer material and the blockade of its technology of preparing for breaking developed countries.And the achievement in research that will have the s-generation conductor of high-temperature superconductor coat of independent intellectual property right for China is acquired plays further in-depth and application turns usefulness into.
Sm in addition
1-xCa
xBiO
3Impact plies is by Sm
2O
3, CaO, Bi
2O
3Extension becomes phase thermal treatment to make Sm
2O
3, CaO, Bi
2O
3Lattice parameter mostly be cubic structure or tetragonal, and good matching is arranged, the Sm that generates by their solid solutions with REBCO superconducting layer lattice
1-xCa
xBiO
3Also should be with good with REBCO superconducting layer lattice match.The fusing point of CaO is about 2580 ℃, far above the fusing point (about 1050 ℃) of REBCO superconducting layer, with SmBiO
3Impact plies Sm element carries out the alternative Sm that makes of Ca element
1-xCa
xBiO
3Impact plies will keep the stable of structure in the preparation process of the superconducting layer of subsequently conductor of high-temperature superconductor coat.
Sm of the present invention
1-xCa
xBiO
3The performance of impact plies will have experiment provided by the present invention to obtain checking.
The present invention also aims to provide a kind of preparation conductor of high-temperature superconductor coat Sm
1-xCa
xBiO
3The method of buffer layer thin film.It is to adopt to prepare in air with the chemical solution deposition of nitrate salt as precursor, has advantages such as with low cost, suitable extensive deposition.To conductor of high-temperature superconductor coat SmBiO
3Alternative and then the extension that impact plies carries out the Ca of Sm becomes phase thermal treatment to generate oxide S m
1-xCa
xBiO
3Sosoloid, 0.1≤x≤0.4 wherein, its preparation method may further comprise the steps:
A, colloid for preparing: with precursor Sm, Ca, the nitrate salt of Bi are in metal cation ratio Sm: Ca: Bi=1-x: x: 1 ratio is dissolved in an amount of ROHM, wherein 0.1≤x≤0.4.The total volumetric molar concentration of final solution is about 0.2mol/L;
B, colloid coating and drying and thermal decomposition process: the colloid that a step is made is coated on the substrate, carries out drying again; After the drying, carry out aerial thermal decomposition process before the sintering, be about to be coated with the colloidal substrate and place sintering oven; Make furnace temperature slowly rise to 180 ℃-230 ℃ from room temperature; And rise at 280 ℃-300 ℃ with the speed of 0.1-2 ℃/min, the speed with 0.1-1 ℃/min rises to 560 ℃-580 ℃ again, is incubated 0.5 hour; So that it is the coating that sintering forms is more smooth, finer and close;
C, sinter phase into: after will being coated with colloidal substrate drying, putting into sintering oven again and sinter phase into, finally obtain Sm
1-xCa
xBiO
3Impact plies; The concrete practice is: in air, furnace temperature is risen to 790 ℃-810 ℃ with the speed of 10-100 ℃/min fast, be incubated 40-60 minute; Let furnace temperature slowly reduce to room temperature again.
When actual fabrication, said b is in the step, and colloid is coated in the on-chip concrete practice and is: on substrate, with the sol evenning machine rotation, make colloid evenly be coated on the substrate colloid drops; Said b in the step temperature when dry be 100 ℃ of-150 ℃ of dryings.
To conductor of high-temperature superconductor coat SmBiO
3Impact plies will make SmBiO after carrying out the substituting of Ca of Sm
3Impact plies element environment and lattice parameter produce fine setting, thus adjustment SmBiO
3The lattice mismatch situation of impact plies and REBCO superconducting layer.Compared with prior art, the invention has the beneficial effects as follows: this method cost is not high, and manufacture craft is simple, controls easily, is fit to extensive deposition.
Description of drawings
Fig. 1 is the Sm of embodiment one
0.9Ca
0.1BiO
3The X ray diffracting spectrum of impact plies.
Fig. 2 is the Sm of embodiment one
0.9Ca
0.1BiO
310000 times of sem (SEM) photo of impact plies.
Fig. 3 is the Sm of embodiment two
0.7Ca
0.3BiO
3The X ray diffracting spectrum of impact plies.
