CN103993277A - Preparation method of template suitable for growing REBCO superconducting layer on metal baseband - Google Patents
Preparation method of template suitable for growing REBCO superconducting layer on metal baseband Download PDFInfo
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- CN103993277A CN103993277A CN201410217749.1A CN201410217749A CN103993277A CN 103993277 A CN103993277 A CN 103993277A CN 201410217749 A CN201410217749 A CN 201410217749A CN 103993277 A CN103993277 A CN 103993277A
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Abstract
The invention relates to a preparation method of a template suitable for growing a REBCO superconducting layer on a metal baseband, belonging to the technical field of preparation of high-temperature superconducting materials. The method comprises the following steps: (1) cleaning the surface of the metal baseband; (2) preparing an isolating layer on the metal baseband by a chemical solution flattening process (SDP); (3) preparing a biaxial-structure magnesium oxide layer on the isolating layer by an ion beam assisted radio-frequency magnetron sputtering process (IBAD-MgO); (4) preparing a lanthanum manganate by a radio-frequency magnetron sputtering process; and (5) preparing a cerium oxide layer by a direct-current magnetic-control reactive sputtering process. By comprehensively using the physical and chemical preparation processes, the method provides a low-cost preparation method for large-scale production of the high-temperature superconducting strip template.
Description
Technical field
The invention belongs to conductor of high-temperature superconductor coat band preparing technical field, is the method for preparing template that is applicable to the growth of REBCO superconducting layer on a kind of metal base band.
Background technology
Conductor of high-temperature superconductor coat band is one of the study hotspot in high temperature superconducting materia field, and its preparation comprises two portions: the preparation of biaxial texture base band and the preparation of superconduction functional layer.Biaxial texture base band preparation technology can be divided into two large classes: ion beam assisted deposition (Ion Beam Assisted Deposition, be abbreviated as IBAD) and the auxiliary biaxial texture technology (Rolled Assisted Biaxially Textured Substrates, is abbreviated as RABiTS) of rolling.RABiTS technology has that efficiency is high, the simple advantage of equipment, but base band is had to special requirement, now mainly uses Ni-W alloy, bad mechanical property, and cost is higher, and has magnetic, is unfavorable for applying under alternating magnetic field environment.Ion beam assisted deposition (IBAD) does not have particular requirement to the material of metal base band, can alternative costs lower Hastelloy and stainless steel are as base band material, and, the magnesian speed of ion beam assisted depositing biaxial texture is higher, lower from industrial mass production, the magnesian relative cost of ion beam assisted depositing is lower.Ion beam assisted depositing magnesium oxide requires the very smooth metal base band in surface, and polishing metal base band can adopt traditional glossing as mechanical polishing and electrochemical etching.Mechanical polishing process cost is high, efficiency is low, is unsuitable for the surface finish of the long band in flexible metal; Electrochemical etching technique is only applicable to some specific sheet metal strips, and chemical waste fluid is to environment, and treatment cost of waste liquor is higher.A kind of new ganoid method of metal base band that makes is chemical solution flattening method, it passes through at flexible metal base band surface-coated one deck oxide precursor liquid, utilize surface tension effects, few in raised areas debris, many in trench region debris, liquid film plays leveling effect as continuous integral body to base band surface; Then through Overheating Treatment, precursor liquid volatilizees, resolves into amorphous oxide film.The effect of the existing planarized surface of this amorphous oxide thin film, has again the effect of isolation atomic diffusion, is a kind of low cost process.The lattice difference of biaxial texture magnesium oxide and yttrium barium copper oxide high-temperature superconductor is larger, need on biaxial texture magnesium oxide layer, prepare buffer layer, has both kept biaxial texture, again can with superconducting layer lattice match.The present general MgO(home-epi that uses)/LMO (sputtering) multi-layer film structure is as buffer layer, the upper iso-epitaxy MgO of MgO needs hot conditions, make substrate amorphous oxides be converted into crystalline state and make surface irregularity, be unfavorable for subsequent technique, and the speed of isoepitaxial growth MgO is lower, therefore need to find the scheme that substitutes MgO (home-epi).LMO layer lattice parameter is in the middle of MgO and superconducting layer, still larger with superconducting layer lattice parameter difference, is unfavorable for the growth of superconducting layer, therefore needs to find the material more mating with superconducting layer.The invention solves the problems referred to above.
