CN103993277B - It is suitable for the method for preparing template of REBCO superconducting layer growth on metal base band - Google Patents
It is suitable for the method for preparing template of REBCO superconducting layer growth on metal base band Download PDFInfo
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- CN103993277B CN103993277B CN201410217749.1A CN201410217749A CN103993277B CN 103993277 B CN103993277 B CN 103993277B CN 201410217749 A CN201410217749 A CN 201410217749A CN 103993277 B CN103993277 B CN 103993277B
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Abstract
The present invention is the method for preparing template for being suitable for the growth of REBCO superconducting layer on a kind of metal base band, belongs to high temperature superconducting materia preparation technical field.The present invention is the following steps are included: (1) metal base band surface clean；(2) separation layer is prepared on metal base band using chemical solution flattening method (SDP)；(3) biaxial texture magnesium oxide layer is prepared on separation layer using Assisted by Ion Beam radio frequency magnetron sputtering method (IBAD-MgO)；(4) lanthanum manganate layer is prepared using radio frequency magnetron sputtering method；(5) cerium oxide layer is prepared using DC magnetron reactive sputtering method.The present invention passes through the integrated application of physics and chemical preparation process, provides a kind of low cost preparation method for large-scale production high-temperature superconductor band template.
Description
Technical field
It the invention belongs to conductor of high-temperature superconductor coat band preparation technical field, is suitable on a kind of metal base band
The method for preparing template of REBCO superconducting layer growth.
Background technique
Conductor of high-temperature superconductor coat band is one of the research hotspot in high temperature superconducting materia field, its preparation includes two
Point: the preparation of biaxial texture base band and the preparation of superconduction functional layer.Biaxial texture base band preparation process can be divided into two major classes: ion beam is auxiliary
Help deposition technique (Ion Beam Assisted Deposition, be abbreviated as IBAD) and rolling auxiliary biaxial texture technology
(Rolled Assisted Biaxially Textured Substrates, be abbreviated as RABiTS).RABiTS technology has
Advantage high-efficient, equipment is simple, but have special requirement to base band, primarily now uses Ni-W alloy, bad mechanical property, at
This is higher, and has magnetism, is unfavorable for applying under alternating magnetic field environment.Ion beam assisted deposition (IBAD) is to Metal Substrate
The material of band does not have particular/special requirement, can choose lower-cost Hastelloy and stainless steel as based belt material, moreover, ion
The speed of beam assistant depositing biaxial texture magnesia is higher, from industrial mass production it is lower for, ion beam assisted depositing oxygen
Change being of relatively low cost for magnesium.The metal base band that ion beam assisted depositing magnesia requires surface very smooth, polishing metal base
Band can be using traditional polishing process such as mechanical polishing and electrochemical polish.Mechanical polishing process is at high cost, low efficiency, uncomfortable
In the surface polishing of the long band in flexible metal；Electrochemical polishing process is suitable only for some specific sheet metal strips, and chemical waste fluid
It pollutes the environment, treatment cost of waste liquor is higher.A kind of new method for keeping metal base band surface smooth is that chemical solution is flat
Smoothization method, it is by coating one layer of oxide precursor liquid on flexible metal base band surface, using surface tension effects, in protrusion
Region Liquid Residue is few, more in trench region Liquid Residue, and liquid film plays the role of planarizing to base band surface as continuous entirety；So
By Overheating Treatment, amorphous oxide film is resolved into precursor liquid volatilization.This existing planarization surface of amorphous oxide thin film
Effect, and have the function of that atom diffusion is isolated, it is a kind of low cost process.Biaxial texture magnesia and yttrium barium copper oxide high temperature are super
The lattice differences of conductor are larger, need to prepare buffer layer on biaxial texture magnesium oxide layer, not only keep biaxial texture, but can with it is super
Conducting shell Lattice Matching.Typically now use MgO(home-epi)/LMO (sputtering) multi-layer film structure is as buffer layer, MgO
Upper homoepitaxy MgO needs hot conditions, and substrate amorphous oxides is made to be converted into crystalline state and make rough surface, is unfavorable for subsequent work
Skill, and the speed of isoepitaxial growth MgO is lower, it is therefore desirable to find the scheme of substitution MgO (home-epi).LMO layer crystal
Lattice constant is but larger with superconduction layer lattice constant difference among MgO and superconducting layer, is unfavorable for the growth of superconducting layer, because
This needs to find and the more matched material of superconducting layer.The present invention solves the above problem.