Fig. 4 is the Sm of embodiment two
0.7Ca
0.3BiO
310000 times of sem (SEM) photo of impact plies.
Fig. 5 is the Sm of embodiment three
0.6Ca
0.4BiO
3The X ray diffracting spectrum of impact plies.
Fig. 6 is the Sm of embodiment three
0.6Ca
0.4BiO
310000 times of sem (SEM) photo of impact plies.
Fig. 1,3,5 ordinate zou are diffraction intensity (Intensity), A.U. (a.u.); X-coordinate is diffraction angle 2 θ, and unit is degree (deg).
Below in conjunction with accompanying drawing and embodiment the present invention is done further detailed description.
Embodiment
Embodiment one
The present invention provides a kind of impact plies Sm of conductor of high-temperature superconductor coat
0.9Ca
0.1BiO
3And a kind of preparation conductor of high-temperature superconductor coat Sm
0.9Ca
0.1BiO
3The method of buffer layer thin film the steps include:
A, Sm
0.9Ca
0.1BiO
3The impact plies colloid for preparing: with precursor Sm, Ca, the nitrate salt of Bi is dissolved in an amount of ROHM (PAA) by cation concn at 0.9: 0.1: 1, thereby obtains organic-compound system.The total volumetric molar concentration of final solution is about 0.2mol/L.
B, Sm
0.9Ca
0.1BiO
3Buffer coated, dry and decomposition: the colloid that a step is made is coated in LaAlO
3On the monocrystal chip, carry out drying at 100 ℃ again; Be placed in the sintering oven again, in air, make furnace temperature slowly rise to 180 ℃ from room temperature, and rise at 280 ℃ with the speed of 0.1 ℃/min, the speed with 0.1 ℃/min rises to 570 ℃ again, is incubated 30 minutes.
C, sinter phase into: above-mentioned d is gone on foot prepared substrate put into sintering oven, in air, furnace temperature is risen to 790 ℃ with the speed of 10 ℃/min fast, be incubated 50 minutes; Let furnace temperature slowly reduce to room temperature again, finally obtain Sm
0.9Ca
0.1BiO
3Impact plies.
Fig. 5 is the Sm of the embodiment of the invention one
0.9Ca
0.1BiO
3The X ray diffracting spectrum of impact plies.Can find out by figure except Sm
0.9Ca
0.1BiO
3Impact plies (002) diffraction peak and substrate LaAlO
3Diffraction peak outside, no Sm
0.9Ca
0.1BiO
3Other assorted peaks hint out Sm
0.9Ca
0.1BiO
3There is the outer texture of very strong face in buffer layer thin film.
Fig. 2 is the embodiment of the invention one Sm
0.9Ca
0.1BiO
310000 times of sem (SEM) photo of impact plies.Can be known by Fig. 2: film sample surfacing, densification, no hole is seamless.Hence one can see that, and that this embodiment one prepared texture is good, the Sm that surface compact is smooth
0.9Ca
0.1BiO
3Buffer layer thin film.
Embodiment two
The present invention provides a kind of impact plies Sm of conductor of high-temperature superconductor coat
0.7Ca
0.3BiO
3And a kind of preparation conductor of high-temperature superconductor coat Sm
0.7Ca
0.3BiO
3The method of buffer layer thin film the steps include:
A, Sm
0.7Ca
0.3BiO
3The impact plies colloid for preparing: with precursor Sm, Ca, the nitrate salt of Bi is dissolved in an amount of ROHM (PAA) by cation concn at 0.7: 0.3: 1, thereby obtains organic-compound system.The total volumetric molar concentration of final solution is about 0.2mol/L.
B, Sm
0.7Ca
0.3BiO
3Buffer coated, dry and decomposition: the colloid that a step is made is coated in LaAlO
3On the monocrystal chip, carry out drying at 120 ℃ again; Be placed in the sintering oven again, in air, make furnace temperature slowly rise to 200 ℃ from room temperature, and rise at 300 ℃ with the speed of 2 ℃/min, the speed with 0.5 ℃/min rises to 560 ℃ again, is incubated 30 minutes.
C, sinter phase into: above-mentioned d is gone on foot prepared substrate put into sintering oven, in air, furnace temperature is risen to 810 ℃ with the speed of 70 ℃/min fast, be incubated 40 minutes; Let furnace temperature slowly reduce to room temperature again, finally obtain Sm
0.7Ca
0.3BiO
3Impact plies.