Summary of the invention
Object to be solved by this invention is to provide the low-cost method for preparing template that is applicable to the growth of REBCO superconducting layer in the base band of a kind of flexible metal, for commercial scale production conductor of high-temperature superconductor coat band.
The present invention is achieved through the following technical solutions, the present invention prepares sealing coat by chemical solution leveling method successively on metal base band, utilize ion beam assisted depositing to prepare biaxial texture magnesium oxide layer, utilize rf magnetron sputtering to prepare lanthanum manganate layer, utilize direct current reaction magnetron sputtering to prepare cerium oxide layer, obtain being applicable to the low-cost template of REBCO superconducting layer growth.
The present invention prepares the low-cost template that is applicable to the growth of REBCO superconducting layer in the base band of a kind of flexible metal, and template multi-layer film structure is shown in schematic diagram 1, and concrete preparation process comprises the following steps:
(1) metal base band surface cleaning;
(2) adopt chemical solution flattening method (SDP) on metal base band, to prepare sealing coat;
(3) adopt Assisted by Ion Beam radio frequency magnetron sputtering method (IBAD-MgO) on sealing coat, to prepare biaxial texture magnesium oxide layer;
(4) adopt radio frequency magnetron sputtering method on biaxial texture magnesium oxide layer, to prepare lanthanum manganate layer;
(5) adopt DC magnetron reactive sputtering method on lanthanum manganate layer, to prepare cerium oxide layer;
Step (1) adopts our patent equipment (a kind of flexible metal strip surface rapid chemical solution flattening device), and Fig. 2 is shown in by schematic diagram, clean metal strip surface dirt.
Step (2) adopts our patent equipment, a kind of flexible metal strip surface rapid chemical solution flattening device, by continuous tape transport, ladder heating, hyperchannel, repeat plated film and prepare sealing coat, coating speed and surface smoothness have greatly been improved, can prepare amorphous yttrium aluminum oxide or yttrium oxide that surface average roughness is less than 2 nanometers, guarantee subsequent oxidation magnesium quick forming core under ion beam assisted depositing, generate biaxial texture.The amorphous oxides sealing coat of preparation is thicker, and general 800-1300 nanometer, guarantees to be diffused into superconducting layer under barrier metal atoms high temperature.
Step is utilized hyperchannel equipment for Ion Beam Assisted Deposition in (3), see schematic diagram 3, adopt rf magnetron sputtering magnesium oxide target, argon ion at a certain angle auxiliary bombardment is prepared biaxial texture magnesia film, magnesia film thickness range 8-25 nanometer, preparation speed is higher.
Step (4) adopts multi-path-apparatus rf magnetron sputtering lanthanum manganate target, prepares lanthanum manganate film, oxygen pressure scope 0.05-10Pa, and base band Heating temperature scope 650-750 degree, thickness range 40-80 nanometer, preparation speed is higher.
Step (5) adopts multi-path-apparatus DC reactive sputtering to prepare cerium oxide, oxygen pressure scope 0.1-20Pa, base band Heating temperature scope 650-750 degree, thickness range 20-80 nanometer, preparation speed is higher, and cerium oxide is thicker, texture degree is higher, is more conducive to the growth of high-performance superconducting layer.
In the present invention, separation layer thickness is larger, the preparation of employing chemical process, do not need vacuum, and preparation speed is larger, can greatly reduce costs, IBAD-MgO layer and buffer layer (comprising lanthanum manganate layer and cerium oxide layer) desired thickness is less, adopts vacuum preparation, the speed of growth is larger, and relative cost reduces greatly.The present invention is a kind of low-cost method for preparing template of the REBCO of being suitable for superconducting layer growth.
Accompanying drawing explanation
For technical scheme of the present invention and embodiment are clearly described, will the accompanying drawing of required use in invention technical description and embodiment be briefly introduced below.
Fig. 1 is the low-cost template multi-layer film structure schematic diagram that is suitable for the growth of REBCO superconducting layer.
Fig. 2 is continuous tape transport, ladder heating, hyperchannel repetition filming equipment schematic diagram.
Fig. 3 is hyperchannel equipment for Ion Beam Assisted Deposition schematic diagram.
