CN102242357A - Method for preparing YBCO (Yttrium Barium Copper Oxide) coating conductor barrier layer - Google Patents
Method for preparing YBCO (Yttrium Barium Copper Oxide) coating conductor barrier layer Download PDFInfo
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- CN102242357A CN102242357A CN2011101718523A CN201110171852A CN102242357A CN 102242357 A CN102242357 A CN 102242357A CN 2011101718523 A CN2011101718523 A CN 2011101718523A CN 201110171852 A CN201110171852 A CN 201110171852A CN 102242357 A CN102242357 A CN 102242357A
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Abstract
The invention discloses a method for preparing an YBCO (Yttrium Barium Copper Oxide) coating conductor barrier layer. The method comprises the following steps of: firstly preparing a precursor liquid, mixing aluminium isopropoxide with deionized water according to a mole ratio of Al:H2O=1:50-1:100, stirring the precursor liquid by using a magnetic stirring apparatus at 80-90 DEG C, dropwise adding hydrochloric acid to the uniformly stirred precursor liquid and regulating a pH value to be 2-4; stirring the precursor liquid by using the magnetic stirring apparatus at 80-90 DEG C again to obtain transparent Al2O3 gel; coating the Al2O3 gel on a substrate; and placing the substrate coated with the Al2O3 gel in a high-temperature tubular quartz furnace, and carrying out a low-temperature thermal treatment at 300-500 DEG C under an inert atmosphere for 5-10h to obtain an amorphous alumina film. The amorphous alumina film prepared by the method disclosed by the invention is smooth and compact.
Description
Technical field
The present invention relates to the preparation method on blocking layer in a kind of s-generation belt material of high temperature superconduct, particularly on the nickelalloy matrix, prepare the method for amorphous nickel/phosphorus/aluminium oxide film.
Background technology
S-generation belt material of high temperature superconduct is meant the rare earth class barium-copper oxide superconducting coating conductor based on the YBCO-123 series superconducting material.It is made of metal alloy base band, Seed Layer, blocking layer, cap layer, rare earth barium copper oxide superconducting layer, protective layer and stabilizing layer etc., is a kind of multilayered structure.Compare with first-generation Bi based high-temperature superconductive strip, s-generation belt material of high temperature superconduct has the ability of the high electric current of load under the upfield, 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.The Superpower company of the U.S. adopts ion beam assisted depositing (IBAD)+metal organic chemical vapor deposition (MOCVD) method can prepare km level s-generation belt material of high temperature superconduct by mass, the longest single superconducting tape arrives 1311m, the about 300A of critical current is the best result of reporting in the world at present.
The IBAD method is propositions such as Iijmia, and forces sedimentary sull oriented growth to obtain the scheme of biaxial texture sull by the ion beam bombardment that adopts on the base band of non-texture that U.S. Los Alamos National Laboratories etc. further develop.In the IBAD method, the polycrystalline metal base band surface r.m.s. roughness (RMS) of not having orientation is reduced to adopts sputtering method deposited amorphous barrier oxide layers below the 2nm again, on the amorphous blocking layer, deposit transition layer then.Adopt sputtering method deposited amorphous barrier oxide layers to need expensive vacuum system, sedimentation rate is lower, and technology more complicated, cost are very high.S-generation belt material of high temperature superconduct fancy price is the main bottleneck that restricts its large-scale application at present.At present domestic patent about blocking layer in the coating conductor all is to prepare having on the Ni-W alloy base band of biaxial texture.And the blocking layer of preparation YBCO coating conductor yet there are no report on the polycrystalline metal base band that does not have orientation.
Summary of the invention
The objective of the invention is to overcome the high shortcoming of YBCO coating conductor blocking layer cost of prior art for preparing, provide a kind of chemical solution cheaply to prepare the method on amorphous nickel/phosphorus/aluminium oxide blocking layer.
