CN109082708B - Method for preparing c-axis YBCO high-temperature superconducting thick film with two a-axis grains - Google Patents
Method for preparing c-axis YBCO high-temperature superconducting thick film with two a-axis grains Download PDFInfo
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- CN109082708B CN109082708B CN201810824851.6A CN201810824851A CN109082708B CN 109082708 B CN109082708 B CN 109082708B CN 201810824851 A CN201810824851 A CN 201810824851A CN 109082708 B CN109082708 B CN 109082708B
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/16—Oxides
- C30B29/22—Complex oxides
- C30B29/225—Complex oxides based on rare earth copper oxides, e.g. high T-superconductors
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B19/00—Liquid-phase epitaxial-layer growth
Abstract
The invention discloses a method for preparing a c-axis YBCO high-temperature superconducting thick film with two a-axis grains, which comprises the following steps: 1) mixing BaCO3Mixing the powder and CuO powder and sintering to prepare Ba-Cu-O powder; 2) adding Ba-Cu-O powder to Y2O3Heating the crucible to high temperature, adding Ba-Cu-O powder with fixed weight into the crucible after the powder is fully melted, and carrying out long-term heat preservation to obtain a Y-Ba-Cu-O solution with constant initial state; 3) adding Ba-Cu-O powder with fixed weight into the high-temperature solution, and changing the melting time delta t of the Ba-Cu-O powdermTo adjust the intermediate state U of undersaturationintTo make the state of the solution reach Uint2(ii) a 4) Cooling the solution to a second temperature; 5) inserting the seed crystal material fixed on the connecting rod into the step 4) to grow for 5-15 s. According to the invention, the supersaturation degree of the solution is finely adjusted, so that the Y-Ba-Cu-O solution accurately reaches the specified supersaturation state in the metastable zone, and the c-axis YBCO high-temperature superconducting thick film with two a-axis grains is grown, and the method has the advantages of simple process and convenience in operation.
Description
Technical Field
The invention relates to a preparation method of a high-temperature superconducting material, in particular to a method for preparing a c-axis YBCO high-temperature superconducting thick film, and more particularly relates to a method for preparing a c-axis YBCO high-temperature superconducting thick film with two a-axis crystal grains.
Background
Since the discovery of high temperature superconductors, a large number of crystal workers have been invested in the fundamental research and manufacturing fields of high quality films. Due to YBa2Cu3OxThe (YBCO, Y123 and yttrium barium copper oxide for short) has a superconducting transition temperature Tc higher than the temperature of liquid nitrogen, and shows the characteristics of a Meissner effect, a zero resistance effect and the like in a temperature environment lower than the Tc. Due to these important properties of YBCO high temperature superconducting materials, thick YBCO superconducting films have many potential applications in superconducting devices such as current limiters, filters, etc.
The application of the material depends on the performance of the material, and the structure of the material determines the performance of the material, thereby influencing the application of the material in practice. Generally, since the lattice constants of the YBCO superconducting crystals are approximately equal in both directions, the a-axis and the b-axis, the YBCO superconducting thick film has two orientations, i.e., the a-axis orientation and the c-axis orientation. The c-axis oriented REBCO high-temperature superconducting thick film has higher critical current density, so that the film has important application in the aspect of power transportation, and the a-axis oriented REBCO high-temperature superconducting thick film has important application in the aspect of Josephson junction devices.
Liquid Phase Epitaxy (LPE) is widely considered as a preparation method of a very potential YBCO superconducting thick film. In the process of growing the YBCO superconducting thick film by liquid phase epitaxy, seed crystals are fixed on a connecting rod and slowly approach the surface of a saturated solution to be used as unique nucleation points to induce the growth of the YBCO superconducting thick film. Because the growth condition of LPE is close to the equilibrium state, the thick film obtained by using the thin film material as seed crystal for induction growth has the characteristics of low defect, high flatness, high crystallization performance and the like. In addition, because the LPE is carried out under the non-vacuum condition, the method has the advantages of low preparation cost and the like. And compared with the common film forming technology, the LPE has a faster growth speed.
Therefore, the method can prepare the specific C-axis oriented YBCO high-temperature superconducting thick film by using LPE, and has important significance for developing Josephson junction devices and basic research of superconducting mechanisms.
Disclosure of Invention
In view of the above-mentioned defects of the prior art, the technical problem to be solved by the present invention is to provide a convenient and efficient method for growing a c-axis YBCO high-temperature superconducting thick film inlaid with two a-axis grains on an NGO substrate, which overcomes the problems that the initial state of the solution cannot be fixed, and the supersaturation state of the solution cannot be adjusted to σint2And the like.