Embodiment
The present embodiment be take technical solution of the present invention and is implemented as prerequisite, provided detailed embodiment and concrete operation steps, but protection scope of the present invention is not limited to following embodiment.
Embodiment mono-: on Hastelloy C alloys-276, be suitable for the preparation of the low-cost template multilayer film of REBCO superconducting layer growth, comprise the steps:
(1) preparation precursor liquid 1: aluminum nitrate and alcohol solvent are dissolved by predetermined proportion, use ultrasonic oscillation to accelerate to dissolve, until completely dissolved, add a certain proportion of acetic acid yttrium, be stirred and heated to 60 degree and accelerate to dissolve, then add and add again ethanol, make in precursor liquid 1, aluminum ion is 1:1 with the ratio of ruthenium ion concentration, and aluminium ion concentration is 0.1mol/l.
(2) metal base band acetone cleans: by installing flexible metal band shown in Fig. 2,1800 milliliters of acetone are poured into respectively shown in Fig. 2 in 3 liquid baths, guarantee to flood sheet metal strip, three liquid baths are inserted in the ultrasonic container being filled with water, ultrasonic device work, make simultaneously sheet metal strip with the speed order of 40 ms/h through three acetone liquid baths.The work of coming and going 3 times.
(3) metal base band ethanol cleans: three liquid baths in step (2) are changed to ethanol, ultrasonic device work, sheet metal strip with the speed order of 60 ms/h through three ethanol liquid baths.The work of coming and going 3 times, opens tube furnace for the last time, and A, B, tri-sections of temperature of C are all set as 250 degree.
(4) apply also thermal treatment precursor liquid 1: in 3 liquid baths shown in Fig. 2, contain respectively 600 milliliters of precursor liquids 1, the temperature difference of first opening 2,4,6, three warm areas of tube furnace equates, be 10 degree, setting C district temperature is 580 degree, and sheet metal strip passes through liquid bath with the speed of 60 ms/h, then heating.After metal base band is covered to the right, then walk left, now close 2,4,6 tube furnaces, open 1,3,5 tube furnaces, the temperature difference of three warm areas equates, is 10 degree, and setting C district temperature is 580 degree, sheet metal strip with the speed of 60 ms/h through liquid bath, then heating.Repeat 2 times like this, surfaceness is 1.0 nanometers.
(5) utilize hyperchannel equipment for Ion Beam Assisted Deposition, adopt rf magnetron sputtering magnesium oxide target, argon ion at a certain angle auxiliary bombardment is prepared biaxial texture magnesia film, and the thickness that makes biaxial texture magnesium oxide layer is 12 nanometers.
(6) adopt multi-path-apparatus rf magnetron sputtering lanthanum manganate target, prepare lanthanum manganate film, oxygen pressure 0.5Pa, base band Heating temperature 700 degree, thickness 60 nanometers.
(7) adopt multi-path-apparatus DC reactive sputtering to prepare cerium oxide, oxygen pressure 5Pa, base band Heating temperature 680 degree, thickness 40 nanometers.
Finally obtain being suitable for the low-cost multilayer film template of REBCO superconducting layer growth.
Embodiment bis-: on Hastelloy C alloys-276, be suitable for the preparation of the low-cost multilayer film template of REBCO superconducting layer growth, comprise the steps:
(1) preparation precursor liquid 1: aluminum nitrate and alcohol solvent are dissolved by predetermined proportion, use ultrasonic oscillation to accelerate to dissolve, until completely dissolved, add a certain proportion of acetic acid yttrium, be stirred and heated to 60 degree and accelerate to dissolve, then add and add again ethanol, make in precursor liquid 1, aluminum ion is 1:1 with the ratio of ruthenium ion concentration, and aluminium ion concentration is 0.2mol/l.
(2) metal base band acetone cleans: by installing flexible metal band shown in Fig. 2,1800 milliliters of acetone are poured into respectively shown in Fig. 2 in 3 liquid baths, guarantee to flood sheet metal strip, three liquid baths are inserted in the ultrasonic container being filled with water, ultrasonic device work, make simultaneously sheet metal strip with the speed order of 40 ms/h through three acetone liquid baths.The work of coming and going 3 times.