Fig. 5 is the Sm of the embodiment of the invention two
0.7Ca
0.3BiO
3The X ray diffracting spectrum of impact plies.Can find out by figure except Sm
0.7Ca
0.3BiO
3Impact plies (002) diffraction peak and substrate LaAlO
3Diffraction peak outside, no Sm
0.7Ca
0.3BiO
3Other assorted peaks hint out Sm
0.7Ca
0.3BiO
3There is the outer texture of very strong face in buffer layer thin film.
Fig. 4 is the embodiment of the invention two Sm
0.7Ca
0.3BiO
310000 times of sem (SEM) photo of impact plies.Can be known by Fig. 4: film sample surfacing, densification, no hole is seamless.Hence one can see that, and that this embodiment one prepared texture is good, the Sm that surface compact is smooth
0.7Ca
0.3BiO
3Buffer layer thin film.
Embodiment three
The present invention provides a kind of impact plies Sm of conductor of high-temperature superconductor coat
0.6Ca
0.4BiO
3And a kind of preparation conductor of high-temperature superconductor coat Sm
0.6Ca
0.4BiO
3The method of buffer layer thin film the steps include:
A, Sm
0.6Ca
0.4BiO
3The impact plies colloid for preparing: with precursor Sm, Ca, the nitrate salt of Bi is dissolved in an amount of ROHM (PAA) by cation concn at 0.6: 0.4: 1, thereby obtains organic-compound system.The total volumetric molar concentration of final solution is about 0.2mol/L.
B, Sm
0.6Ca
0.4BiO
3Buffer coated, dry and decomposition: the colloid that a step is made is coated in LaAlO
3On the monocrystal chip, carry out drying at 150 ℃ again; Be placed in the sintering oven again, in air, make furnace temperature slowly rise to 230 ℃ from room temperature, and rise at 290 ℃ with the speed of 1 ℃/min, the speed with 1 ℃/min rises to 580 ℃ again, is incubated 30 minutes.
C, sinter phase into: above-mentioned d is gone on foot prepared substrate put into sintering oven, in air, furnace temperature is risen to 800 ℃ with the speed of 100 ℃/min fast, be incubated 60 minutes; Let furnace temperature slowly reduce to room temperature again, finally obtain Sm
0.6Ca
0.4BiO
3Impact plies.
Fig. 5 is the Sm of the embodiment of the invention three
0.6Ca
0.4BiO
3The X ray diffracting spectrum of impact plies.Can find out by figure except Sm
0.6Ca
0.4BiO
3Impact plies (002) diffraction peak and substrate LaAlO
3Diffraction peak outside, no Sm
0.6Ca
0.4BiO
3Other assorted peaks hint out Sm
0.6Ca
0.4BiO
3There is the outer texture of very strong face in buffer layer thin film.
Fig. 6 is embodiment of the invention Three S's m
0.6Ca
0.4BiO
310000 times of sem (SEM) photo of impact plies.Can be known by Fig. 6: film sample surfacing, densification, no hole is seamless.Hence one can see that, and that this embodiment one prepared texture is good, the Sm that surface compact is smooth
0.6Ca
0.4BiO
3Buffer layer thin film.
A kind of buffer layers of high-temperature superconducting coating conductors Sm of the present invention
1-xCa
xBiO
3And preparation method thereof, employed Sm in its preparation process, Ca, the nitrate salt of Bi are analytical pure.ROHM of the present invention (PAA) organic solvent system is that Acrylic Acid Monomer is added N, and in the dinethylformamide (DMF), polymerization generates ROHM, thereby forms organic solvent system.