The conception of the invention is as follows: when in NdGaO3When YBCO crystal is epitaxially grown on (NGO, neodymium gallate) substrate in liquid phase, a-axis crystal grains a with two different nucleation directions can be obtained on the c-axis film according to the different supersaturation states of the solution1And a2. Normally, only a in the grown c-axis film1YBCO film with crystal grains and a in grown c-axis film1And a2Two solution supersaturation conditions (sigma) required for YBCO films of crystalline grainsint1And σint2) Between a very large and a very small degree of supersaturation. In the past, when the NGO single crystal substrate is used for preparing the liquid phase epitaxial YBCO film, the supersaturation state of the solution is generally adjusted by controlling the weight of the added fresh Ba-Cu-O powder and the length of the heat preservation time, but the method ignores the solutionThe initial state of the liquid is usually difficult to adjust the supersaturation degree of the solution to an intermediate state, and can only be adjusted to two extreme supersaturation degree states of extremely large and extremely small. The invention is characterized in that: firstly, obtaining a relatively constant solution initial state U through long-time heat preservation at high temperature0(ii) a Then, a fixed weight of Ba-Cu-O powder was added and the melting time Deltat was adjusted by changingmTo adjust the intermediate state U of undersaturationint. Unlike previously reported techniques, under which U is presentintCan be easily subdivided into Uint1And Uint2. Finally, corresponding intermediate supersaturation degree state sigma is obtained at the growth temperatureint1And σint2. At σint2Under the condition, a c-axis YBCO high-temperature superconducting thick film with two a-axis crystal grains can be reliably prepared on the substrate material.
In order to achieve the purpose, the invention provides a method for preparing a c-axis YBCO high-temperature superconducting thick film with two a-axis crystal grains, which comprises the following steps:
a) preparing precursor powder of a Ba-Cu-O phase;
b) y adding precursor powder of Ba-Cu-O into crystal growth furnace2O3In a crucible of material;
c) mixing the precursor powder of Ba-Cu-O in the step b) with Y2O3Heating a crucible of the material to a first temperature for heat preservation to obtain a Y-Ba-Cu-O solution;
d) growing a YBCO superconducting thick film in a crystal growth furnace by liquid phase epitaxy through a seed crystal pulling method at the top; wherein the liquid phase epitaxial growth in the step d) comprises the following steps:
e) adding precursor powder of Ba-Cu-O into the Y-Ba-Cu-O solution in the step c), and carrying out heat preservation for a long time at a first temperature;
f) reducing the Y-Ba-Cu-O solution in the step e) to a second temperature at a first cooling speed;
g) adding precursor powder of Ba-Cu-O into the Y-Ba-Cu-O solution in the step f), and heating to a first temperature at a first heating speed for heat preservation;
h) reducing the Y-Ba-Cu-O solution in the step g) to a second temperature at a first cooling speed;
i) inserting seed crystal materials fixed on the connecting rod into the Y-Ba-Cu-O solution obtained in the step h), and taking out after epitaxial growth for a period of time to obtain the c-axis YBCO high-temperature superconducting thick film with two a-axis grains.
Further, the step a) includes:
BaCO is added according to the proportion of 0.3-0.8 of Ba to Cu3Mixing with CuO powder, placing into a ball milling tank, adding anhydrous ethanol or water, and wet milling to obtain BaCO3Wet grinding the mixed slurry with CuO for 2-4 hours;
mixing BaCO3Heating and drying the mixed slurry with CuO at the temperature of between 90 and 120 ℃ to obtain BaCO3And CuO;
mixing BaCO3And sintering the mixed powder of CuO and 890-910 ℃ in air for 40-50 hours to obtain precursor powder of Ba-Cu-O phase.
Further, the first temperature in the step c) is 5-35 ℃ above the peritectic temperature of YBCO, and the heat preservation time is 20-24 hours.
Further, the addition amount of the Ba-Cu-O precursor powder in the step e) is 15-20 g, and the heat preservation time is 11-13 hours. In the process of the invention, the inventors find that the shorter holding time in the step e) is not favorable for obtaining the Y-Ba-Cu-O solution with constant initial state. In fact, when a short holding time is adopted, the Y-Ba-Cu-O solution with unfixed initial state is easy to obtain, so that only an extremely large or extremely small supersaturation state can be obtained when the solution state is adjusted in the next step, and an intermediate supersaturation state is difficult to obtain. Based on the above, the inventor innovatively provides an optimized process that the addition amount of the Ba-Cu-O precursor powder is 15-20 g and the heat preservation time is 11-13 hours through repeated tests.