Summary of the invention
Purpose to be solved by this invention, which is to provide, is suitable for the low of REBCO superconducting layer growth in a kind of flexible metal base band
Cost template preparation method is used for industrial-scale production conductor of high-temperature superconductor coat band.
The invention is realized by the following technical scheme, and the present invention passes sequentially through chemical solution leveling method in metal base band
On prepare separation layer, prepare biaxial texture magnesium oxide layer using ion beam assisted depositing, prepare mangaic acid using rf magnetron sputtering
Lanthanum layer prepares cerium oxide layer using direct current reaction magnetron sputtering, obtains the low cost template for being suitable for the growth of REBCO superconducting layer.
The present invention prepares the low cost template for being suitable for the growth of REBCO superconducting layer in a kind of flexible metal base band, and template is more
Film structure is shown in schematic diagram 1, specific preparation process the following steps are included:
(1) metal base band surface clean；
(2) separation layer is prepared on metal base band using chemical solution flattening method (SDP)；
(3) biaxial texture oxidation is prepared on separation layer using Assisted by Ion Beam radio frequency magnetron sputtering method (IBAD-MgO)
Magnesium layer；
(4) lanthanum manganate layer is prepared on biaxial texture magnesium oxide layer using radio frequency magnetron sputtering method；
(5) cerium oxide layer is prepared on lanthanum manganate layer using DC magnetron reactive sputtering method；
Step (1) is using a kind of (the flexible metal strip surface rapid chemical solution planarization of our own patent equipment
Equipment), schematic diagram is shown in Fig. 2, cleans sheet metal strip surface dirt.
Step (2) uses our own patent equipment, a kind of flexible metal strip surface rapid chemical solution planarization
Equipment repeats plating film preparation separation layer by continuous tape transport, ladder heating, multichannel, substantially increases coating speed and surface
Finish can prepare amorphous yttrium aluminum oxide or yttrium oxide of the surface average roughness less than 2 nanometers, guarantee subsequent oxidation
Magnesium quick forming core under ion beam assisted depositing generates biaxial texture.The amorphous oxides separation layer of preparation is thicker, general 800-
1300 nanometers, guarantee to be diffused into superconducting layer under barrier metal atoms high temperature.
Multichannel equipment for Ion Beam Assisted Deposition is utilized in step (3), is seen schematic diagram 3, is aoxidized using rf magnetron sputtering
Magnesium target, argon ion assist bombardment to prepare biaxial texture magnesia film, magnesia film thickness range 8-25 at a certain angle
Nanometer, preparation speed are higher.
Step (4) uses multi-path-apparatus rf magnetron sputtering lanthanum manganate target, prepares mangaic acid lanthanum film, oxygen pressure model
0.05-10Pa is enclosed, base band heating temperature range 650-750 degree, 40-80 nanometers of thickness range, preparation speed is higher.
Step (5) prepares cerium oxide, oxygen pressure range 0.1-20Pa, base band using multi-path-apparatus DC reactive sputtering
Heating temperature range 650-750 degree, 20-80 nanometers of thickness range, preparation speed is higher, and cerium oxide is thicker, and texture degree is higher,
More be conducive to the growth of high performance superconductor layer.