Claims (5)
1. conductor of high-temperature superconductor coat Sm
1-xCa
xBiO
3The preparation method of impact plies, wherein Sm
1-xCa
xBiO
3Impact plies is to conductor of high-temperature superconductor coat SmBiO
3Alternative and then the extension that impact plies carries out the Ca of Sm becomes phase thermal treatment to generate oxide S m
1-xCa
xBiO
3Sosoloid, 0.1≤x≤0.4 wherein, its preparation method may further comprise the steps:
A, colloid for preparing: with precursor Sm, Ca, the nitrate salt of Bi are in metal cation ratio Sm: Ca: Bi=1-x: x: 1 ratio is dissolved in an amount of ROHM, 0.1≤x≤0.4 wherein, and the total volumetric molar concentration of final solution is about 0.2mol/L;
B, colloid coating and drying and thermal decomposition process: the colloid that a step is made is coated on the substrate, carries out drying again; After the drying, carry out aerial thermal decomposition process before the sintering, be about to be coated with the colloidal substrate and place sintering oven; Make furnace temperature slowly rise to 180 ℃-230 ℃ from room temperature; And rise at 280 ℃-300 ℃ with the speed of 0.1-2 ℃/min, the speed with 0.1-1 ℃/min rises to 560 ℃-580 ℃ again, is incubated 0.5 hour; So that it is the coating that sintering forms is more smooth, finer and close;
C, sinter phase into: after will being coated with colloidal substrate drying, putting into sintering oven again and sinter phase into, finally obtain Sm
1-xCa
xBiO
3Impact plies; The concrete practice is: in air, furnace temperature is risen to 790 ℃-810 ℃ with the speed of 10-100 ℃/min fast, be incubated 40-60 minute; Let furnace temperature slowly reduce to room temperature again.
2. conductor of high-temperature superconductor coat Sm as claimed in claim 1
1-xCa
xBiO
3The preparation method of impact plies is characterized in that: said b is in the step, and colloid is coated in the on-chip concrete practice and is: on substrate, with the sol evenning machine rotation, colloid evenly is coated on the substrate colloid drops.
3. conductor of high-temperature superconductor coat Sm as claimed in claim 1
1-xCa
xBiO
3The preparation method of impact plies is characterized in that: said b in the step temperature when dry be 100 ℃ of-150 ℃ of dryings.
4. conductor of high-temperature superconductor coat Sm as claimed in claim 1
1-xCa
xBiO
3The preparation method of impact plies is characterized in that: the dry back in above-mentioned b step, c step sinter the phase front into, also carry out aerial thermal decomposition process before the sintering; Be about to be coated with the colloidal substrate and place sintering oven; Make furnace temperature slowly rise to 180 ℃-230 ℃ from room temperature, and rise at 280 ℃-300 ℃ with the speed of 0.1-2 ℃/min, the speed with 0.1-1 ℃/min rises to 560 ℃-580 ℃ again; Be incubated 0.5 hour; Handle through the predecomposition before such sintering, the coating that can make sintering form is more smooth, and is finer and close.
5. conductor of high-temperature superconductor coat Sm
1-xCa
xBiO
3Impact plies is characterized in that, adopts the conductor of high-temperature superconductor coat Sm of above claim or 1 or 2 or 3
1-xCa
xBiO
3Buffer layer method makes, for to conductor of high-temperature superconductor coat SmBiO
3Alternative and then the extension that impact plies carries out the Ca of Sm becomes phase thermal treatment to generate oxide S m
1-xCa
xBiO
3Sosoloid, wherein 0.1≤x≤0.4.
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CN103515026A (en) * | 2013-10-17 | 2014-01-15 | 西南交通大学 | Preparation method of high temperature superconducting coated conductor La0.7Sr0.3MnO3 buffer layer thin film |
CN104129985A (en) * | 2014-07-08 | 2014-11-05 | 西南交通大学 | High-temperature super-conducting coating conductor Eu0.6Sr0.4BiO3 buffer layer with nanoparticle precipitated phases on surface and preparation method thereof |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN103515026A (en) * | 2013-10-17 | 2014-01-15 | 西南交通大学 | Preparation method of high temperature superconducting coated conductor La0.7Sr0.3MnO3 buffer layer thin film |
CN104129985A (en) * | 2014-07-08 | 2014-11-05 | 西南交通大学 | High-temperature super-conducting coating conductor Eu0.6Sr0.4BiO3 buffer layer with nanoparticle precipitated phases on surface and preparation method thereof |
CN104129985B (en) * | 2014-07-08 | 2016-04-06 | 西南交通大学 | Surface conductor of high-temperature superconductor coat Eu0.6Sr0.4BiO3 buffer layer with nano particle precipitated phase and preparation method thereof |
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