(3) metal base band ethanol cleans: three liquid baths in step (2) are changed to ethanol, ultrasonic device work, sheet metal strip with the speed order of 50 ms/h through three ethanol liquid baths.The work of coming and going 3 times, opens tube furnace for the last time, and A, B, tri-sections of temperature of C are all set as 240 degree.
(4) apply also thermal treatment precursor liquid 1: in 3 liquid baths shown in Fig. 2, contain respectively 600 milliliters of precursor liquids 1, the temperature difference of first opening 2,4,6, three warm areas of tube furnace equates, be 10 degree, setting C district temperature is 570 degree, and sheet metal strip passes through liquid bath with the speed of 50 ms/h, then heating.After metal base band is covered to the right, then walk left, now close 2,4,6 tube furnaces, open 1,3,5 tube furnaces, the temperature difference of three warm areas equates, is 10 degree, and setting C district temperature is 570 degree, sheet metal strip with the speed of 50 ms/h through liquid bath, then heating.Repeat 3 times like this, surfaceness is 0.8 nanometer.
(5) utilize hyperchannel equipment for Ion Beam Assisted Deposition, adopt rf magnetron sputtering magnesium oxide target, argon ion at a certain angle auxiliary bombardment is prepared biaxial texture magnesia film, and the thickness that makes biaxial texture magnesium oxide layer is 16 nanometers.
(6) adopt multi-path-apparatus rf magnetron sputtering lanthanum manganate target, prepare lanthanum manganate film, oxygen pressure 0.1Pa, base band Heating temperature 710 degree, thickness 50 nanometers.
(7) adopt multi-path-apparatus DC reactive sputtering to prepare cerium oxide, oxygen pressure 10Pa, base band Heating temperature 690 degree, thickness 60 nanometers.
Finally obtain being suitable for the low-cost multilayer film template of REBCO superconducting layer growth.
Claims (10)
1. a method for preparing template that is applicable to the growth of REBCO superconducting layer on metal base band, is characterized in that, the method comprises the following steps:
(1) metal base band surface cleaning;
(2) adopt chemical solution flattening method (SDP) on metal base band, to prepare sealing coat;
(3) adopt Assisted by Ion Beam radio frequency magnetron sputtering method (IBAD-MgO) on sealing coat, to prepare biaxial texture magnesium oxide layer;
(4) adopt radio frequency magnetron sputtering method on biaxial texture magnesium oxide layer, to prepare lanthanum manganate layer;
(5) adopt DC magnetron reactive sputtering method on lanthanum manganate layer, to prepare cerium oxide layer.
2. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that adopting our patent equipment in described step (1), a kind of flexible metal strip surface rapid chemical solution flattening device clean metal base band is surperficial; Step (2) adopts same equipment, and tape transport, ladder heating, hyperchannel repeat chemical solution leveling method and prepare amorphous oxides multilayer film as sealing coat continuously, thickness range 800-1500 nanometer, and surface average roughness is less than 2 nanometers.
3. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that utilizing hyperchannel equipment for Ion Beam Assisted Deposition in described step (3), adopt rf magnetron sputtering magnesium oxide, biaxial texture magnesia film is prepared in the auxiliary bombardment of argon ion.
4. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that the biaxial texture magnesia film thickness range 8-25 nanometer of preparation in described step (3).
5. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that described step (4) adopts multi-path-apparatus, rf magnetron sputtering is prepared lanthanum manganate film, base band Heating temperature scope 650-750 degree.
6. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that described step (4) adopts multi-path-apparatus, rf magnetron sputtering is prepared lanthanum manganate film, oxygen pressure scope 0.05-10Pa.
7. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that described step (4) adopts multi-path-apparatus, rf magnetron sputtering is prepared lanthanum manganate film, thickness range 40-80 nanometer.
8. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that described step (5) adopts multi-path-apparatus, DC reactive sputtering is prepared cerium oxide, base band Heating temperature scope 650-750 degree.
9. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that described step (5) adopts multi-path-apparatus, DC reactive sputtering is prepared cerium oxide, oxygen pressure scope 0.1-20Pa.
10. on a kind of metal base band as claimed in claim 1, be applicable to the method for preparing template of REBCO superconducting layer growth, it is characterized in that described step (5) adopts multi-path-apparatus, DC reactive sputtering is prepared cerium oxide, thickness range 20-80 nanometer.
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