Separation layer thickness is larger in the present invention, is prepared using chemical method, does not need vacuum, and preparation speed is larger,
Cost can be substantially reduced, it is IBAD-MgO layers smaller with buffer layer (including lanthanum manganate layer and cerium oxide layer) required thickness, it uses
Vacuum preparation, the speed of growth is larger, and relative cost substantially reduces.The present invention be it is a kind of be suitable for REBCO superconducting layer growth it is low
Cost template preparation method.
Detailed description of the invention
It, below will be in inventive technique description and embodiment in order to clearly illustrate technical solution of the present invention and embodiment
The required attached drawing used is briefly introduced.
Fig. 1 is the low cost template multi-layer film structure schematic diagram for being suitable for the growth of REBCO superconducting layer.
Fig. 2 is continuous tape transport, ladder heating, multichannel repetition filming equipment schematic diagram.
Fig. 3 is multichannel equipment for Ion Beam Assisted Deposition schematic diagram.
Specific embodiment
The present embodiment is implemented premised on technical solution of the present invention, gives detailed embodiment and specific behaviour
Make step, but protection scope of the present invention is not limited to following embodiments.
Embodiment one: it is suitable for the system of the low cost template multilayer film of REBCO superconducting layer growth on Hastelloy C alloys -276
It is standby, include the following steps:
(1) it prepares precursor liquid 1: aluminum nitrate and alcohol solvent being dissolved by predetermined ratio, accelerated using ultrasonic oscillation molten
Solution, until completely dissolved, is added a certain proportion of acetic acid yttrium, is stirred and heated to 60 degree of quickening dissolutions, is then added and adds second
Alcohol makes in precursor liquid 1, and the ratio between aluminium ion and ruthenium ion concentration are 1:1, aluminium ion concentration 0.1mol/l.
(2) metal base band acetone cleans: installing flexible metal strip as shown in Figure 2,1800 milliliters of acetone are fallen respectively
Enter in 3 liquid baths shown in Fig. 2, guarantees to flood sheet metal strip, three liquid baths are placed in the ultrasonic container being filled with water, ultrasonic device work
Make, while making sheet metal strip with 40 ms/h of speed order by three acetone liquid baths.Round-trip work 3 times.
(3) metal base band ethyl alcohol cleans: three liquid baths in step (2) are changed to ethyl alcohol, ultrasonic device work, sheet metal strip
Pass through three ethyl alcohol liquid baths with 60 ms/h of speed order.Round-trip work 3 times, for the last time opens tube furnace, A, B, C
Three sections of temperature are set to 250 degree.
(4) it coats and is heat-treated precursor liquid 1: containing 600 milliliters of precursor liquids 1 respectively in 3 liquid baths shown in Fig. 2, first open
Open tube furnace 2,4,6, it is 10 degree that the temperature difference of three warm areas is equal, set the area C temperature as 580 degree, sheet metal strip with 60 meters/it is small
When speed pass through liquid bath, then heat.It after metal base band is covered to the right, then walks to the left, closes 2,4,6 tube furnaces at this time, open
Open 1,3,5 tube furnaces, it is 10 degree that the temperature difference of three warm areas is equal, set the area C temperature as 580 degree, sheet metal strip with 60 meters/it is small
When speed pass through liquid bath, then heat.It is repeated 2 times in this way, surface roughness is 1.0 nanometers.
(5) multichannel equipment for Ion Beam Assisted Deposition is utilized, using rf magnetron sputtering magnesium oxide target, argon ion is with one
Determine angle auxiliary bombardment prepare biaxial texture magnesia film, be made biaxial texture magnesium oxide layer with a thickness of 12 nanometers.
(6) multi-path-apparatus rf magnetron sputtering lanthanum manganate target is used, prepares mangaic acid lanthanum film, oxygen pressure 0.5Pa,
700 degree of base band heating temperature, 60 nanometers of film thickness.
(7) cerium oxide, oxygen pressure 5Pa, base band heating temperature 680 are prepared using multi-path-apparatus DC reactive sputtering
Degree, 40 nanometers of thickness.