The present invention adopts chemical solution method to prepare the amorphous nickel/phosphorus/aluminium oxide film, and the concrete steps order is as follows:
(1) according to Al: H
2O=1: 50-1: 100 molar ratio mixes aluminum isopropylate and deionized water;
(2) with the solution of above-mentioned steps (1) preparation under 80-90 ℃ of condition through magnetic stirrer 1-3h;
(3) add hydrochloric acid in the solution that above-mentioned steps (2) makes, the pH value of regulating described solution is to 2-4;
(4) solution that above-mentioned steps (3) is prepared through magnetic stirrer 4-8h, obtains transparent Al under 80-90 ℃
2O
3Gel.
(5) the described Al that step (4) is made
2O
3The gel precursor liquid is coated on the substrate.Coating method can be spin coating (spin-coating) or lift (dipping) method that the coating time is 0.5-1.5min.Described substrate can be nickel-base alloy or stainless steel;
(6) substrate that step (5) has been applied film places the quartzy stove of high-temperature tubular, carries out the low-temperature heat treatment of 5～15h under 300 ℃ of-500 ℃ of temperature, can obtain the amorphous nickel/phosphorus/aluminium oxide film; The temperature rise rate of this step is 5 ℃/h; This step is carried out in inert atmospheres such as argon gas or nitrogen.
Compared with prior art, the present invention has following beneficial effect:
The present invention adopts chemical solution method to prepare the amorphous nickel/phosphorus/aluminium oxide film, needs expensive vacuum system to compare with present employing sputtering method deposited amorphous barrier oxide layers, and the present invention does not need vacuum system, and cost is lower.And it also has the sedimentation rate height, and composition is controlled easily, prepares advantages such as high-quality film in surfaces of complex shape.Adopt the amorphous nickel/phosphorus/aluminium oxide film of this method preparation smooth, fine and close, surfaceness is less than 5nm.
Description of drawings
Fig. 1 is the scanning electron microscope diagram sheet of the amorphous nickel/phosphorus/aluminium oxide film of embodiment 1 preparation;
Fig. 2 is the scanning electron microscope diagram sheet of the amorphous nickel/phosphorus/aluminium oxide film of embodiment 2 preparations;
Fig. 3 is the scanning electron microscope diagram sheet of the amorphous nickel/phosphorus/aluminium oxide film of embodiment 3 preparations;
Fig. 4 is the scanning electron microscope diagram sheet of the amorphous nickel/phosphorus/aluminium oxide film of embodiment 4 preparations.
Embodiment
Embodiment 1
(1) takes by weighing aluminum isopropylate 0.1mol, aluminum isopropylate is dissolved in wiring solution-forming in the deionized water of 135mL.
(2) solution that step (1) is made under 80 ℃ of conditions through magnetic stirrer 1h;
(3) in the solution that above-mentioned steps (2) makes, add hydrochloric acid, regulate the pH value to 2 of described solution;
(4) solution that above-mentioned steps (3) is prepared through magnetic stirrer 4h, obtains transparent Al under 80 ℃
2O
3Gel.
(5) the described Al that step (4) is made
2O
3Gel is spin-coated on the nickel-base alloy substrate with 5000 rev/mins speed, and the spin coating time is 0.5min;
(6) will place the quartzy stove of high-temperature tubular through the substrate that step (5) applied film, the 500sccm argon gas will be fed reaction chamber, be warming up to 300 ℃ with the temperature rise rate of 5 ℃/h from room temperature, and insulation 5h, sample cools to room temperature with the furnace then.With field emission scanning electron microscope sample has been carried out the surface topography observation, the amorphous nickel/phosphorus/aluminium oxide thick film surface is smooth, fine and close, as shown in Figure 1.
Embodiment 2
(1) takes by weighing aluminum isopropylate 0.1mol, aluminum isopropylate is dissolved in wiring solution-forming in the deionized water of 200mL.
(2) solution that step (1) is made under 85 ℃ of conditions through magnetic stirrer 2h;
(3) in the solution that above-mentioned steps (2) makes, add hydrochloric acid, regulate the pH value to 3 of described solution;
(4) solution that above-mentioned steps (3) is prepared through magnetic stirrer 6h, obtains transparent Al under 85 ℃
2O
3Gel.