Further, the first cooling speed in the step f) is 1.5-3 ℃/min, and the second temperature is 3-30 ℃ below the peritectic temperature of YBCO.
Further, the addition amount of the Ba-Cu-O precursor powder in the step g) is 15-20 g, and the heat preservation time is 2-4 hours. The inventors have found that in step g), two different incubation times are obtainedIntermediate supersaturation degree state σ ofint1And σint2. Wherein, when the holding time is shorter, a lower intermediate supersaturation degree state sigma is obtainedint1When the holding time is longer, a higher intermediate supersaturation degree state sigma is obtainedint2. In the state of intermediate supersaturation degree sigmaint1Under the condition of (2), the c-axis YBCO high-temperature superconducting thick film with a kind of a-axis crystal grains is easy to obtain. Only in the intermediate supersaturation state σint2Under the condition of (1), the c-axis YBCO high-temperature superconducting thick film with two a-axis crystal grains can be obtained. In the invention process, the inventor creatively summarizes that the solution can obtain sigma by finely adjusting the supersaturation degree of the solution when the addition amount of the Ba-Cu-O precursor powder is 15-20 g and the heat preservation time is 2-4 hoursint2The intermediate supersaturation state is beneficial to the preparation and growth of the c-axis YBCO high-temperature superconducting thick film with two a-axis crystal grains.
Further, the first temperature rise speed in the step g) is 1.5-3 ℃/min.
Further, the seed material in step i) is NdGaO3A single crystal substrate having dimensions of 10mm by 3 mm.
Further, the rotation speed of the epitaxial growth in the step i) is 10-20 rpm, and the growth time is 5-15 s.
In summary, the present invention discloses a method for preparing a c-axis YBCO high temperature superconducting thick film having two a-axis grains, comprising the steps of: 1) mixing BaCO3Mixing the powder and CuO powder and sintering to prepare Ba-Cu-O powder; 2) adding Ba-Cu-O powder to Y2O3Heating the crucible to high temperature, and carrying out long-term heat preservation to obtain a Y-Ba-Cu-O solution with a constant initial state; 3) adding a fixed weight of Ba-Cu-O powder into the high-temperature solution, and changing the melting time delta t of the Ba-Cu-O powdermTo adjust the intermediate state U of undersaturationintTo make the state of the solution reach Uint2(ii) a 4) Cooling the solution to a second temperature; 5) inserting the seed crystal material fixed on the connecting rod into the step 4) to grow for 5-15 s. The invention creatively introduces a long-term heat preservation program at the initial stage of the solution, solves the problem that the initial state of the solution is not fixed, and is a fine solution at the later stageThe fine adjustment of the solution state lays a foundation, so that the solution finally and accurately reaches a specified state, and a c-axis YBCO high-temperature superconducting thick film with two a-axis grains is grown.
The technical effects are as follows:
1. Ba-Cu-O powder is added for the first time at the high-temperature stage of the liquid phase epitaxy method, and heat preservation is carried out for 11-13 hours, so that a solution with a constant initial state is obtained. Adding Ba-Cu-O powder again at the high-temperature stage of the liquid phase epitaxy method, preserving heat for 2-4 hours, finely adjusting the supersaturation degree of the solution by controlling the weight of the added Ba-Cu-O powder and the length of the heat preservation time, enabling the Y-Ba-Cu-O solution to accurately reach the specified supersaturation degree state in the metastable zone, and growing to obtain the c-axis YBCO high-temperature superconducting thick film with two a-axis grains.
2. The invention can artificially regulate and control the growth time of liquid phase epitaxy, thereby controlling the thickness of the YBCO epitaxial film with the required mixed crystal boundary structure.
3. The liquid phase epitaxy method of the invention grows the YBCO superconducting thick film with specific mixed orientation, so that a-axis YBCO crystal grains with two different orientations are widely distributed in the YBCO thick film with c-axis orientation, and the method is used for obtaining the crystal boundary of the two a-axis YBCO films connected with the a-axis YBCO crystal grains, and has important significance for developing Josephson junction devices and basic research of superconducting mechanism.
Detailed Description
The method adopts an NGO single crystal substrate as seed crystal, grows the c-axis YBCO high-temperature superconducting thick film with two a-axis crystal grains through liquid phase epitaxy, and grows the c-axis YBCO high-temperature superconducting thick film with two a-axis crystal grains through liquid phase epitaxy by fixing the initial state of the solution and controlling the supersaturation degree of the solution.