Finally obtain the inexpensive multilayer film template for being suitable for the growth of REBCO superconducting layer.
Embodiment two: it is suitable for the system of the inexpensive multilayer film template of REBCO superconducting layer growth on Hastelloy C alloys -276
It is standby, include the following steps:
(1) it prepares precursor liquid 1: aluminum nitrate and alcohol solvent being dissolved by predetermined ratio, accelerated using ultrasonic oscillation molten
Solution, until completely dissolved, is added a certain proportion of acetic acid yttrium, is stirred and heated to 60 degree of quickening dissolutions, is then added and adds second
Alcohol makes in precursor liquid 1, and the ratio between aluminium ion and ruthenium ion concentration are 1:1, aluminium ion concentration 0.2mol/l.
(2) metal base band acetone cleans: installing flexible metal strip as shown in Figure 2,1800 milliliters of acetone are fallen respectively
Enter in 3 liquid baths shown in Fig. 2, guarantees to flood sheet metal strip, three liquid baths are placed in the ultrasonic container being filled with water, ultrasonic device work
Make, while making sheet metal strip with 40 ms/h of speed order by three acetone liquid baths.Round-trip work 3 times.
(3) metal base band ethyl alcohol cleans: three liquid baths in step (2) are changed to ethyl alcohol, ultrasonic device work, sheet metal strip
Pass through three ethyl alcohol liquid baths with 50 ms/h of speed order.Round-trip work 3 times, for the last time opens tube furnace, A, B, C
Three sections of temperature are set to 240 degree.
(4) it coats and is heat-treated precursor liquid 1: containing 600 milliliters of precursor liquids 1 respectively in 3 liquid baths shown in Fig. 2, first open
Open tube furnace 2,4,6, it is 10 degree that the temperature difference of three warm areas is equal, set the area C temperature as 570 degree, sheet metal strip with 50 meters/it is small
When speed pass through liquid bath, then heat.It after metal base band is covered to the right, then walks to the left, closes 2,4,6 tube furnaces at this time, open
Open 1,3,5 tube furnaces, it is 10 degree that the temperature difference of three warm areas is equal, set the area C temperature as 570 degree, sheet metal strip with 50 meters/it is small
When speed pass through liquid bath, then heat.It is repeated 3 times in this way, surface roughness is 0.8 nanometer.
(5) multichannel equipment for Ion Beam Assisted Deposition is utilized, using rf magnetron sputtering magnesium oxide target, argon ion is with one
Determine angle auxiliary bombardment prepare biaxial texture magnesia film, be made biaxial texture magnesium oxide layer with a thickness of 16 nanometers.
(6) multi-path-apparatus rf magnetron sputtering lanthanum manganate target is used, prepares mangaic acid lanthanum film, oxygen pressure 0.1Pa,
710 degree of base band heating temperature, 50 nanometers of film thickness.
(7) cerium oxide, oxygen pressure 10Pa, base band heating temperature 690 are prepared using multi-path-apparatus DC reactive sputtering
Degree, 60 nanometers of thickness.
Finally obtain the inexpensive multilayer film template for being suitable for the growth of REBCO superconducting layer.
Claims (6)
1. being suitable for the method for preparing template of REBCO superconducting layer growth on a kind of metal base band, which is characterized in that this method includes
Following steps:
(1) metal base band surface clean is first cleaned with acetone, after cleaned with ethyl alcohol；
(2) separation layer is prepared on metal base band using chemical solution flattening method (SDP), is added by continuous tape transport, ladder
Heat, multichannel repeat chemical solution leveling method and prepare amorphous oxides multilayer film as separation layer, thickness range 800-
1500 nanometers, surface average roughness is less than 2 nanometers；
(3) biaxial texture magnesia is prepared on separation layer using Assisted by Ion Beam radio frequency magnetron sputtering method (IBAD-MgO)
Layer；
(4) lanthanum manganate layer is prepared on biaxial texture magnesium oxide layer using radio frequency magnetron sputtering method, is penetrated using multi-path-apparatus
Frequency magnetron sputtering lanthanum manganate target prepares mangaic acid lanthanum film, oxygen pressure range 0.05-10Pa, base band heating temperature range
650-750 degree；
(5) cerium oxide layer is prepared on lanthanum manganate layer using DC magnetron reactive sputtering method, it is anti-using multi-path-apparatus direct current
It should sputter and prepare cerium oxide, oxygen pressure range 0.1-20Pa, base band heating temperature range 650-750 degree.