(5) the described Al that step (4) is made
2O
3Gel is spin-coated on the nickel-base alloy substrate with 5000 rev/mins speed, and the spin coating time is 1min;
(6) will place the quartzy stove of high-temperature tubular through the substrate that step (5) applied film, the 500sccm argon gas will be fed reaction chamber, be warming up to 400 ℃ with the temperature rise rate of 5 ℃/h from room temperature, and insulation 10h, sample cools to room temperature with the furnace then.With field emission scanning electron microscope sample has been carried out the surface topography observation, the amorphous nickel/phosphorus/aluminium oxide thick film surface is smooth, fine and close, as shown in Figure 2.
Embodiment 3
(1) takes by weighing aluminum isopropylate 0.1mol, aluminum isopropylate is dissolved in wiring solution-forming in the deionized water of 270mL;
(2) solution that step (1) is made under 90 ℃ of conditions through magnetic stirrer 3h;
(3) in the solution that above-mentioned steps (2) makes, add hydrochloric acid, regulate the pH value to 4 of described solution;
(4) solution that above-mentioned steps (3) is prepared through magnetic stirrer 8h, obtains transparent Al under 90 ℃
2O
3Gel.
(5) the described Al that step (4) is made
2O
3Gel is spin-coated on the nickel-base alloy substrate with 5000 rev/mins speed, and the spin coating time is 1.5min;
(6) will place the quartzy stove of high-temperature tubular through the substrate that step (5) applied film, the 500sccm argon gas is fed reaction chamber, and be warming up to 500 ℃ and be incubated 10h from room temperature with the temperature rise rate of 5 ℃/h, sample is chilled to room temperature with stove then.With field emission scanning electron microscope sample has been carried out the surface topography observation, the amorphous nickel/phosphorus/aluminium oxide thick film surface is smooth, fine and close, as shown in Figure 3.
Embodiment 4
(1) takes by weighing aluminum isopropylate 0.1mol, aluminum isopropylate is dissolved in wiring solution-forming in the deionized water of 200mL.
(2) solution that step (1) is made under 85 ℃ of conditions through magnetic stirrer 2h;
(3) in the solution that above-mentioned steps (2) makes, add hydrochloric acid, regulate the pH value to 3 of described solution;
(4) solution that above-mentioned steps (3) is prepared through magnetic stirrer 6h, obtains transparent Al under 85 ℃
2O
3Gel.
(5) the described Al that step (4) is made
2O
3Gel is coated on the nickel-base alloy substrate with the pull rate of 5 cels, and the spin coating time is 1min;
(6) will place the quartzy stove of high-temperature tubular through the substrate that step (5) applied film, the 500sccm argon gas will be fed reaction chamber, be warming up to 400 ℃ with the temperature rise rate of 5 ℃/h from room temperature, and insulation 10h, sample cools to room temperature with the furnace then.With field emission scanning electron microscope sample has been carried out the surface topography observation, the amorphous nickel/phosphorus/aluminium oxide thick film surface is smooth, fine and close, as shown in Figure 4.
Embodiment 5
(1) takes by weighing aluminum isopropylate 0.1mol, aluminum isopropylate is dissolved in wiring solution-forming in the deionized water of 200mL.
(2) solution that step (1) is made under 85 ℃ of conditions through magnetic stirrer 2h;
(3) in the solution that above-mentioned steps (2) makes, add hydrochloric acid, regulate the pH value to 3 of described solution;
(4) solution that above-mentioned steps (3) is prepared through magnetic stirrer 6h, obtains transparent Al under 85 ℃
2O
3Gel.
(5) the described Al that step (4) is made
2O
3Gel is spin-coated on the stainless steel substrate with 5000 rev/mins speed, and the spin coating time is 1min;
(6) will place the quartzy stove of high-temperature tubular through the substrate that step (5) applied film, the 500sccm argon gas will be fed reaction chamber, be warming up to 400 ℃ with the temperature rise rate of 5 ℃/h from room temperature, and insulation 10h, sample cools to room temperature with the furnace then.