Example one
The embodiment provides a method for preparing a c-axis YBCO high-temperature superconducting thick film with two a-axis grains, which comprises the following steps:
1. according to the weight ratio of Ba: ratio of Cu to 0.6 BaCO3Mixing the powder and CuO powder, placing into a ball milling tank, adding anhydrous ethanol or water, and wet milling to obtain BaCO3And CuO for a wet milling time of 3 hours.
2. The BaCO obtained in the step 13Heating and drying the mixed slurry with CuO at the temperature of 105 ℃ to obtain BaCO3And CuO.
3. The BaCO obtained in the step 23And sintering the mixed powder of CuO and Ba-Cu-O phase for 48 hours at 900 ℃ in the air to obtain the precursor powder of the Ba-Cu-O phase.
4. Y adding precursor powder of Ba-Cu-O into crystal growth furnace2O3In the crucible of the material, precursor powder of Ba-Cu-O is added until the precursor powder is level with the upper edge of the crucible.
5. The precursor powder of Ba-Cu-O in the step 4 and Y2O3Heating the crucible of the material to 1030 ℃ (namely 25 ℃ above the peritectic temperature of YBCO) and preserving heat for 24 hours to obtain Y-Ba-Cu-O solution;
6. 20g of precursor powder of Ba-Cu-O was added to the Y-Ba-Cu-O solution obtained in step 5, and the incubation was continued at 1030 ℃ for 12 hours.
7. The Y-Ba-Cu-O solution obtained in step 6 was cooled to 985 c (i.e. 20 c below the peritectic temperature of YBCO) at a cooling rate of 2.25 c/min.
8. 15g of Ba-Cu-O precursor powder is added into the Y-Ba-Cu-O solution obtained in the step 7, and then the temperature is raised to 1030 ℃ at the heating rate of 2.25 ℃/min and is kept for 3 hours.
9. The Y-Ba-Cu-O solution obtained through step 8 was cooled to 985 ℃ at a cooling rate of 2.25 ℃/min.
10. Adopting an NGO single crystal substrate with the size of 3mm multiplied by 10mm as a seed crystal and fixing the substrate on a connecting rod, inserting the surface of the NGO substrate into Y-Ba-Cu-O solution, and adopting a top seed crystal pulling method to grow a YBCO superconducting thick film in a liquid phase epitaxy manner. The specific process parameters in the growth process are as follows: the seed crystal was rotated at 16rpm for a growth time of 10 s.
Example two
The embodiment provides a method for preparing a c-axis YBCO high-temperature superconducting thick film with two a-axis grains, which comprises the following steps:
1. according to the weight ratio of Ba: ratio of Cu to 0.6 BaCO3Mixing the powder and CuO powder, placing into a ball milling tank, adding anhydrous ethanol or water, and wet millingTo obtain BaCO3And CuO for a wet milling time of 4 hours.
2. The BaCO obtained in the step 13Heating and drying the mixed slurry with CuO at the temperature of 120 ℃ to obtain BaCO3And CuO.
3. The BaCO obtained in the step 23And sintering the mixed powder of CuO and Ba-Cu-O phase for 50 hours at 910 ℃ in the air to obtain precursor powder of the Ba-Cu-O phase.
4. Y adding precursor powder of Ba-Cu-O into crystal growth furnace2O3In the crucible of the material, precursor powder of Ba-Cu-O is added until the precursor powder is level with the upper edge of the crucible.
5. The precursor powder of Ba-Cu-O in the step 4 and Y2O3Heating a crucible of the material to 1020 ℃ (namely 15 ℃ above the peritectic temperature of YBCO), and preserving heat for 24 hours to obtain a Y-Ba-Cu-O solution;
6. 15g of precursor powder of Ba-Cu-O was added to the Y-Ba-Cu-O solution obtained in step 5, and the temperature was kept at 1030 ℃ for 10 hours.
7. The Y-Ba-Cu-O solution obtained in step 6 was cooled to 985 c (i.e. 20 c below the peritectic temperature of YBCO) at a cooling rate of 1.75 c/min.
8. 16g of Ba-Cu-O precursor powder is added into the Y-Ba-Cu-O solution obtained in the step 7, and then the temperature is raised to 1020 ℃ at the heating rate of 1.75 ℃/min and is kept for 3 hours.