2. it is suitable for the method for preparing template of REBCO superconducting layer growth on a kind of metal base band as described in claim 1, it is special
Sign is to clean metal tape using a kind of flexible metal strip surface rapid chemical solution flattening device in the step (1)
Material surface.
3. it is suitable for the method for preparing template of REBCO superconducting layer growth on a kind of metal base band as described in claim 1, it is special
Sign is to utilize multichannel equipment for Ion Beam Assisted Deposition in the step (3), using rf magnetron sputtering magnesia, argon from
Son auxiliary bombardment prepares biaxial texture magnesia film.
4. it is suitable for the method for preparing template of REBCO superconducting layer growth on a kind of metal base band as described in claim 1, it is special
Sign is 8-25 nanometers of the biaxial texture magnesia film thickness range prepared in the step (3).
5. it is suitable for the method for preparing template of REBCO superconducting layer growth on a kind of metal base band as described in claim 1, it is special
Sign is the step (4) using multi-path-apparatus, and rf magnetron sputtering prepares mangaic acid lanthanum film, and thickness range 40-80 receives
Rice.
6. it is suitable for the method for preparing template of REBCO superconducting layer growth on a kind of metal base band as described in claim 1, it is special
Sign is the step (5) using multi-path-apparatus, and DC reactive sputtering prepares cerium oxide, 20-80 nanometers of thickness range.
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| CN103255369A (en) * | 2013-06-07 | 2013-08-21 | 上海超导科技股份有限公司 | Simplified baffle layer suitable for IBAD-MgO (ion beam assisted deposition-magnesium oxide) growth on metal substrate and preparation method thereof |
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| CN100365839C (en) * | 2003-12-15 | 2008-01-30 | 北京有色金属研究总院 | Multilayer biaxial orienting insulation layer structure and high-temperature superconductive coating conductor and preparing method thereof |
| US8809237B2 (en) * | 2008-02-19 | 2014-08-19 | Superpower, Inc. | Method of forming an HTS article |
| US8748349B2 (en) * | 2011-04-15 | 2014-06-10 | Ut-Battelle, Llc | Buffer layers for REBCO films for use in superconducting devices |
| CN102306702B (en) * | 2011-05-31 | 2013-06-05 | 上海超导科技股份有限公司 | Method suitable for continuously preparing high-temperature superconductive belt material |
| CN102242357A (en) * | 2011-06-24 | 2011-11-16 | 中国科学院电工研究所 | Method for preparing YBCO (Yttrium Barium Copper Oxide) coating conductor barrier layer |
| CN103695859B (en) * | 2013-12-11 | 2016-01-13 | 电子科技大学 | The two-sided LaMnO of superconducting tape 3the preparation method of buffer layer |
| CN103985479B (en) * | 2014-04-28 | 2018-03-30 | 赵遵成 | A kind of preparation method of conductor of high-temperature superconductor coat band |
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| CN103255369A (en) * | 2013-06-07 | 2013-08-21 | 上海超导科技股份有限公司 | Simplified baffle layer suitable for IBAD-MgO (ion beam assisted deposition-magnesium oxide) growth on metal substrate and preparation method thereof |
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| 溶液沉积平整化法优化金属基带表面平整度的工艺研究;程崛;《中国优秀硕士学位论文全文数据库 工程科技Ⅱ辑》;20140115(第01期);第20-23、35-36、44-46页 * |
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