Claims (2)
1. the preparation method on a YBCO coating conductor blocking layer is characterized in that, comprises the steps:
(1) according to Al: H
2O=1: 50-1: 100 molar ratio mixes aluminum isopropylate and deionized water;
(2) with the solution of above-mentioned steps (1) preparation under 80-90 ℃ of condition through magnetic stirrer 1-3h;
(3) add hydrochloric acid in the solution that above-mentioned steps (2) makes, the pH value of regulating described solution is to 2-4;
(4) solution that above-mentioned steps (3) is prepared through magnetic stirrer 4-8h, obtains transparent Al under 80-90 ℃
2O
3Gel;
(5) the described Al that step (4) is made
2O
3Gel adopts spin coating or method of pulling up to be coated on the substrate;
(6) substrate that step (5) was applied film places the quartzy stove of high-temperature tubular, carries out the low-temperature heat treatment of 5-10h under 300 ℃ of-500 ℃ of temperature, can obtain the amorphous nickel/phosphorus/aluminium oxide film; The temperature rise rate of this step is 5 ℃/h; This step is to carry out in inert atmospheres such as argon gas or nitrogen.
2. the preparation method on a kind of YBCO coating conductor as claimed in claim 1 blocking layer is characterized in that substrate is nickel-base alloy or stainless steel described in the described step (5).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443792A (en) * | 2011-12-02 | 2012-05-09 | 西安理工大学 | Low-fluorine solution deposition and heat treatment process of YBCO (Yttrium Barium Copper Oxide) superconducting thin film |
| CN102618871A (en) * | 2012-02-14 | 2012-08-01 | 中国科学院电工研究所 | Method for preparing tritium resistance Er2O3 coating by using chemical solution method |
| CN103993277A (en) * | 2014-05-22 | 2014-08-20 | 赵遵成 | Preparation method of template suitable for growing REBCO superconducting layer on metal baseband |
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| TW200728203A (en) * | 2006-01-20 | 2007-08-01 | Taiwan Tft Lcd Ass | Manufacturing method of alumina insulated layer |
| CN101456567A (en) * | 2008-12-25 | 2009-06-17 | 中国计量学院 | Method for synthesizing high temperature stabilizing type alpha-Al2O3 nano powder |
| CN101567242A (en) * | 2009-02-10 | 2009-10-28 | 武汉理工大学 | Method for preparing magnetic nano composite particles of FeCr alloy dispersed in ceramic crystal grain |
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2011
- 2011-06-24 CN CN2011101718523A patent/CN102242357A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW200728203A (en) * | 2006-01-20 | 2007-08-01 | Taiwan Tft Lcd Ass | Manufacturing method of alumina insulated layer |
| CN101456567A (en) * | 2008-12-25 | 2009-06-17 | 中国计量学院 | Method for synthesizing high temperature stabilizing type alpha-Al2O3 nano powder |
| CN101567242A (en) * | 2009-02-10 | 2009-10-28 | 武汉理工大学 | Method for preparing magnetic nano composite particles of FeCr alloy dispersed in ceramic crystal grain |
Non-Patent Citations (2)
| Title |
|---|
| 史桂梅: "溶胶-凝胶法Al2O3纳米粉体的制备及表征", 《沈阳工业大学学报》 * |
| 杨辉等: "透明氧化铝薄膜的疏水性能研究", 《稀有金属材料与工程》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102443792A (en) * | 2011-12-02 | 2012-05-09 | 西安理工大学 | Low-fluorine solution deposition and heat treatment process of YBCO (Yttrium Barium Copper Oxide) superconducting thin film |
| CN102618871A (en) * | 2012-02-14 | 2012-08-01 | 中国科学院电工研究所 | Method for preparing tritium resistance Er2O3 coating by using chemical solution method |
| CN103993277A (en) * | 2014-05-22 | 2014-08-20 | 赵遵成 | Preparation method of template suitable for growing REBCO superconducting layer on metal baseband |
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Application publication date: 20111116 |