9. The Y-Ba-Cu-O solution obtained through step 8 was cooled to 985 ℃ at a cooling rate of 1.75 ℃/min.
10. Adopting an NGO single crystal substrate with the size of 3mm multiplied by 10mm as a seed crystal and fixing the substrate on a connecting rod, inserting the surface of the NGO substrate into Y-Ba-Cu-O solution, and adopting a top seed crystal pulling method to grow a YBCO superconducting thick film in a liquid phase epitaxy manner. The specific process parameters in the growth process are as follows: the rotation speed of the seed crystal was 20rpm, and the growth time was 8 s.
The foregoing detailed description of the preferred embodiments of the invention has been presented. It should be understood that numerous modifications and variations could be devised by those skilled in the art in light of the present teachings without departing from the inventive concepts. Therefore, the technical solutions available to those skilled in the art through logic analysis, reasoning and limited experiments based on the prior art according to the concept of the present invention should be within the scope of protection defined by the claims.
Claims (4)
1. A method for preparing a c-axis YBCO high-temperature superconducting thick film with two a-axis grains comprises the following steps:
a) preparing precursor powder of a Ba-Cu-O phase;
b) y adding precursor powder of Ba-Cu-O into crystal growth furnace2O3In a crucible;
c) mixing the precursor powder of Ba-Cu-O in the step b) with Y2O3Heating a crucible of the material to a first temperature for heat preservation to obtain a Y-Ba-Cu-O solution; wherein the first temperature is 5-35 ℃ above the peritectic reaction temperature of YBCO, and the heat preservation time is 20-24 hours;
d) growing a YBCO superconducting thick film in a crystal growth furnace by liquid phase epitaxy through a seed crystal pulling method at the top;
characterized in that the liquid phase epitaxial growth in the step d) comprises the following steps:
e) adding precursor powder of Ba-Cu-O into the Y-Ba-Cu-O solution in the step c), and carrying out heat preservation for a long time at a first temperature to obtain a solution with a constant initial state; the addition amount of the Ba-Cu-O precursor powder is 15-20 g, and the heat preservation time is 11-13 hours;
f) reducing the Y-Ba-Cu-O solution obtained in the step e) to a second temperature at a first cooling speed; wherein the first cooling speed is 1.5-3 ℃/min, and the second temperature is 3-30 ℃ below the peritectic temperature of YBCO;
g) adding precursor powder of Ba-Cu-O into the Y-Ba-Cu-O solution obtained in the step f), and heating to a first temperature at a first heating speed for heat preservation; wherein the addition amount of the Ba-Cu-O precursor powder is 15-20 g, the first heating speed is 1.5-3 ℃/min, and the heat preservation time is 2-4 hours;
h) reducing the Y-Ba-Cu-O solution obtained in the step g) to a second temperature at a first cooling rate;
i) inserting seed crystal materials fixed on the connecting rod into the Y-Ba-Cu-O solution obtained in the step h), and taking out after epitaxial growth for a period of time to obtain the c-axis YBCO high-temperature superconducting thick film with two a-axis grains.
2. The method as set forth in claim 1, wherein the process a) includes:
BaCO is added according to the proportion of Ba to Cu = 0.3-0.83Mixing with CuO powder, placing into a ball milling tank, adding anhydrous ethanol or water, and wet milling to obtain BaCO3Wet grinding the mixed slurry with CuO for 2-4 hours;
mixing the BaCO3Heating and drying the mixed slurry with CuO at the temperature of 90-120 ℃ to obtain BaCO3And CuO;
mixing the BaCO3And sintering the mixed powder of CuO and the Ba-Cu-O phase for 40-50 hours at 890-910 ℃ in the air to obtain the precursor powder of the Ba-Cu-O phase.
3. The method of claim 1, wherein the seed material in step i) is NdGaO3A single crystal substrate having dimensions of 10mm by 3 mm.
4. The method of claim 1, wherein the rotation speed of the epitaxial growth in step i) is 10-20 rpm, and the growth time is 5-15 s.
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| US5968877A (en) * | 1995-04-10 | 1999-10-19 | Lockheed Martin Energy Research Corp | High Tc YBCO superconductor deposited on biaxially textured Ni substrate |
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| CN103276447B (en) * | 2013-06-18 | 2016-06-01 | 上海交通大学 | A kind of method preparing specific blend orientation YBCO high temperature superconductive thick film |
| CN103526283B (en) * | 2013-10-31 | 2016-07-06 | 上海交通大学 | A kind of method of the YBCO liquid phase epitaxy film preparing pure a axle orientation |
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